ARMY MIL-T-50611-1970 TRINITRORESORCINOL (STYPHNIC ACID)《(收敛酸)三硝基间苯二酚》.pdf

1、 -1 . a .: .- *? MIL-T-50611 13 m 7777906 0328731 4 MIL-T-50 6 1 l(MU) 6 May 1970 MiLITARY SPXZFICATION TRINITRORESORCJ?OL (STYPHNIC ACID) 1. SCOPE AND CLASSIFICATION 1.1 Scope. This specification covers trinitroresorcinol for use in the nianufacture of lead styphnate. 1.2 Classification. The trinit

2、roresorcinol shall be of the following types: !i?ype I - Cream color (see table I) Type II - Reddisbbrown (see table I 2.1 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: . SPECIF

3、ICATIONS -, Y.y and Paste, Packaging and Packing of iber PZIGSTD-105 - Sampling Procedures and Tables for inspection by Attributes mTi)1129 - Marking for Shipment and Storage Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-SObLL 13 979990b 0328

4、932 b W *. mT40611 (m) (Copies of specifications, standards, drawjngs , and publications required by suppliers in Connection with specific procurement functions should be obtained from the procuring activity or as directed by the contracting- officer,) The following documents form a part of this spe

5、cification to the extent specified herein, Unless otherwise indicated, the issue in effect on date of hvitatiQn for bids or request for proposal sha31 apply, 2.2 Other publications. AblERIC. SOCIETY FOR TESTING AND MATERIALS ASTM DU9366 - Reagent Water (Application for cogies of publications should

6、be addressed to the American Society for Testing and Materials, 1916 ype II Cream-colored Reddish-brown 4.51 98. o 98. O 4.5.2 99.0 99.0 4- 5.3 Less than 180 0.07 0.07 4.5.5 6.02 0.02 4.5.6 0.01 0.01 4.5.7 1.00 1.30 4.5*8 Appearance Assay by determination of NO2 groups, min.,percent Assay by titrati

7、on with standard alkali, min ercent powder . powder Moisture, percent 21-27 2-27 Melting point (final) : C Greaker than Greatgr than 4.5.4 170 C 170 C ess than :-7e0c Residue on ignition, max. percent Hater-insoluble matter, max. percent Alcohol-insoluble , max. percent Sulfate? including resor- cin

8、ol disuifonic acid (as %SO ), max. percent sieve, Run. percent GranuLaL mnutes to displace the air. the flow of gas during the entire titration procedure. Pipet an accurately measursd 25 ml. aliquot of the solution of the sample into the titration flask (see fig. 2). Add 40.00 mi. of 0.2 PP titanous

9、 chloride solution. Add 25 ml. of i5 gercent hydrochloric acid and a few glass beads (to prevent bumping) and connect the flask to a reflux condenser. Place the flask and condenser on a hot plate and bo= gently for 5 minutes. Without disconnec-iing the condenser, remove the flask from the hot plate,

10、 Increase the current of inert gas and cool the solution to rooin temperature in a cold water bath. ammonium thiocyanate solution, and titrate with 0.15 N ferric ammonium sulfate solution to the end point, as indicated by the first permanent red color. of reagents as above. This will provide a value

11、 for the amount of ferric arsaioniwp sulfate solution equivalent to U.00 ml. of titanous chloride solution. Transfer to 2 25ml. volumetric flask and dilute to the nark Continue Disconnect the condenser, add 5 niL. of 20 percent Conduct a blatik determination using exactly the same amount Calculate t

12、he percent t1.initroresorcino3 as follows: 1.362 (A-B)N w Percmt trinitroresorcinoi = where A = ferric ammonium sulfate solution for blank, ml. B = ferric ammonium sulfate solution for sample, a, N = normality of ferric ammonium sulfate solution W = weight of sample in aliquot, grams, Glacial acetic

13、 acid has a high coefficient of expansion; therefore, to -. insure accuracy in the aliquot, the solution must be maintained at the same temperatur until after the aiiquat is take-fi. 8 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-i MLL-T-50hLl 13

14、m 7777706 0328737 7 MILT- 50611 (MU) 4.5.3 Assay hy titration with standard alkali. Transfer 0.4 gram of Add 1!j ml. of wann Run a blank determination. the dried sarqle (from the moisture determination), accurately weighed to O.lmgt, to a wide mouth 500 mi. Erlenmeyer flask. water and swirl until di

15、ssolved. of 2 percent alcoholic phenolphthalein solution and titrate to a pink color with 0.1N sodium hydroxide solution. Calculate the percent trinitroresorcinol as follows: Cool to room temperature, Add 5 drops 12.26 (A-B)N w Percent trinitroresorcinol = where A = sodium hydro,xide solution for ti

16、tration of sample, m. B = sodium hydroxide solution for titration of blank, ml. N = normality of sodium hydroxide solution, H = weight of sample, grams. t 4.5.4 Melting point. Dry a sample for the melting point determination, residue on ignition,water-insoluble natter, alcohol-insoluble matter, sulf

17、ate, and granulation by transierring about 30 gram gortign to a large porcelain dish (or watch glass) and heating at 68 f 2 C for 8 to i6 hours. Add a sample to a melting point capiiary tube (0.9 to 1.2 mm in diameter and 10 cm high) (see 6.3.1). in 3 portions until the height of the trinitroresorci

18、nol in the column is about 3-4 mm. Detemine the rnsltin;: point by the use of a Vanderkamp apparatus (or other suitable apparatus) (see 6.3.2) . ReguLate the electrical heating system so that the rise in temperature in the vicinity of the melting point is 1% every 3 minutes. Observe the capilary tub

19、e through the magnifying giass and record as %he melting point, the point at which the last solid particles have disappeared. Transfer to a stoppered bottle. Tap the capillary on the table top after each addition. 4.5.5 Residue on ignition, Transfer 3 grams 0.t the dried sample to a tared platinum d

20、ish. Add 4. nl. of nitric acid and evaporate to dryness on the hot plate at moderate heat, Add 15 ml. of nitric acid and 3 ml. of sulfuric acid and evaporate to dryness on the hotplate at the highest heat. until the sulfuric acid has evaporated and then heat in a muffle furnace at 750C for 15 minute

21、s. the pexent residue on ignition as follows: Carry along a blank determination. Heat over a Meker burner Cool in a desiccator and weigh. Calculate 100 (A-B) w Percent residue on ignition = where A = weight of residue, grams B = weight of residua in blank, grams W = weight of sample, grams 9 Provide

22、d by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-KELT- 506XI(W) 4.5.6 Fater-insoluble matter, to a 400 mi., beaker and add 300 ml. of water. Heat to boiling and stir crucibhe of msdium porosity and transfer and wash with hot water. at 105 C for 1 hour, cool

23、in a desiccator and weigh. percent water-insoluble matter as foilows: Transfer 2 grams of the dried sainple Dry . untildissolvsd. Filter immediately through a tared sintered glass Calculate the Percent wate-insoluble matter = - 100A w where A = weight of residue, grams W - weight of simple, grms 4.5

24、.7 Alcohol insoluble matter. TransTer 4 grams of the dried sample to a 250 gil. beaker. Add 120 ml. of 95 percent ethyl alcohol and stir with a stirring rod. Cover with a watch glass and heat to boiling on an electrc hot plate with occasional stirring, Filter while hot through a tared sintered glass

25、 crucible of medimorosity. Transfer and wash with 95 percent ethyl alcohol Dry at 105 C for 30 minutes, cool in desiccator, and weigh. Calculate the percent alcohol-insoluble matter as follows: Percent alcoho-insoluble matter = - 1OUA W where A = weight of residue, grams W = weight of sample, grams

26、4.5.8 Sulfate. Transfer 5 grams of the dried sample to a 2% ml, beaker. Add 0.5 gram of sodium chloride, 25 mL. of hydrochloric acid, and 25 in. of nitric acid, to volume of about 1 to 2 ml. Add LO ml. of hydrochioric acid and again evaporate to a volume of 1 to 2 ml. aboutl(i0 mi, of hot water. Fil

27、ter through a Whatman No. wash with warm water, and discard the filter paper. Heat the filtrate to boiling, add 10 ml. of 10 percent barium chloride solution (10 percent), and boil for 1 or 2 minutes. Allow to stand overnight, a Whatman No. 42 filter paper and transfer and wash with 1 percent hydro-

28、 chloric acid solutioa. platinum crucible and carefully char and burn off the filter paper at duU red heat, Finally ignite at red heat for 45 minutes. Cool in a desiccator and weigh. Carry along a blank determination, Evaporate Add 5 ml. of hydrochloric acid and filter paper, Filter through Transfer

29、 the filter paper and precipitate to a tared Calculate the percent sulfate (as H$OL) as follows: 7 42-02 (A-BZ B Percent sulfate including resorcinol dsulfonic acid (as l$Xlk) = where A = weight of residue, grams B = weight of residue in blank, grams W c weight of sample, grams . Provided by IHSNot

30、for ResaleNo reproduction or networking permitted without license from IHS-,-,-c MIL-T-50bLl 13 777770b 0328743 7 t MILT-506 11 (MU) 4.5.9 Granulation. Transfer 10 grams of the dried sample to a U, S. standard sieve No. 40 (conforming to the requirements of RRc-366), 3 inches i.i diameter, to which

31、a bottom pan has been attached, by hand or with a standard vibrating machine. the sieve, brush it out into a tared weighing dish, dry at 68 C for 2 hours, cool in a desiccator, and weigh, Caculate the material that does not pass through the KO. 40 sieve as follows: Shake for 3 minutes If any residue

32、oremains on Material not passing through Mo. 40 siive = - 1OOA w where A = weight of residue, grams Note. Wash the sieve and pan well with water after finishing a.test, W = weight of sample, grams 5. PFBPARATION MIR DlCJVERY 5.1 Packing. 5,1bl. Level A. Trnitroresorcinol shall be packaged in a heat

33、sealed polyetfiylene bag in accordance with PPP-C-301 inside a lined fiber drum conforming ix PPP-by23 type III, class 1, Ekch drum shal not exceed 200 pounds net (see 6.2). 5.1.2 Level B. Trinitroresorcinol shall be packaged in a heat-sealed polyethylene bag in accordance withPPP-E301inside a lined

34、 fiber drum conforming to PPP-D-723, type II, grade A. Each drum shall not exceed 100 pounds net (see 6,2). 5.1.3 Level C. Trinitroresorcino, shall be packed in shipping con- tainers in accordance with PPP-(3-301 for shipment from the supply source to the first receiving activity for hediate use. co

35、mply with Consolidated Freight Classification Rules or other common . carrier regulations applicable to the mode of transportation (see 6.2). 5.2 Marking, in addition to aqy special marking specified, shipping containers shall be marked In accordance with MIGSTLl29. Containers shall 5.2.1 Special la

36、beling. Each container of trinitroresorcinol shall be abelec as follows: TRINITRRESORCINOL Do not take internally Avoid breathing dust Can cause skin irritation Can be absorbed . Wash thoroughly through the skin after handling u Provided by IHSNot for ResaleNo reproduction or networking permitted wi

37、thout license from IHS-,-,-.& MIL-T-50611 13 W 777770b 0328742 7 W MIGT-506ll (MU) 6. NOTES 6.1 Intended use. Trnitroresorcinol covered by this specification is intended for use in the nanufacture of lead styphnate and as a constituent in some primers. 6.2 Ordering data. Procurement documents shodd

38、specify the following: Title, number and date of this specification. Type required. Sim and type of shipping container. Level of packing desired (see section 5). Weight of trinitroresorcino1 to be packed in a shipping container. f Special labeling (see 5.2.l), g Moisture content of materi+l to be sh

39、ipped. 6.3 Sources of equipment, 6.3.1 Capillary tubes, Catalog No. 641-2P, can be procured from Arthur . H. Thomas, Philadelphia, Pa. 6.3.2 Vanderkmp apparatus, Catalog No. 63, ML1945, can be procured from Scientific Glass Apparatus Co., Inc., Bloomfield, N. J. 6.4 Ssnrpling and testing precautions

40、. Trinitroresorcino1 when shock& or exposed to heat is an explosion hazard and should be handled with care. Gust odian: AZllJT-MIJ Review activities: Anny-W Preparing activity: Aw=m Project No. 1376-AO7g 12 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-.- MIL-T-50611 13 1 . TO SOURCE OF INERT TITRATION td GAS FLASK -=J=j=jTC HUMIDIFIER f V 90 I 8tOD) PYREX GLASS FLASK. BULB CAPACITY - SOO mi. AU. DIMENSIONS IN MILLIMETERS. . 1 I Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-