ARMY A-A-59339-1998 GUANIDINE NITRATE《硝酸盐》.pdf

1、 A-A-59339 9018054 0003356 03b METRIC A-A- 5 93 3 9 September 15, 1998 SUPERSEDING MIL-G-63431 (AR) September 15, 1981 COMMERCIAL ITEM DESCRIPTION GUANIDINE NITRATE The General Services Administration has authorized the use of this commercial item description, for all federal agencies. 1. SCOPE. Thi

2、s CID covers the general requirements for Guanidine Nitrate (GN) used in military explosives. 2. SALIENT CHARACTERISTICS. 2.1 Properties. The GN shall meet the requirements in Table I when tested in accordance with the applicable paragraphs. The quantity shall be as specified in the contract or orde

3、r (see 6.2). 2.2 Granulation. The GN shall be a white, free flowing material which is free from dirt, oil, grease, or other visible impurity and shall conform to the requirements specified herein. The GN shall have a U.S. Standard Sieve Number of 16 and the quality of material passing through the si

4、eve shall be at least 95% GN by weight. 3. QUALITY ASSURANCE PROVISIONS. 3.1 Product Conformance. characteristics of this commercial item description, confrm to the producers own drawings, specifications, standards, and quality assurance practices, and be the same product offered for sale in the com

5、mercial market. The government reserves the right to require proof of such conformance. Beneficial comments (recommendations, additions, deletions) and any pertinent data which may be of use in improving this document should be addressed to: Commander, US Army TACOM-ARDEC, Attn.: AMSTA-AR-QAW-E, Bld

6、g. 12, Picatinny Arsenal, NJ 07806-5000 by using the Standardization Document Improvement Proposal (DD Form 1426) appearing at the end of this document or by letter. AMSC N/A FSC 6810 The products provided shall meet the salient DISTRIBUTION STATEMENT A. Approved for public release; distribution is

7、unlimited. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-A-A-59339 m 9018054 0003357 T72 I Properties Requirements Test Paragraphs A-A-5933 9 Total Volatiles (Percent Purity (%) Ammonium Nitrate (%) Melamine (%) Ash (%) Sulfate as Na2S04 (%) Free A

8、mmonia (%) Water Insolubles (%) Temperature Rise (OC) (%) 0.8 (Maximum (Max.) 96. O (Minimum) 1.8 (Max.) 0.2 (Max.) 0.5 (Max.) 0.1 (Max.) 0.5 (Max.) 0.2 (Max.) 36 (Max.) 3.4.1 3.4.2 3.4.3 3.4.4 3.4.5 3.4.6 3.4.7 3.4.8 3.4.9 3.2 Granulation. The granulation of the GN shall be determined in accordance

9、 with method 204.1 of MIL-STD-650. Free flowing of the GN shall be determined by visual examination when the GN is poured on the nest of sieves. 3.3 Sampling. Two individual representative 2OOg samples from each batch or lot of the GN shall be obtained as specified in ASTM E300, section 25. Each sam

10、ple shall be tested independently in accordance to the applicable methods specified in 3.4. If either sample fails to meet any of the test requirements, the batch or lot shall be rejected. 3.4 Test methods. The tests used to determine compliance with the requirements stated in Table I shall be perfo

11、rmed on the GN samples obtained in 3.3. All tests given in this section shall be performed using prescribed procedures for replicate determinations given in standard analytical chemistry textbooks or in accordance with ASTM D2905. Unless otherwise specified herein, all chemicals shall be Reagent Gra

12、de or ACS Grade. 3.4.1 Total volatiles. Transfer to a tared glass-stoppered weighing bottle (or a tared aluminum can with a lid) an accurately weighed portion of approximately two grams (4) of the sample. With the stopper off, place the sample, weighing bottle and stopper in an oven at 1,OO“C to 105

13、% for three hours, remove and cool in a desiccator, and weigh. Calculate the loss in weight as percent total volatiles as follows: Percent total volatiles = A-B (100) A Where : A = Weight of specimen before drying (9) B = Weight of specimen after drying (9) 3.4.2 Purity. 3.4.2.1 Preparation of preci

14、pitation/waching solution. Add 7.5g of reagent qrade picric acid, 0.075g of reagent grade GN, and 8 milliliters (mL) of concentrated ammonium hydroxide to a 1000mL volumetric flask. Add 5OOmL of distilled water to the flask and mix thoroughly. Fill the flask with distilled water to the calibration m

15、ark and allow to stand for approximately 10 days before use. 2 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- A-A-59339 m 90L8054 0003358 909 m A-A- 5 9 3 3 9 b 3.4.2.2 Procedure. Weigh 0.2g of reagent grade GN into a 250mL flask. Add 15mL distille

16、d water and 5 to 10 drops concentrated ammonium hydroxide. Heat the flask and contents on a hot plate until the GN dissolves. Remove the flask from the hot plate and allow it to cool to room temperature and filter through filter paper. To the filtrate slowly add 100mL of the precipitation solution p

17、repared in 3.4.2.1 to the GN solution while continually swirling the flask. Allow the solution to stand 8 to 12 hours at room temperature, then filter through a porcelain filtering crucible, of fine porosity, which is attached to a vacuum system containing a crucible holder and filtering flask. Rins

18、e the flask with portions of the precipitating/washing solution. Wash the precipitate with the washings in the flask. Evacuate the crucible to dryness. Dry the filtering crucible and contents to a constant weight in a drying oven at 105OC + SOC. Cool the filtering crucible and contents in a desiccat

19、or and weigh. Calculate the value of the GN to guanidine picrate factor (A) as follows : A = C (D) 100 (B) Where : A = GN to guanidine picrate factor B = Weight of precipitate in crucible (9) C = Weight of sample used (9) D = Purity of GN reagent in percent (%) 3.4.2.3 GN purity determination. Repea

20、t the procedure described in 3.4.2.2 using the GN sample instead of the reagent grade GN. Calculate the percent GN as follows: Percent GN = E (A) (100) W Where : E = Weight of precipitate in crucible (9) W = Weight of sample used (g) A = GN to guanidine picrate factor determined in 3.4.2.2 3.4.3 Amm

21、onium nitrate. 3.4.3.1 Preparation of the formaldehyde solution. Add a few drops of phenolphthalein to a 25mL of formaldehyde. Slowly titrate the solution with 0.5N or 0.33N sodium hydroxide to a faint pink color. 3.4.3.2 Procedure. Add an accurately weighed portion of the sample, approximately log,

22、 to a 400mL beaker containing 200mL water. Heat the contents of the beaker on a hot plate and stir the solution until all the GN dissolves. To the beaker and contents add 5.0mL of the standardized formaldehyde, then 2 to 3 drops of phenolphthalein solution. Titrate the solution with 0.5N or 0.33N so

23、dium hydroxide to a faint pink color. Calculate the percent ammonium nitrate as follows: Percent ammonium nitrate = A (N) (M) (100) 1000 (W) Where : A = mL of sodium hydroxide used in titration N = Normality (N) of sodium hydroxide M = Molecular weight of ammonium nitrate W = Weight of GN sample (9)

24、 3.4.4 Melamine. To a 250mL volumetric flask, containing 200mL hot water (7OOC to 80C), quantitatively transfer an accurately weighed portion of the sample, 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-A-A-59339 90313054 0003359 45 A-A-5 93 3 9

25、approximately log. Mix the contents of the flask until sample dissolves completely. Allow the contents of the flask to cool to room temperature and fill the flask to the mark with distilled water and mix. Pipette a 50mL portion of the solution into a 250mL beaker and perform a potentiometric titrati

26、on on the solution using 1N sulfuric acid and a calomel/antimony electrode. The potential shift occurs at a pH of approximately 3.5 (190 to 200 millivolts). Calculate the percent melamine as follows: Percent melamine = A (N) (M) (100) 100 (P) Where : A = mL of sulfuric acid used in potentiometric de

27、termination N = Normality (N) of the sulfuric acid M = Molecular weight of melamine (126) P = Weight in grams of GN introduced in the potentiometric determination. This value may be calculated as follows: P = A (B) C Where : A = Weight of GN dissolved (9) B = Volume of solution used in analysis (mL)

28、 C = Capacity of volumetric flask (mL) P = 2.0 when sample size, flask size, and solution volume drawn with pipette are exactly as detailed in the procedure 3.4.5 - Ash. a tared porcelain crucible which was properly cleaned and dried. Carefully and slowly heat the crucible until sample decomposes. C

29、ontinue heating in an electric furnace (900OC allow to stand for two minutes, then record the temperature (NOTE: The temperature should be between 25OC and 3OoC.) Add a weighed portion of 18g f 0.lg of the GN sample, using a triple beam balance (of at least 2OOOg capacity), into the flask. At the en

30、d of two minutes, record the temperature; then dispose of the mixture in the approved waste container. Calculate the temperature rise by subtracting the initial temperature from the final temperature. A duplicate determination should be made. 4, PACKAGING. Preservation, packing, and marking shall be

31、 as specified in the contract or order. 5. NOTES. 5.1 Source of documents. 5.1.1 The Code of Federal Regulations (CFR) is available by mail order from the Superintendent of Documents, ATTN: New Order, PO Box 371954, Pittsburgh, PA 15250-7954. 5.1.2 ASTM standards are available from the American Soci

32、ety of Testing and Materials, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959. 5.2 Ordering data. Procurement documents should specify the following: a. Title, number, and date of this CID. b. Issue of Department of Defense Index of Standards and Specifications (DODISS) to be cited in the so

33、licitation, and if required, the specific issue of individual documents referenced. c. Quantity required (see 2.1). d. Packaging and marking requirements (see 4). 5.3 Lot formation. An indefinite quantity of GN produced by one manufacturer, in accordance with the same specification, or same specific

34、ation revision, under one continuous set of operating conditions. Each lot shall consist of that quantity of GN that has been subjected to the same unit chemical or physical process intended to make the final product homogeneous. 5.4 Material Safety Data Sheets. Products meeting the requirements of

35、this CID may be subject to the requirements of 29 CFR 1910.1200 and FED-STD-313 for Material Safety Data Sheets (MSDS). 5.5 Transportation issues. be subject to the requirements of 49 CFR 100-185 for transportation of Products meeting the requirements of this CID may explosives and other dangerous a

36、rticles. 5.6 Precautionary information. Precaution: This CID covers sampling and testing of toxic or hazardous materials. Accordingly, it is emphasized that 6 c Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-A-A-59339 901805q 00033b2 33T A-A- 5 9 3

37、3 9 all applicable safety rules, regulations, and procedures must be followed in handling and processing these materials. 5.7 Keywords. Ammonia Ammonia hydroxide Ammonium nitrate Barium chloride Chemi ca 1 s Explosives Formaldehyde Hydrochloric acid Isopropyl alcohol Phenolphthalein Picric acid Sodi

38、um hydroxide Sodium sulfate Silver nitrate Sulfuric acid MILITARY INTEREST: Custodian Amy-AR Review Activity DLA-GS CIVIL AGENCY COORDINATING ACTIVITY: GSA-FSS Preparing Activity: Amy-AR Project 6810-1603 7 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-