1、rr TT-T-65bC W 9999974 0333297 975 D TT-T-656C 5 OCTOBER 1992 SUPERSEDING TT-T-656B 15 MAY 1965 FEDERAL SPECIFICATION TRICRESYL PHOSPHATE This specification is approved by the Commissioner, Federal Supply Service, General Services Administration, for the use of all Federal agencies. 1. SCOPE 1.1 Sco
2、pe. This specification covers tricresyl phosphate, a reaction product of cresylic acid and a phosphorus compound. from petroleum or coal tar is acceptable. Cresylic acid derived 2. APPLICABLE DOCUMENTS * 2.1 Government documents. * 2.1.1 Specifications and standards. The following specifications, st
3、andards, 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 in the solicitation (s
4、ee 6.2). SPECIFICATIONS FEDERAL TT-N-97 Naphtha; Aromatic O-E-751 Ether, Petroleum; Technical-Grade 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 Air Warfare Center A
5、ircraft Division Lakehurst, Systems Requirements Department, Code SR3, Lakehurst, NJ 08733-5100, by using the self-addressed Standardization Document Improvement Proposal (DD Form 1426) appearing at the end of this document or by letter. AMSC NIA FSC 6810 DISTRIBUTION STATEMENT A. Approved for publi
6、c release; distribution is unlimited. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-TT-T-b5bC m 999997q OLL3298 BOL m TT-T- 656C STAN DARDS FEDERAL FED-STD-141 FED-STD-791 MI LI TARY MI L-STD-105 MI L-STD- 1 2 9 MIL-STD-290 Paint, Varnish, Lacquer,
7、 and Related Materials; Methods of Inspection, Sampling, and Testing Lubricants, Liquid Fuels, and Related Products; Methods of Testing Sampling Procedures and Tables for Inspection by Attributes Marking for Shipment and Storage Packaging of Petroleum and Related Products ib (Unless otherwise indica
8、ted, copies of federal and mi li tary specifications, standards, and handbooks are available from the Navy Publication and Printing Service Office, Standardization Documents Order Desk, Building 4D, 700 Robbins Avenue, Philadelphia, PA 19111-5094.) * 2.2 Non-government publications. The following do
9、cuments form a part of this document to the extent specified herein. Unless otherwise specified, the issues of the documents whichare DOD adopted are those listed in- the issue of the DODISS cited in the solicitation. documents not listed in the DODISS are the issues of the documents cited in the so
10、licitation (see 6.2). Unless otherwise specified, the issues of AMERICAN SOCIETY FOR TESTING AND MATERIALS (ASTM) ASTM O891 Standard Test Methods for Specific Gravity, Apparent, of Liquid Industrial Chemicals ASTM D1208 Standard Test Method for Color of Halogenated Organic Solvents and their Admixtu
11、res (Platinum-Coba1 t Scale) ASTM D1296 Standard Test Method for Odor of Volatile Solvents and Di 1 uents ASTM 01721 Standard Test Method for Permanganate Time of Tricresyl Phosphat e ASTM 02369 Standard Test Method for Volatile Content of Coatings ASTM E832 Standard Specification for Laboratory Fi
12、1 ter Papers (Application for copies should be addressed to the American Society for Testing and Materials, 1916 Race Street, Philadelphia, PA 19103.) (Non-Government standards and other pub1 ications are normally avai lable from the organizations that prepare or distribute the documents. may be ava
13、ilable in or through libraries or other informational services.) These documents also 2 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-*r TT-T-b5bC m 74 OLL3299 748 m TT-T-656C * 2.3 Order of precedence. In the event of a conflict between the text o
14、f this specification and the references cited herein (except for related associated detail specifications, specification sheets or MS standards), the text of this document shall take precedence. supersedes applicable laws and regulations unless a specific exemption has been obtained. Nothing in this
15、 document, however, 3. REQUIREMENTS 3.1 Quantitative requirements. The quantitative requirements of the tricresyl phosphate shall be as specified in table I. 3.2 Qualitative requirements. 3.2.1 Appearance. The tricresyl phosphate shall be clear and free from sediment and suspended matter when examin
16、ed by transmi tted light. 3.2.2 Water. The tricresyl phosphate shall be miscible without turbidity with 19 volumes of 10 degree heptane at 20C when examined as specified in 4.5.5. 4. QUALITY ASSURANCE PROVISIONS * 4.1 Responsibility for inspection. Unless otherwise specified in the contract or purch
17、ase order, the contractor is responsible for the performance of all inspection requirements (examinations and tests) 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 inspec
18、tion requirements specified herein, unless disapproved by the Government. The Government reserves the right to perform any of the inspections set forth in this specification where such inspections are deemed necessary to ensure supplies and services conform to prescribed requirements. * 4.1.1 Respon
19、sibility for compliance. All items shall 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 absence of any inspection requirements in the specification shall not relieve th
20、e 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 part of manufacturing operations, is an acceptable practice to ascertain conformance to requirements, however,
21、 this does not authorize submission of known defective material, either indicated or actual, nor does it commit the government to accept defective material. * 4.2 Classification of inspections. The inspection requirement specified herein is classified as follows: a. Quality conformance inspection (s
22、ee 4.3). 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-TT-T-65bC m 9999934 O113300 29T r* TT-T-656C 4.3 Quality conformance inspection. Quality conformance inspection shall 4.3.1 M. consist of the examinations and tests specified herein. storage
23、tank or in containers into which tricresyl phosphate has been transferred from a single storage tank with no concurrent addition of new material taking place during transfer. 4.3.2 Sampling. Sampling for inspection and acceptance shall be in accordance with MIL-STD-105. A lot shall consist of all th
24、e tricresyl phosphate in a single 4.3.3 Inspection. The inspections specified herein shall be conducted in accordance with FED-STO-791, method 9601, “Inspection requirements“. 4.3.4 Inspection level. The inspection level shall be S-2 and the Acceptable Quality Level (AQL) shall be 4.0, as specified
25、by MIL-STD-105. 4.4 Qual i ty conformance tests. 4.4.1 gual i ty conformance tests. 4.3.2 shall be subjected to the tests specified in 4.5. The sample selected in accordance wl th 4.5 Test procedures. 4.5.1 Tests shall be conducted as specified in table II and 4.5.2 through 4.5.5. 4.5.2 Acidity. Pla
26、ce 100 milliliters (ml) of the sample in a weighed stoppered 500 ml Erlenmeyer flask, stopper the flask, and reweigh. of neutral methyl or ethyl alcohol and mix thoroughly by swirling. 0.02 normal (N) potassium hydroxide (KOH) in 99 percent methyl or ethyl alcohol using phenolphthalein as the indica
27、tor. The end point shall be considered that point in the titration where the pink color persists after continuous swirling of the solution for 30 seconds. volume of the aiccholic KOH used, the volume (ml) of KOH required for the neutralization of 1 gram (g) of the sample shall be calculated. Add 100
28、 ml Titrate with From the weight of the sample taken and the 4.5.3 Ester content. 4.5.3.1 Reagents. 4.5.3.1.1 Potassium hydroxide. Reagent grade potassium hydroxide (KOH) pel lets. 4.5.3.1.2 Ethyl ether. Reagent grade ethyl ether. 4.5.3.1.3 Nitric acid. Mixture of 1 ml of nitric acid “03 (specific g
29、ravity (sp. gr.) 1.42) and 99 ml of distilled water. 4.5.3.1.4 Ammonium molybdate solution. Mix 100 g of pure molybdic anhydride or 188 g of 85 percent molybdic acid with 400 ml of distilled water and add 80 ml of ammonium hydroxide (sp. gr. 0.09). filter and pour the solution slowly with constant s
30、tirring into a mixture of 400 ml of nitric acid. (sp. gr. 1.42) and 600 ml of distilled water. for 24 hours and filter again. When solution is complete, Let settle 4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-i 4 TT-T-65bC D 4 OLL33OL 126 TT-T-6
31、56C 4.5.3.1.5 Potassium nitrate solution. Dissolve 10 g of potassium nitrate 4.5.3.1.6 Potassium hydroxide solution. (KNO3) in freshly distilled water and dilute to 1 liter. dissolving 28 g of KOH in freshly distilled water and diluting to 1 liter. sufficient barium hydroxide (BaOH) to precipitate t
32、he carbonate. Allow the precipitate to settle out and decant the clear solution. Standardize the solution. Prepare a 0.5 N of KOH solution by Add 4.5.3.1.7 Sulfuric acid. Prepare 0.5 N solution of sulfuric acid (H2SO4) and standardi ze . 4.5.3.1.8 Phenolphthalein indicator. Dissolve 1 g of phenolpht
33、halein in 100 ml of alcohol. 4.5.3.2 Procedure. Weigh 200.0 * 0.1 mg of the tricresyl phosphate into a 100 ml silver or nickel crucible. water. slowly. of the crucible frequently unti 1 al 1 the tri cresyl phosphate has decomposed and the oily matter has disappeared, about 15 to 20 minutes. Allow to
34、 cool and add a small amount of water to dissolve the contents of the crucible. Transfer the contents of the crucible to a 300 ml beaker, wash the crucible with water to bring the solution to 50 to 75 ml. 1.42) and add 1 to 2 ml in excess. Transfer the solution to a 200 ml separatory funnel and extr
35、act with 50 ml portions of ether until the acid solution is clear and the ether layer is practically colorless. sufficient to accomplish this. Erlenmeyer flask and add water to bring its volume to 100 ml. Heat on a steam bath for 30 minutes to remove all traces of ether. Cool, neutralize with ammoni
36、um hydroxide (NH40H) (sp. gr. 0.90) and add “03 (1 to 99) dropwise until the solution is slightly acid. Add 100 ml of the ammonium molybdate solution. Place the flask in a water bath maintained at 40“ to 45C and allow the precipitate to digest for 1 hour. Swirl the contents of the flask occasionally
37、 to agitate the precipitate during the digestion. Filter through a medium speed, ashless type filter paper, ASTM E832, Type II, Class F, (No. 40 Whatman or equal), by decanting the liquid from the precipitate. precipitate 5 times with 10 to 20 ml portions of the 1 percent KNO3 solution and filter th
38、e washings by decanting from the precipitate in the flask. filter paper containing most of the precipitate until the washings no longer show an acid reaction, with like portions of the KNO3 solution, usually 5 to 10 times. When the filter paper has completely drained, transfer it with the precipitat
39、e to the 500 ml Erlenmeyer flask. contents of the flask. the flask to dissolve any precipitate that might be clinging to it. rod to macerate the filter paper and break up any lumps of precipitate that might have formed, until all yellow particles have dissolved. Wash down the inside of the flask wit
40、h approximately 100 ml of water, add 3 drops of phenolphthalein indicator and titrate the excess KOH with 0.5 N H2SO4. blank titration on 30 ml of the KOH solution. Add 6 g of the KOH pellets and 5 drops of Heat the crucible over a low flame until the melt begins to bubble Maintain sufficient heat t
41、o ensure slow bubbling, swirling the contents Neutralize the solution with “03 (sp. gr. 1 to 3 extractions should be Transfer the aqueous layer to a 500 ml Wash the flask and Wash the Add 30 ml of the 0.5 N KOH to the Allow the KOH solution to flow slowly down the inside of Use a glass Run a 5 Provi
42、ded by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-TT-T-b5bC - 9999979 0113302 Ob2 TT-T-656C c 4.5.3.3 Calculation. Calculate the percentage of tricresyl phosphate as fol lows : Percent tricresyl phosphate = (A - B) X c x o.0165 x 100 w where : A = Volume di
43、fference (in ml) of 0.5 N H2SO4 required for titration of 30 ml blank of 0.5 N YOH and volume (ml) of H2SO4 required to titrate the excess 0.5 N KOH in sample. B = Volume (ml) of 0.5 N KOH required for titration of the free acid in a sample equal in weight to that used for the ester determination. C
44、 = Normality (NI of the KOH solution. = Weight (g) of sample used. - Note. a mixture of cresols and xylenols. 112 not 108. ammonium phosphomolybdate, 1 ml of 1.0 N KOH is equivalent to 0.165 g tricresyl phosphate. The cresols generally used for the manufacture of tricresyl phosphate are Therefore, t
45、he average molecular weight is Since 23 mols of KOH are required for the titration of 1 mol 4.5.4 Phosphite content. 4.5.4.1 Reagents. a. 10 percent solution of hydrochloric acid. b. Saturated solution of sodium chloride. c. 0.05 N solution of iodine. d. 0.05 N solution of sodium thiosulfate. 4.5.4.
46、1.1 Procedure. Weigh 10 g of the sample, add 25 g of the hydrochloric acid (HC1) solution, and reflux the mixture for 2 hours. Cool the mixture and transfer to a separatory funnel. Add 25 ml of petroleum ether conforming to O-E-751 or aromatic naphtha conforming to TT-N-97 and 25 ml of the sodium ch
47、loride solution. Mix the contents of the separatory funnel by shaking and al low to stand unti 1 the nonaqueous layer completely separates from the water layer. Draw off and retain the water layer. Wash the nonaqueous layer four successive times with 25 ml portions of the saturated sodium chloride s
48、olution, adding each portion of the separated salt solution to the original water layer. Discard the nonaqueous solution. Neutralize the combined aqueous salt solution with solid sodium bicarbonate and dilute to a volume of 2300 ml with distilled water in a glass-stoppered flask or bottle. Add 10 ml
49、 of 0.05 N iodine solution from a burette, thoroughly mix, and allow to stand in the dark for 30 minutes. Cautiously acidify the mixture with 25 percent acetic acid and titrate with 0.05 N sodium thiosulfate solution, using the same reagents. Run a blank determination as specified above, 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-di TT-T-b5bC m 9979974 0113303 TT9 m TT-T- 6 5 6C 4.5.4.1.2 Calculati
