UC BERKELEY MASTER NEGATIVE STORAGE NUMBER 03-67.66 (National version of master negative storage number: CU SNO03067.66) MICROFILMED 2003 UNIVERSITY OF CALIFORNIA AT BERKELEY LIBRARY PHOTOGRAPHIC SERVICE REPRODUCTION AVAILABLE THROUGH INTERLIBRARY LOAN OFFICE MAIN LIBRARY UNIVERSITY OF CALIFORNIA BERKELEY, CA 94720-6000 COPYRIGHT The copyright law of the United States (Title 17, United States Code) governs the making of photocopies or other reproductions of copyrighted materials including foreign works under certain conditions. In addition, the United States extends protection to foreign works by means of various international conventions, bilateral agreements, and proclamations. Under certain conditions specified in the law, libraries and archives are authorized to furnish a photocopy or other reproduction. One of these specified conditions is that the photocopy or reproduction is not to be "used for any purpose other than private study, scholarship, or research." If a user makes a request for, or later uses, a photocopy or reproduction for purposes in excess of "fair use," that user may be liable for copyright infringement. University of California at Berkeley reserves the right to refuse to accept a copying order if, in its judgment, fulfillment of the order would involve violation of copyright law. Wright, J. Buford The chemical composition of various silicates formed by the metamorphism of imeston at Crestmore, Riverside Co. California 1913 BIBLIOGRAPHIC RECORD TARGET University of California at Berkeley Library Master negative storage number: 03-67.66 (national version of the master negative storage number: CU SN03067.66) GLADIS NUMBER: 184788698J AD:991013/FZB LEVEL:b BLT:am DCF:a CSC:d MOD: EL:7 UD:030604 /MAP CP:cau L:eng INT: GPC: BIO: FIC: CON: ARCV: PC:s PD:1913/ REP: CPI: FSI: ILC: II:0 CUScCU SbDISS.WRIGHT.GEOL 1913 Wright, Budford J. The chemical composition of various silicates formed by the metamorphism of limeston at Crestmore, Riverside Co. California. Scl913. 18 p. ;$c29 cm. Thesis (B.S. in Mining) -- University of California , Berkeley, Dec. 1913... 20 University of California, Berkeley.S$bDept. of Mining Engineering$xDissertations. 0 Dissertations, Academic$xUCB$xMining Engineering$y1913. Microfilmed by University of California Library Photographic Service, Berkeley, CA FILMED AND PROCESSED BY LIBRARY PHOTOGRAPHIC SERVICE, UNIVERSITY OF CALIFORNIA, BERKELEY, 94720 DATE: 07/03 REDUCTION: 10 X ~ PM-13%"x4” PHOTOGRAPHIC MICROCOPY TARGET NBS 1010a ANSI/ISO #2 EQUIVALENT I ll 2.8 25 10 Bh x 54 3.2 ll : = ww PP ® = as IZ ie pe pg TI pgp vor lo 1] le "2 le ' 3 le "4 le '5 le 6 “- cr, ol &1 &[1 gt 11,0 bv le [m [gee " SIL SIL LOE al bund hod oll El hi hE EE II RY R’ Eh ut SELECTION AND PREPARATION OF SAUPLE METHODS OF ANALYSHS ‘The samples of vesuvianite and garnet were selected from crystal portions,which existed in rather large sizes DETERMINATION OF COMBINED WATER and could be separated without difficulty from the adhering Penfieldl!s Method: calcite. From two to three-tenths of a gram Sufficent quantity of these minerals was: taken to of rock powder was ignited in a thoroughly dried tube allow in each case sufficent sample for duplicate analyses: of hard glass,closed at one end: the heated end contain- using separate portions for combined water,main analysis, ing the powder was pulled off,leaving the balance of the ferrous iron determination and alkali determination.Half tube closed,and containing the expelled water. This was gram samples were used in each of the determinations,with weighed, thoroughly dried,and weighed again. The difference the exception of the combined water.Two to three-tenths being the combined water. ni CoE of a gram were used here. Where a large quantity of combined water was suspecti- As these minerals require fusion to render them ed,as in the brucite-calcite analysis an enlargement soluble, they were ground to the finest powder: Theselec ted was made in the middle of the tube. portions were broken to a size convenient for the mortar The powder was introduced into the tube by means on a steel plate.These were then ground by hand in an agate of a small thistle-tube;care being taken to prevent the mortar to a powder containing no grit. 1 soiling of the upper portions of the tube. 1 The powdered minerals were kept in labeled and 1 All water was expelled in about fifteen minutes, corked test tubes. using a nearly full Bunsen flame. The brucite=-calcite mixture and the howlite. being At least three to four operations were carried out before an approximate check was arrived at. soluble in HCL did not require such fine grinding. A sample of brucite-calcite mixture was first analyzed. A sample of calcite was then carefully separated 4 from the dark brucite and its composition determined. i (2) 4 2 The howlite occured in white masses and its selection was made with certainty. DETERMINATION QF SILICA A half gram portion of tne rock powder was weighed in a watch-glass and thorougnly mixed with a flux,consist- ing of a one to one mixture of sodium carbonate and acid potassium carbonate, in a platinum crucible. The ratio of flux to rock powder was about one to five. The covered crucible was gently heated,allowing the carbon dioxide to pass off without spattering, and was finally brought to complete fusion at a bright red heat.This was continued until a state of quiet fusion was reached. The crucible was allowed to thorough- ly cool. It was then placed in a beaker, covered with water and gently heated until the cake was thomroughly loosened.The crucible was removed and ten to fifteen cubic centimeters of con.HCL were added. When effervescence had ceased the liquid was transe fered to a platinum dish and evaporated to dryness,on the water bath,untill no more fumes of Hcl were given off.The contents were then moistened with a little con. HCl and taken up with water. The ingluble silica was filtered off on a 9 cm. ashless filter paper and washed with cold water. (3) The filtrate was again evaporated to dryness, taken up as before and filtered through the same filter paver. Washing of the precitate was carried out until a few drops from the end of the funnel gave no chlorine react- ion with silver nitrate. The free edges of the filter were folded down up- on the silica, sdas to completely enclose it. It was then removed from the funnel and placed in a weighed platinum crucible. The precipitate was dried over a low flame; the filter carbonized and finally incinerated over the full Bunsen flame.When the carbon was nearly consumed a blast was substituted for the Bunsen burner and the crucible blasted for twenty minutes. The crucible was then cooled in the desiccator and weighed. The result noted as crucible+silica+x. The weighed silica was then moistened with water and volatilized with nydrofluoric acid,by heating under a hood. The heating was continued untill the crucible was completely dry. The crucible was then ignited at red heat, cooled and weighed,and its weight noted as=- crucible+x,below that of crucible+silicat+x. The differ- ence between the two gave the weight of silica.This crucible was saved for the ignition of the precipitate of aluminia and iron oxides. (4) . DETERMINATION OF ALUMINIA AND IRON To the filtrate from the silica,which amounted to about a hundred cubic centimeters, c.c.s of con. HCl were added. The liquid was heated 2lmost to boiling and ammonium hydroxide added until it smelled rather strongly of it. The beaker was then heated to boiling for about a minute. The: bulky, gelatious precipitate was allowed to settle and was then filtered through a 9 cm. filter; the filtrate being caught in a 800 cc beaker. After being washed free from chlorides the pre- cipitate was loosened, folded as before and ignited in the crucible from the silica determination, at a bright red heat. After cooling in the desiccator the crucible was weighed and the difference between this and the empty crucible, obtained prior to the ignition of the silica, is that of aluminia and total iron as ferric oxide, The aluminia was determined by a difference. The ferric oxide was determined as follows: The ignited precipitates of aluminia and ferric oxide were fused with about 2-3 gms of coarsly powdered acid potassium sulphate. When cool the crucible was placed in a beaker,covered with water and about 10 cc con. sulphuric acid,and heated until complete solution of the cake. (8) The iron was then completely reduced to the ferrous condition by boiling with metallic zinc. The absgence of ferric iron being determined by testing a few drops of the solution with KSCN. The solution was then titrated with standard potassium permangate untill tinged aper- manent red. The number of cubic centimeters of permanganate solut- ion used was multiplied by the amount of ferric oxide equivalent to 1 cc of the standard; the product giving the total iron in the rock as ferric oxide. From this was deducted the iron as ferrous oxide. This weight of ferric oxide found subtracted from the combined precipitate of aluminia and ferric iron gave the weight of aluminia present. ~ DETERMINATION OF MANGANESE AND COPPER To the filtrate from the iron and aluminia precipit= ate, in a 200 ce flask, enough’ ammonium nydroxiddwas | added to make the contents strongly alkaline and a current of hydrogen sulphide passed through it for fifteen minutes, The flask was corked and allowed to stand for 24 hours. The precipitated sulphides were collected on a 7 cm. filter and washed with water containing a little ammonium chloride and ammonium sulphide. The filtrate was received in a 400 cc beaker and reserved for the determination of lime and magnesia. The sulphide of manganese was dissolved by passing Sel. i a few cubic centimeters be sulphide, acified 6 {4 5 - it ol tan af 3 i § Prt 4 with one-fifth of its bulk of HCl through the filter and washing several times.The liquid was received in a small porcelain dish and evaporated to dryness.A few cC. of sodium carbonate were added and the contents again evaporated to dryness to destroy ammonium salts. The dried salts were then dissolved in about 1l0cc of water to which a few drops of Hel were added, and precipitated with sodium carbonate. The manganese carbon=- ate was collected on a five and one-half cm. filter, washed, ignited in a weighed porcelain crucible and re- ported as 1linz04. The filter was incinerated in a porcelain crucible, dissolved in afew drops of aqua-regia,evaporated to dryness in the crucible,dissolved in a little water and HCl and H,8 water addedwhich precipitated the copper. This was filtered,washed and weighed as CuQ. The precipitates of copper and manganese were al- ways tested with the borax bead to prove their identity. It was noticed that a small amount of silica was present with the manganese and copper sulphides.This was due to the attack of the strong ammonium hydroxide solution on the flask,as was shown by the frosted appearance of the sides of the flask.This silica was filtered off before the final precipitation of the copper sulphide and was found in one case,after ignitingto weigh .0025 £8 (7) DETERMINATION OF LIME The filtrate from the manganese determination was acdtied with HCl and warmed to destroy the ammonium sulph- ide. The precipited sulphur was filtered off. To this filtrate which amounted to about 400 cc ammonia was added. until the liquid smelled slightly of it,and the liquid brought to a boil. To this was added about one gm. of am=- mon ium oxalate,dissolved in about 25 cc of water. Boiling was continued for a few minutes and the beaker allowed to stand untill the finely divided precipitate of calcium oxalate was settled, It was then filtered through a 9 cm. filter, the precipitate being thoroughly washed with warm water, The precipitate was placed ,moist,in a weighed and covered platinum crucible, incinerated and finally blast=- ed for fifteen minutes to constant weight. DETERMINATION OF MAGNESIA To the filtrate from the lime about 3 gms. of hydrogen=- ammonium-sodium phosphate,dissolved in a little water were added.This solution was made strongly alkaline with ammonia,well stirred with a glass rod and covered and set aside for 24 hours, The precipitate was then filtered through a 9 cm. filter,washed two or three times with water containing some ammonia, incinerated in a weighed platinum crucible, with the full flame of the Bunsen and weighed as ligoP20 ye (8) DETERMINATION OF FERROUS IRON A half gm. portion was weighed into a platinum crucible containing a close fitting cover. It was moistened with a little water and a few coils of platinum wire dropped in, to prevent bumping. In another crucible a mixture was made which consisted of 10 cc HF1l and 10 cc of sulphuric acid diluted with its own volume of water. This was poured over the rock powder which was immediately covered, placed under a hood and gently heated for five to seven minutes, until complete decomposition had occurred. The covered crucible is then placed in a beaker contain- ing about 400 cc of water and the contents immediately titrated with standard permanganate solution. DETERMINATION OF SODIUM A half gm. portion of the rock powder was thoroughly mixed with its own weight of ammonium chloride and about eight times its weight of calcium carbonate, in a platinum crucible. The crucible was covered and heated over & low flame for about ten minutes,until: no more vapors of ammonia or smmonium chloride were given off.The heating was then continued over the nearly full Bunsen flame for three- quarters of an hour,when the crucible was removed and allowed to cool. When cold the cake was transfered to a porcelain dish, covered with water and warmed until. it disintegrated into a powdery mass.lt vas then filtered and washed with warm water. To the filtrate a little ammonia water was added and the liquid brought to a boil. About two gms. of ammonium carbonate, previously dissolved in 50 cc water were then added and boiling continued for a minute or so. The bulky precipitate of calcium was allowed to settle and then was filtered through a 9 cm. filter into a porcelain basin. The basin wae placed on the water bath and evaporat- ed to dryness. It was then gently heated until. all ammonium chloride was driven off. After cooling a little water was added and a few drops of ammonium carbonate; the basin was again evaporated to dryness. Two or three cc of water were poured in to dissolve the salts and the liquid filtered through a 7 cm, filter into a previously ignited and weigh=- od plating dish: A-drop of Hcl was added to decompose any alkali carbonates present and the contents evaporated to dryness. When dry, the dish was gently heated to drive off the ammonium chloride and the contents weighed as- crucible+ NaCl. Agthe amount of NaCl was so small in each case, potas- ium was not determined. DETERMINATION OF BORIC ACID In the mineral determinations, containing borates, the boric acid was eliminated before the filtering of the gilica,by the continued eveporation of the solution of powder with methyl alcohol. Three evaporations removed the boric acid completely. acid The boric,was determined by titration with standard NaOH solution,as follows, A nalf gm. portion was dissolved in HCl,a few drops of methyl orange added and NaOH stirred in until. a lemon yellow was reached.Afew drops of barium chloride and phenolphthalein were added and about one gm. of mannite. This wee then titrated to neutrality with standard NaOH. Using thymolphthalein in place of the phenolphthalein equally sharp end points were reached. The change hexe from lemon yellow to blue being more attractive than the change from lemon yellow to pink. In decomposing the borate samples, tried not to heat them over 80°C.as I found a loss in BgOs occurred if this wag done. (11) 8102 Al203 Fey0z FeO MnQ Cul Cal lig0 Nao0 Ho0 Gravity 5102 Alo03 Feo03 FeQ CuO Cal MgO Nao0 Ho0 Gravity RESULTS OF ANALYSES VESUVIANITE #1 A 36.80 17.58 3410 45 1.23 1432 33,18 4.77 32 .68 3.37 VESUVIANITE #2 33440 22.70 2.86 42 «32 35.20 5099 «40 «55 Se 31 (12) B 36.96 17.64 3.12 .48 1,78 .80 33.36 4.69 37 .55 3.35 33.68 | 22.96 2.84 +40 «60 35448 392 «34 «63 Total Total 100,32 «61 99.57 3436 «41 +46 35.34 3493 037 59 8109 Al203 Fes03 FeO CuO Cal Nao0 Ho0 Gravity GARNET (Grossularite) A 35.56 21.04 3.92 «61 «60 36.04 «78 «19 1.28 3.40 B 35.48 21.18 3499 «959 » 80 36.08 079 «21 1.19 3.38 Total MEAN 35.52 21.11 390 «60 «70 36.06 «78 «20 1.23 100.15 de 39 Cal Ig.Loss 8i0o Alo03 Fes03 Cal MgO Ig.Lloss Computations: from above analyses,assuming BRUCITE to BRUCITE=CALCITE A 45.34 9.57 43456 . 69 58 062 CALCITE 85.29 2.01 44.66 45.32 9.22 43461 «68 +06 «54 83.36 1.99 44.56 MEAN 45,33 9.38 43,58 +68 «57 Total 100.17 Total be a constituent of the mineral with CALCITE: CALCITE: 53.32 2.00 —448.01 99,93 53.32 x 100 =95,1% CaC03,containing 41.68% COg 56 —X 100 = 4.2% MgCOz, 47.6 a 44.61=-4388 =.73% hydroscopic water in calcite BRUCITE~CALCITE; 45,33 81.00% CaC0z in mixture FF fe 5 (continued on next page) (14) om —————) C SEor— X 41.68=35.50% COz in mixture as CaCO “ST: -. " " " " SEL X 202 = 1.70% MgCO3 soll X «73= 62% Ha0'" " 95.1 % 93 4.22% " for 9.38% MgO to form Mg(OH)2 42.04% lost as water and COp 43.58-42,04=1.54% Ho0 and CO, (which is probably taken up by the 8i02,Al50, and Feg0s3,) (15) HOWLITE Ry A Cal 28.68 510, 14.48 Bo03 45.59 50 11.16 ULEXITE G CaO 14.88 B20; 43.99 Na, 0 8.02 ito 28.88 14.56 45.26 11.02 Total io 15.04 44.41 28.178 14.52 45.42 11,909 99.81 MEAN 14.96 44.20 7.52 7 Total GARNET aod rf REMARKS In the analytical results,where a difference of more 8105 34.83 . 35a56 35.48 than three to four-tenths of one percent occurred between i Al 0, 21.64 21.04 21.18 any of the constituents of the duplicate samples;a repétit- | CaO 37.24 36.04 36.08 ion of that portion of the analysis containing the discrepancy HOWLITE was preformed. The two results agreeing most closely were B03 (1)35.28 1.30.78 chosen to represent the amount of that constituent in the | | (2)45.59 45.26 | Ho0 12.23 11402 11,16 mineral. The results of the various repdtitions are noted | Great variation here due to over heating sample during - decomposition in (1),resulting in volatilization of the Bg0, below. : | In sample (A) of the analysis of vesuvianite #2,in the | fi ULEXITE determination for manganese a precipitate Weighing .0018 gms. 1 Na,0 Be lB 8,02 Bs cccurred. This was tested and found to be iron, which had not heen thrown down in the previous precipitation. This was calculated as ferric oxide and added to the amount of ferric oxide determined by the permanganate titration. REPETITIONS (under-lined results were those chosen in the fore- going analyses) VESUVIANITE #1 810, 36.16 36.80 364986 A120, 18.13 17.58 17.64 Cao 32.08 33.18 33436 | MgO 5e52 4.77 4.69 | 20 .96 +68 «55 | : ¥ (18) (17) END OF TITLE