1、- MIL-L-q766 68 7777706 0121223 5 G -5b-07 MIL-L-48766(PA) 19 June 1975 MILITARY SPECIFICATION LITHIUM TETRAFLUOROBORATE (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 li
2、thium tetrafluoroborate (LiBF4) for use in lithium reserve type batteries. (See 6.3) . 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 M
3、ILITARY MIL-A-48078 - : 100 50 100 50 50 50 100 200 1000 None Detectable 50 80 4.4.3.4 4.4.3.5 4.4.3.6 4.4.3.7 4.4.3.8 4.4.3.9 4 0 4 0 3.11 4.4.3.8 4.4 . 3.10 3.1.5 Properties. The material shall onform with the following properties when tested in accordance with the applicable test paragraph . - .
4、. . . 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-L-48766 (PA) Property equirement Test Paragraph 4.4 . 3.12 4.4.3.13 4.4.3 0 14 Solubility in MF,% 98 Hydrolysis/Dehydration Dimethyl ether, % max Methanol, % max 200hrs 12 e200hrs 0.1 Thru a
5、 SS No.25, %,min Thru a SS No.120, %,min Particle Size 4.4.3.15 90 75 3.2 First article testing. This specifiuation makes provisions for first article testing. the submission of first article samples by the contractor shall be as specified in the contract. (see 6.1). Requirements for 4. QUALITY ASSU
6、RANCE PROVISIONS 4.1 Responsibility for Inspection and Standard Quality Assurance Provisions. 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 clas
7、sified as follows: First Article Inspection (see 4.3) Quality Conformance Inspection (see 4 . 4 ) Unless otherwise specified herein or a. b . 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 a
8、ccordance with provisions of 4.3.2. The first article shall consist of 2 pounds of LiBF4 obtained by sampling as described 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, pro- cedures and equipment as will
9、be used in fulfilling the contract. All materials, shall be obtained from the same sources of supply as will be used in regular production. 4 I Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-L-YA76b 68 7777906 0323227 2 NIL-L-48766 (PA) 4.3.2 In
10、spections to be performed. The sample will be subjected by the Government to any or-all 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
11、LiBF4 produced by one manufacturer, in accordance with the same specification, or same specification revision, under one continuous set of operating conditions. Each lot shall consist of that quantity of LiBF4 that has been sub- jected to the same unit chemical or physical mixing process intended to
12、 make the final product homogeneous. shall be submitted for inspection in accordance with MIL-STD-105. The product 4.4.2 Testing. Sampling and testing shall be performed in 4.4.2.1 Sampling. Approximately 1 pound of LiBF4 shall be a dry atmosphere. withdrawn from each batch to be sampled using hSTM
13、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 the batch represented by the sample shall be rejected. batches produced between the time that the last b
14、atch 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 test requirements, that batch shall also, be rejected. In addition, after any failure of a batch the contractor
15、 will return to 100% inspection until iiiit successive batches are accepted as required by MIL-STD-1235. The samples shall be subjected to the tests listed below: (Sampling shall be performed in a dry atmosphere). All Inspection/Requirement Form & Color (see 3.1.1) X-ray Diffraction (see 3.1.2) Infr
16、a-red Spectroscopy (see 3.1.3) Oxygen Containing Compounds (see 3.1.4) Moisture (see 3.1.4) pH (see 3.1.5) Solubility (see 3.1.5) Defect Classification Major B Major B Major B Major B Major B Major B Major B 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from
17、IHS-,-,-MIL-L-LI8766 68 777770b 0323228 4 a MIL-L-48766 (PA) 4.4.2.2 Inspection Equipment. The government reserves the right to inspect the contractors equipment and determine that he has available and utilizes correctly, measuring and test equipment of the required accuracy and precision and that t
18、he Instruments are of the proper type and range to.make measure- ments of the required accuracy. Commercial inspection equip- ment, shall be employed where applicable for all tests and examinations specified in 4.4.3. for assuring proper calibration procedures are followed. overn- ment approval of i
19、nspection equipment is required prior to its .use for acceptance purpose. 4.4.3 Test methods and procedures (see 6.2) The tests in 4.4.3.4 thru 4.4.3.15 shall be performed using prescribed analytical procedures for replicate determinations given in standard analytical textbooks. a dry atmosphere. Th
20、e contractor is responsible Testing shall be performed in 4.4.3.1 Form. Spread approximately 1/2 pound of the sample on a flat surface and examine the material visually for the pre- sence of contamination and form at a magnification of 25X. 4.4.3.2 X-Ray Diffraction. An X-ray diffraction pattern of
21、the material shall be obtained using a powder X-ray diffraction technique described in a standard for reference textbook on X-ray diffraction. graphic analysis of the material in accordance with method given in 4.4.3.3 Infra-red Spectroscopy. Perform an infra-red spectro- ASTM-E168. 4.4.3.4 Metallic
22、 Impurities. Determine the metallic impurities using a Atomic Absorption method described in a standard or reference textbook . 4.4.3.5 Nitrogen. Determine the nitrogen content using the standard method described in ASTM-E258-07 except that copper sulphate shall be used as the catalyst. 6 1 .- _cL_c
23、_- . . o Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- MIL-L-48766 68 9999906 OL2L229 b W MIL-L-48766 (PA) 4.4.3.6 Halogens. Determine the halogens present in the compound using a spectrophotometric method described in the literature or reference
24、textbook (see 6.4). 4.4.3.7 Sulfur. Determine the sulfur present in the compound using a method appearing in the literature or a ref- erence textbook (see 6.5). compound using a direct combustion method appearing in a reference textbook. It is suggested that the direct com- bustion method utilize pu
25、rified nitrogen gas and a two part combination tube, 500-7OOmg of sample in the rear section and Copper Oxide (CuO) catalyst in the forward section and the following procedure be used. a. Heat catalyst to 500C. b. Heat samples to 18OOC for 1/2 hour. c. Absorb CO2 in an Ascarite filled cartridge and
26、absorb water in an Anhydrone filled cartridge . d. Weigh cartridges e. Calculate % carbon and % hydrogen according to the following equations : 4.4.3.8 Carbon. Determine the carbon present in the x100 (Wt CO21 (12) %C= (4 4) ( grams of sample) (Wt H2O) (2) (18) (grams of sample) %H= x100 4.4.3.9 Oxy
27、gen 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. method which is described in a standard or reference textbook. 4 . 4 . 3 -10 Fluorides . Use a
28、 Specific Ion Electrode 4.4.3.11 Water. Determine the moisture content of the material using the Karl Fischer method given in ASTM-E203. 4.4.2.12 pH. Prepare a 1 Molar Solution of the LiBFq by dissolving 93.75 g of the sample in a liter of distilled water and determine the pH of the resultant soluti
29、on in ac- cordance with the method given in ASTM-E70. 7 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-HIL-L-8766 68 7777706 0323230 2 MIL-L-48766 (PA) In addition, prepare a 2 Molar solution of the LiBF4 by dissolving 187.5 g of sample in a.liter o
30、f Methyl Formate. Quantitatively transfer 100 ml of this solution to a 1000 ml -volumetric flask and dilute to the mark with distilled water. Determine bhe pH of this solution in accordance with the method given in ASTM-E70. 4.4.3.13 Solubility in Methyl Formate. Transfer 18.75 grams of the sample t
31、o a tall form 200 ml beaker and add 100 ml Methyl Formate. Add a magnetic stirring bar to the beaker and allow to stir for3O minutes, at ambient temperature, on a mag- netic stirrer. During mixing seal the beaker to prevent loss of methyl formate. Remove the magnetic stirring bar and quantitat- ivel
32、y filter the contents of the beaker thru a clean., tared glass medium porosity filtering crucible. Use a small amount of MF to aid in the transfer. Dry the crucible and contents in an oven maintained at 85OC + 5OC for 1 hour and weigh. Calculate the percent insolubles by the following equation. % In
33、solubles = Wt of residue X100 18.75 4.4.3.14 Hydrolysis/Dehydration. Determine the hydrolysis/ dehydration of the 2 Molar solution prepared in 4.4.3.12 as follows : 4.4.3.14.1 Equipment a Injection port packed with glass wool b. Column - Chromosorb 101, 4 x 1/8“ diameter c. Detector - Flame ionizati
34、on d. Carrier Gas - Helium at 20 cc/min 4.4.3.14.2 Procedure. Add 10% distilled water to 4 ml of the MF solution. a suitable glass container (5cc vial) capable of being sealed air tight with stopper and withstanding 100 psi. Remove stoppered container and measure by standnrd gas chromatographic tech
35、niques: Store this solution at 57 2 l0C for 200 hours in Methanol - 200 hours Dimethyl Ether - 200 hours 4.4.3.15 Particle Size. Superimpose the sieves of the meshes required in 3.1.5 as defined in ASTM-Ell-61 and attach the receiving pan to the bottom. Place 100 grams of the sample in the top sieve
36、, mount the assembly on a shaker and operate the shaker for 5 minutes. At the end of 5 minutes weigh the granules retained in each sieve and in the pan and calculate the percentages of each. 8 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-L-Y7b
37、b b 7777706 0121231 Y m MIL-L-48766 (PA) 5PREPARATION FOR DELIVERY 5.1 Packing 5.1.1 Level A and Level C. Unless otherwise specified, the LiBF4 shall be packed in accordance with manufacturers commercial practice to assure acceptance by common carrier.for safe delivery at first destination for immed
38、iate use. tainers shall be marked in accordance with MIL-STD-129, and shall include the lot number. 5.2 Marking. Unless otherwise specified, the shipping con- 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 method
39、s. method should be submitted thru the Contracting Officer 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 prec
40、ision and drawings of any special equipment required. 6.3 Material meeting the requirements of this specification was previously obtained from: Foote Mineral Company Route 100 Exton, Penna. 19341 A description of the proposed 6.4 Method described in F.W. Chapman Jr and R.M. Sherwood, Anal, Chem. 29
41、(2), 172 (1957) has been found applicable. Chem. 29 (i) 1581 or Standard Methods of Chem. Analysis II B, 2483 have been found applicable. in Sadtler collection of inorganic spectra under Infra-Red Spectrogram No. Y-1025K. 6.5 Methods described in J.S. Fritz, S.S. Yamamura, Anal. 6.6 A qualified infrared spectrum of LiBF4 can be found Custodian: Army-PA Preparing Activity: Army-PA Project Number: 6810-AA66 * U. S. GOVERNMENT PRINTING OFFICE 1975 -603-766/0476 9 -_ I Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-
