1、MIL-0-60 863A (AR) 7 March 1986 SUPERSEDING MIL-0-60863 MU 15 December 1967 MILITARY SPECIFICATION OXAMIDE This Specification is approved for use within the US Army Armament, Munitions and Chemical Command and is available for use by all Departments and Agencies of the Department of Defense. 1. SCOP
2、E c 1.1 Scope. This specification covers two types of oxamide for use in explosives as follows: Type I - Oxamide meeting the particle size requirements Type II - Oxamide meeting the granulation requirements given in 3.1. given in 3.1. 2. APPLICABLE DOCUMENTS 2.1 Government documents. 2.1.1 Specifica
3、tions and standards. Unless otherwise specified, the following specifications and standards of the issue listed in that issue of the Department of Defense Index of Specifications and Standards (DoDISS) specified in the solicitation form a part of this specification to the extent specified herein. SP
4、ECIFICATIONS FEDERAL RR-S-366 - Sieves, Standard for Testing Purposes PPP-C-301 - Chemicals, Dry and Paste, Packaging and PPP-D-723 - Drums, Fiber Packing of MIL ITARY MIL-D-6054 - Drums, Metal - Shipping and Storage Beneficial comments (recommendations, additions, deletions) and any pertinent data
5、which may be of use in improving this document should be addressed ta: Commanda, US Army Armament Research and Development Center, Attn: AMSMC-QA, Dover, New Jersey 07801-5001 by Uang the self-addressed Standardization Document ImDrovement 1 Proposai (DD Form 1426) appearing at the end of this docum
6、ent ot by letter. I fl AMSC N/A THIS DOCUMENT CONTAINS /o PAGES. FSC 6810 Approved for public release; distribution is unlimited. DISTRIBUTION STATEMINT A. Licensed by Information Handling ServicesNIL-O-bb3A b 777770b 03222q7 2 MIL-O- 60 86 3A STANDARDS MIL-STD-105 - Sampling Procedures and Table fo
7、r MIL-STD-109 - Quality Assurance Terms and Definitions MIL-STD-129 - Marking for Shipment and Storage MIL-STD-650 - Explosive, Sampling, Inspection and MIL-STD-1218 - ACS Chemicals MIL-STD-1235 - Single and Multi Level Continuous I nspec t i on by At t r i bu tes Testing Sampling Procedures and Tab
8、les for Inspection by Attributes (Copies of Specifications, standards, drawings and publications required by contractors in connection with specific acquisition functions should be obtained from the contracting activity or as directed by the contracting officer.) 2.2 Other publications. The followin
9、g other publications form a part of this specification to the extent specified herein. The isse of the documents which are indicated as-DoD adopted shall be the issue listed in the current DoDISS and the supplement thereto, if applicable. AMERICAN SOCIETY FOR TESTING AND MATERIALS (ASTM) ASTM Design
10、ation E300 - Recommended Practice for ASTM Designation D1193 - Reagent Water ASTM Designation D2905 - Statement of Number of Sampling Industrial Chemicals Spec imens Required to Determine the Average Quality . of a Textile Material (Application for copies should be addressed to the American Society
11、for Testing and Materials, 1916 Race Street, Philadelphia, PA. 19103.) (Technical society and technical association specifications and standards are generally available for reference from libraries. They are also distributed among technical groups and using federal agencies .) the text of this speci
12、fication and the references cited herein, the text of this specification shall take precedence. 2.3 Order of precedence. In the event of a conflict between 3 . REQUIREMENTS 3.1 Chemical and physical requirements. Oxamide shall conform to the applicable chemical and physical requirements specified in
13、.Table I when tested as specified in the applicable par ag r aph . 2 . Licensed by Information Handling ServicesTEST MIL -0-6 O 86 3 A TABLE I. Chemical and physical requirements for oxamide TEST TYPE I TYPE II PARAGRAPH Purity, percent, min 99.0 Moisture content, percent, max 0.1 Acidity, as oxalic
14、 acid, O. 05 percent, max 1 Residue, percent, max O. 05 Particle size, microns 422 Granulation, percent Thru US Standard Sieve No. 30 Thru US Standard Sieve No. 100, min 99.0 4.6.1 0.1 4.6.2 0.05 4.6.3 4.6.4 0.05 4.6.5 4.6.6 4.6.7 100.0 80.0 3.2 First article. When specified, a sample shall be subje
15、cted to first article inspection (see 4.3 and 6.1.1). 3.3 Workmanship. The manufacturer shall use procedures and controls which assure the oxamide produced does not contain foreign materials such as dirt, rust, paint or metal chips, etc. Compliance with this requirement shall be as specified in 4.6.
16、8. 4. QUALITY ASSURANCE PROVISIONS 4.1 Responsibility for inspection. Unless otherwise smcified in the contract or purchase order, the sup.plier is responsible for the performance of all inspections specified herein. Except as otherwise specified in the contract or purchase order, the supplier may u
17、se his own or any suitable facilities, acceptable to the government for the performance of the inspections. The government reserves the right to perform any of the inspections set forth in the specification where such inspections are deemed necessary to assure supplies and services conform to the pr
18、escribed requirements. Reference shall be made to MIL-STD-109 to define terms used herein. 4.2 Classification of inspections. The following inspection requirements specified herein are classified as follows: a. First article inspection (see 4.3). b. Quality conformance inspection (see 4.4). c. Packa
19、ging inspection (see 4.4.2 and 5). 3 Licensed by Information Handling ServicesMIL-O-bOb3A 68 999990b 0322249 b H- MIL-0-60 863A 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 wit
20、h provisions of 4.3.2. article shall consist of three kilograms (6.6 pounds) of the composition obtained by sampling as described in 4.5.1. The samples shall be obtained from a production batch which has been produced by the contractor using the same production processes, procedures and equipment as
21、 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. 4.3.2 Inspections to be performed. The sample will be subjected by the government to any or all of the examinations and tests specified in Table II of this
22、 specification and any or all requirements of the applicable drawings. The first 4 4.3.3 Rejection. If any sample fails to comply with any of the applicable requirements, the first article quantity shall be rejected. The government reserves the right to terminate its inspection upon any failure of a
23、 sample to comply with any of the stated requirements. TABLE II. First article inspection E XAMI NAT1 ON OR TEST Purity Moisture Acidity PH Residue Particle Size G r anul at ion Wor kmanship REQUIRl3MEEJT INSPECTION PARAGRAPH METHOD PARAGRAPH 3.1 3.1 3.1 3.1 3.1 3.1 3.1 3.1 4.6.1 4.6.2 4.6.3 4.6.4 4
24、.6.5 4.6.6 4.6.7 4.6.8 4.4 Quality conformance inspection. 4.4.1 Lot formation. A lot shall consist of a single production batch of not more than 1000 lbs (454Kg) which has been subjected to the same unit chemical or physical process intended to yield a substantially uniform final product. The lot s
25、hall be submitted for inspection in accordance with MIL-STD-105 (or MIL-STD-1235 when applicable) . 4 I - Licensed by Information Handling Services- I -=- A RIL-0-60863A 68 7779906 0122250 2 = MIL-0-6 O 86 3A 4.4.2 Examination. Sampling plans and procedures for the classifications of defects shall b
26、e in accordance with MIL-STD-105, except that inspection for critical defects shall be 100 percent. Contractors sampling plans, if used shall be approved by the government and shall provide, as a minimum, the protection afforded the government by the sampling plans in MIL-STD-105. Continuous samplin
27、g plans in accordance with MIL-STD-1235 may be used if approved by the procuring activity. 4.5 Testinq. PRECAUTION WARNING This specification covers sampling, testing and use of toxic or hazardous materials. Accordingly, it is emphasized that all applicable safety rules, regulations and procedures m
28、ust be followed in handling and processing these materials. 4.5.1 Samplinq. Using a cement-sampling thief a representative sample of about two pounds in accordance with ASTM Designation Method E300 for solids shall be taken from a container randomly chosen from those comprising the lot. 4.5.2 Accept
29、ance/rejection procedures. The lot represented by the sample shall be tested for compliance with the requirements specified in Table I. The lot shall be accepted if all of the test results comply with the requirements given in Table I. If the test results fail to meet any of the requirements the ent
30、ire lot shall be rejected. 4.5.3 Classification of defects. The classification of defects shall be as given in Table III. TABLE III. Classification of defects TEST CLASSIFICATION Pur i ty Moist Ure Acidity PH Residue Par ticle size Granulat ion Major defect Major defect Major defect Major defect Maj
31、or defect Major defect Major defect 5 Licensed by Information Handling Services-_. NIL-O-hOb3A b M 779970b O122251 4 M MIL-0-60863A 4.5.4 Inspection equipment. Commerciallyavailable inspection equipment shall be used for all examinations and tests specified in 4.4 and 4.6. The contractor is responsi
32、ble to have the necessary equipment available, use it correctly and to assure that proper calibration procedures are followed. Government approval of all inspection equipment is required prior to its use for acceptance purposes (see 6.4). 4.6 Methods of inspection. The following tests shall be I per
33、formed using prescribed analytical procedures for replicate I +I required. Unless otherwise specified herein, all chemicals and -I I 1 required in all test procedures. I determination given in standard analytical textbooks. ASTM Method D2905 may also be used to determine the number of replicates rea
34、gents used in the test methods shall be ACS Grade in accordance with MIL-STD-1218 or Reagent Grade. Purified and distilled water in accordance with ASTM Designation D1193 shall be used as 4.6.1 Purity. Accurately weigh to the nearest O.lmg approximately 0.359 of oxamide and transfer to a clean 600mL
35、 beaker. Add 200mL of 5 percent sodium hydroxide solution, stir, and place on a steam bath for 1 hour. Cool to room temperature an add about 270mL of water. Neutralize with 1:l sulfuric acid and add 40mL 1:l sulfuric acid in excess. Titrate with standard 0.2 N potassium permanganate solution, adding
36、 the reagent rapidly at first and then drop by drop as the end point is approached. The end point is a pink color which persists for 30 seconds. Calculate the percent oxamide as follows: Percent oxamide = 4.403AN W Where: A = potassium permanganate solution, mL. N = normality of potassium permangana
37、te solution. W = weight of sample on a moisture-free basis, gm. 4.6.2 Moisture (volatiles). Accurately weigh to the nearest O.lmg approximately 5g of the sample into a tared (with cover) low form 60mm diameter weighing bottle. for three hours, cool in a desiccator and weigh. Calculate the percent mo
38、isture as follows: Place in a 105 2 30 oven Percent moisture = 100A-B B Where: A = the weight of sample before drying. B = the weight of sample after drying. 6 Licensed by Information Handling Servicesi I I l I I I t t P I I t I I I I I I I I L I I I I I I I I I I I I l I l MIL-0-608b3A b W 7779706
39、0122252 b W MIL-O-6 O 86 3A 4.6.3 Acidity. Accurately weigh approximately 2g of the sample to the nearest 0.001g and quantitatively transfer to a 400mL beaker. Add about 200mL of water which has been made neutral to phenolphthalein and a teflon coated stirring bar and stir on a magnetic stirrer for
40、5 2 1 minutes. Filter the mixture through No. 40 Whatman Filter paper into a 600mL beaker. Wash the residue several times with the neutral water and allow the washings to flow into the 600mL beaker. Add 2 or 3 drops of phenophthalein indicator to the water and titrate to a light pink end point with
41、0.01N sodium hydroxide which has been standardized * 1 to 0.0001 N. Calculate the acidity of the oxamide as follows: Percent acidity (as oxalic acid) = 4.5AN W-WM Where: A = the volume of sodium hydroxide solution in mL B = the normality of the sodium hydroxide solution W = the weight of the oxamide
42、 sample M = the percent moisture of the oxamide expressed as a decimal as determined in 4.6.2 4.6.4 pH. Accurately weigh to the nearest 0.0019 approximately 2g of Oxamide sample and transfer to a clean 400mL beaker. Add 100mL of freshly boiled and cooled distilled water and stir for several minutes.
43、 Allow the solids to settle to the bottom of the beaker, then filter a portion of the water through No. 40 Whatman filter paper into a 200mL beaker. Determine the pH of the water with a pH meter using glass and calomel electrodes. The pH meter shall be calibrated with a standard buffer solution havi
44、ng a pH in the 6-7 range. a- 4.6.5 Residue on isnition. Accurately weigh to the nearest 0.hng a 29 sample of the oxamide into a tared platinum crucible. Place the crucible on a supported wire triangle and heat with a Fisher or Meeker or equal gently at first to a red heat. Heat for an additional 15
45、minutes after all of the organic matter appears to have been completely burned off. Cool the crucible in a desiccator and weigh. Calculate the percent residue on ignition as follows: Residue = 100A-B W-WM Where: A = the weight of the crucible and contents after ignition B = the tare weight of the cr
46、ucible W = The weight of sample in g. M = the percent moisture as determined in 4.6.2 expressed as a decimal 7 - I Licensed by Information Handling ServicesMIL-O-bOb3A b 777770b 0322253 W MIL -0-6 O 8 6 3A 4.6.6 Particle size (type I). The particle size of Type I oxamide shall be determined in accor
47、dance with Method 205.1 of MIL-STD-650. The density of oxamide is 1.667g/cc. 4.6.7 Granulation (type II). Nest a No. 30 and a No. 325 US Standard sieves conforming with the requirements of RR-S-366 with the No. 352 sieve on the bottom. Nest a bottom pan below the No. 325 sieve and transfer 1OOg accu
48、rately weighed to the nearest 0.01g in the No. 30 sieve, Place a cover on the No. 30 sieve and shake on a mechanical sieve shaker set to produce 300 f. 15 gyrations and 150 5 10 striker taps per minute for 5 minutes 5 15 seconds. Transfer the oxamide on the sieves and in the bottom pan to appropriat
49、e tared weighing containers and weigh each fraction accurately to the nearest 0.01g and calculate the percent oxamide passing through the No. 30 and the No. 325 sieve as follows : Percent oxamide passing thru No. 30 sieve = 100-100A W Percent oxamide passing thru No. 325 sieve = 100B W Where: A = the weight of oxamide left on the No. 30 sieve in g in g B = the weight of oxamide in the bottom pan W = the weight of the oxamide sample in g 4.6.8 Workmanship. Visually examine the contents of the container sampled and the sample taken for the presence of foreign materials . 5
