ARMY MIL-R-60864-1967 RESORCINOL《雷琐酚》.pdf

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1、MIL-R-60864( HU) 15 December 1967 - FAPD-MI-2450 26 April 1961 MILITARY SPECIFICATION RESORCIIQOL 1. SCOPE AND CLASSIFICATION 1.1 ScoDe. This specification covers resorcinol for use in explosives. 1.2 lasrification. The resorcinol shall be of the following types and classes. Type 1 - Crystal Class 1

2、 - General Class 2 - Special Type II - Powder Type III - Flake, Technical Grade 2. APPLICABLE DOCUMENTS 2.1 The following documents of the issue in effect on date of invitation for bids or request for proposal, form a patt of this specification to the extent specified herein: SPECIFICATIONS R-S-366

3、- Sieves, Standard or Testing Purposes PPP-C-302 - Chemicals, Dry and Paste, Packaging and Packing of PPP-D-723 - Drums, Fiber FSC 6810 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-R-bO8b4 b8 m 9997706 0322258 7 m MIL-R-6 O 864( Hu) STBPJDbRDS

4、 FEDERAL Fed. Test Method Standard No. 791 - Lubricants, Liquid Fuels, and Related Products; Methods of Testing MIL-STD-105 - Sampling Procedures and Tables for inspection by Attributes MIL-STD-129 - Harking for Shipment and Storage (Copies of specifications , standards, drawings, and publication6 r

5、equired by suppliers in connection with specific procurement functions should be obtained from the procuring activity or as directed by the contracting officer .) 2.2 Other ubiications. The following documents form a part of this specification to the extent specified herein. Unless otherwise indicat

6、ed, the issue in effect on date of invitation for bids or request for proposal shall apply. MBIGAN SOCIETP FOR TESTING AND MbTEaLs ASIM D-1193-66 - Reagent Water ASTM D-1631-58T - Method of Test for ASm Color of Petroleum Products AS!iM D-1631-59T - Uater in Phenol and Related Materials by the Iodin

7、e Re a ge nt Me thod (Application for copies of ASTM publications should be addressed to the American Society for Testing and Materials, 1916 Race Street, Philadelphia, Pa., 19103.) CONSOLIDATED CUSSIFICATION COMITTEE Uniform Freight Classification Rules (Application for copies should be addressed t

8、o the Consolidated Classi- fication Conmiittee, 202 Chicago Union Station, Chicago 6, Illinois.) . Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-R-606 bB W 7779906 0122257 9 3. UQUIREMENTS 3.1 mterial. The materials used in the manufacture of t

9、he resorcin The resorcinol shall conform to the applicable shall be of high quality. requirements a8 epecified herein and shall be visibly free of contaminants and foreign material such as grit and dirt. 3.2 Chemical and Dhveical proverties. The chemical and physical properties of resorcinol shall c

10、onform to the requirements of table I. 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-R-6086q 68 = 7779706 O322260 5 . m al 4 U & al a O & a d 9 o d m h c a m E 9 ri I o rl a a H al FI n 8 w w w 9) a 8 W H al a c e I l l r C H U a c I I l i al

11、 IL, ri VI O 1? VI O moo Q Y?“! 1I.i ao Q)V o0 I I& ao G 4 B H 4 8 i). i Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-. MIL-R-60bLI 68 W 9777906 0322263 7 3.3 Workmenshiii. The resorcinol shall be uniform in quality and shall conform to the requir

12、ements of this specification. 4. QIIALITY ASSUBANCE PROVISIONS 4.1 Insiiection resiionsibilit. Unless otherwise specified in the contract or purchase rder, the supplier is responsible for the performance of all inspection requirements as specified herein. Except as otherwise specified, the supplier

13、may utilize his own or any other inspection facilities and services acceptable to the Government. The Government reserves the right to perform any of the inspections set forth in the specification where such inspections are deemed necessary to assure that supplies and services conform to prescribed

14、requirements. 4.2 Acceptance insii ectioq. Conformance of the resorcinol to the require- ments of this specification shall be determined entirely by means of acceptance inspection. The acceptance inspection shall consist of an examination for acceptability of facilities and quality control methods u

15、sed by the manufacturer, examining and testing the acceptance samples (4.3.2) for all of the requirements of this specification, and an examination of the sample of filled containers (4.3.3) for conformance to section 5. 4.3 Sampling. 4.3.1 u. A lot shall consist of all resorcinol of the same type a

16、nd class, manufactured by the same process, packed as specified in the contract or order (see 6.2) and offered for acceptance at one time. 4.3.2 Sample for test. From each lot offered for acceptance under con- tract, a random sample shall be selected in accordance with MIL-STD-105, inspection level

17、II. removed from each container selected and stored in a large mouth glass stoppered bottle. Each primary sample shall be labeled so that the contain- er from which it was taken can be easily identified. shall be made of equal portions of these samples and a minimum of one pint shall be used for acc

18、eptance tests as specified in 4.4. be labeled to show the name and address of the manufacturer, plant, name of product, specification number, lot number, date of sampling, and contract number. A primary sample of one pint of material shall be A composite sample The sample shall 5 Provided by IHSNot

19、for ResaleNo reproduction or networking permitted without license from IHS-,-,-4.3.3 Samole for examination of filled containers. A random sample of filled containers shall be selected from each lot of resorcinol offered for acceptance under contract, in accordance with MIL-STD-105, inspection level

20、 I and acceptable quality level (AQL) = 2.5 percent defective, to determine compliance with the requirements of section 5. 4.4 JnsDection methodg. Unless otherwise specified, all examinations and tests shall be conducted as specified herein to determine compliance with the applicable requirements of

21、 section 3. Water in accordance with ASTH D-1193 and reagent chemicals shall be used. 4.4.1 Visual inmectiou. Conformance of the resorcinol to the require- ments for material (3.1) and workmanship (3.3) shall be determined by visual inspection. 4.4.2 Resorcinol con tenL. 4.4.2 . 1 peanents . 4.4.2.1

22、.1 Starch indicator solution. Mix 2 gm. of soluble starch and several milligrams of the mercuric iodide (which acts as a preservative) with a little water. Add the mixture slowly to 500 tal. of boiling water and boil for 5 minutes. Cool to room temperature. 4.4.2.1.2 Standard sodium thiosulfate solu

23、tion (aDDroximatelv 0,lN). Dissolve 26 p. of sodium thiosulfate pentahydrate and 0.1 gm. of sodium carbonate in sufficient freshly boiled and cooled water to make 1 liter. Let stand at least 24 hours before standardization. Standardize the solution as follows: Dissolve 0.20 to 0.23 gm. of potassium

24、dichromate, weighed to 0.1 mg. in 60 ml. of water in an iodine titration flask and add 20 ml. of 1 N hydrochloric acid solution. few seconds, and let stand for 10 minutes in the dark. thiosulfate (swirling continuously) until a light greenish brown color appears. until the deep blue starch-iodide co

25、l& changes to a pale bluish green. Calculate the normality of the sodium thiosulfate solution as follows: Stopper the flask, swirl for a Titrate with sodium Add 5 ml. of starch indicator solution, and continue titration A O .04904B Normality of sodium thiosulfate solution = where: A = weight of pota

26、ssium dichromate, gm. B = volume of sodium thiosulfate, ml. 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-1 MIL-R-606Y 68 9999906 0322263 O W MIL-I- 60864(W) 4.4.2.1.3 Potassium bromate-bromide solution (approximatelv 0.2N). Dry potassium bromate

27、 in an oven for 2 hours at 100C and weigh 5.6 gm. into a pyrex bottle. Add 30 gm. of potassium bromide. Dissolve in water and dilute to 1 liter. 4.4.2.2 Procedure. Dissolve 1.5 gm. of the sample (weighed to 0.1 mg.) in water and dilute to 500 ml. in a volumetric flask. Transfer a 20 ml. aliquot to a

28、n iodine flask. Add 25.00 ml. of the bromate- bromide solution to the flask, dilute with 100 ml. of water, add 10 ml. of hydrochloric acid, and immediately stopper the flask. Shake the flask and allow it to stand for 3 minutes. Place 15 ml. of 15 percent potassium iodide solution in the lip of the f

29、lask and remove the stopper just sufficiently to allow the potassium iodide solution to enter the flask without allowing any bromine vapor to escape. shake the flask thoroughly. Wash down the stopper and the neck of the flask with about 20 ml. of water. Titrate the liberated iodine with standard sod

30、ium thiosulfate solution until the solution assumes a light yellow color. Add 5 ml. of starch solution and continue the titration carefully until the blue color in the eolution disappears. Carry out a blank titration using 75 ail. of water, 25.00 ml. of bromate-bromide solution and 10 ml. of hydroch

31、loric acid. ml. of potassium iodide solution, and titrate the liberated iodine by the same procedure used for the sample. Calculate the resorcinol content as follaws : Mix thoroughly. With the stopper in place, After the 3 minute waiting period, add 15 Percent resorcinol = A-B)N x 1.835 W where: A =

32、 volume of thiosulfate solution for titration of blank, ml. B = volume of thiosulfate solution for titration of sample, ml. N = normality of thiosulfate solution. W = weight of sample in aliquot, gm. 4.4.3 AA. Transfer a 5 gm. sample to a tared porcelain crucible and heat gently with a Bunsen burner

33、 until the material is ignited at the surface. After all of the free carbon on the sides of the crucible has burned-off completely, heat the residue with a strong flame or in a muffle furnace at 700“ to 750C until all the carbonaceous material has disappeared, then heat for an additional 30 minutes.

34、 Calculate the percent ash as follows : &move the burner and allow the material to burn completely. Cool in a desiccator and weigh. Percent ash P W where: A =weight of residue, gm. W = weight of sample, gm. 7 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from I

35、HS-,-,-4.4.4 Voi sture. The moisture shall be determined in accordance with ASIM D-1631-59T of Fed. Test Method Std. No. 791, method 3253. 4.4.5 Phenol. Dissolve 1 gm. of the sample in 20 m1. of water and warm gently. Phenol is not present if its odor is not detectable. 4.4.6 Catechol. 4.4.6.1 Reage

36、nts. Lead acetate solution (35 percent). Dissolve 35 gm. of lead acetate trihydrate in water and dilute to 1 liter. should be filtered through No, 40 Whatman filter paper juot before using so that it is free from lead carbonate. This solution 4.4.6.2 Procedure. Weigh a 10 gm. sample into a 400 ml. b

37、eaker. Add 100 ml. of carbon dioxide-free water and stir until dissolved. Add 75 ml. of clear, freshly filtered lead acetate solution, rtir, cover, and allow to stand for 3 hours, protected from fumes of H2S and S02. Filter through a tared fritted glass crucible of medium porosity, woeh with water a

38、nd dry for 2 hours at 105 to 110OC. Calculate the percent catechol as follows: Cool in a desiccator and weigh. Percent catechol = W where: A = weight of precipitate, gm. W = weight of sample, gm. Note: It is essential that water used in the determination be free of carbon dioxide, which reacts with

39、lead acetate to form insoluble lead carbonate. 4.4.7 &. Weigh 5 gin. of the sempie into a 150 ml. beaker. Add 50 al. of water having a pH of 6.8 f 0.2. dissolved and determine the pH by means of a pH meter equipped with glass- calomel electrodes, Stir the mixture until the sample is 4.4.8 Water inso

40、luble. Weigh a 10 gm. sample into a 400 ml. beaker. Add 100 ml. of water and stir until dissolved. glass crucible of medium porosity, wash with water, and dry for 1 hour at 105 to 110C. insoluble as follows: Filter through a tared fritted Calculate the percent Cool in a desiccator and weigh. Percent

41、 insoluble = W where: A = weight of residue, gm. W = weight of sample, gm. 8 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-IL-R-608bV 68 M 7779706 0322265 V MIL-B-60864 (XI) - 4.4.9 Color when molten. The molten color shall be determined in accorda

42、nce with ASTM D-1500-58T. 4.4.10 Solidification or freezing point and melting rame. 4.4.10.1 Amaratus. As shown in figure 1. The thermometer shall include the range of 90 to 120C and shall be corrected. 4.4.10.2 procedure. watch glass overnight in a desiccator containing an efficient desiccant such

43、as fresh Drierite. of water significantly affects the freezing point. Heat the inner test tube (fig. 1) moderately over a flame to remove moisture. 35 p. of sample in this test tube and heat carefully to effect liquefaction. After approximately half of the sample has liquefied, insert the stirrer, s

44、tir with a reciprocating action of the stirrer to effect an even distrihu- tion of the heat, and carefully heat further until complete fusion has been obtained. 12OoC which is desirable. liquid level is at the immersion line of the thermometer. thermometer is free from crystals, heating further if n

45、ecessary. assembly in the insulating jacket and allow to cool while stirring at a rate of about 120 strokes per minute. cooling, meanwhile noting the sample for the appearance of crystals. mally, the sample super-cools slightly, then as crystallization starts, the temperature rises to a plateau, whi

46、ch is maintained for at least one-half minute, and may be retained for several minutes if the assembly is suf- ficiently insulated. This plateau is the freezing point. In the case of impure resorcinol, the plateau may be difficult to observe. seeding the sample near the estimated freezing point with

47、 a few crystals of pure resorcinol usually reduces super-cooling and results in a sustained plateau. First dry the sample of approximately 40 gm. on a This drying is necessary because a small amount Place about The temperature of the fused material may thus be kept bel= Insert the thermometer and st

48、opper so that the Stir until the Place the Obrerve the temperature during Nor- In such a case, 4.4.11 Granulatioq. Place 100 gm. of the sample on a No. 8 U. S. standard sieve (conforming to R-S-366). Cover and shake for 10 minutes in a mechanical shaker geared to produce 300 f 15 gyrations and 150 f

49、 10 taps of the striker per minute. calculate to percentage of sample that is retained. Weigh the portion that is retained and 9 ,. . . ._. . Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-R-6086q 68 7797706 OL222bb 6 MIL-R- 60 8 64( MU) 5. PREPARATION FOR DELIVERY 5.1 Packinn and DackaPinq. 5.1.1 Level A. Resorcinol shall be pa