1、1 MIL-DTL-46225D 15 February 2012 SUPERCEDINGMIL-L-46225C (AR) 26 August 1968 MILITARY SPECIFICATION LEAD AZIDE RD-1333 This specification is approved for use by all Departments and Agencies of the Department of Defense. 1. SCOPE 1.1 Scope. This specification covers lead azide RD-1333 for use in the
2、 loading of detonators, blasting caps, percussion primers, fuzes, and in the manufacture of priming compositions. 2. APPLICABLE DOCUMENTS 2.1 General. The documents listed in this section are specified in sections 3 and 4 of this specification. This section does not include documents cited in other
3、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 sections 3 and 4 of this specification,
4、 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 of these documents are those cited in
5、the solicitation or contract. AMSC N/A FSC 1376 Distribution Statement A. Approved for public release; distribution is unlimited. INCH-POUND Comments, suggestions, or questions on this document should be addressed to: Commander, U.S. Army ARDEC, ATTN: RDAR-QES-E, Picatinny Arsenal, New Jersey 07806-
6、5000 or e-mailed to ardecstdznconus.army.mil. Since contact information can change, you may want to verify the currency of this information using ASSIST Online database at https:/assist.daps.dla.mil. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MI
7、L-DTL-46225D 2 DEPARTMENT OF DEFENSE SPECIFICATIONS MIL-S-51132 - Sodium Carboxymethyl Cellulose (For Ammunition Use) DEPARTMENT OF DEFENSE STANDARDS MIL-STD-1916 - DOD Preferred Methods for Acceptance of Product (Copies of these documents are available online at https:/assist.daps.dla.mil/ or from
8、the Standardization Document Order Desk, 700 Robbins Avenue, Building 4D, Philadelphia, PA 19111-5094.) 2.3 Order of precedence. Unless otherwise noted herein or in the contract, in the event of a conflict between the text of this document and the references cited, the text of this document takes pr
9、ecedence. Nothing in this document, however, supersedes applicable laws and regulations unless a specific exemption has been obtained. 3. REQUIREMENTS 3.1 First article. When specified (see 6.2), first article inspection shall be performed in accordance with 4.3. 3.2 Conformance inspection. Conforma
10、nce inspection shall be performed in accordance with 4.4. 3.3 Crystal growth control agent. Lead Azide RD-1333 shall be precipitated from a solution of Sodium Carboxymethyl Cellulose (NaCMC) which shall be used as the crystal growth control agent. 3.4 Physical characteristics. 3.4.1 Color. The color
11、 shall be white to buff. 3.4.2 Bulk powder. Powder shall be free flowing. 3.4.3 Particle size and shape. Particles shall be irregular in size and shape or regular bars of material (rectangles, pointed bars, etc) which may be slightly translucent. No transparent needle shaped crystals (length to widt
12、h of 7 to 1 or greater, similar to those in Figure 4) or platelets shall be present (similar to those in Figure 5). 3.5 Chemical tests. 3.5.1 Purity. The purity shall be 97.5 percent minimum (min). 3.5.2 pH. The lead azide shall not be greater than a pH of 7.5 and shall not be less than a pH of 5.0.
13、 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-46225D 3 3.5.3 Solubility in water. The solubility of the lead azide in water shall not be greater than 1.0 percent. 3.5.4 Matter insoluble in nitric acid. The insoluble matter of the lead azid
14、e in nitric acid shall not be greater than 0.05 percent. 3.5.5 Iron and copper. There shall be no more than 3 parts per million (ppm) of iron and no more than 3 ppm of copper present in the prepared test solutions. 3.5.6 Chlorides, nitrates and acetates. There shall be no more than 4 ppm of chloride
15、s, 15 ppm of nitrates and 72 ppm of acetates in the prepared test solutions. 3.5.7 Lead carboxymethyl cellulose. The carboxymethyl cellulose when determined as the lead salt shall be 0.50 percent min. and 1.20 percent maximum (max). 3.6 Bulk density. The bulk density shall be 1.0 gram (g) per milliL
16、iter (mL) min. 3.7 Workmanship. The lead azide shall be free from grease, wood slivers or chips, rubber or plastic particles or any other foreign particles (see 6.8). Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-46225D 4 4. VERIFICATION TA
17、BLE I. Requirement/Verification cross reference matrix. Methods of Verification Classes of Verfication 1 Analysis A First Article 2 Demonstration B Conformance 3 Examination 4 Test Section 3 Requirements Description Verification Method Verification Class Section 4 Verification Method 1 2 3 4 A B 3.1
18、 First article inspection X X X X 4.3 3.2 Conformance inspection X X X X 4.4 3.3 Crystal growth control agent X X X 4.6.4 3.4.1 Color X X X 4.6.1.1/4.5.1 3.4.2 Bulk powder X X X 4.6.1.2/4.5.1 3.4.3 Particle size and shape X X X 4.6.1.3/4.5.1 3.5.1 Purity X X X 4.6.2.1/4.5.1.1 3.5.2 pH X X X 4.6.2.2/
19、4.5.1.1 3.5.3 Solubility in water X X X 4.6.2.3/4.5.1.1 3.5.4 Matter insoluble in nitric acid X X X 4.6.2.4/4.5.1.1 3.5.5 Iron and copper X X X 4.6.2.5/4.5.1.1 3.5.6 Chlorides, nitrates, and acetates X X X 4.6.2.6/4.5.1.1 3.5.7 Lead carboxymethyl cellulose X X X 4.6.2.7/4.5.1.1 3.6 Bulk density X X
20、X 4.6.3/4.5.1 3.7 Workmanship X X X 4.6.5/4.5.1 4.1 Classification of inspection. The inspection requirements specified herein are classified as follows: a. First article inspection (see paragraph 4.3) b. Conformance inspection (see paragraph 4.4) 4.2 Inspection conditions. Unless otherwise specifie
21、d, all inspection shall be performed in accordance with the test conditions specified in 4.4, 4.5, and 4.6. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-46225D 5 4.3 First article. When specified, a sample shall be subjected to first artic
22、le verification in accordance with Table II. The testing shall apply to three (3) consecutive batches of lead azide that have been produced by the contractor using the same production process, procedures, and equipment as will be used in regular production. For a continuous process, samples shall no
23、t be pulled until steady state has been reached. All material before steady state shall be discarded. All materials, except packaging, shall be obtained from the same sources as will be used in regular production. 4.3.1 First article quantity. The first article inspection shall be performed on the q
24、uantities listed in Table II. 4.3.2 Inspection to be performed. The first article inspection shall be performed in accordance with Table II. 4.3.3 First article rejection. If any item of the sample fails to comply with all first article requirements, the first article shall be rejected. TABLE II. Fi
25、rst article tests and inspection. Examination or Test No. of Consecutive Batches Requirement Paragraph Paragraph Reference/ Inspection Method Crystal growth control agent 3 3.3 4.6.4 Physical characteristics 3 3.4 4.6.1 Chemical tests 3 3.5 4.6.2 Bulk density 3 3.6 4.6.3 Workmanship 3 3.7 4.6.5 Prov
26、ided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-46225D 6 4.4 Conformance inspection. 4.4.1 Lot formation. Lot formation of lead azide shall be in accordance with the lot formation requirements of MIL-STD-1916, paragraph “Formation and identificat
27、ion of lots and batches”. a. A lot shall consist of one or more batches of lead azide produced by one manufacturer in accordance with the same specification or same specification revision under one set of operating conditions. b. There shall be no intermixing of batches (see 6.12). Each batch shall
28、be identified with a batch identification number, name of manufacturer, date of manufacture as well as dry weight of lead azide contained. c. A new makeup of any one of the solutions (i.e., lead salt, sodium azide or sodium CMC) constitutes the formation of a new lot. 4.5 Testing. (see 6.8 for preca
29、ution) 4.5.1 Sampling. The tests depicted in 4.6.1, 4.6.3 and 4.6.5 shall be performed on an individual specimen from each batch. If any samples fail to comply with the requirements specified herein, the batch shall be rejected. The tests depicted in 4.6.2 shall be performed on a composite sample ob
30、tained by removing equal quantities of lead azide from each batch of lead azide in the lot and mixing to form a composite sample. 4.5.1.1 Preparation of composite sample. The tests depicted in 4.6.2 shall be performed on a composite sample from each lot. An equal portion of damp lead azide shall be
31、removed from each batch in the lot, by means of a conductive plastic spoon to form a sample of approximately 25 grams (dry weight). (Note: Samples may be taken directly from the process equipment or storage container). The sample shall be blended wet until uniform. Water shall be added in case the s
32、ample appears dry. The sample, thoroughly wetted, shall be transferred to an appropriate conductive container closed and secured with adhesive tape. The container shall be labeled to show the name of the material, manufacturer, plant, lot number and quantity of material in the lot. If the sample fai
33、ls to comply with the requirements specified herein, the lot shall be rejected. 4.6 Test methods and procedures. (see 6.10) 4.6.1 Physical characteristics. 4.6.1.1 Color. Determine the color of the lead azide by visual examination. 4.6.1.2 Bulk powder. Determine that the powder is free flowing by vi
34、sual examination. 4.6.1.3 Particle size and shape. Spread a small portion of the wet or dry sample on a clean glass slide so that approximately an area of one square inch is covered with a thin layer of widely spaced particles. Allow wet samples to dry at room temperature. Examine under an Provided
35、by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-46225D 7 optical microscope using magnifications of 50x to 200x, using a systematic approach to view a significant portion of the particles. At least 1 photomicrograph of each sample shall be retained. P
36、articles shall be similar to those in Figures 1, 2, or 3. Particles as shown in Figure 4 or 5 are unacceptable and the batches of lead azide containing such particles shall be rejected. 4.6.2 Chemical tests. 4.6.2.1 Purity. (see 6.8.2 for precaution) 4.6.2.1.1 Solutions for purity determination. a.
37、Ceric Ammonium Nitrate (CAN). Dilute with deionized or distilled water 60 mL of 70-72 % perchloric acid solution to approximately 700 mL, and add this solution to 60 g of reagent grade ceric ammonium nitrate. Heat and stir the mixture until solution takes place. Depending on the source CAN solutions
38、 can appear perfectly clear or have considerable insoluble matter. Allow to cool and let stand for forty eight hours. Filter the solution through a Gooch crucible fitted with GF/F filter mats to eliminate all insoluble matter. b. Perchloric acid solution. Dilute with deionized or distilled water 60
39、mL of 70-72 % perchloric acid solution to a volume of 1 liter. c. Ferrous Perchlorate solution (FP). This may be prepared in two ways. 1. Commercially available ferrous perchlorate can be used, if the color is still green. A brown color indicates the iron has oxidized to ferric and is no longer usab
40、le. Add 30 g of the solid ferrous perchlorate into a liter beaker. Add 700 mL deionized or distilled water and 60 mL of 70-72 % perchloric acid. Stir until all solid is dissolved. Filter through a Gooch crucible fitted with GF/F filter mats and make the volume up to 1 liter. Pass nitrogen gas throug
41、h the solution for two hours before using. Store solution in a closed container. 2. The second method involves making the solution from iron wire and perchloric acid. Add 6 g of iron wire into a liter beaker. Add 700 mL deionized or distilled water and 60 mL of 70-72 % perchloric acid solution. Heat
42、 beaker on a steam bath in a fume hood until the metal dissolves. There will be black residue. Filter through a Gooch crucible fitted with GF/F filter mats. Make volume up to 1 liter. Pass nitrogen gas through the solution for two hours before using. d. Ferroin indicator solution. Commercially avail
43、able ferroin indicator can be used. 4.6.2.1.2 Determination of CAN/FP ratio. Pipet 40 mL of the CAN solution into a 150 mL beaker. Add 25 mL of perchloric acid solution. Add two drops of the ferroin indicator solution. The color shall be yellow. Titrate with FP. Gradually the color lightens until th
44、e Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-46225D 8 yellow disappears, and the solution shall be a very pale blue. Continue titration drop wise with FP while stirring until the solution turns pink. Divide the volume of CAN by the volum
45、e of FP to get the CAN/FP ratio. 4.6.2.1.3 Standardization of CAN solution. Weigh about 0.3 g of sodium oxalate into a 250 mL beaker. Add a magnetic stir bar. Pipet 40 mL CAN solution into the beaker. Add 25 mL perchloric acid solution. Add two drops ferroin indicator solution. Cover the top of the
46、beaker with a watch glass, and stir the solution magnetically until all the sodium oxalate is dissolved. If the yellow color completely disappears, then the aliquot of sodium oxalate was too large. Try again with a smaller quantity. Titrate the contents of the beaker with FP until the solution just
47、turns pink. Normality of CAN N = (100xA)/ 6.701 x (40 BxC) Where: A = weight of sodium oxalate in grams B = mL of ferrous perchlorate used C = CAN/FP ratio 4.6.2.1.4 Determination of lead azide purity. Pipet 40 ml of CAN into a 150 mL beaker. Add 25 mL of perchloric acid solution. Add two drops of f
48、erroin. Cover the beaker with a watch glass, and place it in an ice bath for fifteen minutes. Use Teflon-coated spatulas and forceps for handling lead azide. Perform weighings in a high humidity (about 50-60 %) weighing room. Accurately weigh an amount of approximately 0.4 g of lead azide into a tar
49、ed small (1-2 mL) beaker. Using the forceps, plunge the small beaker into the 150 mL beaker. Wash the forceps tips with a spray of deionized water into the beaker. Gently stir the contents of the beaker with a glass or plastic stirring rod until all the solid has reacted. If the yellow color disappears, then the lead azide sample was too large. Repeat with a smal
