NAVY DOD-T-82666 A-1978 TRIS-1-(2 METHYL AZIRIDINYL) PHOSPHINE OXIDE《-1-(2-甲基氮丙啶)氧化膦》.pdf

1、DOD-T-82bbbA 68 7797906 OL23L27 8 6 November 1978 Superseding (see 6.3) MILITARY SPECIFICATION TRIS-1-( 2-METHYL AZIRIDINYL) PHOSPHINE OXIDE This specification is approved for use by all Departments and Agencies of the Department of Defense. 1. SCOPE 1.1 Scope. This specification covers the requirem

2、ents for 3 1.2 Classification. The tris-l-(2-methyl aziridinyl) phosphine grades of tris-l-(2-methyl aziridinyl) phosphine oxide. oxide shall be of the following grades as specified in the contract (see 6.2): Grade A - Distilled Grade B - High Purity Grade C - Crude 2. APPLICABLE DOCUMENTS 2.1 Issue

3、s of documents. The following documents of the issue in effect on date of invitation for bids or request for proposal, form a part of this specification to the extent specified herein. STANDARDS . FEDERAL FED-STD-313 Material Safety Data Sheets, Preparation and the submission of MI LI TARY MIL-STD-1

4、29 MIL-STD-414 Marking for Shipping and Storage Sampling Procedures and Tab1 es for Inspection by Variables for Percent Defective MIL-STD-1218 ACS Chemicals * Beneficial comments (recomendation, additions, deletions) and any pertinent data which may be of use in improving this document should be add

5、ressed to: ization Division (611), Indian Head, Maryland 20640 by using the self-addressed Standardization Document Improvement Proposal (DD Form 1426) appearing at the end of this document or by letter. Commanding Officer, Naval Ordnance Station, Standard- IFSC 68101 THIS DOCUMENT CONTAINS - 12 PAG

6、ES. - i ?, Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-DOD-T-82bbbA b8 W 7777706 O123128 T W DOD-T-82666A PUBL I CAT IONS NAVAL SEA SYSTEMS COMMAND (Code Ident. 10001) OD 18893 Water Content, Determination of (Copies of specifications, standards,

7、 drawings, and pub1 ications required by suppliers in connection with specific procurement functions should be obtained from the procuring activity or as directed by the contracting officer. ) this specification to the extent specified herein. indicated, the issue in effect on the date of the invita

8、tion for bids or the request for proposal shall apply. * 2.2 Other publications. The following documents form a part of Unless otherwise AMERICAN NATIONAL STANDARDS INSTITUTE (ANSI) ANSI Z 129.1-1976 Precautionary Labeling of Hazardous Industrial Chemicals (Application for copies should be addressed

9、 to the American National Standards Institute, 1430 Broadway, New York, NY 10018.) CODE OF FEDERAL REGULATIONS 49 CFR 100-199 Transportation (The Code of Federal Regulations is available from the Superintendent of Documents, US Government Printing Office, Washington, DC 20402. Orders should specify

10、“49 CFR 100-199 (latest revision)“.) are generally available for reference from libraries. distributed among technical groups and using Federal agencies.) 3. REQUIREMENTS (Technical society and technical association specifications and standards They are also 3.1 Chemical properties. The chemical pro

11、perties shall conform to Table I. * TABLE I. Chemical properties. 2 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-DOD-T-82666A 68 m 9999906 0123129 1 m DOD-T-82666A * 3.2 Material safety data sheets. The contractor shall prepare and submit material

12、 safety data sheets in accordance with FED-STD-313 as specified in the contract (see 6.8). material shall make no changes in processing techniques or other factors affecting the quality of the product without prior approval of the procuring activity. contamination, foreign material or any other defe

13、ct that would prevent its use for the purpose intended. 3.3 Processing changes. The suppliers of crude and distilled 3.4 Workmanship. The material shall be uniform, free from 4. QUALITY ASSURANCE PROVISIONS 4.1 Responsibility for inspection. Unless otherwise specified in the contract, the contractor

14、 is responsible for the performance of all inspection requirements as specified herein. 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 Government. to perform any of the ins

15、pections set forth in the specification where such inspections are deemed necessary to assure that supplies and services conform to perscri bed requirements. all inspections shall be performed under the following conditions: Except as otherwise specified The Government reserves the right 4.2 Inspect

16、ion conditions. Unless otherwise specified (see 6.2), a. Temperature: Room ambient 18 to 35C (65 to 95F) b. Altitude: Normal ground c. Vibration: Not applicable d. Humidity: Room ambient to 95 percent relative, maximum 4.3 Sampling. Sampling for qual i ty conformance inspection shall be in accordanc

17、e with MIL-STD-414, inspection level III, sections A and C. 4.3.1 M. Unless otherwise specified in the contract (see 6.2), a lot shall consist of all material manufactured in one continuous production run or in one batch, under essentially identical conditions, from the same raw materials, and to be

18、 offered for acceptance at one time. batches, manufactured from the same raw materials, may be blended to form a uniform larger batch which shall then constitute a lot for inspection purposes. accordance with 4.3 shall be subjected to the tests of 4.5. acceptable quality levels (AQLs) for the lower

19、specification limits (LSL) and the upper specification limits (USL) shall be as specified in TABLE II. When specified in the contract (see 6.2.2), three copies of the laboratory analysis shall be furnished to the procuring activity for each lot of material. The unit of product shall be one container

20、 of material. Several 4.4 Quality conformance inspection. Each sample obtained in The 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-DOD-T-BZbbbA 68 9999906 OL23L30 Requirement AQLs, % defective LSL USL Water - 1.5 As say - Imine number 2.5 - Tota

21、l phosphorus . 4.0 - Total ni trogen 4.0 - Total chlorides - 1.5 Hydrolyzable chlorides - 2.5 Test Method 4.5.1 4.5.2 4.5.3 4.5.4 4.5.5 4.5.6 * 4.5.1 Water content. The water content shall be determined accordance with either the direct or the indirect titration method OD 18893. The sample shall be

22、approximately 10 grams (g) weighed the nearest mg with 100 milliliters (mL) methanol as carrier. n of to 4.5.2 Assay by imine number. The following procedure shall be used to determine the assay by imine number of tris-l-(2-methyl aziridinyl) phosphine oxide. 4.5.2.1 Special reagents. a. Potassium t

23、hiocyanate solution - Dissolve 160 g of potassium thiocyanate in methanol and dilute to one liter (L) with additional methanol. b. Hydrochloric acid in methanol, 0.4 Normal (N): 34 mL of concentrated hydrochloric acid in 1.0 L of reagent grade methanol. c. Mixed indicator solution: 0.1% alcoholic br

24、omothymol blue sodium salt and 0.1% alcoholic phenol red sodium salt in a 1:l mixture. d. Potassium hydroxide solution, 0.1 N. 4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- DOD-T-826bbA 68 9999906 0123131 T DOD-T-82666A 4.5.2.2 Procedure. a. Add

25、 50 mL of potassium thiocyanate solution to a 250-mL Erlenmeyer flask fitted with a nitrogen purge to prevent carbon dioxide absorption. and start the magnetic stirrer. are thoroughly mixed before addition of the sample. Weigh a 0.20 to 0.25 g sample to the nearest 0.1 mg, transfer to the flask, and

26、 stir for five to six minutes. standard 0.1 Pi potassium hydroxide solution to a purple end point. thiocyanate solution to a 250-mL Erlenmeyer flask fitted with a nitrogen purge to prevent carbon dioxide absorption. acid reagent into the flask and start the magnetic stirrer. Titrate the same as for

27、the sample. required for the blanks. Pipet 10 mL of 0.4 M hydrochloric acid reagent into the flask It is very important that the two solutions Add six drops of mixed indicator and titrate visually with b. Run two blank standardizations by adding 50 mL of potassium Pipet 10 mL of 0.4 14 hydrochloric

28、Record the volume of potassium hydroxide solution c. Calculate the assay by imine number as follows: Assay, weight percent (wt%) = (v1 - v2) (N) (7.168) W Where: V1 = Average volume of potassium hydroxide used for blank, mL V2 = Volume of potassium hydroxide used for sample, mL N = Normal i ty of po

29、tassium hydroxide W = Weight of sample, g. content shall be determined in accordance with the following: 4.5.3 Assay by total phosphorus content. The total phosphorus 4.5.3.1 Digestion of sample. a. Weigh a 2.0 g sample, to the nearest 0.1 mg, into an iodine flask. stand until reaction subsides, and

30、 cool to room temperature. 6. Add 10 mL of 1:l nitric acid: distilled water and 10 mL of 1:l perchloric acid: distilled water to the flask and digest carefully on a hot plate. an additional 10 mL of 1:l nitric acid: distilled water. Carefully add 10 mL of 1:l nitric acid: distilled water, let flask

31、When sample has turned black remove from hot plate, cool , and add * c. Repeat digestion of sample and evaporate almost to dryness. Sample should be colorless (4.5.3.2.b.). to room temperature, and transfer quantitatively to a 500-mL volumetric flask with distilled water. Dilute to volume. Remove sa

32、mple from hot plate, cool 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-DOD-T-82bbbA 68 7777706 DI23132 1 H DOD-T-82666A 4.5.3.2 Analysis of sample. a. beaker. ammonium hydroxide, dropwise, until the color changes from pink to yellow. Add an exce

33、ss of 9 mL of ammonium hydroxide. Pipet a 20 mL aliquot of the digested sample into a 400-mL Add three drops of methyl orange indicator solution and concentrated b. the beaker. ammonium molybdate solution (4.5.3.2.c) , stir vigorously, and let mixture stand 20 to 30 minutes. plates and an asbestos m

34、at. solution until filtrate is neutral to litmus paper. If sample is still black at this point, add an additional 10 mL of 1:l nitric acid:distilled water and repeat digestion. Carefully add 10 mL of concentrated nitric acid while swirling (This reaction is exothermic.) To the hot solution add 25 mL

35、 Filter precipitate through a gooch crucible containing Wash precipitate with 1% ammonium nitrate c. Dissolve 100 g of molybdic acid in a mixture of 400 mL of cold distilled water and 80 mL of ammonium hydroxide. and with continuous stirring into a mixture of 400 mL of nitric acid and 600 mL of dist

36、illed water. dissolved in a few mL of distilled water and stir the mixture. After 24 hours, decant the clear solution through a filter paper into a reagent bottle Pour the solution slowly Add 0.05 g of sodium ammonium phosphate d. Quantitatively transfer the precipitate, plates, and asbestos mat to

37、the beaker which originally contained the precipitate. Carefully wash the crucible with a known volume of 0.5 N sodium hydroxide until all adhering precipitate is dissolved. Rinse crucible with distilled water. Collect all washings in the beaker. with 0.5 N sodium hydroxide solution. Record total vo

38、lume of sodium hydroxide solution used (25 to 30 mL is usually sufficient). 10 drops of phenophthalein indicator solution and titrate with 0.1 N hydrochloric acid to the colorless end point. Dissolve the precipitate in the beaker Add 5 to e. Calculate assay by total phosphorus content as follows: As

39、say, wt% = (A-B) (23.374) W Where: A = Mole equivalents (Meg) of sodium hydroxide used, mL x Pi B = Meg of hydrochloric acid used, mL x N W = Weight of sample, g. 4.5.4 Assay by total nitrogen content. The total nitrogen content shall be determined in accordance with the following: a. Weigh a 0.2 g

40、sample to the nearest 0.1 mg using a paper weighing Place in a dry Kjeldahl flask and add approximately disc (nitrogen-free). 18 g of potassium sulfate, one Hengar granule, and approximately 25 mL of concentrated sulfuric acid. mixture becomes cl ear. Digest the sample for one hour after the 6 Provi

41、ded by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-DOD-T-2bbbA b m 77777b 0123133 3 m CQD-T-82666A b. Cool the sample, add 150 mL of distilled water, mix, and again cool to room temperature. Accurately deliver 35.0 mL of standard 0.1 N sulfuric acid into a 3

42、00-mL Berzelius beaker. methyl purple indicator and 40 mL of distilled water. Immerse the delivery tube of the distillation apparatus in the solution to about 1.3 centimeters from the bottom of the beaker. Add two drops of c. Add 80 mL of saturated sodium hydroxide solution (55 g/100 mL water) to th

43、e Kjeldahl flask and immediately connect to the condenser of the distillation apparatus. until the solution starts bumping. Disconnect the flask, rinse the condenser and delivery tube with a small amount of distilled water. Remove the beaker. Distill the solution for 20 to 25 minutes, or d. Titrate

44、the excess acid in the beaker with standard 0.1 N sodium hydroxide solution to a faint green end point. e. Calculate assay by.tota1 nitrogen content as W Assay, wt% = (A-B) (7.168) Where: A = Meg of sulfuric acid used, mL x N B = Meg of sodium hydroxide used, mL x N W = Weight of sample, mg. 4.5.5 T

45、otal chlorides. The total chlorides sha accordance with the following: fol 1 ows : 1 be determined in in a gelatin to the fusion CUP of a. Weigh a 0.25 g sample, to the nearest 0.1 mg capsule (Parr No. 3601 , size 00, or equivalent). Add the ueroxide bomb, (Parr, or equivalent, electric ign tion, 42

46、-mL) 7.5 g and cover .I with In ., 11.3 * I g of sodium peroxide and 013 g of potassium ntrate-benzoic acid mixture (2:l). Mix thoroughly. Place the capsule - in the fusion . cup I of sodium peroxide and 0.3 g ot potassium nitrate-Denzoic acia (z:i) m1xr;ure. Sprinkle approximately 50 mg of benzoic

47、acid on top of the fusion reagents. b. Assemble the bomb and ignite electrically. Cool the bomb in a water bath for approximately 10 minutes. a fine jet of distilled water wash the underside of the head collecting the washings in a 400-mL beaker. Dismantle the bomb and with Wash again with 5 to 10 m

48、L of 50% nitric -;.A -.A ,.,+h A,-+llfiA ,.,-+e- aLiu aiiu I iiiae WILII UILI I ICU wac.ci. c. Remove the fusion cup from the bomb with a pair of tongs. Remove any materials adherins to the outer surface of the cup by washing with rigs th water and discard. from the underside of the head and cover b

49、eaker immediately with a watch glass. distilled water. Lay the cup on its side in the beaker containing wash When the melt has dissolved, remove the cup and wash thoroughly w Collect washings in the beaker. 7 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-DOD-T-82666A 68 7799706 0123134 5 DOD-T-82 666A d. Partly cover the beaker with a watch glass and slowly add 18 to 20 mL of