m .ASSIFIED UNCLASSIFIED Y-824 Subject Category: CHEMISTRY UNITED STATES ATOMIC ENERGY COMMISSION SUPPLEMENTARY INFORMATION ON PRODUCTION OF ZR AT Y-12 By J. W. Ramsey W. K. Whitson, Jr. JNIV. OF FL LIB. DOCUMENTS DEPT. DEPOSITORY November 15, 1951 Y-12 Plant Carbide and Carbon Chemicals Company Oak Ridge, Tennessee Technical Information Service, Oak Ridge, Tennessee Date Declassified: November 18, 1955. This report was prepared as a scientific account of Govern- ment-sponsored work and is made available without review or examination by the Government. Neither the United States, nor the Commission, nor any person acting on behalf of the Commis- sion makes any warranty or representation, express or implied, with respect to the accuracy, completeness, or usefulness of the information contained in this report, or that the use of any infor- mation, apparatus, method, or process disclosed in this report may not infringe privately owned rights. The Commission assumes no liability with respect to the use of, or for damages resulting with respect to the use of any information, apparatus, method, or proc- ess disclosed in this report. This report has available copy. been reproduced directly from the best Issuance of this document does not constitute authority for declassification of classified material of the same or similar content and title by the same authors. Printed in USA, Price 25 cents. Available from the Office of Technical Services, Department of Commerce, Wash- ington 25, D. C. Y-82U CARBIDE AND CARBON CHEMICALS COMPANY A DIVISION OF UNION CARBIDE AND CARBON CORPORATION' Y-12 PLANT W-7l+05-eng-26 CHEMICAL DIVISION Mr. J. M. Herndon, Superintendent CHEMICAL DEPARTMENT Mr. G- A. Strasser, Superintendent SUPPLEMENTARY INFORMATION ON PRODUCTION OF ZR AT Y-12 J. W. Ramsey W. K. Whitson, Jr. ABSTRACT Information is given about production of zirconium at Y-12, supple- mentary to report Y-817. Oak Ridge, Tennessee November 15, 1951 Supplementary Information on Production of Zr at Y-12 A meeting was held at Y-12 October 17-18, 1951 of representatives of firms interested in obtaining information about zirconium production in order to b9 able to submit bids for zirconium work requested by the AEC. A report was compiled to present important facts about Y-12 zirconium operations, Y-817, Production of Zirconium at Y-12. Tours of the zirconium plant at Building 9211 were made by visitors and question-and-answer sessions were held. In these sessions several questions were asked about points of operation which it had not been possible to cover completely in prepared literature or lectures. It was stated that these questions would be answered in a supplementary report to be distributed later. This report covers that information. The following sections are includedj A. Usage and Unit Cost of Chemicals B. Purity Specifications C. Typical Purity Values of Y-12 Feed and Product Materials D. Operating Personnel Assignments E. Power Requirements F. Construction Costs G. Pump List H. Plant Operating Procedures It should be noted that this ini'orraation is issued supplementary to report Y-817 and reference to that report should be made in studying the material presented here. 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I_ I- < < E-f <-* a] . u -h a CD ■H al a u oooaJoacio □ ■P tur earn eat ect g T) TJ T3 kHH B L> o K a 3 •hJ>>>>>»3 n O 2 CO HI ^ >, ^ -^ Bo SPECIFICATIONS FOR 2R- ABC LETTER, JUNE 14, 1951 Cross Zr Zr Crude Pre iduct Section Stri •P Spon S e ZrCl Zr0 2 ZrCl 4 % Product (min) 0.19 99. 8 99. 7 98 97 95 Hf ppm (max) 0.51 100 100 100 100 2% N 0.11 50 50 _-_ Al 120 120 30 30 400 Ti 0.11 80 80 100 100 500 B 60 • 1 O 1 .1 .1 .1 No chlorinated C 500 500 carbon compounds _„_ Le s s than 1% Less than 1000 1000 non-vo lat: Lies — ?- non-volatile Mg 20 500 =-> P • 5 5 200 200 300 ff 5 5 50 1000 100 CI 0.84 5 500 ___ ■BOW Ca 20 20 40 40 100 V 0.08 50 50 50 50 50 Cr 0.05 100 100 100 100 100 lb 0.21 50 50 10 10 10 Fe 0.04 700 700 150 150 1000 Co 0.54 10 10 15 15 15 Ni 0.07 100 70 300 300 500 Zn 0.01 10 100 — ___ Mo 0.02 200 — _-= Cd 24.4 • 3 • 3 .3 .3 .3 W 0.09 50 — — Cross Sec tion max, , barns • 21 Hardness (10 nun ball, max 150 3000 1 Cg), min 80 1. Barns/atom Zr/% impurity; based on information in NY0-108 except Zr Cross Section of 0.19 barns is used. 2. For direct melting into ductile, corrosion resistant ingots. C. Typical Purity Values of Y-12 Feed & Product Materials Typical Analysis of Element 2rCl4 Feed From TAM Ag <1 Al 170 B 0.8 Ba 6 Be 0.08 Ca 80 Cd 0.8 Co <1 Cr 20 Cu 16 Fe 900 K 20 U < 0.4 Mg 15 Mn 4 Mo <10 Na 20 Ni 5 P 150 Pb 4 Si 150 Sn < 2 Ti 500 W <: 2 Zn <40 Hf 22000 Typical Analysis of Zr02 Product Materials From Y-12 ** -CI 12 0.6 2 £0.02 20 0.3 1 3 30 90 15 < 0.2 6 2 <10 20 100 125 4 90 < 2 < 100 £ 100 125 Average of Fifteen (15) Separate Batches, June, 1951 ** Average of Twenty (20) Composites, April to August, 1950 8 D. Operating Personnel Assignments The zirconium plant has been operated as outlined below. Insufficient operating experience is available to clearly define the manpower requirements for the permanent plant, which are expected to be less. No. Shifts No. Men/Shift Total Men Foremen 3 1 3 Assistant Foremen 3 1 3 Extraction 3 2 6 Purification 3 2 6 Feed Makeup & Hf Processing 2 2 li Burning 3 2 6 Total — W E. Power Requirements Except for gas heating, all power for the permanent zirconium plant is electrical o Electrical costs for this project are obtained from allocations of plant electrical costs made by the engineering department. These estimates show power consumption by the permanent zirconium plant to be approximately 25,000 KHH per month - Based on five day per week operation, there are 520 operating hours per month. Thus the average power load is calculated to be I4.8 kilowatts. An estimated breakdown of power consumption is given as follows: Jtercent of Average Total Power KWE/lfonth Load Kilowatts Lights 10 2,500 U-8 Pumps 50 12,500 2U„0 Drives 4 Agitators 20 5,000 9.6 Venilators & Fans 20 5,000 9.6 Total 25,000 kB.Q 10 F- Construction Costs The following table gives a breakdown of construction costs of the permanent zirconium plant « Data are taken from accumulation of actual costs from labor and material accounting in plant construction,, The permanent zirconium plant was constructed in the existing building 9211 and a number of tanks and pumps were available for re-activation* The amount of this item is listed under "Existing Equipment*,, Cost of the building is not included, "New Equipment" includes that equipment purchased specifically for construction of the permanent plant. "Labor" includes cost of labor directly applicable to construction of the permanent plant,, System Chem Supply and Storage Feed Makeup and Storage Extraction System Ammonium Thiocyanate Recovery Purification (Precip. & Filt.) Drying and Calcining Hafnium Purification Chlorination Waste Neutralization Grand Totals New Exist. Equip- & Total Equip* Mtlso Equipo Labor Tctal §13,200 $8,000 $21,200 $7,000 $2lJ7200 24,900 25,000 14,800 78,126 4,200 12,000 31,700 16,000 700 78,000 6,600 8,000 24,100 27,833 2,100 5,000 49,900 25,000 74,900 92,926 62,500 155,426 16,200 4,000 20^,200 47,700 26,000 73,700 78,700 30,000 108,700 14,600 6,000 20,600 51,933 50,482 102,415 7,100 2,019 9,119 $122,300 $257,959 $380,259 $213,001 $593,260 Cost of Labor Plus New Equipment Total Value of Equipment and Installation $470,960 $593,260 11 ID O •H > u w in a> u -p o => o • -rH: ° t£ o o ■H -P Q Q o o a rt M i— i , Ol o o O o o o a a o ^ u •H •H u V, 3 p o H to 1— 1 c> u p 0) ° M 0) Cd fl ** o => o tH ^ Cl O •H a< o Jh VL& a -P u a o c ■p t, -p ra Kt o H Vl pq >si O Ph « .-I ■P X as W .— I -d •H O O «! 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O o N"\ ■H * vO o *»— " -P 0) | $ VhO •H 00 gallon or 800 gallon batch is needed. 2) Measure water into empty tank a) Either Tank 9 or Tank 12 b) Record batch number, time started, etc. on Daily Work Sheet 16 Z-l Feed Makeup - (Continued) 3) Adjust depth of ZrCli discharge hose into tank until it is about 2 inches under surface of water, tighten down wing nuts on packing gland to hold hose. h) Clamp down hinged section of tank port. 5) Turn steam and water on ejector. a) On platform just outside building 6) Start circulation pump to agitate solution in tank. Pump out of the top of the tank into the bottom through the heat exchanger. Be sure that the cooling water is on the heat exchanger. 7) Prepare drum of ZrCli for unloading. a) Set drum on scales and check gross weight b) Turn on exhaust fan c) Remove lid from drum d) Gas mask and elbow-length rubber gloves are required safety equipment for this job 8) Swing ZrCli unloading hose into drum and let the vacuum draw the ZrCl, powder into the tank. 9) When drum is empty, check tare weight and subtract from gross weight to get net weight of ZrCli in drum. Repeat 6 and 7 until 3/h of the needed ZrCL for the complete batch is in the tank. 10) Using the ammonium hydroxide measuring tank, add the full amount of ammonium to the batch. a) Record ammonium hydroxide added on Daily W^rk Sheet 11) Add remain de. of ZrCli up to full weight required for batch, a) Record ZrCL added on Daily Work Sheet 17 Z-l Feed Makeup - (Continued) 12) Using the same method as when adding ZrCl. , draw the required amount of ammonium thiocyanate into the tank. a) Record total weight ammonium thiocyanate added on Daily Work Sheet 13) When all chemicals are in the tank, check total gallons and if necessary, add water up to final gallons of formula. lU) When batch is completed, continue to agitate for 30 minutes. Then: a) Cut down steam on ejector, leave enough to provide slight vacuum. b) Open tank port 15) Take 100 ml sample of batch Z~2 Control of Extraction Plant Feed It is extremely important that each batch of extraction plant feed meet these specifications: Specific Gravity 1.28 to 1.30 Lbs. Zr Per Gal. 1.00 to 1.10 Molarity of HC1 .80 to 1.2 Molarity of CNS 2.U5 to 2.55 - or as specified l) After a feed batch is completed and sampled, the operator will take the sample to a titration table and: a) Check specific gravity and record on Work Sheet b) Titrate for molarity of HC1 and record. See "Method for Titrating in Feed Solution". c) Titrate for molarity of CNS and record. See "Method for Titrating Solutions for CNS". 18 Z-2 Control of Extraction Plant Feed (Continued) 2) Now re -sample the batch and another operator will run a check titration on the solution for HC1 and CNS. a) If the solution was well mixed and both sets of titrations are accurate, the answers should check with 0.0£ b) If the answers do not check, take a third sample of the batch and again titrate. This should establish which of the first answers is correct 3) If the final control measurements do not fall within the limit set up, the batch must be further adjusted. In this case, contact the shift foreman for directions} 1;) For best plant operation, it is desirable that each feed batch be completed and sampled far enough in advance of plant needs that the analytical answer in lbs/ gal. is reported. 5) It is the responsibility of each operator to see that all information con- cerning any part of an operation is properly and promptly recorded on Daily Work Sheet. At the end of the shift, the operator will check his work sheet to see that all items are complete for his shift, including time, signature, etc. All samples sent to the analytical laboratory must be recorded in the sample log book as well as on their respective work sheet. Z-3 Filtering of Extraction Plant Feed 1) No. 1 filter press (NE corner) is used for filtering feed solution. 2) When a batch is ready - set valves at tank and at press to circulate through filter back to makeup tanks. 19 Z-3 Filtering of Extraction Plant Feed (Continued) 3) Start pump (with by-pass open so as not to put too much pressure on press) and 1st solution from press return to feed makeup tank for a few minutes until it becomes clear. Then change valves to put the solution in Tank No. 3- (filtered feed salvage). h) Continue to filter entire batch or part batch, depending upon plant needs, a) Be sure and record time started filtering and by whom and time finished filtering and by whom Z-U Daily Inventory 1) At 7s00 AM each morning the operator coming on shift will take an inventory of solutions in all tanks in the tank pit and the extraction plant head tank on the third floor. 2) This inventory will be recorded in space provided on the Daily Work Sheet for feed and product collected. a) On the sheet for the day ending, record the inventory under Ending Inventory. Record the same information on the new sheet under Be- ginning Inventory. 20 2-5 Extraction plant Control 1. Concentration and rates of extraction solutions are checked every two to four hours at important control points in the extraction system. Values are obtained by sampling solutions and analyzing for components. Simple analyses are run on samples by plant operators and more complex analyses are run on samples submitted to the production analytical laboratory. 2. Control points and measurements are listed as follows; (A) Zirconium Product Stream (1) Zr Concentration - Lbs/gal. '2) Hafnium Concentration - PPM y) CNS Concentration - Molarity (B) Hafnium Product Stream (1) Concentration Hf Lbs/gal. Zr Concentration - PPM CNS Concentration - Molarity gl (C) Aqueous Solution from Stripper No. 1 (1) CNS Concentration - Molarity (2) Specific Gravity (D) Aqueous Solution from Stripper No. 2 (1) CNS Concentration - Molarity (2) Specific Gravity (E) Aqueous Thiocyanate Solution from CNS Recovery Neutralizer (1) PH (2) Thiocyanate Concentration - Molarity 0) Flow Rate - GPH (F) HC1 Feed to Stripper (1) HCi Concentration •- Molarity (2) Flow Rate - GPH (G) H 2 S0l Feed to Scrubber (1) Concentration HgSOj, - Molarity (2) Flow Rate - GPH * Sample to Analytical L&boratoryo 21 Extraction Plant Control - Continued (H) ZrOCl 2 Feed Solution (1) CNS Concentration - Molarity (2) Flow Rate - GPH (i) Hexone from Thiocyanate Recovery Column (l) CNS Concentration - Molarity (J) Hexona from No. 1 Extraction Column (1) CNS Concentration - Molarity (2) Specific Gravity (K) Hexone from HV>SOl Scrubber Column (l) CNS Concentration - Molarity (L) Hexone from CNS Recovery Neutralizer (1) CNS Concentration - Molarity (M) Hexone to Extraction Columns (1) Flow Rate - GFH (N) Hexone to CNS Recovery Neutralizer (1) Flow Rate - GFH (0) Hexone to CNS Recovery Column (1) Flow Rate - GFH (P) Paw Hexone to Plant Makeup (1) Flow Rate - GPH Operating limits of control variables and frequency of sampling are as indicated by the following values • Frequency Normal of Sampling Av. Value Variation Limits A-l Zr Product Lbs/gal. 2 Hrs. 0.75 0.7-0.8 A-2 Hf PPM n 100 50-250 500 A-3 CNS Molarity n 0.40 M •35- .45 - B-l Hf Product Lbs/gal. 1+ Hrs. .01+ .035-. 01+5 „ B-2 Zr PPM HI 15000 1000-2+0,000 - B-3 CNS Molarity n .25 M .20-. 30 - C-l No. 1 Stripper CNS Molarity 2 Hrs. ■35 .25-. 1+5 - C-2 Sp.G. tt 1.055 I.0I+5-I.065 - 22 •acti on Plant Control - Continued Frequency of Sampling Av. Value Normal Variation Limits D-l D-2 No. 2 Stripper CNS Molarity Sp.G. 2 Hrs. n 2.8 1.300 2.2-3.2 1.27-1.33 1.25-1.35 E-l E-2 E-3 CNS Solution pH CNS Molarity GPH Z Hrs. n M 7.0 2.5 25 6-9 2.2-2.8 20-30 U-10.5 F-l F-2 HC1 Molarity GFH 2 Hrs. ■ 3-5 22 3-4-3.6 19-25 G-l G-2 HoSOi Normality GPH 8 Hrs. 5-0 30 4.5-5-5 28-32 H-l H-2 Feed CNS Molarity GPH 2 Hrs. 2.8 2.7-2.9 2.6-3.0 1-1 Hexone CNS Mol. 2 Hrs. 2.U 2.0-2.8 J-l J-2 Intermediate Hexone CNS Mol. Sp.G- 2 Hrs. ■ 2.8 .916 2.1+-3.2 .905-927 K-I L-l Scrubber Hexone CNS Mol. CNS Recovery Hexone Mol. 2. Hrs. 2 Hrs. 2.3 0.1 2.0-2.6 0.0-0.2 0.2 M-l Entering Hexone GPH 4 Hrs. 100 95-105 N-l Hexone to Neutralizer GPH 1+ Hrs. l+o 35-45 0-1 Neutralized Hexone GPH k Hrs. 40 35-45 P-l Hexone Makeup GPH - k 0-10 23 Extraction Plant Control - Continued I4.. Sampling: Samples are of two types: a. Spot samples* Take sample from sampling valve in line. First drain valve and discard* Then take sample in clean sample bottle. b. Tank samples- Use vacuum samplers provided. Return first portion sampled to tank. Then take sample in clean sample bottle. 5« Chemical Analysis- Procedures are given for testing acidity and CNS concentration in various solutions in Section Z-6 which follows. 6. Flow Measurement Method: Flow measurements are made by either of two methods depending on the line and tank arrangement. a. Measure time to fill one pint measure. Rate (GPH) s 14.50/sec. b. Measure gallonage tank change in two hours. Rate (GPH) = Gallons/2 7. Corrective Measures for Plant Control* In general, follow limiting values listed in Section 3° Specific measures for plant control are outlined below. a. A-2 Hf PPM. When Hf exceeds 500 ppm, notify foreman immediately. If value is very high and plant has been known to be out of balance for appreciable time, flow should be diverted to tank reserved for high Hf product until balance is restored to columns. b. D-J+ No. 2 Stripper Sp.G° If Sp.G. varies outside limits 1.25-1.35 and values are consistently high or low with CNS molarity, HC1 rate is indicated to be off. Condition should be corrected by making small changes in HCl pump rate at thymatrol control positioner. 24 Extraction Plant Control - Continued c. Any high or low values of variables listed in Section 3 should be noted and immediate measurements should be made of related values in order to obtain a correct diagnosis of troubles. Any of these values out of control for an appreciable length of time will be reflected in subsequent values of product purity. By attention to plant control measurements, operating personnel should find and correct any bad conditions before product is affected. 25 Z-6 Titration Methods 1) Method of Titration of Acid in Zirconium Feed Solution The calculations in this titration are set up for the determination of acid in zirconium-hafnium mixture analyzing 2% Hf . Pipette 2.0 ml of sample into 75-100 ml of distilled water. Add 10 drops of brom-cresol purple indicator. Titrate with 0.5 N NaOH until a definite purple end point is reached. (pH 6.5). The acid concentration is calculated as follows: acid normality - ( ml of NaOH)(N of NaOH ) - 2.35 (#/gal of Zr) (ml of sample) In the past the feed solutions averaged 1.05#/gal. Zr. 2) Method of Titration of Acid Concentration of Hydrochloric Acid and Sulfuric Acid Feed Solutions Pipette 2.0 ml of sample into 50 ml of distilled water. Add U-5 drops of phenolphthalein indicator. Titrate with 0.5N NaOH until a pink endpoint is reached. If the hydrochloric acid feed solution contains ammonium thiocyna ( te, methyl orange indicator should be used in place of phenolphthalein. In this case the endpoint is a change from orange to yellow. The acid normality of the solution is calculated as follows: N = ( ml of NaOH) (N of NaOH ) (ml of sample) 3) Method of Titration of Acid in Hafnium Feed Solution The calculations in this titration are set up for a zirconium-hafnium mixture analyzing I4.O5S Hf . Pipette 2.0 ml of sample into 75-100 ml of distilled water. Add 10 drops of brom-cresol purple indicator. Titrate with 0.5N NaOH until a definite purple 26 Z-6 Titration Methods (Continued) 3) Method of Titration of Acid in Hafnium Feed Solution (Continued) end point. (pH of 6.5). The acid concentration is calculated as follows: Acid Normality = ( ml of NaOH) (N of NaOH ) - 1.68 (#/gal of Zr-Hf Soln. ) (ml of sample) At the present time the feed soln. analyses about 0.63#/gal. U ) Method of Titration of Solutions for Thiocya nate Pipette 2.0 ml of sample into a 25 ml volumetric flask. Dilute the sample so that the bottom of meniscus coincides with the mark on the stem. Dilute the sample with distilled water if it is an aqueous solution or denatured alcohol in the case of hexone solutions. Shake the flask well. Pipette 1.0 ml of this solution into $0 ml of diluted hydrochloric acid (1 part 12NHC1 to h parts distilled water). Add U-5 drops of ferroin indicator. Titrate with 0.1N ce(HS0i ), until the light blue end point is reached. The thiocynate molarity is calculated as follows: M of CNS - [jnl of Ce(HS0i 1 )r] x factor. For a 0.1000N CediSO^)^ solution the factor is 0.2083. H-l Collection and Precipitation of Hafnium with Ammonia In the Extraction Plant, hafnium is extracted from the feed solution into the hexone, and in the scrubber it goes from the hexone into the sulfuric acid stream. The sulfuric acid is taken to the Tank Pit and collected in either Tank No. 11 or No. lU. 1) Collect the sulfuric acid (containing the hafnium) in one tank for a 2U- hour period. a) Change over to an empty tank at 7:00 AM each morning 27 H-l Collection and Precipitation of Hafnium with Ammonia (Continued) 2) With the metering pump (P-2), continuously feed a stream of ammonium hy- droxide into the same tank that is collecting the sulfuric acid (No. 11 or 1U) a) This should be adjusted to maintain a pH of 7»0 to 8.0 in the collection tank b) Maintain air agitation on the tank to get proper mixture of the solutions. c) Ammonia added to the sulfuric acid will give a slurry of hafnium hy- droxide and water. H-2 Filtering of Hafnium Hydroxide 1) At 7s00 AM each morning change the sulfuric acid from the plant and the ammonium hydroxide from metering pump (P-2) into the empty tank. a) Mark up Daily Work Sheet showing the change-over 2) Agitate the tank full thoroughly with a circulation pump for 1$ minutes. 3) Take a sample of the mixture in the tank and check for pH. a) If pH is correct and slurry is settling out of solution, the batch is ready to filter b) If pH is low and solids do not settle more ammonia is needed. This must be corrected before starting to filter batch k) Start filtering the mixture through the steel filter press (center, east wall). a) This is No. 2 press 5) When press is full, shut off pump, and using air for about 5 minutes, blow excess filtrate from press 28 H-2 Filtering of Hafnium Hydroxide (Continued) 6) Wash cake in press for about 10 minutes with water. Repeat with air for 5 minutes. a) Water on line on press 7) Wash for additional 10 minutes, use air again and for about 10 minutes after water stops coming out of press. 8) Break, down press and drop cake into stainless steel dolly. Transfer cake to clean drum and label. 9) Repack press and repeat proceedure until the tank is empty. a) The hafnium hydroxide cake will probably be high in sulfate (SOr) which will have to be removed by further washing. H-3 Rewashing of Hafnium Hydroxide Cako to Remove Sulfates 1) Put 200 gal. water into reactor a) Tank No. l£ or No. 16 2) Add 300 to 3^0 lbs. hafnium hydroxide cake a) Have agitator going when adding cake 3) When cake is all in the reactor, agitate for 30 minutes, or until all cake is thoroughly mixed. h) Filter through rubber press in SE corner. Repeat filtering and washing procedure as in II. a) This is No. 3 press 5) Put cake into clean wooden drum. For each drum full, sample and request lbs. Hf/lb. and % SOj^. Weigh and label "Washed Hf Cake. A. R # , Net Wt. ." 29 H-3 Rewashing of Hafnium Hydroxide Cake to Remove Sulfates (Continued) a) List each drum No., A. R. #, net wt., etc., in log for rewashed Hf cake. H-U Dissolving of Rewashed Hafnium Cake in Hydrochloric Acid 1) When 1^00 to 2000 lbs. of rewashed hafnium cake is collected and the analysis is available, prepare to dissolve it in hydrochloric acid. 2) Make a list of all drums ready for dissolving. Total weight of hafnium metal in each of the drums. a) This information will be in the washed hafnium log book 3) For each 5 pounds of hafnium metal in the batch, add 1 gallon HC1 in a reactor. a) Either Tank No. 15 or No. 16 k) With the agitator going and using a wood and rubber loading funnel, add the cake to the reactor. 5) Heat to 70-80 C and continue to agitate until solution becomes clear. 6) When solution is ready, filter through No. 3 press and collect the solution in Tank No. 13. a) Tank No. 13 to be used for storage of dissolved hafnium only H-5 Precipitation of Hafnium from HC1 Solution 1) Sample solution in T-13 and get lbs. Hf/gal. 2) When analysis is available, pump enough of this solution into either T-l£ or T-l6 to have 50 lbs. hafnium metal. 30 H-5 Precipitation of Hafnium from HC1 Solution (Continued) a) Divide $0 by the number of pounds hafnium per gallon to determine the number of gallons needed 3) Add enough water to bring the total gallons in the reactor to 200. U) Turn on agitator drive. 5) Add 90 lbs. salicylic acid. 6) Turn on steam and bring temperature to 80 C. 7) Hold this temperature for 30 minutes aging period. 8) Filter through No. 3 press. a) Take continuous drip sample of filtrate from press b) Make a composite sample of all filtrate from precipitation batch c) One precipitation batch will make several press batches of cake 9) While the batch is filtering, make up wash solution in the other reactor (T-15 or T-16, whichever is not used for above) a) Use: 200 gallons water 1 gallon HC1 2 lbs. salicylic acid 10) When press is full of cake, use the same pump and wash the cake with 100 gallons wash solution. 11) Dry cake thoroughly. Approximately l£ minutes after water stops coming from press. 12) Break down press and drop cake into clean dolly. a) Transfer into clean drums and hold until ready to rewash 31 H-6 Rewashing of Hafnium Salicylate 1) Put 200 gal. water into a reactor and prepare as wash solution and start agitation. a) Add: 1 gal HC1 2 pounds salicylic acid 2) Add approximately 3^0 lbs. hafnium salicylate cake to reactor. 3) Agitate 30 minutes or until all cake is thoroughly broken up. k) Filter. Slurry through No. 3 press. 5) When press is full, wash with 100 gallons wash solution 6) After washing, dry press with air, break it down and collect cake. Store the cake in clean wooden drums. 7) Remove the drum from the pit, weigh and label them, and enter them in the log book. Take them to proper storage area. GP 90 3O0Z UNIVERSITY OF FLORIDA 3 1262 08909 0301