NAVY MIL-T-82825-1989 TRIPHENYLBISMUTH《三苯基铋》.pdf

1、MIL-T-82825 13 7777706 0230533 O = - I I I INCH-POUND I MIL-T-82825(OS) 29 December 1989 SUPERSEDING WS 20883 8 November 1983 (See 6.7) MILITARY SPECIFICATION TRIPHENYLBISMUTH This specification is approved for use by the Naval Sea Systems Command, Department of the Navy and is available for use by

2、all Departments and Agencies of the Department of Defense. 1. SCOPE 1.1 Scope. This specification defines one grade of triphenylbismuth, referred to herein as triphenylbismuth (TPB) (see 6.1). 2. APPLICABLE DOCUMENTS 2.1 Government documents. 2.1.1 Specifications, standards and handbooks. The follow

3、ing specifica- tions, standards and handbooks form a part of this document to the extent specified herein. Unless otherwise specified, the issues of these documents are those listed in the issue of the Department of Defense Index of Specifications and Standards (DODISS) and supplement thereto, cited

4、 in the solicitation a ;ee 6.2). Beneficial comments (recommendations, additions, deletions) and any pertinent data which may be of use in improving this document should be addressed to: Commanding Officer, Naval Ordnance Station, Standardizatior Branch (3730), Indian Head, MD 20640-5000, by using t

5、he self-addressed Standardization Document Improvement Proposal (DD Form 1426) appearing at the end of this document or by letter. AMSC N/A FSC 1376 DISTRIBUTION STATEMENT A. Approved for public release; distribution is unlimited. Licensed by Information Handling ServicesPlIL-T-2825 13 7979706 02305

6、14 2 W b STANDARDS . FEDERAL FED-STD-313 Material Safety Data, Transportation Data and Disposal Data for Hazardous Materials Furnished to Government Activities MILITARY MIL-STD-129 Marking for Shipment and Storage (Unless otherwise indicated, copies of federal and military specifications, standards

7、and handbooks are available from: Military Specifications and Standards, Bldg. 4D, 700 Robbins Avenue, Philadelphia, PA 19111-5094.) 2.1.2 Other Government documents, drawings, and publications. The following other Government documents, drawings, and publications form a part of this document to the

8、extent specified herein. Unless otherwise specified, the issues are those cited in the solicitation. CODE OF FEDERAL REGULATIONS (CFR) 49 CFR 100-199 Transportation (Application for copies of CFRs should be addressed to the Superintendent of Documents, U. S. Government Printing Office, Washington, D

9、.C. 20402-0001.) 2.2 Non-Government publications. The following documents form a part of this document to the extent specified herein. Unless otherwise specified, the issues of the documents which are DoD adopted are those listed in the issue of the DODISS cited in the solicitation. Unless otherwise

10、 specified, the issues of documents not listed in the DODISS are the issues of the documents cited in the solicitation (see 6.2). AMERICAN TRUCKING ASSOCIATION, INC National Motor Freight Classification (Application for copies should be addressed to the American Trucking Asso- ciation, Inc., Attn: T

11、raffic Dept., 2200 Mill Road, Alexandria, VA 22314-5094.) NATIONAL RAILROAD FREIGHT COMMITTEE Uniform Freight Classification (UFC) 6000 (Application for copies should be addressed to the National Railroad Freight Committee, 222 South Riverside Plaza, Suite 1106, Chicago, IL 60606- 5945. ) 2 Licensed

12、 by Information Handling Services-. P Melting point, degrees Celsius (OC) MIL-T-2825 33 W 7777706 0230535 4 76.0 MIL-T-82825(OS) (Non-Government standards and other publications are normally available from the organizations that prepare or distribute the documents. These documents also may be availa

13、ble in or through libraries or other informational services.) 2.3 Order of precedence. In the event of a conflict between the text of this document and the references cited herein, the text of this document takes precedence. Nothing in this document, however, supersedes applicable laws and regulatio

14、ns unless a specific exemption has been obtained. 3. REQUIREMENTS 3.1 First article. When specified (see 6.2), a sample shall be subjected to first article inspection (see 6.3) in accordance with 4.3. 3.2 Chemical and physical properties. Chemical and physical properties of triphenylbismuth shall co

15、nform to the requirements specified in table I. TABLE I. Chemical and phvsical properties. I I Limits Property I- I Minimum Maximum - - 0.10 O. 003 0.05 3.3 Safety. 3.3.1 Toxic products and formulations. The material shall have no adverse Questions effect on the health of personnel when used for its

16、 intended purpose. pertinent to this effect shall be referred by the contracting activity to the appropriate departmental medical service who will act as an advisor to the contracting agency (see 4.1.2). 3.3.2 Material Safety Data Sheet (MSDS). The contractor shall prepare and submit a MSDS in accor

17、dance with FED-STD-313 as specified in the contract (see 6.2). 3 Licensed by Information Handling Services3.4 Shelf life. The triphenylbismuth shall have a shelf life of 12 months after date of acceptance testing when stored at ambient temperatures and in the absence of ultraviolet light. 3.4.1 Shel

18、f life extension. The shelf life expiration date of an individual lot may be extended for additional 12-month periods provided the triphenylbismuth, upon retest conforms to the purity, melting point, and acetone insoluble requirements. 3.5 Workmanship. The triphenylbismuth shall be uniform in appear

19、ance and free of impurities and foreign matter. 4. QUALITY ASSURANCE PROVISIONS 4.1 Responsibility for inspection. Unless otherwise specified in the contract or purchase order, the contractor is responsible for the performance of all inspection requirements (examinations and tests) specified herein.

20、 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 the right to perform any of the inspect

21、ions set forth in the specification where such inspections are deemed necessary to ensure supplies and services conform to prescribed requirements. 4.1.1 Responsibility for compliance. All items shall meet all require- ments of sections 3 and 5. become a part of the contractors overall inspection sy

22、stem or quality program. The absence of any inspection requirements in the specification shall not relieve the contractor of the responsibility of ensuring that all products or supplies submitted to the Government for acceptance comply with all requirements of the contract. Sampling inspection, as p

23、art of manufacturing operations, is an acceptable practice to ascertain conformance to requirements, however, this does not authorize submission of known defective material, either indicated or actual, nor does it commit the Government to accept defective material. The inspection set forth in this s

24、pecification shall 4.1.2 Toxicological product formulations. The contractor shall have the toxicological product formulations and associated information available for review by the contracting activity to evaluate the safety of the material for the proposed use, 4.2 Classification of inspections. Th

25、e inspection 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 inspection. First article inspection shall consist of the quality conformance inspections (see 4.4). requirements specified here

26、in shall be cause for rejection of the first article sample. Failure to meet all of the 4 a a e Licensed by Information Handling ServicesMIL-T-82825 13 777770b 0230537 W 4.4 Quality conformance inspection. Quality conformance inspection shall consist of the examination and tests specified in table I

27、I. TABLE II. First article and quality conformance inspections. Examination and tests Visual examination Purity test Melting point test Acetone insoluble matter test Magnesium test Total halides test Requirement 3.5 and Section 5 3.2 3.2 3.2 3.2 3.2 Test method 4.5.1 4.5.2 4.5.3 4.5.4 4.5.5 4.5.6 4.

28、4.1 Sampling for inspection. 4.4.1.1 Lot. For inspection purposes, a lot shall consist of all of the triphenylbismuth subject to inspection at one time from one or more batches or a homogeneous blend of all batches of triphenylbismuth manufactured using the same set of materials and processing opera

29、tions and conditions and submitted for acceptance at one time. If all the batches in the lot were mixed to make a homogeneous blend, the lot shall be considered to consist of one batch for purpose of sampling and testing. 4.4.1.2 Selection of sample containers. Sample containers of the Sample materi

30、al shall be selected as triphenylbismuth shall be selected at random from each lot for the inspections specified in 4.5.1 through 4.5.6. specified in 4.4.1.3. minimum sample selected at random from each batch (see 6.5.1). The batch samples shall not be blended. and test results shall be recorded for

31、 each batch. Sampling to determine conformance to section 5 shall consist of all the containers in the lot. Sampling for tests shall consist of one 50-gram (g) All the tests shall be performed on each sample, 4.4.1.3 Sample material. Sufficient material shall be selected at random from each sample c

32、ontainer to perform all the inspections specified in 4.5.1 through 4.5.6. 4.4.1.4 Noncompliance of samples. Failure of one or more of the sample containers of material to meet all of the specified requirements shall be cause for rejection of the lot. 5 Licensed by Information Handling Services4.5 Me

33、thods of inspection. The following inspection methods shall be used, Unless otherwise specified in the method, all weights, volumes, temperatures, and times shall be measured to the nearest specified unit or decimal. NOTE: Reagent grade chemicals shall be used for chemical reactions in the conduct o

34、f all tests defined herein. Solvents and indicators may be commercial nonreagent grade materials. 4.5.1 Visual examination. Each sample of material shall be visually examined to determine conformance to 3.5. 4.5.2 Purity test. The purity of triphenylbismuth shall be determined as follows : 4.5.2.1 a

35、. b. 4.5.2.2 a. b. C. d. e. f. 4.5.2.3 a. Apparatus. Liquid chromatograph equipped as follows: (1) Detector. Ultraviolet (W) variable wave-length with LC flow-thru assembly. (2) Column C18. Bonded reversed phase, 5-10 micrometers. (3) Pump. Capable of operating up to 4000 psi pressure. Laboratory gl

36、assware. Reagents and standards. Triphenylbismuth. absorbance, Triphenylmethane. Reagent grade. Recrystallized from heptane to maximum Water. High pressure liquid chromatography (HPLC) grade. Methanol. HPLC grade. Acetone. W grade. Acetonitrile. HPLC grade. Procedure. Prepare a stock solution of int

37、ernal standard triphenylmethane (TPM) by weighing 0.5 & 0.1-g of TPM in a 100-milliliter (mi) volumetric flask and diluting to the mark with 50 ml acetone and 50 ml acetonitrile. 6 Licensed by Information Handling Servicesb. Weigh 0.5 5 0.1 g of TPB sample to be analyzed to the nearest 0.1 milligram

38、 (mg) in each of three 100-ml volumetric flasks and dilute to the mark with 50 ml acetone and 50 ml acetonitrile. c. Weigh 0.5 5 0.1 g of TPB standard to the nearest 0.1 mg in each of two 100 ml volumetric flasks and dilute to the mark with 50 ml acetone and 50 ml acetonitrile. d. Accurately transfe

39、r a 1.0-ml aliquot from each of the 100-ml flasks into five separate 25-1111 volumetric flasks. e. Accurately pipette 1.0 ml of the TPM internal standard stock solution in each of the five 25-1111 flasks. Dilute to the mark with 50:50 acetone and acetonitrile. f. Analyze the three samples and two st

40、andard solutions using a liquid chromatograph. been found satisfactory in this analysis. The following instrument parameters have (1) Detector. UV variable wavelength, such as Varian UV 50, set at 226 nanometers, (2) Eluent. 80 percent methanol - 20 percent water. (3) Flow rate. Approximately 2.0 ml

41、/minute (4) Injection volume. Use the same injection volume for sample and standard solutions. Adjustment of these parameters may be necessary to provide proper peak separation and quantification, g. Determine the areas under both TPM and TPB peaks for each sample and standard. h. The internal stand

42、ard corrected response factors for the standards should agree within 2 parts per hundred. If not, repeat the test. Calculate the average response factor: Average response factor (R) = 1/2 W1(I,/A1) + W2(12/A2) Where A = area of standard TPB peak. W = standard concentration, mg/ml. I = area of standa

43、rd TPM peak. 1 = standard 1 I1/A, 2 = standard 2 IJA2 7 Licensed by Information Handling Servicesi. 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 TPB peak. Is = area of sample TPM peak. C = sample co

44、ncentration, mg/ml. j. Record TPB as the average of three determinations, to the nearest 0.1 percent. 4.5.3 Melting point test. The melting point of the triphenylbismuth shall be determined as follows: 4.5.3.1 Apparatus. a. Capillary melting point apparatus - Electro-thermal, Mettler, Vanderkamp, or

45、 similar apparatus. b. Rheostat control. c. Capillary tubes - approximately 3 inches long. d. Thermometer - covering desired range with 0.2% or smaller subdivision. 4.5.3.2 Procedure. a. Reduce the sample to a very fine powder, and desiccate for 4 hours. b. Completely seal one end of a capillary tub

46、e. Charge the tube by taking a watch glass covered with test material and pressing the open end of the tube against the watch glass. c. Closely pack the material in the bottom of the capillary to a depth of 3.0 f. 0.6-mm by repeatedly dropping the capillary inside a 12-inch length of 1/4-inch OD gla

47、ss tubing which is held vertically with the lower end about 1 inch above the table top. d. Set up the Vanderkamp melting point apparatus near a standard electrical outlet with two receptacles. directly, and connect the heater through the rheostat control. Plug in the light cord 8 Licensed by Informa

48、tion Handling Servicesc -. MIL-T-8225 13 m 7777706 0230523 T m e. Inset a thermometer into the hole of the top center of the Vanderkamp apparatus, and lower the thermometer all the way in. Lower one capillary tube into one of the small holes near the thermometer hole. f. Heat until 25% below the exp

49、ected melting temperature, then carefully regulate the rate of temperature rise by means of the rheostat to about 3OC per minute until the material begins to melt. collapse definitely against the sides of the tube at any point.) From this time, carefully regulate the temperature rise to 1/2 degree/minute until the material becomes liquid throughout. (This is the temperature at which the sample is observed to g. h. Record the temperature at which the material completely melts as the melting point. 4.5.4 Acetone insoluble matter test. Acetone insoluble matter shall be determ