1、y 69W7 MIL -A- 8 2 66 7A (OS) 22 September 1978 Superseding 31 January 1977 MIL-A-82667 (OS) MILITARY SPECIFICATION MNIUM PERWRATE, GENERAL SPECIFICATION FOR This specification is approved for use by the Naval S,ea Systems Comd, Department of the Navy, and is available for use by all Departments and
2、 Agencies of the Department of Defense. 1. SCOPE 1.1 SCO e. This specification covers the general requirements for ammonium perc + lorate. 1.2 Classification. Ammonium perchlorate shall be supplied with Purity and granulation shall be as specified in or without tricalcium phosphate (TCP) as specifie
3、d i9 the applicable detail specification. the applicable detail specification. 2. APPLICABLE DOCUMENTS . 2.1 Issues of documents. The following documents of the issue in effect on date of invitation for bids or request for proposals, form a part of this specification to the extent specified herein S
4、PECIFICATIONS * MILITARY MIL-D-3464 Desiccants, Activated, Bagged, Packaging Use and Static Dehumidification MIL-P- 82646 Plastic Film,Conductive, Heat-Sealable, Flexible - MIL-A- 82667/1 Ammonium Perchlorate, High Purity MIL-A- 82667/2 Ammonium Perchlorate, Conditioned Beneficial comments (reconune
5、ndations, additions, deletions) and any pertinent data which may be of use in improving this document should be addressed to: Standardization Division (611), Indian Head, Md 20640, by using the self-addressed Standardization Document Improvement Proposal (DD Form 1426) appearing at the end of this d
6、ocument or by letter. - Commanding Officer, Naval Ordnance Station, m , -5 i THIS DOCUMENT CONTAINS /-/ PAGES. i B, -. Licensed by Information Handling ServicesFEDERAL FED- STD- 31 3 MILITARY MIL- STD- 105 MIL-STD-129 MIL-STD-414 Material Safety Data Sheets, Preparation and the Submission of Samplin
7、g Procedures and Tables for Inspection by Attributes Marking for Shipment and Storage Sampling Procedures and Tables for Inspection by Variables for Percent Defect ive MIL-STD-1218 ACS Chemicals PUBLICATIONS NAVAL SUPPLY SYsm cm Publication SOS/MCO P4030.19 Packaging and Handling of Dangerous Materi
8、als for Transporting by Military Aircraft (Copies of specifications, standards, drawings and publications required by suppliers in connection with specific procurement functions should be obtained fran the procuring activity or as directed by the contracting officer). this speciFkation to the extent
9、 specified herein. indicated, the issue in effect on date of invitation for bids or request for proposal shall apply. 2.2 Other publications. The following documents form a part of Unless otherwise AMERICAN SOCIETY KIR TESTING AND MATERIALS 2 MIL-A- 82667A(OS) STANDARDS MIL-STD- 1234 Pyrotechnics, S
10、ampling, Inspection and Testing ASIM B 330-65 Average Particle Size of Refractory Metals and Canpounds by the Fisher Sub-sieve Sizer ASIM D 1348-61 Moisture in Cellulose Licensed by Information Handling ServicesMIL-A-82bb7A b 777770b OL23L42 4 W ASTM E 11-70 MIL-A-82667A Wire-Cloth Sieves for Testin
11、g Purposes ASTM E 203-75 (Application for copies should be addressed to the American Society Water Using Karl Fischer Reagent for Testing and Materials, 1916 Race Street, Philadelphia, PA 19103). CODE OF FEDERAL REGLATIONS 46 CFR 140-149 Shipping 49 CFR 100-199 (The Interstate Cormnerce Cammission R
12、egulations are now a part of the Code of Federal Regulations, available from the Superintendent of Documents, Government Printing Office, Washington, DC 20402. Orders should cite “46 CFR 140-149 or 49 CFR 100-199 the latest issue and supplements thereto). Transpor tat ion NATIONAL MOTOR FREIGHT TRAF
13、FIC ASSOCIATION, INC AGENT National Motor Freight Classification (Application for copies should be addressed to American Trucking Associations,. Attn: D.C. 20036). Traffic Department, 1616 P Street, Washington, UNIFORbI CLASSIFICATION CmTEE, AGENT Uniform Freight Classification (Application for copi
14、es should be addressed to the Uniform Classification Cmittee, Rom 1106, 222 South Riverside Plaza, Chicago, IL 60606). standards are generally available for reference from libraries. are also distributed among technical groups and using Federal agencies). (Technical society and technical association
15、 specifications id They 3. REQUIREMENTS 3.1 Detail specifications. The individual material requirements shall be as specified herein and in accordance with the applicable detail specifications. this specification and the detail specification, the latter shall govern. requirements shall be drawn from
16、 the poperties in TABLE I. The detail specification shall delineate the specific requirements. In the event of any conflict between requirements of 3.2 Chemical and physical requirements. The chemical and physical 3 Licensed by Information Handling ServicesMIL-A-82bhA 68 7779706 0123143 b MIL-A- 826
17、67A(OS) 3.3 Granulation and form. The average particle size, the size distribution and the form of the crystals shall be as given in the detail specification. 3.4 Material safety data sheets. The contractor shall prepare and submit material safety data sheets in accordance with FED-STD-313 as specif
18、ied in the contract (see 6.4). minants, foreign material for the purpose intended. TABE I. 3.5 Workmanship. The material shall be uniform, free from conta- or any other defect that would prevent its use Chemical and physical properties. :omposition requirements (wt%) Purity Chloride, as NH4Cl Chlora
19、te, as NH4ClO3 Bromate, as NH4BrO3 Chromate, as K2Cr04 Sulfate, as (NH4)2SO4 Sulfated ash, calculated Sulfated ash, calculated Sodium and potassium Nonalkali metals as oxides Tricalcium phosphate, as Moisture, surface Moisture, total Water insolubles Ether soluble Total volatiles as NaCl04 Iron, as
20、Na2soi! as e203 Ca3 (PO41 2 Stability (hr) PH Friability, %passing Color Granulat ion No. 100 (150pm) sieve 4. QUALITY ASSURANCE PROVISIONS 4.1 Responsibility for inspection. Unless otherwise specified in the contract, the contractor is responsible for the performance of all inspection requirements
21、as specified herein. Except as otherwise specified 4 Licensed by Information Handling ServicesMIL -A- 8 2 667A(OS) in the contract, the contractor may use his own or any other facilities suitable for the performance of the inspection requirements specified herein, unless disapproved by the Governmen
22、t. The Government reserves the right to perform any of the inspections set forth in the specification where such inspections are deemed necessary to assure that supplies and services conform to prescribed requirements. 4.2 Lot. Alot shall consist of the total quantity of cross-blended material. For
23、non-cross-blended material, a lot shall consist of the quantity produced in a single-batch; or when manufactured by a continuous process, a lot shall consist of the total quantity to be offered for acceptance at one time- The number of containers sampled shall be in accordance IV. The containers sam
24、pled shall be selected by a random process. approximately one (1) pint is taken by means of a grain thief or by another appropriate device inserted to the maximum depth at random locations in the container. label each jar with the name, lot number and container number. The primary samples from a lot
25、 shall be grouped and blended to form three composite samples. Each composite sample shall consist of an approximately equal amount of each primary sample from the specified number of primary samples. When a lot consists of less than three containers each container shall be sampled. The sample porti
26、ons thus obtained shall be grouped and blended to fonn three composite samples as follows: From each container to be sampled, a primary sample of Seal each primary sample in a one (1) pint glass jar and If one container is received, three (3) samples are taken, each being treated as a composite samp
27、le. If two containers are received, two (2) samples are taken from one container, one sample is taken from the other container, and each is treated as a composite sample. Blend each composite thoroughly and label with the name, date, lot number and container numbers. of the composite samples represe
28、nting the lot. The average of the test values obtained on the composites shall be used for acceptance purposes. However, if during the sampling or testing it becomes apparent that the lot is not unifonn throughout, the inspector may test any of the primary samples for compliance with the specificati
29、on. Primary samples shall be held for possible future examination, should the composite samples fail to meet the requirements. Ail acceptance-tests shall be made on each 4.4 Acceptance tests. The following acceptance tests as well as any additional test listed in the detail specification shall be pe
30、rformed on each lot. The test results shall be compared with the detail specifi- cation requirements. Any deviation from the specified value shall result in rejection of the lot. supplier shall submit a report giving the results obtained for all inspections performed and a certified statement that t
31、he lot meets all the requirements of this specification. When specified in the contract (see 6.2) , the Unless otherwise specified, all 5 Licensed by Information Handling ServicesMIL- A- 8 2 66 7A (OS) chemicals shall be ACS grade in accordance with MIL-STD-1218. any suitable apparatus. shhil be by
32、titration of a solution of the sample in a 3:l mixture of pyridine and methanol. The surface moisture is determined by titration of a slurry of the solid sample in a solution or liquid medium saturated with ammonium.perchlorate. or electrometrically by means of either a direct or back titration of a
33、 measured excess of KF reagent. with ASTM E 203-75 and the back titration shall be in accordance with AST4 D 1348-61. equivalent of the KF reagent and the precision of the determination shall be in accordance with the detail specification. the KF reagent shall be performed daily in accordance with A
34、STM E 203-75. All the standard precautions must be taken to protect the specimens against change in moisture content and to protect all reagents, solvents and the titration mixture against the entry of water. the stirring action shall be at the highest speed which will not cause splashing or bubble
35、formation. 4.4.1 Moisture. The Karl Fischer (KF) method shall be used with The general procedure for total moisture content The end point may be determined either visually The direct titration shall be in accordance The number of replications, the specimen weight, the water The standardization of Du
36、ring all the titrations, The purity of the ammonium perchlorate shall be determined 4*4*2 by %i?- ion of the sample with sodium carbonate followed by dissolution in nitric acid, adjustment of the pH with sodium bicarbonate and determination of chloride ion by a Mohr or a Volhard titration with silve
37、r nitrate. of solution and quantities of reagents as those used in the determination. A blank titration shall be conducted on the same volumes + Alternatively the perchlorate may be determined by a direct electro- metric titration of chloride ion after sodium carbonate fusion and dissolu- tion in ni
38、tric acid. In the calculation of perchlorate, the equivalent of chloride ion corrections shall be applied for chloride arid chlorate percentages as impurities in the ammonium perchlorate. sodium perchlorate may be made if required by the detail specification. chloride after a determination by a turb
39、idimetric method, a Volhard or a Mohr titration with silver nitrate. determined by a direct potentiometric titration. be conducted on the same volumes of solution and quantities of reagents as those used in the determination. A correction for 4.4.3 Chloride. The chloride content shall be calculated
40、as ammonium Alternatively, chloride may be A blank titration shall 4.4.4 Chlorate. The chlorate content shall be calculated as ammonium chlorate and shall be determined by reduction with ferrous sulfate solution followed by a Mohr titration with silver nitrate. be conducted on the same volumes of so
41、lution and quantities of reagents as those used in the determination. be determined colorimetrically in acid solution using o-tolidine reagent by comparison with a standard chlorate solution. A blank titration shall Alternatively, the chlorate shall 6 Licensed by Information Handling ServicesUIL-A-8
42、2667A 68 7777706 OL23L4b L = MIL-A- 82667A(OS) 4.4.5 Bromate. The brinate content calculated as anunonium broniate shall be detenninea by oxi,dation of iodide to free iodine followed by a thiosulFate titration. same volumes of solution and quantities of reagents as those used in the determination. c
43、alculated as sodium perchlorate shall be determined by sulfuric acid digestion of the sample followed by volatilization of volatile salts and weighing the residue. 4.4.7 Iron. oxide shall betermined on the residue frm the sulfated ash determina- tion. and diluted in a volumetric flask. colorimetrica
44、lly with a standard solution with a hown iron content ushg either potassium permanganate ,and thiocyanate or hydroxylamine and o-phenanthroline for the colorimetric end point. 4.4.8 pH. The pH shall be determined on a saturated solution of the sample dissolved in hot distilled water and reprecipitat
45、ed wing a suitable potentiometer having glass-calomel electrodes. A blank titration shall be conducted on the 4.4.6 Sulfated ash. The sulfated ash weighed as sodium sulfate and The iron content of the sample, calculated as ferric The residue shall be dissolved in concentrated hydrochloric acid The r
46、esulting solution shall be campared 4.4.9 Sodium and potassium. The sodium and potassium content shall be determines by flame photometry. 4.4.10 Phosphate. The phosphate content of the sample shall be determined by comparing the absorbance of the sample solution with a Cali- bration curve of concent
47、ration of a vanadate molybdate complex versus absorbance. 4.4.11 Water insolubles. - A sample of the amqium perchlorate shall be dissolved in distilled water. residue on the filter weighed. distribution shall be determined by one of the following four methods in accordance with the detailed specific
48、ation. The solution shall be filtered and the 4.4.12 Granulation. The average particle size and the particle size a. Particle size shall be determined in accordance with ASIM B Particle size shall be determined in accordance with Particle size shall be determined using a stack of eight-inch The resu
49、lts shall be 330-65. b. MIL-!XD-1234, Method 201.1. (8“) diameter U.S. Standard sieves conforming to ASM E 11-70 shaking with a RO-Top shaker and timing with an automatic timer. reported as cumulative weight percent retained on each sieve. c. . d. The she procedure of c. above shall be used and the results calculated as a umulative weight percent and a weighted average mean diameter. 7 Licensed by Information Handling Services4.4.13 Visual inspection. All samples shall be visuallyiiispected to verify conformance ta the worlananship requirements. 4.4.14 Packaging inspecti
