ARMY MIL-F-70676-1988 FERRIC ACETYLACETONATE《乙酰丙酮铁》.pdf

1、f s-379 MIL-F-70676 68 m 7977906 0322536 7 m I MIL-F-70676 (AR) 29 June 1988 MILITARY SPECIFICATION FERRIC ACETYLACETONATE 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

2、Defense. 1. SCOPE 1.1. Scope. This specification covers the requirements and quality assurance provisions for the manufacture and acceptance of one type of ferric acetylacetonate (see 6.1). 2. APPLICABLE DOCUMENTS 2.1. Government documents. 2.1.1 Specifications and standards. The following specifica

3、tions and standards form a part of this specification to the extent specified herein. Unless otherwise specified, the issues of these documents shall be those listed in the issue of the Department of Defense Index of Specifications and Standards (DODISS) and supplement thereto, cited in the solicita

4、tion. SPECIFICATIONS MIL I TARY MIL-A-48078 - Ammunition, Standard Quality Assurance Provisions, General Specification for STANDARDS MILITARY MIL-STD-10.5 - Sampling Procedures and Tables for Inspection by Attributes Beneficial comments (recommendations, additions, deletions) and any pertinent data

5、which may be of use in improving this document should be addressed to: Commander, U.S. Army Armament,Munitions and Chemical Command, Attn. AMSMC-QA. Picatinny Arsenal, New Jersey 07806-5000 by using the self-addressed Standardiza- tion Document Improvement Proposal (DD Form 1426) appearing at the en

6、d of this document or by letter. FSC 6810 AMSC N/A DISTRIBUTION STATEMENT A. Approved for public release; distribution is unlimited. , THIS DOCUMENT CONTAINS / PAGES. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- -.- _-_ MIL-F-70676 68 W 7777906 0

7、322537 O W MIL-F-70676 (AR) MIL-STD-129 - Marking for Storage and Shipment MIL-STD-286 - Propellants, Solid: Sampling, MIL-STD-1168 - Lot Numbering of Ammunition MIL-STD-1218 - ACS Chemicals Examination and Testing (Copies of specifications, standards, handbooks, drawings, publications, and other Go

8、vernment documents required by contractors in connection with specific acquisition functions should be obtained from the contracting activity or as directed by the contracting activity.) 2.1.2 Other government documents, drawings - and p.- publications. I- The following other goverment documents, dr

9、awings, and publications form a part of this specification to the extent specified herein. Unless specified, the issues shall be those in effect on the date of the solicitation. CODE OF FEDERAL REGULATIONS Title 49, Transportation, Parts 100-199 (Application for copies should be addressed to the Sup

10、erintendent of Documents, Government Printing Office, Washington, D.C. 20402. Orders for the above publication should cite: 49 CFR 100-199 (latest revision.) . 2.2 Other publications. The following documents form a part of this specification. to the extent specified herein. Unless otherwise specifie

11、d, the issues of the documents which are DOD adopted shall be those listed in the issue of the DODISS shall be the issue of the nongovernment documents which is current on the date of the solicitation. AMERICAN SOCIETY FOR TESTING AND MATERIALS (ASTM) ASTM E300-73 - Recommended Practice for Sampling

12、 Industrial Chemicals (Application for copies should be addressed to the American Society For Testing and Materials, 1916 Race Street, Philadelphia, PA 19103.) UNTIED NATIONS United Nations - Transport of Dangerous Goods (Recommendations of the Committee of Expert on the Transport of Dangerous Goods

13、.) Sales Section, First Ave., New York, N.Y.) (Application for copies should be addressed to United Nations, 2 0 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-F-70676 68 m 7797706 0122538 2 m 0 a ! MIL-F-70676 (AR) 2.3 Order of precedence. In t

14、he event of a conflict between the text of this specification and the references cited herein (exce-t for associated detall specificati-ons, specification sheets or YS standards), the text of this specilicat.ion shall- take precedence. Nothing in this specification, however, shall. supersede applica

15、ble laws and regulations unless a specific exemption has been obtained. 3. REQUIREMENTS 3.1 Material. The ferric acetylacetonate shall conform to the following requirements when tested in accordance with the applicable test method. ProEer ty Iron Content, % - App 1 i cab le Min - Max Test Method 14.

16、4 16.2 4.5.1 Methylene Chloride Insolubles,% - 1.0 4.5.2 Moisture, % - 0.5 4.5.3 3.2 Color. The ferric acetylacetonate shall be an orange- red crystalline solid, when tested in accordance with 4.5.4. 3.3 First article inspection. This specification contains techinical provisions for first article in

17、spection. Requirements for the submission of first article samples by the contractor shall be as specified in the contract. 3.4 Workmanship. The manufacturer shall implement procedures and controls to assure that the process and the product produced are not compromised by foreign materials and conta

18、minants or any other conditions which may degrade the composition. Determination of foreign materials shall be in accordance with 4.5.5. 4. QUALITY ASSURANCE PROVISIONS 4.1 Responsibility for inspection. Unless otherwise specified in the contract or purchase order, the contractor is responsible for

19、the performance of all inspection requirements as specified herein. Except as otherwise specified in the contract or purchase order, the contractor may use his own or any other facilities suitable for the performance of the inspection requirements specified herein, unless disapproved by the Governme

20、nt. 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 prescribed requirements. 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without licens

21、e from IHS-,-,- MIL-F-70676 68 7777906 0322539 4 MIL-F- 706 7 6 (AR) 4.1.1 Responsibility for compliance. All items must meet all requirements of sections 3 and 5. The inspection set forth in this specification shall- become a part of the contractors overall inspection system or quality program. The

22、 absence of any inspection requirements in the specification shall not relieve the contractor of the responsibility of assuring that al1 products or supplies submitted to the Government for acceptance comply with al.1 requirements of the contract. Sampling in quality conformance does not authorize s

23、ubmission of known defective material, either indicated or actual, nor does j-t commit the Government to acceptance of defective material. 4.2 Classification of inspections. The inspection requirements specified herein are classified as follows: a. First article inspection (see 4.3). b. Quality conf

24、ormance inspection (see 4.4). 4.3 First article inspection. 4.3.1 Submission. The contrator shall submit a first article sample as designated by the Contracting Officer for evaluation in accordance with provisions of 4.3.2. The first article sample shall be ten (10) pounds of ferric acetylacetonate.

25、 The sample shall be obtained from the first production lot which has been produced by the contractor using the same production processes, procedures and equipment as will be used in fulfilling the contract. AI.1 meterials shall be obtained from the same sources of supply as wil.1 be used in regular

26、 production. subjected by the Government to any or all of the examinations or tests specified in Table II (see MIL-A-48078). 4.3.2 Inspection to be performed. The sample will be 4.3.3 Rejection. See MIL-A-48078. 4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license f

27、rom IHS-,-,-c O ci u a, rn C .FI a, rl u .FI ci L-4 a 4-J rn $4 -I- Eri .rl e H H 2 5 EQ MIL-F-70676 68 W 7779706 0322540 O = I l q I 5 u! fd- 2: SB! W is: a 2 0 W D I L u =I u a Yf rn a, rl a !3 rl O rn c H a, ru -rl 8 rl cis CU a, 5 Provided by IHSNot for ResaleNo reproduction or networking permit

28、ted without license from IHS-,-,- s- HIL-F-70b7b b M 7777906 O122541 2 MIL-F-70676 (AR) 4.4 Quality conformance inspection. 4.4.1 Lot formation. A lot shall consist of one or more batches of ferric acetylacetonate produced by one manufacturer, in accordance with the same specification, or same speci

29、fication revisj.on, under one continuous set of operating conditions. Each lot shalt consist of that quantity of ferric acetylacetonate that has been subjected to the same unit chemical or physical process intended to make the final product homogeneous. The lot shall comply with the provisions for s

30、ubmission of product as specified in MIL-STD-105. The criteria and procedure for the assignment of lot numbers shall be in accordance with MIL-STD-1168. Also, MIL-A-48078 applies. 4.4.2 Examination. See MIL-A-48078. a. Workmanship. Examination for workmanship shall be conducted on each sample select

31、ed for testing in accordance with 4.4.3.1. If .any sample fails to meet any test requirement the batch represented by the sample shall be rejected. 4.4.3 Testing. PRECAUTION: This specification covers sampling and testing of toxic and hazardous materials. Accordingly, it is emphasized that all appli

32、cable safety rules, regulations and procedures must be followed in handling and processing the triphenyl bismuth. 4.4.3.1 Sampling. Approximately 500 grams of the composition shall be selected from each batch to be sampled using ASTM Method E300-73 for solids. Samples shall be selected for inspectio

33、n in accordance with table below. If any sample fails to meet any test requirement the batch represented by the sample shall be rejected. Each required test shall be performed in duplicate. No composite samples shall be used. shall be as given in Table III. The classification of defects Number of co

34、ntainers in batch 2- 100 100 - 200 200 - 300 300 - 50 5G0 - 1000 1000 - 3000 3000 - 10,000 Number of containers to be sampled 2 5 8 10 13 20 32 6 i Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-F-70676 (AR) TABLE III. Classification of defects

35、Test Examination . Defects Paragraph Classif icat%on Iron Content. 3.1 Methylene Chloride Insolubles 3.1 Mo ist ur e 3.1 Color 3.2 Wor kmanship 3.4 Major Major Major Major Major 4.4.4 Inspection equipment. For the performance of all tests The contractor shall have available and examinations specifie

36、d in 4.4 and 4.5, commercial inspection equipment should be employed. and utilize correctly, this equipment and is charged with the responsibility of assuring that proper calibration procedures are followed. 4.5 Methods of inspection . All tests given in this section shall be performed using prescri

37、bed procedures for replicate determinations given in standard analytical chemistry textbooks. Also, unless otherwise specified herein, all chemicals shall be Reagent Grade or ACS Grade in accordance with MIL-STD-1218. See 6.3 for use of equivalent test methods. 4.5.1 Iron content. The.iron content o

38、f ferric 4.5.1.1 Method. Organic matter is first removed by treatment acetylacetonate shall be determined as follows: with sulfuric and nitric acids. stannous chloride solution and titrated with standard potassium di.chromate solution to the diphenylamine sulfonate end point. The iron is then reduce

39、d with 4.5.1.2 Apparatus. a. Erlenmeyer flask; 300ml b. Buret; 50ml c. Graduated cylinder 4.5.1.3 Reagents. a. Phosphoric acid; reagent grade, 85% b. Sulfuric acid; reagent grade c. Nitric acid; reagent grade 7 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from

40、 IHS-,-,- . MIL-F-70676 68 m 779970b 0122543 6 MIL-F-7 O 67 6 (AR) d. Hydrochloric acid; reagent grade e. Stannous chloride solution; 60g stannous chloride dissolved in 50ml of hydrochloric acid - dilute to 1 liter with water. f. Mercuric chloride solution; 5g mercuric chloride/ 700ml water. g. Pota

41、ssium dichromate solution; 0.1N prepare as primary standard from oven dried crystal (4.9032g/ liter water) h. Diphenylamine indicator; 0.2 sodium diphenylamine sulfonate/ 100ml water 4.5.1.4 Procedure. a. b. C. d. e. f. 9- h. Accurately weigh a lg sample into a 300ml flask. Carefully add 10ml of sul

42、furic acid and 5ml of nitric acid. Heat until heavy white fumes of SO3 are evolved. Cool slightly and very carefully repeat the nitric acid addition. Again heat until heavy white fumes are evolved. Repeat the nitric acid addition and heating cycle until all the organic matter has been removed. . The

43、 solution should be nearly colorless (white salts of ferric sulfate may form). No brown color should be visible. Before continuing remove any residual nitric acid by heating strongly until heavy white fumes are evolved. Cool to nearly room temperature and add 100ml of water and 5ml of hydrochloric a

44、cid. Heat to near boiling to dissolve any precipitate that may have formed. While the solution is still hot, add stannous chloride solution dropwise to discharge the yellow color. Add 1-2 drops excess. The sample solution should now be colorless. Cool to. room temperature, and quickly add with stirr

45、ing .Om1 pf mercuric chloride solution. A small amount of white precipiBate should form. (No precipitate formation indicates that an insufficient amount of stannous chloride was used. Formation of a grayish precipitate indicates too large an excess of stannous chloride was used. In either case, the

46、sample should be discarded.) Add 15ml of phosphoric acid and 5-10 drops of diphenylamine sulfonate indicator. 0.1N potassium dichromate to the violet endpoint. Titrate with standard 8 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-F-70676 68 m 7

47、777706 0122544 B m MIL-F-70676 (AR) x O * 4.5.1.5 Calculations. ml Ky3207 x N K2Cr207 x 5.585 = % Fe sample weight (9) 4.5.2 Methylene chloride insolubles. The methylene chloride insolubles shall be determined as follows: 4.5.2.1 Apparatus. a. Beaker; 150ml b. Gooch crucible; medium frit c. Filter F

48、lask and vacuum system d. Oven capable of maintaining looo to 105OC 4.5.2.2 Reagents. Methylene chloride 4.5.2.3 Procedure. a. Accurately weigh two grams of sample in a 150ml beaker. b. Add 100ml of methylene chloride and mix without heating. c. Filter thru a tared medium porosity pyrex crucible (dr

49、ied at 105OC for 1 hour, cooled in desiccator and weighed), using suction. d. Rinse beaker with four 20ml aliquets of methylene chloride, pour washes into crucible. Aspirate for 10 minutes to air dry the residue. e. Place the crucible and contents in a 105OC oven for one hour. f. Cool. in a desiccator and weigh. 9. Calculate the percent insoluble material as follows: (weight of residue, 9) (100) = ins