ARMY MIL-B-153 A-1964 BARIUM PEROXIDE《过氧化钡》.pdf

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1、I i I 1 I 1 .I 1 t t I ! MIL-B-LC3A 68 9779906 OLL3351 7 M - MIL=B-l53A 30 SEPTEnIBER 196rE SUPERSEDING JAN-B-153 30 NOVEMBER 1944 AMENDMENT 1 21 APRIL 1953 MILITARY SPECIFICATION BARIUM PEROXIDE This apeoifioation has bem approved by the Departmsnt of Defense and ia man- datopy for we bu all Depart

2、mente and Agentxh of ths Department of Defense. 1. SCOPE 1.1 Scope. This specification covers anhy- drous barium peroxide for use in pyrotech- nic mixtures. 1.2 Classification. Barium peroxide shall be of the following grades and classes, as specified (see 6.2) : Grade A Class 1 Class 2 Grade B -2.

3、APPLICABLE DOCUMENTS 2.1. The following documenta of the issue in effect on date of invitation for bids or re- quest for proposal, forms a part of this spe- cification to the extent specified herein. SPECIFICATIONS FEDERAL EP-378 - Polyethylene Film, Thin Gauge RR-S-366 - Sieves ; Standard, Teat- in

4、g MILITARY MILD-3464 - Desiccants, Activated, Bagged, Packaging Use and Static De- humidification MIL-D-6064 - Drums, Metal-Shipping and Storage MIED-26993 -Drum, Fiber, for Do- mestic Shipment of Desiccant STANDARD MILITARY MILSTD-129 - Markhg for Shipment and Storage THIS MCUMEiW CONTAJNS PAGES. /

5、t/ Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-B-153A 68 m 777990b 0113352 9 m MIEB-153A (Copies of spedcations, standards, drawings, and publications required by mxppiers in wnnec- . tion with specific procurement frrnctions should be obtain

6、ed from the procuring activity or as directed by the contracting officer.) 2.2 Other publications. The foilowing docu- ment forms a part of this specification to the extent specified herein. Unless otherwise in- dicated, the issue in effect on date of invita- tion for bids or request for proposal sh

7、all apply * INTERSTATE COMMERCE COMMISSION 49 CFR 71-78 - Interstate Commerce Commission Rules and Regulations for the Transportation of Explosives and Other Dangerous Articles ” (TG interstate Commerce Commission reguia- tions are now a part of the Code of Federal lliremsnta. Thru No. 100 U.S. Stan

8、dards deve . Thru No. 140 U.S. standards sieve, min. Thru No. 170 U.S. etandard Sieve, min. i. 96 Thru No. 200 U.S. standard sieve, min. Thru No. 326 U.S. standard aieve, min. 3.4 Workmanship. The barium peroxide shall be free flowing and free from lumps, grit, foreign matter or injurious material.

9、4. QUALITY ASSURANCE PROVISIONS 4.1 Responsibility for inspection. Unless otherwise specified in the contract or pur- chase order, the supplier is responsible for the performance of all inspection require- ments as specified herein. Except as other- wise specified, the supplier may utilize his own f

10、acilities or any commercial laboratory acceptable to the Government. The Govern- ment reserves the right to perform any of the inspections set forth in the specification where such inspections are deemed necessary 6 assure supplies and services conform to prescribed requirements. 4.2 Lot. A lot shal

11、l consist of 6,000 pounds maximum. ? 4.3 Sampling. Select 10 percent but in no case more than 10 of the containers in such a manner as to be representative of the lot. Select by thief method a one pound sample from each 6th consecutively numbered con- tainer; Le., Sth, loth, 16th, etc. drum until 10

12、 samples have been obtained representing a 6,000 pound lot. Divide each-sample. into y2 one-half pound samples placing them in sealed airtight containers properly labeling each to identify it with the drum number and lot number. Blend half the number of one-half pound samples and take one pound of t

13、his blend tg make a composite sample for acceptance analysis in accordance with re- quirements set forth in paragraph 3.2. The additional samples will be analyzed for avail- able oxygen content and half in storage for possible future tests. If during sampling, it becomes apparent that the lot is not

14、 uniform throughout, the inspector may test or require tests to be made on any portion of the lot for compliance with the requirements of the spe- cification. 4.4 Tests. 4.4.1 Moisture content. Accurately weigh approximately 10 gms. of the samples in a tared weighing bottle, approximately 6 cm. ln d

15、iameter and place in an oven at 276“ plus or minus 2F for 11/2 hours. Cool in a desic- cator, weigh and calculate the loss in weight as percent moisture in the sample. 4.4.2 Apparent density test. Assemble a Scott volumeter as shown in figure 1, having a No. 8 U. S. standard sieve in the upper hop-

16、per, so that the tared receiving cube, one cubic inch in volume, is directly under the lower funnel and rests on the base of the ap paratus. Slowly pour approximately 15 to 20 gm. of the sample into the hopper and brush if necessary through the sieve in order to fill the receiving cube to overflowin

17、g. By means of a spatula, carefully strike off the excess barium peroxide from the cube taking care not- to jar the cube during this operation. Weigh the cube and contents, and from the volume and weight of barium peroxide cal- culate its apparent density. Make three tests and calculate the average

18、of the apparent density values as follows: 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-B-153A 68 777770b 0113354 2 9 W D=- V where D = apparent density W = gm. of sample V = volume of receiving cube in ml. 4.4.3 Avaihxble oxygen content. We

19、igh 0.36 ta 0.40 gm. of sample on a tared watch glass. To a 300 ml. tall form beaker add 70 mi. of acid solution (100 mi. of 70 percent perch- loric acid, 30 mi. of 86 percent phosphoric acid and 0.1 gm. of manganese chloride made up to one liter with distilled water.) From a burette run into the b$

20、aker about % of the amount of N/10 potassium permanganate needed for the titration. Then while this so- lution is being mechanically stirred, carefd- ly add the sample to it and wash down the watch glass with a fine stream of acid solu- tion. Cover the beaker with a holed watch glass. .After solutio

21、n of the sample is com- plete, titrate with N/10 potassium perman- ganate. Calculate the percent available oxy- gen as follows: 0.8 VN Percent available oxygen = - W where V r: ml. of *N/O potassium perman- . ganate solution used N =normality of N/O potassium permanganate solution . W 5 gm. of sampl

22、e (Note. Prime importance ahodd be attached to time and spiution of the sample in testing barium peroxide, as with ali peroxides. The sample should -be dissolved completely a8 rapidly as possible, and Che titration must fdow immediately. Any delay will mue a lower muit regardless of e crucible and w

23、mh thoroughly with hot water. Dilute the solution to 160 ml., pass through a Jones re- ductor, and titrate with approximately 0.03N potassium permanganate solution. Run a blank determination on 200 ml. of 6 percent sulfuric acid passed through the reductor. 6.6VN Percent iron = - W Provided by IHSNo

24、t for ResaleNo reproduction or networking permitted without license from IHS-,-,-flIL-B-L53A 68 7777906 OLL3355 4 where V = ml. of potassium permanganate used, corrected for blank N = normality of the permanganate solution W = gm. of sample 4.4.4.2 Calcium content. Transfer 2 gm. of sample to a nick

25、el crucible and fuse with about 10 gm. of anhydrous sodium carbon- ate. Dissolve the melt by boiling with 200 ml. of distilled water in a 400 ml. beaker. Cool, remove the crucible, and wash with hot wa- ter. Filter the solution and wash with hot water. (Retain the filtrate for the determina- tion of

26、 chlorides). Place the filter paper con- taining the residue into a 260 ml. beaker to which is added a minimum but sufficient amount of 1 :1 nitric acid to dissolve the resi- due. Boil the solution for a few minutes and filter. Wash with warm water. Evaporate the filtrate carefully to dryness. Disso

27、lve the res- idue in a minimum amount of water, add 60 ml. of amyl-alcohol, and boil (away from flame) until the volume is reduced to 20 ml. Filter and wash the residue with 3 ml. por- tions of amyl alcohol. Save the residue for the determination of strontium. Evaporate the filtrate to dryness, add

28、10 ml. of distilled water, and boil for 10 minutes. Filter the so- lution and wash with distilled water, keep- ing the volume of the filtrate at not more than 76 ml. Add 6 ml. of concentrated am- monium hydroxide, 6 ml. of 10 percent am- monium chloride solution and 5 ml. of sat- urated ammonium oxa

29、late solution. Heat on a steam bath for at least 2 hours. Filter and wash thoroughly with hot 1 percent am- monia solution. Place paper and precipitate in a weighed pIatinum crucible. Dry and burn off the paper at a low temperature. Ignite at red heat for 3 minutes. Cool, and weigh. Calculate the pe

30、rcent calcium as follows: 71.47A Percent calcium = - B where A = gm. af calcium oxide 3 = gm. of sample MIGB-153A 4.4.4.3 Strontiwn content. Dissolve the midud nitrates from the calcium determin- ation in approximately 76 ml. of water. Transfer to 100 ml. volumetric flask, dilute to mark with water

31、and mix. Remove a 25 mI. aliquot. Add 76 ml. of water and acidify solution with acetic acid. Add 2 gm. of am- monium chloride and add ammonium hydrox- ide until the solution has a faint odor of am- monia. Heat to boiling, let the precipitate settle, and filter. Wash the precipitate with hot 1 percen

32、t ammonium chloride solution made ammoniacal to methyl red. Discard the precipitate. Acidify the filtrate with acetic acid and add 10 ml. of 30 percent ammonium acetate solution (neutralized with ammoni- um hydroxide). Bring the solution to boil- ing and while swirling, add sufficient 10 per- cent a

33、mmonium dichromate solution to pre- cipitate all the barium. Allow to settle, de- cant the clear liquid through a filter, and wash the precipitate with neutral 1 percent ammonium acetate solution until the filtrate is no longer perceptibly colored. Save the filtrate, Transfer the precipitate by a je

34、t of water to a beaker, place the beaker under the funnel, dissolve the precipitate on the paper with warm 1:l nitric acid and wash the paper with hot water. Add more acid if necessary until the precipitate is completely dissolved. Add a few drops of 10 percent ammonium dichromate followed by dilute

35、 ammonium hydroxide slowly and with stir- ring until the precipitate first formed no longer redissolves. Add 10 ml. of neutral 30 percent ammonium acetate solution, bring the solution to boiling while keeping it in swirling motion, and cool slowly. Filter and wash with 1 percent ammonium acetate so-

36、 lution. Discard the residue. Add a little ni- tric acid to the combined filtrates, and evap- orate to a small volume. Add ammonium hy- droxide until the solution has a faint odor of ammonia. Then add an excess of 1 percent ammonium carbonate solution. Allow the pre- cipitate to settle, filter and w

37、ash with a little hot water. Dissolve the residue in just enough I :1 hydrochloric acid. Add a ten-foId excess of dilute sulfuric acid and then a Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-B-353A b 9999706 0333356 b volume of alcohol equal t

38、o that of the solu- tion. Stir, let stand for 12 hours, filter and wash with 60 percent alcohol containing a little sulfuric acid, then with 95 percent al- cohol till the acid is displaced. Dry paper and residue, transfer to a platinum crucible burn off the paper at as low a temperature- as possible

39、. Heat to dull redness, cool, and weigh as strontium sulfate. Calculate the percent strontium as follows : 190.8A Percent strontium = - w where A = gm. of strontium sulfate W = gm. of sample 4.4.4.4 Magnesum content. Transfer 5 gm. of the sample to a 250 ml. beaker and decom- pose the peroxide by th

40、e addition of 10 ml. of concentrated hydrochloric acid in small portions. Dilute to 50 ml. and warm until the sample is completely dissolved. Add 6 gm. of ammonium acetate and a slight ex- cess of ammonium hydroxide. Heat to boil- ing, boil for 1 minute and lter, washington with hot water. Heat the

41、filtrate to approx- imately 176F and add a fresh 2 percent al- coholic solution of 8-hydroxyquinoline in 95 percent ethyl alcohol in small amounts until the solution is distinctly yellow. Add am- monium hydroxide until the solution is al- kaline to phenolphthalein paper. Stir vigor- ously, scratchin

42、g the sides of the beaker, un- til precipitation begins, Let settle while warm and cool in running water for 30 min- utes. Filter through a medium paper and wash with a hot solution containing 6 per- cent ammonium acetate and 6 percent am- monium hydroxide until the washings are coIorless. Dissolve

43、the precipitate from the paper in 50 ml. of 10 percent hydro- chloric acid, catching the solution in a 260 ml. Erlenmeyer flask. Add 3 drops of 1 per- cent aqueous indigo-carmine solution and ti- trate plith approximately 0.05 N potassium bromate-bromide solution until the color of the solution turn

44、s yellow and add 2 ml. in excess. Immediately ad& 5 ml. of freshly pre- pared 20 percent potassium iodide solution and titrate with approximately 0.06 N so- dium thiosulfate solution until the brown color has .almost disappeared. Add 5 ml. of 1 percent starch solution and stir vigorously after the a

45、ddition of each drop of thiosulfate solution near the end point. Determine the bromate-bromide titer of the thiosulfate so- lution as follows: Pipet 10 ml. of the bro- mate-bromide solution into a 250 ml. Erlen- meyer flask, add 5 ml. of concentrated hy- drochloric acid and 5 ml. of a freshly pre- p

46、ared 20 percent potassium iodide solution. Titrate with the thiosulfate solution until the yellow color has almost disappeared, add 60 ml. of 1 percent starch solution, and con- tinue the titration to the disappearance of the blue color. The titer is equal to 10.00 divided by the number of ml. of th

47、iosulfate solution used. Calculate the percent magne- sium as follows : 0.304 (V - vF) N W Percent magnesium = where V = ml. of bromate-bromide used v = ml. of thiosulfate used F = bromate-bromide titer of the thiosulfate solution N z normality of the bromate-bro- mide solution W = gm. of sample 4.4

48、.4.5 Sodum content a. Magnesum uranyl acetate reagent. Prepare magnesium uranyl acetate reagent as follows : Prepare solution A by mixing 86 gm. of crystallized uranyl acetate with 60 gm. of glacial acetic acid and diluting to 1 liter with distilled water. Prepare solution B by mixing 500 gm. of cry

49、stallized magne- sium acetate with 60 gm. of glacial acetic acid and diluting to 1 liter with distilled wa- ter. Heat each mixture at approximately 168F until the salts are dissolved. Mix the 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-WIL-B-153A 68 m 7777906 OLL3357 8 m two solutions and cool to 68F. Place the beaker containing the mixture in water at 68F and maintain it at this temperature for 2 hours. With the a