ARMY MIL-T-70681-1988 TRIPHENYL BISMUTH《三苯基铋》.pdf

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1、i Beneficial comments (recommendations, additions, deletions) and any pertinvnt date which may be of use in Improving this document should be addressed to: Commander, U.S. Army Armament,Munitions and Chemical Command, Ath. AMSMC-QA, Picatinny Arsenal, New Jersey 07806-5000 by using the self-addresse

2、d Stendardim- tion Document Improvement Proposai (DD Form 1426) appearing al the end of this document or by letter. - . Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-_-_ _I_ MIL-T-7068L h 777770b O322548 5 MIL-T-70681 (AR) MIL-STD-129 MIL-STD-1168

3、MIL-STD-1218 - ACS Chemicals - Marking For Shipment and Storage - Lot Numbering of Ammunition (Copies of specifications, standards, handbooks, drawings, publications, and Government documents required by contractors in connection with specific acquisition functions should be obtained from the contra

4、cting activity or as directed by the contracting act i vi ty . ) 2.1.2 ublications. Other Government documents, drawings, and End publications form a part of this specification to the extent specified herein. those in effect on the date of the solicitation. The following other Government documents,

5、drawings, Unless otherwise specified, the issues shall be CODE OF FEDERAL REGULATIONS Title 49, Transportation, Parts 100-199 (Application for copies should be addressed to the Superintendent of Documents, Government Printing Off ice, cite: 49 CFR 100-199 (latest revision). 2.2 Other publications. T

6、he following document(s) form a 2art of this specification to the extent specified herein. Unless otherwise specified, the issue of the documents which are DOD adopted shall be those listed in the issue of the DODISS specified in the solicitation. documents not listed in the DODISS shall be the issu

7、e of the nongovernment documents which is current on the date of the solici tat ion. . Washington, D.C. 20402. Order for the above publication should Unless otherwise specified, the issues of AMERICAN SOCIETY FOR TESTING AND MATERIALS (ASTM) ASTM E168 ASTM E300-73 - Recommended Practices for General

8、 Techniques - Recommended Practice for Sampling Industrial in Infrared Quantitative Analysis Chem i ca Is (Application for copies should be addressed to the American Society For Testing and Materials, 1916 Race Street, Philadelphia, PA 19103.) 2 Provided by IHSNot for ResaleNo reproduction or networ

9、king permitted without license from IHS-,-,-a 3 i MIL-T-70b3 68 W 999770b 0322547 7 W MIL-T-70681 (AR) UNITED NATIONS United Nations - Transport of Dangerous Goods (Recommendations of the Committee of Experts on the Transport of Dangerous Goods) (Applications or copies should be addressed to United

10、Nations, Sales Section, First Ave., New York, N.Y.) 2.3 Order of precedence. In the event of a conflict between the text of this specification and the references cited herein (except for assoicated detail specifications, specification sheets or MS standards), the text of this specification shall tak

11、e precedence. Nothing in this specification, however, shall supersede applicable laws and regulations unless a specific exemption has been obtained. 3. REQUIRElrlENTS 3.1 Material. The Triphenyl Bismuth shall conform to the following requirements when tested in accordance with the applicable test me

12、thod. Property Applicable Nax Test Method - Min - Pur i ty 97.0 - 4.5.1 Melting Point, OC 76. O 78.5 4.5.2 Acetone Insolubles, % - 0.1 4.5.3 Magnesium Content, % - O. 003 4.5.4 Total Halide Content,% - 0.05 4.5.5 3.2 Infrared spectrum. The IR spectrum of the sample shall contain the maior peaks show

13、n in Figure 1 when tested in accordance with 4.5.6. 3.3 First article inspection. This specification contains technical provisions for first article inspection. Requirements for the submission of first article samples by the contractor shall be as specified in the contract. 3.4 Workmanshie. The manu

14、facturer- shall implement procedures and controls to assure that the process and the product produced are not compromised by foreign materials and contaminants or any other conditions which may degrade the composition. Determination of foreign materials shall be in accordance with 4.5.7. 4. QUALITY

15、ASSURANCE PROVISIONS 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-7 O 6 81 (AR) 4.1 Responsibility for inspection. Unless otherwise specified in the contract or purchase order, the contractor is responsible for the performance of all inspe

16、ction 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 Government. The Government reserves

17、the right to perform any of the inspections set forth in the specification where such inspection are deemed necessary to assure supplies and services conform to prescribed requirements. 4.1.1 Responsibility for compliance. All items must meet all requirements of sections 3 and 5. The inspection set

18、forth in this specification shall become a part of the contractors overall inspection system or quality program. The absence of any inspection requirements in the specification shall not relieve the contractor of the responsibility of assuring that all products or supplies submitted to the Governmen

19、t for acceptance comply with all requirements of the contract. Sampling in quality conformance does not authorize submission of known defective material, either indicated or actual, nor does it commit the Government to acceptance of defective material. 4.2 Classification of inspections. The inspecti

20、on requirements specified herein are classified as follows: a. First article inspection (see 4.3). b. Quality conformance inspection (see 4.4) 4.3 First article insuection. 4.3.1 Submission. The contractor shall submit a first article sample as designated by the Contracting Officer for evaluation in

21、 accordance with provisions of 4.3.2. The first article sam2le shall be ten (10) pounds of triphenyl bismuth. 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 fulfilli

22、ng the contract. All materials shall be obtained from the same sources of supply as will be used in.regular production. 4.3.2 Inspection to be performed. The sample will be subjected by the Government to any or all of the examinations or tests specified in Table II (MIL-A-48078). 4 Provided by IHSNo

23、t for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-70683 68 7777706 0322553 5 W *. . O rJ O O m w m I G O li U (d k U U V G g u i rl d Q) PI I . . MIL-T-70681 (AR) , _. :, , . :. . ._ 8. .;. . .- - . . .- . . 5 :.: . . . _. . ,I. . . ._ ,- rl B I U Provided by IHS

24、Not for ResaleNo reproduction or networking permitted without license from IHS-,-,-_-_ MIL-T-70bL b 7797706 0322552 7 MIL-T-70681 (AR) 4.3.3 Rejection. See MIL-A-48078. 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-c O ci u vi c .d a, fi u .d ci

25、LI rd .d E H H NIL-T-7068L 68 W 7777706 0322553 7 7 L O LL Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-70bl b m 774770b 0322554 O a MIL-T-70681 (AR) 4.4 QuaLitymance inspection. 4.4.1 Lot formation. A lot shall consist of one or more batche

26、s of triphenyl bismuth produced by one manufacturer, in accordance with the same specification, or same specification revision, under one continuous set of operating conditions. Each lot shall consist of that quantity of triphenyl bismuth that has been subjected to the same unit chemical or physical

27、. process intended to make the final product homogeneous. The lot shall comply with the provisions for submission 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 Examinati

28、on. See MIL-A-48078. a. Workmanship. Examination for workmanship shall be conducted on each sample selected 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 co

29、vers sampling and testing of toxic and hazardous materials. Accordingly, it is emphasized that all applicable 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

30、 each batch to be sampled using ASTM Method E300-73 for solids. Samples shall be selected for inspection 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 comp

31、osite samples shall be used. The classification of defects shall be as given in Table III. Number of containers in batch Number of containers to be sampled 2- 100 2 100 - 200 5 200 - 300 8 300 - 500 10 500 - 1000 13 1000 - 3000 20 3000 - 10,000 32 8 Provided by IHSNot for ResaleNo reproduction or ne

32、tworking permitted without license from IHS-,-,-MIL-T-70683 68 9977706 0322555 2 6 MIL-T-70681 (AR) TABLE III. Classification of Defects Defects Test Examination Paragraph Classification Pur i ty Melting Point Acetone Insolubles Magnesium Content Total Halide Content Infrared Spectrum Workmanship 3.

33、1 3.1 3.1 3.1 3.1 3.2 3.4 Major Major Major Major Major Major Major 4.4.4 Inspection equipment. For the performance of all tests and examinations specified in 4.4 and 4.5, commercial inspection equipment should be employed. The contractor shall have available and utilize correctly, this equipment an

34、d 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 prescribed procedures for replicate determinations given in standard analytical chemistry textbooks. Also, unless othe

35、rwise 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 Purity. The purity of triphenyl bismuth shall be determined as follows: 4.5.1.1 Apparatus a. Liquid Chromatograph equipped as follows: (1) Dete

36、ctor Ultraviolet (UV) variable wavelength with LC flow- through assembly (2) Column C18 bonded reversed phase, 5-10 micrometers, 30 cm in length (3) Pump Capable of operating up to 4000 psi pressure b. Laboratory glassware 9 a Provided by IHSNot for ResaleNo reproduction or networking permitted with

37、out license from IHS-,-,-MIL-T-70bL b W 774970b OL2255b 4 MIL-T-70681 (AR) 4.5.1.2 a. b. C. d. e. f. 4.5.1.3 Reagents and standards. Triphenyl Bismuth Recrystallized from heptane Triphenylmethane Reagent grade to maximum absorbance Water Methanol Acetone Acetonitrile Procedur es. High pressure liqui

38、d chromatography (HPLC) grade HPLC grade UV grade HPLC grade a. Prepare a stock solution of internal standard triphenylmethane (TPM) by weighing approximately 0.5 g TPM into a 100-millileter (mi) volumetric flask and diluting to the mark with 50 ml acetone and 50 ml acetonitrile. b. Weigh 0.5 g of T

39、PB sample to be analyzed to the nearest 0.1 milligram (mg) into each of three volumetric flasks. nearest 0.1 mg into each of two 100-ml volumetric flasks. ml of the internal standard stock solution. the mark with acetonitrile. c. Weigh approximately 0.5 g of TPB standard to the d. Accurately pipette

40、 into each of the five flasks 1.0 Dilute the flasks to e. Analyze the three samples and two standard solutions using liquid chromatograph instrument conditions as follows: (i) Detector - Set at lowest wavelength below 226 mm at which a stable baseline can be obtained. (2) (3) Flow Rate - Approximate

41、ly 2.0 ml/minute. Eluent - 80 percent methanol - 20 percent water. (4) Injection - Use the same injection volume for sam;?le and standard solutions. 10 .- Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- flIL-T-706L 68 7797706 0122557 b = MIL-T-70 68

42、1 (AR) f. Determine the areas under both TPN and TPB peaks for each sample and standard. the standards should agree within 2 parts per hundred. If not, repeat the test. Calculate the average response factor: g. The internal standard corrected response factors for Average response factor (R) = w1 (11

43、/A1) + w2 (I2/A2) Where A = area of standard TPB peak, W = standard concentration, mg/ml I = area of standard TPM peak 1 = standard 1 2 = standard 2 h. Calculate the percent TPB in each sample as follows: Percent TPB = R x B x 100 c x Is Where: R = response factor defined above B = area of sample TP

44、B peak Is = area of sample TPM peak C = sample concentration, mg/ml i. Report TPB to nearest 0.1 percent. 4.5.2 Melting po int. The melting point shall be determined as follows: 4.5.2.1 Apparatus. a. Fisher-Johns melting point apparatus. b. Optical cover glass. 4.5.2.2 Procedure. a. Press a small qu

45、antity of the sample between two optical cover glasses. Place the glasses (with sample) on the heating block of a Fisher-Johns melting point apparatus. b. Set the temperature control at 30“. 11 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-flIL-T-7

46、0bL b m 7777906 0122558 m MIL-T-70681 (AR) c. Observe the sample through the small magnifying glass provided with the equipment . d. When the sample is seen to soften (begin to melt) note the temperature and record to the nearest 0.lOC. e. Continue observing the sample until al1 solid has turned to

47、liquid. Again note the temperature and record to the nearest 0.lOC. f. Report the two temperatures described above as the melting range. 4.5.3 Acetone insolubles. Acetone insoluble matter shall be 4.5.3.1 Apparatus. determined as follows: a. 250 ml beaker b. Gooch crucible, 40 ml capacity c. Glass f

48、iber filter, Reeve Angel 934 AH or equivalent, d. Oven, gravity convection, regulated at 100 + 2% 2.4 cm - 4.5.3.2 Procedure. a. Weigh to the nearest mg, approximately 5 grams (9) of sample into a 250 ml beaker and dissolve in 200 ml of acetone. b. Filter the solution through a tared Gooch crucible

49、containing the giass fiber filter, rinsing out the beaker with acetone and passing the rinsings through the crucible. the washings are colorless. % c. Wash the residue in the crucible with acetone until d. Dry the crucible at loo0 - + 2oC for one hour, cool in a desiccator; and weigh. - e. Calculate the acetone insoluble matter as fo