ARMY MIL-E-14828-1969 ETHYLENE DIMETHACRYLATE (ETHYLENE GLYCOL DIMETHACRYLATE)《二甲基乙烯(乙二醇 二甲基)》.pdf

1、MIEE.uc82mJ) 25 April 1969 MILITARY SPECIFICATION DIMETHACBYLATE (Ethylene Glycol, Dimethacryiate) 10 SCOPE 1.1 This specification covers ethylene dimethacrylate used as a coating on propellants (see 6.3). 2. APPLICArn DocmTs 2.1 The following documents of the issue in effect on date of invitation f

2、or bids or request for proposal, form a part of this specification to the extent specified herein. STANDARD MILITARY WTiLI.29 - Marking for Shipment and Storage (Copies of specifications, standards , drawings , and publications required by suppliers in connection Kith specific procurement functions

3、should be obtained from the procuring activity or as directed by the contracting officer.) 2.2 Other publications. The following documents form a part of this specification to the extent specified herein. Unless otheluise indicated, the issue in effect on date of imitation for bids or request for pr

4、oposal, o, pounds of ethylene dimethacrylate offered for delivery at one time, If the 4m2.2 At place of deiiveq. For the purpose of sampling, a lot of ethylene dimethacryate shall consist of all the ethylene dimethacrylate in a single shipment. 4.3 Sarnp.lhqa For chemical tests, a 1/$ ml of water th

5、rough the top of the condenser, remove the flask, and cool to room temperature, Add 5 drops of phenolphthalein solution and titrate with standard O.LN hydrochloric acid solution. Gamy a blank determination through the procedure using 10 ml. of the ethyl alcohol instead of the aliquot of the sample.

6、Calculate the percent ethylene dimethacrylate as follows: 9.906 (B-A)B W Percent ethylene dimethacrylate = where: B U ml. of hydrochloric acid for titration of blank determination. A ep ml. of hydrochloric acid for titration of sample. N U normality of hydrochloric acid. W gm. of sample in aliquot.

7、4.4.3 Monomer. 4.4.3.1 Reagents. 4.4.3.Li. Potassium bromate - bromide solution (0.2 NZ. Dry potassium bromte for 2 hours at 100C. Place 5.6 gm, into a Pyrex bottle and add 30 ga. of potassium bromide and enough water to dissolve the salts. 4,4,3.1.2 Starch indicator solution. Eiiix 2 gm. of soluble

8、 starch and aeveral. mg. of mercuric iodide (as a preservative) with a little water. Add Lhe mixture slowly to Ijoo nil, of boiling water. Boil for 5 minutes and cool to room temperature. 4.4.3LL.3 Potassium iodide solution (10 percent) Dissolve 10 gm, of !his solution Wu1 keep potassium iodide in w

9、ater and dilute to 100 nil. approximately 3 days. 4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-E-l4828(lW) - 4.k.3.l.l+ Sodium thiosulfate solution (0.lN). For each liter of solution desired, dissolve 26 gm. of sodium thiosulfate pentahydrat

10、e and 0.1 gm. of sodium carbonate in sufficient boiled and cooled water to make 1 liter. Allow to stand at least 24 hours. Standardise as follows: Dissolve 0.20 to 0.23 gm. of potassium dichromate (NEE Std 136, dried for 2 hours at 100C) in 60 ml. of water. Add 15 ml. of potassium iodide solution (1

11、0 percent)and 20 ml. of 1 N hyrochloric acid. Stopper the flask, swirl the contents for a few seconds, and allow to stand in the dark for 10 minutes. Titrate with the sodium thiosulfate solution, swirling continuously until a light greenish- brown color appears. Add 5 nil. of starch indicator soluti

12、on and continue the titration until the deep blue starch-iodide color changes to a pale bluish green. solution as follows: Calculate the normaltiy of the sodium thiosulfate A 0*04qOrcB Normality of sodium thiosulfate solution = where: A 3: gm. of potassium dichromate. B = ml. of sodium thiosulfate s

13、olution. 4.4.3.2 Procedure. Add approximately i5 ml. of glacial acetic acid to a dry LOO mi volumetric flask by means of a long-stemmed funnel, remove the funnel, and stopper the flask. approximately 1 ml. of ethylene dimethacrylate by means of a delivery pipet. Stopper the flask, weigh again to 0.1

14、 mg., and calculate the weight of the sample by difference. Dilute to the 100 ml. mark with glacial acetic acid. 0.2 N potassium bromate-bromide solution, a 10.00 ml. aliquot of the solution of the sample, and LO ml. of hydrochloric acid. Immediately stopper the flask and allow to stand for 20 minut

15、es in the dark. Add LO ml. of potassium iodide solution (10 percent) to the gutter of the flask and allow t5i.s solution to trickle through the loosened stopper. Swirl, wash down the gutter and sides of the flask with water from a wash bottle, and titrate immediately with standard 0.1 N sodium thio-

16、 sulfate solutin until the color is light yellow. Add 5 d. of starch solution and titrate carefully until the blue color of the solution disappears. bromate-bromide solution and 10-d. of glacial acetic acid (instead of the sample) . Calculate the percent ethylene dimethacrylate monomer as Weigh to 0

17、1 mg. Add Into a 500 ml. iodide flask, measure 25.00 mL. of Run a blank determination using the same volume of potassium ollows : Y. 4.953 (SA) N W Percent ethylene dimethacrylate monomer = where: B = ml. of thiosulfate solution for titration of blank determination. A = ml. of thiosulfate solution

18、for titration of sample. N = normality of thiosulfate solution. W = gm. of sample in aliquot. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-4.4.4 Free aciditg, Transfer 50.0 nil, of the sample to a 125 d, Erlenmeyer flask, Add 50 d. of diluted ethy

19、l alcohol (30 percent) and 2 drops of phenolphthalein solution (see 4.1.1,2) and titrate with 0.1 N sodim hydroxide solution. Run a blank determination. Calculate the free acidity (as methacrylic acid) as follows: A-B x 0,86 ( Percent free acidity, calculated as methacrylic acid = where: A E mZ, of

20、0,lN sodiun hydroxide solution for titration of sample. B ? nil, of 0,lM sodium hydroxide solution for titration of blank, V di., of sample taken. D = density (gm,/ml,) 4,4, 5 Hgdroquinon+ 4,4,5.2 Reagents. 4,4,!Ll,i, Dilute acetic acid (1 to 201. Dilute 50 ml. of glacial acetic acid to 1 liter with

21、 water, 4,+,5.1,2 Sodium acetate solution (2 N). 4,4.5,1.3 Iod-e .solution (O4lN), Dissolve 13.5 gm, of iodine and Dissolve 272 gm. of sodium acetate trihydrate in water and dilute to 1 liter, 24 gm, of potassium iodide in 50 mi, of water and dilute to 1 liter, 4,4,5,I.,rC. Sodium thiosulfate soluti

22、on (0.1 N). See 4.4.341,4, 4,4,5.2 Proc-edure, Transfer 50.0 nil. of the sample to a 500 d. Erlenmeyer flask, Ad 5 d, of dilute acetic acid (1 to 20), l mi4 of methanoland 20 nil. of 2 N sodium acetate solution, while swirling. Add 5, mi of 0.1 N iodine soluixion, swirl, and allow to stand for 1 min

23、uke, using no starch, Run a blank titration using the same amounts of reagents, Calculate the percent hydroquinone as follows: Titrate the excess iodine with 0.1 N sodium thiosulfate solution, ELA) x 0.Q ( Percent hydroquinone = VxD where: B = d of sodium thiosulfate solution for titration of blank

24、A = mi., of sodium thiosulfate solution for titration of sanple. V a mi. of sample taken, D =I density of sample (gni,/ml,) determination . 4.,4,6 Densitz, Perform the density determination (at 25OC) using the Pycnometer method described jn ASTM D9fd-55. Any Pycnometer method of equivalent accuracy

25、can also be used. 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-E-L482 b 7777706 OLL6752 7 M 4.4.7 Index of refraction. Determine the index of refraction, ND25, as described in ASTI4 D1218-61. 5. PREPAMTION FOB DELIVERY 5.1 PackEinFa; and pac

26、kinq. 5.l.l Level C. The ethylene dimethacrylate shall be packed in uniform quantities in conformance with the manufacturers commercial practice, or as specified in the contract, to provide protection against damage during shipment from the supply source to the first receiving activity for hediate u

27、se. Containers shall comply with Department of Transportation rules or other carrier regulations applicable to the mode of transportation. 5.2 Marking. in addition to any special marking required by the - contract or order, marking for identification and shipment shall be in accordance with MIL-STD-

28、iZ9 5.2.1 Each unit shall have the following precautionary label: Warning: Flammable! May cause skin irritation. Keep away from heat, sparks, and open flame. Keep container closed. Use with adequate ventilation. Avoid prolonged breathing of vapor. Avoid contact with skin, eyes, and clothing. 6. NOTE

29、S 6.1 Intended use. Ethylene dimethacryhte is intended for use as a coating agent on propellants. 6.2 Ordering data. Procurement documents should specify the following: Title, number and date of this specification, E Packaging and packing (see. 5.1) . 6.3 Ethylene dimethacrylate is a monomer and est

30、er with the following formula: H2C diglycol dimethacrylate; and ethylene ester, methacrylic acid. compound is assigned Registry Number 97905 in the CAS Registry System. The Custodian: Aw-MU Preparing activity: Amiy-MU Review interest: Project No. 68lGA842 User interest: I AW - MD, m, * U. S. GOVERNMENT PRINTING OFFICE: 1969 -341-519/A-6754 Army - MI 7 “ Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-