1、MIL-T-63qbb b m 99999Ob 0322Li22 5 m MILITARY SPECIFICATION MIL-T-63466 (AR) 12 May i981 THIONYL CHLORIDE (For Use in Ammunition) This specification approved for use by the US Army Armament Research and Development Command and is available for use by ali Departmenst and Agencies of the Department of
2、 Defense. 1. SCOPE 1.1 This specification covers requirements, quality assurance provisions and packaging for the manufacture of thionyl chloride for use in lithium (SO Cia), reserve type batteries (see 6.3). 2. APPLICABLE DOCUMENTS 2.1 Issue of Documents - The following documents of the issue in ef
3、fect on. date of invitation for bids or request for proposal form a part of this specification to the extent specified herein. - SPEC IF ICATIONS M I LI TARY MIL-A-48078 - Ammunition, Standard Quality Assurance Provisions, General Specification for STANDARDS MILITARY MIL-STD-105 - Sampling Procedure
4、s and Tables for MIL-STD-129 - Marking for Shipping and Storage MIL-STD-1218 - ACS Chemicals 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
5、or as directed by the contracting officer.) FSC: 6810 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-7 - - MIL-T-63qbh b 99999Ob 0322423 7 M MIL-T-63466 (AR) 2.2 Other publications. The following documents form a part of this specification to the ex
6、tent specified herein. Unless otherwise indicated, the issue in effect on date of invitation for bids or request for proposal shall apply. ASTM-ELO 3 Water Using Karl Fischer Reagent ASTM-E 3 O0 Sampling Industrial Chemicals ASTM-D1217 Density and Specific Gravity of Liquids by Bingham Pycnometer AS
7、TM-D2905 Statements on Number of Specimens Required to Determine the Average Quality 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 association specificat
8、ions and standards are generally available for reference from libraries. They are also distributed among technical groups and various federal agencies). 3. REQUIREMENTS 3.1 Material. The material shall be thionyl chloride conforming to the following requirements: (see 6.3) 3.1.1 Appearance. The thio
9、nyl chloride shall be a clear, colorless to pale yellow volatile liquid with a very pungent odor when determined as specified in 4.6.1. 3.1.2 Properties. The thionyl chloride shall conform with the following table when determined as specified with the applicable paragraphs : . TABLE 1 Requirements f
10、or Thionyl Chloride Proper ties Test Paragraph Req u i remen t s Thionyl Chlor ide Percent (%) Sulfur Dioxide % Maximum Specific Gravity Minimum (Min) 93.6 (Max) 0.3 25O/15.5OC 1.63 Iron, PPM. Max 20 Water, parts per million (PPM) 20 o Sulfur Chloride % Max 0.1 4.6.2 4.6.2 4.6.4 4.6.3 4.6.5 4.6.2 .
11、K 2 . .- Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-L - MIL-T-b34bb b 7797706 0122q24 9 MIL-T-63466 (AR) - 3.2 First Article Inspection. This specification makes -I_ provisions for first article inspection. Requirements for the subinission of fi
12、rst article samples by the contractor shall be as speciiied in the contract (see 6.1). 4. QUfiLITY ASSURANCE PROVISIONS 4.1 Hesponsiblity 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
13、hereby made a part of this detail specification. 4.2 Classification of Inspection. The inspection require- ments specified herein are classified 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
14、 shall submit a first aticle sample as designated by the Contracting Officer for evaluation in accordance with provisions of 4.3.2 The first article shall consist of 50 milliliters of thionyl chloride obtained by sampling as described in 4.5.1 (smaller size samples may be taken that are consistent w
15、ith the requirements of the test). The sample shall be obtained from a production lot which i-ias been produced by the contractor using the same production processes, procedures and equipment as will be used in fulfill- ing the contract. All materials, shall be obtained from the same sources of supp
16、ly as will be used in regular production. jetted by the Government to any or all of the examinations for tests specified in 4.6 of this specification. 4.3.2 Inspections to be Performed. The sample will be sub- - 4.3.3 Rejection. See MIL-A-48078. 4.4 Quality Con for mance Inspec tion. 4.4.1 Lot Forma
17、tion. A lot shall consist of one or more batches of thionyl chloride 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 thionyl chloride that has been su
18、bjected to the same unit chemical or physical 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- / MIL-T-634bb 68 m 777770b 0122425 O m MIL-T-63466 (AR) process intended to make the final product homogeneous (See MIL-A-48078) . accordance with MIL-ST
19、D-105 . The product shall be submitted for inspection in 4.5 Testinq (see 6.3) PRECAUTION. This specification covers sampling aii testing of toxic or hazardous materials. Accordingly, it is emphasized that all applicable safety rules, regulations and procedures must be followed in handling and proce
20、ssing these materials. 4.5. Sampling. Two (2) independent and representative samples (approx. 50 mi) of Thionyl Chloride shall be sampled as specified in ASTM E300. The samples shall be tested indepen- dently in accordance, with the applicable methods given in 4.6. If either sample fails to meet any
21、 of the test requirements, the lot shall be rejected. The samples shall be subjected to the tests listed below: Table II Inspec ti on/Requiremen t Appearance (see 3.1.) Properties (see 3.1.2) De f ec t/C 1 ass i f i cat ion Major Major 4.5.2 Inspection equipment The contractor shall use commercial i
22、nspection equipment for all tests and examination specified in par 4.6. bility of assuring that proper calibration procedures are followed. Government approval of all inspection. equipment is required prior to its use. determine compliance with the requirements given in Table I shall be performed on
23、 the thionyl chloride samples obtained in 4.5.1. prescribed proceures for replicate determinations given in standard analytical chemistry textbooks or ASTM D2905. Also, unless otherwise specified herein, all chemicals shall be ACS Grade in accordance with MIL-STD-1218 or reagent grade. 4.6.1 Appeara
24、nce. The sample shall be examined visually to determine compliance with 3.1.1. He is also charged with the responsi- 4.6 fest Methods and Procedures. (see 6.2) - The tests to All tests given in this section shall be performed using .- 4 . 6 .2 Thionyl Chlor ide, Sulfur Dioxide and Sulfur Chlor ide j
25、see 6.2) . . Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-63qbb b M 7779706 0322q2b 2 MIL-T-63466 (AR) 4.6.2.1 Instrument conditions The thionyl chloride, sulfur dioxide and sulfur chloride shall be determined by gas chroma- tography using t
26、he following conditions. Instrument: Perkin, Elmers, Model 900 or equivalent. Detector: Thermal conductivity. Columns: 2 meter glass tubing, 4mm diameter. Column packing: 10% QF-1 on Chromosorb G (AW. DMCS). Oven temperature 53 - 85oC programmed 10C per minute In ec ti on block temper at ur e: 145OC
27、. Detector temper at ur e: 200C Carrier gas: 50 ml/min. helium. Sample size: 6 ul. 4.6.2.2 Procedure. Check the gas chromatographic opera- ting conditions, make necessary adjustment and allow, the instrument to stabilize. Inject a-6 u1 sample into the gas chromatograph set in accordance with the con
28、ditions specified in 4.6.2.1. Allow each component to elute from the column and measure its area with an integrator. 4.6.3 Determination of iron 4.6.3.1 Reaqents and apparatus Hydrochloric acid, conc. Nitric acid, conc. Iron standard solution, 10 Mg/ml Pipettes, 20 ml, 10 ml, 5 ml Beakers, 250 ml Vo
29、lumetric flasks, 50 ml Atomic Absorption spectrophotometer - Varian Model AA5 or equivalent 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-63466 (AR) 4.6.3.2 Procedure. Place 25 ml of concentracted hydro- chloric acid into each of 2-250 ml b
30、eakers and then add 2 ml of concentrated nitric acid. Pipet 20 ml of sample (32.76 9) into each beaker. Allow vigorous action to subside and then place on a hot plate and evaporate to about 10 ml. Cool and dilute with distilled water. Transfer (filter if necessary into a 50 mi volumetric flask and m
31、ake up to volume with distilled water. Adjust the instrument to the conditions given in 4.6.3.3.- With the digital readout control in the absorbance mode, aspirate the samples. Measure and record the absorbance readings of each solution. 4.6.3.3 Parameters Iron Lamp Var i an . Lamp current 25 ma Sli
32、t width Wavelength Oxid iz er Fuel 4.6.3.4 Calculations ppm Fe = 50 248.3 nm air 7.5 Acetylene 3.5 50 A-J (A2 - Al) 32.76 A1 = absorption of solution without standard added A2 = absorption of solution with standard added 4.6.4 Specific Gravity. The specific gravity shall be determined in accordance
33、with ASTM-D1217. 4.6.5 Determination of Water 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-b3Yhh 68 W 7777706 O322428 b = MIL-T-63466 (AR) 4.6.5.1 Infrared Spectrophotometer Method 4.6.5.1.1 Procedure. Working in an area having a relative
34、humidity of 3 percent (glovebox or dry room) fill a dried 10mm cylindrical spectrophotometric cell having near-infrared (NIR) silica windows with tnionyl chloride. This is best accomplished employing a glass pipette fitted with a rubber bulb. Stopper the cell with a ground glass or teflon stopper. P
35、lace the filled cel in the sample beam of a Beckman Model 4240 or equivalent infrared spectrophotometer and 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 peak at approximately 2800 c
36、m-1 absorbance employing the following equation. Calculate the value of Po A = loglo - P If it is found that the absorbance of the 2800 cm -1 peak is greater than approximately 1.2, reanalyze the solution using a 5 mm cell. 4.6.5.1.2 Calculation Calculate the water concentration of the thionyl chlor
37、 ide as follows: i) 10mn Cell ppm H20 = A 0.009033 2) 5mm Cell 2A ppm H20 = -Lii_ 0.009033 4.6.5.2 Alternate Method by Karl Fischer. The water shall be determined in accordance with ASTM-E203. 5. PACKAGING 5.1 Packinq 7 Provided by IHSNot for ResaleNo reproduction or networking permitted without lic
38、ense from IHS-,-,-MIL-T-63466 68 7777706 0122427 8 E - MIL-T-63466 (AR) 5.1.1 Level C. Unless otherwise specified the thionyl chioride shall be packed in accordance with manufacturer s commercial practice to assure acceptance by common carrier far safe delivery at first destination for immediate use
39、. 5.2 Marking. 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 Ordering data. See MIL-A-48078 6.2 Prior approval of the Contracting Officer is required for use of equivalent test methods. A descriptio
40、n of the proposed method should be submitted thru the Contracting Officer 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 precis
41、ion and drawings of any special equipment required. Thionyl chloride which has been found satisfactory for use in lithium batteries is manufactured by MCB. Manufacturing Chemist, Cincinnati, Ohio, 45212, Eastman Kodak Co., Rochester, N.Y. 14650, and Mobay Chemical Corporation, Penn Lincoln Parkway W
42、est, Pittsburgh, PA 15205. Thionyl chloride from other sources should be evaluated by ARRADCOM, ATTN: DRDAR-QAR-R, Dover, NJ 07801 before being approved as an equivalent. 6.3 Custodian: Preparing Activity: * U.S. GOVERNMENT PRINTING OFFICE: 1981-703-023/4515 Project No. : 6810-AB-ll Ar my- AR Army (AR) 8 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-
