1、e C5-g 0s- MIL-L-98772A 68 W 9999306 0121268 5 MIL-L-4 8 7 7 2A (AR) 12 May 1981 SUPERSEDES MIL-L-48772 (PA) 19 June 1975 MI LI TARY SPEC IFICATION LITHIUM (For Use in Ammunition) This specification approved for use by the US Army Armament Research and Development Command and is available for use by
2、. all Departments and Agencies of the Department of Defense. 1. SCOPE 1.1 This specification covers requirements, quality assurance provisions and packaging for the manufacture of two grades of lithium for use in Vanadium Pentoxide (V2O5) and Thionyl Chloride (SO C12) , reserve type batteries (see 6
3、.4). 1.2 Classification. Lithium shall be of the following grades specified: (see 6.1). Grade A - Lithium with Sodium Content 0.015 percent, Grade B - Lithium with Sodium Content 0.05 percent, max imum maximum 2. APPLICABLE DOCUMENTS 2.1 Issue of documents. The following documents of the issue in ef
4、fect on date of invitation for bids or request for proposal form a part of this specification to the extent speCf ied herein. SPECIFICATIONS MILITARY MIL-A-48078 - Ammunition, Standard Quality Assurance Provisions, General Specification for FSC: 6810 Q US. GOVERNMENT PRINTING OFFICE: 1981-703-023/37
5、39 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- MIL-L-LI772A 68 7979706 OLZL267 7 MIL-L-48772A (AR) STANDARDS MIL I TARY MIL-STD-105 - Sampling Procedures and Tables for MIL-STD-129 - Marking for Shipping and Storage MIL-STD-1218 - ACS Chemicals
6、Inspection By Attributes (Copies of specifications, standards, drawings and publications required by suppliers in connection with specific procurement function should be obtained from the procuring activity or as directed by the contracting officer.) part of this specificationto the extent specified
7、 herein. Unless otherwise indicated, the issue in effect on date of invitation for bids or request for proposal shall apply. 2.2 Other publications. The following documents form a ASTM-E300 Sampling Industrial Chemicals ASTM-D2905 Statements on Number of Specimens Required to Determine the Average Q
8、uality of a Textile Material (-Application for copies should be addressed to the American Society for Testing and Materials, 1916 Race Street, Philadelphia, PA 19013). (Technical society and technical associations specifications and standards are generally avai 1 able for reference from libraries. T
9、hey are also distributed among technical groups and using federal agencies). 3. REQUIREMENTS 3.1 Material. - The material shall be lithium conforming to the following requirements: (see 6.3 and 6.4). 3.1.1 Form. The material shall have a silver metalic lus- ter. No oizr other protective coatings sha
10、ll be on the metal surface. The material shall be examined as specified in 4.6.1. the following table when analyzed in accordance with the applicable paragraphs: 3.1.2 Chemical analysis. The material shall conform with 2 Provided by IHSNot for ResaleNo reproduction or networking permitted without li
11、cense from IHS-,-,-MIL-L-q877ZA 68 = 777770b 0323270 3 MIL-L-48772A (AR) TABLE 1 Requirements for Lithium Chemical Property Requirement Grade A B Lithium, %, min 99.9 99.8 Sodium, %, max 0.015 0.05 Potassium, % max 0.01 0.01 Calcium, %, max 0.02 0.02 Chlorides plus Iron % max 0.06 0.06 Test Paragrap
12、h 4.6.4 4.6.2 4.6.2 4.6.2 4.6.3 3.2 First article inspection. This specification makes Provisions for first article inspection. Requirements for the submission of first article sampies by the contractor shall be as specified in the contract (see 6.1). 4. QUALITY ASSURANCE PROVISIONS 4.1 Responsibili
13、ty for inspection and standard quality assurance 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 inspection. The inspection requirements specified herein are cla
14、ssified as follows: a. First Article Inspection (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. The
15、first article shall consist of approximately 5 grams of lithium obtained by sampling as described in 4.5.1 (smaller weight samples may be taken that are consistent with the requirements of the test). The sample shall be obtained from a production lot which has been produced by the contractor using t
16、he 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 regular production (see 6.3). 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license
17、from IHS-,-,-MIL-L-48772A b = 7777706 0323273 5 MIL-L-48772A (AR) 4.3.2 Inspections to be performed. The sample will be subjected by the Government to any or all of the examinations for- tests .specified in 4.6 of this specification. 4.3.3 Rejection. See MIL-A-48078. 4.4 Quality Conformance Inspecti
18、on. 4.4.1 Lot Formation. A lot shall consist of one or more batches of lithium 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 lithium that has been s
19、ub- jected to the same unit chemical or physical process intended to make the final product homogeneous (See MIL-A-48078). The product shall be submitted for inspection in accordance with MIL-STD-105. 4.5 Testing (see 6.2) PRECAUTION. This specification covers sampling and testing of toxic or hazard
20、ous materials. Accordingly, it is emphasized that all applicable safety rules, regulations, and procedures must be followed in handling and processing these materials. 4.5.1 Sam ling. Independent and representative samples approx 59) _fr sha be withdrawn from each batch or lot of ithium using the pr
21、ocedure specified in ASTM E300, section 25. The samples shall be tested independently in accordance with the applicable methods given in 4.6. If either sample fails to meet any of the test requirements, the batch or lot shall be rejected. The samples shall be subjected to the tests listed bel ow: I
22、Table-II Inspection/Requi rement Form (see 3.1.1) Chemical Analysis (see 3.1.2) Defect C 1 ass if i cat i on Mi nor Major 4.5.2 Inspection equipment. The contractor shall use commercial inspection equipment for all tests and examinations specified in para. 4.6. He is also charged with the responsibi
23、lity of assuring that proper calibration procedures arefollowed. Government approval of all inspection equipment is required prior to its use 4 L Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-. MIL-L-g772A b 7777706 O323272 7 W MIL-L-48772A (AR) 4.
24、6 Test methods and procedures. (see 6.2 and 6.5) The tests to determine comP1iance with the reauirements aiven in Table I shall be performed on the samples obtained in 4.5.1. All tests given in this section shall be performed using prescribed procedures for replicate determinations given in standard
25、 analytical chemistry textbooks or ASTM D2905. Also, unless otherwise specified herein, all chemicals shall be reagent grade or ACS Grade in accordance with MIL-STD-1218. 4.6.1 Form. After performing the analyses given in 4.6.2 take the necessary samp1.e and spread out in a thin layer on a sheet of
26、white paper* Visually inspect the sample to determine compliance with 3.1.1. 4.6.2 - Calcium, Potassium and Sodium 4.6.2.1 Standards. Standard calcium solution (50 ppm). Weigh 0.6243 g of Calcium Carbonate (CaC03 into a 500 ml volumetric flask, add water and just enough Conc. Hydrochoride Acid HC1 t
27、o dissolve the CaCO3. Dilute to mark with water and mix. Transfer 50 ml aliquot to a 500 ml volumetric flask and dilute to mark. Standard potassium solution (50ppm). Weigh 0.4765 g of Potassium Chloride (KC1) which has been previously dried at 1lOOC into a 500 ml volumetric flask, dissolve in water
28、and make to mark and mix. Transfer 50 ml aliquot to a 500 ml volumetric flask and dilute to mark. Standard sodium solution (50 ppm). Weigh 0.6355 g of NaC1 which has been previously dried at 1lOOC into a 500 ml volumetric flask, dissolve in water and made to mark and mix. Transfer 50 ml aliquot to a
29、 500 ml volumetric flask and dilute to mark. Working standards for potassium and sodium. Into individual 500 ml volumetric flasks, place the following: Flask # ml Stock KC1 ml Stock Na C1 Conc. ml HC1 3 (2 PPm) 20 20 2 4 (3 PPm) 30 30 2 5 (4 PPd 40 40 2 Dilute all to the mark and store in polyethyle
30、ne bottles. The standards will contain K and Na from O to 4 ppm. 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-L-48772A b 7779906 OL2Li73 7 MIL-L-48772A (AR) Working standards for calcium. Into individual 500 ml volumetric flasks, place the f
31、ollowing: Flask # ml of stock Ca CO3 g KC1 ml conc HC1 1 (0 PPm) O 0.1 2 3 (2 PPm) 20 0.1 2 4 (3 PPm) 30 0.1 2 5 (4 PPm) 40 0.1 2 Dilute all to the mark and store in polyethylene bottles. The standard will contain Ca from O to 4 ppm. 4.6.2.2 Procedure Prepare cleaned 400 ml plastic beakers by washin
32、g with HCI and rinsing with demineralized water. Weigh to 0.01 g about 2 grams of sample into the beakers, cover with a watch glass and add about 100 ml of demineralized water. After the sample is in solution, neutralize with HC1 using phenolphthalein as indicator plus 4 ml in excess of the HC1. Qua
33、ntitatively transfer the solution to clean 1000 ml volumetric flasks and dilute to the mark with demineralized water. Burn for potassium against standards using either Emission spectroscopy or Atomic Absorption (a.A.) and calculate concentration by an approved method. Make a 1 to 1 dilution of the s
34、ample and burn for sodium against standards using either Emission spectroscopy or A.A. and calculate concentration by an approved method. Using the dilution for sodium, add about 0.2 g/liter of solid KC1. After dissolving, mix and burn for calcium by A.A. (acetylene/nitrous oxide flame) using the st
35、andards made as above. Calculate the concentration by any approved method. 4.6.2.3 Calculations ppm K = pprn K in solution X 1000 Wt of sample ppm Na = ppm Na in solution X 2000 Wt of sample ppm Ca = ppm Ca in solution X 2000 Wt of sample 6 Provided by IHSNot for ResaleNo reproduction or networking
36、permitted without license from IHS-,-,-MIL-L-48772A 68 W 7779706 0323274 O MIL-L-48772A (AR) 4.6.3 Chloride plus iron. 4.6.3.1 Chl or i des. 4.6.3.1.1 Standards. Standard Chloride solution (0.001 N HC1). Dilute 10 ml of 0.10 N HC1 to 1000 ml. This solution is 0.001 N HC1 and will contain 0.0355 mg/m
37、l of chlorides. Silver nitrate solution (5%) Dissolve 5.0 g of silver nitrate in 100 ml water. Chloride working curve. Into individual clean 100 ml volumetric flasks add: Flask ml C1 Solution ml HNOS ml Ag NO3 mg C1 Present 1 O 2 2 3 4 4 6 5 8 6 10 O 0.071 O. 142 0.213 0.283 0.355 Dilute to the mark
38、, allow to stand five minutes in a dark place and determine turbidity (hellige, DRT 100, Spectronic 20 or other instrument). Plot turbidity units versus mg C1. 4.6.3.1.2 Procedure. Weigh about 0.49 of the lithium metal sample and transfer into a clean 400 ml plastic beaker. Add about 50 ml demineral
39、ized water into; and when reaction ceases, neutralize with conc. HNO3 using phenolphthalein as indicator, plus 4 ml of the HNO3 excess. Transfer the solution into a clean 100 ml volumetric flask, add 3 ml AgN03 solution, make up to mark mix and let stand for five minutes in the dark. Run on turbidim
40、eter against a blank made up with water and reagents. Determine mg contained C1 from previously drawn working curve. 4.6.3.1.3 Calculation for C1 PPB c1 = mit. c1 x 1000 , samp e 4.6.3.2 Iron - 4.6.3.2.1 Standards and Solutions. Standard iron solution (0.01 mg/ml) - Weigh 0.1000 g of pure iron metal
41、 into a one-liter volumetric flask. Add about 50 ml demineralized 7 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-L-48772A b W 7777906 0121275 2 W MIL-L-48772A (AR) water and 25 ml of concentrated HC1. When the iron has dissolved, dilute to mar
42、k with demineralized water and mix. Transfer a 50 ml aliquot to 500 ml volumetric flask, dilute to mark and mix. This solution will contain 0.01 mg/ml iron. 1,lO-phenanthroline (2.5%). Disolve 2.5 g of 1.10 - phenanthroline in 100 ml of ethanol. Hydroxylamine hydrochloride - (10%). Dissolve 50 g of
43、hydroxylamine hydorchloride in 500 ml of water. Sodium acetate - (saturated). Add about 100 ml water to a reagent grade sodium acetate bottle. 4.6.3.2.2 Establishing standard working curve. Pipette O, 1, 3, 5, 8 and 10 ml aliquots of 0.01 mg/ml iron solution into 100 ml volumetric flasks and dilute
44、to about 50 ml. Add 5 ml of hydroxylamine hydrochloride to flask and a small square of Congo Red paper. Add sodium acetate solution, with mixing, until the paper turns red. Add 1 ml of 1, 10- phenanthroline solution, dilute to volume and mix. Read absorbances at 510 mu, setting the instrument at O w
45、ith the O standard. Plot absorbance vs mg Fe. 4.6.3.2.3. Procedure Weight about 2 g of lithium metal into a dry 250 ml beaker and add 50 to 100 ml hexane. Cover with a watch glass and slowly add water until sample is in solution (do in a hood). Neutralize to phenalphthalein end point with conc HC1 a
46、nd add several drops in excess. Heat to drive off hexane and reduce volume to about 50 ml. Cool and transfer to a 100 ml volumetric flask. Add 5 ml of hydroxylamine hydrochloride solution and a small square of Congo Red paper. Add sodium acetate solution until paper turns red. Add 1 ml of 1, 10-orth
47、ophenanthroline solution, dilute to mark and mix. Run a blank at the same time but without sample and read absorbnce, at 510 mu, setting instrument to O with - this blank. 4.6.3.2.4 Calculation for Fe. Read mg of from previously drawn curve. Ppm Fe = mg Fe X 1000 Wt sample contained Fe 4.6.3.3 Calcu
48、lation for Chlorides Plus Ir values in 4.6.3.1 and 4.6.3.2 to obtain the su n. Add the - . 4.6.4 Determine the purity of Lithium by subtracting the 8 percent impurities-found in 4.6.2 and 4.6.3 from 100%. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,
49、-,- NIL-L-q8772A 68 W 7777706 0323276 4 W MIL-L-48772A (AR) 5. PACKAGING 5.1 Packing (see 6.3) . 5.1.1 Unless otherwise specified, the lithium shall be packed in accordance with manuf acturers commercial practice to assure acceptance by common carrier for safe delivery at first desti nati on for immediate use. 5.2 Markin . Unless otherwise specified, the shipping containers -TQ sha be marked in accordance with
