1、I - HIL-T-634 20 (AR) 12 Nay 1981 MILITARY SPECIFiCATION c-92 -2g 5 k s. THIONYL CHLORIDE ELbCTROLYTli (For use in Ammunition) This specification approved for use by the US Army Armament Research and Development Command and is available for use by all Departments and Agencies of the Department of De
2、fense. 1. SCOPE 1.1 This specification covers requirements an quality assurance provisions for the manufacturer of Thionyl Chloride Electrolyte Solution for use in batteries. 2. APPLICABLE DOCUMENTS 2.1 Issue of documents. The following documents of the issue in effect on date of invitation for bids
3、 or request for proposal form a part of this specification to the extent spec i fi ed here in . SPECIFICATIONS MILITARY MIL-A-48078 - MIL-L-63470 - MIL-A-63471 - MIL-T-63466 - STANDARDS MILITARY MIL-STD-105 MIL-STD-129 MIL- STD- i2 18 Ammunition, Standard Quality Assur- ance Provisions, General Spec
4、ifica- tion for Lithium Chloride (For Use in Ammuni- tion) Aluminum Chloride (Anhyrous) Thionyl Chloride (For Use in Ammunition) - Sampling Proceures and Tables for Inspection by Attributes - Marking for Shipping and Storage - ACS Chemicals Q U.S. GOVERNMENT PRINTING OFFICE 1981-703-023/4558 FSC 681
5、0 7. THIS DOCUMENT CONTAINS 9 PAGES. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-63420 (AR) z (Copies of specifications, standards, drawings and publica- tions required by suppliers in connection with specific procurement function should be
6、 obtained from the procuring activity or as directed by the Contracting Officer.) part of this specification to the extent specified 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 docum
7、ents form a ASTM-E300 Sampling InCiustrial Chemicals ASTM-D2905 Statements on Number of Specimens Required to Determine the Average Quality of a Textile Material. (Appplication for copies should be addressed to the American Society for Testing and Materials, 1916 Race Street, Philadelphia, PA 19013)
8、. 3. REQUIREMENTS 3.1 Thionyl Chloride Electrolyte Solution. Materials used in the mixing of a Thionyl Chloride Electrolyte solution shall conform with the specifications given below. The nominal composition of the Electrolyte solution shall be Thionyl Chloride 89.5% and Lithium Aluminum Chloride (L
9、i, Al, Cl4) 10.5% (See 6.3 and 6.4). APPLICABLE MATERIALS Lithium Chloride Aluminum Chloride Thionyl Chloride SPECIFICATION MIL-L-63470 MIL-A-63471 MIL-T-63466 - 3.2 Properties. The electrolyte shall conform to the following properties when tested in accordance with applicable paragraphs: TABLE I Re
10、quirements for Electrolyte I- Properties Requirements Test Paragraph Water, ppm, maximum 850 4.6.1 Iron, ppm, maximum 50 4.6.2 Density, g/mL at 24OC 1.68 4.6.3 (2 0.01) 2 I Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-b3420 68 W 7779706 0122
11、3.72 5 MIL-T-6 34 20 (AR) 3.3 - First article inspection. This specification makes provisions for first article inspection. 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
12、 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 class
13、ified 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
14、 first article shall consist of Thionyl Chloride Electrolyte Solution 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 u
15、sing the same production processes, procedures and equipment as will be used in fulfilling the contract. All materials, shall be obtained in the same sources of supply as will be used in regular production. 4.3.2 Inspections to be performed. The sample will be subjected by the Government to any or a
16、ll of the examina- tions for tests specified in 4.6 of this specification. 4.3.3 Rejection. See MIL-A-48078. 4.4 Quality conformance inspection. 4.4.1 Lot formation. A lot shall consist of one or more batches of Thionyl Chloride Electrolyte produced by one manufacturer, in accordance with the same s
17、pecification, or same specification revision, under one continuous set of 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-63420 68 7779706 0322373 7 MIL-T-63420 (AR) operating conditions. Each lot shall consist of that quantity of Thionyl Chl
18、oride Electrolyte that has been subjected 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 6.4). PRECAUTION: This specification covers samplin
19、g and testing of toxic or hazardous materials. Accordingly, it is emphasized that all applicale safety rules, regulations and procedures must be followed in handling and processing these materials. 4.5.1 Samplinq. Two (2) individual 100 ml samples from each batch or lot of the Thionyl Chloride Elect
20、rolyte solution shall be sampled as specified in ASTM E300. The sample 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 De
21、fect Classification listed below: Inspection/Requirement Defect Classification Thionyl Chloride Electrolyte Solution Major Proper ti es Major 4.5.2 Inspection equipment. The contractor shall use commercial inspection equipment for all tests and examina- tions specified.in para 4.6. He is also charge
22、d with the responsibility of assuring that proper calibration procedures are followed. Government approval of all inspection equipment is required prior to its use. 4.6 Test methods and procedures. (See 6.2 and 6.4). The tests to determine compliance with the requirements given in Table I shall be p
23、erformed on the Thionyl Chloride Electrolyte samplesobtained in 4.5.1. All tests given in this section shall be performed using prescribed procedures for replicate determinations given in standard analytical chemistry textbooks or ASTM-D2905. Also, unless otherwise specified herein, all chemicals sh
24、all be Reagent Grade or ACS Grade in accordance with MIL-STD-1218. 4 ,. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-63420 68 7799706 0122374 7 i MIL-T-63420 (AR) 4.6.1 Determination of water. Working in an area having a relative humidity of
25、L3 percent (glovebox or dry room) fill a dried 1Omm cylindrical spectrophotometric cell having near-infrared (NIR) silica windows with the manufactured electroLyte solution. This is best accomplished employing a glass pipette fitted with a rubber bulb. Stopper the cell with a ground glass or Teflon
26、stopper. Place the filled cell in the sample beam of a Beckman Model 4240 or equivalent infrared spectrophotometer and an identical unfilled cell in the reference beam. Scan from 4000 to 2500 cm-l at a rate of 600 cml/min. Determine the percent transmission values (Po) and (P) for the peaks at appro
27、ximately 3379 cml and 2780 cm-l as shown in Figure-l. each peak employing If it is found that Calcuiate the value of absorbance for the following equation. the absorbance of the 3379 cml peak is greater than approximately 1.2, reanalyze the soltion using a 5mm cell. If the absorbance is still greate
28、r than 1.2 repeat once again using a 2mm cell. Calculate the water concentration corresponding to the 2780 cm-1 peak (as measured in the 10mm cell) as follows: ppm H20 = A at 2780 cm-1 O .O09033 Calculate the water concentration corresponding to the 3379 cm-1 peak as follows (using A = absorbance at
29、 3379 cm-I): 10mm cell ppm H20 = A - 0.009 O. 006332 5mm cell ppm H2O = A - 0.005 O 003169 2mm cell ppm H20 = A - 0.005 0.000791 -= 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-63420 68 W 777770b 0322375 O MIL.T-63420 (AR) 100 90 80 70 60
30、50 40 30 20 10 O 4 I I I I I I I I I I I P 1 I ! 1 t I 1 ! 10 3800 3600 3400 3200 3000 2800 2600 2400 Wave Number, cm” Figure I. Typical Infrared Spectrum of a 1. OM LiAlCl4 /SoCl, Solution Showing How the Percent Transmigsion Values used in .the Absorbance Calculations are Obtained Provided by IHSN
31、ot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-63420 68 m 7977906 0122376 2 m MIL-T-63420 (AR) The total water concentration of the solution is obtained by summing the results: ppm H20 (Total) = p m H20 (2780 cm-l peak) + ppm H20 (3370 cm-? peak) 4.6.2 Determ
32、ination of iron. Working in an area having a relative humidity ofL 3 percent (glovebox or dry room), pipette 5.0 + 0.1 ml of-1.OM LiAlC14/SOC12 solution into a dried 100 hl volumetric flask. If the work is being done in a glovebox, the flask may be stoppered and removed at this time. Slowly add 15-2
33、0 ml of deionized water and allow solution to stand for several minutes in order to dissipate the heat generated. Add 15-20 ml of deionized water to a similar volumetric flask and then add the following reagents, in the order listed, to each flask. a. 30+0.5 mL of a 50-50 (by volume) mixture of meth
34、yl ethyl ketone and methanol. b. 10+0.2 - mL of 1:l Hydrochloric Acid solution. c. 5+0.1 mL of a 30 percent by weight Ammonium Thiocyanate (NH4SCN) solution. d. 5+0.1 mL of a 10 percent by weight Ammonium e. Dilute to mark with deionized water and mix well. Thiosulfate (NF4) 2S203) solution. Fill a
35、0.75 inch diameter spectrophotometric test tube (Fisher Scientific Catalog No. 7-144-40 or equivalent) with . each of the two solutions. Read the absorbance of the test-solution at 475 nm versus the blank employing a Bausch & Lomb Spectronic 20 or equivalent spectrophotometer. Calculate the concentr
36、ation of iron as follows: X = AbC - 0.004 O. 003243 Where X = Iron concentration, mg Abs = absorbance at 475 nm 7 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-63920 68 7777906 0322377 Lt MIL-T-63420 (AR) 4.6.3 Determination of density. Worki
37、ng in an area having a relative humidity ofe3 percent (glovebox or dry room) fill a dried, tared 25 ml volumetric flask to the volume mark with the manufactured electrolyte solution. Stopper the flask and weigh to 0.1 gram. Measure the temperature of the electrolyte solution to 0.5% with a glass the
38、rmometer. Calculate the density of the electrolyte solution as follows: d=G-T 25 Where, d = solution density, g/mL G = gross weight of volumetric flask, gm T = Tare weight of volumetric flask, gm Correct the density value to 24OC using the following equation: d24 = 0.001631 (T-24) + dT Where d24 = s
39、olution density at 24OC, g/mL T = measured temperature of solution, OC dT = measured solution density at temperature (T), g/mL 5. PACKAGING 5.1 Packinq. (see 6.4) 5.1.1 Level C. Unless otherwise specified the electrolyte solution shall be packed to afford protection against damage during direct ship
40、ment from supply source to the first receiving activity for immediate use. 5.2 Markinq. Unless otherwise specified, the shipping containers shall be marked in accordance with MIL-STD-129, and shall include the lot number. 6. NOTES 6.1 Orderinq data. See MIL-A-48078 6.2 Prior approval of the Contract
41、ing Officer is required for use of equivalent test methods. A description 8 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-, MIL-T-63420 b m 9999906 0122378 b m MIL-T-63420 (AR) of the proposed method should be submitted thru the Contracting Officer
42、 to: Commander, ARRADCOM, ATTN: DRDAR-QAR-R, Dover, NJ 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 equipment required. 6.3 Molar. A concentr
43、ation in which one molecular weight in grams (one mole) of a substance is dissolved in one liter of solution. The Thionyl Chloride Electrolyte solution contains a five mole percent excess of Lithium Chloride which will cause a small amount of insoluble material. 6.4 Preparation and storage. The Thio
44、nyl Chloride Electrolyte solution is prepared and stored in a working area having a relative humidity of55 percent (glovebox or dry room). The solution is prepared in a glass vessal or glass lined vessal, and stored in a dry room. Record the following: Electrolyte Batch Number Lithium Chloride manuf
45、acturer and lot number. Aluminum Chloride manufacturer and lot number. Thionyl Chloride manufacturer and lot number. Date of Electrolyte manufactured . Custodian: Army-AR Preparding Activity : Project Number: 6810-AB18 Army-AR 9 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-
