1、I . MIL-L-q765 68 7777406 OL2L207 7 9 I MIL-L-48765 (PA) 19 June 1975 MILITARY SPECIFICATION LITHIUM HEXAFLUOROARSENATE (FOR USE IN AMMUNITION) This specification is approved for use by all Departments and Agencies of the Department of Defense. 1. SCOPE 1.1 This specification covers one grade of Lit
2、hium Hexafluoroarsenate (LiAsFg) for use in lithium reserve type batteries. (see 6 .T) . 2. APPLICABLE DOCUMENTS 2.1 The following documents of the issue in effect on date of invitation for bids or request for proposal form a part of this specification to the extent specified herein. SPECIFICATIONS
3、MILITARY MIL-A-48078 - Ammunition, Standard Quality Assurance Provisions, General Specification For STANDARDS MILITARY MIL-STD-129 - Marking for Shipping and Storage (Copies of specifications, standards, drawings, and publica- tions required by suppliers in connection with specific procurement funct
4、ion should be obtained from the procuring activity or as directed by the contracting officer.) 2.2 Other publications. The following documents form a part of this specification to the extent specified herein. Unless otherwise indicated, the issue in effect on date of invitation for bids or request f
5、or proposal shall apply. FSC: 6810 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-L-48765 (PA) AMERICAN SOCIETY FOR TESTING AND MATERIALS ASTM-E11 ASTM-E70 ASTM-E168 ASTM-E203 ASTM-E258 ASTM-E300 - Sampling Industrial Chemicals (Application for
6、copies should be addressed to the American Society for Testing and Materials, i916 Race Street, Phila- delphia, Pennsylvania 19103) . - Wire-Cloth Sieves for Testing Purposes - pH of Aqueous Solutions with the Glass - Infrared Quantitative Analysis, Rec. - Water Using Karl Fischer Reagent - Total Ni
7、trogen in Organic Materials by Electrode Practices Modified Kjeldahl Method 3. REQUIREMENTS 3.1 Material. The material shall be lithium Hexafluoro- arsenate (LIAsF6) conforming to the following requirements: (6.7) 3.1.1 Form. The material shall be in the form of white crystalline powder at room temp
8、erature and shall be free of dirt, chips, grease and other foreign matter when exainined as specified in 4.4.3.1 (see 6.3). diffraction pattern which conforms to Table I when tested as specified in 4.4.3.2. 3.1.2 X-ray diffraction. The material shall have an x-ray Table I Peak, d-value (decreasing o
9、rder of intensity) 3.63 4.14 2.17 4.33 1.81 3.1.3 Infra-red spectroscopy. The material shall possess an infrared spectrum conforming to Table II given below and the infrared spectrum given in Figure 1 when tested as specified in 4.4.3.3. 2 I Provided by IHSNot for ResaleNo reproduction or networking
10、 permitted without license from IHS-,-,-NIL-L-Lt765 68 m 9999906 OL2L209 O m MIL-L-48765 (PA) Table II Peak, Microns Range 2.96 2.85-3.05 as a doublet) 6.00-6.30 6 . 15 (this peak may appear 14.60 13.50-14.90 26.60 25.50-31.00 3.1.4 Impurities. The impurities present in the material shall not exceed
11、 the values given in Table III when tested in accordance with the applicable paragraph. In addition, the total of all impurities shall not exceed 2500 ppm. Table III impurities Metallic Impurities Copper Magnesium Sodium Silver Iron Aluminum Nickel Chromium Calcium Silicon Nitrogen Halogens Chlorine
12、 Bromine Iodine Sulfur Carbon Hydrogen Oxygen Containing Water Compounds Maximum Allowable Concentration 50 50 300 50 200 50 50 50 50 LOO 50 50 50 50 50 300 800 Test Paraqraph 4.4.3.4 4 . 4.3.5 4.4.3.6 4.4.3.7 4.4.3.8 4.4.3.8 None Detectable 4.4.3.9 200 4 . 4.3.10 3.1.5 Properties. The material shal
13、l conform with the following properties when tested in accordance with the ap- plicable test paragraph. 3 I Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-L-48765 b = 7777706 OL21210 7 MIL-L-48765 (PA) Property Test Requirement Paragraph 4.4.3.1
14、1 4.0 to 7.0 3.8 to 7.5 PH in Water in Methyl Formate (MF) Solubility in MF, $ 100 4.4.3.12 Hydrolysis/Dehydration Dimethylether, $ max Methanol,$ max e200 hrs 12 8200 hrs 0.1 Particle Size Thru a SS No. 25,X min 50 Thru a SS No. 120,%min 25 4.4.3 .i3 4.4.3 .i4 Potential (450 mv 4.4.3 .i5 3.2 First
15、article testing. This specification makes provisions for first article testing. Requirements for the submission of first article samples by the contractor shall be as specified in the contract (see 6.1) 4. QUALITY ASSURANCE PROVISIONS 4.1 Responsibility for Inspection and Standard Quality Assurance
16、Provisions. Unless otherwise specified herein or in the contract, the provisions of MIL-A-48078 shall apply and are hereby made a part of this detail specification. 4.2 Classification of Inspections. The inspection requirements specified herein are classified as follows: a. First Article Inspection
17、(see 4.3) b, Quality Conformance Inspection (see 4.4) 4.3 First article inspection 4.3.1 Submission. The contractor shall submit a first article sample as designated by the Contracting Officer for evaluation in accordance with provisions of 4.3.2. of 2 pounds of LiAsF6 obtained by sampling as descri
18、bed in 4.4.2.1. The sample shall be obtained from a production lot which has been produced by the contractor using the same production processes, procedures and equipment as will be used in fulfilling the contract. All materials, shall be obtained from the same sources of supply as will be used in r
19、egular production. The first article shall consist 4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-L-48765 68 m 9777706 OL2L2LL 7 m MIL-L-48765 (PA) 4.3.2 Inspections to be performed. The sample will be subjected by the Government to any or all
20、 of the examinations or tests specified in 4.4.3 of this specification. 4.3.3 Rejection. See MIL-A-48078 (PA). 4.4 Quality Conformance Inspection 4.4.1 Lot formation. A lot shall consist of one or more batches of LiAsF6 produced by one manufacturer, in accordance with the same specification, or same
21、 specification revision, under one continuous set of operating conditions. Each lot shall consist of that quantity of LiASF6 that has been subjected to the same unit chemical or physical mixingprocess intended to make the final product homogeneous. The product shall be submitted for inspection in ac
22、cordance with MIL-STD-105. performed in a dry atmosphere. drawn from each batch to be sampled using ASTM Procedure E300-70 for solids. Samples shall be selected for inspection in accordance with MIL-STD-1235, CSP-1 Plan, Inspection Level II, AQL 6.5%. If any sample fails to meet any,test requirement
23、 the batch represented by the sample shall be rejected. All batches produced between the time that the last batch was tested and accepted and the batch which failed should be tested in accordance with the applicable methods given in paragraph 4.4.3. If any of these batches fail to meet any of the te
24、st requirements, that batch shall also, be rejected. In addition, after any failure of a batch the contractor will return to 100% in- spection until successive batches are accepted as required by MIL-STD-1235. The samples shall be subjected to the tests listed below: 4.4.2 Testing (see 6.3 and 6.6).
25、 Sampling and testing shall be 4.4.2.1 Sampling. Approximately 1 pound of LiAsF6 shall be with- Inspection/Requirement Defect Classification Form 500-700 mg of sample in the rear section and Copper Oxide (CuO) catalyst in the forward section and the following procedures be used: a. Heat catalyst to
26、5OOOC b. Heat samples to 180OC for 1/2 hour. c. Absorb CO2 in an Ascarite filled cartridge and absorb water in an Anhydrone filled cartridge. d. Weigh cartridge e. Calculate % carbon and % hydrogen according to the .following equations: $C = (Wt C02)(12) x10 o (44) (grams of sample) %H= (Wt H30) (2)
27、 x100 (18) grams of sample) 4.4.3.9 Oxygen Containing compounds. Determine the presence of oxygen containing compounds present in the material by using a pyrolysis mass spectrographic method which appears in a standard or a reference textbook 4.4.3.10 Water (see 6.3). Determine the moisture content
28、of the material using the Karl Fischer method given in ASTM-E203. 4.4.3.11 pH. Prepare a 1 Molar solution in the LiAsF6 by dissolving 195.86g of the sample into a liter of distilled water and determine the pH of the resultant solution in accordance with the method given in ASTM-E70. In addition, pre
29、pare a 2 Molar solution of the LiASF6 by dissolving 391.72g of the sample into a liter of Methyl Formate. Quantitatively transfer 100 ml of this solution to a 1000 ml volumetric flask and dilute to the mark with distilled water. Determine the pH of this solution in accordance with the method given i
30、n ASTM-E70. The pH measurement is continued until a constant value is observed for at least a 10 minute period. Carbon dioxide should be excluded by an inert atmosphere. In the above procedures smaller solutions can be prepared with respective corresponding weights of materials reduced accord- ingly
31、. 7 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-k MIL-L-g87b5 68 7777906 01212/11 4 MIL-L-4 8765 (PA 4.4.3.12 Solubility in Methyl Formate. Transfer 9.79 grams of the sample to a 100 ml beaker and add 25 ml Methyl Formate. Add a magnetic stirring
32、 bar and allow to stir for 30 minutes at ambient on a magnetic stirrer. Remove stirring bar from beaker and allow beaker to stand for 3 minutes. During mixing the container must be sealed to prevent loss of methyl formate. residual solute or turbidity. 4.4.3.13 Hydrolysis/Dehydration. Determine the
33、hydrolysis/ dehydration of the 2 molar solution prepared in 4.4.311 as follows: Observe for any 4.4.3.13.1 Equipment a. Injection part packed with glass wool. b. Column - Chromosorb 101, 4 X 1/8“ diameter c. Detector - Flame .ionization d. Carrier Gas - Helium at 20 cc/min 4.4.3.13.2.Procedure: Add
34、10% distilled water to 4 ml of the MF solution. Store this solution at 57 5 l0C for 200 hours in a suitable glass container (5cc vial) capable of being sealed air tight with stopper and withstanding 100 psi. container and measure by standard gas chromatographic techniques: Remove stoppered Methanol
35、- 200 hours Dimethyl Ether - 200 hours 4.4.3.14 Particle Size. Superimpose the sieves of the meshes required in 3.1.5 as defined in ASTM Ell and attach the receiving pan to the bottom. mount the assembly on a shaker and operate the shaker for 5 minutes. At the end of 5 minutes weigh the granules ret
36、ained in each sieve and in the pan and calculate the percentages of each. 4.4.3.15 Potentiometric Value. Check the potentiometric value (EMF) of a 2 Molar solution of the sample in methyl fomrate (see 4.4.3.11) in accordance with ASTM-E70 or equivalent except that meter shall be set to indicate mill
37、ivolts and electrodes shall be: Saturated Calomel and Platinum. Place 100 grams of the sample in the top sieve, 5. PREPARATION FOR DELIVERY 5.1 Packing 8 I Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-*-. ,I MIL-L-48765 68 W 7797706 0121215 b W MI
38、L-L-48765 (PA) 5.1.1 Level A and Level C. Unless otherwise specified the LiAsF6 shall be packed in accordance with manufacturers comm- ercial practice to assure acceptance by common carrier for safe delivery at first destination for immediate use. 5.2 Marking. Unless otherwise specified, the shippin
39、g containers shall be marked in accordance with MIL-STD-129, and shall include the lot number. 6. NOTES 6.1 Ordering data. See MIL-A-48078 (PA). 6.2 Prior approval of the Contracting Officer is required for use of equivalent test methods. A description of the proposed method should be submitted thru
40、 the Contracting Office to: Commander, ATTN: SARPA-&A-A-P, Picatinny Arsenal, Dover, New Jersey 07801. This description should include but not be limited to the procedures used, the accuracy and precision of the method, test data to demonstrate the accuracy and precision and drawings of any special
41、equipment required. the sample should be in a strictly anhydrous atmosphere or should be conducted with dry, closed samplers. All equipment needs to be dried in a vacuum oven at 5OoC or higher. Anal, Chem., 29 (2), 172 (1957) has been found applicable. 6.5 Methods described in J.S. Fritz, S,S. Yamam
42、ura, Anal. Chem., 29(1) i58 (1957) or Standard Methods of Chem. Analysis, IIB, 2483 have been found applicable. 6.6 Toxicity. Specific information regarding toxicological properties of lithium hexafluoroarsenate is not available. Normal precautionary procedures associated with the use of inorganic a
43、rsenate salts should be observed. In addition, since hydro- fluoric acid is formed in acidic aqueous media, appropriate pre- cautions for hydrofluoric acid should be taken. 6.3 The material is extremely hygroscopic and the handling of 6.4 Method described in F.W. Chapman Jr and R.M. Sherwood, 9 Prov
44、ided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-L-48765 (PA) 6.7 Material meeting the requirements of this specification was previously obtained from. U.S. Steel Corporation Agri. Chemicals Division 30 Pryor Street S. W. P. O. Box i685 Atlanta, Georg
45、ia 30301 6.8 A suitable colorimetric method for nitrogen is described in Methods for Chemical Analysis of Water and Wastes, pi54, Envir- onmental Protection Agency, 1971, Cincinnati, Ohio 45268. Custodian: Project Number: 6810-AA65 Army-PA Preparing Activity: Army-PA 10 Provided by IHSNot for Resale
46、No reproduction or networking permitted without license from IHS-,-,- flIL-L-487bS b 79779Ob 0323237 T .O O m O O 2 O O 2 O O 0 O O 2 O O OD - O O % O O ln N 3 3 3 0 2 2 t O k u F 2 MIL-L-48765 (PA) Y) O s: r-. . n. * U. S. GOVERNMENT PRINTING OFFICG 1975 -603-766/0483 _ - Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-
