NAVY MIL-S-14195 A-1970 STYRENE MONOMER《苯乙烯》.pdf

1、MIL-S-14195A 93 m 9999906 0474790 7 m MI L-S-l4195A(OS) 17 February 1970 SUPERSEDING MIL-S-l4195(Ord) 22 November 1955 MILITARY SPE CIFIGATION STYRENE MONOMER This specification has been approved by the Naval Ordnance Systems Command, Department of the Navy. 1. SCOPE 1.1 This specification covers on

2、e grade of high purity styrene monomer (see 6. i). 2. APPLICABLE DOCUMENTS 2.1 The following documents of the issue in effect on date of in- vitation for bids or request for proposal, form a part of the specification to the extent specified herein: SPECIFICATIONS Feder a L PPP-D- 729 Drum: Metal, 55

3、-Gallon (For Shipment of Non- corrosive Material) STANDARDS Feder a 1 Fed. Test Method Std. No. 141 Military Paint, Varnish, Lacquer and Related Materials; Methods of Inspection, Sampling, and Testing MIL-STD- 105 Sampling Procedures and Tables for Inspection by Attributes MIL- STD- 12 9 Marking For

4、 Shipment and Storage 4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-S-34395A 93 9999906 0474793 9 MIL-S-l4195A( OS) (Copies of specifications, standards, drawings, and publications required by suppliers in connection with specific procurement

5、 functions should be obtained from the procuring activity or as directed by the coiitracting officer. ) 2.2 . Other publications - The following documents form a part of this specification to the, extent specified herein. Unless otherwise indicated, the issue in effect on date of invitation for bids

6、 or request for proposal shall apply. American Society for Testing and Materials ASTM D 445 Viscosity of Transparent and Opaque Liquids (Kinematic and Dynamic Viscosities) (Application for copies should be addressed to the American Society for Testing and Materials, i916 Race Street, Philadelphia, P

7、ennsylvania 19103. ) 3. REQUIRFmNTS 3.1 Material - The styrene monomer shall be a clear colorless liquid aromatic hydrocarbon suitably inhibited to prevent premature polymerization. 3.2 Physical and chemical properties - When tested as specified in Section 4, the physical and chemical properties of

8、the styrene monomer shall conform to the requirements specified in Table I. TABLE I PHYSICAL AND CHEMICAL PROPERTIES - PROPERTY - Specific gravity (absolute) 25 degrees/25 degrees Centigrade (O C) Refractive index, ND at 25O C Ri3QUIREMENTS MINIMUM I MAXIMUM O. 9035 1.5434 O. 9050 - Provided by IHSN

9、ot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-S-14195A 93 = 9999906 0474792 O MIL-S- 14195A(OS) TABLE I (Continued) PROPERTY I Color Viscosity, centipoises at 25O C Peroxides, as hydrogen peroxide by weight, percent Polymer content, by weight, percent Inhibito

10、r, as para-tertiary (p-tert) butylcatechol, by weight, parts per million (ppm) (see 6.3) REQUIREMENTS MINIMUM - 10 MA%IMUM 15 platinum-cobalt O. 80 o. o1 O. 20 50 33 Workmanship - The styrene monomer shall be processed in a manner that will produce the high quality product necessary to meet the requ

11、irements of this specification, and shall be free of defects which could cause the material to be unsuitable for the purpose intended. 4. QUALITY ASSURANCE PROVISIONS 4.1 Responsibility for inspection - Unless otherwise specified in the contract or purchase order, the supplier is responsible for the

12、 performance of all inspection requirements as specified herein. Except as otherwise specified in the contract or order, the supplier may use his own or any other facilities suitable for the performance of the inspection requirements specified herein, unless disapproved by the Government. The Govern

13、ment reserves the.right to perform any of the in- spections set forth in the specification where such inspections are deemed necessary to assure supplies and services conform to prescribed requirements. e 4.2 Classification of inspection - The examination and testing of the styrene monomer shaU1 be

14、entirely by quality conformance inspection. 4.3 Test conditions - The laboratory testing conditions shall be in accordance with Fed. Test Method Std. No. 141 and as described herein. 4.4 Sampling - 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MI

15、L-S-14195A 93 W 9999906 0474793 2 MIL-S- 14195A(OS) 4.4.1 Quality cbnformance samples - Quality conformance samples shall consist of a sample for tests (4.4.1.2) and a sample for examination of filled cofltaihers (4.4.1.3). Samples shali be labeled completely with information identi- fying the purpo

16、se of the sample, name of product, specification number, lot and batch number, date of sampling, ahd cohtfact humber. 4.4.1.1 Inspectida lot - rI ihspectioh lot size shall consist of the styrene monomer manufactured from oie batch or blendihg operation, undeh essentially the same conditions and pres

17、ented for accptahc at one time. 4.4, I. 2 Sampling fdr tests - An 8-ounce sample shall be selectd at random from each lot. The sample shall be placed in an aiktight glass bottle havirrg a glass stopper or cap containihg a cork or cardboard liner covered with metal foil and labeled as specified ih 4.

18、4; 1. All qtialitfr confcirmanice tests shll be made on this sample. 4.4.1.3 Sabidiw foii ejralhination of filled cntainers - A rclndoni sample of one container shall be selected from filled containers fully prepared for delivery, in accakdhce *ith MiL 4. i. 2) as specified in4.5, and an examination

19、 of the fdie cottailier (4.4.1.3) as specified in 4.6. 4; 5 Test methods - 4.5. i Spebific glrslvity - wo specimens shall be tested in accordance with Fed. Test MethMl St0002 to the apparent specific gravity in air. 4; 5.2 Refractive index - The refractive index a 2 specimens shall be determined wit

20、h an Abbe refractometer OP any equally accurate instrument at 25 +io C to an accuracy of +O; OU01 unit, and vising Iight having a wave length equivalent tu the IDft line of soditim; 4.5.3 color - 4.5.3.1 Prepai-ation of color standards - Color standards shall be pre- pared as follows: 4 Provided by

21、IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-S-14195A 93 9999906 0474794 4 = MILS- 14195A (OS) Dissolve 1.245 grams (gm. ) of potassium chloroplatinate (K2PtC16) containing O. 500 gm. of platinum, and 1.000 gm. of crystallized cobaltous chloride (CoC12. 6

22、H20), containing about O. 278 gm. of cobalt, in water containing 100 milliliters (mi. ) of concentrated hydrochloric acid, and dilute to 1 liter with distilled water. If KzPtC16 is not available, the following procedure shall be used: by repeated evaporation to dryness after adding an excess of hydr

23、ochloric acid, Dissolve this product with 1.000 gm. of CoC12. 6H20, Dissolve O. 5 gm. of metallic platinum in aqua regia. Remove the nitric acid 4.5.3.2 Procedure - Fifty ml. of the sample shall be transferred to a 50-ml; Nessler tube. The color of the sample shall be compared with color standards p

24、re- pared by diluting O. 5, 1. O, 1. 5, and 2. O ml. of the standard solution (see 4.5.3.1) to 50 ml. in similar 50-ml. Nessler tubes. The platinum cobalt number of the sample shall be the number of milligrams of platinum contained in 1000 ml. of the standard solution which matches the sample. The s

25、tandard solution has a color of 500, The Nessler tube containing i. 5 ml. of the standard solution diluted to 50 ml. has a color of 15 platinum-cobalt (see 6.4). 4.5.4 Viscosity - Two specimens shall be tested, using a modified Ostwald viscosimeter, in accordance with ASTM Method D 445, except that

26、the temperature of the water bath may be allowed to fluctuate plus or minus O. 1“ C and the bath temperature need be read only to the nearest O. 1“ C. reported shall be absolute viscosity in centipoises instead of kinematic viscosity The value in centistokes. The viscosity sh:ill be calculated as fo

27、llows: tl x d1 x n I A Viscosity at 25 C, centipoises = t2 d2 where : tl = time of flow of the unknown at 25“ C. t2 = time of flow of the standard material (Bureau of Standards or dl = density of the unknown, grams per milliliter (gm./ml.) at 25“ C. API oil) at 25“ C. (dl may be determined by adding

28、 O. 0027 to the value of specific gravity 25“/25“ C determined as specified in 4.5.1). d2 = density of standard material gm./ml. at 25“ C. n = viscosity, centipoises, of the standard material at 25“ C. 4.5.5 Peroxides - 4.5.5.1 Reagents - Approximately O. 02 normal (N) solution of titanous chloride

29、shall be made by diluting the 20 percent reagent grade solution. sulfate solution shall be made by dissolving 35.1 gm. of crystallized ferrous ammonium sulfate hexahydrate in 400 ml. of distilled water. sulfuric acid shall be added, and the solution warmed slightly. Potassium permanganate Ferric amm

30、onium Twenty-five ml. of concentrated 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-S-14175A 93 = 9799906 0474795 b MILS- 14195A(OS) solution shall now be added until the iron is completely oxidized, and the solution is diluted to 1 liter wit

31、h distilled water. O. 005 gram of ferric iron. Ferrous ammonium sulfate solution shall be made by dissolving 19.6 gm. of hexahydrate salt in 800 ml. of distilled water and adding 50 ml. of concentrated sulfuric acid. made to 1 liter. The ferrous iron solution shall be approximately O. 1N and does no

32、t require standardization. A 10-percent aqueous solution of potassium thiocyanate shall be used as an indicator; sulfuric acid diluted to a ratio of 1:l with distilled water, concentrated hydrochloride acid, and absolute methanol are also necessary for carrying out the determination. One ml. of this

33、 solution will contain After solution is complete, dilution should be 4.5.5.2 Apparatus - A 50-ml. long-tipped burette shall be used for the titanous chloride solution. advantageous to assemble equipment for storing the titanous chloride solution under an inert atmosphere (see 6.5). The nitrogen use

34、d shall be passed through a pyrogallic acid solution to remove the oxygen and a slow flow of nitrogen shall be main.tained at all times. A satisfactory apparatus is shown in Figure 1. If the determination is to be run each day, it is 4.5.5.3 Standardization of titanous chloride solution - Ten inl. o

35、f the standard ferric ammonium sulfate solution shall be pipetted into a 250-ml. wide- mouth Erlenmeyer flask containing 50 ml. of distilled water, 15 ml. of concentrated hydrochloric acid, and 10 ml. of the potassium thiocyanate indicator. A small lump of “dry ice“ shall be added to the flask in or

36、der to maintain an inert atmosphere over thesolutionat all times. The tip of the burette shall be kept low in the flask and the titration with titanous chloride solution shall be carried out until the pink color of the ferric thiocyanate has just disappeared. This titration shall be recorded. calcul

37、ation shall be made to obtain the factor of the titanous chloride solution: If the peroxide is to be considered as diethyl peroxide, then the following O. 05 x 45.04 Ts x 55.85 factor = where: Ts = ml. of titanous chloride required for titration of the O. 05 gm. of factor = gril. of diethyl peroxide

38、 equivalent to 1 ml. of the titanous ferric iron contained in 10 ml. of standard iron solution. chloride. 4.5.5.4 Procedure - Five ml. of the potassium thiocyanate solution, 2 ml. of the dilute sulfuric acid, and 10 ml. of the approximately O. 1N ferrous ammonium sulfate solution shall be pipetted i

39、nto a 250-ml. wide-mouth Erlenmeyer flask con- taining 100 ml, of the methanol. A small lump of “dry ice“ shall be placed in the flask, the solution mixed by swirling, the flask covered with 8 watch glass, and allowed to stand for 15 minutes. While the burette is low in the flask, the titanous chlor

40、ide solution shall be carefully added until the pink color just disappears. amount of titanous chloride is not required in the calculation since this procedure This 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-S-L4195A 93 m 9999706 0474796 8

41、 m MIL-S- 14195A(OS) e Figure 1. Apparatus for titrations with titanous chloride 7 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- MIL-S-14195A 93 7999906 0474797 T MIL-S- 14195A(OS) is intended only to reduce any ferric sulfate present in the ferro

42、us ammonium suifate solution used. The measured sample of styrene shall then be added. Twenty- five ml. of styrene monomer shall be pipetted, mixed, covered with a watch glass and allowed to stand for 2 hours. The ferric sulfate formed from the reaction shall then be titrated with a standard titanou

43、s chloride solution until the pink color of the ferric cyanate just disappears, The titration shall be carried out in a manneridenticai with the one used to dispel the ferric sulfate from the ferrous ammonium sulfate. The weight percent of diethyl peroxide shall be calculated as follows: Percent by

44、weight of peroxides as diethyl peroxide T x factor x 100 - 25 x 0.9 where: T = ml. of standard titanous chloride required for the ferric iron factor = gm. of diethyl peroxide equivalent to 1 ml. of the titanous produced by the peroxides in the sample. chloride as determined in the standardization 4.

45、5.6 Polymer content - 4.5.6.1 Quick alcohol method - Where the amount of polymer is negligible and rapid work is desired, the following method shall be used: Determine the amount of polymer at the time of assay by placing 10 ml. of dry methanol in a test tube and adding 1 to 2 ml. of styrene. If, af

46、ter shaking the mixture vigQrous1y for a few seconds, only a light cloud of precipitate is produced, the material shall be considered satisfactory. However, if a heavy precipitate is formed, use the gravimetric method (see 4.5.6.2). 4.5.6.2 Gravimetric method - The polymer content shall be determine

47、d as follows: Add 25 gm. of the sample to 100 ml. dry chemically pure (C.P.) methanol in a 250-ml. beaker. Stir this mixture well and place on a steam bath for 5 minutes or longer to aid coagulation. Allow the solution to cool and filter on a tared Gooch crucible or a fine porosity fritted glass cru

48、cible. Place the precipi- tate under an infrared lamp for 5 minutes and then dry to a constant weight at 70 C. Cool the polymer in a desiccator and weigh. Calculate the polymer content as follows : m. polymer x 100 grna sample Percent by weight of polymer = 4.5.7 Inhibitor - Presence, ppm, of inhibi

49、tor as TBC shall be deter- mined by Method A (4.5.7.1) or Method B (4.5.7.2). 8.5.7.1 Method A - 8 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-c MIL-S-14L95A 93 W 9997906 Y7Y798 1 W * MIL- S- 14 19 5A (OS) 4.5.7.1.1 Reagents - Sodium hydroxide solution, 1N is needed for this determination. Styrene stock solution, containing 1 gm. of p-tert butylcatecho