1、MIL-A-63467 68 m 777770b 0322433 6 m NIL-A-6 34 6 7 (AR) 12 May 1981 MILITARY SPECIFTCATION .- ACETYLENE BLACK (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 Departme
2、nt of: Defense. 1. SCOPE 1.1 This specification covers requirements, quality assurance provisions and packaging for the manufacture of Acetylene Black (100% compressed) for use in Thionyl Chloride (SO C12) type battery (see 6.3 and 6.4). 2. APPLICABLE DOCUMENTS 2.1 Issue of Documents. The following
3、documents of the issue in effect on date of invitation for bicis or request for proposal form a part of this specification to the extent spec if i ed here in. SPECIFICATIONS MILITARY MIL-A-48078 - Ammunition, Standard Quality Assurance Provisions, General Specification for STANDARDS MILITARY NIL-STD
4、-105 - Sampling Proceuures 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 fro
5、m the procuring activity or as directed by the contracting officer.) FSC 6810 .-. THIS DOCUMENT CCNU“liNS PAGES. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- MIL-A-634b7 68 W 7779706 0122432 U MIL-A-63467 (AR) 2.2 Other publications. The followin
6、g 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 for proposal shall appy. ASTM-E300 Sampling Industrial Chemicals ASTM-C57i Chemical Analysis of Carbon ASTM-D2905 Statements of Numb
7、er of Specimens and Carbon Ceramic Refractories Required to Determine the Average 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 specification
8、s and standards are generally available for reference from libraries. using Federal agencies.) They are also distribute among technical groups 3. REQUIREMENTS 3.1 Material. The acetylene black (Shawinigan), when examined by an electronmicroscope as specified in 4.6.1, shall show spherical particles
9、(approximately 100 to 1000 Angstroms) arranged in a chain like fashion. 3.2 Properties. The acetylene black shall conform with the requirements listed in Table I when tested in accordance with the applicable paragraphs: TABLE 1 REQUIREWNT FOR ACETYLENE BLACK Proper ties Requirements - Bulk density p
10、ounds per cubic foot, -lb/cu. ft. 11.0 - 14.0 Moisture, percent, Max. 0.20 Ash %, Max. 0.iO Cyclohexane extract, %, Max. 0.10 Test - Paraqraph 4.6.2 4.6.3 4.6.5 4.6.7 2 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-A-63q67 68 = 7779706 0322q33
11、T MIL-A-63467 (AR) Grit, % Max. 0.20 Carbon, 8 Minimum (Min) 99.5 Absorption, Stiffness (A.S.) value, Min., milliliters per 5 gram (ml/gm) 17 4.6.6 4.6.8 4.6.4 3.3 First Article Inspection. This sp-cification makes provisions for first article inspection. Requirements for the submission of first art
12、icle samples by the contractor shall be as specified in the contract (see 6.1). 4. QUALITY ASSURANCE PROVISIONS 4.1 Responsiblity 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 m
13、ade a part of this detail specification. 4.2 Classification of Inspection. The inspection requirements 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 shall su
14、bmit a first article sample as designated by Lhe Contracting Officer for evaluation in accordance with provisions of 4.3.2. The first article shall consist of 454 g of acetylene black obtained by sampling as described in 4.5.1. The sample shall be obtained from a production lot which has been produc
15、ed 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 regular production (see 6.3) 4.3.2 Inspections to be Performed. The sample will be subjec
16、ted 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 Inspection. 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-A-63Yb7 68 7777906 O
17、L22q34 Z MIL-A-63467 (AR) 4.4.1 Lot-formation for- continuous process. A lot shall consist of acetylene black produced by one manufacturer, in accordance with- the same specification, or same specification revision, under-one continuous set of operating conditions. Each inspection lot shall consist
18、of that quantity of acetylene black that has been subjected to the same unit chemical or physical processintended to make the final product homogeneous inspection in accordance with MIL-STD-105. “(See MIL-A-48078). The product shall be submitted for 4.5 -Testinq_(see 6.2). - PRECAUTION: This specifi
19、cation covers sampling and testing of toxic or hazardous materials. Accordingly, it is emphasized that all applieable safety rules, regulations and procedures must be followed in handling and processing these materials. 4.5.1 Samplinq. - TWO, (2) independent and representative (approximately 454 g)
20、samples shall be withdrawn from each lot of Acetylene Black using the procedures as 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 lot shall be reje
21、cted. The samples shall be subjected to the tests listed below. _ TABLE II -_ Defect Classification .* Inspection/Requirement Material (see 3.1) Proper ties (see 3.2) Major Major 4.5.2 -Inspection Equipment. The contractor shall use commercial inspection equipment for all tests and examinations spec
22、ified in para 4.6. -He is also charged 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) The tests to determine compliance with the requirements
23、 given in Table I shall be performed on the Acetylene Black samples obtained 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,
24、 all chemicals shall 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-A-b3Llb7 b W 979770b 0322435 3 W MIL-A-6 3467 (AR) 4.6.1 Material. The acetylene black shall be examined under a
25、 electron microscope to determine compliance with 3.1. 4.6.2 Determination of Bulk Density: Remove spatul 250 ml with a any lar a. Add , clean rubber ge lumps in the sample being used with a approximately 200 ml of the sample to a tared and dry, graduate cylinder which is fitted stopper. Tap the bot
26、tom of the cylinder on a large rubber stopper 50 times to settle the material. Read the volume (V) and reweigh the cylinder to 01. g (B). Calculate the bulk density as follows: 4.6.2.1 Calculation Bulk density (g/cm3) = (B - A) V Bulk density (lb/cu.ft.) = B.D. (g/cm3) x 62.4 Where: B = Wt. of cylin
27、der + stopper + sample, g A = Wt. of cylinder + stopper v = Volume of sample after tapping, cm3 4.6.3 Determination of Moisture. 4.6.3.1 Apparatus: weighing bottle with ground-in cover drying oven desiccator 4.6.3.2 Procedure: Quantitatively transfer an accurately weighed portion approximately 5 g)
28、of the sample to a tared weighing bottle fitted with a cover. Place the weighing bottle containing the sample, into an oven and heat at 1050 + 5OC until constant weight is obtained. Remove bottle, cover, cool in a dessicator and reweigh. 4.6.3.3 Calculation. Calculate the moisture as follows: % mois
29、ture = M x i00 (B - A) 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-A-63967 68 m 7777706 0322436 5 MIL-A-6 3467 (AR) A = Weight of bottle + cover, g. B = Weight of bottle + cover + sample before C = Weight after heating, g. heating, g. 4.6.4
30、 Determination of Abosrption - Stiffness (A.S.) Value 4.6.4.1 Apparatus: 500 cm3 Erlenmeyer flask 500 cm3 burette 4.6.4.2 Reagents: 10% acetone in water solution (See 4.6) 4.6.4.3 Procedure: Transfer a 5.0 g portion of the sample into a 500 ml conical flask. The acetone solution is added in the foll
31、owing manner. Initially add 10 ml and shake for 20 seconds, then add 2 ml and shake for 10 seconds. 2 ml additions and 10 seconds shaking are continued until small pellets having a diameter of 1/8“ (0.3 cm) to 1/4“ (0.6 cm) are formed. At this point the addition of liquid is cut to 1 ml. and continu
32、ed until the pellets grow to 1/2“ (1.3 cm) diameter. The additions are then again cut down to 1 ml. until finally over 2 or 3 spheres are present. From here 1/2 ml additions are used until one sphere is formed. This sphere, however, at first is fragile and will break on shaking. The solution is now
33、added, at 2 drops at a time until the sphere stands fairly vigorous shaking without breaking up. This is the end point. Read the burette. It will be found that a few drops beyond this point, smearing of black on the walls of the flask appears. Report the number of ml. required to form the ball for a
34、 5.0 g sample but before the walls of the flask are smeared. 4.6.5 Determination of Ash 4.6.5.1 Apparatus: procelain crucible muffle furnace desiccator 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-A-63467 bB W 7777706 0322437 7 W MIL-A-63467
35、 (AR) 4.6.5.2 Procedure: Weigh accurately a 10 tared porcelain crucible. muffle furnace maintained at 950 + 5OoC until the sample is completely ignited as evidenced by constant weight. Remove crucible from muffle furnace, cool in a de ssica tor and we igh . 0.lg portion of the sample into a Place cr
36、ucible with contents in a 4.6.5.3 Calculation: %ASH = q of residue x 100 g of sample of black . 4.6.6 Determination of Grit 4.6 . 6 . 1 Apparatus: See Figure 1 drying oven 4.6.6.2 Reaqents (See 4.6) : acetone 4.6.6.3 Procedure: Accurately weigh the 200 mash sieve cup (see Figure 1) and install in th
37、e apparatus. Quantitatively transfer an accurately weighed portion of the sample, approximately 50 g. to the funnel (see Figure 1). Wet the sample, contained in the funnel, with 100 ml of acetone and allow to filter thru. Then wash the sample with filtered water until the tiltrate is clear. Finally,
38、 wash the sample with a 100 ml portion of the acetone. Remove the sieve contain- ing the washed sample, dry at 1050 Y ?! Dia. 201: lilesh screenE i /e nj a - 1 nia o It - APPARATUF FOR GRIT PIGLTF I a - i. Flete1 E“ r;Y 3“ screens Vet a. cg1 in6 er IC Dia. Provided by IHSNot for ResaleNo reproductio
39、n or networking permitted without license from IHS-,-,-MIL-A-63467 68 W 9977706 0122Li33 O SS MIL-A-63467 (AR) 4.6.7 Determination of Cyclohexane Extract 4.6.7.1 Apparatus: Soxhlet apparatus Platinum dish 4.6.7.2 Reaqents: reagent grade cyclohexane 4.6.7.3 Procedure: . Quantitatively transfer an acc
40、urately weighed portion of the sample, approximately log, into a 43x1233 mm extrac- tion thimble and pack the thimble above the sample with glass wool. Place the thimble containing the sample in a Soxh let apparatus containing cyclohexane and extract for a minimum of 8 hours with a 10 minute cycle.
41、Then, remove thimble, remove glass wool and transfer the extracted sample to a tared platinum dish. Dry the dish and contents in an oven, 6O-OC maximum, until constant weight is obtained. Remove dish and contents from the oven, cool in a essicator, and reweigh. 4.6.7.4 Calculation: - % CYCLOHEXANE E
42、XTRACTABLE = q of residue x 100 g of sample 4.6.8 Carbon. The carbon shall be determined in accordance with ASTM C571 Section 30 to 32. 5. PACKAGING 5.1 Packinq. Unless otherwise specified, the Acetylene black shall be packed in accordance with manufacturers commercial practice to assure acceptance
43、by common carrier for safe delivery at first destination for immediate use. 5.2 Markinq. Unless otherwise specified, the shipping container shall be marked in accordance with MIL-STD-129, and shall include the lot number. 6. NOTES 9 Provided by IHSNot for ResaleNo reproduction or networking permitte
44、d without license from IHS-,-,-MIL-A-b3q67 68 m 7797706 OL22qqO 7 m MIL-A-63467 (AR) 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 description of the proposed method should be submitted thru the Contracting Officer
45、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 Acetylene black wh
46、ich has been found satisfactory for use in lithium batteries is manufactured by Shawinigan Product Corporation, 111 Charlotte Place, Englewood Cliffs, N.J. Acetylene Black from other sources should be evaluated by ARRADCOM, ATTN: DRDAR-QAR-R, Dover, NJ 07801 before being approved as an equivalent. 6
47、.4 The Acetylene black material is made by thermal decomposition of Acetylene at temperatures above 800OC. It has a more nearly crystalline structure than most Acetylene blacks, hence its unique use as a conductor in batteries. 6.5 The acetylene black is stable indefinitely. Since it is very light a
48、nd tends to dust easily, personnel should as a precaution use appropriate dust masks when handling. Custodian: Army-AR f7U.S. GOVERNMENT PRINTING OFFICE: 1981-703-023/4513 Pr epar ing Activity Project Number: 6810-AB14 ARMY (AR) 10 i) Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-
