1、INCH - POUNDS MIL-DTL-757C 5 March 2012 SUPERSEDING MIL-L-00757B 16 May 1994 MIL-L-757A 01 September 1967 DETAIL SPECIFICATION LEAD STYPHNATE, NORMAL This specification is approved for use by all Departments and Agencies of the Department of Defense. 1. SCOPE 1.1 Scope. This specification covers the
2、 requirements and quality assurance provisions for the manufacture and acceptance of Normal Lead Styphnate for use in primer compositions (Section 6.1). 2. APPLICABLE DOCUMENTS 2.1 General. The documents listed in this section are specified in sections 3 and 4 of this specification. This section doe
3、s not include documents cited in other sections of this specification or recommended for additional information or as examples. While every effort has been made to ensure the completeness of this list, document users are cautioned that they must meet all specified requirements of documents cited in
4、sections 3 and 4 of this specification, whether or not they are listed. 2.2 Government documents. 2.2.1 Specifications, standards, and handbooks. The following specifications, standards, and handbooks form a part of this document to the extent specified herein. Unless otherwise specified, the issues
5、 of these documents are those cited in the solicitation or contract. AMSC N/A FSC 1376 DISTRIBUTION STATEMENT A. Approved for public release; distribution is unlimited. Comments, suggestions, or questions on this document shall be addressed to: Commander, US Army ARDEC, Attn: RDAR-QES-E, Picatinny A
6、rsenal, New Jersey 07806-5000 or emailed to ardecstdznconus.army.mil. Since contact information can change, you may want to verify the currency of this address information using the ASSIST online database at https:/assist.daps.dla.mil Provided by IHSNot for ResaleNo reproduction or networking permit
7、ted without license from IHS-,-,-MIL-DTL-757C 2 DEPARMENT OF DEFENSE STANDARDS MIL-STD-650 - Explosive: Sampling Inspection and Testing MIL-STD-1168 - Ammunition Lot Numbering and Ammunition Data Card MIL-STD-1916 - DoD Preferred Methods for Lot Acceptance (Copies of this document are available onli
8、ne at https:/assist.daps.dla.mil/quicksearch/ or from the Standardization Document Order Desk, 700 Robbins Avenue, Building 4D, Philadelphia, PA 19111-5094.) 2.2.2 Other Government documents, drawings, and publications. The following other Government documents, drawings, and publications form a part
9、 of this document to the extent specified herein. Unless otherwise specified, the issues are those cited in the solicitation. NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY NIST SRM 136 - National Institute of Standards and Technology, Standard Reference Material, Potassium Dichromate (Copies of thi
10、s document are available online at http:/www.nist.gov/index.html.) 2.3 Non-Government publications. The following documents form a part of this document to the extent specified herein. Unless otherwise specified, the issues of these documents are those cited in the solicitation or contract. AMERICAN
11、 SOCIETY FOR TESTING AND MATERIALS INTERNATIONAL ASTM E11 - Standard Specification for Woven Wire Test Sieve Cloth and Test Sieves ASTM E70 - Standard Test Method for pH of Aqueous Solutions With the Glass Electrode ASTM E300 - Standard Practice for Sampling Industrial Chemicals ASTM E323 - Standard
12、 Specification for Perforated-Plate Sieves for Testing Purposes (Copies of ASTM standards may be ordered online at http:/www.astm.org or from ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959) 2.4 Order of precedence. Unless otherwise noted herein or in the contract, in the
13、 event of a conflict between the text of this document and references cited herein, the text of this document takes precedence. Nothing in this document however, supersedes applicable laws and regulations unless a specific exemption has been obtained. Provided by IHSNot for ResaleNo reproduction or
14、networking permitted without license from IHS-,-,-MIL-DTL-757C 3 3. REQUIREMENTS 3.1 Requirement inspections. 3.1.1 First article. When specified (see 6.3), a sample shall be subjected to first article inspection in accordance with 4.2. 3.1.2 Conformance inspection. A sample shall be subjected to co
15、nformance inspection in accordance with 4.3. 3.2 Appearance. Normal lead styphnate shall be free of visible impurities or foreign materials. 3.3 Crystal form. Normal lead styphnate shall be crystalline. The longest dimension of any crystal shall not be greater than three times the next longest axis.
16、 Hexagonal plates shall be acceptable. 3.4 Crystal dimension. Unless otherwise specified, the largest dimension of any normal lead styphnate crystal or aggregate of crystals shall not be greater than 0.5 mm. 3.5 Chemical and physical characteristics. The chemical and physical characteristics of norm
17、al lead styphnate shall conform to the requirements given in TABLE I. TABLE I. Chemical and physical characteristics. Characteristics Requirement Granulation 100% through U.S. standard # 100 sieve Granulation (alternate method), microns 99% smaller than 176.0 microns 100% smaller than 250.0 microns
18、Apparent density, gm/cc 1.30 to 1.60 Acidity, pH 5.0 to 6.6 Material insoluble in ammonium acetate, max Percent 0.3 Material soluble in ether, max percent 0.1 Lead, percent 43.2 to 44.3 Nitrogen, percent 8.87 to 9.07 Instantaneous flash point (Differential Scanning Calorimeter, DSC), C 270 to 290 3.
19、6 Lot numbering. Each lot of lead styphnate shall be identified by a lot number. Lot numbering identification shall be in accordance with MIL-STD-1168. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-757C 4 4. VERIFICATION TABLE II. Requireme
20、nt/verification cross reference matrix. Method of Verification Classes of Verification 1 Analysis 2 Demonstration 3 Examination 4 Test A First article B Conformance Section 3 Requirement Description Verification Methods Verification Class Section 4 Verification Method 1 2 3 4 A B 3.1.1 First article
21、 X X X X 4.2, TABLE III 3.1.2 Conformance inspection X X X X 4.3, TABLE IV 3.2 Appearance X X X 4.4.2 3.3 Crystal form X X X 4.4.3 3.4 Crystal dimension X X X 4.4.4 TABLE I Granulation X X X 4.4.5 TABLE I Granulation (alternate method), microns X X X 4.4.5.1 TABLE I Apparent density X X X 4.4.6 TABL
22、E I Acidity X X X 4.4.7 TABLE I Material insoluble in ammonium acetate X X X 4.4.8 TABLE I Material soluble in ether X X X 4.4.9 TABLE I Lead X X X 4.4.10 TABLE I Nitrogen X X X 4.4.11 TABLE I Instantaneous flash point (DSC) X X X X 4.4.12 3.6 Lot numbering X X X 4.4.13 4.1 Classification of verific
23、ation. The inspection requirements specified herein are classified as follows: a. First article inspection (see 4.2) b. Conformance inspection (see 4.3) 4.2 First article. When specified, a sample shall be subjected to first article verification in accordance with TABLE III. 4.2.1 First article quan
24、tity. The first article sample shall consist of 500 g of normal lead styphnate. The first article inspection shall be performed on the quantities listed in TABLE III. 4.2.2 Inspection to be performed. The first article inspection shall be performed in accordance with TABLE III. Provided by IHSNot fo
25、r ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-757C 5 4.2.3 First article rejection. If any item of the sample fails to comply with the first article requirements, the first article shall be rejected. TABLE III. First article inspection. Examination or Test Samp
26、ling Quantity Requirement Paragraph Inspection Method Reference Appearance 1 g 3.2 4.4.2 Crystal form 1 g 3.3 4.4.3 Crystal dimensions 1 g 3.4 4.4.4 Granulation 30 g TABLE I 4.4.5 Granulation (alternate method) 1 g TABLE I 4.4.5.1 Apparent density 2 g TABLE I 4.4.6 Acidity 1 g TABLE I 4.4.7 Material
27、 insoluble in ammonium acetate 1 g TABLE I 4.4.8 Material soluble in ether 2 g TABLE I 4.4.9 Lead 0.55 g TABLE I 4.4.10 Nitrogen 0.8 g TABLE I 4.4.11 Instantaneous flash point (DSC) .5 mg TABLE I 4.4.12 Lot numbering 1/ 3.6 4.4.13 Notes: 1/ The first article sample shall be manufactured and assigned
28、 a first article lot number. All raw materials used in producing the normal lead styphnate shall be from the same sources as will be used in regular production. 4.3 Conformance inspection. 4.3.1 Lot formation. Lot formation shall be in accordance with the lot formation requirements of MIL-STD-1916,
29、paragraph Formation and identification of lots and batches. A lot shall consist of one or more batches not exceeding 226.5 kg (500 pounds) produced by one manufacturer, in accordance with the same specification revision, under one continuous set of operating conditions. 4.3.2 Inspection by classific
30、ation of characteristics. Known characteristics are classified in TABLE IV. The definitions of critical, major and minor defects are provided in paragraph “Definitions” of MIL-STD-1916. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-757C 6 T
31、ABLE IV. Conformance inspection classification of characteristics. Chemical and physical characteristics Classification Examination or Test Conformance Criteria Requirement Paragraph Inspection Method Reference Critical None defined Major 101 Appearance 4.3.3.2 3.2 4.4.2 102 Crystal form 4.3.3.2 3.3
32、 4.4.3 103 Crystal dimensions 4.3.3.2 3.4 4.4.4 104 Granulation 4.3.3.3 TABLE I 4.4.5 105 Apparent density 4.3.3.2 TABLE I 4.4.6 106 Acidity 4.3.3.2 TABLE I 4.4.7 107 Material insoluble in ammonium acetate 4.3.3.3 TABLE I 4.4.8 108 Material soluble in ether 4.3.3.3 TABLE I 4.4.9 109 Lead 4.3.3.3 TAB
33、LE I 4.4.10 110 Nitrogen 4.3.3.3 TABLE I 4.4.11 111 Instantaneous flash point (DSC) 4.3.3.3 TABLE I 4.4.12 Minor 201 Lot numbering 100% 3.6 4.4.13 Notes: 4.3.3 Testing. (see 6.6) 4.3.3.1 Sampling. Obtain two random 30 g samples from each batch of normal lead styphnate being submitted for inclusion i
34、n a lot. The samples shall be obtained from the process vessel prior to pack out using procedures described in ASTM E300 for slurries. 4.3.3.2 Testing for batch acceptance. One sample obtained according to 4.3.3.1 from each batch shall be tested in accordance with applicable test methods for conform
35、ance with requirements of appearance (see 3.2), crystal form (see 3.3), crystal dimension (see 3.4), apparent density (see TABLE I), and acidity (see TABLE I). If any sample fails to meet any of these requirements, the batch represented by the sample shall be rejected. 4.3.3.3 Testing for lot accept
36、ance. The second samples from the batches not rejected under provisions of 4.3.3.2 shall be placed in a suitable container of sufficient volume to hold a composite sample from all batches in the lot. The composite sample shall be thoroughly mixed to assure homogeneity, and two sub-samples of approxi
37、mately 30 g each shall be obtained from Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-757C 7 this composite sample. Both sub-samples shall be tested in accordance with the applicable test methods of 4.4 to determine conformance with the req
38、uirements of granulation (see TABLE I), material insoluble in ammonium acetate (see TABLE I), material soluble in ether (see TABLE I), lead content (see TABLE I), nitrogen content (see TABLE I), and instantaneous flash point (DSC) (see TABLE I). If either sub-sample fails to meet any of the test req
39、uirements, the lot represented by the composite sample shall be rejected. 4.4 Methods of inspection. All tests described in this section shall be performed using prescribed procedures. 4.4.1 Preparation of dry sample. Transfer a portion of the wet sample containing about 10 g of lead styphnate to a
40、Buchner funnel containing a medium texture filter paper and apply suction until sample is almost dry. While working behind a safety shield, spread the sample over a watch glass. Dry the sample by placing the watch glass in a desiccator over drying agent for 24 hours at ambient temperature or in an o
41、ven no higher than 75C until constant weight is obtained (this will take at least 2 hours). Use this dry sample for all determinations unless otherwise specified. 4.4.2 Appearance. Take a portion of the well stirred wet sample from 4.3.3.1 and spread over an area of approximately 4 cm2on a glass mic
42、roscope slide. Allow the sample to air dry. Examine the material microscopically for impurities using magnification of 50x, under illumination. Any sample containing visible impurities or foreign matter shall be rejected. Retain the slide for the determination of crystal form (see 4.4.3) and crystal
43、 dimensions (see 4.4.4). 4.4.3 Crystal form. Using the slide prepared in 4.4.2, observe the crystalline form (shape) under a microscope using a magnification of l00x under reflected light, and optionally, take a photomicrograph at 50x magnification. Any sample containing crystal form with the longes
44、t dimension greater than three times the next longest axis shall result in rejection of the batch. 4.4.4 Crystal dimensions. Using the slide prepared in 4.4.2, measure the longest dimension of the larger crystals observed when scanning the field with the aid of a mechanical stage. Use the most accur
45、ate means available to determine the longest crystal dimension. Consider the longest dimension to be the distance between the most remote points of any one crystal. 4.4.5 Granulation. Transfer about 30 g of the wet sample to a Buchner funnel and apply suction for 2 to 3 minutes. Weigh out a 10 g por
46、tion of the damp sample and transfer it to a clean three inch US Standard #100 Sieve which conforms to the requirements of ASTM E11 and ASTM E323. Carefully examine the sieve to be sure it is free of foreign material. Place the sieve in a porcelain evaporating dish which contains enough water to cov
47、er the wire screen of the sieve to a depth of about one half inch. Shake the sieve for a few minutes in such a manner that the lead styphnate is below the surface of the water and any material passing through the sieve is caught in the evaporating dish. When most of the lead styphnate has passed thr
48、ough the sieve, run a gentle stream of water through the sieve while brushing the residue gently with a soft natural hair brush until all in the sample that will pass through the sieve has passed through it. Behind a safety shield, visually examine the screen of the sieve for the presence of lead Pr
49、ovided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-757C 8 styphnate, at the completion of this operation. Thoroughly rinse the brush to ensure that lead styphnate particles are removed. After the final rinse, a small presence of visible lead styphnate on the sieve shall be cause for reject
