* I .> / Class Book _ M 5^2. . Gcpightlf_ \ Q 7.^ COPYRIGHT DEPOSIT* EXPERIMENTS IN PRACTICAL CHEMISTRY TO ACCOMPANY NEWELL’S PRACTICAL CHEMISTRY BY LYMAN C. NEWELL, Ph.D. (johns hopkins) PROFESSOR OF CHEMISTRY, BOSTON UNIVERSITY, BOSTON, MASS. AUTHOR OF “EXPERIMENTAL CHEMISTRY,” “DESCRIPTIVE CHEMISTRY,” “GENERAL CHEMISTRY,” “INORGANIC CHEMISTRY FOR COLLEGES,” “LABO¬ RATORY MANUAL OF INORGANIC CHEMISTRY,” “COLLEGE CHEMISTRY,” “EXPERIMENTS IN COLLEGE CHEMISTRY,” “PRACTICAL CHEMISTRY,” “brief COURSE IN CHEMISTRY,” “LABORATORY EXERCISES FOR A BRIEF COURSE IN CHEMISTRY” REVISED EDITION Part II D. C. HEATH AND COMPANY BOSTON NEW YORK CHICAGO ATLANTA SAN ERANCISCO DALLAS LONDON i?**- I?8 '*■ This book is the experimental part of the author’s textbook entitled Practical Chemistry. These experiments are essential for teaching the fundamental facts and principles of chemistry. Many practical experiments are included. The experiments vary in length, difficulty, and application. There are more experiments than a class can do in a year of chemistry. Teachers should select experiments which provide a course adapted to their require¬ ments. Ample material is available for different courses — practical, fun¬ damental with practical applications, college preparatory, short, and long. The directions for performing the early experiments are rather full. In the quantitative experiments, besides detailed directions, the object is stated and the calculation is indicated or illustrated. The apparatus for the pupil’s experiments is simple. Many parts are interchangeable, and several types of apparatus are shown. The quantities of chemicals have been carefully chosen, and, as a rule, the chemicals are the less expensive ones. The Appendix contains lists of apparatus and chem¬ icals. The Demonstration Experiments are intended for use in the class¬ room. The apparatus for these experiments is in List C in the Appendix. The Introduction contains general laboratory directions. The direc¬ tions for weighing (§ 8) are given in detail. The author is indebted to many teachers for advice, especially to his as¬ sociates in the chemistry department of Boston University. He is under special obligation to Mr. Harold C. Spencer, Boston University, 1914, for making the drawings. L. C. N. January, 1923 PREFACE TO REVISED EDITION Several experiments have been revised and minor corrections made in this edition. L. C. N. April, 1929 Copyright, 1923, 1929, By Lyman C. Newell. 2H9 Printed in U. S. A. OCT 11 I9?9 ©CIA 14099 CONTENTS Numbers indicate experiments. College preparatory experiments are marked (C) — (C*) recommended, demonstration experiments (D), and quantitative experiments (Q). PAGE Introduction .i General directions — Bunsen burner — Cutting and bending glass tubing — Filtering — Constructing and arranging appa¬ ratus — Pouring liquids and transferring solids — Collecting gases — Weighing — Measuring — Smelling and tasting — Accidents Chemical Change — Compounds — Elements . . .13 1. Chemical Change (C) — 2. Properties and Chemical Change (C*) —3. Mixture and Compound (C) — 4. Compound and Elements (C*) Oxygen.16 5. Preparation (Short) — 6. Preparation and Properties (C*) — 7. Oxidation of Copper (C) — 8. Heating a Metal in Air (C*) (Q)—9. Rapid and Slow Oxidation (D) — 10. Air and Combustion (C*) Carbon — Carbon Dioxide — Carbon Monoxide . . 22 n. Distribution of Carbon (C) — 12. Combustion and Carbon Dioxide (C) —13. Fermentation and Carbon Dioxide (C*) (D) — 14. Preparation and Properties of Carbon Dioxide (C*) — 15. Beverages and Carbon Dioxide (D) — 16. Plants and Carbon Dioxide (D) —17. Fire Extinguishers and Carbon Dioxide (D) — 18. Carbon Monoxide (D) Hydrogen.. . . .29 19 Preparation (Short) (C) — 20. Preparation and Properties (C*) — 21. Water and Sodium (C*) (D) — 22. Burning (D) — 23. Reduction of Copper Oxide (C*) Measurement of Gases.35 24. Weight of a Liter of Oxygen (C*) (Q) 111 IV CONTENTS PAGE Water — Hydrogen Peroxide.37 25. In Food—26. Purification — 27. Distillation (C) — 28. Distillation (C) (D) — 29. Physical Properties (C) — 30. Water Vapor and Steam (C) (D) —31. Water Vapor and Pres¬ sure (D) — 32. Chemical Properties (C) — 33. Solubility of Gases (C*) — 34. Solubility of Liquids (C*) — 35. Solubility of Solids (C*) — 36. Heat and Solubility (C*) — 37. Shape and Sol¬ ubility (C*) —38. Saturated Solutions (C*) — 39. Solubility of a Given Solid (C) (Q) — 40. Crystals (C) — 41. Water of Crystal¬ lization (C*) — 42. Crystallized Copper Sulphate (C*) (Q) —- 43. Anhydrous Compounds (C) — 44. Efflorescence (C) — 45. Deliquescence (C) — 46. Efflorescence and Deliquescence (D) — 47. Supersaturation (C) — 48. Qualitative Composition (D) — 49. Electrolysis (D) — 50. Hydrogen Peroxide Laws of Constant Composition and Multiple Proportions 52 51. Constant Composition (C) (Q) — 52. Multiple Propor¬ tions (C) (Q) Nitrogen — Air ..56 53. Preparation and Properties of Nitrogen (C) — 54. Nitrogen and Ammonia — 55. Per Cent of Oxygen in Air (C*) (Q) — 56. Water Vapor in Air — 57. Carbon Dioxide in Air (C*)— - 58. Testing Air Chlorine — Hydrogen Chloride — Hydrochloric Acid . 60 59. Preparation and Properties of Chlorine (Short) (C*) — 60. Preparation and Properties of Chlorine (Long) (C*) — 61. Electrolysis of Sodium Chloride (D) — 62. Chlorine Water — 63. Bleaching (C) — 64. Hydrogen Chloride (C*) —- 65. Hydrogen Chloride and Hydrochloric Acid (C*) — 66. Tests (C) — 67. Aqua Regia — 68. Insoluble Chlorides (C*) Acids, Bases, and Salts — Neutralization ... 67 69. Acids (C) — 70. Bases (C) — 71. Salts (C)—-72. Com¬ position — 73. Testing for Acids and Basis — 74. Neutraliza¬ tion (C*) — 75. Neutralization (C*) (Q) — 76. Preparation of a Salt (C*) Ammonia — Ammonium Compounds.72 77. Ammonia and Ammonium Hydroxide (C*) — 78. Am¬ monia — 79. Ammonium Salts — 80. Testing Salts (Review) (C) CONTENTS v v PAGE Nitric Acid — Nitrates — Nitrogen Oxides 75 81. Nitric Acid (C*) — 82. Nitrates (C) — 83. Nitric Acid and Metals (C*) — 84. Test for Nitric Acid and Nitrates (C) — 85. Nitric Oxide and Nitrogen Dioxide (C*) — 86. Nitrous Oxide (C*) Molecular Weights.80 87. Weight of 22.4 Liters of Carbon Dioxide (C) (Q) Equivalent Weights.82 88. Zinc (to Hydrogen) (C*) (Q) — 89. Magnesium (C*) (Q) — 90- Aluminium (C) (Q) — 91. Calcium (C) — 92. Zinc (to Oxygen) (C*) (Q) — 93. Zinc (to Chlorine) (C*) (Q) Ions and Ionization . . . . . . . .8 7 94. Electrolytes and Non-electrolytes (C) (D) — 95. Chemi¬ cal Behavior of Salts (C) —■ 96. Electrolysis of Copper Sul¬ phate (Short) (D) — 97. Electrolysis of Copper Sulphate (Long) (D) — 98. Electrolysis of Sodium Sulphate (D) — 99. Electrolysis of Potassium Iodide (D) — 100. Effect of Dis¬ solved Substance on the Boiling Point (C*) — 101. Effect of Dissolved Substance on the Freezing Point (C*) — 102. Col¬ ored and Colorless Ions (C) — 103. Ionization and Concen¬ tration (D). Sulphur — Hydrogen Sulphide — Sulphides ... 93 104. Physical Properties — 105. Chemical Properties — 106. Orthorhombic (Rhombic) (C*) — 107. Monoclinic (C*) —- ic8. Amorphous (C*) —109. Hydrogen Sulphide-(Short) (C*) — no. Hydrogen Sulphide (Long) (C*) — in. Sulphides (C*) Sulphur Dioxide — Sulphurous and Sulphuric Acids — Salts.98 112. Sulphur Dioxide (C*) —-113. Sulphur Dioxide and Sul¬ phurous Acid (C*) — 114. Sulphuric Acid (C) — 115. Tests (C) Carbon — Carbonic Acid — Carbonates — Oxides . . 102 116. Graphite (C*) — 117. Charcoal (C*) — 118. Testing for Carbon (C) — 119. Reduction by Carbon (C) — 120. Car¬ bonic Acid (D) — 121. Carbonates (D) — 122. Testing for Carbonates—123. Carbon Monoxide (C*) (D) Fuels — Illuminating Gas — Flame.106 124. Composition—125. Analysis of Coal (Q) — 126. Gaso¬ lene (C)—127. Kerosene —128. Davy Safety Lamp (C) — 129. Coal Gas — 130. Testing Illuminating Gas — VI CONTENTS page 131. Gas Flame— 132. Candle Flame—133. Bunsen Burner and Flame (C) —134. Reduction and Oxidation with the Blowpipe (C) — 135. Testing for Metals and Non-metals Other Carbon Compounds.116 136. Sucrose and Dextrose — 137. Starch — 138. Detection of Starch by Iodine — 139. Ethyl Alcohol — 140. Tests for Ethyl Alcohol — 141. Acetic Acid — 142. Tests for Acetic Acid and Acetates (C*) — 143. Vinegar—144. Preparation of Soap (C*) — 145. Properties of Soap (C) — 146. Carbon Tetrachloride Food and Nutrition.120 147. Nutrients -— 148. Water —- 149. Mineral Matter — 150. Bread — 151. Butter and Substitutes — 152. Milk (C*) — 153. Baking Powders (C) Silicon.125 154. Sodium Silicate — 155. Silicic Acid —156. Test for Silicon — 157. Carborundum Fluorine — Bromine — Iodine. 127 158. Etching —159. Bromine (C*)—160. Bromides (C) — 161. Iodine (C*) — 162. Tests for Free Iodine (C) — 163. Iodides -(C) — 164. Halogen Acids (C*) Phosphates — Arsenic — Antimony — Bismuth . . .131 165. Orthophosphoric Acid and Orthophosphates (C) — 166. Phosphate Fertilizer — 167. Test for Arsenic (C*) — 168. Test for Antimony (C*) — 169. Test for Bismuth — 170. Fusible Alloys Sodium — Potassium .132 171. Sodium (C*) — 172. Tests for Sodium (C) — 173. Sodium Chloride (C) — 174. Sodium Carbonate (LeBlanc Process) — 175. Hydrolysis of Sodium Carbonate — 176. Sodium Bicarbonate (C) — 177. Sodium Hydroxide — 178. Electrolysis of Sodium Chloride (D) — 179. Borax (C) — 180. Borax Beads (C) — 181. Potassium — 182. Tests for Potassium (C*) — 183. Potassium Nitrate (C*) Calcium — Strontium — Barium.137 184. Calcium Carbonate — 185. Tests for Calcium (C) — 186. Testing for Calcium — 187. Calcium Oxide and Hydrox¬ ide (C*) — 188. Mortar —189. Cement — 190. Analysis of Cement (C) (Q) — 191. Hand Water (C*) — 192. Plaster of CONTENTS Vll Paris—193. Tests for Strontium and Barium (C*) — 194. Red Fire and Green Fire (D) Iron. 195. Properties — 196. Slag — 197. Ferrous Compounds (C*) — 198. Ferric Compounds (C*) — 199. Reduction and Oxidation of Iron Compounds (C*) — 200. Hydrolysis of Ferric Chloride (C) — 201. Testing for Iron Aluminium. 202. Properties —• 203. Aluminium Hydroxide (C) — 204. Clari¬ fication of Water— S 205. Thermit (D) — 206. Tests for Alu¬ minium (C*) — 207. Alum—208. Mordants—209. Hydrolysis of Aluminium Chloride (C) Copper . 210. Properties — 211. Tests (C)—■ 212. Copper Sulphate — 213. Copper Alloys—-214. Displacement (Copper) (C*) Magnesium — Zinc — Mercury. 215. Magnesium and Zinc—216. Tests for Magnesium (C) — 217. Testing for Magnesium—218. Tests for Zinc (C) — 219. Zinc Hydroxide—220. Mercury —- 221. Mercurous and Mercuric Compounds (C) — 222. Displacement (Magnesium, Zinc, and Mercury) (C*) Tin — Lead. 223. Tin and Lead — 224. Test for Tin (C) — 225. Tests for Lead (C) — 226. White Lead — 227. Displacement (Tin and Lead) (C*) — 228. Testing for Lead — 229. Qualitative Analy¬ sis (Lead, Silver, and Mercury) (C*) Silver — Gold. 230. Tests for Silver (C) — 231. Displacement of Metals (Silver) (C*) — 232. Cleaning Silver—233. Silver Salts — 234. Photography—235. Gold. Chromium — Manganese. 236. Tests for Chromium (C) — 237. Potassium Chromate and Dichromate (C) — 238. Tests for Manganese (C) Appendix . Pressure of Water Vapor — Laboratory Equipment Index .... . PAGE 142 144 147 I48 151 153 155 158 165 Frontispiece Fig. I. — Apparatus frequently used in the laboratory EXPERIMENTS IN PRACTICAL CHEMISTRY INTRODUCTION 1 . General directions for the pupil. — The apparatus you will use frequently is shown on the opposite page. The pieces are lettered as follows: — A — Thistle tube. B — Test tube holder. C — Glass plate. D — Pinch clamp. E — Glass tube. F — Crucible block. G — Porcelain crucible (covered). H — Triangle. I — Forceps. J — Blowpipe tube. K — Test tube brush. L — Blowpipe. M — Right-angle bend. N — Glass rod. O — Porcelain evaporating dish. P — Glass plug. Q — Mor¬ tar and pestle. R — Rubber stopper (2-hole). S — Bottle. T —De¬ flagrating spoon. U — Rubber stopper (i-hole). V — Erlenmeyer flask. W — Iron clamp. X — Wire gauze. Y — Iron ring. Z —• Iron stand. AA —'Funnel. BB — Test tube (small). CC — Test tube (large). DD — Graduated cylinder. EE — Beaker. FF — Test tube rack (shown in part). Use Fig. I in preparing a list of the apparatus in your desk. When your set of apparatus agrees with the list, hand the com¬ pleted list to the Teacher. Some general apparatus will be found in the laboratory and special apparatus will be supplied as needed. Use this apparatus as directed. Besides the apparatus in your desk, you will need a rubber apron and a pair of sleeves, or something similar, to protect your clothes. You will need a laboratory notebook. Write your name and the number of your desk on the notebook. In this book you should keep a neat and accurate account of a-11 the experiments you perform. The Teacher will give special directions for writing the notes, handing in the book, and correcting errors. In general, your record of each experiment should include: — (1) The number and title of the experiment and the date. (2) An account of the experiment — brief, but full enough to permit a correct repetition of the experiment or its essential parts. 2 EXPERIMENTS IN PRACTICAL CHEMISTRY (3) Answers to all questions — not merely yes or no, but an answer involving the question. (4) The numbers and letters which correspond to those in the directions, e.g. 1, I, (1), a, etc. (5) All numerical data, e.g. weights and volumes, in the form given in the directions. (6) A simple sketch of the apparatus (if time permits). (7) A table of contents. To do experiments successfully, you must meet certain require¬ ments. Before the laboratory period find out what experiment is to be done, read the directions carefully, and plan the work as well as you can. When you enter the laboratory, open your desk at once, or have it opened, take out the necessary apparatus, and begin to work without delay. When you are doing an experiment in the laboratory, follow the directions carefully, especially about quantities of chemicals, heating, and weighing; work and think independently. If you need assistance, ask the Teacher, not your neighbor. Your work will be more profitable if you follow these suggestions : — (a) Learn as soon as possible the name of each piece of apparatus, and how to use it. ( b ) Learn how to perform skillfully the operations so frequently done in the laboratory, e.g. heating, filtering, weighing (see §§ 2, 4 ,8 below). (c) Learn how to set up apparatus, inspect it, and correct defects. (1 d ) Learn how to do arithmetical work quickly and accurately, and to check results. Before you leave the laboratory, be sure your apparatus is clean and put away, the water and the gas are turned off, and your desk is in just as good order as you would like to find it. 2 . How to use the Bunsen burner. — The Bunsen burner (Fig. II) is used as a source of heat. It is attached to a rubber tube {A), which is connected with the gas supply. To light the burner, turn on the gas and hold a lighted match a short distance above the top of the burner tube ( B ). The flame should be a faint blue. If it is yellow, turn the ring at the bottom of the burner until the flame is blue. Fig. II. — Bunsen burner INTRODUCTION 3 A suitable height for most experiments is about io cm. (or 4 in.). Adjust the gas pressure until the flame is about this height. The hot¬ test part of the flame is near the top. In heating with the Bunsen burner follow these directions: — a. Light the burner before a piece of apparatus is held over it or be¬ fore it is placed beneath a wire gauze which supports a dish or a flask. b. Test tubes — used frequently — should be dry on the outside. If the test tube contains a solid, heat gradually by moving the tube in and out of the flame. If the test tube contains a liquid, only the part containing the liquid should be put in (or above) the flame. When the liquid begins to boil, the test FlG - IIL Cutting a glass tube tube should be removed from the flame for an instant or held over it. As a rule a test tube holder should be used (Fig. 3). c. Do not heat empty glass apparatus, e.g. beakers. In heating a beaker containing a liquid, do not use the free flame, but place the vessel on a wire gauze which stands on an iron ring. Porcelain dishes should also be placed on a gauze. Porcelain crucibles may be heated with a free flame. All porcelain apparatus should be heated and cooled gradually. 3 . Cutting, bending, and drawing glass tubing. — a. Cutting. — Determine the length needed, lay \\ the tube on the desk, and with / forward strokes of a triangular file / ma ke a short, deep scratch where the tube is to be cut. Grasp the N/ 7 tube in both hands, and hold the thumbs together opposite the ' scratch; now push gently with the - - thumbs, pull at the same time ^= 32 ^ with the hands, and the tube will Fig. IV. ■ —• Fire polishing a glass break at the desired point (Fig. tube HI). The sharp ends should be smoothed by rotating them slowly in the Bunsen flame until a yellow color is distinctly seen or until the end becomes red hot; this operation is called fire polishing (Fig. IV). 4 EXPERIMENTS IN PRACTICAL CHEMISTRY Fig. V. — A wing- top burner b. Bending.— Glass tubes can be bent in an ordinary illuminating gas flame, but the Bunsen flame is usually flattened by a wing-top (Fig. V). Attach the wing-top to the top of the burner tube before lighting the gqs. The flattened Bunsen flame should be slightly yellow and about 7 centimeters (2.5 inches) wide for ordinary bends. A right-angle bend is easily made. Determine the part where the tube is to be bent. Grasp the tube in both hands, and hold it so that this part is directly over the flame (Fig. VI). Slowly rotate it between the thumbs and forefingers, and gradually lower it into the flame. Con¬ tinue to rotate it until the glass feels soft and ready to bend. Then remove it from the flame, and slowly bend FlG - VI - ~ Bending a tube into a right angle - it into a right angle ^ rst step (Fig. VII). Use a block of wood to assist the eye in making an Fig. VII. — Bending a tube into a right angle — second step Fig. VIII. — Bending a tube into an oblique angle — first step coated with soot, and then allowing it to cool slowly. Tubes can be bent into an oblique angle by heating them through about twice the space required for a right angle (Figs. VIII, IX); a very slight bend can be made by holding the INTRODUCTION 5 tube across the flame, heating a short space, and then bending slightly. c. Drawing. — Glass tubes can be drawn into two pointed tubes thus: Heat the tube as in b through about 2.5 centimeters (1 inch) of its length, remove it from the flame and slowly pull it apart a short distance; let it cool for a few seconds, and then pull it quickly to the desired length. Stirring rods can be made from glass rod in the same way. 4. Filtering. — A solid may be separated from a liquid by filter- Fig. IX. — Bending a tube into an ing. A circular piece of filter oblique angle - second step paper is folded to fit a glass funnel, and when the mixture is poured upon this paper the solid — called the residue or precipitate — is retained, while the liquid — called the fil¬ trate — passes through and may be caught in a test tube or any other vessel. The filter paper is prepared for the funnel by folding the circular piece A (Fig. X) into the shapes B and C. The folded paper is then opened so that three thicknesses are on one side and one on the other. To filter, the cone - shaped paper (from C) is placed in the funnel ( D) and moistened with water, so it will stick to the funnel. The liquid Fig. XI. - Funnel supported for filtering to be filtered may be poured directly from the vessel upon the paper or down a glass rod which touches the edge of the Fig. X. — Preparing a filter paper 6 EXPERIMENTS IN PRACTICAL CHEMISTRY vessel (6 a); the lower end of the rod should nearly touch the paper inside the funnel. The funnel can be supported as shown in Fig. XI. 5 . Constructing and arranging apparatus. — The various parts of the apparatus should be assembled and put together as completely as possible before starting the experiment. The parts that are to fit each other should be connected so that all joints are gas-tight. In long experiments or those involving weighing the apparatus should be inspected by the Teacher. a. To insert a glass tube into a rubber tube. — Cut one end of the rubber tube at an angle, moisten the smoothed end of the glass tube with water, place the end of the glass tube in the angular-shaped cavity so that both tubes are at about a right angle, grasp the end of the rubber tube firmly and slip it slowly up and over the end of the glass tube. b. To push a glass tube through a hole in a stopper. — Wet one end of the tube with water and grasp it firmly near this end; hold the stopper between the thumb and fore¬ finger of the other hand, and work the tube through the hole by a gradual rotary motion. Never point the tube toward the palm of the hand that holds the stopper. Never grasp a bent tube at the bend when inserting it into a stopper — it may break and cut the hand severely. c. To bore a. hole in a cork. — Select a Fig. XII. —■ Cork borer cork free from cracks or channels and use a in a cork borer which is one size smaller than the de¬ sired hole. Hold the cork between the thumb and forefinger, press the larger end against a firm board, and slowly push the borer (previously moistened with water or soap solution) by a rojtary movement through the cork, taking care to bore perpendicularly to the cork (Fig. XII). If the hole is too small, enlarge it with a round file. Push the small cylinder of cork finally out of the borer with the handle. d. To make a test wire. — (i) Platinum. Rotate one end of a piece of glass rod, about io centimeters (4 inches) long, in the flame until it softens. At the same time grasp a piece of platinum wire about 7 centimeters (3 inches) long firmly in the forceps about 1 INTRODUCTION 7 centimeter (0.5 inch) from the end, and hold it in the flame. When the rod is soft enough, gently push the hot wire into the rod. <0-^- ) ¥> / / / 5 Fig. XIII. — Test wires — platinum (upper), nichrome (lower) (2) Nichrome. Wind a piece of nichrome wire around a match stick. The completed wires are shown in Fig. XIII. 6 . Pouring liquids and transferring solids. — a. Liquids can be poured from a test tube or dish without spilling by moistening a glass rod with the liquid, holding the rod against the edge of the vessel, and then pouring the liquid slowly down the rod (Fig. XIV). b. Liquids should be poured from a bottle by holding the bottle as shown in Fig. XV. Note „ „ . r ., , , 1 0 1 1 Fig. XIV. — Pouring a liquid down a rod that the stopper and bottle are held in the same hand. The stopper is first removed by hold¬ ing the palm of the hand upward and grasping the stopper between the fingers before the bottle is lifted (Fig. XVI). All stoppers 8 EXPERIMENTS IN PRACTICAL CHEMISTRY should be removed this way when possible, and not laid down on the desk. The drop on the lip of the bottle should be touched with the stopper before the latter is put into the bottle. c. Solids should never be poured directly from a large bottle into a test tube or dish. Use a spoon, spatula, or piece of smooth paper; or rotate the bottle slowly so that the solid will roll out in small quantities. If the Fig. XVII. Putting a solid into a tube so tid j s dirty ( e.g . charcoal ) f first step catch the solid on a nar¬ row strip of paper creased lengthwise, and introduce the solid from the paper into the test tube as shown in Figs. XVII, XVIII. 7. Collecting gases. — Gases are usually collected over water in a pneumatic trough; one form is shown in outline in Fig. XIX (right). The bottle (or tube) to be filled with gas is first filled with water, covered with a piece of filter paper, inverted (Fig. XIX — left), and placed mouth down¬ ward on the support of the trough, which is previously filled Fig. XVIII. — Putting a solid into a tube — second step with water just above the support (Fig. XIX). The paper is then removed. Glass plates instead of filter paper may be used to cover !ig. XIX. Pneumatic trough in the bottle. The gas escapes from of^water (left ^'*'* the delive ^ tube > bubbks through the water into the vessel, and forces the water out of the vessel. Gases not very soluble in water (e.g. oxygen and hydrogen) are collected in this way. INTRODUCTION 9 Fig. XX. Scales Some heavy gases, e.g. hydrochloric acid, chlorine, and sulphur dioxide, are collected by allowing the gas to flow downward into an empty bottle, i.e. by downward dis¬ placement (Fig. 41). Ammonia and other light gases are collected by allowing the gas to flow upward into a bottle, i.e. by upward dis¬ placement (Fig. 48). 8 . Weighing. — Weighing may be approximate or accurate. Ap¬ proximate weighings are made on the scales (Fig. XX) and accurate weighings on the horn pan balance (Fig. XXI) or on the chemical balance (Fig. XXII). The Met¬ ric System of Weights is used and should be studied before weigh¬ ing is attempted. (See Appen¬ dix, § 1.) Note these general directions: — (1) Before weighing, see that the scales and balances are clean and properly adjusted. If out of order, do not adjust them your- Fig. XXI. — Horn pan balance hanging in a box (open in front and closed in back) to protect the balance from air currents self, but report to the Teacher. (2) Put objects on the left side and weights on the right. Heavy objects and weights should be put near the center of the pan. (3) Substances should not be i / —at —a -f=Sr Fig. XXII. — Chemical balance in a glass case (front partly raised) placed directly on the platform or pan, except pieces of certain metals, e.g. zinc or aluminium, or porcelain and glass objects. io EXPERIMENTS IN PRACTICAL CHEMISTRY In weighing on the scales, put a piece of paper of about equal size on each platform; the paper on the left should be creased. Take the substance from the bottle with a clean spoon or spatula, or pour it out by rotating the bottle as described in 6 c above; if too much is taken out, do not put it back into the bottle, but throw it into the waste jar or a special bottle. Approximate weighings are made on the scales, e.g. the quantities of chemicals usually needed in or¬ dinary experiments. Objects and quantities weighing over ioo gm. should be weighed on the scales. In weighing on the horn pan or the chemical balance, if the sub¬ stance itself should not be placed directly on the pan, weigh a small watch crystal or crucible and then weigh the substance in this vessel. Sometimes a piece of apparatus is hung from the balance hook. Ac¬ curate weighings are made on the balance, e.g. the exact quantities needed in quantitative experiments. Record the total weight at once in the proper place in the Record in the laboratory notebook — not on a scrap of paper. Enter the weight as grams and a decimal fraction, e.g. 5.29 grams, not 5 grams, 2 decigrams, and 9 centigrams. Record all weighings — temporary and final — in the notebook. The process of weighing is as follows: — A. Scales. — Put the object, or the paper containing the proper substance, on the left side; on the right side put one or more weights which are judged to be the approximate weight. Now add or re¬ move (substance or) weights until the pointer swings the same num¬ ber of spaces each side of the middle division. Weighings of small quantities, e.g. 5 grams or less, are usually made by sliding a rider along a graduated beam on the front of the scales. B. Chemical balance. — Release the beam by turning the screw or lever. The pointer should swing the same (or very nearly the same) number of spaces each side of the central line. If it does not, consult the Teacher. If it does, proceed with the weighing. Put the* object {e.g. crucible, dish, tube, or special substance) on the left pan and the weight judged to be equal on the right pan. Release the beam carefully by turning the screw or lever, and note the move¬ ment of the pointer. If the added weight is correct, the pointer will swing the same (or very nearly the same) number of spaces each side of the central line on the scale. If incorrect (as it usually is), slowly turn back the screw or lever and bring the balance to rest. Add or INTRODUCTION ii remove the weight which is next heavier or lighter — as needed — and release again. If not correct, bring the balance to rest, and change the weights accordingly, taking care to add or remove the weights in order ( i.e. next heavier or lighter). Continue to change the weights, bringing the balance to rest each time, until the correct weight is obtained, i.e. when the pointer swings the same number of spaces each side of the central line as it did at the beginning. As soon as the substance or object is weighed, note the weights on the pan and record their sum at once in the notebook, then compare the weights with those missing from the box; if correct, so indicate in the notebook, and finally check the total weight by adding the weights as they are returned to the box. The following rules should be rigidly observed: — a. Always bring the balance to rest before changing the weights, the object, or the substance. b. If on releasing, the beam does not swing, arrest and release again, or fan one pan very gently. c. Handle all weights with the forceps — not the fingers. C. Horn pan balance. — The horn pan balance must be counter¬ poised before each weighing. This is readily done. Clean the pans with soft paper or cheesecloth. Allow them to swing freely and note which side is lighter by estimating the distances to right and left. Add bits of wire or compact wads of paper to the proper pan until the balance is counterpoised, i.e. until the pointer swings equal distances to the right and left. Proceed with the weighing as in B (noting that there is no releasing screw). 9. Measuring. — Liquids are measured accurately in graduated cylinders and burettes (Figs. I, DD, 46). The lowest point of the curved surface of the liquid, called the meniscus, is its correct height (Fig. 47). Time can be saved by learning and remembering that the average ordinary test tube (15 X 1.8 centimeters or 6 X } inch) holds about 30 cc. (cubic centimeters), while the large test tube (20 X 2.8 cen¬ timeters or 8 X 1 inch) holds about 75 cc. (cubic centimeters). 10. Smelling and tasting. — Unfamiliar substances should never be smelled or tasted except according to directions, and even then with the utmost caution. Never inhale a gas vigorously, but waft it gently with the hand toward the nose. Never ask another pupil to 12 EXPERIMENTS IN PRACTICAL CHEMISTRY inhale a gas. Taste acids, bases, and salts by touching a minute portion of the dilute solution to the tip of the tongue, and as soon as the sensation is detected, reject the solution at once — never swallow it. 11 . Accidents. — Cuts should be washed in clean cold water and then covered with collodion or court plaster if slight, or bandaged if severe. Burns should be covered with a paste made by mixing sodium bicarbonate (baking soda) and carron oil (an emulsion of lime water and oil) and then bandaged. Acids and alkalies if spilled on the hands or spattered on the face should be washed off at once with water; if a burn is produced, this may be treated as described above. Fires may be extinguished by sand or by carbon tetrachloride. If the clothing catches fire, a damp towel or asbestos blanket should be used. An emergency box or cabinet containing “ first aid ” articles should be kept in a convenient place. For contents, see Appendix, § 6, List F. EXPERIMENTS CHEMICAL CHANGE — COMPOUNDS — ELEMENTS (Practical Chemistry, pp. i-io, §§ 1-14) Experiment 1 — Chemical Change Materials. — Candle, lime water. Apparatus. — Block of wood, bottle. Light a candle and stick it to a block of wood with a drop of melted candle wax. a. Hold a cold, dry bottle over the lighted candle (Fig. 1). Remove the bottle in a moment and examine the inside. Describe what you see. What is the sub¬ stance ? b. Pour some clear lime water into the bottle, and shake. Describe the change. What gas caused the change? Answer : 1. What are the two products of a burning candle ? 2. Does the candle really “burn away”? Fig. i. — Studying a 3. What does this experiment illustrate? chemica^ change Experiment 2 — Properties and Chemical Change Materials. — Sulphur, copper wire, concentrated nitric acid, magnesium ribbon. Apparatus. — - Test tubes, block of wood, forceps, Bunsen burner. a. Examine a piece of sulphur. Note and record its properties, e.g. color, odor, physical state. Put a small piece on a block of wood and light the sulphur by directing the flame upon it. Observe the color and size of the flame of the burning sulphur. Note (very cautiously) the odor of the gas by brushing a little gently toward the nose. Compare the properties (e.g. color, odor) of the gas with those of the sulphur. 13 14 EXPERIMENTS IN PRACTICAL CHEMISTRY What characteristic of chemical change does this experiment illustrate ? Do not let the sulphur burn longer than necessary. Extinguish it with a little sand, or by pressing it with a piece of stiff paper. b. Examine a piece of clean copper wire. Note and record its properties, especially color, appearance ( e.g . luster), and flexibility. Grasp one end of the wire with the forceps, and hold the other end in the hottest part of the Bunsen flame until the copper melts and undergoes a definite change (Fig. 2). Remove, and examine the product. Compare it with unheated copper. Is the product a different substance from the copper Fig. 2. — Heating copper wire in a Bunsen flame ? Why? c. Roll a piece of copper wire into a ball, drop it into a test tube one fourth full of concentrated nitric acid, and warm gently. What is the evidence of chemical change? d. Examine a piece of magnesium ribbon. Note and record its properties, as in a. Grasp one end firmly with the forceps, hold the other end in the flame for an instant, and then remove it. Observe the result. Examine the product. How does it differ from magne¬ sium? Answer: 1. What is a conspicuous property of sulphur? Of copper? Of magnesium ? 2. How does this experiment illustrate chemical change? 3. What characteristic of chemical change does this experiment illus¬ trate? Experiment 3 — Mixture and Compound Materials. — Powdered sulphur, powdered iron (or clean, fine iron filings), dilute hydrochloric acid, carbon disulphide. Apparatus. — Scales, magnet, lens, test tubes and holder, Bunsen burner, mortar and pestle. Weigh about 4 gm. of powdered sulphur on a piece of paper on the scales (see Introduction §8A). Weigh about 7 gm. of powdered iron (or clean, fine iron filings) on another paper. a. Note and record their conspicuous properties. Try the effect of a magnet on each by moving it along the under side on the paper. Record the result. CHEMICAL CHANGE — COMPOUNDS 15 Put a pinch of each in separate test tubes, add a little dilute hydro¬ chloric acid, and warm gently. Note and record the result in each case, especially the odor of the gas from the tube containing the iron. Put a pinch of each in separate test tubes, add about 5 cc. of carbon disulphide, and shake well. (Caution. Carbon disulphide catches fire readily. Do not use carbon disulphide near a flame.) Note and record the result. Mix the sulphur and iron thoroughly by grinding them together in a mortar. Divide the mixture into two equal portions. Use one in b, and the other in c. b. Examine the mixture from a with a lens. Can you detect sulphur and iron? Try the effect of a magnet on some of the mixture, and state the result. Divide this portion into two parts. Put one part in a test tube, and add dilute hydrochloric acid. Warm the acid mixture gently until there is evidence of action, note the odor and compare with the odor from the iron and acid in a. Put the other part in a test tube, add 5 cc. of carbon disulphide, shake well, let it settle, pour the liquid into a dish, and stand the dish in the hood. When the carbon di¬ sulphide has evaporated, examine the solid product. What is it? c. Put the other half of the mix¬ ture from a in a test tube, attach the holder, and heat (Fig. 3). When the mass begins to glow, take the test tube out of the flame. Heat again intensely for a few minutes. Let the tube cool, hold it over the mortar, break off the lower end with the pestle. Remove the glass, grind the product, and use it in d. d. Examine the powder from c with a lens. Is iron or sulphur detected? Note and record the effect of a magnet. Put a pinch in a test tube, add a little hydrochloric acid, note the odor of the gas, and pour the contents immediately into a waste jar in the hood. Compare the odor of the gas with similar tests ( e.g . in a). Is there evidence of iron? Of a new substance? Put a pinch in another test tube, add 5 cc. of carbon disulphide, and shake well. As soon as the solid has settled, pour the liquid into a dish, stand the dish in the hood, and let the liquid evaporate. Is any sulphur left in the dish ? 16 EXPERIMENTS IN PRACTICAL CHEMISTRY Answer: i. What are some characteristics of a mixture? Of a com¬ pound ? 2. Is the product in c a mixture or a compound? Why? 3. If the product in c had been weighed, how would its weight be related to the weight of the sulphur and iron ? 4. How does this experiment illustrate the first characteristic of chemical change ? The second characteristic ? Experiment 4 — Compound and Elements Materials. — Oxide of mercury, joss stick (or small splint of wood). Apparatus. — Test tube clamped to iron stand (Fig. 4), Bunsen burner. J Put a little oxide of mercury (the same as mercuric oxide) on the end of a narrow piece of paper creased length¬ wise, and slip the powder into a test tube (Fig. 5 ). The powder should nearly fill the round end of the test tube. Hold the test tube in a horizontal position, shake it to spread the powder into a thin layer, and then clamp the test tube as in Fig. 4 . a. Heat the whole test tube at first; then heat intensely the part that contains the sub¬ stance. After heating for several minutes insert a glowing joss stick well into the test tube. Observe and describe the change. The change is due to oxygen. If there is no change, heat intensely again and insert the glowing joss stick. b. Examine the deposit on the upper part of it? If you are in doubt, scrape out a little (Note. — Some unchanged Fig. 4. — Apparatus for decomposing oxide of mercury the tube. What is upon a piece of paper and examine it. oxide will probably be left; throw it in the waste jar.) Answer: 1. To what class of substances does mercuric oxide belong? 2. To what class does the product from a belong? Fromb? 3. Into what substances can mercuric oxide be decomposed? OXYGEN (Practical Chemistry, pp. 12-22, §§ 15-30) Experiment 5 — Preparation of Oxygen — Short Methods Materials. •— Lead dioxide, barium dioxide, potassium chlorate, sodium peroxide, hydrogen peroxide, dilute sulphuric acid, potassium perman¬ ganate solution, joss stick. OXYGEN n Apparatus. — Test tube clamped to an iron stand (as in Fig. 4), burner. (Note. — Hereafter the pieces of apparatus provided each pupil will not be included.) a. Put a little lead diox¬ ide into a test tube and proceed with the heating as in Exp. 4. If more con¬ venient, the substance may be heated as in Exp. 3 c (see Fig. 3). Test with a glowing joss stick. State the result. b. Proceed as in a, using barium dioxide. State the result. c. Proceed as in a, using potassium chlorate. State the result. d. Fill a test tube nearly full of water and stand it in the test tube rack. Obtain from the Teacher a little sodium peroxide on a creased paper, cautiously slip the sodium peroxide into the water, and put a glowing joss stick into the gas in the upper part of the test tube. State the result. e. Fill a test tube half full of fresh hydrogen peroxide, add half the volume of dilute sul¬ phuric acid, shake, and then Fig. s A. -Putting a powder into a nearl y fiU the test tube with test tube —second step potassium permanganate solu- tion. Immediately test the escaping gas with a glowing joss stick. State the result. Experiment 6 — Preparation and Properties of Oxygen— Long Method Materials. — 5 gm. of potassium chlorate, 5 gm. of manganese dioxide, joss stick, sulphur, piece of charcoal fastened to one end of a copper wire (30 cm. long), wad of iron thread (“steel wool”). Fig. 5. — Putting a powder into a test tube —• first step 18 EXPERIMENTS IN PRACTICAL CHEMISTRY Apparatus. — As in Fig. 6 . A is a large test tube (20 cm. or 8 in.) provided with a one-hole rubber stopper, to which is fitted a short glass tube B; the latter is connected by the rubber tube C with the delivery tube D. E is a pneumatic trough with a support for a collecting bottle. I. Preparation. — Weigh the potassium chlorate on the scales on a piece of paper creased lengthwise, and slip it into the test tube; Shake the test tube until the chemicals are thor¬ oughly mixed. Hold the test tube in a horizontal position and roll or shake it until the mixture is spread along about one half of the tube. Insert the stopper with its tubes, and clamp the test tube to the iron stand, as shown in Fig. 6, taking care not to crush the tube or disturb the contents. The end of the delivery tube D should rest on the bottom of the trough under the hole in the support. Be sure there are no leaks. Before proceeding, ask the Teacher to inspect the apparatus. Add water to the pneumatic trough E until the hole in the support is covered. Fill one bottle full of water, cover it with a piece of filter paper, invert it in the trough, remove the paper, and stand the inverted bottle upon, or near, the support (Fig. XIX). Fill three more bottles and have them ready to replace the one filled with gas. Heat the test tube gently with a small Bunsen flame about 10 cm. (4 in.) high. Move the flame slowly along the test tube, taking care not to heat the tube too long in one place nor too near the rubber stopper. As soon as the gas bubbles regularly through the water, slip the inverted bottle over the hole in the support. The gas will rise in the bottle and force out the water. If the gas comes off too rapidly, remove the flame for an instant; if too slowly, increase the heat; if not at all, examine the stopper and the rubber connecting tube for leaks, and adjust accordingly. When the first bottle is full of gas, remove it, cover it tightly with a piece of filter paper, and stand it (mouth upward) upon the desk. Invert another bottle in the trough, remove the paper, and slip the bottle over the hole. Fill it with oxygen. Fill all the bottles in the do the same with the manganese dioxide. OXYGEN 19 same way. When the last bottle of gas has been collected, im¬ mediately remove the end of the delivery tube D from the water. (Note. — After the test tube is cool, the contents can be removed with warm water.) Perform II at once. II. Properties. — a. Thrust a glowing joss stick into one bottle, and observe the result. Remove the joss stick, make it glow again, and repeat as many times as possible. How does the glowing joss stick change? Does oxygen burn? b. Put a small piece of sulphur in the deflagrating spoon, and heat it until the small, blue flame of burning sulphur is seen. Then lower the spoon into a bottle of oxygen. Notice any change in the flame. Very cautiously waft a little of the contents of the bottle toward the nose. Of what does the odor remind you? (As soon as the results are conclusive, remove the spoon and plunge it into the water in the trough to extinguish the burning sulphur. Cover the bottle with a piece of filter paper.) c. Heat the charcoal (fastened to the wire) long enough to produce a faint glow, then lower it into a bottle of oxygen. Observe the result. d. Twist one end of the copper wire (used in c) firmly around the wad of iron thread, heat the ends of a few strands for an instant, and quickly lower it into a bottle of oxygen. The iron should change conspicuously. Observe the result. Required Exercises. — 1. Write a brief account of Exp. 6 I in your notebook. 2. Write a brief account of Exp. 6 II, answering all questions. 3. State some physical properties of oxygen, e.g. color, solubility in water. 4. Describe the chemical conduct of oxygen. 5. (Optional.) Sketch the apparatus used to pre¬ pare oxygen. Experiment 7 — Oxidation of Copper Apparatus. — Evaporating dish, test tube fitted with a cork. Fig. 7. — Evaporat- p u t about 4 gm. of clean copper borings in ing dish on a gauze- an evaporating dish and stand the dish on a covered ring for gauze-covered ring attached to an iron stand oxidation of copper (jrjg 7). Heat the dish carefully but intensely 20 EXPERIMENTS IN PRACTICAL CHEMISTRY about ten minutes. Then heat the contents of the dish directly with the free flame for about five minutes. Describe any marked change in the copper. When the dish is cool, transfer the contents to a test tube, cork tightly, and save for Exp. 23. (Note. — The dish can be cleaned by warming dilute nitric acid in it.) Answer: 1. What chemical compound was formed ? 2. What elements combined? 3. What general name is given to this kind of chemical change? What special name? Experiment 8 — Heating a Known Weight of a Metal in Air Material. — Zinc dust. Apparatus. — Crucible block (Fig. 8), covered crucible (Fig. 9). CD Cony the form of Record (see below) in your notebook. When you weigh, take the notebook to the bal¬ ance (or scales) and enter all weights in the proper place as soon as the weighing is made. Do this hereafter in all experi¬ ments which involve weighing. Clean and dry a porcelain crucible and cover. Place the covered crucible on the Fig. 8. - Block for carrying a crucible crucible block (Fig. 8), and carry it to the balance (or scales); always use this block in carrying the crucible to and from the balance (or scales). Weigh the covered crucible (see Introduction § 8 ). Enter the weight in the proper place in the Record. Record Wt. of crucible, cover, and zinc. gm. Wt. of crucible and cover. .gm. Wt. of zinc . gm. Wt. of crucible, cover, and contents after heating .... gm. Wt. of crucible and cover.. . gm. Wt. of contents after heating. gm. Wt. of zinc. gm. Change in weight. gm. Crease a slip of paper lengthwise, pour about 3 gm. of zinc dust into the crease, slide the zinc dust into the crucible (Fig. 5), and weigh accurately (including the cover). Enter the weight. OXYGEN 21 ^>0 Place the covered crucible on the triangle supported by a ring on an iron stand (Fig. o). Heat gently with a low flame to avoid breaking the crucible. Gradually increase the heat until the flame is just above the bottom of the crucible. Lift the cover occasionally by grasping the ring firmly with the forceps. If the zinc glows and a smoke escapes, cover the crucible at once to prevent loss. Heat for about twenty minutes. Cool the crucible gradually by moving the flame slowly beneath it. As soon as the crucible is cool, weigh. Enter the weight, and complete the Record. Show the final weight to the Teacher before throwing away the contents of the crucible. (Note. — The crucible can be cleaned with dilute hydrochloric acid.) Fig. 9. Covered crucible supported Answer: 1. What is the name of the product? on a Wangle 2. What is the result of heating a known weight of a metal in air? 3. To what is the difference in weight due? Experiment 9 — Slow and Rapid Oxidation (Demonstration Experiment) Materials. — Powdered potassium nitrate, charcoal, phosphorus-tipped match, bottle of oxygen, iron thread, phosphorus (for c), magnesium (for d), bottle of oxygen (for d). Apparatus. — As in Fig. to, iron pan. a. Lay a piece of charcoal on an iron pan, heat it with a direct flame, and when hot, cautiously sprinkle powdered potassium nitrate upon the hot surface. Stand back as soon as the chemical action begins. Observe the action, especially its violence and rapidity, also the effect on the charcoal. b. Rub the head of a phosphorus-tipped match with the finger in a dark place, and observe and describe the result. c. Teacher’s Experiment. Put a small piece of phosphorus (Care!) in an evaporating dish nearly full of water, cut off a thin slice, return the rest of the phosphorus to the bottle, and place the slice on an iron pan or a brick. Stand back, and observe the result. 22 EXPERIMENTS IN PRACTICAL CHEMISTRY d. Teacher’s Experiment. Grasp one end of a short piece of magnesium firmly with the forceps, hold the other end in the flame for an instant, then re¬ move it, and let the magnesium burn in the air. In a similar way light another piece and quickly thrust it into a bottle of oxygen. Compare the results. In which case was oxidation more rapid ? e. Fill a test tube half full of iron thread, add io cc. of water, and moisten the iron. Cover the open end, and invert the test tube in a dish nearly full of water. Slip a rubber band upon the test tube to mark the height of the water, and clamp the test tube to the iron Fig. io. — Appara- tus for showing stan( j so that the Q p en enc j touches the bottom s ow oxi ation (jrjg IO ) L e t the whole apparatus stand undisturbed for a day or two, taking care to keep the open end of the test tube covered with water. Observe and explain the final result. Experiment 10 — Air and Combustion Materials. — Wood, paper, candle. Apparatus. — Two blocks of wood, lamp chimney. a. Set fire to a small piece of wood, drop it while burning into a bottle of air, and cover the bottle with a block of wood. Observe and state the final result. b. Proceed as in a, using a piece of paper and another bottle. Observe and state the final result. c. Attach a short candle to a block of wood with melted candle wax. Stand a lamp chimney tightly over the lighted candle. How is the flame affected? d. Hold the chimney a short distance (i cm. or 0.5 in.) above the lighted candle. Does the candle continue to burn? Why? Keep the chimney in the same position and cover the top with a block of wood. What is the result? Why? Answer: 1. What is your conclusion from these experiments about the relation of air to combustion ? 2. Apply 1 to oxygen. 3. How could the conclusion in 2 be verified by a simple experiment in the laboratory? CARBON AND ITS OXIDES 23 CARBON AND ITS OXIDES (Practical Chemistry, pp. 25-37, §§ 31-47) Experiment 11 — Distribution of Carbon Materials. — Sand, wood, cotton, starch, sugar, candle. Apparatus. — As in Fig. 11; block of wood. a. Cover the bottom of the crucible ( A ) with sand. Put in a small piece of wood, a wad of cotton, and a lump of starch. Fill the crucible with dry sand, and slip it into the ring of an iron stand (Fig. 11). Heat intensely until the smoking ceases (about 20 minutes). While the crucible is heating, proceed with b, etc. When the crucible is cool, pour the contents upon a block of wood or an iron pan. Separate the lumps from the sand. Examine and compare them with the original substances. What is the residue? b. Heat a little sugar in a test tube until the smoking ceases. What is the most obvious solid product ? c. Close the holes at the bottom of a lighted burner, and hold a glass tube in the upper part of the flame long enough for a thin deposit to form. Examine it. What is it? State its source. d. Hold a glass tube in the flame of a candle which stands on a block of wood, and note the with c. What is the deposit? Experiment 12 — Combustion and Carbon Dioxide Materials. — Copper wire, charcoal, limewater, wood, paper, denatured alcohol, gasolene. Apparatus. — Bent tube as in Fig. 12 for h. a. Wind one end of a copper wire around a small lump of charcoal, hold it in the flame until the edges glow, and then lower it into a bottle. Let it remain for a minute or two, then remove. Fill the bottle one- fourth full of fresh limewater, cover with the hand, and shake. Ob¬ serve and state the result. b. Recall and record the result of adding limewater to a bottle which was held over a burning candle. (See Exp. 1.) Fig. 11. — Appara¬ tus to show the distribution of carbon result. Compare 24 EXPERIMENTS IN PRACTICAL CHEMISTRY c. Burn wood (e.g. a match) and paper in separate bottles and test as in a. State each result. d. Put several drops of denatured alcohol in an evaporating dish, set it on fire, and hold a bottle over the flame. Test as in a. State the result. e. Proceed as in d, using gasolene instead of alcohol (Care!). State the result. f. Hold a bottle over a low Bunsen flame for a minute or so, and then test as in a. State the result. g. Optional. Draw smoke through limewater, and state the result. h. Exhale the breath through a glass tube into a bottle half full of limewater (Fig. 12). De¬ scribe the result. What gas does the breath Fig. 12.-Testing contain? the breath Answer: i. Is carbon dioxide a product of com- bastion in each case? 2. What are two tests for carbon in a compound? Experiment 13 — Fermentation and Carbon Dioxide (Demonstration Experiment) Materials. — Karo or molasses, yeast cake, limewater, kerosene. Apparatus. — Bottles and bent tube as in Fig. 13. Put 20 cc. of karo or molasses in a 250 cc. bottle (A in Fig. 13), add 175 cc. of water, and mix well. Grind one-fourth of a fresh yeast cake to a paste with about 10 cc. of water, add it to the solution and shake well. Fill the bottle B half full of limewater and cover this solution with a little kerosene (to protect it from the air). Connect as in Fig. 13 and let the apparatus remain a day or more where the temperature is 25 0 to 30° C. Examine the liquid in B at intervals. Fig I3 ._ Apparatus to show What is the evidence that carbon diox- the relation of fermenta- ide is a product of fermentation? tion and carbon dioxide CARBON AND ITS OXIDES 25 Experiment 14 — Preparation and Properties of Carbon Dioxide Materials. — Calcium carbonate, dilute hydrochloric acid, candle fastened to a wire, joss stick, calcium hydroxide solution. Apparatus. —■ As in Fig. 14. A is a 250 cc. bottle provided with a two-hole stopper, through which passes the dropping tube B and the right- angle bend C; the tube D (15 cm. or 6 in.) is attached to the bent tube by the rubber tube E. The dropping tube is made as follows: Cut off the top of a thistle tube about 2.5 cm. (1 in.) below the juncture of the stem and cup, and heat the sharp ends a minute or two in the flame; when cool, slip a thick-walled rubber tube (5 cm. or 2 in. long) over one end of the stem, attach a pinch-clamp to the rubber tube, and connect the tube with the cup, taking care to have the ends of the glass tubes as close together as possible. If properly con¬ structed, the cup will remain Fig. 14. Apparatus for preparing car- upright when full of liquid. bon dioxide Note. — Instead of the apparatus shown in Fig. 14, one of the simpler forms shown in Fig. 15 may be used; in these the end of the thistle tube must be beneath the acid. I. Preparation. — Put about 20 gm. of calcium carbonate into the bottle, and arrange the apparatus as in Fig. 14. Fill the pneumatic trough with water, fill a bottle with water, cover with filter paper, invert, stand it on the support, and remove the paper (see Fig. XIX). Fill three other bottles and have them ready. Introduce enough dilute hydro¬ chloric acid through the dropping tube B to cover the calcium carbonate. Car¬ bon dioxide will be evolved at once. Fig. 15. — Optional forms of apparatus for preparing carbon dioxide 26 EXPERIMENTS IN PRACTICAL CHEMISTRY Collect four bottles, cover tightly with filter paper, and stand aside till needed. Proceed at once with II. II. Properties. — a. Plunge a blazing joss stick several times into a bottle. Observe and state the result. b. Lower a short, lighted candle into a bottle of air, and quickly invert a bottle of carbon dioxide over it, holding the bottles mouth to mouth. Observe and state the final result. c. Pour a little calcium hydroxide solution into a bottle of carbon dioxide, cover with the hand, and shake vigorously. Describe and explain the result. d. Fill a bottle of carbon dioxide one-third full of water,' cover it tightly with the hand, and shake vigorously. Invert the bottle, still covered, in the pneumatic trough and remove the hand. Observe and state the result. Note. — As soon as d is performed wash the acid from the marble and save the solid for other experiments. Answer: i. Describe briefly the preparation of carbon dioxide. 2. What do a and b show about the relation of carbon dioxide to com¬ bustion? 3. What does b show about the relative weights of carbon dioxide and air? 4. What does d show about the solubility of carbon dioxide ? Experiment 15 — Beverages and Carbon Dioxide Fig. 16. — A siphon of water charged with carbon dioxide (Demonstration Experiment) Materials. — Siphon of charged water, bottle of ginger ale (or similar beverage), calcium hydrox¬ ide solution, joss stick. Apparatus. — As in Fig. 16, bent tube fitted to a one-hole stopper, beaker (or bottle.) a. Draw off some charged water from a siphon (Fig. 16) into a beaker (or bottle), and let it stand a minute or two. Then show the presence of carbon dioxide in the beaker (or bottle). b. Remove the metal cap from a ginger ale bottle, pour off a little of the liquid, and insert the rubber stopper with its tubes and arrange the apparatus so that the outer end rests on CARBON AND ITS OXIDES 27 the bottom of an empty beaker (or bottle). Let the whole remain undisturbed a few minutes, and then show that the beaker (or bottle) contains carbon dioxide. c. Proceed as in ( b ) with the same bottle, but fill the beaker (or bottle) half full of calcium hydroxide solu¬ tion, and have the outer end of the tube dip beneath the surface of the solution (Fig. 17). If necessary, warm the bottle of ginger ale. Answer: 1. What is the evidence of carbon dioxide in these experiments ? 2. What is the evidence that the car¬ bon dioxide was under pressure in the siphon and the bottle? In which was Fig. 17. —Testing the gas from the pressure greater? a charged beverage Experiment 16 — Plants and Carbon Dioxide (Demonstration Experiment) Materials. — Fresh green leaves, water saturated with carbon dioxide, joss stick. Proceed as in the author’s Practical Chemis¬ try , bottom of page 31. Use the apparatus shown in Fig. 18. Required Exercises. — 1. Describe this ex¬ periment. 2. What is the evidence that green plants (a) absorb carbon dioxide and ( b ) give off oxygen ? Experiment 17 — Fire Extinguishers and Carbon Dioxide (Demonstration Experiment) Materials. — Dilute sulphuric acid, saturated ^ „ sodium bicarbonate solution. Fig. 18. — Experiment to show the relation Apparatus. — Bottle with one-hole stopper and of carbon dioxide to tubes as in Fig. 20, fire extinguisher (the port- plants able type as in Fig. 19). 28 EXPERIMENTS IN PRACTICAL CHEMISTRY a. Add dilute sulphuric acid to a test tube half full of saturated sodium bicarbonate solution and show that the escaping gas is car¬ bon dioxide. b. Unscrew the top of a portable fire extinguisher (Fig. 19) and examine the parts, noting especially the opening of the escape tube, bottle of acid, stop¬ per, and collar. Remove a little of the solution, and test it as in a. Replace the cap, take the ex¬ tinguisher to the roof, yard, or street and show how to use it in extinguishing a small fire. c. Optional. Make a simple extinguisher like that shown in Fig. 20. The bottle and tubes are those used (as A-C-E-D ) in the apparatus shown in Fig. 14. The bottle is filled about two-thirds full with saturated sodium bicarbonate solution, the small tube (inside the bottle) contains dilute sul¬ phuric acid and a piece of lead to hold it down after it is lowered into the solution. Connect the Fi G . 19. — Port- tubes with the stopper and push the stopper well able fire extin- down into the neck of the bottle, guisher (cut Build a small fire in a dish or on some bricks, away to show Hold the end of the tube in one hand, with acid bottle) the 0 ther grasp the bottle by the neck, taking care to hold the stopper tightly with the fingers, invert the bottle, and direct the stream upon the fire. Answer: 1. Why are sulphuric acid and sodium bicarbonate used in a fire extinguisher? 2. Why does the liquid flow out of a fire extinguisher with such force? 3. Does a “chemical” fire engine differ essentially from a portable extinguisher? If so, how? Experiment 18 — Carbon Monoxide (Demonstration Experiment) Proceed as in Exp. 142, or postpone until carbon monoxide is studied. Fig. 20. — Simple modification of a fire extinguisher HYDROGEN 29 HYDROGEN (Practical Chemistry, pp. 39-48, §§ 48-57) Experiment 19 — Preparation of Hydrogen — Short Methods Materials. — Zinc, magnesium, aluminium, iron, dilute hydrochloric acid, dilute sulphuric acid, sodium hydroxide. a. Fill a test tube half full of dilute hydrochloric acid, stand it in the rack, and drop in a small piece of zinc. Test the escaping gas by holding a lighted match at the mouth of the test tube. (If the test is not decisive, add more zinc, warm gently, or wait until more gas accumulates in the test tube.) What gas is it? What was its source? Proceed in the same way with magnesium and iron (in the form of tacks or filings); use separate test tubes, and heat, if the action is slow. Observe the result in each case, and apply the questions asked about zinc. b. Proceed as in a, using dilute sulphuric acid. Observe the result in each case. Answer the questions asked in a. c. Roll two or three small, thin pieces of aluminium into a ball, drop it into a test tube, slip in a piece of sodium hydroxide about 2.5 cm. (or 1 in.) long, and add a little water. Warm gently. Observe the result, and test as above. Answer the questions asked in a. Experiment 20 — Preparation and Properties of Hydrogen — Long Method Materials. — 10 gm. of granulated zinc, dilute sulphuric acid, copper sulphate solution, wax taper. Apparatus. — As in Fig. 21. See also Fig. 15 for optional forms. I. Preparation. — Slip the zinc into the bottle (or test tube) — Fig. 21. Insert the stopper with its tubes. Be sure there are no leaks. Fill the pneumatic trough with water as usual, and ad- Fig. 21. — Apparatus for preparing hydrogen 30 EXPERIMENTS IN PRACTICAL CHEMISTRY just the apparatus so that the end of the delivery tube rests on the bottom of the trough under the hole in the support. Fill the bot¬ tles with water, and cover each with filter paper; invert one in the trough, remove the paper, and stand the inverted bottle upon the support (see Fig. XIX). Put 2 or 3 cc. of copper sulphate solution in the cup, fill with dilute sulphuric acid, and let the acid mixture run into the bottle by pinch¬ ing the clamp ; if the acid does not flow freely down the tube into the bottle, loosen the stopper for an instant. (The copper sulphate has¬ tens the chemical change.) The gas will bubble through the water up into the bottle. Collect and remove four bottles of gas as in the Preparation of Oxygen (Exp. 6), taking care to cover each bottle tightly with a piece of wet filter paper. If the evolution of gas slackens or ceases, add a little more acid through the dropping tube. Perform II at once. II. Properties. — a. Uncover a bottle for an instant to let a little air in, and then hold a lighted match at the mouth of the bottle. Ob¬ serve the result. b. Remove the paper from another bottle and allow it to remain uncovered for three minutes — by the clock. Then show the pres¬ ence or absence of hydrogen by holding a lighted match at the mouth of the bottle. Observe the result. What property of hydrogen does this experiment show? c. Stand a covered bottle of hydrogen on the desk, place a bottle of air over it, remove the paper, and bring the mouths of the bottles together. Let them remain in this position for a minute or two, then remove the upper bottle and cover both with wet filter paper. Remove the paper from one bottle and hold a lighted match at the mouth. Observe the result. Do the same with the other bottle. What property of hydrogen does this experiment show? d. Invert a covered bottle of hydrogen, remove the paper, and quickly thrust a lighted taper up into the bottle. Withdraw the taper slowly. Then insert and withdraw it several times, and observe carefully (i) if the hydrogen burns, (2) if so, where, and (3) if the taper burns both inside and outside the bottle. Feel of the neck of the bottle; describe and explain. What properties of hydrogen are shown by this experiment? Note. — As soon as II is completed, wash the zinc several times, and save it for other experiments. Required Exercises. — 1. Write a brief account of Exp. 20 I. 2. Write a brief account of Exp. 20 II, answering all questions. HYDROGEN 31 3. State the conspicuous physical properties of hydrogen. 4. What is a test for hydrogen? 5. Why was there an explosion in a? Why none in d? 6. Does hydrogen support combustion? 7. (Optional.) Sketch (from memory, if possible) the apparatus used to prepare hydrogen. Experiment 21 — Interaction of Water and Sodium (Demonstration Experiment) Materials. — Sodium, tea lead (or wire gauze). Apparatus. — Test tube clamped over dish as in Fig. 22. Caution. — Sodium is a dangerous substance. It should be handled cautiously and used strictly according to directions. Small frag¬ ments obtained for experiments should be pro¬ tected from water by a mortar or dish. If any sodium is left from an experiment, it must not be thrown into the refuse jar, but returned to the bottle. Fill an evaporating dish two-thirds full of water. Fill a test tube full of water, cover and invert it, and clamp it as shown in Fig. 22. Wrap a small piece of clean sodium loosely in a piece of dry tea lead about 5 cm. (2 in.) square, make two or three small holes in the tea lead, and slip it under the test tube. (Wire gauze may be used instead of tea lead.) A gas will Fig. 22. Appara- rise in the test tube. Proceed similarly with additional pieces of sodium and dry tea lead until the test tube is full of gas. Then unclamp it, keep it mouth downward, and hold a lighted match at the mouth. Observe the result imme¬ diately, especially at the mouth of the tube. What is the gas? What was its source ? Experiment 22 — Burning Hydrogen (Demonstration Experiment) Materials. — 20 gm. of granulated zinc, dilute sulphuric acid, copper sul¬ phate solution, platinum wire (optional), small bottle. Apparatus. — As in Fig. 23. The platinum tip is shown (about actual size) in Fig. 24. Directions for making the platinum tip may be found tus for collecting the gas liberated by the interaction of water and so¬ dium 32 EXPERIMENTS IN PRACTICAL CHEMISTRY in the author’s Experimental Chemistry , page 340. If platinum is not available, a piece of capillary glass tubing about 5 cm. (2 in.) long may be used. Fig. 23. — Apparatus for burning hy¬ drogen Caution. — Perform this experiment with extreme care, since a mixture of hydrogen and air explodes violently if ignited. Put the zinc in the bottle (Fig. 23). Fill the U-tube two-thirds full of calcium chlo¬ ride, put a wad of cotton upon the solid, insert the stopper in each arm, and con¬ nect the U-tube with the gen¬ erator and the exit tube. Ex¬ amine all joints to be sure they are tight. Extinguish all flames in the vicinity, and proceed exactly according to directions. Introduce through the drop¬ ping tube about 25 cc. of dilute sulphuric acid containing 5 cc. of copper sulphate solution. Acid may be added slowly after the evolution of gas begins, but no air should be introduced. Let the gas bubble through the acid two minutes, then attach the rubber connector and the capillary glass tube (or the platinum tip) to the end of the exit tube, leaving a short space between the ends of the two glass tubes so the rubber tube may be compressed suddenly, if necessary. Let the gas run half a minute to drive air out of the tip (Fig. 24). Slip a small test tube over the tip, and when it is full of hydrogen gas remove the test tube (still inverted or closed with the thumb), take it a few feet away from the generator, and hold a lighted match at the mouth; if an explosion results, collect another test tube and test again, repeating until the gas lights with only a faint noise and . a lnum burns quietly at the mouth of the tube. Then light the p hydrogen at the tip, and observe at once the faint flame. a. Show that the flame is very hot by holding a match or platinum wire over it. b. Hold a small, dry bottle over the flame in such a position that HYDROGEN 33 the tip of the flame is just inside the bottle. Note the deposit in¬ side the bottle. Remove the bottle, and extinguish the flame at once by pinching the rubber connector. Examine the inside of the bottle. What is the deposit? Explain its formation. Answer : i. What is the product of burning hydrogen ? 2. How does this experiment illustrate oxidation? Combustion? Experiment 23 — Reduction of Copper Oxide by Hydrogen Materials. — Copper oxide, io gm. of granulated zinc, dilute sulphuric acid, copper sulphate solution. Apparatus. — As in Fig. 25. The parts lettered A, B, C, D, E constitute the hydrogen generator used in Exp. 20. F is a large test tube fitted with a two-hole stopper; the delivery tube E passes through one hole and extends nearly to the bottom of the test tube. The right-angle tube G passes just through the other hole; the tube G is lengthened by the rubber tube H. While the parts of the apparatus are being collected and arranged put the copper oxide prepared in Exp. 7 in an evaporating dish, stand the dish on a gauze- covered ring attached to an iron stand (Fig. 7), and heat gently. (If Exp. 7 was omitted, use 5 gm. of copper oxide.) Slip the copper oxide into the dry test tube F (Fig. 25), hold the tube in a horizontal position and tap it gently to spread the solid into a thin layer. Connect this test tube with the rest of the apparatus, and clamp it into the proper posi¬ tion, taking care not to Fig. 2- — Apparatus for the reduction of copper oxide by hydrogen crush the tube. Put the zinc into the bottle A. Ask the Teacher to inspect the apparatus, and do not proceed un¬ til permission is given. After obtaining permission, put 2 cc. of cop¬ per sulphate solution into the cup, fill the cup nearly full with dilute sulphuric acid, pinch the clamp, and let about half the acid run into 34 EXPERIMENTS IN PRACTICAL CHEMISTRY the generator bottle. If the hydrogen does not bubble freely, let more acid run in, taking care to keep a little acid in the cup. Add enough acid to keep the gas flowing steadily through the apparatus for at least two minutes before lighting the Bunsen burner. Heat gently the lower part of the test tube where the copper oxide is located. Do not let the flame come near the rubber tube H. The gas must flow slowly through the apparatus during the heating; if it does not (as you can tell by the bubbles in the bottle or by smell¬ ing the gas at the end of the rubber exit tube), introduce more acid. If the test tube F should break, pinch the rubber tube D an instant to cut off the flow of hydrogen, and then extinguish the Bunsen burner flame. Continue to heat until a marked and permanent change is observed inside the test tube F. Then stop heating, and extinguish the Bunsen burner flame at once. Note the two products in the test tube (dis¬ regarding any unchanged copper oxide). What is each product? Required Exercises. — i. Describe briefly the whole experiment, and sketch the apparatus. 2. What chemical compound was formed in F? 3. How was the copper oxide changed? What special name is given to this kind of change? 4. Recall Exp. 7 (Oxidation of Copper). In Exps. 7 and 23, what was oxidized, what was reduced, and what substances accomplished the oxida¬ tion and the reduction? 5. Summarize in a few words how Exps. 7 and 23 illustrate oxidation and reduction. MEASUREMENT OF GASES (Practical Chemistry, pp. 50-57, §§ 58-66) Experiment 24 — Weight of a Liter of Oxygen Note. — This Experiment may be postponed until the pupil has acquired more experience in the laboratory. Object. — To find the weight of a certain volume of oxygen, reduce this volume to standard conditions, and calculate the weight of 1 liter of oxygen. (N ote. — See Introduction, § 8, for directions about weighing.) Materials. — Potassium chlorate, manganese dioxide, calcium chloride, glass wool or shredded asbestos. Apparatus. — As in Fig. 26. A is a test tube attached to the bent tube F by a rubber stopper. B is a large bottle (2500 cc.) to be filled with MEASUREMENT OF GASES 35 water; it is provided with a two-hole rubber stopper, through which pass F and C, the latter being connected with a rubber tube C' to which is attached the short glass tube G. A Hofmann screw is attached at the point E. Another bottle (2500 cc.) D serves to catch the water forced over from B through CC' by the oxygen generated in A . The hook 5 of aluminium wire permits A to be hung from the balance beam in weighing. Thermometer, barometer. Copy the form of Record, as given below, in the notebook. Enter all weights and volumes in the proper place as soon as the weighing and measuring are done. Fill the space 1 in A with a mixture of equal weights of powdered manganese dioxide and powdered potassium chlorate (Fig. 26). The mixture should be dried before use by heating it in an F oven to about no° C. Push glass wool, or shredded asbes¬ tos (previously ig¬ nited to a red heat), into the space 2 in A . Put small lumps of calcium chloride into 3 and glass wool into 4. Push the stopper well into the test tube. Wipe jr IG ^ — Apparatus for finding the weight of a A carefully with liter of oxygen soft paper. Weigh AF accurately on the balance and enter the weight in the proper place in the Record. Weigh the empty, dry, clean bottle D to a decigram on the scales, and record the weight. Fill B with water nearly to the neck. Fill CC' with water and tighten the Hofmann screw to prevent the water from running out. Insert F into the stopper of B. Push the stopper into the bottle, slowly at first, then hard; if water rises in F, loosen the screw at E slightly, remove A, and blow gently into F to force the water back into B. When properly adjusted, the water should be in B and CC' but not in F. Replace A, taking care not to crush the thin glass by pushing it too hard upon its stopper. Open the screw at E. If the apparatus is tight, little or no water will flow out. It should be adjusted until air tight. Leave the screw open. 36 EXPERIMENTS IN PRACTICAL CHEMISTRY Heat A gently with a low flame, keeping the flame back of the space 2 . The liberated oxygen will force the water from B into D. Heat A just hot enough to cause a gentle flow of water into D. When B is about half empty, stop heating. While A is cooling sufficiently to weigh, stand a thermometer in D ; also read the barometer. When A is cold, raise B until the water is at the same level in B and D, pinch C' tight and remove it from D. Read and remove the ther¬ mometer. Dry D on the outside, if necessary, and then weigh it on the scales; record the weight. The gain in weight (in grams) of D gives the volume of oxygen liberated (since i gm. of water = i cc.). Weigh AF on the balance; record the weight. Its loss in weight is the weight of the oxygen that passed into B. Record Weight of tube AF before heating.. . Weight of tube AF after heating.. . Weight of oxygen (W) . Weight of bottle D and water. Weight of bottle D empty. Weight of water . Volume of water. Observed volume of oxygen (F'). Temperature (t) . Pressure read on barometer (P'). Pressure caused by water vapor (a) . Corrected pressure. Corrected volume of dry oxygen (F). Corrected volume of dry oxygen expressed in liters (VI) Weight of i liter of oxygen. gm. .gm. gm. gm. . gm. gm. cc. cc. °C. mm. mm. cc. 1 . gm. Correct the observed volume (F 7 ) of oxygen for temperature (t ), pressure (P'), and pressure of water vapor (-"- y / ^ Fig. 29. — Test wires — platinum (upper), nichrome (lower) b. Teacher’s Experiment. — Remove a lump of potassium from the bottle, cut off two or three small slices, and put the rest back in the bottle. Fill a pneumatic trough nearly full of water. Throw a piece on the water and stand back until the slight explosion is heard Note the result, especially the difference from sodium. Repeat with the rest, piece by piece. Test the water (near the surface) with red litmus paper. State the result. Compare with the test in a (1). What substance is in the water? c. (1) Put a little water in a bottle. Set fire to a small piece of sulphur in a deflagrating spoon and lower the burning sulphur into the bottle. Let it burn a minute or two, then extinguish the flame by dipping the spoon into the water. Remove the spoon, cover the bottle with the hand, and shake well. Dip a glass rod into the liquid, draw the moistened end across a piece of blue litmus paper, and ob¬ serve the change in color. This change in the color of blue litmus is caused by acids; in this case the acid is sulphurous acid, which was produced by the combination of the sulphur oxide and water. (2) Boil a small piece of calcium oxide with a little water in a test tube. Test with red litmus paper as in (1). If the result is indiffer¬ ent, put the paper in the test tube and shake well. Observe the re¬ sult in a minute or two. Compare with (1). Required Exercises. — 1. State briefly the essential chemical change that took place in c (1) and (2). 2. State these chemical changes as equations (using the names of the substances). WATER — HYDROGEN PEROXIDE 43 Experiment 33 — Solubility of Gases in Water a. Fill a bottle half full of water, close with the hand and shake vigorously several minutes. Fill a test tube nearly full and warm the test tube gently. What is the immediate evidence of dissolved gas? What effect has increased heat on the dissolved gas ? b. Heat the following in separate test tubes as in a : Faucet water, ammonium hydroxide, dilute hydrochloric acid. State in each case the evidence of dissolved gas. (Note. — As soon as the observation is made, pour the liquids down the sink and flush it well with water.) Answer: i. Does distilled water contain dissolved gases? 2. What gas does soda water contain? 3. In which are gases more soluble, hot or cold water? Experiment 34 — Solubility of Liquids in Water Materials. — Alcohol (ethyl or methyl), gasolene, glycerin, aniline, ether, carbon tetrachloride. a. To a test tube one-third full of water add a little alcohol and shake. Is there evidence of solution ? Add a little more and shake well. Add a third portion and shake. Is there still evidence of solution? Draw a conclusion as to the mutual solubility of alcohol and water. b. Repeat a, using successively gasolene, glycerin, aniline, ether, and carbon tetrachloride. Observe the results in each case and con¬ clude accordingly. c. Tabulate the results of a and b under the headings Mutual Solubility, Limited Solubility, Very Slight Solubility. Experiment 35 — Solubility of Solids in Water Materials. — Sand, calcium sulphate, sodium chloride, potassium per¬ manganate, sodium hydroxide (solid), calcium carbonate (powder). Put about 1 gm. of the substances in separate test tubes, add 10 cc. of water, and stand the tubes in a rack. Shake well and note the evidence of solubility. In case of doubt, let the solid settle, and transfer half of the clear liquid to an evaporating dish by pouring it down a glass rod (Fig. XIV), and evaporate by heating the dish on a gauze. What is the final evidence of solubility ? Tabulate the difference in solubility as below, using the terms Very soluble, Moderately soluble, Slightly soluble, Insoluble. 44 EXPERIMENTS IN PRACTICAL CHEMISTRY Difference in Solubility of Solids Solvent —10 cc. Solid — i gm. Result 1. Sand 1. 2. Calcium Sulphate 2. Water at temperature 3. Sodium Chloride 3 - of Laboratory 4. Potas. Permanganate 4- 5. Sodium Hydroxide 5- 6. Calcium Carbonate 6.. Experiment 36 —Effect of Heat on the Solubility of Solids Materials. — About 5 gm. each of powdered copper sulphate and potas¬ sium chlorate, calcium hydroxide solution for c. a. Label two test tubes, I, II. Put 10 cc. of water into each. To I add 1 gm. of powdered copper sulphate, and to II add 1 gm. of powdered potassium chlorate. Shake each test tube, and then allow them to stand undisturbed until the solid settles. Is there evidence of solubility in each case? (Save for b.) b. Heat I, and add gradually 2 gm. of powdered copper sulphate. Does it all dissolve? Heat II and add 2 gm. of powdered potassium chlorate. Does it dissolve? Add the rest of each solid to the re¬ spective. tubes, and heat (but do not boil). What effect has in¬ creased heat on the solubility of the solids? (Save for Exp. 38.) c. Fill a test tube half full of clear calcium hydroxide solution, and heat it to boiling. Observe the result. Compare with the cold solution. What effect has increased heat on the solubility of cal¬ cium hydroxide? How does the result differ from b? Experiment 37 — Effect of Shape on the Solubility of a Solid Material. — Crystallized alum. Apparatus. — 2 large test tubes fitted with corks. Weigh about 2 gm. of crystallized alum (in one lump, if possible) on the scales, and counterpoise it with a second quantity of equal weight. Pulverize the latter in a mortar. Put each in a test tube, add 25 cc. of water, and insert the cork. Note the time. Shake the tubes gently until the powder has dissolved. Note the time again. Estimate the amount of alum left in the other tube, or, if time per¬ mits, continue to shake at intervals until the solid has dissolved, and note the time again. WATER — HYDROGEN PEROXIDE 45 Compare the times required to dissolve the powder and the crystal. Why does dissolving occur faster in one case than in the other? Experiment 38 — Saturated Solutions Materials. - — Solutions from Exp. 36 b, sodium chloride. Apparatus. — Large flask or bottle, hydrometer (specific gravity — direct reading) for liquids heavier than water, tall jar (e.g. a 250 cc. graduated cylinder). a. If the test tubes with contents from Exp. 36 b were saved, use them; if not, prepare new solutions. If the contents of the test tube is not liquid, add a little water, and heat gently until the solid dissolves. Cool each solution quickly by holding the lower end of the test tube in a stream of water. Are crystals formed? Are they formed at once? Are they large or small ? b. Wipe each test tube dry and heat gently until the liquid is clear. Stand the tubes in a rack, and let each solution cool slowly and stand undisturbed until the next laboratory period. Observe the result. Compare the size and general shape of the crystals with those formed in a. c. Demonstration Experiment. — Prepare a satu¬ rated solution of sodium chloride by shaking about 100 gm. of fine salt with 275 cc. of water in a flask or bottle until no more salt dissolves. Let the undissolved salt settle and carefully pour the clear solution into the tall jar. Take the temperature. Let the hydrometer sink carefully into the solution. When the instrument becomes still, read the num¬ ber on the scale (on the stem) that is level with the surface of the liquid (Fig. 30). This number is the specific gravity of the solution. Compare the concentration with that read from the solubility curve shown in Fig. 43 on page 72 of the author’s Practical Chemistry Fig. 30. — Find¬ ing the spe¬ cific gravity of a solution with the hy¬ drometer Experiment 39 — Solubility of a Given Solid Object. — To find the number of grams of potassium dichromate dissolved in 100 gm. of water. Material. — Potassium dichromate solution (concentration known only to Teacher). Apparatus. — Water bath as in Fig. 31. 46 EXPERIMENTS IN PRACTICAL CHEMISTRY Copy the form of Record in the notebook. Enter all weights in the proper place as soon as weighings are made. Weigh an evaporating dish on the balance, and enter the weight at once in the Record in the notebook. Obtain from the Teacher exactly 25 cc. of the potassium dichromate solution. Pour the solu¬ tion into the weighed dish. Weigh the dish and contents, and record the weight. Record Weight of dish and solution. gm. Weight of dish. gm. Weight of solution. gm. Weight of dish and solid — I gm. II. gm. Ill. gm. Weight of dish. gm. Weight of solid. gm. Weight of water ( i.e . solution — solid). gm. Weight of solid dissolved in 100 gm. of water. gm. Stand the dish on a water bath and evaporate the solution to dryness (Fig. 31). Complete the evaporation by transferring the dish to a gauze-covered ring and heating intensely. When the dish is cool, weigh, and record the weight. Heat again on the gauze, cool, and weigh; if the two weights are the same (or nearly so), accept the first weighing, but if the weights are considerably different, heat intensely (but do not melt the solid), cool, and weigh a third time. Complete the entries in the Record. Cal¬ culate the weight of the solid dissolved in 100 gm. of water. Submit the result to the Teacher before throwing away the contents of the dish. Experiment 40 — Formation of Crystals Material. — Powdered alum or borax. Apparatus. — Thread, lens. Prepare a hot, concentrated solution of alum or borax by boiling about 10 gm. of alum or 5 gm. of borax in 10 cc. of water in a large test tube. Pour the solution into an evaporating dish (or a Fig. 31. — Water bath for evaporating a solution to dryness WATER — HYDROGEN PEROXIDE 47 beaker). Suspend a piece of thread in the solution (as in Fig. 32). Stand the whole aside to crystallize. Examine at intervals, and when well¬ shaped crystals have formed on the thread, remove the thread. Dry the crystals carefully with filter paper. Examine them, using a lens if the crystals are small, and observe the properties, partic¬ ularly the shape, luster, and color. Test a crystal for water of crystallization. Required Exercises. — 1. Describe this experiment. 2. What is the name of the shape of a typical alum crystal? (A borax crystal?) i 3. What term describes the luster? 4. Do the crystals contain water of crystal¬ lization ? Is the amount conspicuously large ? Fig. 32. — Crystallizing alum Experiment 41 — Testing for Water of Crystallization Materials. — Sodium carbonate, potassium dichromate, ferrous sulphate, borax, barium chloride, zinc sulphate, sodium sulphate, calcium sul¬ phate, sodium chloride, potassium nitrate, sugar, magnesium sulphate, potassium bromide. Test several of the substances for water of crystallization by heat¬ ing a dry specimen in a dry test tube inclined so that the open end is the lower. Observe in each case the change in appearance of the solid during the heating, relative amount of water liberated (if appre¬ ciable), and appearance of the residue. State each result. Experiment 42 — Per Cent of Water of Crystallization Object. — To find the weight of water lost by heating a weighed amount of crystallized copper sulphate, and to calculate the per cent of watei of crystallization. Material. — Crystallized copper sulphate (powdered). Copy the form of Record, as given below, in the notebook, and enter all weights as soon as the weighing is completed. Clean and dry an evaporating dish and weigh it to a decigram on the scales. Put about 10 gm. of powdered copper sulphate in the dish and weigh to a decigram. Record the weight at once. 48 EXPERIMENTS IN PRACTICAL CHEMISTRY Record Weight of dish and copper sulphate before heating . . . gra. Weight of dish .. gm. Weight of copper sulphate. gm. Weight of dish and copper sulphate before heating . . . gm. Weight of dish and contents after heating..gm. Weight of water of crystallization. gm. Per cent of water of crystallization. per cent Stand the dish with its contents on a gauze-covered ring attached to an iron stand, heat gently for five or ten minutes, and then intensely until the substance becomes a gray powder. Do not touch the sub¬ stance, and take special pains not to lose any. Cool slowly and weigh as before. Record the weight at once. Complete the entries in the Record, and calculate the per cent of water of crystallization. Sub¬ mit the result to the Teacher before throwing away the contents of the dish. Experiment 43 — Anhydrous Compounds Materials. — Hydrated (crystallized) copper sulphate and cobalt chloride. a. Pulverize a little hydrated copper sulphate and note the color. Put it in a test tube, hold the tube horizontal, and spread the powder along the tube. Hold the mouth of the tube slightly lower than the other end, and heat gently. Begin to heat at the closed end and move the tube in the flame so that all the liberated water is finally driven from the tube. Note the color of the anhydrous solid. Let the tube cool. Meanwhile do b. When the tube is cool, cautiously add a little water, and let it run down upon the solid. What effect does the water have on the color of the solid ? b. Proceed as in a, using hydrated cobalt chloride. Answer: i. What is the difference between a hydrated and an anhydrous compound ? 2. What is the color of hydrated copper sulphate? Dehydrated? An¬ hydrous ? 3. As in 2 for cobalt chloride. Experiment 44 — Efflorescence Materials. — Sodium carbonate, sodium sulphate, ferrous sulphate, potas¬ sium ferrocyanide, barium chloride, magnesium sulphate. WATER — HYDROGEN PEROXIDE 49 Put a fresh, or a recently broken, crystal of several of the substances on a piece of filter paper, and label each. Let them remain exposed to the air for an hour or more. Describe any marked change in the appearance. Answer: i. What does the change, if any, show about the air? About the crystal? 2. To what is the change due? Experiment 45 — Deliquescence Materials. — Sodium hydroxide, calcium chloride, potassium hydroxide, magnesium chloride, table salt, zinc chloride, potassium carbonate, sodium nitrate. Proceed and answer as in Exp. 44. Experiment 46 — Efflorescence and Deliquescence (Demonstration Experiment) Materials. — Crystallized copper sulphate, concentrated sulphuric acid, sodium hydroxide. Apparatus. — 4 test tubes fitted with corks, thread, copper or iron wire. a. Select two pieces of crystallized copper sulphate which will just slip into a test tube. Tie a thread around each piece. Put 10 cc. of water into one test tube, and 10 cc. of con¬ centrated sulphuric acid into the other, taking care not to leave any drops on the inside of the test tube. Hang a piece of the solid in each test tube and insert the cork tightly (Fig. 33); smear a little vaseline around the upper edge of the test tube containing the acid to make the joint air-tight. Let the test tubes stand in the rack undisturbed for several hours (or until the next laboratory period), and then ex¬ amine each solid. Compare them with each other and with a sample of the original substance. State the change, if any, in each case; state also the degree of change, if possible. Why do the changes differ in degree? Explain. b. Proceed as in a, using sodium hydroxide. Wind the wire around the solid and attach the wire to the thread. Observe, answer, and explain as in a. Fig. 33. — Solid sus¬ pended in a closed test tube to show efflorescence and deliquescence 50 EXPERIMENTS IN PRACTICAL CHEMISTRY Experiment 47 — Supersaturation Material. — Sodium thiosulphate. Apparatus. — Test tube fitted with a cork. Fill a test tube half full of crystallized sodium thiosulphate and add 2 or 3 cc. of water. Warm slowly until all the solid has dissolved. Pour the solution into a warm, clean, dry test tube, insert a cork, and let it stand undisturbed until cool. Note the change in the solution, if any. Drop in a small crystal of sodium thiosulphate and watch for a definite change. What happens? Observe and state the final result. Answer: i. What is the difference between a saturated and an unsat¬ urated solution? 2. How could you determine whether a cold solution is saturated, un¬ saturated, or supersaturated? Experiment 48 — Qualitative Composition of Water (Demonstration Experiment) Materials. — Chlorine water (see Exp. 6o), joss stick. Apparatus. — Chlorine tube (tube about i m. long closed at one end). Fill the tube with chlorine water, cover the open end with the thumb or finger, invert the tube, and. immerse the open end in a mortar or an evapo¬ rating dish, which should be nearly full of chlorine water (Fig. 34). Clamp the tube in an upright position, and stand the whole apparatus where it will receive the direct sunlight for several hours. Bubbles of gas will collect at the top. When sufficient gas for a test has collected, unclamp the tube, cover the open end with the thumb or finger, invert, and put a glowing joss stick into the gas. Repeat as long as any of the gas remains. State the result. What is the gas ? p IG 24._Appara- Required Exercises (Review). — 1. What evi- tus for showing dence does the interaction of water and sodium give that oxygen is a about the composition of water? constituent of 2. Apply Exercise 1 to the burning of hydrogen, water 3. Apply Exercise 1 to the reduction of copper oxide. WATER — HYDROGEN PEROXIDE 51 Experiment 49 — Electrolysis of Water (Demonstration Experiment) Materials. — Sulphuric acid, joss stick, taper. Apparatus. — Hofmann apparatus. Fill the Hofmann apparatus (Fig. 35) with water containing 10 per cent of sulphuric acid, so that the water in the reservoir tube stands a short distance above the gas tubes after the stopcock in each has been closed. Connect the platinum terminal wires with a battery of at least three cells (or a street current reduced by suitable resistance). As the action proceeds, small bubbles of gas rise and collect at the top of each tube. Allow the current to run until the smaller volume of gas is 8 to 10 cc. Measure the height of each gas column. As¬ suming that the tubes have the same diameter, the volumes are in approximately the same ratio as their heights. How do the volumes com¬ pare? Test each gas. a. Open the stopcock of the tube containing the smaller quantity of gas long enough to allow the water (or air) to run out of the glass tip, and then close it immediately. Let out a little gas upon a glowing joss stick, and observe the result. Close the stopcock as soon as the result is seen. What is the gas? Repeat, if gas is available. b. Open the other stopcock long enough to force out the water (or air) in the glass tip and then close it. Open the stopcock again, let out a little gas slowly, hold a lighted match for an instant at the end of the tip, and immediately thrust a taper into the small and almost colorless flame. Watch for a change in the taper. Close the stopcock as soon as the change is seen. What is the gas ? Fig. 35. — Hofmann apparatus for the electrolysis of water Required Exercises. — 1. Describe this experiment and sketch the apparatus. 2. What does this experiment show about the composition of water? 3. Compare answer to 2 with answers at the end of Experiment 48. 52 EXPERIMENTS IN PRACTICAL CHEMISTRY Experiment 50 — Properties of Hydrogen Peroxide Materials. — Hydrogen peroxide, manganese dioxide, potassium perman¬ ganate solution, lead nitrate solution, hydrogen sulphide (or ammonium sulphide) solution, joss stick. a. Heat a little hydrogen peroxide, and observe the result. Now add a little powdered manganese dioxide to the heated liquid, and observe the result. Test the escaping gas for oxygen. What is the result ? b. Add several drops of potassium permanganate solution to a little hydrogen peroxide, and observe the result. Is a gas evolved? If so, test it with a glowing joss stick. If not, add more potassium permanganate solution, and then test. What is the gas? c. Prepare a little lead sulphide by adding a few drops of hydro¬ gen sulphide (or ammonium sulphide) solution to dilute lead nitrate solution. Note the color of the lead sulphide. Shake well, add hydrogen peroxide, and warm gently. Observe the change in color. To what is the change due? d. Examine the inner end of the cork stopper of a bottle of hydro¬ gen peroxide. Explain the color. LAWS OF CONSTANT COMPOSITION AND MULTIPLE PROPORTIONS (Practical Chemistry, pp. 87-100, §§ 96-109) Experiment 51 — Law of Constant Composition Object. — To find the weight of oxygen that combines with a definite weight of magnesium. Material. — Powdered magnesium. Apparatus. — Porcelain crucible and cover, triangle. Copy the form of Record (see below) in your notebook and enter each weight as soon as the weighing is made. Clean and dry the crucible and cover, and weigh both together accurately on the balance. (See Introduction, § 8, for directions about weighing.) Enter the weight in the notebook. Put from 0.4 to 0.5 gm. of magnesium in the crucible, and weigh (with cover) exactly the amount taken. Enter the weight. In carrying the cru¬ cible to and from the balance, it should be placed in the crucible block (Fig. 37). Support the covered crucible as in Fig. 36, and heat for five min- LAW OF CONSTANT COMPOSITION 53 utes with a flame which touches the bottom of the crucible. Grasp the cover firmly by the ring with the clean forceps, cautiously lift it, and if the magnesium glows, cover the crucible instantly. Repeat this operation at frequent intervals, gradually increasing the heat, until the glow ceases to spread through the mass. Then adjust the cover so that a small opening is left between the cover and the crucible, and heat intensely for ten or fifteen minutes. If the contents has ceased to glow, heat the crucible, uncovered, for five or ten min¬ utes. Cool the cru¬ cible gradually. When cool, weigh, and enter this weight as I in the Fig. 37. — Crucible block for carrying a crucible Fig. 36. — Covered crucible supported on a triangle proper place. Heat the uncovered crucible again intensely for five or ten minutes. Cool, and weigh as before; enter this weight as H. If the weight is not the same, submit the result to the Teacher. Record Wt. of crucible, cover, and magnesium. gm. Wt. of crucible and cover. gm. Wt. of magnesium. gm. Wt. of crucible, cover, and magnesium oxide I gm., II gm., Ill. gm. Wt. of crucible and cover. gm. Wt. of magnesium oxide. gm. Wt. of magnesium oxide. gm. Wt. of magnesium. gm. Wt. of oxygen. gm. From the weights of the magnesium and the oxygen, calculate the ratio in which the two elements combined. Submit the result to the Teacher before throwing away the contents of the crucible. Note. — The crucible, if blackened, can be cleaned by heating a little sodium hydroxide solution in it and then washing thoroughly with water. 54 EXPERIMENTS IN PRACTICAL CHEMISTRY Experiment 52 — Law of Multiple Proportions Object. — To find the weight of oxygen liberated by heating known weights of potassium chlorate and potassium perchlorate. Materials. — Powdered potassium chlorate and potassium perchlorate. Apparatus. — As in Exp. 51. Copy the form of Record (see below) in your notebook and enter each weight as soon as the weighing is made. I. (For one section of the class.) Clean and dry the crucible and cover, and weigh both together accurately on the balance. Put in the crucible about 1.5 gm. of dry powdered potassium chlorate and weigh (with cover) the exact amount taken. Support the covered crucible as in Fig. 36. Heat with a flame about an inch below the bottom of the crucible. The potassium chlorate melts, begins to decompose, and the oxygen bubbles through the molten mass. Heat about fifteen minutes. Then lower the crucible or raise the burner, until the flame covers the bottom of the crucible. Heat about twenty minutes. If the flame is too high, the potassium chlorate may spatter and adhere to the inside of the cover. Remove the cover with the forceps occasionally, and if it is coated with potassium chlorate, replace it, and let the crucible cool somewhat. Remove the cover, lay it (ring side down) on a piece of paper on the crucible block (Fig. 37), and loosen the thin layer with a pin. Grasp the cover with the forceps, turn out the pieces upon the paper, and finally scrape them from the paper into the crucible. When there is no danger of loss by spattering, remove the cover, lay it (ring side down) on the crucible block, and heat the crucible for twenty or thirty minutes. Let the crucible cool gradually, and when cool, weigh the crucible, cover, and contents, as before. Record the weight as I in the proper place. Heat the uncovered crucible again strongly for five or ten minutes, then cool, weigh as before, and record as II. If the weight is the same as after the first heating, proceed with the calculation; if not the same, heat, weigh again, and record as III. From the weights of the potassium chlorate and the oxygen, calcu¬ late the per cent of oxygen in potassium chlorate. Do this before throwing away the contents of the crucible. LAW OF CONSTANT COMPOSITION 55 Record Wt. of crucible, cover, and potassium chlorate. gm. Wt. of crucible and cover..gm. Wt. of potassium chlorate. gm. Wt. of crucible, cover, and contents before heating .... gm. Wt. of same after heating I gm., II gm., Ill..gm. Wt. of oxygen in potassium chlorate. gm. Per cent of oxygen in potassium chlorate. II. (For one section of the class.) Proceed as in I, using dry potas¬ sium perchlorate. Enter all weights in the Record, and calculate the per cent of oxygen in potassium perchlorate. III. (For the class.) Calculation. (See § 99 in the author’s Practical Chemistry.) According to the law of multiple proportions, if we adopt a fixed weight of one part of a compound as a basis, and express the composition in terms of this weight, then the weights of the other part can be expressed in a simple multiple relation. Let us take potassium chloride as the fixed part and oxygen as the multi¬ ple part. Our problem is to find the small whole numbers which show the simple multiple relation between the weights of oxygen in the two compounds potassium chlorate and potassium perchlorate. a. First, we subtract each per cent of oxygen from 100 (per cent) to find the per cent of the potassium chloride part of each compound. Thus, if we take the exact per cents of oxygen, the per cents of potas¬ sium chloride are 60.82 ( i.e 100 — 39.18) and 53.79 ( i.e . 100 — 46.21) b. Second, we adopt 1 as the fixed weight of the potassium chlo¬ ride part. And we reduce each per cent of potassium chloride to 1, thus, 60.82 -f- 60.82 = 1 and 53.79 4 - 53.79 = 1 c. But in order to keep the correct proportion of potassium chloride to oxygen (found by our experiments), we must also divide each per cent of oxygen by the corresponding number used in b. Thus, 39.18 4 - 60.82 = 0.644 and 46.21 -T- 53.79 = 0.859 These numbers (0.644 and 0.859) represent the weights of oxygen, if the weight of potassium chloride were 1 in each compound. d. Our final step is to find the small whole numbers which cor¬ respond to 0.644 an d 0.859. If we divide 0.644 by 0.859 and express the quotient as a common fraction, we obtain f. This means that 0.644 and 0.859 are in the same relation as 3 and 4. This means that 56 EXPERIMENTS IN PRACTICAL CHEMISTRY the weights of oxygen in the two compounds are in the simple multi¬ ple relation 3: 4. Note. — The per cents of oxygen obtained by individual experiments will probably not give numbers which are in exactly the ratio 3: 4, but a class average is usually very near 3:4. NITROGEN — AIR (Practical Chemistry, pp. 102-113, §§ 110-131) Experiment 53 — Preparation and Properties of Nitrogen Materials. —Ammonium chloride, sodium nitrite, joss stick, iron thread, sulphur. Apparatus. — As in Fig. 38. I. Preparation. — Weigh 8 gm. of ammonium chloride and 10 gm. of sodium nitrite, put them in the flask, add 50 cc. of water, and shake well. Arrange the apparatus, as in Fig. 38, to collect the gas over water. Fill the bottles with water and invert one in the trough. Have two more bottles ready to replace this one. Fill the cup of the dropping funnel with water, and then ask to have the ap¬ paratus inspected by the Teacher. Heat the flask gently with a low flame, and as soon as the nitrogen bubbles regularly through the water, slip the bottle over the hole in the support. Heat gently, but enough to keep the gas bubbling slowly through the Fig. 38. — Apparatus for preparing water. Collect three bottles nitrogen of nitrogen. Caution. — If the mixture in the flask begins to froth or the gas comes off too rapidly, re¬ move the flame and let in a little water; if it continues to froth, pinch the clamp to let out the excess of gas. As soon as the froth¬ ing lessens, close the clamp and heat gently. Remove the end of the NITROGEN — AIR 57 delivery tube from the water as soon as the last bottle of nitrogen has been collected. Proceed at once with II. II. Properties. — a. Thrust a blazing joss stick into a bottle of the gas. Observe and state the result. b. Put a piece of sulphur in a deflagrating spoon, light the sulphur, lower it into a bottle of nitrogen, and keep it there about half a minute. Observe the result. Withdraw, and observe the result. If the sul¬ phur is still burning, repeat. State the results. c. Wind one end of a copper wire around a wad of iron thread, heat a few strands, and quickly thrust the glowing iron into a bottle of nitrogen. Observe and state the result. Required Exercises. — i. Describe briefly the preparation of ni¬ trogen. 2. Sketch the apparatus. 3. Compare the characteristic properties of nitrogen with those of oxygen found by similar experiments. Experiment 54 — Transformation of Combined Nitrogen into Ammonia (Test for Combined Nitrogen) Materials. — Albumin, soda-lime, gelatin, meat, peas, beans, flour, bread, fertilizer. a. Put a little egg albumin in a test tube and add about five times its bulk of soda-lime. Mix by shaking. Heat gently (in the hood) and hold a piece of wet red litmus paper in the escaping smoke. Ob¬ serve and state the change in the color of the litmus paper. (One product of the interaction is ammonia gas, but its odor is usually masked by the burning albumin. The nitrogen needed for the ammo¬ nia comes from the compound (albumin in this case).) b. Proceed as in a, using gelatin, meat, peas, beans, flour, bread. State each result. c. Proceed as in a, using samples of fertilizers. State each re¬ sult. Experiment 55 — Per Cent of Oxygen in Air Object. — To find the volume of oxygen absorbed from a measured volume of air. Materials. — Solutions of pyrogallic acid (10 per cent) and sodium hy¬ droxide (50 per cent). Apparatus. — As in Fig. 39; pneumatic trough half full of water at room temperature, 250 and 25 cc. graduated cylinders. The bottle holds 58 EXPERIMENTS IN PRACTICAL CHEMISTRY about 250 cc. and is provided with a tightly fitting one-hole rubber stopper through which passes a glass plug. The plug is made by clos¬ ing both ends of a glass tube about 10 cm. (4 in.) long, and should fit tight. Copy the form of Record as given below in your notebook and enter each volume as soon as the readings are made. First find the volume of the bottle. Fill the pneumatic trough with water and add hot water, if necessary, to raise the temperature to that of the room. Fill the bottle full of water from the pneu¬ matic trough. Push the stopper into the bottle as far as it will go, insert the glass plug until the inner end is flush with the inner surface of the stopper, and then draw a line around the stopper with a lead pencil to mark its position. Remove the plug and then the stopper carefully, to avoid loss of water. Pour water from the bottle into the 250 cc. graduate until the graduate is full (to the 250 cc. mark) or the bottle is empty; read the volume. If the bottle holds more than 250 cc., the rest of the water in the bottle may be poured into the 25 cc. graduate. Re¬ total volume of the bottle as shown below. Record a. Volume of bottle .. cc. b. Volume of original solution (total)..cc. c. Volume of air taken (a — b) . cc. d. Volume of final liquid.. cc. e. Volume of water which entered ( d—b ). cc. /. Per cent of water which entered (e -=-c). The per cent of entering water equals the per cent of gas absorbed. Therefore: — g. Per cent of oxygen in the sample of air. h. Per cent of nitrogen (100— g) . Measure exactly 10 cc. of pyrogallic acid in the 25 cc. graduate, and pour it carefully into the bottle. Measure also exactly 20 cc. of sodium hydroxide solution, and pour it into the bottle. (Cau¬ tion. — The sodium hydroxide solution is corrosive. Do not spill it on the hands or clothing.) Insert the rubber stopper (with its plug) quickly to the proper mark. Shake the bottle vigorously for a few minutes, and then invert it Fig. 39. — Ap¬ paratus for finding the per cent of oxygen in air NITROGEN — AIR 59 and watch the surface of the liquid for bubbles of air, which will enter if the apparatus leaks. If a leak is detected, ask the Teacher for directions before proceeding. If the apparatus is tight, continue the shaking for about half an hour. During this operation the oxygen is absorbed by the solution. Place the bottle on its side beneath the water in the pneumatic trough, inclining it slightly so that the lower edge of the bottle rests upon the bottom of the trough and the hole in the stopper is beneath the surface of the water. With one hand grasp the bottle firmly by the neck and stopper, and with the other gradually pull out the plug to let the water run in. Water will run in quickly to fill the space left by the oxygen. Take care not to pull out the stopper and not to let any of the solution run out. Be sure also to keep the hole in the stopper constantly beneath the surface of the water. After the water has stopped running in, lift out the bottle, and measure care¬ fully the volume of the liquid in the bottle by pouring it into a gradu¬ ate. Complete the entries in the Record. Note. — This experiment disregards the argon and carbon dioxide in air. Experiment 56 — Water Vapor in Air Material. — Calcium chloride or sodium hydroxide. Place a piece of calcium chloride or sodium hydroxide on a glass plate or a block of wood, and let it remain exposed to the air for an hour or more. Observe and state the result. How does this experi¬ ment show that air contains water vapor? Experiment 57 — Carbon Dioxide in Air Materials. — Calcium hydroxide and barium hydroxide solutions. Apparatus. — Air blast or suction apparatus (for b). a. Pour 25 cc. of calcium hydroxide solution into a bottle, and let it stand exposed to the air for an hour or more. Examine the sur¬ face of the liquid. State and explain the change. b. Optional. Force, or draw, air through a bottle half full of clear barium hydroxide solution until the liquid is conspicuously changed. Describe and explain the change. Answer: 1. What do a and b show about carbon dioxide in air? 2. What does b show about the relative amount (large or small) ? 6o EXPERIMENTS IN PRACTICAL CHEMISTRY Experiment 58 — Testing Air Materials. — As in Exps. 56, 57. Apparatus. — As in Exps. 56, 57. a. Apply Exps. 56 and 57 to the air in different parts of the school building. Start the tests at the same time to obtain comparable re¬ sults. b. Apply Exp. 56 to the air on several days. c. Apply Exp. 57 to the air in the laboratory, out doors, and in a recitation room which has just been vacated. Proceed with the testing as in a (this experiment). Tabulate the results of the whole experiment. CHLORINE — HYDROGEN CHLORIDE — HYDRO¬ CHLORIC ACID (Practical Chemistry, pp. 129-141, §§ 142-160) Experiment 59 — Chlorine — Short Method Materials. — Potassium permanganate, concentrated hydrochloric acid, wax taper, wad of iron thread, 2 pieces of copper wire about 15 cm. long, colored cloth, piece of newspaper, litmus paper (both colors), cotton, turpentine. Fig. 40. — Wads of cotton and iron thread for studying the properties of chlorine Caution. — Do not inhale chlorine. Do this experiment in the hood. I. Preparation. — Put 5 or 6 crystals of potas¬ sium permanganate in each of 4 bottles, add 3 to 5 cc. of concentrated hydrochloric acid, shake, and cover the bottles with a piece of filter paper pressed down to form a loose cap. Chlorine is liberated and will slowly fill the bottles. When the color shows that a bottle is full, proceed at once with it as in II a. Use the other bottles when full as directed. II. Properties. — a. Remove the paper from a bottle of chlorine and thrust a blazing wax taper into the gas. Observe the result. Does the gas burn? Does the taper burn? What is the deposit inside the bottle? b. Using the same bottle as in a, hold a lighted wax taper just inside the bottle. Move it up and down slowly. If it goes out, relight it, and con- CHLORINE oi tinue. (If a taper is unsatisfactory, use a candle.) Observe the result. The wax consists mainly of compounds of hydrogen and car¬ bon. Is carbon detected? What becomes of the hydrogen?. (Sug¬ gestion. Compare with e below.) c. Twist one end of a copper wire around a wad of iron thread (Fig. 40), heat the wad for an instant in the flame, and quickly lower it into the second bottle of chlorine. Observe and describe the re¬ sult, especially the evidence of chemical action. d. Into the third bottle of chlorine hang (by a wire) pieces of colored cloth, litmus paper (both colors), newspaper, and paper con¬ taining writing in lead pencil, ink (black and red) — all moistened with water. Let the whole remain undisturbed for a few minutes (1 e.g . while e is being done). Then observe and describe the change. What is bleached? What is not bleached? e. Twist one end of the copper wire around a wad of cotton, satu¬ rate the cotton with turpentine (preferably warm), and lower the cotton into the fourth bottle of chlorine. Observe at once the for¬ mation of a white smoke and then the conspicuous result. What two products are formed by the interaction of chlorine and turpen¬ tine? Note. — As soon as II e has been completed, fill each bottle with water (in the hood) and pour the contents into a waste jar in the hood. Answer: 1. What is the color of chlorine ? Is this gas heavier or lighter than air? 2. What compound was formed in c? 3. Were the pencil mark and printing ink bleached in d? Why? 4. Of what elements is the compound (or are the compounds) in turpen¬ tine composed ? 5. What experiments show that chlorine is an active element? Experiment 60 — Chlorine — Long Method Materials. — Concentrated hydrochloric acid, 10 gm. of manganese diox¬ ide, and as in Exp. 59 (except potassium permanganate). Apparatus. — As in Fig. 41. A is a 250 cc. Erlenmeyer flask which stands on a gauze-covered ring ; the parts lettered B, C, D, E have been used in preceding experiments. F is a piece of stiff paper. If desired, the optional apparatus shown in Fig. 42 may be used. Caution. — As in Exp. 59. I. Preparation. — Slip the manganese dioxide into the flask. Ar- 62 EXPERIMENTS IN PRACTICAL CHEMISTRY range the apparatus as shown in Fig. 41. Introduce enough concen¬ trated hydrochloric acid through the dropping tube B to cover the man¬ ganese dioxide. Heat the flask A gently with a small flame. Avoid heating so high that steam or hydrogen chloride is evolved. Chlorine is evolved, and passes into the bottle G , which should be removed when full (as seen by the color) and covered tightly with a piece of filter paper; the bottle may be easily re¬ moved by holding the paper cover F in one hand and pulling the bottle G aside, bending the whole delivery tube at the same time at the rubber connection D. If the evolution of gas slackens, introduce more acid. Collect four bottles, and pro¬ ceed at once as in II. II. Properties. — a to e as in Exp. 59 a to e. Experiment 61 — Preparation of Chlorine by Electrolysis (Demonstration Experiment) Materials. — Sodium chloride, litmus solution, dilute hydrochloric acid. Apparatus. — As in Fig. 43. A is a small battery jar (or a beaker), the electrodes E and F are pieces of electric light carbon, and B is a piece of glass (or cardboard). A battery of at least six cells, or a reduced street current, is also needed. Fill A two-thirds full of dilute sodium chloride solution, add a few cubic centimeters of litmus solution, and just enough dilute hydrochloric acid to produce a faint pink color. Slip the partition into the vessel to lessen the diffusion of the Fig. 42. — Op- liquid. Insert the electrodes and connect them tiona.1 appara- with the battery. Turn on the current. Smell !" us P re P ar " cautiously of the gas evolved. Note its effect on mg C ° rme the litmus in this compartment. Turn off the current as soon as the observations have been made. Fig. 41. — Apparatus for preparing chlorine in large quantities CHLORINE 63 What is the gas? What is the change in color in the other com¬ partment? Explain it (in general terms). Experiment 62 — Chlorine Water Materials. — Chlorine water, litmus paper, colored cloth or paper, dark sponge, ink-stained and fruit-stained cloth, gold leaf. Prepare chlorine water by letting the gas bubble for fifteen minutes or more through a bottle or a test tube nearly full of water. a. Try the bleaching action of chlorine water on litmus paper, bright colored cloth or paper (that is not decolorized by water alone), a piece of dark sponge, ink-stained and fruit- stained cloth. State the results. b. Stand a test tube in the rack. Moisten the end of a glass rod, touch it to a small piece of gold leaf, hold the rod with the adhering gold leaf inside a test tube, and wash the gold leaf into the test tube by pouring about 15 cc. of chlorine water down the rod. Remove the rod. Warm the test tube gently and shake until a definite change in the gold is ob¬ served. State the final result. Into what has the gold been changed ? Answer: 1. What happens when chlorine water is exposed to the sun¬ light ? 2. What two equations express the reactions in 1 ? Experiment 63 — Bleaching Materials. — Bleaching powder, dilute sulphuric acid, colored cloth for a; sodium hypochlorite solution, dilute hydrochloric acid, white cloth for b. Apparatus. — 3 Beakers (or bottles), glass rod. a. Demonstration Experiment. — Put a little bleaching powder into one beaker and add enough water to make a thin paste. Fill the second beaker one-third full of dilute sulphuric acid, and the re¬ maining beaker one-third full of water. Press the lower half of the colored cloth into the bleaching powder with the rod, and then into the acid, passing it back and forth several times. Finally wash the cloth thoroughly in the beaker of water, squeeze out the excess of water, and compare the cloth with the sam- Fig. 43. — Apparatus for preparing chlo¬ rine by electrolysis 64 EXPERIMENTS IN PRACTICAL CHEMISTRY pie. Describe the change in the appearance of the cloth. If the change is not marked, try other kinds of cloth. b. Let a drop or two of ink fall from a fountain pen upon a piece of white cloth. Lay the cloth over an evaporating dish and pour a little sodium hypochlorite solution drop by drop upon the spot. Then pour slowly a little dilute hydrochloric acid upon the spot. Wash well with water and note the result. Experiment 64 — Hydrogen Chloride — Short Method Materials. — Sodium chloride, concentrated sulphuric acid, silver nitrate solution, litmus paper, ammonium hydroxide. Put a few grams of sodium chloride in a test tube, and add several drops of concentrated sulphuric acid. Hydrogen chloride is evolved. a. Hold a piece of moist blue litmus paper at the mouth of the test tube. Observe the result. b. Blow the (moist) breath across the mouth of the tube. Hold a piece of wet filter paper in the gas. Observe the result in each case. Explain it. c. Hold a glass rod moistened with ammonium hydroxide in the gas. Observe the result. What is the product? d. Moisten a clean glass rod with silver nitrate solution and hold it in the gas. Observe the result. What is the product? State the result. Experiment 65 — Hydrogen Chloride and Hydrochloric Acid Materials. — Sodium chloride, concentrated sulphuric acid, litmus paper (blue), ammonium hydroxide. Apparatus. — As in Fig. 41 (or 42). I. Preparation. — • (1) Hydrogen chloride. — Put 8 cc. of water into a small bottle or an evaporating dish, cautiously add 10 cc. of concentrated sulphuric acid, and stir until the two are mixed. While this mixture is cooling, weigh 10 gm. of sodium chloride, slip it into the flask, and arrange the apparatus as shown in Fig. 41. Introduce half of the cold acid mixture into the flask, let it settle through the sodium chloride, and then introduce the remaining acid. Heat the flask gently with a low flame, as in the preparation of chlorine. Hydrogen chloride is evolved, and passes into the bottle G, which should be removed when full, as directed under chlorine. (A piece of moist blue litmus paper held near the mouth of the bottle will show when it is full. Let the gas enter a minute or so after the HYDROCHLORIC ACID 65 first test.) Collect three bottles of the gas, cover each tightly, when filled, with a piece of dry filter paper, and set aside for II. (2) Hydrochloric acid. — As soon as the third bottle of gas has been collected, put in its place a bottle one-fourth full of water. Ad¬ just the delivery tube E so that the lower end is a short distance above the surface of the water. Continue to heat the flask at intervals, and the gas will be absorbed by the water. Shake the bottle occasion¬ ally. Meanwhile perform II. II. Properties of hydrogen chloride. — a. Insert a blazing joss stick once or twice into a bottle of the gas, and observe the result. Compare the behavior of hydrogen chloride with that of hydrogen, oxygen, carbon dioxide, and chlorine under similar conditions. b. Hold a piece of wet filter paper near the mouth (or drop it inside) of the same bottle. Observe and describe the result. What is the cause? c. Invert a bottle of the gas, and stand it in a vessel of water ( e.g . the pneumatic trough). Shake the bottle up and down, still keep¬ ing its mouth under water. Observe any change inside the bottle. What property of the gas does the result illustrate? Verify the observation by a simple test applied to the contents of the bottle. State the result. d. Drop into the remaining bottle of gas a piece of filter paper wet with ammonium hydroxide. Describe the result. What is the name of the product ? e. State other properties of hydrogen chloride observed during these experiments, e.g. color, odor, density, behavior with moist lit¬ mus paper. III. Properties of hydrochloric acid. — Remove the bottle in which the hydrogen chloride is being absorbed. a. Determine its general properties, e.g. taste (cautiously), ac¬ tion with litmus, and with magnesium (using 10 cc. of the hydro¬ chloric acid). State the results. b. Add to a test tube half full of the hydrochloric acid a few drops of silver nitrate solution. Describe the precipitate. What is its name? Shake the test tub*e, filter part of the contents, and expose the precipitate upon the paper to the sunlight. Describe the change in the precipitate which soon occurs. To the remaining contents of the test tube add considerable ammonium hydroxide, and shake. Describe the result. Note. — As soon as III b has been performed, add water to the flask, shake well, and pour the contents into a waste jar in the hood. 66 EXPERIMENTS IN PRACTICAL CHEMISTRY Experiment 66 — Test for Hydrogen Chloride, Hydrochloric Acid, and Chlorides a. Recall properties which would serve as a test for (i) hydrogen chloride and (2) hydrochloric acid. b. Apply the silver nitrate test to a solution of several soluble chlorides in separate test tubes (e.g. ammonium chloride, ferric chloride, and calcium chloride). State each result. Note. — It is customary, though not always necessary, to add nitric acid to dissolve compounds other than chlorides which might be formed in testing with silver nitrate. Experiment 67 — Aqua Regia Materials. — Gold leaf, concentrated nitric and hydrochloric acids. Touch a small piece of gold leaf with the end of a moist glass rod, and wash the gold leaf into a test tube by pouring a few cubic cen¬ timeters of concentrated hydrochloric acid down the rod. Warm gently. Does the gold dissolve? Wash another piece of gold leaf from a clean glass rod into another test tube with concentrated nitric acid. Warm as before. Does the gold dissolve ? Pour the contents of one tube cautiously into the other. Warm gently, if no change occurs. Does the gold dissolve ? Answer: 1. What compound of gold is formed by its interaction with aqua regia? 2. Does chlorine water act like aqua regia on gold? Experiment 68 — Insoluble Chlorides Materials. — Silver, lead, and mercurous nitrate solutions. a. Put about 5 cc. of silver nitrate, lead nitrate, and mercurous nitrate in separate test tubes, and label each tube. Add 5 cc. of dilute hydrochloric acid to each solution, shake, and note the result. Describe each precipitate. Name each. * b. Shake well, and pour about half of each precipitate into separate test tubes. Save the rest of the precipitates for c. Fill each of the three test tubes half full of water, and heat to boil¬ ing. Note each result. Which chloride dissolves in hot water? c. Fill each of the test tubes saved in b with ammonium hydroxide. Shake well. Warm gently. Note each result. What is the effect of ammonium hydroxide on each chloride? ACIDS, BASES, AND SALTS — NEUTRALIZATION 67 d. Optional. Test unknown solutions for (1) a chloride and (2) lead, silver, and mercurous compounds. State each result. Answer: 1. In what are these three chlorides insoluble ? 2. How could the three chlorides be separated from one another? 3. What is a test for (a) a soluble chloride, ( b) an unknown solution sup¬ posed to contain a chloride, (c) a lead compound, ( d ) a silver compound, (e) a mercurous compound, (/) lead chloride, ( g) silver chloride, ( h ) mer¬ curous chloride? 4. How can a chloride be distinguished from a sulphate? ACIDS, BASES, AND SALTS — NEUTRALIZATION (Practical Chemistry, pp. 142-146, §§ 161-167) Experiment 69 — General Properties of Acids Materials. — Litmus paper (both colors), magnesium ribbon, sodium carbonate. Fill three test tubes half full of water; add about 5 cc. of dilute sulphuric acid to one, of hydrochloric acid to another, and of nitric acid to the third. Shake the test tubes thoroughly, and label each. a. Dip a clean glass rod into each acid successively and cautiously taste it. Describe the taste by a single word. b. Dip a clean glass rod into each acid successively and put a drop on both kinds of litmus paper. Note the decided change in color. The change is characteristic of acids. c. Pour out the acids and replace the hydrochloric and sulphuric acids with dilute acid from the bottle. Omit the nitric acid. Slip a small piece of magnesium ribbon into each test tube. Note the results. If no marked chemical action results, warm gently. Test the most obvious product by holding a lighted match inside of each tube. What gas comes from the hydrochloric and sulphuric acids? d. Fill a test tube half full of dilute sulphuric acid, have ready a blazing joss stick, add a lump of sodium carbonate to one tube, and test the escaping gas. Do the same with the other two acids. What is the gas ? Experiment 70 — General Properties of Bases Materials. — Sodium hydroxide and potassium hydroxide solutions, am¬ monium hydroxide, litmus paper (both colors). Prepare a very dilute solution of each base as in Exp. 69. 68 EXPERIMENTS IN PRACTICAL CHEMISTRY a. Cautiously taste each liquid by touching to the tip of the tongue a rod moistened with each, and describe the result. Compare with acids. b. Test each solution with litmus paper (both colors). Describe the result. Compare with acids. c. Rub a little of each undiluted solution from the bottle between the fingers, and describe the feeling. Experiment 71 — A Property of Many Salts - i — .... - ) ^- ^ J I / / - ) Fig. 44. —Test wires — upper platinum, lower nichrome Materials. — Litmus paper (both colors), dilute solutions of chemically pure sodium chloride, potassium nitrate, potassium sulphate, barium chloride, potassium chlorate, potassium bromide, and strontium nitrate. a. Test the solutions with litmus paper. Describe the result in each case. Compare the litmus reaction of salts with the reaction of acids and bases. b. Dip a clean glass rod into each solution (except barium chloride) successively and cautiously taste it. Do not swallow the liquid. De¬ scribe the taste. Experiment 72 Composition of Acids, Bases, and Salts I. Acids. — a. Recall or devise an experiment to show that hydrogen is a constituent of acids, e.g. hydro¬ chloric, sulphuric, acetic. b. Recall or devise an experiment to show that another constituent of acids is a non-metallic element or group, e.g. Cl, S 0 4 . II. Bases. — a. Recall or devise an experiment to show that hy¬ droxyl (OH) is a constituent of bases. (See Exp. 32 a (3).) b. Show by the flame test that a constituent of bases is a metal, e.g. sodium, potassium, calcium, barium. Dip a clean test wire (Fig. 44) into each solution and hold the end of the wire in the flame Fig. 45. — Testing for metals by the color of the flame ACIDS, BASES, AND SALTS — NEUTRALIZATION 69 as in Fig. 45. The flame is colored yellow by sodium, pale violet by potassium, red by calcium, and green by barium. Concentrated calcium hydroxide, or the powdered substance, should be used. III. Salts. — a. Recall or devise experiments to show that a con¬ stituent of salts is a metal, e.g. sodium, potassium, calcium, barium, silver, lead, mercury (mercurous). b. As in a, also a non-metallic element or group of elements — the same as in I b. Answer: 1. What is a constituent common to acids ? To bases? 2. What class of elements, single or in groups, is a constituent of acids? Of bases ? 3. What classes of elements, single or in groups, are constituents of salts ? Experiment 73 — Testing for Acids and Bases Materials. — Lemon juice, vinegar, sweet and sour milk, wood ashes, faucet water, cream of tartar, the juice of any ripe fruit and any un¬ ripe fruit, household ammonia, potash, limewater, pickles, jelly, grape juice, lye, “unknowns.” Apply the litmus test to the substances enumerated above. Make a solution of each of the solids before testing. Tabulate the results under the terms, Acid and Basic. Experiment 74 — Neutralization Materials. — Sodium hydroxide (solid), blue litmus paper. Dissolve a small piece of sodium hydroxide in an evaporating dish one-third full of water. Add a little dilute hydrochloric acid, and stir thoroughly; continue to add the acid, until a drop of the well- mixed solution taken from the dish by a clean glass rod just reddens blue litmus paper. If the dish becomes too full, pour out some of the solution. Evaporate the solution to dryness by heating the dish on a gauze- covered ring. Heat until the yellow color (due to the slight excess of hydrochloric acid added) disappears, then moisten the whole residue carefully with a little warm water, and heat again to evaporate the last traces of acid; add and evaporate two portions of water. Test small portions of the residue. (1) Apply the litmus test. Has the residue acid, basic, or neutral properties? (2) Taste a little. Is it an acid, base, or salt ? (3) Dissolve some in water and 70 EXPERIMENTS IN PRACTICAL CHEMISTRY test the solution for a chloride. State the result. (4) Test for sodium by heating a little on a test wire in the flame. State the result. What is the residue? Write the equation for the re¬ action. Experiment 75 — Neutralization by Titration Object. — To find the number of grams of the compound HC 1 in 1 cc. of a solution of hydro¬ chloric acid (i.e. HC 1 dissolved in water) by neu¬ tralizing the acid with a solution of sodium hy¬ droxide of known concentration. Materials. — Phenol-phthalein solution, and so¬ lutions of hydrochloric acid and sodium hydrox¬ ide (the latter of known concentration and ob¬ tained from the Teacher). Apparatus. — Burettes, beakers, and glass rod as in Fig. 46, waste beaker. Copy the form of Record given below in the notebook and enter each volume as soon as the reading is made. Fill each burette (or start with each full) — one with the acid solution and one with the base solution (Fig. 46). Be sure the tip of the burette is free from air bubbles. Place the waste beaker under each burette in turn and allow the solution to run out slowly until the bottom of the meniscus rests on the o line when the eye is on a level with the same line. (See Fig. 47.) Fig. 46. — Burettes for accurate ex¬ periments in neu¬ tralization Set the waste beaker aside. Put a clean beaker under the base bu¬ rette and let exactly 15 cc. run into the beaker; enter in I in the Record. Remove the beaker, add 2 or 3 drops of phenol- phthalein solution, put the beaker under the acid burette, and let the acid solution run in slowly, stirring constantly with the clean rod until the red color just disappears and the solution becomes colorless. Read the exact volume of acid solution added and enter in I. 12- Fig. 47. — Meniscus (correct reading along line I) ACIDS, BASES, AND SALTS — NEUTRALIZATION 71 Record I. NaOH sol. o — 15 = 15 HC 1 sol. o - = II. NaOH sol. 15 — 30 = 15 HC1 sol. III. NaOH sol. 30 — 45 = 15 HC 1 sol. - .*. 1 cc. NaOH sol. = 1 cc. NaOH sol. = cc. HC 1 sol. 1 cc. NaOH sol. = cc. HC 1 sol. 1 cc. NaOH sol. = cc. HC 1 sol. cc. HCl sol. (average) Pour the solution out of this beaker, wash the beaker, and proceed, as before, with a second 15 cc. of NaOH solution. Enter in II. Wash the beaker and proceed with a third 15 cc. of NaOH solution. Enter in III. Calculation. — Our problem is to calculate the number of grams of HCl in 1 cc. of the solution of hydrochloric acid used in this ex¬ periment. (a) First write the equation for the reaction, thus : — HCl + NaOH = NaCl + H 2 0 36.5 40 58.5 18 This equation means that 36.5 gm. of HCl are needed to neutralize 40 gm. of NaOH. (b) Next find (from I, II, III, above) the average number of cubic centimeters of hydrochloric acid solution which would be neutralized by 1 cc. of sodium hydroxide solution. For example, suppose 1.5 cc. HCl sol. = 1 cc. NaOH sol. (Your result, of course, may be differ¬ ent from this value.) (c) Learn from the Teacher the concentration of the sodium hy¬ droxide solution. For example, suppose 1 cc. of sodium hydroxide solution contains 0.00641 gm. of NaOH. ( d ) Now from the equation in ( a ) we see that 40 gm. of NaOH re¬ quire 36.5 gm. of HCl. Then the number of grams of HCl required by 0.00641 gm. of NaOH would be found by the proportion 40 : 36.5 :: 0.00641 : x x = o 00585 (Your result depends on the concentration of your NaOH solution.) But 0.00585 gm. of HCl would be dissolved in 1.5 cc. of hydrochloric acid (according to our supposition in ( b )). Therefore, to find the number of grams of HCl that would be dissolved in 1 cc. of the acid solution, we divide 0.00585 by 1.5, i.e. 0.00585 -f- 1.5 = 0.0039. Ans. 0.0039 g m - HCl in 1 cc. 72 EXPERIMENTS IN PRACTICAL CHEMISTRY Experiment 76 — Preparation of a Salt by Various Methods Materials. — Calcium, calcium oxide, carbonate, and chloride, silver nitrate solution. a. Acid and a metal. — Put a small piece of calcium in an evapo¬ rating dish, add a little dilute hydrochloric acid, stand the dish on a gauze-covered ring, and heat gently in the hood until the calcium disappears, adding more acid if necessary. Then evaporate the solution to dryness; heat gently toward the end to prevent spatter¬ ing. Moisten the residue with water, and evaporate again to dry¬ ness. Heat the residue until no more fumes of hydrochloric acid are evolved. Let the dish cool, and loosen the solid with a glass rod. Test small portions of the residue for (i) calcium (flame test), and (2) a chloride. State the result. b. Acid and an oxide. — Proceed as in a, using hydrochloric acid and a small piece of calcium oxide. Test the final residue as in a. State the result. c. Acid and a salt. — Proceed as in a, using hydrochloric acid and a small piece of calcium carbonate. Test the final residue (as in a). State the result. d. Two salts. — Add silver nitrate solution to calcium chloride solution, and describe the result. Required Exercises. — 1. What is the name and formula of the resi¬ due in each part of this experiment? Write the equation for each re¬ action. 2. Suggest a simple experiment to verify the answer in 1. 3. Suggest experiments to prove that the residue is neither an acid nor a base. e. Acid and base. —Recall an experiment in which a salt was formed by the interaction of an acid and a base. Name all the com¬ pounds involved in the reaction. Write the equation. AMMONIA — AMMONIUM COMPOUNDS (Practical Chemistry, pp. 148-157, §§ 168-181) Experiment 77 —Ammonia (Gas) and Ammonium Hydroxide Materials. — Lime (calcium oxide), ammonium chloride, concentrated hydrochloric acid. Apparatus. — As in Fig. 48. The test tube A is provided with a one-hole AMMONIA — AMMONIUM COMPOUNDS 73 rubber stopper to which is fitted a glass tube B which reaches well up into the bottle C, 3 bottles, pneumatic trough filled as usual. Optional forms of apparatus (as in Fig. 49) may be used. Caution. — Do not inhale ammonia (gas). Perform this experiment in the hood. Weigh 10 gm. of lime and 10 gm. of ammonium chloride separately, and mix them thoroughly on. a piece of paper. Slip the mixture into A , and add a little water, thereby transforming the calcium oxide into calcium hydroxide. Mix well. Quickly insert the stopper with its tube, and clamp A as in Fig. 48. Stand the bottle C over the tube B. Heat A gently with a low flame. (Begin to heat the test tube near the closed end and slowly work forward to the delivery tube.) Ammonia (gas) will pass up into the bottle, which should be removed, when full, and covered tightly with a glass plate or filter paper. A piece of moist red litmus paper held near the mouth will show (by change in color) when the bottle is full. Do not smell at the mouth of the bottle. Collect two bottles of the gas. a. Test the gas in one bottle or test tube with a blazing joss stick. Ob¬ serve the result. Compare with the behavior of oxygen, carbon dioxide, hydrogen, and hydrogen chloride under similar circumstances. b. Invert the same bottle in the pneumatic trough, and shake it vig¬ orously, taking care to keep the mouth under water. Observe the change inside the bottle. What prop¬ erty of the gas is revealed? Is it a marked property? Test the contents of the bottle with litmus paper (both colors), and state the result. c. Pour a few drops of concentrated hydrochloric acid into an empty, warm, dry bottle. Rotate the bottle until the inside is well moistened with the acid. Cover it with a glass plate, invert it, and for preparing am¬ monia (gas) Fig. 48. — Apparatus for preparing am¬ monia 74 EXPERIMENTS IN PRACTICAL CHEMISTRY stand it upon a covered bottle of ammonia (gas). Remove both plates at once, and hold the bottles together by grasping them firmly about their necks. Observe the result. Describe the result, giving the evidence of the chemical action. What is the white substance? d. State other properties of ammonia (gas) you have observed in this experiment, e.g. color, odor, density, and behavior with moist litmus paper. Experiment 78 —Ammonia (Gas) from Various Substances Materials. — Gelatin, soda-lime, litmus paper, concentrated hydrochloric acid, substances enumerated in b, ammonium sulphate, ammonium nitrate, sodium hydroxide solution, calcium cyanamide (for f), am- moniacal liquor (for g). a. Mix a little gelatin and soda-lime on a piece of paper, slip the mixture into a test tube, attach a test tube holder, heat, and test the escaping gas with moist red litmus paper, or by a glass rod moistened with concentrated hydrochloric acid. State the result. b. Repeat a, using soda-lime with hair, feather, leather scraps, or pieces of horn. Observe and state the results. c. Dissolve a little ammonium chloride in water, add a little sodium hydroxide solution, warm gently, and test (cautiously) the liberated gas by its odor. What is the gas ? d. Repeat c, using ammonium sulphate and sodium hydroxide solution. State the result. e. Proceed as in d, using ammonium nitrate. Test (by the odor) the gaseous product, and state the result. f. Put about 5 gm. of calcium cyanamide in a test tube, add io cc. of water, shake, boil, and test for ammonia. State the result. g. Optional. Add powdered calcium oxide (lime) to a test tube half full of ammoniacal liquor, warm gently, and test the escaping gas for ammonia. State the result. Experiment 79 — Properties of Ammonium Salts Materials. — Ammonium chloride, sodium hydroxide, sand, ammonium nitrate, ammonium carbonate. a. Examine ammonium chloride and state its characteristic prop¬ erties. b. Add a few grams of ammonium chloride to a test tube half full of water, shake well, and observe the result. Does ammonium chloride dissolve easily in water? Add a little more of the salt, shake, NITRIC ACID — NITRATES — NITROGEN OXIDES 75 and note how the dissolving affects the temperature of the solvent. Save the solution for c. c. Add a small piece of sodium hydroxide to the solution from b, warm gently, and very cautiously observe the odor of the gaseous product. What is the gas? Explain its formation. d. Put a little crude ammonium chloride (or a mixture of ammo¬ nium chloride and sand) in a clean, dry test tube, heat the closed end gently, and observe the result. What is the white deposit? Heat intensely. Is there a residue? If so, compare it with the white deposit. What general name is given to this process? To the prod¬ uct? e. Add a little ammonium nitrate to sodium hydroxide solution in a test tube, warm gently, and cautiously note the gaseous product. What is it ? Moisten a glass rod with concentrated nitric acid and hold it at the mouth of the test tube (after warming again, if neces¬ sary). Describe the result. What is the product? f. Smell of a lump of ammonium carbonate. To what substance is the odor due? Moisten with water and smell again. What is the product ? Answer: 1. What is the test for ammonium compounds? 2 . What is the equation for the reaction in c? For the two reactions in e? Experiment 80 — Testing Salts (Review) Materials. — Chlorides, sulphates, carbonates, and nitrates of sodium, potassium, calcium, barium, and ammonium; nitrates of silver, lead, and mercury; dilute hydrochloric acid. Obtain several “ unknowns ” from the substances enumerated above and test a separate portion of each for (a) the metal part, i.e. sodium, potassium, calcium, barium, silver, lead, ammonium, and (b) the non-metal part, i.e. a chloride, a sulphate, and a carbonate. State each result. Give the name and formula of each salt. NITRIC ACID — NITRATES — NITROGEN OXIDES (Practical Chemistry, pp. 159-170, §§ 182-197) Experiment 81 — Nitric Acid Materials. — Sodium nitrate, concentrated sulphuric acid, quill tooth¬ pick, copper wire, zinc, magnesium ribbon. Apparatus. — Glass stoppered retort, etc., as in Fig. 50. 76 EXPERIMENTS IN PRACTICAL CHEMISTRY Caution. — Concentrated nitric acid and sulphuric acid are very corrosive. Do not spill them on the flesh or the clothing. Note. —I may be omitted and II done with concentrated nitric acid from the laboratory bottle. I. Preparation. — Weigh 20 gm. of sodium nitrate and slip it into the retort through the tubulure. Fill the bottle nearly full of water. Put a large empty test tube into the bottle, insert the neck of the retort into the test tube, and arrange the apparatus as shown in Fig. 50. Stand a funnel in the tubulure of the retort so that the end is well inside the bulb, and pour 20 cc. of concentrated sulphuric acid through the funnel. Remove the funnel and insert the stop¬ per of the retort tightly. Heat the retort gently as long as any nitric acid runs down the neck into the test tube. Then unclamp the retort and remove the test tube carefully, taking care not to get any nitric acid on the hands. Note. — Allow the contents of the retort to cool, add a little water, boil until the solid in the bulb is reduced to a small bulk or dissolved, and pour it into a waste jar in the hood. II. Properties. — a. Observe the color of the concentrated nitric acid prepared in I. Compare it with the concentrated nitric acid in several bottles in the laboratory and with the typical specimen of concentrated nitric acid placed upon the side shelf by the Teacher. State the result. b. Hold a piece of wet filter paper at the mouth of the test tube of concentrated nitric acid. Observe and state the result. c. Repeat b, using a piece of filter paper moistened with ammo¬ nium hydroxide. What is the name of the product? d. Pour 5 cc. of concentrated nitric acid very carefully into a test tube, drop in a piece of a quill toothpick, and observe any change in the color of the quill. Heat very gently, and observe the effect on the quill. State the final result. Fig. 50. —Apparatus for preparing nitric acid in the laboratory NITRIC ACID — NITRATES — NITROGEN OXIDES 7 7 e. Put about 1 gm. of sulphur in a test tube, add a little water and then very carefully 5 cc. of concentrated nitric acid. Attach the test tube holder, and boil cautiously — in the hood — for a few minutes. Add 10 to 15 cc. of water, filter the solution, if it is not clear, and test the filtrate for a sulphate by adding barium chloride solution. State the result. Explain it. f. Stand three test tubes in the test tube rack, put a piece of zinc into one, copper into another, and magnesium ribbon (rolled into a ball) into the third. Add a little concentrated nitric acid to each test tube. Observe the result. Test the gaseous product for hydro¬ gen, and state the result. Required Exercises. — 1. What property of nitric acid was shown by b? Byd? Bye? 2. How does the action in b and c compare with that of hydrochloric, acid under similar circumstances? 3. Apply Exercise 2 to f. (If in doubt, try the experiment.) Experiment 82 — Properties of Nitrates Materials. — Copper nitrate, lead nitrate, potassium nitrate, charcoal. a. Put a little copper nitrate in a test tube, attach the holder, heat gently, and observe the result, especially the color of the gaseous product and of the final solid product. Test the gaseous product for oxygen. State the result. Devise an experiment to determine the qualitative composition of the solid product; consult the Teacher before proceeding. b. Pulverize a little lead nitrate and proceed with it as in a. State the results. c. Proceed as in Exp. 9 a. Experiment 83 — Interaction of Nitric Acid and Metals Materials. — Zinc, copper, tin, iron, concentrated nitric acid. Stand four test tubes in the test tube rack. Slip into one a few pieces of zinc, into another a small piece of tin, into the third a small quantity of copper borings, and into the fourth a small quantity of clean iron filings. Add to each test tube in succession enough con¬ centrated nitric acid to cover the metal. Warm slightly, if there is no action. Observe and describe the changes, particularly (1) the vigor of the action, (2) the properties of the solid products, espe¬ cially color and solubility, and (3) the properties of the gaseous prod- 78 EXPERIMENTS IN PRACTICAL CHEMISTRY ucts. Name the solid product and the gaseous product of the re¬ action in each case. Experiment 84 — Test for Nitric Acid and Nitrates Materials. — Ferrous sulphate, sodium nitrate. a. To io cc. of water add i or 2 cc. of concentrated nitric acid and shake. Prepare a ferrous sulphate solution by dissolving a clean crystal in 10 cc. of cold water. Pour this solution into the nitric acid. Mix well. Incline the test tube and pour about 5 cc. of concentrated sulphuric acid down the inside of the tube. The sulphuric acid will sink through the other liquid. At the surface where the two solutions meet, a brown or black layer will appear (Fig. 51). b. Proceed as in a, using a concentrated solution of sodium nitrate instead of nitric acid. Record the result. Experiment 85 — Nitric Oxide and Nitrogen Dioxide Materials. — Copper (borings or fine pieces of sheet metal), concentrated nitric acid, piece of copper wire (15 cm. or 6 in. long). Put 10 gm. of copper in the bottle, and arrange the apparatus to collect the gas over water (Fig. 52). Fill three bottles with water, and invert one of them in the trough. Have the others ready. Dilute 25 cc. of concentrated nitric acid with an equal volume of water, and introduce just enough of this dilute acid through the dropping tube to cause gentle chemical action. If the action is too vigorous, add water through the dropping tube; if too weak, add a little of the dilute nitric acid. Fig. 51. — Test Collect three bottles of the gas, which is nitric for nitric acid oxide, and cover them with glass plates, and nitrates a. Observe the general properties of nitric oxide while covered. b. Uncover a bottle. Observe the result. Is the brown gas, which is formed, identical in color with the one observed in the gen¬ erator at, the beginning of the experiment? What is the brown gas? c. Uncover a bottle, let the brown gas form, then pour in about 25 cc. of water, cover with the hand and shake vigorously, still keep¬ ing the bottle covered. Does the brown gas disappear? NITRIC ACID — NITRATES — NITROGEN OXIDES 79 d. With the third bottle, determine whether the gases will burn or support combustion. A convenient flame is a burning match Fig. 52. — Apparatus for preparing nitric oxide fastened to a copper wire. Uncover a bottle and plunge the lighted match quickly to the bottom of the bottle and immediately replace the glass plate. Observe the result. Remove the glass plate and observe the result. Required Exercises. — 1. Sum¬ marize the properties of nitric oxide. Of nitrogen dioxide. 2. What is the general chemical relation of the two gases to each other? To the air? 3. Why cannot nitrogen dioxide be collected over water? Experiment 86 — Preparation and Properties of Nitrous Oxide Materials. — Ammonium nitrate, wad of iron thread, copper wire, sul¬ phur, joss stick. Put 10 gm. of ammonium nitrate in the flask A . Construct and arrange the apparatus as shown in Fig. 53. The large test tube B remains empty. The end of H rests on the bottom of the pneumatic trough, which is filled as usual. Be sure the apparatus does not leak. I. Preparation. — Heat the flask gently with a low flame, and read¬ just the appara¬ tus if it leaks. The ammonium nitrate melts at first and soon ap¬ pears to boil, owing p IG ^ — Apparatus for preparing nitrous oxide to the decomposi¬ tion of the salt and escape of nitrous oxide. Regulate the heat so 8 o EXPERIMENTS IN PRACTICAL CHEMISTRY that the evolution of the nitrous oxide is slow. Notice the liquid which collects in B. Collect three bottles of nitrous oxide, cov¬ ering each with a piece of filter paper as soon as removed from, the trough. When the last bottle has been collected and covered, remove the end of the delivery tube from the trough. II. Properties. — a. Allow a bottle to remain uncovered for a few seconds. How does nitrous oxide differ from nitric oxide ? Nitrogen dioxide ? b. Thrust a glowing joss stick into the same bottle of gas. Ob¬ serve the result. Is the gas combustible ? Does it support combus¬ tion? c. Put a piece of sulphur in a deflagrating spoon, light it, and lower the burning sulphur at once into another bottle of gas. Observe the result. d. Twist one end of the copper wire around a wad of iron thread. Heat the edge of the wad an instant in the flame and then lower it quickly into a bottle of the gas. Observe the result. Recall a simi¬ lar experiment with oxygen. Compare the two results. Required Exercises. — i. Summarize the essential properties of nitrous oxide. 2. What is the other product (seen in B) of the chemical change in this experiment ? 3. How could you distinguish ammonium nitrate from other nitrates? 4. How could you distinguish nitrous oxide from ( a ) the other oxides of nitrogen, ( b ) air, (c) oxygen, ( d) hydrogen, ( e ) nitrogen, (/) carbon dioxide ? MOLECULAR WEIGHTS (Practical Chemistry, pp. 171-180, §§ 198-208) Experiment 87 — Weight of 22.4 Liters of Carbon Dioxide Object. — To find the volume of carbon dioxide liberated from a weighed amount of calcium carbonate and to calculate the weight of 22.4 1. of this gas. Materials. — Crystallized calcium carbonate, concentrated hydrochloric acid. Apparatus. — As in Fig. 54, glass plug for stopper of A. A is a 125 cc. Erlenmeyer flask in which the carbon dioxide is generated. The large bottles C and E are dry and empty. G is a 750 cc. bottle filled with water and inverted in the pneumatic trough as usual. MOLECULAR WEIGHTS 81 Copy the form of Record as given below in your notebook and enter each item as soon as the weighing or measuring is made. Construct and ar¬ range the apparatus as in Fig. 54. Put 20 cc. of concentrated hydrochloric acid and 5 cc. of water in A, mix well, add a small piece of unweighed cal¬ cium carbonate, insert the stopper loosely, and let the flask remain undisturbed until the calcium carbonate dis¬ appears ; the object of this is to fill A with carbon dioxide before weighing (since it is full of the gas at the end). Meanwhile weigh accurately on the balance 2.5 to 3 gm. of calcium carbonate. (See Introduction, § 8, for instructions about weighing.) Enter the weight as ( b ) below. When the evolution of gas stops in A insert a glass plug in the hole of the stopper and weigh the whole on the balance. Record the weight as (a) below. Remove and preserve the plug. Fig. 54. - Apparatus for finding the weight of 22.4 liters of carbon dioxide Record Thermometer (/).... 0 Barometer ( P ') . . mm. (a) Weight of flask, stopper, plug, and acid. gm. (b) Weight of calcium carbonate. gm. (c) Weight of flask, stopper, plug, etc. — before action . . gm. (1 d ) Weight of flask, stopper, plug, etc. — after action --gm. (e) Weight of carbon dioxide ( (c) — (d) ). gm. (/) Volume of carbon dioxide (observed). cc. ( g ) Volume of carbon dioxide (corrected). cc. (h) Weight of a liter of carbon dioxide . gm. ( i ) Weight of 22.4 liters of carbon dioxide. gm. Carefully push A with its stopper upon the tube B, remove the flask, hold it near the stopper, slip in the weighed calcium carbonate and instantly push the flask firmly upon the stopper. The carbon dioxide soon forces air into G. If no bubbles arise in G, examine the apparatus for a leak and quickly readjust, if necessary. Let the operation continue until the gas ceases to rise in G. Then 82 EXPERIMENTS IN PRACTICAL CHEMISTRY carefully joggle G to dislodge any bubbles which may be underneath the support. Slide the bottle from the support down upon the bot¬ tom of the trough. Add water to the trough, if the level is below the level inside the bottle; if unnecessary, raise the bottle until the water is at the same level inside and outside. Slip two pieces of filter paper beneath the bottle, cover the mouth firmly, invert and remove, and stand it right side up on the table. Stand a thermome¬ ter in the bottle, and read and record the temperature (t) after a few moments. Also read and record the barometer (P'). Fill a large graduate (preferably 1000 cc.) with water to the mark and pour water carefully from the graduate into G until full. Read the exact volume of the water added to G and record as (/); this is the volume of carbon dioxide liberated. Correct it for temperature, pressure, and aqueous tension by the method given in Exp. 24. Enter the corrected volume as (g). Weigh A with its contents, stopper, and plug, and enter the weight as ( d ). From the weight of carbon dioxide ( (c) — (d) ) and the corrected volume (g) calculate the weight of a liter, and record as (h) above. Multiply this weight {h) by 22.4 and record as (t). Answer: 1. What is the exact weight of a liter of carbon dioxide? What weight did you obtain? What is the class average? 2. What is the weight of 22.4 liters of carbon dioxide calculated from the class average of the weight of one liter? 3. What is the weight of 22.4 liters of oxygen calculated from the class average of Exp. 24? EQUIVALENT WEIGHTS (Practical Chemistry, pp. 182-190, §§ 209-216) Experiment 88 — Equivalent of Zinc (to Hydrogen) Object. — To find the number of grams of zinc chemically equivalent to one gram of hydrogen. Apparatus. — As in Fig. 55, pneumatic trough (not zinc), thermometer, barometer. Copy the form of Record in the notebook and enter each weight or volume as soon as the weighing or measuring is made. Construct and arrange the apparatus (Fig. 55) to collect a gas over water, and have it inspected by the Teacher. EQUIVALENT WEIGHTS 83 Weigh from 0.45 to 0.5 gm. of zinc on the balance. Take a single piece and weigh it exactly. Enter in the Record as Zn. Record Weight of zinc taken {Zn) . Observed volume of hydrogen (F') . . Temperature (t) . Pressure (P') . Vapor pressure ( a ). Corrected volume of hydrogen (F) . . Weight of corrected volume of hydrogen (W) Equivalent of zinc (£). Put the weighed zinc into the bottle A. Fill the bottle with water and insert the stopper with all its tubes. Next fill the re¬ mainder of the apparatus with water by first filling the cup with water and then admitting it repeatedly until all air is forced out of the bottle and tubes; take care never to let the water in B fall below the lower opening of the cup. Note that the inner end of the tube C does not extend below the stopper. Fill a 250 cc. bottle with water and invert it upon the Fig ' 55 -- Apparatus for finding the support in the trough (a sheet equivalent of zinc zinc trough must not be used). Put the end of the delivery tube under the support and ask for a final inspection. Heat about 50 cc. of dilute sulphuric acid in a test tube. Fill the cup and introduce the hot acid in separate por¬ tions slowly into the bottle A, taking the same care as before. The liberated hydrogen will slowly accumulate in the receiving bottle. Let the action continue until the zinc is used up. Then force over into the collecting bottle all gas in the apparatus by admitting water carefully as before. Lay a piece of dry filter paper upon the bottom of the bottle, grasp the bottle firmly, carefully joggle it to dislodge any gas bubbles which may be underneath the support, gm. cc. o mm. mm. cc. gm. gm. 84 EXPERIMENTS IN PRACTICAL CHEMISTRY slide the bottle from the support, and lower it into the water until the water is at the same level inside and outside the bottle; then slip two pieces of filter paper beneath the bottle, cover the mouth firmly, lift the bottle from the trough and stand it, right side up, upon the table. Stand a thermometer in the trough. Fill a 250 cc. graduate exactly to the mark with water, remove the paper cover from the bottle, and very carefully fill the bottle with water from the graduate; read and enter (as V') the exact volume of water added; this is the volume of hydrogen liberated. Read the thermometer while the bulb is in the water, and enter as t. Read the barometer, and enter as P'. Find the vapor pressure correspond¬ ing to the observed temperature (see Appendix, § 4), and enter as a. Correct the observed volume (F') of hydrogen for temperature, pressure, and vapor pressure, and enter as F. Since 1000 cc. of dry hydrogen weigh 0.09 gm., the weight ( W ) of the corrected volume (F) is found by 1000: F :: 0.09 : IF. And the weight of zinc equiva¬ lent ( E ) to one gram of hydrogen is found by W : Zn :: 1 : E. Enter the equivalent of zinc as E. Submit the result to the Teacher before taking the apparatus apart. Required Exercises. — 1. Calculate the atomic weight of zinc by multiplying the equivalent weight (found in this experiment) by 2. 2. Compare this calculated atomic weight with the approximate atomic weight. 3. Calculate, as in Exercise 1, from the class average. 4. Compare the number obtained in 3, as in Exercise 2. Experiment 89 — Equivalent of Magnesium (to Hydrogen) Object. — To find the number of grams of magnesium equivalent to 1 gm. of hydrogen. Materials. — Magnesium ribbon, concentrated hydrochloric acid. Apparatus. — A 100 cc. tube, pneumatic trough (not zinc), thermometer, barometer, tall jar ( e.g . 1000 cc. graduate). Prepare a form of Record like that in Exp. 88 and enter the items, when available, in the proper place. Weigh accurately from 0.06 to 0.07 gm. of magnesium ribbon, preferably in a single piece. Enter the exact weight as Mg. Have the trough (not zinc) half full of water. Pour 10 cc. of concentrated hydrochloric acid into the 100 cc. tube and fill the tube completely with cold water. Put the magnesium into the water in the tube, cover the end of the tube with the thumb or finger, invert and stand EQUIVALENT WEIGHTS 85 it in the trough, but keep the end loosely closed to prevent the mag¬ nesium from slipping out. As the acid sinks through the water and reaches the magnesium, action begins vigorously. Hydrogen rises rapidly in the tube and usually carries the magnesium with it. Watch the operation, and shake the tube to prevent the magnesium from sticking to the inside. If a piece of magnesium should stick to the inside of the tube, close the end of the tube tightly, lift it from the water, incline it enough to let the liquid run down and loosen the magnesium, and then quickly put the end of the tube beneath the water. When all the magnesium has disappeared, close the end of the tube, remove the tube to a tall jar of water, and let it stand five or more minutes; then, by a clamp (without touching the tube with the hands) adjust the height so that the water levels are the same inside and outside of the tube. Read the volume of hydrogen, and enter as the observed volume (F')« Read the barometer and the ther¬ mometer (keeping the bulb in the water). Correct the observed volume (F 7 ) for temperature, pressure, and vapor pressure, and enter as the corrected volume ( V '). Find the weight (IF) of this volume (F) of hydrogen. Calculate the equiva¬ lent of magnesium to hydrogen, as in Exp. 88. Enter the equiva¬ lent of magnesium as E. Required Exercises. — As in Exp. 88. Experiment 90 — Equivalent of Aluminium (to Hydrogen) Proceed as in Exp. 88. Use about 0.17 gm. of aluminium (taking care to weigh exactly the amount used). Use hot concentrated hy¬ drochloric acid instead of dilute sulphuric acid. Record and cal¬ culate as in Exp. 88. Required Exercises. — As in Exp. 88. Note. — The multiplier in Exercise 1 is 3. Experiment 91 — Equivalent of Calcium (to Hydrogen) Proceed as in Exp. 89. Use about 0.11 gm. of calcium. Record and calculate as in Exp. 89. Required Exercises. — As in Exp. 88. Experiment 92 — Equivalent of Zinc (to Oxygen) Object. — To prepare zinc oxide from a weighed amount of zinc and to find the relative weights of zinc and oxygen. 86 EXPERIMENTS IN PRACTICAL CHEMISTRY Apparatus. — Evaporating dish fitted with a glass cover, pointed glass tube, water bath. Copy the form of Record given below in your notebook, and enter each weight as soon as the weighing is made. Clean and dry an evaporating dish. Weigh it on the balance accurately. Put about i gm. of zinc in it, weigh again, and enter the exact weight. Record Weight of dish and zinc. gm. Weight of dish. gm. Weight of zinc. gm. Weight of dish and zinc oxide I gm., II gm., Ill gm. Weight of dish. gm. Weight of zinc oxide. gm. Weight of zinc. gm. Weight of oxygen. gm. Stand it on a crucible block, add 5 cc. of water, cover the dish with a glass cover (preferably a watch glass — convex side down), and add concentrated nitric acid, a little at a time, by letting the acid run into the dish from a pointed tube held in the opening between the cover and the lip of the dish. Add acid at intervals until the zinc disappears. Then remove the glass cover, hold it edgewise over the dish, and rinse off the drops into the dish by pouring a little water upon the upper part of the cover. Stand the dish on a water bath and let the liquid evaporate (with¬ out the glass cover). When only a small amount of sirupy liquid is left, transfer the dish from the water bath to a crucible block, carry it to the hood, stand it on a gauze-covered ring, and heat very gently with a low flame. Hold the burner in the hand, and regulate the heat to prevent spattering. Continue to heat as the mass thickens and gives off red fumes; as soon as the mass becomes perfectly dry, heat strongly for about five minutes. Cool, weigh, and enter the weight as I. Heat again intensely for five minutes, cool, weigh, and enter as II. If the weights are not the same, submit the result to the Teacher. A third heating and weighing may be necessary. The zinc was changed to zinc nitrate by the acid, and the nitrate to zinc oxide by heating. The equivalent weight of oxygen is 8. Calculate the equivalent weight of zinc to oxygen. Submit the re¬ sult to the Teacher before removing the zinc oxide from the dish. Required Exercises. — As in Exp. 88. IONS AND IONIZATION *7 Experiment 93 — Equivalent of Zinc (to Chlorine) Object. — To prepare zinc chloride from a weighed amount of zinc and to find the relative weights of zinc and chlorine. Apparatus. — As in Exp. 92, desiccator (optional). Prepare a form of record like that in Exp. 92, substituting chloride for oxide and chlorine for oxygen. Weigh a clean, dry porcelain dish accurately. Add from 1.5 to 2 gm. of zinc, and weigh exactly. Record each weight. Introduce concentrated hydro¬ chloric acid (instead of nitric acid) into the covered dish as in Exp. 92. Evaporate on the water bath until nothing escapes from the dish. Then transfer the dish to a gauze- covered ring and heat gently with a low flame to remove the last portion of water. Zinc chloride is volatile at a low temperature. Hence, it must be heated gently. Remove the flame as soon as fumes begin to appear. Pass the flame over the surface occasionally to assist the removal of the last traces of water. When it is judged that all the water has been removed, put the dish in a desiccator (Fig. 56), let it cool, and then weigh. Zinc chloride is deliquescent. Hence the dish and contents must be weighed quickly. It is hardly possible to get weights which agree, but the variation should not be much. The equivalent of chlorine is 35.5. Calculate the equivalent of zinc to chlorine. Submit the result to the Teacher before removing the contents from the dish. Required Exercises. — As in Exp. 88. IONS AND IONIZATION (Practical Chemistry, pp. 201-216, §§ 230-247) Experiment 94 — Electrolytes and Non-Electrolytes (Demonstration Experiment) Object. — To find out whether a substance forms a conducting or a non¬ conducting solution. Materials. — Hydrochloric acid, sodium hydroxide, calcium chloride, sugar, alcohol, glycerin. Fig. 56. — A desiccator for keeping zinc chlo¬ ride dry §8 EXPERIMENTS IN PRACTICAL CHEMISTRY Apparatus. — As in Fig. 57. A is a beaker for the solution, B and C are electrodes (of aluminium or platinum) which are supported on the top of the beaker by a strip of wood. D is an electric light bulb which is connected with the wire from the electrode B and with one end of the wire E. The wire from the electrode C and the other end of the wire E are connected with the street current (reduced) or with a storage battery. a. Construct and ar¬ range the apparatus as in Fig. 57. Fill the beaker two-thirds full of dilute hydrochloric acid, see that all connections are tight, and turn on the current. Does the bulb glow ? Why ? b. Proceed as in a, using successively solu¬ tions of sodium hydrox¬ ide, calcium chloride, Fig. 57. — Apparatus for showing what solu¬ tions conduct electricity sugar, alcohol, and glycerin. Clean the beaker each time. Observe and state each result. Answer: 1. What substances form solutions which conduct electricity? 2. What substances form non-conducting solutions? 3. What is the name of the classes of substances in 1 ? In 2 ? Experiment 95 — Chemical Behavior of Solutions of Salts Materials. — For a, solutions of silver nitrate, silver sulphate, and chlorides of ammonium, barium, calcium, magnesium, sodium, and potassium; potassium chlorate, potassium perchlorate. For c, solutions of barium chloride, barium nitrate, sulphates of copper, sodium, aluminium, mag¬ nesium, and zinc. a. Test separately a dilute solution of the substances enumerated under a by adding a few drops of silver nitrate solution. State the result in each case. b. Add a few drops of silver sulphate solution to several of the solutions used in a. State the result. c. Test separately a dilute solution of substances enumerated under c, by adding to each a few drops of barium chloride solution. State the result in each case. IONS AND IONIZATION d. Proceed as in c, using a few drops of barium nitrate solution in place of barium chloride. Required Exercises. — i. What ion is common to solutions of chlo¬ rides? Of sulphates? 2. Explain the general result in a in terms of the theory of ionization. Also the results in b. 3. What ion is in solutions of all barium salts? All silver salts? 4. What ion other than hydrogen is in a solution of sulphuric acid? What ion other than potassium ion is in a solution of potassium chlorate ? Of potassium perchlorate ? 5. What ion is in solutions of all acids? Of all bases? Of all sodium salts ? 6. Make a list df the salts used in the whole experiment and their cor¬ responding ions, indicating the ions by name and formula. Experiment 96 — Electrolysis of Copper Sulphate Solution — Short Method (Demonstration Experiment) Material. — Dilute copper sulphate solution. Apparatus. — Small battery jar (or beaker), two electrodes (pieces of electric light carbon) and connection wires, battery of four or more cells (or other source of electric current). Fill the battery jar about two-thirds full of dilute copper sulphate solution. Wind the end of a piece of the wire around one end of each electrode and hang the electrodes in the solution by bending the wire over the edge of the jar (or supporting them by a strip of wood which rests across the top of the jar). Connect the ends of the wires with the battery. Before turning on the current (or making the final connection ) t examine each electrode and note the absence of a deposit. Turn on the current and observe at which electrode bubbles of gas form. Let the current run about ten minutes, and then examine each electrode. Compare with their appearance before the electrolysis took place. Upon which electrode (anode or cathode) is there a deposit? What is the deposit? Sketch the apparatus, and describe the electrolysis of copper sul¬ phate in terms of the theory of ionization, using the sketch in your interpretation. go EXPERIMENTS IN PRACTICAL CHEMISTRY Experiment 97 — Electrolysis of Copper Sulphate Solution — Long Method (Demonstration Experiment) Materials. — Copper sulphate solution, joss stick. Fill the Hofmann apparatus (Fig. 58) full of copper sulphate solu¬ tion. Connect with a reduced street current or a storage battery. Turn on the current and let it run until about 10 cc. of gas collects. At which electrode (anode or cathode) was a gas liberated? A solid deposited? Have a glowing joss stick ready, let out a little gas, and test it with the glowing joss stick. What is the gas ? What is the solid ? Answer: 1. What ions are in copper sulphate solution ? 2. To what electrode does each kind of ion mi¬ grate? 3. What happens when the ions reach the elec¬ trodes? 4. What secondary action takes place at one elec¬ trode ? Experiment 98 — Electrolysis of Sodium Sulphate Solution (Demonstration Experiment) Fig. 58. —Hofmann Materials. — Sodium sulphate solution, neutral apparatus for litmus solution, joss stick, wax taper, showing electrol) - jqq t p e Hofmann apparatus (Fig. 58) full of sodium sulphate solution colored with neutral litmus solution. Proceed as in Exp. 97. Let the current run until the smaller volume of gas measures about 10 cc. Observe the color of the solution in each tube; also the relative quantity of gas. Test the gases as in Exp. 49. State the result. Interpret the electroly¬ sis of sodium sulphate by the theory of ionization. Answer: 1. What is the name of each gas? 2. At which electrode was each gas liberated? 3. Why was the color changed in each tube? IONS AND IONIZATION 9i Experiment 99 — Electrolysis of Potassium Iodide Solution (Demonstration Experiment) Materials. — Starch, potassium iodide. Apparatus. — Sheet of metal (tin or irori), battery of two or more cells. Grind together in a mortar a lump of starch and a crystal of potas¬ sium iodide. Add enough water to make a thin liquid. Dip a piece of filter paper into the mixture, and spread the wet paper upon the sheet of metal. Press the end of one wire upon the metal, and draw the end of the other wire across the sheet of paper. Observe the result. If there is no result, reverse the ends of the wires. The dark marks are caused by iodine which is liberated from the potas¬ sium iodide and colors the starch. Required Exercises. — i. Describe briefly this experiment. 2. Iodine is a non-metal. Are iodine ions anions or cations? At what electrode is iodine liberated? Experiment 100 — Dissolved Substance and Boiling Point Materials. — Sodium chloride, sugar (both finely powdered). Apparatus. — Thermometer, 250 cc. Erlenmeyer flask. a. Stand a 250 cc. Erlenmeyer flask on a gauze-covered ring at¬ tached to an iron stand and clamp it about the neck. Pour 100 cc. of water into the flask, heat the water to boiling, hold the thermom¬ eter in the steam a minute or two, then lower it into the water, and observe the highest temperature. Record, and call this the boiling point. Remove the burner, and carefully slide 10 gm. of sodium chloride from a creased paper into the flask, taking care not to let any of the solid stick to the inside of the flask. Heat to boiling, and as soon as the solution boils steadily, observe and record the temperature. In the same way add another 10 gm. portion of sodium chloride, and find the boiling point of the solution. Compare the three boiling points. What effect has dissolved sodium chloride on the boiling point of water? b. Proceed as in a, using finely powdered sugar in place of sodium chloride. Compare the general result with a. Answer: 1. What effect has a dissolved substance on the boiling point of water? 2. Does the effect differ with the substance (in comparable solutions)? How? Why? 92 EXPERIMENTS IN PRACTICAL CHEMISTRY 3. Does the effect differ with the quantity of the substance (in the same quantity of water) ? How? Why? 4. Suppose a mole of sugar were dissolved in 1000 gm. of water, how would it affect the boiling point? Would the effect of a mole of sodium chloride be the same or different? Why? Experiment 101 — Dissolved Substance and Freezing Point Materials. — Ice, finely powdered sodium chloride and sugar. Apparatus. — Bottle, thermometer. a. Fill the bottle one-third full of cold water, drop in several small pieces of ice, and shake well. Insert the thermometer, stir, and ob¬ serve the lowest temperature. Make at least three readings. Re¬ cord the temperatures. Call the lowest one the freezing point of water (although it may be a little higher than the actual freezing point). Carefully slide 10 gm. of sodium chloride into the bottle, shake a minute or two, then stir with the thermometer, and observe and re¬ cord the lowest temperature. Proceed in the same way with another 10 gm. portion of sodium chloride. Compare the lowest temperatures. Compare them with the lowest temperature of the water. What effect has dissolved sodium chloride on the freezing point of water? b. Proceed as in a, using sugar in place of sodium chloride. Com¬ pare the general result with a. Answer: 1. Apply 1 in Exp. 100 to the freezing point of water. 2, 3, 4. As in Exp. 100. Experiment 102 — Colored and Colorless Ions Materials. — Solutions (dilute) of copper sulphate, copper nitrate, cop¬ per bromide, nickel chloride, nickel sulphate, cobalt chloride, cobalt nitrate, potassium dichromate, ammonium dichromate, sodium dichro¬ mate, potassium chromate, potassium permanganate — prepared for the class. a. Observe and state the color of the copper solutions. To what ion is the color due? Give its ionic name and formula. Are the other ions in the copper solutions colored or colorless? What is a simple proof of your answer? b. As in a with the nickel, etc., solutions. Required Exercises. — 1. Write the formula of each substance and the corresponding ions. SULPHUR — SULPHIDES 93 2. Make a list of colored ions. 3. Make a list of 10 colorless anions. Of 10 colorless cations. Experiment 103 — Ionization and Concentration (Demonstration Experiment) Apparatus. — Oblong battery jar or deep dish, carbon electrodes which reach to the bottom of the jar, separatory funnel (100 cc.), source of electric current ( e.g . street current — direct), and two 40-watt bulbs. a. Fill the jar nearly full of water. Insert the electrodes in the water, put the two bulbs in the circuit, make the proper connections, and turn on the current. Note the effect on the bulbs. Turn off the current. b. Put about 50 cc. of concentrated sulphuric acid in the separa¬ tory funnel, let enough run out to fill the stem, and quickly lower the stem into the water until the end rests on the bottom of the jar. Let the acid run in slowly beneath the water. Lift out the funnel. Turn on the current. Note the effect on the bulbs. Compare with a. c. Stir the acid slowly into the water and note the result, as in b. Compare with a and b. Required Exercises. — 1. Describe the experiment (using a sketch of the apparatus). 2. What does this experiment show about the comparative conductivity of water, concentrated sulphuric acid, and dilute sulphuric acid? 3. In which is there greater ionization, concentrated or dilute sulphuric acid? 4. How does this experiment show the relation of ionization to concentration ? SULPHUR — SULPHIDES (Practical Chemistry, pp. 218-227, §§ 248-258) Experiment 104 — Physical Properties of Sulphur Materials. — Brimstone, flowers of sulphur, lump of sulphur, thread. Apparatus. — Graduated cylinder (500 cc.). a. Examine and describe specimens of brimstone and flowers of sulphur. b. Tie a thread around a lump of sulphur, and weigh it on the scales. Slip it carefully into a graduated cylinder (Fig. 59) previ¬ ously filled with water to a known point. Note the increase in the volume of water. The increase in volume equals the volume of the 94 EXPERIMENTS IN PRACTICAL CHEMISTRY cc sulphur. Calculate the specific gravity by: Sp. gr. = Wt. of sul¬ phur -7- Wt. of equal vol. of water. State the result. c. Fill a test tube one-fourth full of small lumps of sulphur, attach the test tube holder, and heat until all the sulphur is melted. Ob¬ serve the color and consistency. Heat intensely, and observe the result. Continue to heat until the sulphur boils and then observe as before. Let the test tube cool, and save it for Exp. 108. Summarize the effects of heating sulphur. Note. — If the test tube should break during the heating, extinguish the burning sulphur with sand. Experiment 105 - Chemical Properties of Sulphur Fig. 59. — Appa- Materials. — Sulphur, iron thread. ratus for finding Set £ re to a sulphur i n a deflagrat- the specific grav- . , . . ^ ity of sulphur in g spoon, and lower the spoon into a bottle. Cautiously waft the fumes toward the nose, and observe and describe the odor. What is the product of burning sulphur ? b. Fill a test tube one-fourth full of iron thread, and add an equal bulk of flowers of sulphur. Heat the part containing the sulphur —• gently at first and then intensely until there is marked evidence of chemical action. Remove the test tube from the flame as soon as the action begins. Observe and describe the result. What is the name of the product of the chemical change? Experiment 106 — Orthorhombic (Rhombic) Sulphur Materials. — Powdered roll sulphur, carbon disulphide. Apparatus. — Lens. Put about 2 gm. of powdered roll sulphur in a test tube and add about 5 cc. of carbon disulphide — remember to keep the carbon disulphide away from flames. Shake until most of the sulphur is dissolved, then filter the solution (or pour the clear liquid) into an evaporating dish to crystallize. Stand the dish in the hood or out of doors, where there is no flame and where the offensive vapor will be quickly removed. Allow the liquid to evaporate; watch the crystallization toward the end, if convenient, and remove and dry the best crystals. SULPHUR — SULPHIDES 95 Examine the crystals with the eye and with a lens. Note the color, luster, and shape. Draw the best shaped one. Experiment 107 — Preparation of Monoclinic Sulphur Materials. — Sulphur (roll), carbon disulphide. a. Fix a folded filter paper firmly in a funnel, and place the fun¬ nel in a test tube which stands in a rack. Fill a test tube two-thirds full of roll sulphur, heat it at first throughout its length, and gradu¬ ally increase the heat until all the sul¬ phur is melted. Then quickly pour it upon the filter paper. Let it cool until crystals appear just below the surface, and then pour out the remaining melted sul¬ phur at once into a dish of water. Remove the paper and adhering sul¬ phur, and cut, or break, open the cone of crystallized sulphur (Fig. 60). Observe and record the properties of the crystals, especially the shape, size, color, luster, and brittleness. Allow the best crystals to remain un¬ disturbed for a day or two; then examine again, and record any marked changes. Experiment 108 — Amorphous (Plastic) Sulphur Materials. — Sulphur, or test tube and contents from Exp. 104 c. Put a few pieces of roll sulphur in a test tube, or use the test tube saved in Exp. 104 c, heat carefully until the sulphur boils, and then quickly pour the molten sulphur into a dish of cold water. This is the plastic variety of amorphous sulphur. Note its properties. Compare with orthorhombic and monoclinic sulphur. Preserve, and examine it after twenty-four hours. Describe it, and compare its properties with those previously observed. Pul¬ verize a small piece and test its solubility in carbon disulphide. State the result. Experiment 109 — Hydrogen Sulphide — Short Method Materials. — Ferrous sulphide, dilute hydrochloric acid, lead nitrate solution. Apparatus. — As in Fig. 61 for d. Caution. — Perform this experiment in the hood. Fig. 60. — Monoclinic sulphur g 6 experiments in practical chemistry Slip a small piece of ferrous sulphide carefully into a test tube, add 5 cc. of dilute hydrochloric acid, and cau¬ tiously note the odor of the gas. Describe the odor. b. Wet a piece of filter paper with lead nitrate solution and hold it in the escaping gas. Note the change in color. Into what lead compound has the lead nitrate been changed ? c. Add a little more ferrous sulphide and di¬ lute hydrochloric acid to the test tube, and hold a lighted match at the mouth of the tube. Observe the result. Cautiously note the odor of the gas. What is the gas ? d. Arrange an apparatus as in Fig. 61. Fill B half full of water. Put ferrous sulphide and dilute hydrochloric acid in the test tube A Fig. 6i. — Appara¬ tus for preparing hydrogen sul¬ phide water and let the gas bubble through the water in the test tube B for a few minutes. Use the solution in Exp. in. Cork it tightly unless it is to be used soon. Experiment 110 — Hydrogen Sulphide — Long Method Materials. — Ferrous sulphide, dilute hydrochloric acid. Apparatus. — As in Fig. 62 ; stoppered bottle. Caution. — Hydrogen sul¬ phide is a poisonous gas and has an offensive odor. It should not be inhaled nor al¬ lowed to escape into the labora¬ tory. All experiments with hydrogen sulphide should be performed in the hood. I. Preparation. — Construct and arrange an apparatus like that shown in Fig. 62. Put 10 gm. of coarsely powdered fer¬ rous sulphide in the bottle A, insert the stopper tightly, and adjust the apparatus so that the end of the delivery tube pneumatic trough. Introduce a the dropping tube. Hydrogen Fig. 62. — Apparatus for preparing hydrogen sulphide will be under the support of the little dilute hydrochloric acid through sulphide is rapidly evolved. If the SULPHUR — SULPHIDES 97 evolution of gas slackens or stops, add more hydrochloric acid. Col¬ lect three bottles, removing each as soon as full and covering tightly with a piece of dry filter paper. Set aside until needed. When all the bottles have been filled with gas, proceed at once with II. II. Properties. — a. Waft a very little of the gas cautiously to¬ ward the nose, and describe the odor. This odor is characteristic of hydrogen sulphide, and is a decisive test. Has the gas color? b. Test the gas from the same bottle with both kinds of moist litmus paper. Is hydrogen sulphide acid, alkaline, or neutral? c. Hold a lighted match at the mouth of the same bottle. Ob¬ serve the color of the flame. Observe cautiously the odor of the prod¬ uct of the burned gas; to what compound is the odor due? What, then, is one constituent of hydrogen sulphide? d. Burn another bottle of hydrogen sulphide and hold a cold, dry bottle over the burning gas. What additional experimental evidence does this result give regarding the composition of hydrogen sulphide ? e. Pour several drops of concentrated nitric acid into a bottle of hydrogen sulphide, cover, and shake. Note the solid product. What is it ? Explain its formation. Required Exercises. — i. Summarize briefly the properties of hy¬ drogen sulphide gas. 2. State the experimental evidence of its composition. Experiment 111—Preparation and Properties of Sulphides Materials. — Hydrogen sulphide water, clean copper wire, clean sheet lead, bright silver coin, lead oxide (litharge); solutions of lead nitrate, arsenic trioxide (in hydrochloric acid), tartar emetic, zinc sulphate, cadmium nitrate, silver nitrate, and mercuric chloride {Poison!). a. Obtain a bottle half full of hydrogen sulphide water, and hang (by a wire or thread) inside the bottle (i) a clean copper wire, (2) a clean strip of lead, and (3) a bright silver coin. Describe the result in each case. The products are sulphides of the respective metals; give the name and formula of each. b. Put a little litharge — the brownish yellow oxide of lead — in a test tube, cover it with hydrogen sulphide water, and warm gently. The product is lead sulphide. Describe it. c. Add hydrogen sulphide water to lead nitrate solution. De¬ scribe the product. What is the name of the product ? d. Proceed as in c with the arsenic solution. Observe the color of the product. Compare with c. What is the product? e. Proceed as in c with the tartar emetic solution. Tartar emetic g8 EXPERIMENTS IN PRACTICAL CHEMISTRY is a compound of antimony. Observe the color of the product. Com¬ pare with c and d. What is the product? f. Proceed as in c with the zinc sulphate solution. Observe the color of the product. Compare with c, d, and e. What is the prod¬ uct? g. Proceed as in c with solutions of cadmium nitrate, silver nitrate, and mercuric chloride (Poison!). Use separate test tubes. Observe the color in each case, and name the product. Required Exercises. — i. Prepare a list of sulphides, including the name, formula, and color of each. 2. Write the equation for the interaction of (a) lead nitrate and hydro¬ gen sulphide, ( b ) arsenic trichloride and hydrogen sulphide. 3. Write the equations in 2 in ionic form. 4. How could hydrogen sulphide be used to identify the metallic part • of many salts? 5. Suggest a test for sulphide ions. SULPHUR DIOXIDE — SULPHUROUS AND SULPHURIC ACIDS — SULPHITES AND SULPHATES (Practical Chemistry, pp. 229-241, §§ 259-276) Experiment 112 — Sulphur Dioxide — Short Method Materials. — Sulphur, joss stick, litmus paper, potassium permanganate solution (dilute), colored flower. Apparatus. — Bottle fitted with cork. Caution. — Perform this experiment in the hood. Fill a deflagrating spoon with sulphur, set it afire, and lower the spoon into a bottle. In a minute or two, remove the spoon, and cover the bottle with a glass plate or (tightly) with a piece of filter paper. In the same way prepare and cover two more bottles of sul¬ phur dioxide. a. Cautiously note the odor. After the smoke (which is not sul¬ phur dioxide) has settled, observe whether the gas has any color. Is it heavier or lighter than air? Save for b. b. Hold a blazing joss stick or a burning match in the bottle of gas saved from a. Does the gas burn? Does it support combus¬ tion? c. Stand the second bottle of gas mouth downward in a vessel of water (e.g. pneumatic trough). Shake, still keeping the mouth submerged. Observe the result. What does the result show about SULPHUR DIOXIDE 99 the solubility of sulphur dioxide in water ? Slip a piece of filter paper under the mouth of the bottle, remove, invert, and test the liquid with litmus paper. State the result. To what compound is the re¬ sult due? Save for d. d. Pour a few drops of very dilute potassium permanganate solu¬ tion into the bottle saved from c, and shake well. Compare the color of the two liquids. If the result is not satisfactory, repeat, and use a bottle full of sulphur dioxide to which only 5 cc. of water has been added. Explain the chemical change. e. Moisten a few petals of a colored flower with water, put them in the third bottle of sulphur dioxide, and insert the cork. Observe and describe any change in color. Experiment 113 — Sulphur Dioxide and Sulphurous Acid gm. of Materials. — Sodium sulphite, dilute sulphuric acid, litmus paper, joss stick, colored flower, potassium permanganate solution. Apparatus. — As in Fig. 63. Caution. —■ Perform this experiment in the hood. I. Preparation. — a. Sulphur Dioxide. — Put about 10 sodium sulphite in the flask, and insert the stopper with its tubes. Adjust the apparatus as shown in Fig. 63. Fill the cup with dilute sulphuric acid, press the pinch-clamp a little, and let the acid flow drop by drop upon the sodium sul¬ phite. Sulphur dioxide is evolved and passes into the bottle, which should be removed when full, as previously de¬ scribed. Warm gently, if the action slackens. Moist blue litmus paper held for an instant at the mouth of the bot¬ tle will show (by change in color) when the latter is full. Collect two bottles of gas, cover each tightly with a piece of filter paper or a glass plate, and set aside until needed for II a. b. Sulphurous Acid. — As soon as the second bottle of gas has been re¬ moved and covered, put in its place a bottle one-fourth full of water. Adjust its height (if necessary) by wooden blocks, so that the end of the delivery tube is just above the Fig. 63. — Apparatus for preparing sulphur dioxide and sulphurous acid 100 EXPERIMENTS IN PRACTICAL CHEMISTRY surface of the water. Continue to add the acid and to heat at inter¬ vals. Shake the bottle occasionally. When II a, etc., have been done, proceed with this solution as in III a, etc. II. Properties of Sulphur Dioxide Gas. a, b, c, d, e. Proceed as in Exp. 112 a, b, c, d, e. III. Properties of Sulphurous Acid. — a. Observe the odor and the taste cautiously. State each result. b. Apply the litmus test, and state the result. c. Drop a short piece of magnesium ribbon into 10 cc. of the solu¬ tion. Warm slightly if there is no action. State the result. d. Add a few drops of potassium permanganate solution to 5 cc. of sulphurous acid. Observe and state the result. What chemical change has the sulphurous acid undergone ? e. Put about 10 cc. of sulphurous acid in an evaporating dish, support the dish on a gauze-covered ring attached to an iron stand, heat in the hood, gradually, and note the odor of the liberated gas. Blow the gas out of the dish frequently, and then smell of the liquid. Boil until most of the liquid is evaporated, and test the remainder with litmus paper. What effect has heat on sulphurous acid? f. Put 10 cc. of sulphurous acid into a test tube, cover loosely, and let it stand exposed to the air for a day or two. Add 10 cc. of water, boil for a minute or two, and test as in Exp. 115 b. State and ex¬ plain the result. g. Put 10 cc. of sulphurous acid in a test tube, add 2 cc. of con¬ centrated nitric acid, and boil gently for a minute or two. Add about 10 cc. of water, shake, and test as in Exp. 115 b. State and explain the result. Compare with d and f. Experiment 114 — Properties of Sulphuric Acid Materials. — Concentrated sulphuric acid, thin stick of wood, sugar. Apparatus. — Graduated cylinder (100 cc.), hydrometer for heavy liquids. Caution. — Concentrated sulphuric acid is a corrosive liquid. Do not spill it on the flesh or clothing. a. Weigh a 25 cc. graduated cylinder, pour in concentrated sul¬ phuric acid to a convenient height (e.g. 20 cc.) and weigh again. Read the exact volume of the acid. From the weight and volume of the acid, calculate its specific gravity. Find the specific gravity of a sample of the same acid by reading the hydrometer which floats in the acid (Fig. 64). (This apparatus should be arranged for the class by the Teacher. See Exp. 38.) b. Add an equal volume of concentrated sulphuric acid to a test SULPHURIC ACID IOI tube one-fourth full of water, shake well, and observe at once the change in temperature by holding the tube in the hand. Save the solution for c and d. c. Dip a glass rod into the sulphuric acid from b and write some letters or figures on a sheet of paper. Move the paper back and forth slowly over a low flame, taking care not to set fire to the paper. As the water evaporates the dilute acid be¬ comes concentrated. Observe and describe the result. (Paper is largely a compound of carbon, hydrogen, and oxygen, and the hydro¬ gen and oxygen are present in the proportion to form water.) Explain the general chem¬ ical change in this experiment. d. Warm the acid in the test tube saved from b, stand a stick of wood in the acid, and allow it to remain for fifteen minutes or more. Then remove the stick and wash off the acid. Describe and explain the change in the wood. e. Put 5 gm. of sugar in an evaporating dish, add just enough warm water to make a thick sirup, and stand the dish on a block of wood (or in the sink). Cautiously pour 5 or 10 cc. of concentrated sulphuric acid upon the liquid. Stand back and observe the result. Fig. 64. — Finding the specific gravity of sulphuric acid with the hydrometer Explain the result. Experiment 115 — Tests for Sulphuric Acid, Sulphates (Soluble and Insoluble), and S0 4 -ions Materials. — Sulphuric acid, sodium sulphate, barium chloride solution, calcium sulphate, charcoal, powdered charcoal, silver coin. Apparatus. — Blowpipe and blowpipe tube. a. Sulphuric Acid. — Recall a test for concentrated sulphuric acid. How could the same test be utilized for dilute sulphuric acid ? b. Sulphuric Acid and Soluble Sulphates, i.e. solutions containing S 0 4 -ions. — Add barium chloride solution to the solution of the acid or the sulphate, and boil with dilute hydrochloric acid. If no sul¬ phur dioxide gas is liberated and an insoluble precipitate remains, the original solution contained SCVions. c. Insoluble Sulphates. — Proceed as in Exp. 134 A b, using cal¬ cium sulphate (or any sulphate insoluble in water). 102 EXPERIMENTS IN PRACTICAL CHEMISTRY CARBON — CARBONIC ACID — CARBONATES — OXIDES (Practical Chemistry, pp. 244-258, §§ 277-295) Experiment 1!6 — Properties of Graphite Materials. — Graphite, thread, articles for d. Apparatus. — Graduated cylinder (500 cc.), test wire. a. Rub a piece, of graphite with the finger, and describe the feeling. Draw a piece slowly across a sheet of paper, and state the result. b. Proceed with a lump of graphite as in Exp. 104 b (Fig. 65). Record the result. c. Wind the end of a test wire around a small piece of graphite and hold it in the hottest part of the flame for five or ten minutes (Fig. 66). State the result. d. Examine stove polish, plumbago crucible, core of a lead pencil, electrodes, or lubricant. How would you test them for graphite? Fig. 65. — Appa¬ ratus for finding the specific grav¬ ity of graphite Experiment 117 — Properties of Charcoal Apparatus. Materials. — Wood charcoal (lump and powder), animal charcoal, copper wire, crucible, vinegar, hy¬ drogen sulphide solution. Test tube fitted with a cork, crucible and support. Wood charcoal. — Wind the end of a test wire around a piece of charcoal, hold it in the flame, and observe the result, especially the ease or difficulty of ignition, presence or absence of flame and smoke, formation of ash. Compare with graphite (Exp. 116 c). Animal charcoal. — a. Cover the bottom of a crucible with animal char¬ coal, stand the crucible on a triangle Iig. 66 . — Apparatus for heat¬ ing graphite in a hot flame and heat intensely for about half an hour. Examine the residue. What is it? b. Fill a test tube one-fourth full of powdered animal charcoal (refer to Fig. 5). Add 10 cc. of hydrogen sulphide solution, and CARBON — CARBONATES 103 cork securely. Shake well. After ten minutes, remove the stopper and smell of the contents. Is the odor much less offensive? What property of animal charcoal does this experiment illustrate? c. Fill a test tube one-fourth full of powdered animal charcoal, (refer to Fig. 5), add 10 cc. of vinegar, shake thoroughly for a minute, and then warm gently. Filter through a wet paper. Com¬ pare the colors of the filtrate and the original vinegar. Describe briefly. What property of animal charcoal does this experiment illustrate ? Experiment 118 — Testing for Carbon Test various substances for carbon by heating in a test tube or a crucible, as in Experiment n e. State the result. Experiment 119 — Reduction of Copper Oxide by Carbon Materials. — Powdered copper oxide, powdered wood charcoal, calcium hydroxide. Apparatus. —■ As in Fig. 67, lens. Grind together in a mortar about 5 gm. of copper oxide and 1 gm. of wood charcoal. Put the mixture on a creased paper (refer to Fig. 5) and slip it into the test tube A. Fill the bottle B half full of calcium hydroxide. Arrange the apparatus as in Fig. 67. Heat the test tube gently at first, and adjust the height so the evolved gas will bubble through the calcium hydroxide in B. Heat intensely for about ten minutes, moving the burner along the part of the test tube that con¬ tains the mixture. Observe the change in the calcium hydroxide. To what is the change due? As soon as a definite change is noted in B, remove the end of the delivery tube from B, and stop heating. Let the test tube cool and pour the contents into a mortar. Examine it carefully with the eye and with a lens. What is detected besides carbon? Interpret the chemical change and write the equation for the re¬ action. Fig. 67. — Apparatus for re¬ ducing copper oxide with carbon 104 EXPERIMENTS IN PRACTICAL CHEMISTRY Experiment 120 — Carbonic Acid (Demonstration Experiment) Materials. — Solutions of sodium hydroxide and phenol-phthalein. Apparatus- — Carbon dioxide generator with washing tube. Construct and arrange the carbon dioxide generator like that shown in Fig. 68. (A bottle may be used in place of the test tube A.) Put marble chips in A and water in B (to wash the gas free from acid). Use dilute hydrochloric acid. Fill a bottle half full of water, add a few drops of phenol-phthalein solution and just enough sodium hydroxide solution to color the liquid a faint pink (after shaking). Pass a slow current of carbon dioxide from the generator through the liquid in the is produced in the absorbing liquid. Experiment 121 — Normal and Acid Calcium Carbonate (Demonstration Experiment) Apparatus. — Carbon dioxide generator (as in Exp. 120). Fill the bottle C one-fourth full of calcium hydroxide solution and pass carbon dioxide through it until the precipitate at first formed disappears. Filter, if the liquid is not perfectly clear. Put 15 cc. into a test tube and heat gently. Observe all the changes. State the results of heating the clear solution. Required Exercises. — 1. What is the name of the first precipitate? 2. Into what soluble compound was this precipitate formed by inter¬ action with carbon dioxide? 3. Into what was the soluble compound formed by heating? 4. Write equations for (1) preparation of carbon dioxide, (2) forma¬ tion of the precipitate, (3) formation of the soluble compound, (4) decom¬ position of the soluble compound. Experiment 122 — Testing for Carbonates Materials. — Barium hydroxide solution, baking soda, washing soda, baking powder, native chalk, tooth powder, white lead, whiting, old mortar (or plaster), “unknowns.” Fig. 68 . — Apparatus for pre¬ paring and washing carbon dioxide bottle until a definite change Describe and explain it. CARBON — CARBONATES 105 Put some of the fine solid in a test tube, add a little water and dilute hydrochloric acid, and shake. Then hold a glass tube, which has been dipped into barium hydroxide solution, inside the test tube for a minute or two about 3 cm. above the mixture. If the action is not marked, gently warm the test tube. State the result in each case. Experiment 123 — Carbon Monoxide (Demonstration Experiment) Materials. — Oxalic acid, calcium hydroxide solution. Apparatus. — As in Fig. 69. - Caution. — Carbon monoxide and oxalic acid are poisonous. Hot sulphuric acid is dangerous. Perform this experiment in the hood with unusual care. I. Preparation. — Put 10 gm. of oxalic acid in the flask A (Fig. 69), and add 25 cc. of concentrated sul¬ phuric acid. Put enough calcium hydroxide solution in B to cover the end of the tube E. Arrange the ap¬ paratus as in Fig. 69. The end of H should rest on the bottom of the pneumatic trough just beneath the hole in the sup¬ port. Heat the flask A gently, and car¬ bon monoxide will be evolved. Col¬ lect all the gas, but do not use the first bottle, covering the Fig - 6 9 - ~~ Apparatus for preparing carbon monoxide bottles with glass plates as they are filled, and setting them aside temporarily. When the last bottle has been collected and covered, loosen the stopper in B, and remove the end of H from the water in the trough. Proceed at once with II. II. Properties. — a. Note that the gas is colorless. b. Hold a lighted match at the mouth of a bottle. Note the flame, especially its color. After the flame has disappeared, drop a lighted match into the bottle. Describe the result. Draw a conclusion and verify it by c. io6 EXPERIMENTS IN PRACTICAL CHEMISTRY c. Burn another bottle of gas, note the flame again, and after the flame has disappeared pour calcium hydroxide solution into the bot¬ tle and shake. Explain the result. Required Exercises. — i. Describe briefly the preparation of car¬ bon monoxide. 2. Summarize the observed properties of carbon monoxide. 3. What gas besides carbon monoxide was produced in I? FUELS — ILLUMINATING GAS — FLAME (Practical Chemistry, pp. 260-288, §§ 296-338) Experiment 124 — Composition of Fuels Materials. — Soft coal, wood, alcohol, gasolene, calcium hydroxide solu¬ tion. Apparatus. —- Crucible (porcelain or iron). a. Put a little powdered soft coal in a test tube, attach the holder, and heat intensely in the flame (Fig. 70). Note the formation of moisture and volatile matter (smoke). Describe the result. b. Optional. Put a little powdered soft coal in a crucible (porcelain or iron), support the crucible on a tri¬ angle (Fig. 71), and heat intensely. After the smoking has stopped, note the black, hard mass of fixed carbon. Continue to heat until the carbon has disappeared. The residue is ash (or ashes). Describe it. c. Proceed as in a, using shavings or small pieces of wood. Describe the result. Continue to heat until the carbon is burned. Is ash left? Fig. 70. — Heating soft coal to detect volatile matter d. Put several drops of alcohol in a dish, set it afire, and hold a cold, dry bottle over the flame. When the flame goes out, remove the bottle, and stand it mouth upward on the desk. What is the film inside the bottle? Add calcium hydroxide solution, cover the bottle with the hand, shake well, and note the result. What do these two tests show about the composition of alcohol? e. Proceed as in d, using gasolene instead of alcohol (Care 0 f. Hold a cold dry bottle for a minute or two over a small Bunsen flame. Note the obvious product. What is it ? What is the other FUELS — ILLUMINATING GAS — FLAME 107 product? Verify your answer by a simple test. Apply thq last question asked in d. Experiment 125 — Analysis of Coal Object. — To find the per cent of moisture, volatile matter, fixed carbon, and ash in a sample of coal. Material. — Coal (powdered very fine). Apparatus. — 2 crucibles, 2 covers, triangle, drying oven. Note. — Parts of this experiment may be assigned to sections or individ¬ uals. To save time, a may be omitted and the experiment started with b ; see directions in b. This experiment may be deferred until § 299 in the author’s Practical Chemistry is studied. As in previous experiments, copy first the forms of Record ; enter the weights as soon as weighings are made. a. Moisture. — Weigh a clean, dry porcelain crucible and cover accurately on the balance. Remove the crucible from the balance pan, and slip about 2 gm. of the powdered coal into the crucible, taking care not to leave any dust on the edges or sides of the crucible. Weigh (with the cover). Put the crucible, uncovered, in an oven and heat for about an hour to 105 ° C. ( 104 - 107 ). Cool, and weigh with the cover. The loss in weight is the weight of the moisture. Save the crucible and con¬ tents for b. Calculate the per cent of moisture and enter it in Record —I. Record — I Weight of crucible, cover, and coal before heating . . . gm. Weight of crucible and cover..gm. Weight of coal. gm. Weight of crucible, cover, and coal before heating . . . gm. Weight of crucible, cover, and coal after heating .... _gm. Weight of moisture. gm. Per cent of moisture. per cent b. Volatile Matter. — If a has been done, use the crucible and contents. If a was omitted or is being done, start b with a new por¬ tion of coal. Enter the weights in Record — II. The loss in this case is the total volatile matter (that is, other volatile matter besides moisture). io8 EXPERIMENTS IN PRACTICAL CHEMISTRY Place the covered crucible on a triangle which rests on a ring at¬ tached to an iron stand (Fig. 71). Heat gently at first, and then intensely for eight minutes, or for two or three minutes after the gases cease to burn between the crucible and cover. Cool the crucible slowly, and weigh (with the cover). The loss in weight is the vola¬ tile matter (combustible, if the crucible from a was used, total, if a new portion was used). Save the crucible and contents for c. Cal¬ culate the per cent of total volatile matter (and if a was done, the per cent .of combustible volatile matter) and enter in the proper place in Record — II. Record — II Weight of crucible, cover, and coal before heating . . . gm. Weight of crucible and cover.. Weight of coal.. & m - Weight of crucible, cover, and coal before heating . . . gm. Weight of crucible, cover, and contents after heating . . gm. Weight of volatile matter. S m - Per cent of volatile matter. P er cent c. Fixed carbon and ash. — If the crucible and contents from b are used, proceed at once to heat the uncovered crucible as in the next paragraph. If b was not done or the crucible is not available, start with a new portion as in a; heat the covered crucible containing the new portion of coal gently until most of the volatile matter has been expelled. Then remove the cover and proceed as in the next paragraph. Enter the weights in the proper places in Record — III. Incline the uncovered crucible slightly (Fig. 72), heat gently at first and then intensely un¬ til all the carbon has been burned; if any car¬ bon remains on the inside of the cover, burn it * t us ' f or determin- °ff very carefully. Cool and weigh the covered ing the volatile crucible. The final weight of the substance in matter in coal the crucible is the weight of the ash. Calcu¬ late the per cent of ash. Calculate also the per cent of fixed carbon, utilizing the results in a and b for this calcula¬ tion and enter in Record — III. "FTn i t — Annara- FUELS — ILLUMINATING GAS — FLAME 109 Record — III Weight of crucible, cover, and coal before heating ... gm. Weight of crucible and cover.. .gm. Weight of coal. gm. Weight of crucible, cover, and ash. I gm. II . . . gm. Weight of crucible and cover. gm. Weight of ash. gm. Per cent of ash. per cent Weight of coal. gm. Weight of volatile matter (total). gm. Weight of fixed carbon and ash. gm. Weight of ash. gm. Weight of fixed carbon. gm. Per cent of fixed carbon. per cent Experiment 126 — Properties of Gasolene O-csl Apparatus. — Hydrometer (specific gravity — direct reading) for liquids lighter than water, tall jar, medicine dropper, bottle fitted with cork. Caution. — Gasolene vapor catches fire quickly. Keep all flames away except as the experiment requires. a. Pour a few drops of gasolene into an evaporating dish. Note the odor. Cautiously bring a Bunsen flame near the surface of the liquid. Observe and state the result. b. Put a few drops of gasolene on a glass plate and note the result. Is gasolene vola¬ tile? Very volatile? c. Warm a 250 cc. bottle. Drop in (from a medicine dropper or a pointed glass tube) two or three drops of gasolene. Insert the cork and fill the bottle with vapor by rolling and shaking it. Uncork it, and hold a blazing joss stick at the mouth for an instant. Note the result. If the result is not striking, repeat with five or six drops of gasolene. State the result. Does gasolene explode? What does explode ? d. Determine the specific gravity of one or more samples of gaso¬ lene with the hydrometer (Fig. 73) as in Exp. 38. Fig. 72. — Apparatus for determining the fixed carbon in coal no EXPERIMENTS IN PRACTICAL CHEMISTRY Experiment 127 — Properties of Kerosene Apparatus. — As in Fig. 74, thermometer. Compare the cor- a, b, c, d. Proceed as in Exp. 126 a, b, c, d. responding results of each experiment. e. Determine the flashing point of kerosene with the apparatus shown in Fig. 74. Fill the large beaker nearly full of water. Suspend the small beaker in the water by winding a copper wire around the top and twisting the ends of the wire around the large beaker just below the rim. Stand the large beaker on a gauze-covered ring or a piece of asbestos board. Fill the small beaker nearly full of kerosene. Clamp the thermometer so that the bulb is submerged in the kerosene. Heat the water gently and at intervals slowly pass a lighted match or a blazing joss stick about half an inch above the surface of the kerosene; when the vapor catches fire and a flash passes down to the surface of the kerosene, read and record the temperature. Let the water cool somewhat, and repeat the test. The lowest temperature at which the flame, ^===b Fig. 73. — Ap- paratus for finding the specific grav- cause d by the burning vapor, passes completely ity of gasolene over the surface may be accepted as the flashing point of kerosene. Note. — The legal flashing point of commercial kerosene varies, but in most states it is about 44 0 C. Experiment 128 — The Principle of the Davy Safety Lamp a. Press a ,wire gauze down upon a Bunsen flame. Where is the flame? Remove the gauze, let it cool (or use another gauze), lower it upon the flame, and hold a lighted match just above the gauze. Now where is the flame? b. Extinguish the flame. Turn the gas on full, hold the gauze in the escaping gas, about 15 cm. (6 in.) above the top of the burner, and thrust a lighted match into the gas above Fig. 74.;—Apparatus for finding the flash¬ ing point of kerosene FUELS — ILLUMINATING GAS — FLAME hi the gauze. Move the gauze slowly back and forth. Where is the flame? Lower the gauze slowly and describe the final result. c. Hold the gauze in the flame in one position for a minute or two. Where is the flame at the end of this time? Why? Experiment 123 — Illuminating (Coal) Gas Materials. — Soft coal, litmus paper, lead nitrate solution. Apparatus. — As in Fig. 75. Fill the test tube two-thirds full of coarsely powdered soft coal, insert the stopper with its tube, and clamp the test tube carefully to the iron stand as shown in Fig. 75. - Heat the whole tube gently at first, gradually increase the heat, and finally heat intensely the part contain¬ ing the coal. a. As soon as the gas begins to escape, hold at the end of th£ tube a piece of fil¬ ter paper which has been moistened with lead nitrate solution; observe the effect upon the paper. The discoloration is caused by lead sulphide which is produced by the interaction of lead nitrate and the sulphides in the liberated gas. b. Lay a piece of wet red litmus paper on the end of the tube and continue to heat intensely; wet the paper, if it dries. Observe any change in the color of the litmus pa¬ per. To what class of compounds in the gas is the change due? c. Heat intensely, and light the gas at the end of the tube. Ob¬ serve and describe the flame. d. Discontinue heating, let the apparatus cool somewhat, dis¬ connect, and break open the test tube. Examine the contents. State the properties of both solid and liquid products; what is the name of each ? Experiment 130 — Testing Illuminating Gas Materials. — Solutions of calcium hydroxide, lead nitrate, potassium permanganate (very dilute). a. Test samples of illuminating gas for carbon dioxide, sulphides (Exp. 129 a), and ammonia. State the results. 112 EXPERIMENTS IN PRACTICAL CHEMISTRY b. Suggest a test for moisture. Submit the details to the Teacher, before proceeding. c. Fill a bottle with illuminating gas as follows: Invert a bottle over a Bunsen burner (not lighted), turn on the gas and slowly dis¬ place the air with illuminating gas. When the bottle is full, turn off the gas, stand the bottle upright, quickly pour in about 5 cc. of very dilute (faint pink) potassium permanganate solution, cover with the hand, and shake well. Note the change in the color of the liquid. The change is caused by the illuminants (ethylene, etc.). Experiment 131 — Illuminating Gas Flame Materials. — Calcium hydroxide solution. Apparatus. — Gas burner (Fig. 76) or tip, glass tube. a. Examine a gas burner tip, noting especially the slit. b. If an ordinary gas burner is not available, attach the tip to a rubber tube and slip the tube over the top (or just inside) of a Bunsen burner. Light the# gas. Note the yellow and black parts. Turn off the gas slowly until the flame is very small and note the change in the size of the parts, and finally the black and the blue parts. Turn on the gas slowly and note the change in the size of the parts. Describe these changes. (See Fig. 76.) c. Hold a glass tube in the upper part of the yellow flame. Note the deposit on the tube. What is it ? Where did it come from? Lower the flame and hold a cold dry bottle low down almost upon the flame. Is a deposit formed? If so, what is it and why was it formed? d. Hold a cold dry bottle mouth down¬ ward just over the flame. What is the deposit inside the bottle? Pour about 10 cc. of calcium hydroxide solution into the bottle, and shake. Describe and explain the result. What are the two products of the combustion of illuminating gas? Experiment 132 — Candle Flame Materials. — Candle, piece of stiff paper, calcium hydroxide solution, lead pencil, copper wire (15 cm. or 6 in. long). FUELS — ILLUMINATING GAS — FLAME II3 Stick a short candle to a block of wood by means of a little melted candle wax. a. Hold a cold, dry bottle over the lighted candle. What is the product seen inside the bottle ? What is its source ? Remove the bottle, pour in a little calcium hydroxide solution, and shake. Describe and explain the result. What are the two main products of a burning candle? b. Blow out the candle flame, and immediately hold a lighted match in the escaping smoke. Does the candle relight? Why? Fig - 77-— Effect of cooling a What is the general nature of this candle flame smoke ? How is it related to the candle wax ? c. Press a piece of stiff paper for an instant down upon the steady candle flame almost to the wick. Repeat several times with different parts of the paper. What do the marks on the paper show about the structure of the flame? d. Roll one end of the copper wire around a lead pencil to form a spiral about 2 cm. (or 1 in.) long. Press the spiral down slowly upon the candle flame (Fig. 77). Cool the wire and repeat. What is the result? Why? Optional Exercises. — 1. Draw a candle flame, showing the parts. 2. Is there any essential difference between a candle and a gas or a lamp flame? 3. Why do candles and lamps often smoke? Experiment 133 — Bunsen Burner and Bunsen Burner Flame Materials. — Powdered wood charcoal, pin, copper wire. a. Take apart a Bunsen burner and study the construction. Write a short description of the burner. Sketch the essential parts. b. Close the holes at the bottom of a lighted burner and hold a glass tube in the upper part of the yellow flame. Note the deposit. What is it? Where did it come from? Open the holes and move the tube up and down in tfie colorless Bunsen flame. What becomes of the deposit ? Why ? c. Dip a glass tube a short distance into some powdered wood char¬ coal, place the end containing the charcoal in one of the holes at the bottom of the lighted burner, and blow gently two or three times into the other end. Describe and explain the result. 114 EXPERIMENTS IN PRACTICAL CHEMISTRY d. Open and close the holes of a lighted burner several times. De¬ scribe the result. Pinch the rubber tube to extinguish the flame, then light the gas at the holes. What change is produced in the flame? What is the object of the holes? e. Lay a match across the top of the tube of a lighted Bunsen burner. When the match begins to burn, remove and extinguish it. Note where it is charred, and explain the result. Press a piece of wire gauze down upon the flame. Describe and explain the appearance of the gauze (Fig. 78). Stick a pin through a match near the head, and suspend it across the burner (Fig. 79). Turn the gas on full and light it. What is the effect on the match? What does the whole of e show about the structure of the lower part of the Bunsen flame? Verify your answer by f. f. Hold one end of a glass tube (about 15 cm. or 6 in. long) in the Bunsen flame about 2 cm. (1 in.) from the top of the burner tube Fig. 78. — Studying the cones of a Bunsen flame k \ l Fig. 79. — Studying the lower part of a Bunsen flame M Fig. 80. ‘— Studying the inner cone of a Bunsen flame (Fig. 80). Hold a lighted match for an instant at the upper end of the tube; raise or lower the tube slightly (still keeping the end in the flame) and observe the result. What does the result show about the structure of the Bunsen flame? How does it verify e? g. Find the hottest part of the flame, when a full current of gas is burning, by holding a copper wire in the flame (Fig. 2). Meas¬ ure its distance, approximately, from the top of the burner tube. h. Examine an imperfect Bunsen burner flame — one which shows the outlines of the inner part. What is the general shape of each main part? Draw a vertical and a cross section. i. Using the same burner as in h, lower the flame gradually until FUELS — ILLUMINATING GAS — FLAME 115 it strikes back. Now observe the place where the gas burns, the odor. Feel cautiously of the tube and describe the result. Note 1 / Fig. 81. — Blow¬ pipe tube Experiment 134 — Reduction and Oxidation with the Blowpipe Materials. — Charcoal, lead oxide, sodium carbonate, sodium sulphate, powdered wood charcoal, silver coin, zinc, lead, tin. Apparatus. — Blowpipe, blowpipe tube. Slip the blowpipe tube (Fig. 81) into the burner tube. Light the gas and lower the flame until it is about 4 cm. (1.5 in.) high. Rest the tip of the blowpipe (Fig. 82) on the top of the blowpipe tube, placing the tip just within the flame. Put the other end of the blowpipe between the lips, puff out the cheeks, inhale through the nose, and exhale into the blow¬ pipe, using the cheeks somewhat as bellows. Do not blow in puffs, but produce a continuous flow of air through the blowpipe (Fig. 83). The flame should be an inner blue cone surrounded by an outer and almost invisible cone (Fig. 84). __ A. Reduction. — a. Make —^ a cavity in one end of the flat side of a piece of charcoal. Fill it with a mixture of equal Fig. 82. Blowpipe parts of powdered sodium carbonate and lead oxide, and heat the mixture in the reducing flame (B in Fig. 84). In a short time bright, silvery globules should appear on the charcoal. Let the mass cool, and pick out the largest globules. Put one or two in a mortar, and strike with a pestle. Are they soft or hard? Malleable or brittle? How do the proper¬ ties compare with A £ those of metallic Fig. 84.— Blowpipe flame lead? What has — A (oxidizing) and B become of the (reducing). The flame is oxygen? coming out of the upper b. Grind to- end of the blowpipe tube gether in a mor¬ tar a little sodium sulphate and powdered r Fig. 83. — Using the blowpipe n6 EXPERIMENTS IN PRACTICAL CHEMISTRY wood charcoal, adding at intervals just enough water to hold the mass together. Heat some of this paste in the reducing flame as in a. Scrape the mass into a test tube, boil in a little water, and put a drop of the solution on a bright silver coin. If a dark brown stain is produced, it is evidence of the formation of silver sulphide. Repeat, if no such stain is produced. The silver sulphide is formed by the interaction of the silver and sodium sulphide. Explain how the experiment illustrates reduction. B. Oxidation. — a. Heat a small piece of zinc on charcoal in the oxidizing flame (A in Fig. 84). Direct the flame across the zinc so that most of the product will form a coating on the charcoal. What is the product? Observe the color of the coating on the charcoal when both hot and cold. Record the result. b. Heat a piece of lead as in a. Observe the color of the coatings (hot and cold). Record the result. c. Optional. Heat a small piece of tin in the oxidizing flame. Ob¬ serve and record as in b. Optional Exercises. — 1. Name the products formed in B. 2. Sketch a flame showing the oxidizing and reducing parts. Experiment 135 — Testing for Metals and Non-metals Materials. — Compounds of zinc, lead, and tin, insoluble sulphates ( e.g. of calcium, barium, lead), charcoal. Obtain “ unknowns ” and apply (1) the blowpipe or the flame test for the metal, (2) the blowpipe test for an insoluble sulphate, and (3) if necessary other tests, e.g. for chloride, sulphate, carbonate, nitrate. State each result. Give the name and formula of each compound. OTHER CARBON COMPOUNDS (Practical Chemistry, pp. 289-305, §§ 339-372) Experiment 136 — Sucrose (Cane Sugar) and Dextrose a. Proceed as in Exp. 114 e. b. Proceed as in a, using dextrose instead of sucrose. Compare the results. c. Add 10 cc. of Fehling’s solution (see App. § 6, List G) to 5 cc. of dextrose solution, and heat to the boiling point. Note the result. The precipitate is cuprous oxide. Describe it. OTHER CARBON COMPOUNDS 117 d. Repeat c, using cane sugar solution instead of glucose. Do not boil the mixed solutions. State the result. Compare with a. e. Apply Fehling’s test for dextrose (and similar sugars) to cheap candy, maple sugar, molasses, table sirups, jelly, jam, etc. Prepare and use clear solutions. State each result. Experiment 137 — Properties of Starch Materials. — Starch, Fehling’s solution, iodine solution. Prepare a starch mixture by boiling about 1 gm. of powdered starch for a few minutes in 50 cc. of water; stir or agitate the mix¬ ture during the boiling. Make three tests with the starch mixture. (1) Pour half of it into an evaporating dish which stands on a gauze-covered ring, add 1 cc. of concentrated sulphuric acid, mix well, and boil for at least ten minutes; add water occasionally to replace that lost by evaporation. Meanwhile proceed with (2). As soon as the mixture (in (1)) has been boiled at least ten min¬ utes, take out a little, add sodium hydroxide solution to alkaline reaction and apply Fehling’s test. Note the result. Continue the heating for ten or more minutes, and test again. State the final re¬ sult. (2) Dilute half of the rest of the original starch mixture with water and test it with Fehling’s solution. Observe and state the final re¬ sult. Compare with (1). (3) Add a drop or two of very dilute iodine solution to the rest of the starch mixture. Observe the color. (This test for starch is delicate, and dilute mixtures should be used.) Experiment 138 — Detection of Starch by Iodine Materials. — Dilute solution of iodine; potato, rice, bread, and sub¬ stances enumerated in b. a. Test potato, rice, and bread for starch by moistening each sep¬ arately with water, and then adding a drop or two of very dilute iodine solution. State the result in each case. b. Proceed as in a, using substances not positively known to con¬ tain starch, e.g. baking powder, leaves of different kinds of trees, roots of vegetables, popped corn, straw, and various kinds of food. State each result. Experiment 139 — Properties of Ethyl Alcohol Materials. — Ethyl alcohol, camphor, shellac, rosin, iodine, ether, carbon disulphide, carbon tetrachloride. n8 EXPERIMENTS IN PRACTICAL CHEMISTRY Apparatus. — Tall jar, hydrometer for light liquids (as in Exp. 126). a. Drop a little ethyl alcohol on a glass plate, and watch it evapo¬ rate. Does it evaporate more rapidly than water? b. Weigh a measured quantity (about 25 cc.) of alcohol in a grad¬ uated cylinder and calculate its specific gravity. (See Exp. 114 a.) c. Determine the specific gravity of alcohol with the hydrometer. State the result. (See Exps. 114 a and 126 d.) d. Try the solvent power of alcohol by adding powdered sub¬ stances to 5 cc. in separate test tubes, e.g. camphor, powdered shellac, rosin, or iodine. Describe each result. Add water to each solution. Describe and explain the result. e. Proceed as in d, using liquids, e.g. water, ether (care!), carbon disulphide (care!), carbon tetrachloride. State each result. f. Burn a little alcohol in a porcelain dish and observe the proper¬ ties of the flame, e.g. color, heat. What are the products of com¬ bustion ? Experiment 140 — Tests for Ethyl Alcohol a. Proceed as in Exp. 142 a. b. To 5 cc. of ethyl alcohol add a crystal or two of iodine and just enough sodium hydroxide solution to dissolve and decolorize the iodine. Warm gently several minutes and then cool. Note the odor of the yellow product. It is iodoform and its formation is a test for alcohol. Experiment 141 — Properties of Acetic Acid Materials. — Acetic acid, magnesium ribbon. a. Put 5 cc. of acetic acid in a test tube. Note the odor and taste (cautiously). Warm a little in a test tube, and smell (cautiously). Describe the odor. Is acetic acid volatile? Test with litmus paper, and describe the result. b. Prepare, or obtain, a solution of 5 cc. of acetic acid in 15 cc. of water and a similar solution of sulphuric acid and water. Drop a short piece of magnesium ribbon into each and note the result. In which acid is the action faster? Is acetic acid a weak or a strong acid? Experiment 142 — Test for Acetic Acid and Acetates Materials. — Concentrated sulphuric acid, acetic acid, ethyl alcohol, sodium acetate solution. OTHER CARBON COMPOUNDS ii 9 a. Cautiously add a few drops of concentrated sulphuric acid to a mixture of 5 cc. each of acetic acid and ethyl alcohol. Shake the mixture and warm gently. Note the odor. The pleasant, fruitlike odor is due to ethyl acetate. b. Proceed as in a, using sodium acetate solution. Experiment 143 — Properties of Vinegar Materials. — Vinegar, solutions for a, sodium cobaltinitrite solution (for b (2)). a. Show that vinegar contains acetic acid. b. Evaporate 15 cc. of vinegar to dryness on a water bath and note the residue. Stand the dish on a gauze-covered ring and heat gently. Note the ash. Test the ash for (1) a carbonate and (2) potassium. (1) Add dilute hydrochloric acid to the residue, and note the effervescence. Warm gently to expel the gas, and filter. (2) To the filtrate from (1) add 5 to 10 cc. of sodium cobaltinitrite solution. The yellow precipitate is a test for potassium (compare Exp. 182 b). Experiment 144 — Preparation of Soap Materials. — Sodium hydroxide, lard, salt. a. Dissolve 10 gm. of sodium hydroxide in 75 cc. of water, add 30 gm. of lard, and boil the mixture in a porcelain (or metal) dish for an hour or more; add water occasionally to replace that lost by evaporation. Then add 20 gm. of fine salt in small portions. Stir constantly during the addition of the salt. Let the mass cool, and remove the cake of soap. b. Optional for Class or Teacher. Prepare soap by the method given on a can of commercial “ lye.” Experiment 145 — Properties of Soap Materials. — Soap, sulphuric acid; calcium sulphate, magnesium sul¬ phate, and acid calcium carbonate solutions for e. a. Leave soap shavings exposed to the air for several days. What does the result show about the presence of water in the soap ? b. Test the soap made in Exp. 144 with wet litmus paper. State the result. Test other samples and compare. Put a few drops of phenol-phthalein solution (alcoholic) on samples of dry soap. State the result. This is a test for “ free alkali.” c. Prepare 25 cc. of a solution of the soap made in Exp. 144 120 EXPERIMENTS IN PRACTICAL CHEMISTRY Warm it and examine the surface for fat (film or globules). Is fat detected? Why? d. Add 20 cc. of dilute sulphuric acid to io cc. of soap solution. Note the result. The precipitate is a mixture of palmitic and stearic acids. Describe it. e. Optional. See Exp. 191. Experiment 146 — Carbon Tetrachloride Materials. — Carbon tetrachloride, joss stick. Apparatus. — Iron crucible, pyrene fire extinguisher (for b). a. Heat the bottom of an iron crucible (or metal pan), drop in some carbon tetrachloride, and hold a blazing joss stick or a piece of burning paper in the vapor. Describe the result. b. Optional. Examine and describe a pyrene fire extinguisher. FOOD AND NUTRITION (Practical Chemistry, pp. 307-314, §§ 373-382) Experiment 147 — Testing for Nutrients in Food Materials. — Foods; Molisch’s, iodine, Fehling’s and sodium hydroxide solutions; gasolene, concentrated nitric acid, soda lime (for d ( 1 ) ), very dilute copper sulphate solution. Apply tests for carbohydrate, fat, and protein to various foods from the Table in §§ 377 and 381 of the author’s Practical Chemistry. a. Carbohydrate. — Apply the Molisch test. To 5 cc. of a clear dilute solution of the carbohydrate (or food), add 2 cc. of Molisch’s solution, and shake. Incline the test tube and carefully pour down the inside 5 cc. of concentrated sulphuric acid so that two layers will form. At the contact zone a red-violet color will appear slowly. State the result. b. Carbohydrate. — Test for starch (Iodine Test — Exps. 137 b (3), 138) and sugar (Fehling’s Test —Exp. 136 c). State each re¬ sult. c. Fat. — Grind the sample with gasolene (care!) in a mortar, I pour off the gasolene into an evaporating dish (filter, if not clear),- let it evaporate, and examine the residue. Rub a little between the fingers. Burn a little on the end of a glass rod. State each result. d. Protein. — (Note. — Use two or more of these tests.) (1) Pro¬ ceed as in Exp. 54 a. FOOD AND NUTRITION I 2 I (2) Grind the sample with 20 cc. of water in a mortar, pour off the water (filter, if not clear). To about 5 cc. of the dilute extract add an equal volume of sodium hydroxide solution and shake well. Then add drop by drop a very dilute copper sulphate solution. A violet color is produced. (3) To 5 cc. of the extract from (2) add an equal volume of con¬ centrated nitric acid. Heat gently until a yellow precipitate or a yellow solution is obtained. Cool in running water and add an ex¬ cess of sodium hydroxide solution. An orange color is produced. (4) To 5 cc. of the extract from (2) add concentrated nitric acid slowly, pouring the acid down the inside of the tube so the two solu¬ tions will not mix. A white cloudy precipitate is formed at the sur¬ face of the two liquids. Experiment 148 — Testing for Water in Food a. Proceed as in Exp. 25 a, using samples from the Table in § 377 of the author’s Practical Chemistry. State each result. Experiment 149 — Testing for Mineral Matter in Food Heat a sample of the food in an evaporating dish or crucible, or on a piece of porcelain, in the hood, until the residue is white or gray. This is the mineral matter. If the food, e.g. beans, cheese, or peanuts, contains considerable mineral matter, tests may be applied to the residue. See Exp. 153 e for phosphorus, Exp. 153 h for calcium, and Exps. 143 b (2) and 182 b for potassium. Experiment 150 — Testing Bread a, b, c. Carbohydrate, Fat, Protein. — Proceed as in Exp. 147 b, c, d, using samples of bread. State each result. d. Water. — ( 1 ) Proceed as in Exp. 25 a, using bread. (2) Optional. Weigh a porcelain dish, put in a piece of fresh bread about 5X5X1 cm., and weigh again. Heat the dish gently in an oven (not above 105° C.) for several hours or let it stand for several days in a desiccator containing concentrated sulphuric acid. Weigh again. What weight of water was lost? What per cent? e. Mineral matter. — Proceed as in Exp. 149, using bread. State the result. Experiment 151 — Testing Butter and Substitutes a. Put a small lump of butter in an evaporating dish, heat gently with a small flame, and note the result. 122 EXPERIMENTS IN PRACTICAL CHEMISTRY b. Proceed as in a, using separately samples of butter substitutes Note the result and compare with a. Experiment 152 — Testing Milk Materials. — Milk, acetic acid, sodium hydroxide, dilute copper sulphate solution, junket tablet, gasolene; ammonium oxalate and ammonium molybdate solutions (for d). Apparatus. — Babcock apparatus — Fig. 85 — (for c (2)). a. Water and solids. — Clean and dry an evaporating dish. Weigh it together with a glass rod (about 8 cm. long) on the balance (or good scales). Record the weight. Pour about 25 cc. of well-mixed milk into the dish and weigh again. Record the weight. The dif¬ ference between these weights is the weight of the milk. Stand the dish on a water bath and evaporate to dryness, stirring occasionally to hasten evaporation. Meanwhile do b, etc. When the residue is dry, let the dish cool, wipe it dry, and weigh. The decrease in weight is due to the loss of water. Save the residue for c. From the weight of the milk taken and the weight of the residue, calculate the per cent of (1) water and (2) solids in the milk. (Milk contains about 88 per cent of water. Unless the resi¬ due is dry, the result will be only approximate.) b. Protein. — (1) Boil about 50 cc. of milk in an evaporating (or other) dish. Note the formation of a scum. Remove this scum with a glass rod to a test tube, collecting several portions, and test it as in Exp. 147 d (2) (or another test). (2) Add 3 or 4 drops of acetic acid to 10 cc. of milk in a test tube, and shake. The curdy precipitate is casein. Filter, and test the solid for protein as in (1). Test the filtrate for albumin (a kind of protein) by boiling; the heat coagulates the albumin into white flakes. (3) Add^a small fragment of a junket tablet to 10 cc. of warm milk. Separate and test as in (2). c. Fat. — (1) To the residue from a add 10 cc. of gasolene (care!) and mix well. Pour off the gasolene into a beaker or a dish and let it evaporate. Save the dish and contents for d. Examine the solid from the gasolene extract. Rub a little between the fingers, and burn a little on the end of a glass rod. Is fat detected? (2) Optional or Demonstration Experiment. The Babcock test. Shake the sample of milk, measure 17.6 cc. into the special milk grad¬ uate (Fig. 85 A), and pour it carefully into the test bottle (Fig. 85 B). If a pipette (Fig. 85 C), instead of a graduate, is used, fill the pipette FOOD AND NUTRITION 123 as follows: Put the lower end well into the milk and the other end into the mouth; suck out the air until the milk rises above the 17.6 cc. mark on the stem, remove the pipette from the mouth and quickly Fig. 85.— Babcock apparatus for testing milk — A, milk graduate; B , test bottle; C, pipette; D, acid graduate; E, centrifugal machine cover the end with the finger; move the finger a little and let milk run out slowly until it reaches the 17.6 cc. mark. Next measure 17.5 cc. of concentrated sulphuric acid into the spe¬ cial acid graduate (Fig. 85 D ). Pour the acid carefully in small por¬ tions into the test bottle. Shake carefully after each addition. This operation dissolves the curd ( i.e . the casein) and facilitates the sep¬ aration of the fat. Label the bottle and put it in the centrifugal machine (Fig. 85 E ) together with three other bottles filled similarly with milk and acid, or with water (if only one test is being made). Whirl the machine rapidly and uniformly for five minutes; the melted fat will rise and collect on the surface of the liquid. Add enough hot water to fill the larger portion of the bottle, and whirl for two more minutes. Then add hot water carefully until the water is just below the top graduation on the stem (not above the graduation), and whirl again for two minutes. Remove the bottle from the machine and stand it in a dish con¬ taining water at 6o° C. In a minute or two, remove the bottle and read the volume of fat, taking care to read from the top of the upper meniscus (curved surface of the fat) to the bottom of the lower menis¬ cus. The difference between the two readings is the per cent of fat 124 EXPERIMENTS IN PRACTICAL CHEMISTRY in the milk. Report the per cent to the Teacher before throwing away the contents of the bottle. If the result is accepted, pour the liquid into a waste jar and wash the bottle clean with hot water. d. Mineral matter. — If the dish and contents (from which the fat was extracted) from c (i) is available, use it. If not, evaporate io cc. of milk to dryness and use the residue. Heat the dish and contents in the hood until the residue is white or gray. Dissolve this mineral matter in water and test portions for calcium and a phosphate (as in Exp. 153 h, e). State the results. What component of milk contains most of the mineral matter? Experiment 153 — Testing Baking Powders Materials. — Baking powder (tartrate, phosphate, alum), barium hy¬ droxide, vinegar, sour milk, lemon juice, solutions of iodine, silver ni¬ trate, ammonium chloride, sodium hydroxide, and ammonium oxalate. Note. — Different varieties of baking powder may be tested by individ¬ uals or sections, and the results compared. a. Carbonates. — (1) Put a little baking powder in a test tube, add a few drops of dilute hydrochloric acid, and test the escaping gas with a tube which has been dipped into barium hydroxide solu¬ tion. State the result. (2) Put 2 gm. of baking powder in a test tube, add 15 to 20 cc. of water, and shake well. Let the action continue a short time, and then test the solution as in (1). State the result. (3) Add sour substances, e.g. vinegar, sour milk, lemon juice, separately to a little baking powder, and state the result. b. Starch.—Apply the iodine test for starch to a little baking powder mixed with water. See Exp. 137 (3). State the result. c. Tartrates. — Prepare a cold solution of baking powder by shak¬ ing about 10 gm. of the substance with 50 cc. of water and stirring until all the gas is liberated. Filter, if not clear, and use the clear solution in this and succeeding experiments. (1) Clean a test tube by boiling sodium hydroxide solution in it and then washing thor¬ oughly with water. Put 10 cc. of silver nitrate solution in the cleaned test tube, and add ammonium hydroxide slowly until the precipitate at first formed redissolves, taking care to mix the solutions. Add 10 cc. of the baking powder solution and warm gently. Tartrates, if present, will reduce the silver compound to silver, which will coat the inside of the test tube. (2) Put about 5 cc. of the solution from c in an evaporating dish, add a few drops of concentrated sulphuric SILICON 125 acid, and heat gently. Tartrates, if present, will char and smell like burnt sugar. d. Sulphates. — To 5 cc. of the baking powder solution (prepared in c) add dilute hydrochloric acid to acid reaction and boil; then test with barium chloride solution. State the result. e. Phosphates. — Warm 5 cc. of the baking powder solution, acidify with concentrated nitric acid, and add 5 cc. of ammonium molybdate solution. A yellow precipitate indicates phosphates. State the result. f. Ammonium salts. — Boil 5 cc. of the baking powder solution with an equal volume of sodium hydroxide solution. The presence of ammonium salts is shown by the liberation of ammonia gas, which can be detected by its odor. State the result. g. Aluminium salts. — Boil 5 cc. of the baking powder solution with 1 or 2 cc. of dilute hydrochloric acid, filter if not clear, and add 10 cc. or more each of ammonium chloride and ammonium hydrox¬ ide to the filtrate. A whitish flocculent precipitate (aluminium hy¬ droxide) indicates aluminium salts. State the result. h. Calcium salts. — Boil 10 cc. of the baking powder solution with dilute hydrochloric acid (to remove the carbon dioxide), add ammonium hydroxide to alkaline reaction, filter, if not clear and then add ammonium oxalate solution. Calcium compounds produce a white precipitate (calcium oxalate). SILICON (Practical Chemistry, pp. 316-327, §§ 383-395) Experiment 154 — Preparation of Sodium Silicate Materials. — Powdered silicon dioxide, sodium carbonate. Apparatus. — Iron crucible. Mix thoroughly about 0.5 gm. of fine sand and 4 gm. of sodium carbonate and put the mixture in an iron crucible. Stand the cru¬ cible on a triangle (or in a small ring) and heat gently until the mass ceases to bubble. Then heat intensely for ten or fifteen minutes. Allow the crucible to cool somewhat, add 25 cc. of hot water, and heat until the water boils. When cold, filter, and evaporate the filtrate to about half its volume. This solution contains sodium silicate. Save it for Exp. 155. State the chemical changes by which silicon dioxide is transformed into sodium silicate. 126 EXPERIMENTS IN PRACTICAL CHEMISTRY Experiment 155 — Silicic Acid Materials. — Sodium silicate solution, hydrochloric acid. a. To the solution from Exp. 154 add dilute hydrochloric acid drop by drop, shaking constantly until a precipitate is formed. The precipitate is silicic acid. Describe it. b. Optional. Put 10 cc. of commercial sodium silicate solution in an evaporating dish, and add 10 to 15 cc. of dilute hydrochloric acid, stirring constantly. The jellylike precipitate is silicic acid. Rub some between the fingers and state the result. Stand the dish on a gauze-covered ring attached to an iron stand and evaporate the solution slowly to dryness in the hood. As the mass thickens, stir it with a glass rod. Toward the end add more hydrochloric acid and evaporate to complete dryness. Then heat intensely for five minutes. When the dish is cool, add about 50 cc. of water, stir well, and filter; wash the residue with water once or twice, dry it, remove as much as possible from the paper, and heat it carefully in an evaporating dish for about five minutes. Rub some between the fingers or across a glass plate. State the result. Collect some within the loop of a test wire and heat it intensely in the flame for several minutes. State the result. What is this resi¬ due? State the chemical changes that occur in changing sodium silicate into the final residue. Experiment 156 — Testing for Silicon Materials. — Powdered calcium fluoride, sand, substances for b. Apparatus. — Lead dish, test wire. a. Put a little sand and calcium fluoride in a lead dish (see Fig. 86, Exp. 158), add enough concentrated sulphuric acid to moisten the mixture, and stir with a match. Dip the looped end of a test wire into water, inclose a film of water within the loop, and hold the loop at several points near the mixture in the dish until the water (in the loop) becomes white. If no change occurs, stir the mixture and hold the loop over the place where there is evidence of chemical action. State the result. What is the white substance in the loop? State in words the chemical changes that led to the formation of the white substance in the loop. Write the equations. b. Apply the test for silicon to several of these substances (omit¬ ting the sand): Powdered calcium fluoride, infusorial earth, pumice (powder), scouring soap, glass (small fragments), carborundum FLUORINE — BROMINE — IODINE 127 (powder), ash from coal, electro-silicon, glass wool, mineral wool, soil. State the result in each case. Experiment 157 — Carborundum Examine and describe carborundum. Try its hardness on glass, wood, and other solids, and state the result. Wind a test wire around a small lump, heat intensely for ten minutes, and state the result. FLUORINE — BROMINE — IODINE (Practical Chemistry, pp. 337-344, §§ 404-418) Experiment 158 — Etching with Hydrogen Fluoride Materials. — Paraffin, powdered calcium fluoride. Apparatus. — Lead dish, glass plate (see Fig. 86). Caution. — Do not inhale hydrogen fluoride. Warm a glass plate about cm. (4 in.) square by dipping it into hot wa- _ PMA€TE€AJL Fig. 86. — Etching with hydrogen fluoride — lead uish (left), etched glass plate (right) ter or by mov¬ ing it slowly above a flame. Coat one sur¬ face uniformly with a thin layer of paraf¬ fin wax. Scratch letters, figures, or a diagram through the wax with a pin or pointed glass rod. The wax should be removed through to the glass, and the lines should be rather coarse. Put about 5 gm. of powdered calcium fluoride in a lead dish and add just enough concentrated sulphuric acid to form a thin paste (Fig. 86). Stir the mixture with a match. Place the glass, wax side down, upon the lead dish and let the whole stand in the hood for several hours. Remove the glass and scrape off the wax with a knife. The last portions can be removed by rubbing with a cloth moistened with hot water. Do not attempt to melt off the wax over the flame. Ex¬ amine and describe the glass (Fig. 86). State in words the essential chemical changes in this experiment. Write the equations. Note. —The lead dish should be cleaned in the hood by scraping the contents carefully into a waste jar and washing the whole dish with watei. 128 EXPERIMENTS IN PRACTICAL CHEMISTRY Experiment 159 — Preparation and Properties of Bromine Materials. — Potassium bromide, manganese dioxide, sulphuric acid. Apparatus. — As in Fig. 87 for b; bottle fitted with a cork. The large test tube has a one-hole rubber stopper to which is fitted the bent glass tube; the total length of the glass tube is about 30 cm. (12 in.). Caution. — Bromine is a corrosive liquid, which readily forms a suffo¬ cating vapor. Perform all experiments with bromine in the hood. a. Short method. — Put a little powdered potassium bromide and twice the bulk of manganese dioxide in a test tube. Add 5 cc. of dilute sulphuric acid and mix well. At¬ tach a test tube holder and heat gently. Bromine vapor is evolved. Note the color and very cautiously the odor. If any of the vapor condenses on the inside of the test tube, describe the liquid. (See Note below.) b. Long method. — Put about 3 gm. of potassium bromide in a large test tube, and add 5 gm. of manganese dioxide ; shake well, and add 10 cc. of dilute sulphuric acid. Insert the stopper and its tube (Fig. 87), attach the test tube holder, and warm gently. Bromine vapor soon ap¬ pears in the test tube and, if the heat is sufficient, some vapor will escape from the delivery tube. Note the color and very cautiously the odor. Is the vapor heavier or lighter than air? Heat to such a temperature that the vapor will condense and col¬ lect in the bend A of the delivery tube. When no further boiling produces bromine vapor in the test tube, transfer the bromine from the delivery tube into a bottle half full of water by holding the end of the delivery tube over the mouth of the bottle and heating the test tube slightly; the expanding gases will force the liquid bromine out of the bend into the bottle. Observe and record the physical properties of this bromine, espe¬ cially the color, solubility in water, specific gravity, volatility, and physical state. As soon as these observations have been made, cork the bottle tightly and shake it vigorously. Observe the result, and draw a conclusion about the solubility of bromine in water. Note. — Wash the delivery tube free from bromine, taking care to get none on the hands. Throw the contents of the test tube into a waste jar in the hood and wash the tube. Fig. 87. — Apparatus for preparing bromine FLUORINE — BROMINE — IODINE 129 Experiment 160 — Tests for Bromides Materials. — Potassium bromide, silver nitrate solution, carbon tetra¬ chloride. a. Add a little concentrated sulphuric acid to a little potassium bromide in a test tube; warm slightly, if the action is not marked. Observe the result, especially the color of the liquid or of the vapor just above the liquid. What element does the color suggest ? b. Dissolve a crystal of potassium bromide in a test tube half full of water, add a little silver nitrate solution, and shake. Observe the properties of the precipitate, especially the color and texture. Determine the solubility by warming a little of the precipitate in ammonium hydroxide. State the result. Compare silver bromide and silver chloride (Exp. 65 III b). c. To a solution of a bromide, add a little chlorine water and a few drops of carbon tetrachloride, and shake. The carbon tetra¬ chloride will be colored yellow or brown by the liberated bromine. Experiment 161 — Preparation and Properties of Iodine Materials. — Potassium iodide, manganese dioxide, concentrated sulphuric acid, cotton, alcohol, carbon tetrachloride, potassium iodide solution. Apparatus. — As in Fig. 88 (for b). Do a or b. a. Short method. — Proceed as in Experiment 159 a, using potassium iodide in place of potassium bromide. Note the color and (cau¬ tiously) the odor of the vapor, and the color of the sublimed iodine. b. Long method. — Grind together in a mortar about 3 gm. of potassium iodide and 5 gm. of man¬ ganese dioxide. Put the mixture in a test tube, add about 3 cc. of water, 5 cc. of concentrated sul¬ phuric acid, and mix well. Clamp the test tube vertically to an iron stand (Fig. 88). Close up the inner end (A in Fig. 88) of the stem of the funnel r with a small plug of cotton. Hold, or place, the funnel over the mouth of the test tube, and heat ^ ^ the test tube gently. The vapor of the liberated paratus for pre¬ iodine will fill the test tube, and crystals will form in paring iodine the upper part of the test tube and in the funnel. Continue to heat until enough iodine for several experiments collects in the funnel. Scrape the crystals into a dish. 130 EXPERIMENTS IN PRACTICAL CHEMISTRY Observe and record the color of the solid and of the vapor, and the odor (cautiously). Determine the volatility by putting a small piece in a bottle and exposing to the sunlight. Heat a crystal in a dry test tube, and invert the test tube when it is full of vapor. What does the result show about the density of iodine vapor? Touch a crystal with the finger. What color is the stain? Try the solubility separately in water, alcohol, carbon tetrachloride, and potassium iodide solution. What do these results show about the solubility of iodine ? Note. — If crystals are left, use them'in the next experiment. Preserve the iodine in a stoppered bottle, if not used at once. Experiment 162 — Tests for Free Iodine Materials. — Very dilute iodine solution, potassium iodide, carbon tetra¬ chloride, cold starch mixture. a. Add a few drops of carbon tetrachloride to a very dilute iodine solution. Shake well, and observe the color of the carbon tetra¬ chloride. b. Add 5 cc. of a cold starch mixture to a test tube nearly full of water, and then add a few drops of dilute iodine solution. Note the color. Pour about 5 cc. of the liquid into a test tube nearly full of water and shake. Note the color. Experiment 163 — Tests for Iodides Materials. — Potassium iodide, chlorine water, starch, carbon tetrachloride, silver nitrate solution. a. Add a few drops of carbon tetrachloride to a very dilute solution of potassium iodide. Then add several drops of chlorine water, and shake well. Note the color. b. Add 5 cc. of cold starch solution to 10 cc. of a very dilute solu¬ tion of potassium iodide. Add a few drops of chlorine water, and shake well. Observe and explain the result. c. To 10 cc. of potassium iodide solution, add a little silver nitrate solution, and shake. Observe the properties of the precipitate, es¬ pecially the color and texture. Test the solubility of a little of the precipitate in ammonium hydroxide, and state the result. Compare silver iodide with silver chloride and silver bromide (see Exps. 65 III b, 160 b). PHOSPHATES — ARSENIC — ANTIMONY I3i Experiment 164 — Halogen Acids Proceed as in Exp. 64 a, b, d (omit c), using ( 1 ) potassium bromide and (2) potassium iodide in separate test tubes. Answer: 1. Which of the three halogen acids is the most stable? Least stable ? 2. In what ways are these acids alike? Different? PHOSPHATES — ARSENIC — ANTIMONY — BISMUTH (Practical Chemistry, pp. 346-358, §§ 419-442) Experiment 165 — Tests for Orthophosphoric Acid and Orthophosphates Materials. — Solutions of disodium phosphate, silver nitrate, ammo¬ nium molybdate, ammonium chloride, magnesium sulphate, and orthophosphoric acid ; bone ash, fertilizer. a. To 5 cc. of disodium phosphate solution add a little silver nitrate solution. Observe and describe the result. What is the name and formula of the precipitate? b. To 5 cc. of disodium phosphate solution add 1 or 2 cc. of dilute nitric acid, and an equal volume of ammonium molybdate solution. Observe and describe the result. Warm, if no precipitate appears. The precipitate is ammonium-phospho-molybdate ((NH 4 ) 3 P0 4 . 12M0O3, approximately). Apply this test to a dilute solution of orthophosphoric acid (in¬ stead of disodium phosphate), and state the result. c. To magnesium sulphate solution add successively solutions of ammonium chloride, ammonium hydroxide, and disodium phosphate. Observe and describe the result. The precipitate is ammonium mag¬ nesium phosphate. d. Shake a little bone ash with warm dilute nitric acid, filter, and apply the ammonium molybdate test to the filtrate. State the result. Experiment 166 — Preparation of Phosphate Fertilizer Materials. — Powdered phosphate rock, concentrated sulphuric acid, ammonium molybdate solution. Put about 10 gm. of powdered phosphate rock in an evaporating dish, add 5 cc. of water, 5 cc. of concentrated sulphuric acid, and mix well. Heat gently about ten minutes, stirring frequently. Add 132 EXPERIMENTS IN PRACTICAL CHEMISTRY io to 15 cc. of water, stir, let the mixture settle, and filter. Test the filtrate for a phosphate. State the result. Experiment 167 — Test for Arsenic See Exp. hi d. Write the equation. Experiment 168 — Test for Antimony See Exp. me. Write the equation. Experiment 169 — Test for Bismuth Add considerable water to 10 cc. of bismuth trichloride solution. The precipitate is bismuth oxychloride. Describe it. What is its formula ? Experiment 170 — Fusible Alloys a. Slip a thin piece of fusible alloy into a test tube half full of water, hold a thermometer in the water, heat the water gradually, and note the temperature at which the alloy melts. State the result. b. Optional. Heat a fusible link or a sprinkler head in water and note the temperature at which the alloy melts. State the result. SODIUM AND POTASSIUM (Practical Chemistry, pp. 360-374, §§ 443-469) Experiment 171 — Properties of Sodium Caution. — See Exp. 21. a. Examine a small piece of sodium, and observe its most obvious physical properties, e.g. color, luster, whether hard or soft. b. Perform, recall, or repeat (if necessary) the experiment on the Interaction of Sodium and Water (Exp. 21). c. Fill a dish nearly full of water. Put a piece of sodium on a piece of filter paper (a little smaller than the dish), lay the paper upon the water, and stand back and observe the result. Wait for the slight explosion which usually occurs soon after the action stops. Describe all you have seen. What burned? To what is the vivid color of the flame probably due ? Experiment 172 — Tests for Sodium Materials. — Sodium compounds, solutions of potassium hydroxide and tartar emetic. SODIUM AND POTASSIUM 133 a. Apply the flame test to several sodium compounds, using a clean test wire in each case (Fig. 89, left). State each result. b. Make a solution of a sodium compound slightly alkaline with potassium hydroxide solution, and to 10 cc. add a little freshly prepared tartar emetic solution. The white precipitate is acid so¬ dium pyroantimonate (H 2 Na2Sb 2 0 7 ). Experiment 173 — Properties of Sodium Chloride Materials. — Sodium chloride (several varieties). a. Prepare about 50 cc. of a nearly saturated sodium chloride solu¬ tion, and proceed with the crystallization as in Exp. 40. Examine and describe the best crystals. b. Heat a few crystals of sodium chloride in a test tube. State and explain the result. c. Put a little sodium chloride ( e.g . table salt) in a test tube, and cork the test tube tightly. Put some of the same sample of salt in an open dish. Place both where they will not be disturbed for a day or two, and then compare the two specimens. State and explain the result. Experiment 174 — Sodium Carbonate — LeBlanc Process Materials. — Sodium sulphate, calcium carbonate, wood charcoal, cal¬ cium hydroxide solution. Apparatus. — Iron crucible. Mix and grind together in a mortar 6 gm. of sodium sulphate, 4 gm. of powdered calcium carbonate, and 1 gm. of powdered wood charcoal. Fuse the whole mixture in an iron crucible or a portion on a platinum foil. When cool, heat with a little water and filter. Apply the flame test for sodium to a little of the filtrate and state the result. Divide the filtrate into two parts. To (1) add 5 cc. of dilute hydrochloric acid and to (2) add 5 cc. of calcium hydroxide solution. Observe and explain each result. Experiment 175 — Hydrolysis of Sodium Carbonate Test a solution of sodium carbonate with litmus paper (both kinds), and state the result. Interpret by the ionization theory. Experiment 176 — Sodium Bicarbonate Materials. — Ammonium carbonate, ammonium hydroxide, sodium chlo¬ ride. Apparatus. — Carbon dioxide generator (see Fig. 68). 134 EXPERIMENTS IN PRACTICAL CHEMISTRY I. Preparation. — Put 8 gm. of powdered ammonium carbonate and 75 cc. of ammonium hydroxide into a bottle; add about 35 gm. of fine sodium chloride, cork the bottle, and shake the mixture vigor¬ ously until most of the solid has dissolved. Pour off the clear solu¬ tion into the bottle C. Construct a carbon dioxide generator (see Exp. 120) like that shown in Fig. 68. Put about 20 gm. of marble in the generator bottle A , introduce dilute hydrochloric acid as usual, and pass carbon dioxide (free from hydrochloric acid) slowly through the solution in the bottle C from thirty to forty-five minutes (or less, if a precipitate forms). Then remove the generator, cork the bottle C, and let it stand an hour or more to allow the sodium bicarbonate to settle out of the solution. Filter, and wash quickly with a very little cold water. Dry the precipitate between filter paper. (Note. — If only a little of the precipitate is formed, use sodium bicarbonate from the laboratory bottle for II.) II. Properties. — a. Subject small portions of the precipitate to the flame test for sodium and the usual test for a carbonate. State the result. b. Put a little on moist litmus paper (both colors). Observe and explain the result. c. Heat a little in a test tube inclined so that the open end is the lower. Observe the result. What is the visible product? Apply the usual test for carbon dioxide to the gas in the test tube; state the result. Continue to heat until there is no further evidence of change. Determine what the final residue is by applying to it tests for sodium, a bicarbonate as in a and b, and sodium carbonate ( e.g . litmus test). State the result. Experiment 177 — Properties of Sodium Hydroxide a. Perform, recall, or repeat (if necessary) experiments with sodium hydroxide which show the effect of (1) exposing it to the air, (2) add¬ ing acid to it, (3) dissolving it in water, (4) heating its solution with aluminium. b. Heat a small piece of sodium hydroxide on a piece of porcelain, and describe the result. c. Expose a little pulverized sodium hydroxide in a dish to the air for a day or more. Describe the final product. Test it for a carbonate, and state the result. d. Fuse a small quantity of sodium hydroxide on a piece of porce¬ lain, add a part of a match stick or a small piece of paper, and con¬ tinue the fusion. State the effect on the wood or paper. SODIUM AND POTASSIUM 135 Experiment 178 — Sodium Hydroxide by Electrolysis (Demonstration Experiment) Proceed as in Exp. 61. See Fig. 43. Experiment 179 — Properties of Borax a. Let a piece of red litmus paper stand in borax solution for about ten minutes. Observe and explain the result. b. Test borax for water of crystallization, and state the result. Expose borax crystals to the air for an hour and state the result. c. Apply the flame test to a little borax on the end of a clean test wire. What element is contained in borax according to this test ? d. Dissolve a little borax in water, add 5 cc. of ethyl alcohol, 5 cc. of concentrated sulphuric acid, and mix well. Test for borax by dipping a clean test wire into the solution and holding it in the outer part of the Bunsen flame. Note the color of the flame. Experiment 180 — Tests with Borax Beads Materials. — Powdered borax, cobalt nitrate, copper sulphate, and man¬ ganese sulphate solutions. Heat the looped end of a clean test wire and dip it into powdered borax. Heat the adhering borax in the flame, rotating the wire slowly, until no further change is apparent; continue to dip it into the borax and heat in the flame until a small bead is formed. a. Cobalt Compounds. — Moisten a borax bead with cobalt nitrate solution. Heat the bead in the oxidizing part of the Bunsen flame (Fig. 89 left); rotate the bead while heating it. Observe the color of the cold bead. If it is black, melt a little more borax into the bead; if faintly colored, moisten again with the cobalt solution. The color is readily detected by looking at the bead against a white object in a strong light, or by examining it with a lens. 136 EXPERIMENTS IN PRACTICAL CHEMISTRY When the color has been definitely determined, heat the bead in the reducing flame (Fig. 89 right). Compare the color of the cold bead with the previous observation. State the result. Note. —The bead may be removed from the wire by dipping it, while hot, into water and then rubbing or scraping it from the wire. b. Copper Compounds. — Proceed as in a with another bead and copper sulphate solution. Compare the colors of the cold beads, and state the result. c. Manganese Compounds. — Proceed as in a with another bead and manganese sulphate solution. Compare the colors of the cold beads, and state the result. Experiment 181 — Properties of Potassium (Demonstration Experiment) Caution. — Observe the same precaution as in using sodium. (See Exp. 21.) a. Examine a small piece of freshly cut potassium, and observe its most obvious physical properties. b. Proceed as in Exp. 32 b. What compound of potassium is in solution? Write the equation. Experiment 182 — Tests for Potassium Materials. — Potassium compounds, sodium cobaltinitrite solution. a. Apply the flame test to several potassium compounds, using a clean test wire in each case. State the result. b. Add 5 cc. of sodium cobaltinitrite solution to 10 cc. of a mod¬ erately concentrated solution of a potassium compound, and shake well. The yellow precipitate is potassium cobaltinitrite (K3Co(N02)e) • Experiment 183 — Potassium Nitrate Materials. — Sodium nitrate, potassium chloride, charcoal. I. Preparation. — Dissolve about 15 gm. of potassium chloride in about 40 cc. of water, warming if necessary. Add about 17 gm. of sodium nitrate, and stir well. Boil several minutes, or until a white solid separates. Let the solid settle somewhat, then pour off the liquid into an evaporating dish and let it stand till crystals sep¬ arate. Pour off the liquid from the crystals. Dissolve the crystals CALCIUM — STRONTIUM — BARIUM 137 in a small volume of hot water and let the solid crystallize out again. Drain off the water and dry the crystals between filter paper. II. Properties. — a. Prepare a solution of the final crystals and test portions for (1) potassium and (2) a nitrate. State the result. b. Test the solution also for (1) sodium and (2) a chloride. State the result. Explain it. c. Proceed as in Exp. 9 a. CALCIUM — STRONTIUM — BARIUM (Practical Chemistry, pp. 376-388, §§ 470-486) Experiment 184 — Properties of Calcium Carbonate a. Put a drop or two of dilute hydrochloric acid on one or more specimens of calcium carbonate. State and explain the result. b. Attach a small lump of marble to a test wire or lay it on a wire gauze, and heat it intensely for ten or fifteen minutes. Test it for a carbonate and state the result. What is the name of the solid product? Write the equation. c. Add 5 cc. of sodium carbonate solution to 5 cc. of calcium chlo¬ ride solution. Describe the precipitate. What is it? Write the equation. Experiment 185 — Tests for Calcium Materials. — Calcium compounds, ammonium oxalate and sodium car¬ bonate solutions. a. Apply the flame test to several calcium compounds, using a clean test wire in each case. What is the color of the flame? b. Add an excess of ammonium oxalate solution to calcium chloride solution, and state the result. The precipitate is calcium oxalate. Di¬ vide it into two parts. To (1) add an excess of dilute hydrochloric acid, warm gently, and state the final result. To (2) add consider¬ able acetic acid and warm gently; observe and state the final result. Compare with (1). c. Add an excess of sodium carbonate solution to calcium chloride solution, and state the result. The precipitate is calcium carbonate. Divide it into two parts, and treat with the acids as in b. State the results and compare with b. d. Devise a test for calcium in calcium carbonate and calcium sulphate. Submit the details to the Teacher before proceeding. 138 EXPERIMENTS IN PRACTICAL CHEMISTRY Experiment 186 — Testing Substances of Calcium Materials. — Mortar, plaster, bone ash, plaster of Paris, tooth powder, whiting, cement, bleaching powder. a. Prepare a solution by boiling a little of each substance with dilute hydrochloric acid (or dilute nitric acid) and filtering. Test the filtrate for calcium by Exp. 185 b (or by the flame test). State each result. b. Test “ unknowns ” for calcium. Experiment 187 — Calcium Oxide and Calcium Hydroxide I. Preparation. — a. Proceed as in Exp. 184 b. Let the residue cool, put it in an evaporating dish, and add a little water. Observe the result. Test the liquid with red litmus paper; apply the flame test for calcium. State the results. What calcium compound was formed by heating calcium carbonate? By treating the product with water? Write each equation. b. Prepare calcium hydroxide by adding water slowly to a lump of lime, and save it for III. II. Properties of Calcium Oxide. — a. Put a lump of fresh cal¬ cium oxide on a glass plate or block of wood and let it remain exposed to the air for a few days. Examine it at intervals and describe it. Describe the final product. What is it ? b. What is the result of mixing calcium oxide and water ? Write the equation. III. Properties of Calcium Hydroxide. —■ a. Add a little solid calcium hydroxide to a test tube half full of water and shake vigorously. Let the suspended solid settle somewhat, and filter. Pour half of the filtrate into an evaporating dish and evaporate it to dryness; save the other half. (Meanwhile b may be performed.) When evaporated, compare the amount of residue in the dish with the amount of solid originally shaken with water. Draw a conclu¬ sion regarding the solubility of calcium hydroxide in water. b. Taste cautiously of the solution saved from a, and describe the taste. Determine the reaction toward litmus; is the solution acid, alkaline, or neutral? Is the reaction marked? Heat the solution slowly to boiling, and describe the result. What is the effect of in¬ creased heat on the solubility of calcium hydroxide in water? c. State the result of (1) exposing calcium hydroxide solution to the air, and (2) exhaling the breath through calcium hydroxide so¬ lution. Express each reaction by an equation. CALCIUM — STRONTIUM — BARIUM 139 Experiment 188 — Mortar Materials. — Lime, sand, old mortar or plaster. Apparatus. — Bottle fitted with cork. a. Prepare slaked lime by adding hot water slowly to about 30 gm. of lime. Add just enough water to make a stiff paste. Add about 50 gm. of sand, more water if necessary, and mix well. Divide into three portions. Spread one portion upon a piece of brick, press an¬ other piece of brick upon it, and let the whole remain undisturbed for several days. State the final result. b. Spread another portion in a thin layer on a board or a glass plate, and let it remain as in a. Test it finally for a carbonate and state the result. c. Put the third portion in a bottle and ©ork tightly. In a day or two test as in b. Compare the results of b and c. d. Test a lump of old mortar or plaster for a carbonate and state the result. Experiment 189 — Properties of Cement a. Mix a little cement with enough water to form a thick paste and spread the paste in a thin layer on a block of wood or a glass plate. Let it remain undisturbed for a day or more, then examine, describe, and explain. b. Prepare two paper cylinders by rolling a sheet of paper around a test tube. Close one end by folding over the edges of the paper. Fill an evaporating dish nearly half full of cement, add about the same bulk of sand, and mix well. Add water and stir until a soft paste is formed. Pour half the mixture into each paper cylinder and slip an elastic band over the upper end to hold the paper in place. Lower one cylinder into a bottle of water and the other into an empty bottle (Fig. 90). Let both stand for a day or two. Then remove, unroll the paper, and compare the contents. State the result. What property of cement is shown by this experi¬ ment? (left), in water (right) Experiment 190 — Analysis of Cement Materials. — Cement, solutions for c and d. a. Preparation of Sample.—Put about 1 gm. of cement in an evaporating dish, add concentrated hydrochloric acid, and heat (in 140 EXPERIMENTS IN PRACTICAL CHEMISTRY the hood) until the cement dissolves. (Filter, if not clear.) Then evaporate to dryness, add a little dilute hydrochloric acid and 25 cc. of water, and warm gently. Filter and wash the precipitate with a little water. Save the precipitate for b and the filtrate for c. b. Silica. — Test the precipitate for silica by Exp. 156. State the result. c. Aluminium and Iron. — To the filtrate from a add ammonium hydroxide to alkaline reaction, warm, and filter. Save this filtrate for d. Proceed with the precipitate as in (1) and (2). (1) Dissolve a portion of the precipitate in sodium hydroxide solution and add ammonium chloride solution; the precipitate is aluminium hydroxide. Describe it. (2) Dissolve another portion in dilute hydrochloric acid, add a little concentrated nitric ^cid, and boil. Cool and add a little potas¬ sium sulphocyanate solution; the red color of the liquid is due to ferric sulphocyanate, and its formation is a test for iron. d. Calcium. — To the filtrate from c add ammonium chloride solution, ammonium hydroxide, and then considerable ammonium oxalate solution. State the result. Experiment 191 — Calcium Compounds and Hardness of Water Materials. — Calcium hydroxide, solutions of soap, calcium sulphate, sodium carbonate, and borax. Apparatus. — Carbon dioxide generator (see Fig. 68). a. Temporary Hardness. — Prepare a solution of acid calcium carbonate by passing carbon dioxide into a mixture of 25 cc. of satu¬ rated calcium hydroxide'and 25 cc. of water (distilled or good quality) until the precipitate is formed and redissolved (see Exp. 121). (1) To 15 cc. of the clear acid calcium carbonate solution add 5 cc. of soap solution. Shake well and observe the result. Describe the product. Rub some between the fingers and describe the result. (2) Boil vigorously 15 cc. of acid calcium carbonate solution for a few minutes, filter, and add 5 cc. of soap solution. Shake well and observe the result. Compare the results of (2) and (1). (3) To 10 cc. of clear acid calcium carbonate solution add 5 cc. of saturated calcium hydroxide, shake, filter, and to the clear filtrate add 5 cc. of soap solution. Shake well and observe the result. Com¬ pare the results of (3), (2), and (1). b. Permanent Hardness. — (1) Proceed as in a (1), using 15 cc. of calcium sulphate solution (instead of acid calcium carbonate so¬ lution). Compare the results of b (1) and a ( 1 )- CALCIUM — STRONTIUM — BARIUM 141 (2) Boil 15 cc. of calcium sulphate solution, add 5 cc. of soap so¬ lution, and shake. Compare the results of b (2), b (1), and a (2). (3) To 15 cc. of calcium sulphate solution add 10 cc. of sodium carbonate solution, filter, add 5 cc. of soap solution, and shake well. Compare the results of b (3) and b (2). c. Optional. Try the effect of (1) ammonium hydroxide (in ex¬ cess, as told by the odor), and (2) borax solution on both temporarily and permanently hard water. Experiment 192 — Plaster of Paris Materials. — Plaster of Paris, vaseline. Mix a little plaster of Paris with enough water to form a thick paste. Put the paste on a block of wood or a glass plate. Rub a very little vaseline on one side of a coin, and press the coin, coated side down, into the paste. Let it stand undisturbed for fifteen or more minutes. Then remove the coin carefully, and examine and de¬ scribe the effect on the hardened plaster. Experiment 193 — Tests for Strontium and Barium Materials. — Strontium compounds, calcium sulphate solution; ba¬ rium compounds, potassium dichromate solution, acetic acid. A. Strontium. — a. Apply the flame test to strontium nitrate and other available strontium compounds, using a clean test wire in each case. How is the flame colored? Compare with the color pro¬ duced by calcium compounds. b. To the solution of a strontium compound add calcium sulphate solution. The precipitate is strontium sulphate. Write the equation. B. Barium. — a. Proceed as in A a, using barium nitrate and other available barium compounds. b. Add dilute sulphuric acid to barium chloride solution (or the solution of any barium compound). The precipitate is barium sul¬ phate. Describe it. Test it's solubility by heating a little of the precipitate in concentrated hydrochloric acid. State the result. c. Add potassium dichromate solution to barium nitrate solution. The precipitate is barium chromate. Describe it. Test its solu¬ bility by heating some of the precipitate separately in acetic acid and concentrated hydrochloric acid. State the results. 142 EXPERIMENTS IN PRACTICAL CHEMISTRY Experiment 194 — Red Fire and Green Fire (Demonstration Experiment) Materials. — Strontium nitrate, powdered potassium chlorate, powdered shellac, barium nitrate. a. Mix carefully small and equal (in bulk) quantities of strontium nitrate, potassium chlorate, and shellac on a sheet of paper. Place the mixture in an iron pan or on a brick in the hood, and set it afire. Describe the result, especially the color. b. Proceed as in a, using barium nitrate instead of strontium nitrate. IRON (Practical Chemistry, pp. 391-413, §§ 487-510) Experiment 195 — Properties of Iron Materials. — Cast and wrought iron, steel; iron wire, thread, and powder; special steels. Apparatus. — Electric bell and battery, magnet. a. Examine typical specimens of cast iron, wrought iron, and steel, and state their characteristic physical properties. b. Hold a piece of iron wire in the flame for a minute or two. Is iron a good conductor of heat? Introduce a piece of iron wire into the circuit with an electric bell. Is iron a good conductor of elec¬ tricity ? c. Determine the specific gravity of a sample of iron and of steel by the method given in Exp. 104 b. d. Try the action of a magnet on iron and steel. State the result. e. Drop a pinch of iron powder into a Bunsen flame. Hold a piece of iron thread in the flame. Describe the results, and draw a con¬ clusion. f. Perform, recall, or repeat (if necessary) experiments which show the action of heated iron and (1) oxygen, (2) chlorine, (3) nitro¬ gen, (4) nitrous oxide, and (5) sulphur. State each result. g. As in f, experiments showing the action of acids with iron. State the results. h. Test the hardness of (1) different varieties of steel and (2) spe¬ cial steels by striking them with a hammer. Experiment 196 — Analysis of Slag Pulverize a sample of slag (or use mineral wool) and test it for (1) silica (Exp. 156) and (2) calcium. State each result. IRON 143 Experiment 197 — Tests for Ferrous Compounds Materials. — Iron powder (or filings), solutions of sodium hydroxide and potassium ferricyanide. Put 1 or 2 gm. of iron in a test tube, add about 10 cc. of dilute hy¬ drochloric acid, and warm gently; ferrous chloride is formed (in solution). Proceed at once with the tests. (1) Pour a little ferrous chloride into a test tube one-third full of sodium hydroxide solution and shake. The precipitate is ferrous hydroxide. Note the color. Shake, and describe the changes in color. (2) Add 5 cc. of ferrous chloride to 5 cc. of potassium/emcyanide solution. The precipitate is ferrous ferricyanide. Note the color. Experiment 198 — Tests for Ferric Compounds Materials. — Solutions of ferric chloride, sodium hydroxide, potassium sulphocyanate, and potassium ferrocyanide. (1) Add 5 cc. of sodium hydroxide solution to 5 cc. of ferric chlo¬ ride solution. The precipitate is ferric hydroxide. Note the color. (2) To 5 cc. of ferric chloride add 5 cc. of potassium /errocyanide solution. The precipitate is ferric ferrocyanide. Note the color. (3) Add 5 cc. of potassium sulphocyanate solution to 5 cc. of ferric chloride solution. The wine-red colored solution is caused by soluble ferric sulphocyanate. This test readily distinguishes ferric from ferrous compounds. Experiment 199 — Reduction and Oxidation of Iron Compounds Materials. — Ferric chloride solution, zinc, ferrous sulphate, potassium chlorate. a. Put a piece of zinc in ferric chloride solution made slightly acid by hydrochloric acid. After the operation has proceeded for about fifteen minutes, test separate portions of the solution for a ferrous and a ferric compound by Exps. 197 (2) and 198 (3). State and explain the results. b. (1) To a solution prepared from fresh, or freshly washed, fer¬ rous sulphate add a little hydrochloric acid, warm gently, and then add a few crystals of potassium chlorate. After heating a short time, test separate portions of the solution for a ferric and ferrous com¬ pound (as in a). State and explain the results. 144 EXPERIMENTS IN PRACTICAL CHEMISTRY (2) Add 10 cc. of concentrated nitric acid, drop by drop, to a hot solution of ferrous sulphate to which a little sulphuric acid has been added, and boil. Test and explain as in (1). Experiment 200 — Hydrolysis of Ferric Chloride Test ferric chloride solution with litmus paper (both kinds). State and explain the result. Compare with Exp. 175. Experiment 201 — Testing for Iron Materials. — Clay, brick, flower pot, bauxite, rusty rock, rouge, sheet tin, iron rust, bluing, solutions of potassium ferricyanide and potas¬ sium sulphocyanate. a. Prepare a solution of the solids by boiling a little of the pow¬ dered material with concentrated hydrochloric acid. Test the clear solution for iron, both ferric and ferrous, and state the result in each case. b. Obtain “ unknowns ” and test them for iron as in a. c. Add considerable sodium hydroxide solution to a dilute solu¬ tion of bluing. Describe and explain the result. ALUMINIUM (Practical Chemistry, pp. 415-424, §§ 511-524) Experiment 202 — Properties of Aluminium a. Proceed with aluminium as in Exp. 195 b, c, d. b. Warm a piece of aluminium with concentrated hydrochloric acid. Test the escaping gas with a blazing joss stick. What is the gas ? What compound of aluminium is formed ? c. Boil a piece of aluminium with concentrated sodium hydroxide solution. Test as in b. Answer the questions in b. Experiment 203 — Aluminium Hydroxide Materials. —- Solutions of aluminium sulphate, ammonium hydroxide, sodium hydroxide, potassium hydroxide, ammonium sulphide, and sodium carbonate. I. Preparation. — a. Add ammonium hydroxide to a solution of aluminium sulphate, and shake well. The precipitate is alumin¬ ium hydroxide ; save it for II. ALUMINIUM H5 b. Proceed as in a, using aluminium sulphate solution and a very little sodium hydroxide solution. Compare-with the result in a. Save this precipitate for II. II. Properties.— a. Examine the precipitate from I a and note its properties, e.g. color, texture, etc. Remove a little and rub it between the fingers ; describe the result. b. To the precipitate from I b add sodium hydroxide slowly and shake constantly until the precipitate dissolves. What aluminium compound is formed? c. To a portion of the precipitate from I a add considerable ammo¬ nium hydroxide, and shake well. Compare with the result in II b. d. Add dilute hydrochloric acid to a portion of the precipitate from I a, and shake well. State the result. Proceed similarly with other acids, e.g. sulphuric and acetic. State the results. Experiment 204 — Clarification of Water See Exp. 26 c. Experiment 205 — Thermit (Demonstration Experiment) Materials. —- Thermit, granulated aluminium, barium dioxide, magnesium ribbon. Apparatus. — Sand crucible 10 cm. (4 in.) deep, brick, sand, iron pan. Caution. — Perform this experiment carefully. The molten metal may spatter. Fill an iron pan with sand and stand it on a brick. Bury the cruci¬ ble about halfway in the sand; a box of sand should be near by in case the crucible should break. Put about 30 gm. of thermit in the crucible. Prepare a fuse mix¬ ture by mixing thoroughly about 5 gm. of barium dioxide and 0.5 gm. of granulated aluminium. Make a hole in the top of the thermit and pour in the fuse mixture; insert a piece of magnesium ribbon into the heap of fuse mixture. Light the magnesium with the Bunsen flame, and stand aside immediately. The reaction is vigorous. De¬ scribe it. When the crucible is cool, break it open and examine the contents. Describe the two parts. What is the name of each? Experiment 206 — Tests for Aluminium Materials. — Aluminium sulphate, cobaltous nitrate solution, charcoal, a. Proceed as in Exp. 203 I a, using an aluminium solution. 146 EXPERIMENTS IN PRACTICAL CHEMISTRY b. To a portion of the aluminium solution add a little sodium hydroxide solution and then an excess. To another portion add an excess of ammonium hydroxide. Note each result. c. Heat a little aluminium sulphate (or any other aluminium com¬ pound) on charcoal in the blowpipe flame (oxidizing — see Exp. 134 B). Cool, and moisten with a drop or two of cobaltous nitrate solution. Heat again, and note the color of the residue. Experiment 207 — Preparation and Properties of Alum Materials. — Aluminium sulphate, potassium sulphate. I. Preparation. — Mix 8 gm. of aluminium sulphate and 4 gm. of potassium sulphate, and dissolve the mixture in about 50 cc. of hot water. Pour the solution into dish or beaker (Fig. 91) and set it aside to crystallize; well-formed crystals may be obtained upon a thread suspended in the solution. (Meanwhile proceed with II a, etc.). Crystals of potassium alum will be deposited. Remove the best ones; dry and examine. De¬ scribe them, giving color, luster, size, and crystal form. II. Properties. — a. Test a solution Fig. 91. — Crystallizing alum of alum separately for aluminium and sulphate ions, and state the result. Cautiously taste the solution, and describe the result. b. Test alum for water of crystallization, and state the result. c. Select several good crystals from those prepared in I and ex¬ amine them carefully. Describe them. Test as in II, and state the results. Allow some crystals to remain exposed to the air for several hours. Compare finally with the original crystals. Explain the difference. Experiment 208 — Aluminium Salts as Mordants Materials. -— Solutions of alum, cochineal, and aluminium acetate; aliz¬ arin paste, cotton cloth. a. Add a little alum solution to a dilute solution of cochineal, then add ammonium hydroxide and shake well. Filter, and compare the colors of the filtrate and precipitate. COPPER 147 b. Boil two small pieces of cotton cloth for several minutes thoroughly in water. Remove the excess of water. (1) Put one piece in a dish or beaker, add 50 cc. of water and 5 cc. of alizarin paste, and heat nearly to the boiling point for about two minutes. Wash the cloth in water, dry, and then examine. (2) Now proceed in the same way with a piece of cotton cloth which has been previously mordanted by boiling for about two minutes in aluminium acetate so¬ lution. Compare the two pieces of cloth. Explain. Experiment 209 — Hydrolysis of Aluminium Salts Test a solution of aluminium sulphate and of alum with litmus paper. State and explain each result. Compare with Exds. 17 c and 200. COPPER (Practical Chemistry, pp. 426-437, §§ 525-527) Experiment 210 — Properties of Copper Apparatus. — Electric bell and battery, magnet. a. Proceed with copper as in Exp. 195, b, c, d. b. Heat a piece of copper wire in the flame until it burns. Note the color. What compound is formed? c. What is the effect of dilute nitric acid on copper? Experiment 211 — Tests for Copper Materials. — Copper wire, copper sulphate solution, ammonium hydrox¬ ide, acetic acid, potassium ferrocyanide solution. a. Heat a copper wire, or a copper compound in the Bunsen flame, and observe the color imparted to the flame. b. Add considerable ammonium hydroxide to copper sulphate solution, shake well, and observe the result. The formation of the blue solution is the usual test for copper. c. Add to a test tube one-fourth full of water an equal volume of copper sulphate solution, and shake ; then add a few drops of acetic acid and of potassium ferrocyanide solution. The brown precipitate is cupric ferrocyanide (Cu2Fe(CN)e). Experiment 212 — Properties of Copper Sulphate a. Examine a typical specimen of crystallized copper sulphate, and state its characteristic properties. See also Exps. 42, 43. 148 EXPERIMENTS IN PRACTICAL CHEMISTRY b. Let red and blue litmus paper remain in copper sulphate solu¬ tion for fifteen minutes or more. State and explain the result. Com¬ pare Exps. 175, 200, 209. Experiment 213 — Tests for Copper in Alloys Materials. —Brass, aluminium bronze, German silver, American cent, nickel, and dime. a. Prepare a solution of one of the alloys enumerated above by boiling a small piece in dilute nitric acid; it may be necessary to treat the alloy with several portions of acid. Filter the final liquid if it is not clear. Apply the test for copper to the clear solution as in Exp. 211 b. Be sure to add an excess of ammonium hydroxide and shake well. State the result in each case. b. Proceed as in a with “ unknowns” and with metallic substances suspected to contain copper, e.g. pins and inexpensive jewelry. Experiment 214 — Displacement of Metals — Copper Materials. — Copper wire, iron nail, zinc, copper sulphate solution, mer¬ curic chloride solution (Poison). a. Put a clean copper wire in a test tube half full of mercuric chlo¬ ride solution (Poison). After a short time remove the wire and wipe it with a soft cloth or paper. Observe and explain the change. b. Put a clean iron nail in a test tube half full of copper sulphate solution. After a short time remove the nail and examine it. What is the deposit ? Explain its formation. c. Repeat b, using a strip of zinc instead of an iron nail. Observe and explain the result. Required Exercise. — Arrange the metals (used in this experiment) in the order of their displacing power with reference to copper. MAGNESIUM — ZINC — MERCURY (Practical Chemistry, pp. 439-45°* §§ 538-560) Experiment 215 — Properties of Magnesium and Zinc a. Proceed with magnesium and zinc as in Exp. 195 b, c, d. b. Perform, recall, or repeat (if necessary) experiments showing the results of heating magnesium and zinc (1) in a limited supply of air and (2) in an abundance of air; and also treating magnesium and zinc with acids. State the results. MAGNESIUM — ZINC — MERCURY 149 Experiment 216 — Tests for Magnesium Materials. — Solutions of magnesium sulphate, ammonium chloride, ammonium hydroxide, discdium phosphate. a. To a solution of a magnesium compound, e.g. magnesium sul¬ phate, add successively solutions of ammonium chloride, ammonium hydroxide, and disodium phosphate. A precipitate of ammonium magnesium phosphate (NH 4 MgP 0 4 ) is formed. Describe it. b. Heat a little magnesium sulphate on charcoal, in a blowpipe flame, as in Exp. 206 c. Note the color of the residue. Compare with Exp. 206 c. Experiment 217 — Testing for Magnesium Materials. — Magnesia (“85 per cent”), substances as in b. a. Boil a gram or two of “ 85 per cent magnesia ” pipe covering with dilute hydrochloric acid. Filter and test the filtrate (diluted) for magnesium. State the result. b. Proceed as in a with (1) magnesia, (2) milk of magnesia, (3) flashlight powder, (4) Epsom salts, (5) magnesite. State each result. Experiment 218 — Tests for Zinc Materials. — Zinc, zinc sulphate and cobalt nitrate solutions, zinc oxide, blowpipe, charcoal. a. Apply tests for metallic zinc (see Exp. 215). b. Add a very little sodium hydroxide solution to a solution of a zinc compound, e.g. zinc sulphate, and shake well. Describe the precipitate. What is it? Divide the mixture into three parts. (1) To one add considerable sodium hydroxide, (2) to another add ammonium hydroxide, and (3) to the third add dilute hydrochloric acid. Shake each well, and observe the result. What is the name and formula of the zinc compound formed in (1) and (3) ? c. Proceed as in Exp. 206 c, using zinc oxide (or any other zinc compound). Note the color on the charcoal. Compare with Exps. 206 c, 216 b. d. Add hydrogen sulphide water to zinc sulphate solution and note the color of the precipitate. What is the name of the precipitate ? Write the equation. Experiment 219 — Zinc Hydroxide Materials. — Solutions of zinc sulphate, ammonium hydroxide, sodium hydroxide, potassium hydroxide, ammonium sulphide, and sodium carbonate. 150 EXPERIMENTS IN PRACTICAL CHEMISTRY Proceed as in Exp. 203, using zinc sulphate instead of aluminium sulphate. Compare the behavior of aluminium and zinc hydroxides when treated with ammonium hydroxide. Experiment 220 — Properties of Mercury Material. — Mercury. a. Pour a drop or two of mercury into an evaporating dish. Ex¬ amine the mercury, and state its characteristic properties. Agitate the dish, and describe the result. b. Stand a funnel in a test tube and carefully pour the mercury from the dish into the test tube. Remove the funnel. Heat the bottom of the test tube gently and observe the result, especially the deposit, if any, upon the upper part of the tube. Scrape a little out of the tube with a glass rod. What is the deposit ? What property of mercury is shown by this experiment ? c. Suggest a method of determining the specific gravity of mer¬ cury. If approved by the Teacher, try it. Experiment 221 — Mercurous and Mercuric Compounds Materials.' —Solutions of mercurous nitrate, mercuric chloride (Poison), and stannous chloride. I. Mercurous. — a. Add a few drops of hydrochloric acid to a little mercurous nitrate solution. The precipitate is mercurous chlo¬ ride. Describe it. Note its insolubility in water and in dilute hydro¬ chloric acid. Add an excess of ammonium hydroxide. The black precipitate is a test for mercury in mercurous compounds. b. Add potassium iodide solution to mercurous nitrate solution. Describe the result. Give the name and formula of the mercury compound formed. Write the equation. II. Mercuric. — a. Add a few drops of hydrochloric acid to a little mercuric nitrate solution. Compare with the result in I a. Add a few drops of ammonium hydroxide, or enough to produce a de¬ cided change. Compare with I b. The precipitate is mercuric am¬ monium chloride. b. Proceed as in I b, using mercuric chloride solution (Poison). Compare the results. Give the name and formula of the mercury compound formed. Write the equation. c. Add a little stannous chloride solution to mercuric chloride and note the result; then add considerable stannous chloride solution TIN — LEAD I 5 i and note the change. Write equations for the reactions. (Note. — This is the usual test for mercuric compounds). Experiment 222 — Displacement of Metals — Magnesium, Zinc, and Mercury Proceed as in Exp. 214, using these metals and solutions of several metallic compounds, e.g. copper sulphate, lead nitrate, silver nitrate, and stannous chloride. Try also other metals and solutions of salts of magnesium, zinc, and mercury. Note each result and prepare a table showing the displacing power of the metals. (Compare Exp. 214.) TIN —LEAD (Practical Chemistry, pp. 452-462, §§ 561-578) Experiment 223 — Properties of Tin and Lead a. Proceed with tin and lead as in Exp. 195 b, c, d. b. Bend a piece of tin and note the crackling noise. c. Heat a small piece of tin in a test tube with concentrated hydro¬ chloric acid in the hood until most of the tin disappears. Stannous chloride is formed. Save this solution for Exp. 224. d. Add a small piece of tin to a test tube one-fourth full of con¬ centrated nitric acid in the hood. Stand the test tube in the rack as soon as the action begins. The product is metastannic acid. De¬ scribe it. Compare the action of nitric acid on tin, copper, and zinc. e. Heat a small piece of tin with aqua regia in a test tube in the hood. Observe the result. What tin compound is formed ? f. Rub a piece of lead on a hard surface, or with the fingers. State the result. Experiment 224 — Test for Tin Materials. — Solutions of stannous chloride and mercuric chloride (Poison). , Add a few drops of stannous chloride solution (saved from Exp. 223 c) to mercuric chloride solution. The white precipitate is mer¬ curous chloride. Add considerable stannous chloride and warm gently. The gray-black precipitate is finely divided mercury. Write the equations for both reactions. 152 EXPERIMENTS IN PRACTICAL CHEMISTRY Experiment 225 — Tests for Lead Materials. — Lead nitrate and potassium dichromate solutions. a. Reduce lead oxide (or other lead compounds) in the blowpipe flame. (See Exp. 134 A a.) b. Add hydrogen sulphide solution to a solution of a lead com¬ pound. Note the color. Give the name and formula of the pre¬ cipitate. c. Add dilute hydrochloric acid to a little lead nitrate solution until precipitation ceases. The insoluble precipitate is lead chloride. Boil some of the precipitate with considerable water. Describe the action. d. Add dilute sulphuric acid to a little lead nitrate solution until precipitation ceases. Give the name and formula of the precipitate. Observe its properties. Is it soluble in hot water? Try it. e. Repeat d, using potassium dichromate solution instead of sul¬ phuric acid. Give the name and formula of the precipitate. De¬ scribe it, especially the color. Experiment 226 — White Lead Materials. —- Lead monoxide, acetic acid, white lead. Apparatus. — Carbon dioxide generator. a. Heat about 15 cc. of acetic acid in a test tube nearly to boiling, and add about 5 gm. of lead monoxide in small portions. Meanwhile do b. Shake and heat at intervals until most of the solid disappears. Then add about 5 cc. of water, and filter, if the liquid is not clear. Pass carbon dioxide (free from acid) through the filtrate (see Exp. 120 and Fig. 68), and note the result. What is the name and formula of the product? Filter, and use the precipitate in c. b. Test white lead for (1) lead and (2) a carbonate. State the results. c. Proceed as in b with the precipitate from a. Experiment 227 — Displacement of Metals — Tin and Lead Proceed as in Exps. 214, 222 using tin and lead with solutions of metals. Tabulate the results and compare with similar experiments. Experiment 228 — Testing for Lead a. Warm thin shavings of solder with dilute nitric acid, filter, and test the filtrate for lead. SILVER — GOLD 153 b. Proceed as in a using one or more of the following: Tea lead, type metal, plumbago, shot, bullets, metallic cap of a bottle, “ lead ” of a lead pencil, and “ unknowns.” c. Apply the (reduction) blowpipe test for lead to white lead, red lead, litharge, dry paint, chrome yellow, and “ unknowns.” Experiment 229 — Qualitative Analysis of a Solution of Lead, Silver, and Mercury (ous) . Materials. — Solution containing lead nitrate, silver nitrate, and mer¬ curous nitrate; hydrogen sulphide water, potassium dichromate. a. To 10 cc. of the solution add dilute hydrochloric acid drop by drop until precipitation ceases. Allow the mixture of precipitated chlorides to settle, pour off the liquid carefully, add about 15 cc. of water, boil, and filter. This operation dissolves the lead chloride. Test the filtrate for lead as in b; save the precipitate for c. b. To separate portions of the filtrate add hydrogen sulphide water and potassium dichromate solution. Note each result. c. Wash the precipitate from a with hot water until the wash water does not give a test for lead. Then stand the funnel in a clean test tube and pour ammonium hydroxide on the mixture of silver and mercurous chlorides. This operation dissolves the silver chloride. Test the filtrate as in d; save the precipitate for e. d. To the filtrate from c add dilute nitric acid to acid reaction and shake. The silver compound is precipitated as silver chloride. e. The black residue on the paper is a sufficient test for mercury. Confirm thus: Pour a little aqua regia (mixture of 3 cc. of concen¬ trated hydrochloric acid and 1 cc. of concentrated nitric acid) upon the black precipitate; catch the filtrate in a porcelain dish, dilute with about 5 cc. of water, and add a clean copper wire; remove the wire in a few minutes, wipe gently, and mercury will be seen on the wire as a bright silvery coating. SILVER — GOLD (Practical Chemistry, pp. 464-472, §§ 579 “ 595 ) Experiment 230 — Tests for Silver Materials. — Silver coin, hydrogen sulphide, silver nitrate solution. a. Hold a silver coin at the mouth of a bottle of hydrogen sulphide water, and note the change in color. What silver compound is formed ? 154 EXPERIMENTS IN PRACTICAL CHEMISTRY b. Add dilute hydrochloric acid to a silver solution, e.g. silver nitrate, and shake. Next add considerable ammonium hydroxide and shake, and then add dilute nitric acid to acid reaction. The precipitation of silver chloride, its solubility in ammonium hydroxide, and its reprecipitation by dilute nitric acid constitute the usual test for silver. Experiment 231 — Displacement of Metals — Silver Summarize the results of previous experiments in which silver or silver solutions were used. Experiment 232 — Cleaning Tarnished Silver Materials. — Silver coin, aluminium, sodium carbonate. Dissolve io gm. of sodium carbonate in about 50 cc. of water and heat to boiling. Put a small piece of aluminium and a tarnished silver coin into the solution; have the metals in contact. Remove and examine the coin after a few minutes. State the result. Experiment 233 — Preparation and Properties of Silver Halides Materials. — Solutions of silver nitrate, potassium chloride, potassium bromide, potassium iodide, sodium thiosulphate. To separate portions of silver nitrate solution add the chloride, bromide, and iodide solution. Observe and state the color of each precipitate. Filter each separately. Test each precipitate separately by (1) exposing a little to the light, (2) shaking some with ammonium hydroxide, and (3) shaking some with sodium thiosulphate solution. State each result. Compare their behavior under the same conditions. Experiment 234 — Silver Salts and Photography Materials. — Dilute silver nitrate (17 gm. to a liter), sodium chloride (5.8 gm. to a liter), and sodium thiosulphate solutions — “hypo” (250 gm. to a liter); commercial developer or a substitute (see App. § 6, List G). Apparatus. — 4 Test tubes (labeled), black paper, 2 plates (preferably lan¬ tern slide plates). Note. — Owing to the rapid action of silver bromide, silver chloride is used. a. Add 5 cc. of the silver nitrate solution to 5 cc. of the sodium chloride solution, shake gently, and expose the precipitate to the CHROMIUM — MANGANESE 1 55 light. Examine frequently and note the time needed for a definite change in color. b. Prepare silver chloride as in a, and add also 5 cc. of the de¬ veloper. Expose, and note the time as in a. Compare the times. c. Wrap a piece of dark paper around a test tube to protect it from the light, and add the three solutions as in b. After half a min¬ ute, examine quickly and note the color. Examine again after half a minute more. Compare with b. d. Prepare silver chloride as in a, add also 5 cc. of “ hypo ” solu¬ tion, and shake well. Note the result. e. Optional. Try a to d with silver bromide (prepared from dilute silver nitrate and potassium bromide solutions) and compare the results with a to d. f. Demonstration Experiment. Expose two photographic plates (preferably lantern slide plates) or films, develop both in the dark room with the class, fix one, and later compare both. Make two prints from the fixed plate, and develop. Wash one, and later com¬ pare the two prints. Experiment 235 — Properties of Gold Materials. — Gold, chlorine water, stannous chloride solution. a. Proceed as in Exp. 62 b. What gold compound is formed? Save the liquid for c. b. Proceed as in Exp. 67. What gold compound is formed? Save the liquid for c. c. Heat (in the hood) the solutions from a and b until most of the chlorine has been driven off, dilute the final solution with water, and then slowly add a little dilute stannous chloride solution. A purple (or black) precipitate of finely divided gold is produced. Its forma¬ tion is a test for gold. CHROMIUM — MANGANESE (Practical Chemistry, pp. 474-477, §§ 596-605) Experiment 236 — Tests for Chromium Materials. — Borax, chrome alum, potassium carbonate, potassium nitrate, acetic acid, nitric acid; sodium hydroxide, lead nitrate, and potassium dichromate solutions. a. Apply the borax bead test to chrome alum or other chromium compounds (see Exp. 180). 156 EXPERIMENTS IN PRACTICAL CHEMISTRY b. Mix equal small quantities of potassium carbonate, potassium nitrate, and powdered chrome alum, place the mixture on a piece of porcelain, hold it with the test tube holder, or stand it on a wire gauze, and heat intensely until the mixture fuses. A yellow mass, due to the presence of potassium chromate, resuits. If the color is not marked, dissolve the mass in water, add acetic acid, slowly.at first, and then boil until the carbon dioxide is expelled. Add a few drops of lead nitrate solution to a portion, and yellow lead chromate is precipitated. (If the precipitate is white, it is lead carbonate, and shows that not all the potassium carbonate was decom¬ posed, as intended.) c. Proceed as in Exp. 225 e, using potassium chromate or dichro¬ mate solution. State the result. Experiment 237 — Potassium Chromate and Dichromate Materials. — Potassium chromate and dichromate, concentrated hydro¬ chloric acid, potassium hydroxide solution. a. Prepare a dilute solution of potassium chromate and dichro¬ mate, and compare the colors. Save for b and c. b. Add concentrated hydrochloric acid to 5 cc. of the solution of potassium chromate prepared in a, shake well, and observe the change in color. Describe it. Compare with the color of the potassium dichromate solution. Into what compound has potassium chro¬ mate been changed ? c. Add potassium hydroxide solution to 5 cc. of the solution of potassium dichromate prepared in a until a change of color is pro¬ duced. Describe the color. Compare with the potassium chromate solution. Into what compound was the potassium dichromate changed ? d. Add a few drops of concentrated hydrochloric acid to powdered potassium chromate and dichromate in separate test tubes. What gas is evolved? Experiment 238 — Tests for Manganese Materials. — Manganese dioxide, potassium carbonate, potassium ni¬ trate, ammonium sulphide, manganese sulphate solution, hydrochloric acid, acetic acid, ammonium hydroxide. a. Apply the borax bead test to manganese dioxide (or any other manganese compound — see Exp. 180). CHROMIUM — MANGANESE 157 b. Fuse on a piece of porcelain (as in Exp. 236 b) a little man¬ ganese dioxide mixed with potassium carbonate and potassium nitrate. The green color of the mass is due to potassium manganate. c. Add ammonium sulphide to manganese sulphate solution. The flesh-colored precipitate is manganese sulphide. Compare with other sulphides as to color (see Exp. hi). APPENDIX 1 . The Pressure of Water Vapor in millimeters of mercury is: — Tem¬ Vapor Tem¬ Vapor Tem¬ Vapor perature Pressure perature Pressure perature Pressure 12 10.5 17 14.4 22 •19.7 12.5 10.8 17-5 14.9 22.5 20.3 13 11.2 18 15-4 23 20.9 I 3-5 11.6 18.5 15-9 23-5 21.5 14 11.9 19 16.4 24 22.2 14.5 12.3 19-5 16.9 24-5 22.8 15 12.7 20 17.4 25 23.6 I 5 -S i 3 -i 20.5 18.0 25-5 24-3 16 13.6 21 18.5 26 25.0 16.5 14.0 21.5 19.1 26.5 25-7 The numbers in the Vapor Pressure columns are the values for a in the formula for the reduction of gas volumes (see the author’s Practi¬ cal Chemistry, § 74). 2 . Laboratory Equipment. — These lists include the apparatus, chemicals, and supplies needed for the experiments in this book. No allowance is made for breakage, duplicate corks and rubber stop¬ pers, and extra glass and rubber tubing. List A — Individual Outfit. This list includes the articles needed by each pupil (see frontispiece). 1 Blowpipe. 1 Blowpipe tube. 1 Beaker, 250 cc. 5 Bottles, wide mouth, 250 cc. 1 Bottle, generator, 250 cc. 1 Bunsen burner. 1 Cork to fit smaller test tube. 1 Cork to fit larger test tube. 1 Crucible and cover, porcelain, No. o. 1 Crucible block, wood, 10 X 10 X 2.5 cm. with 3 cm. hole in center. 1 Deflagrating spoon. 1 Evaporating dish, 7 cm. 1 Flask, Erlenmeyer, 250 cc. 100 Filter papers, 10 cm. 1 Forceps, iron. 1 Funnel, 65 mm. 4 Glass plates, 10 X 10 cm. APPENDIX 159 1 Glass plug (see Exp. 55). 1 Glass rod, 15 cm. 1 Glass tube, 150 cm. 1 1 Graduated cylinder, 25 cc. 1 Iron stand, clamp (medium), ring (8 cm.). 1 Matches (box). 1 Mortar and pestle, 8 cm. 1 Pinch-clamp, Mohr’s. 2 1 Pneumatic trough, complete. 3 1 Rubber stopper, 23 mm., 1-hole. 4 2 Rubber stoppers, 23 mm., 2-hole. 4 1 Rubber tube, 6 mm. (^ in.) diam., 60 cm. long (for burner). 1 Rubber tube, ^ in. diam., 15 cm. long (for connectors). 1 Rubber tube, pressure (^- in. diam.), 15 cm. long (for drop¬ ping funnel). 2 1 Sponge. 12 Test tubes, 15 X 1.8 cm. (6 X f in.) (“small” test tube). 3 Test tubes, 20 X 2.5 cm. (8X1 in.) (“large” test tube). 1 Test tube brush. 1 Test tube holder. 1 Test tube rack. 1 Test wire (see Int. 6, d.). 1 Thistle tube, straight stem. 2 1 Triangle. 5 1 Wire gauze, 10 X 10 cm. 2 Wooden blocks, 15 X 15 X 2.5 cm. List B — Special Apparatus. apparatus needed for a class of ten. to experiments. 1 Balance, chemical ( 24 , 51 , 52 , 87 - 93 , 125 . 3 Balances, horn pan (as above). 6 1 Barometer ( 24 , 87 - 91 , etc.). 4 Beakers, 250 cc. ( 75 ). 1 Bottle, 750 cc. ( 87 ). 5 Bottles, 2500 cc. 4 Burettes, 50 cc. ( 75 ). 1 Burner, gas ( 131 ). 3 Chimneys, lamp. 1 Cork borers, set (Int. § 5 c). 1 Cylinder, graduated, 1000 cc. 2 Cylinders, graduated, 500 cc. 2 Cylinders, graduated, 250 cc. 2 Cylinders, graduated, 100 cc. 5 Crucibles, Hessian, 10 cm. deep ( 11 ). This list includes the special Numbers in parentheses refer 5 Crucibles, iron, 60 cc. ( 124 , 146 , 154 ). 2 Desiccators (optional) ( 93 ). 5 Dishes, lead ( 166 , 158 ). 2 Electric bells ( 196 , etc.). 4 Electrodes, carbon. 1 File, round (Int. § 5 c). 1 File, triangular (Int. § 3 a). 3 Flasks, Erlenmeyer, 125 cc. ( 87 ). 1 Hydrometer (heavy) ( 38 , 114 ). 1 Hydrometer (light) ( 126 , 139 ). 3 Jars, 30 X 10 cm. ( 89 , 91 ). 3 Lenses (magnifiers) ( 3 , 40 , 106 ). 2 Magnets ( 3 , 195 , etc.). 5 Pans, iron, 10 cm. 3 Retorts, stoppered, 250 cc. ( 81 ). 1 To fit the rubber stoppers. 2 See Exp. 14. The stem of the thistle tube should fit the rubber stoppers. 3 Preferable kind is an indurated fiber Keeler No. 4 provided with a shallow flower pot 10 cm. in diameter. An agateware pan may be used. 4 To fit the larger test tube. This size (about 23 mm.) also fits the average 250 cc. Erlenmeyer flask, the 250 cc. generator bottle and the 2500 cc. bottle (acid bottle — See List B). 5 To fit porcelain crucible. 6 A chemical balance costing about twenty-five dollars is sufficiently accu¬ rate. Horn pan balances, if carefully counterpoised, give acceptable re¬ sults. (Int. § 8). i6o APPENDIX 3 Rubber stoppers, i hole (for 125 cc. Erlenmeyer flask) ( 87 ). 2 Scales (Int. § 8) (constantly). 3 Screws, Hofmann ( 24 ). 3 Thermometers, — io° to ioo° C. (frequently). 5 Tubes, graduated, 100 cc. ( 89 , 91 ). 3 Watch glasses, 9 cm. ( 92 , 93 ). 1 Weights for chemical balance, 2 mg. to 50 gm. 3 Weights for horn pan balance, 2 mg. to 50 gm. 3 Weights for scales, 5 gm. to 1000 gm. 3 Wing-top burners (Int. § 3 b). List C — Demonstration Apparatus. This list includes appa¬ ratus — not in other lists — needed for the demonstration experi¬ ments. Numbers in parentheses refer to experiments. 1 Babcock apparatus complete ( 152 ). 1 Battery ( 49 , 61 , 94 , 96 - 99 , 178 ). 1 Battery jar, 12 cm. in diam. ( 61 , 178 ). 1 Chlorine tube ( 48 ). 1 Clamp (large — for condenser) (28 I). 1 Condenser, Liebig, complete (28 I). 2 Electric light bulbs ( 94 , 103 ). 1 Fire extinguisher ( 17 ). 1 Flask, 500 cc. ( 16 ). 1 Funnel, dropping, 100 cc. ( 103 ). 1 Hofmann apparatus ( 49 , 97 , 98 ). 1 Jar, oblong ( 103 ). 1 Platinum tip (optional) ( 22 ). 1 Platinum wire (optional) ( 22 ). 1 Siphon of charged water ( 15 ). 3 Stoppers, rubber, 1 hole, for U- tube (22). 1 Tube, capillary, 8 cm. ( 22 ), 1 Tube, U-, 10 cm. ( 22 ). List D — Chemicals. This list includes the quantities of chemi¬ cals needed for a class of ten. Numbers in parentheses refer to ex¬ periments. Starred items may be bought of a local dealer. Acid, acetic 250 cc. chloride 50 gm. hydrochloric 5 1 - granulated ( 205 ) 25 gm. nitric 1.5 1. lump (202) 100 gm. orthophosphoric 25 gm. sheet 600 sq. cm. oxalic ( 123 ) 100 gm. sulphate 200 gm. pyrogallic ( 55 ) 50 gm. wire 1 m. sulphuric 2.5 1. Ammoniacal liquor 150 cc. Albumin 25 gm. Ammonium carbonate 150 gm. Alcohol, ethyl 1 1 1. chloride 500 gm. methyl IOO cc. dichromate (102) 25 gm. Alizarin (paste) ( 208 ) 10 gm. hydroxide 2.5 1. Alloys, fusible ( 170 ) 25 gm. molybdate 25 gm. Alum 200 gm. nitrate (86) 150 gm. chromium 25 gm. oxalate 50 gm. Aluminium acetate 25 gm. sulphate 25 gm. bronze ( 213 ) 25 gm. sulphide IOO cc. 1 Denatured alcohol is suitable for many experiments. APPENDIX l6l Aniline (34) So cc. sheet* 50 sq. cm. Antimony chloride (168) 25 gm. sulphate 750 gm. Arsenic trioxide 25 gm. wire (No. 20)* 250 gm. Asbestos, shredded (24) 5 gm. Cream of tartar* 25 gm. Baking powder (153)* 250 gm. Dextrose. See Glucose Barium carbonate (80) 25 gm. Electrosilicon (156) 25 gm. chloride 150 gm. Ether 250 cc. chloride (pure) (71) 25 gm. Ferric chloride 50 gm. dioxide (5, 205) 25 gm. Ferrous sulphate 100 gm. hydroxide (solid) 25 gm. sulphide 500 gm. nitrate 100 gm. Gasolene* 2.5 1. sulphate (135) 25 gm. Gelatin* 25 gm. Bauxite (201) 50 gm. German silver 25 gm. Bismuth chloride 25 gm. Glass wool (24, 156) 5 gm. Bleaching powder* 250 gm. Glycerin IOO cc. Bone ash 25 gm. Glucose 150 gm. Borax* 500 gm. Gold leaf 1 bk. Brass (213)* 25 gm. Graphite 250 gm. Cadmium nitrate 25 gm. Hydrogen peroxide* 500 cc. Calcite (87) 100 gm. Hydroquinone (234, List G) 15 gm. Calcium (76, 91) 50 gm. Iodine So gm. carbonate (marble)* 2.5 kg. Infusorial earth (156) 25 gm. chloride 200 gm. Iron filings 50 gm. cyanamide (78) 25 gm. powder 200 gm. fluoride 200 gm. thread (steel wool) 50 gm. oxide (lime)* 500 gm. Joss sticks* 5 Pkg. sulphate 150 gm. Kerosene* 500 cc. Camphor (139)* 25 gm. Lead dioxide 100 gm. Carbon disulphide 500 cc. monoxide (litharge)* 150 gm. tetrachloride 500 cc. nitrate 100 gm. Carborundum, lump 25 gm. red (tetroxide)* 75 gm. powder 25 gm. sheet (thin)* 75 gm. Cement* 1 kg. sulphate (135) 25 gm. Chalk (122) 25 gm. tea (21, 228)* 2500 sq. cm. Charcoal, animal 100 gm. white (carbonate)* 50 gm. blocks 15 blk.- Litmus cubes 5 gm. wood (powd.) 150 gm. paper (each color) 6 sheets Chloroform IOO cc. Magnesium carbonate (217) 25 gm. Chrome yellow* 25 gm. chloride 25 gm. Cobalt chloride (cryst.) 25 gm. oxide 25 gm. nitrate 50 gm. powder (51) 25 gm. Cochineal 1 gm. ribbon 25 gm. Copper borings 200 gm. sulphate 100 gm. bromide 25 gm. Manganese dioxide (gra n.) 750 gm. nitrate 25 gm. dioxide (powd.) 50 gm. oxide (ic) 100 gm. sulphate 25 gm. 162 APPENDIX Mercury 25 gm. bicarbonate* 250 gm : chloride (ic) 25 gm. carbonate* 500 gm. nitrate (ous) 25 gm. chloride 2 kg. oxide ( 4 ) 25 gm. chloride (pure) ( 71 ) 25 gm. Mineral wool ( 156 ) 10 gm. citrate {See Fehling’s Naphthol (Alpha). .See List G. 25 gm. Solution, List G) 100 gm. Nickel chloride 25 gm. cobaltinitrite ( 182 ) See List G. sulphate 25 gm. dichromate 25 gm. Paraffin wax* 25 gm. hydroxide 750 gm. Phenol-phthalein solution 150 cc. hypochlorite (solution) 150 cc. Phosphorus, yellow 25 gm. nitrate 500 gm. Plaster of Paris* 150 gm. nitrite 100 gm. Potassium 1 gm. peroxide 25 gm. bromide 100 gm. phosphate (disodium) 25 gm. carbonate 150 %m. silicate (solution) 150 cc. chlorate (cryst.) 250 gm. sulphate 150 gm. chlorate (powd.) 200 gm. sulphite 200 gm. chlorate (pure) ( 71 ) 25 gm. thiosulphate (“hypo”) 300 gm. chloride 200 gm. Solder* 50 gm. chromate 25 gm. Stannous chloride. SeeLiSTG. 50 gm. dichromate {See also Battery Starch* 250 gm. Solution, List G) 250 gm. Strontium nitrate 50 gm. ferricyanide 50 gm. Sugar (cane)* 500 gm. ferrocyanide 50 gm. Sulphur, flowers 250 gm. hydroxide 150 gm. roll 750 gm. iodide 100 gm. Tannin 25 gm. nitrate 200 gm. Tartar emetic 25 gm. nitrite 50 gm. Thermit ( 205 ) 25 gm. perchlorate 25 gm. Tin, granulated ( 83 ) 100 gm. permanganate 50 gm. rod ( 223 ) 25 gm. sulphate 100 gm. Turpentine* 50 cc. sulphocyanate 25 gm. Type metal ( 228 )* 50 gm. Pumice* 10 gm. Water, distilled 3 b Rosin ( 139 )* 25 gm. Whiting ( 122 )* 25 gm. Shellac (powd.)* 50 gm. Zinc chloride 25 gm. Silver nitrate 50 gm. dust (8) 25 gm. sulphate ( 95 ) 25 gm. granulated 1 kg. Soda lime 250 gm. oxide 25 gm. Sodium 10 gm. sheet* 200 gm. acetate ( 142 ) 25 gm. sulphate 50 gm. List E — Miscellaneous Supplies. The quantities are usually small. Numbers in parentheses refer to experiments. Household ammonia, banana, beans, bluing (201), bullets (228), butter, candle, candy, carrot, celery, clay, colored and unbleached cloth, hard and soft coal, cotton, cracker, cranberry, fertilizer (165), flash light powder APPENDIX 163 (217), flour, flowerpot (201), grape juice (73), hair, horn, cast iron (195), iron nails, iron ores, iron rust, iron wire (195), wrought iron (195), junket tablet (152), karo (13), lard (144), lemon, limestone, lye (144), magnesia covering (217), milk of magnesia (217), magnesite (217), maple sugar, phosphorus tipped matches, meat, milk, mo¬ lasses, old mortar (122), nut butter (151), dry paint (228), (colored) paper, peas, phosphate rock (166), plaster (186), plumbago (116), potash, potato, quill toothpick, raisins, rice, rusty rock (200), rouge (200), sand, shot (228), slag (196), soap, scouring soap, steel (195), stove polish, tacks, (wax) taper, thread, tooth powder, turnip, vase¬ line, vinegar, yeast cake. List F — Emergency Supplies (see Int. § 11). 25 gm. absorbent cotton, 12 bandages (5 cm.), blanket, 50 gm. boric acid solution, 25 gm. camphor solution, 250 gm. carron oil, 12.5 gm. collodion, 1 book court plaster, fire extinguisher, 1 pkg. gauze (picric acid), medicine dropper, 1 paper pins, sand and scoop, scissors, 1 bottle smelling salts, 250 gm. sodium bicarbonate, 1 spool thread, 25 gm. vaseline. List G — Solutions. The solutions needed for most experi¬ ments are approximately 10 per cent. The concentration of special solutions is usually given in the directions for the experiments. Certain solutions should be made as follows: Acetic acid, dilute, 1 vol. to 5 vols. of water. Ammonium carbonate. Dissolve 250 gm. in 1000 cc. of water and add 85 cc. of ammonium hydroxide. Ammonium hydroxide, 1 vol. to 3 vols. of water. Ammonium molybdate. Dissolve 15 gm. in 100 cc. of water and pour this solution into 100 cc. of nitric acid (1 vol. acid to 1 vol. water). Ammonium oxalate, 5 per cent. Ammonium sulphide, 1 vol. to 1 vol. of water. Barium chloride, 5 per cent. Use distilled water or water free from sul¬ phates. Barium hydroxide, 1 per cent. Use clear solution. Battery solution (Grenet). Dissolve 103 gm. of powdered potassium di¬ chromate in 1000 cc. of water and slowly add 103 gm. of concentrated sulphuric acid with constant stirring. (A storage battery or reduced street current is preferable.) Calcium hydroxide. See Lime water. Chlorine water. Saturate water with the gas. Cobaltous nitrate, 5 per cent. Cochineal. Grind a little cochineal with water, dilute as desired, and filter. Developer (photographic). Dissolve 11.5 gm. of hydroquinone, 38 gm. of sodium sulphite, 75 gm. of sodium carbonate, and 2 gm. of potassium bromide in 1000 cc. of water. 164 APPENDIX Fehling’s solution. Dissolve 17.3 gm. of copper sulphate (cryst.) in 150 cc. of water. Dissolve 173 gm. of sodium citrate and 100 gm. of sodium carbonate (anhydrous) in 850 cc. of water. Pour the first solution into the second slowly with constant stirring. The final, clear solution will keep well. Ferric chloride, 5 per cent. Ferrous sulphate, 5 per cent. Must be freshly prepared. Keep a few pieces of iron in the solution. Hydrochloric acid, dilute, 1 vol. to 5 vols. of water. Lead salts. Use distilled water or filter. Limewater. Slake lime, add considerable water, shake occasionally, and siphon off the clear liquid. Litmus. As under Cochineal. Mercuric chloride, 5 per cent. POISON ! Mercurous nitrate, 5 per cent. Add a little mercury. Molisch’s solution. Dissolve 10 gm. of alpha-naphthol in 100 cc. of ethyl alcohol (95 per cent). Nitric acid, dilute, 1 vol. to 5 vols. of water. Phenol-phthalein. Dissolve 1 gm. in 100 cc. of alcohol and dilute slightly with water. Potassium permanganate, 5 per cent. (Add sufficient water to obtain “very dilute” solution.) Potassium sulphocyanate, 5 per cent. Silver nitrate, 5 per cent. Use distilled water (or water free from chlorides). Silver sulphate, 0.5 per cent. See Silver nitrate. Sodium cobaltinitrite. Dissolve 10 gm. of sodium nitrite in 20 cc. of water; dissolve 6 cc. of acetic acid and 1 gm. of cobaltous nitrate in 15 cc. of water. Mix these solutions and filter. Stannous chloride. Reduce concentrated hydrochloric acid with tin, dilute with water, and keep tin in this solution. Sulphuric acid, dilute, 1 vol. to 5 vols. of water. Pour the acid slowly into the water, stirring constantly. INDEX (Numbers indicate pages ) Accidents, 12; supplies, 163. Acid carbonate, 104. Acids, 67-71; acetic, 118; carbonic, 104; composition, 68; halogen, 131; hydrochloric, 64-66; nitric, 75-78; orthophosphoric, 131; sulphuric, 100-101; sulphurous, 42 ; test, 67. Air, 57-60; carbon dioxide in, 59; combustion, 22; heating metal in, 20; oxygen in, 57; testing, 60; water vapor in, 59. Alcohol, ethyl, 117-118. Alizarin, 147. Alloys, copper, 148; fusible, 132. Alum, 146; in baking powder, 125. Aluminium, 144-147; equivalent weight, 85; hydroxide, 1447 in cement, 140; mordants, 146; salts, test, 125; test, 145. Ammonia, 72-75. Ammonium carbonate, 75; chloride, 74; hydroxide, 72; nitrate, 75, 79; salts, 74, 125. Anhydrous compounds, 48. Antimony, test, 132. Apparatus, lists, 158-160; common, Frontispiece. Aqua regia, 66. Arsenic, test, 132. Babcock test, 122. Baking powder, 124. Balance, 9-11. Barium, 141, 142. Bases, 67-71; composition, 68; test, 68. Bismuth, test, 132. Bleaching, 63, 99; powder, 63. Blowpipe, use, 115. Boiling point, water, 40; elevation, 91; solutions, 91. Bone ash, 131. Borax, 135; beads, 135, 136. Bread, 121. Bromides, 129. Bromine, 128. Bunsen burner, 2, 113; flame, 113. Burettes, 70. Butter, 121. Calcium, carbonate, 137; equiva¬ lent weight, 85 ; hydroxide, 138; oxide, 138; salts, test, 125; sul¬ phate, 140, 141; test, 137. Candle flame, 13, 112. Carbon, 23 ; 102-103 ; distribution, 23; fixed, 108; monoxide, 105; test, 103; tetrachloride, 120. Carbon dioxide, 23-28; and bev¬ erages, 26 ; and combustion, 23 ; and fermentation, 24; and fire extinguishers, 2 7; and plants, 27; in air, 59; weight of liter, 80-82. Carbohydrate, 120. Carbonates, 104; testing, 104. Carbonic acid, 104. Carborundum, 127. Cement, 139; analysis, 139. Charcoal, 102. Chemical change, 12, 13; and prop¬ erties, 13. Chemicals, list, 160-162. Chlorides, 66; insoluble, 66. Chlorine, 60-63 5 and gold, 63; bleaching, 61, 63; by electrolysis, 62 ; water, 38, 50, 63. Chromium, test, 141, 155. Coal, analysis, 107; gas, hi. Cobalt, test, 135. College preparatory experiments. See Contents. Color of ions, 92. Combustion and air, 22; and carbon dioxide, 23. 166 INDEX Compound and elements, 16; and mixture, 14. Concentration and ionization, 93. Copper, 14, 147-148; ion, 92; oxi¬ dation, 19; oxide, reduction, 33, 103; oxide, 33; sulphate, 147; sulphate, electrolysis, 89-90; test, 136, 147. Cork boring, 6. Crystallization, 46-49. Deliquescence, 49. Demonstration experiments. See Contents. Dextrose, 116. Displacement of metals, 148, 151, I5 2 , 1 54- Distillation, water, 38. Dyeing, 146-147. Efflorescence, 48, 49. Elements and compound, 16. Electrolysis, chlorine by, 62 ; copper sulphate, 89-90; potassium io¬ dide, 91; sodium chloride, 62 ; sodium sulphate, 90; water, 51. Electrolytes, 87. Emergency supplies, 163. Equipment, laboratory, 158-160. Equivalent weight, aluminium, 85; calcium, 85; magnesium, 84; zinc, 82, 85, 87. Etching, 127. Ethyl acetate, 119. Fat, in milk, 122-124; test, 120.. Fermentation and carbon dioxide, 24. Ferric compounds, 143. Ferrous compounds, 143. Fertilizer, phosphate, 131. Filtering, 5. Fire extinguishers, 27. Flame, blowpipe, 115; Bunsen, 2-3, 113; candle, 13, 112; gas, 112. Flashing point, kerosene, no. Food, 120-125. Freezing point, water, 40; depres¬ sion, 92; solutions, 92. Fuels, 106. Fusible alloys, 132. Gas, coal, m; flame, 112; illu¬ minating, in. Gases, collecting, 8. Gasolene, 109; and water, 43. Glass, bending, 4; cutting, 3; drawing, 5; etching, 127. Gold, 155; and aqua regia, 66; and chlorine, 63; test, 155. Graphite, 102. Green fire, 142. Halogen acids, 131. Hardness of water, 140. Hydrochloric acid, 64-66. Hydrogen, 29-34; burning, 31; by electrolysis, 51; chloride, 64-66; fluoride, 127; from water, 31, 51; peroxide, 52; reduction by, 33; sulphide, 95-97. Hydrolysis, aluminium compounds, 147; ferric chloride, 144; sodium carbonate, 133. Hydrometer, using, 45, 101. Illuminating gas, m; flame, 112. Ink, bleaching, 64. Iodides, 130. Iodine, 129, 130; and starch, 117; test, 130. Iodoform, 118. Ionization, 87-93; and concentra¬ tion, 93. Ions, 87-93; colored, 92 ; colorless, 92. Iron, 142-144; and sulphur, 14; in cement, 140; oxidation, 22; sulphide, 14-16; tests, 142, 143. Kerosene, no; flashing point, no. Law, constant composition, 52; multiple proportions, 54. Lead, 151, 152; separation, 153; test, 152; white, 152. LeBlanc process, 133. Magnesium, 14, 148-149; and oxy¬ gen, 52; equivalent weight, 84; test, 149. Manganese, sulphide, 157; test, 136, 156. Manipulation, 2-11. Meniscus, 70. Mercuric compounds, 150. INDEX 167 Mercurous compounds, 150. Mercury, 150; oxide, 16; separa¬ tion, 153; test, 150. Metal and air, 20. Milk, 12 2-124. Mineral matter, food, 121; milk, 124. Mixture, 14. Mortar, 139. Neutralization, 69-71. Nitrates, 77; test, 78. Nitric acid, 75-78; test, 78. Nitric oxide, 78. Nitrogen, 56; dioxide, 78; test, 57. Nitrous oxide, 79. Non-electrolytes, 87. Normal carbonate, 104. Orthophosphate, 131. Orthophosphoric acid, 131. Oxidation, 21; blowpipe, 116; chromium compounds, 156; cop¬ per, 19; iron compounds, 143 ; metals, 22. Oxygen, 16-22 ; in air, 57 ; in potas¬ sium chlorate, 54; in potassium perchlorate, 55 ; in water, 50, 51; preparation, 16, 17; properties, 17, 18, 19; weight of liter, 34. Phosphates, 125; fertilizer, 131; test, 131. Photography, 154. Plaster of Paris, 141. Potassium, 42, 136; chlorate, com¬ position, 54; chromate, 156; dichromate, 156; iodide, elec¬ trolysis, 91; nitrate, 136; perchlo¬ rate, composition, 55; test, 42, i 36 ; Protein, 120-121; in milk, 122. Qualitative analysis, 66, 153. Quantitative experiments. See Contents. Red fire, 142. Reduction, blowpipe, 115; by alu¬ minium, 145; by carbon, 103; by hydrogen, 33; copper oxide, 33; iron compounds, 143; mercuric compounds, 150. Safety lamp, 110. Salts, 68-72; chemical behavior, 88; composition, 68; ions, 88; preparation, 72. Scales, 9-11. Silica, in cement, 140. Silicates, 125, 126. Silicic acid, 126. Silicon, dioxide, 125; test, 126. Silver, cleaning, 154; halides, 154; photography, 154; separation, 153; test, 153. Slag, 142. Soap, 119; and hard water, 140. Sodium, 132-135; and water, 31, 41; bicarbonate, 133, 134; car¬ bonate, 133; chloride, 133; hy¬ droxide, 134; hypochlorite, 64; silicate, 125, 126; sulphate, elec¬ trolysis, 90; test, 42, 132. Solubility, 43-45; chlorides, 66; gases, 43; liquids, 43; solids, 43-45- Solutions, 163; boiling point, 91; conducting, 87-88; Fehling’s, 164; freezing point, 92; list, 163; making, 163; Molisch’s, 164; saturated, 45; special, 163; su¬ persaturated, 50. Stannous chloride, 150, 151. Starch, 117. Steam, 41. Strontium, 141, 142. Sucrose, 116. Sugar, 116. Sulphate, test, 101. Sulphides, 97-98, 157. Sulphur, 13, 93-101; amorphous, 95; and iron, 14; dioxide, 98-100; monoclinic, 95; orthorhombic, 94; plastic, 95. Sulphuric acid, 100-101. Sulphurous acid, 42, 99, 100. Supersaturated solution, 50. Supplies, 158-164; emergency, 163. Tartrates, 124. Test, acetic acid, 118; acids, 67; alloys, 148; aluminium, 145; aluminium salts, 125; ammo¬ nium salts, 125; Babcock, 122- 124; barium, 141; bases, 68; INDEX 168 bismuth, 132; borax beads, 135 ; bromide, 129; calcium, 40, 137; calcium salts, 125; carbohy¬ drates, 120; carbonate, 124; carbon dioxide, 13, 23; cement, 139; chloride, 40, 66, 67; chro¬ mium, 141, 155; copper, 136, 147; dextrose, 116-117; ethyl alcohol, 118; fat, 120; gold, i 55; hydrochloric acid, 66; hy¬ drogen, 30; hydrogen chloride, 66; hydroxides, 41-42; impure water, 39, 40; iodide, 130; iodine, 130; iron, 143; lead, 66, 152; lime compounds, 40; manganese, 136, 156; mercury, 150; mercury (ous), 66, 150; nitrates, 78; nitric acid, 78; oxygen, 19; phosphate, 125; potassium, 42, 136; protein, 120-121; silicon, 126; silver, 66, 153; sodium, 42, 132 ; sodium hydroxide, 42 ; starch, 117; strontium, 141; sugar, 116; sulphate, 40, 101; sulphuric acid, 101; sulphurous acid, 42, 100; tartrates, 124; tin, 151; zinc, 116, 149. Testing, acids, 69; baking powder, 124; bases, 69; bread, 121; but¬ ter, 121; calcium compounds, 138; carbon, 103; carbonates, 104, 124; food, 120-125; illu¬ minating gas, hi; iron com¬ pounds, 144; magnesium com¬ pounds, 149; metals, 116; min¬ eral matter, 121; salts, 75; silicon compounds, 126; water in food, 121. Test wire, 6. Thermit, 145. Titration, 70. Vapor pressure, 41, 158. Vinegar, 119. Water, 37-51; and sodium, 31, 41; boiling point, 40; calcium compounds, 40, 140; chemical properties, 41; chlorides, 40; chlorine, 38, 50, 63; composition, 50, 51; distillation, 38; elec¬ trolysis, 51; freezing point, 40; hardness, 140; in food, 37, 121; in milk, 122; lime compounds, 40; of crystallization, 47, 48; organic matter, 39; purification, 37-38; physical properties, 40; vapor pressure, 41, 158; solu¬ tion, 43-45; sulphates, 40; tests, 39; vapor, 41; vapor in air, 59. Weighing, 9-11. Weight of liter, oxygen, 34; carbon dioxide, 80-82. White lead, 152. Zinc, 148, 149 ; and air, 20; equiv¬ alent weight, 82, 85, 87; hy¬ droxide, 149; test, 149.