NAVY MIL-A-23442 A-1965 AMMONIUM PERCHLORATE《高氯酸铵》.pdf

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1、MIL -A-23 442A(Wep) 3 March 1965 SUPERSEDING MIL -A-Z3442(wep) 16 October 1962 MILITARY SPECIFICATION AMMONIUM PERCHLORATE This specification has been approved by the Stopper the flask, agitate the solution, and allow to stand in a dark place for one hour. Titrate with 0.02N sodium thiosulfate solut

2、ion until the blue color disappears. Prepare a blank in the same manner, using similar quantties of reagents. Cal- culate the percent sodium bromate in the sample as follows: 1.51 (A - B) (N) W Percent NaBr03 = where: A = Volume of sodium thiosulfate used or sample, ml B = Volume of sodium thiosulfa

3、te used for blank, ml N = Normality of sodium thiosulfate W = Weight of sample, gm 4.5.5 Chlorides as ammonium chloride. The chloride content of the material shall be determined by turbidimetric precipitation as silver chloride and comparison with a standard, a. Preparation of test sample solution.

4、- Dissolve a 1.0-gm portion of sample, weighed to 0.1 me;, in approximately 45 ml of water and filter. Transfer filtrate to a Nessler tube. Add 1 ml of concentrated nitric acid, 1 nil of 2-percent silver nitrate solution, dilute to 50 ml, and mtx thoroughly, . Provided by IHSNot for ResaleNo reprodu

5、ction or networking permitted without license from IHS-,-,-Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-where: W = Weight of sample, gm B = Volume of ammonium thiocyanate added to blank S = Volume of ammonium thiocyanate added to sample N = Normal

6、ity of ammonium thiocyanate solution, ml solution, ml 4.5.6 Chlorates as sodium chlorate. Transfer a 1-gm portion of sample, weighed to the nearest 0.1 mg, to a glass-stoppered Erlenmeyer flask. Add, at a temperature of approximately 40 degrees C, 30 ml of boiled distilled water an 40 ml of a soluti

7、on containing one part by volume concentrated hydrochloric acid to one part water. Heat at approximately 40 degrees C or approximately 30 minutes. Add 1 ml of O-tolidine reagent, made by mixing 1 gm of O-tolidine in one liter of 10 percent hydrochloric acid, and mix. Allow to stand for five minutes

8、at room temperature and compare the color with that of standards prepared from standard potassium chlorate and treated in the same manner as the sample. This determination will include bromate. A correction for sodium bromate shall be included in the calculation as follows: Percent NaC103 = OoA wher

9、e: - 0.69B W A = Weight of sodium chlorate (calculated) equivalent to the weight of potassium chlorate in closest standard, gm B = Percent sodium bromate in sample (4.5.4) W = Weight of sample, gm 4.5.7 Chromates as potassium chromate. Dissolve 1 grn of sample, weighed to the nearest 0.1 mg, in appr

10、oximately 95 ml of water, filter, and dilute filtrate in a Nessler tube to 100,O ml. Add 3.0 ml of a solution containing one part concentrated sulfuric acid to five parts water and mix. Add 1.0 ml of 0.25-percent diphenyl carbazide solution in alcohol and mix. Prepare a blank in the same manner and

11、add standard (0.0004 gm per mi) potassium chromate solution until the color matches that of the sample 8 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- solution. Calculate the-percent potassium chromate as follows: Percent 3Cr04 = 0.04 A where: W A

12、 = Volume of standard potassium chromate solution added to W = Weight of sample, gm blank, ml 4.5.8 Iron. - Transfer 1 gm of sample, weighed to the nearest 0.1 mg, to an evaporating dish. Add approximately 3 ml of distilled water and 2 ml concentrated hydrochloric acid, and evaporate to dryness on s

13、team bath. Dissolve residue in I ml of concentrated hydrochloric acid and approximately 25 ml of water. Transfer solution to a Nessler tube and add 3 ml of 25- percent ammonium thiocyanate. Simultaneously prepare a blank in the same manner and add standard (0.00005 gm of iron per mi) iron solution u

14、ntil the pink color matches that of the sample solution. Calculate the percent iron as follows: Percent Fe = 100 (A) (B) - W where: A = Volume of standard iron solution added to blank, ml B = Weight of.iron per ml of standard solution, gm W = Weight of sample, gm 4.5.9 Sulfated ash. Ignite a silica

15、crucible with lid at a dull red heat for 30 minutes, cool in a desiccator, andweigh to nearest 0.1 gm. Weigh 5.0 gm of sample to the nearest 0.1 gm Place the crucibIe with lid on a hot plate at high heat. Add the sample in small increments and alow to burn completely, covering the crucible after eac

16、h addition. Add several drops of concentrated sul3rfuric acid and allow to fume off. When dry, place in a muffle furnace at 600 to 700 degrees C for 30 minutes, cool in a desiccator, and weigh. l reagent. Ressrd the wlmies iised and determine the satio R (ni1 Karl Fis:her reagmt pes ml water- nietha

17、no1 reagent), Ropawt this determination anid obtain ai average of the imo ratioa. The range of the calciilsted ratios shall be no more than 0.04. rsceckire - Neutralize the moisture in approximately Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-y M

18、IL -A-23442A(Wep) 100 ml of anhydrous methanol by adding an excess of Karl Fischer reagent and back titrating with water -methanol solution to the end point. Record the burette readings. Introduce 5.0 f 0.1 gm of sample to the neutralized methanol solution. Allow to stir for 5 minutes. Add a visual

19、excess of Karl Fischer reagent. Back titrate with water-methanol to the end point. Record the burette readings and calculate the volumes of Karl Fischer reagent and water-methanol added to the sample solution. Cal- culate the percent water as follows: 0.1 F (K - MR) Percent water = where: W F = Weig

20、ht of water equivalent to one rial of Marl fischer K = Volume of Karl Fischer reagent added to sample solution, ml M = Volume of water-methanol added to sample solution, ml R = Ratio of ml Karl Fischer reagent to ml water-methanol reagent, rng/ml W = Weight of sample, gm 4.5.11 Determination of tota

21、l volatile matter, Transfer a 10-gm portion of sample, weighed to the nearest 0.1 mg, to a tared wide-form moisture dich and weigh Place in a gravity-convection oven and ailow to remain for 2 hours at 177 f 2 degrees C. Cool in a desiccator, and weigh. Cal- culate the percent volatile matter as foll

22、ows: w1 - w2 100 Percent volatile matter = where: ?Vi = Weight of dish plus sample, gm W, = Weight of dish plus sample after heating, gm s = tveight of sample, gm 4.5.12 Partide size determination, The weighted average pastide size shall be determined by the follow8ng procedure: 4.5.12.1 Test proced

23、ure: a. Transfer no less than 500 grn o sample to the riffle sampler -. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-(with d, 8, l/Z-inch openings discharging in opposite directions). Divide the sample, using the riffle sampler. Discard the materi

24、al in the right- hand pan. Redivide the alriaterial froin the left-hand pan, using the riffle saqler, Again discard the material in the right-hand pan. b. Asseirirlble the, sieves in order of niesa size (numbers 50, 70, 100, 140, 200, meeting RR-S-366) with the coarsest sieve on top. Include a botto

25、m pan in the assembly. Transfer 100 gm, weighed to the nearest 0.1 gni, of the material from the left-hand pan of the riffle sample to the top sieve. Add cover plate to the assembly and place in sieve shaker, (Ro-Tap with automatic timer; W. S. Tyler Company or equivalent.) Vibrate for 13 1/2 minute

26、s, c. Starting with the top sieve, use a brush to transfer the contents of the sieve to a sheet of glazed paper. Weigh the material to the nearest 0,1 gm and record the weight and sieve number. Repeat the transferring, weighing, and recording for each sieve and the bottom pan. 4.5.12.2 Calculations

27、a. Calculate the weighted average particle size as follows: Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-A-23442A b 7737906 0338296 b MIL -A-23442A(Wep) b. The weight percent of sample passed through the 50-mesh screen shall be calculated as f

28、ollows: - (wt. sample - wt. retahed) X 100 - W5ass weight of sample . c. The weight percent of sample through the ZOO-mesh screen shall be calculated as follows: 1oow an - w2 weigI of sample 4.5.13 Clarity and color. Dissolve a 10-gm portion of sample in 100 ml of water and transfer 106 ml of soluti

29、on to a Nessler tube. Compare with a standard containing 0.005 gm of potassium chromate per liter. 4.5.14 Determination of pH value. ln a volumetric flask, prepare 100 ml of saturated solution of sample in freshly boiled and cooled distilled water. Determine the pH of this solution at room temperatu

30、re using a potentiometric pH meter, (Model 28, Coleman Instruments, Inc., or equiva- lent) with glass and calomel electrodes. 4.5.15 Heat stability determination. Transfer fous 10-gm portions of sample, weighed to 0.1 rng, to 60-millimeter diameter aluminum weighing dishes which have previously been

31、 heated to approximately 700 degrees C and cooled. Place on shelf located four Inches from top of gravity-convection oven. Maintain oven temperature at I97 A 2 degrees C. Remove-one = sample from the oven dter 2 hours and an additional. sample every hour thereafter. Cool the sample pai a desiccator

32、20 to 30 minutes. Add approximately 5 gm sf cooled sample to a aiaimrture of 100 rnl distilled water, 0.5 gm granular potassium iodide, and 5 ml of 0.2-percent starch solution. Stir to disso.lve ammonium perchlorate, The solution shall remain alano& colorless. Hmmedjate appearance of violet or blue

33、color indicates decom- position. Repeat the procedure for each sample removed from the wen. I i / . 13 ! Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-M1L -A-23442A(Wep) 4.6 Acceptance criteria 4.6.1 Reproduetion. Failure of any sample to meet any

34、requirement of this specification shall be cause for rejection of the Iot. ment of this specification shall cause rejection of the lot, Failure of any sample to meet any require- 5, PREPARATION FOR DELIVERY 5.1 Preservation, packaging, and packing. Unless otherwise specified by the procuring activit

35、y, the preservation, packaging, and packing shall be in accordance with the Code of Federal Regulations 49-CFR 71-90, and MIL-P-1.16, method II, optional submethod. MIL-STD-129. Marking shall include, but not be limited to, the following infor mation: 5.2 Marking. Each container shall be marked in a

36、ccordance with a. Manufacturers name and location b. Material trade name c. Net weight or volume d. Lot number, batch number, and date of manufacture e. Shelf life or storage limitations f. Number and revision letter of this specification 6, NOTES 6.1 Intended use. The material purchased in accordan

37、ce with this specification is intended to be used as an ingredient in some types of rocket motor fuels. 6.2 Ordering data. Procurement documents should specify, but not be limited to, the following information: a, Title, number, and revision letter rrf this specification b, Minimum lot size, if applicable c. Whether preproduction sample is required d. Place of delivery e, Size sf container f. Request for test data g, Type and size of container - _=i 14 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-