ARMY A-A-59410-1999 DMDNB (2 3-DIMETHYL-2 3-DINITROBUTANE)《DMDNB(2 3 -二甲基-2 3 -二硝)》.pdf

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1、A-A-59YLO I 9018054 0004709 630 I INCH-POUND A-A-594 1 O 18 March, 1999 COMMERCIAL ITEM DESCRIPTION DMDNB (2,3-dimethyl-2,3-dinitrobutane) The General Services Administration has authorized the use of this commercial item description, for all federal agencies. 1. SCOPE l. 1 Scope. This commercial it

2、em description covers reagent grade 2,3-dimethyl-2,3- dinitrobutane. 2. SALIENT CHARACTERISTICS. 2.1 Material. The material shall be 2,3 dimethyl-2,3-dinitrobutane (DMDNB) meeting the following requirements: (a) Assay, % DMDNB: 2 98.5% (b) MeZtngpoint, degree C: 210 min. to 214 max. (c) Appearance:

3、The DMDNB shall be milled, and in a granular white crystalline solid (d) Water: Water content in the DMDNB shall be equal to or less than 0.50% (e) Methanoz Methanol content in the DMDNB shall be less than 0.5% (0 Chluride: The chloride content shall be less than 0.02% or 200 ppm (g) FTIR: The DMDNB

4、 when subjected to FTIR analysis shall exhibit a spectrum form. conforming to the attached standard, (Fig. 1). 2.2 Workmanship: The best commercial practice shall be used in the manufacture of this product. Procedures and controls shall be employed to prevent product contamination. There shall be no

5、 contamination (such as dirt, paint chips, wood, etc.) that is obvious and readily observable. In addition, the DMDNF3 shall be free of contaminants which are hazardous, corrosive; reactive, or metallic. Beneficial comments (recommendations, additions, deletions) and any pertinent data which may be

6、of use in improving this document should be addressed to: Commander, US Army TACOM-ARDEC, AITN: AMSTA-AR-QAW-E, Bldg 12, Picatinny Arsenal, NJ 07806-5000 by using the Standardization Document Improvement Proposal D Form 1426) appearing at the end of this document or by a letter. AMSC NIA FSC 6810 DI

7、STRIBUTION STATEMENT A. Approved for public release; distribution is unlimited Licensed by Information Handling ServicesA-A-59410 Llll 9038054 0004710 552 H A-A-59410 3. REGULATORY REQUlREMENTS. 3.1 Safety and Health Practices. This standard does not purport to address all of the safety concerns, if

8、 any, associated with the use of the DMDNB material. It is the responsibility of whoever uses this standard to consult and establish appropriate safety and health practices and to determine the applicability of regulatory limitations prior to use. 3.2 Manufacture Safety Data Statement Manufacture Sa

9、fety Data Statement shall be submitted in accordance with requirements as specified in the Code of Federal Regulation, Part 29-19 10 (OSHA). (For shipment to foreign users, the Manufacture Safety Data Statement may have to conform to the formatting and legislative requirements of the host country.)

10、4. QUALITY ASSURANCE PROVISIONS. 4.1 Product conformance. The product provided shall meet the salient characteristics of this Commercial Item Description, conform to the producers own drawings, specifications, standards, and quality assurance practices, and is the same product offered for sale in th

11、e commercial market The Government reserves the right to require proof of such conformance prior to the first delivery and thereafter as may be otherwise provided for under provisions of the contract. For DMDNB product which has been sold on the market for less than two years, the manufacturer shall

12、 have to demonstrate process stability and to verify product quality by submitting analysis data from the most recent 15 consecutive production batches. Procurement shall not proceed until these data are evaluated and approval is obtained from the procuring agency. (See 6.2 and 6.5). 4.2 Responsibil

13、ity for inspection. Unless otherwise specified in the contract or purchase order, the supplier is responsible for the performance of inspections for the verification of all salient characteristics as specified in Section 2 of this CID. The supplier may use his own or any other facility suitable for

14、the performance of the inspection requirements specified herein, unless otherwise specified in the contract or disapproved by the Government. The Government reserves the right to perform any of the inspections set forth in the CID where such inspections are deemed necessary to assure supplies and se

15、rvices conform to the prescribed requirements. 4.2.1 Bid sample submission. Unless otherwise specified, a sample of 100 grams of DMDNB shall be submitted for inspection and approval in accordance with the terms of the procurement contract. The sample will be subjected to any or all of the quality in

16、spections listed in this CID for verification of compliance to any or all requirements listed in this CID. 2 Licensed by Information Handling ServicesA-A-594 10 4.2.2 Test and inspection results. The contractor shall provide a summary of product test results (or an appropriate form of document of an

17、alysis in accordance with acceptable industry practices) to verify conformance to the salient characteristics requirements. (See 2.). The contractor shall maintain a traceable record of inspection test data adhering to general laboratory practices for fbture reference if required. 4.3 Sampling techn

18、iques and inspection procedures When not specified in this CID, the DMDNB shall be inspected by using acceptable industry-wide sampling techniques and test procedures such as ASTM and ACS sampling and test procedures. Also, unless otherwise specified herein, all chemicals and reagents shall be ACS G

19、rade or Reagent Grade chemicals. Tests for the liquid chromatography and the Fourier Transform Infiared Spectroscopy shall be performed as specified below, (see 6.3): NOTE: The test descriptions described below are not intended to be used as step-by- step laboratory procedures, rather they are inten

20、ded to define the test methods used to obtain the required characteristics. The user should prepare their own laboratory procedures taking into consideration and complying with all aspects of the following test method descriptions. In preparation of step-by-step laboratory procedure, the user should

21、 take into account safety precautions fiom the manufacturer, industry safety and health practices, and also determine the applicability of safety and environmental regulatory limitations. The test descriptions below do not purport to address all the safety concerns, if any, associated with their use

22、. It is the responsibility of the user of the procedure to establish appropriate safety and health practices and to determine the applicability of regulatory limitations prior to use. 4.3.1 Fourier Transform Infrared Spectroscopy (FTIR). This method is strictly qualitative. Visual comparison of the

23、ineared spectrum of the sample with the reference spectra (lower graph, Figure 1) serves to identifl the raw material. Each raw material will have a unique spectrum and any bands not specific to that spectrum will serve as a flag to indicate contaminants, or a spectrum that does not match the refere

24、nce will serve to identify the sample as incorrectly labeled, Material with a spectrum that does not match that of the standard should not be accepted. It is recommended that FTIR be conducted by the receiving agency during acceptance of raw material. 4.3. l. 1 FTIR Analysis Procedure (a) Apparatus.

25、 Fourier Transform Infrared Spectrometer, Nicolet 5DX, or equivalent, programmed in accordance with manufacturers instruction for this specific application. (b) Sample preparation: Add approximately 0.5 g of potassium bromide (KJ3r) and just a small amount (approximately 2.5 mg) of sample to a stain

26、less steel chamber. Add a stainless steel ball bearing to the chamber and place a lid on the chamber. Place the chamber in the sample holder of the Wig-L-Bug vibrator (or equivalent), and vibrate for a minimum of 1 minute. Take out the ball bearing and pour the sample into a stainless steel die. Pre

27、ss the sample into the die with the hydraulic jack to a minimum of 20,000 3 Licensed by Information Handling ServicesT t 7“ L“.,. 7“ 3 “- - - i Licensed by Information Handling ServicesA-A-59410 II 70318054 0004733 261 111 A-A-59410 psi. Remove the ends from the die and place the die in the sample h

28、older of the FTIR spectrometer for analysis. (c) Analysis: Following manufacturers instruction, go to the available libraries in the FTIR computer, choose the correct library (where reference spectra for other solids, and for DMDNB are stored.), select Analyze, then select Search. The top five spect

29、rum matches will be shown on the screen. Select Stack Display of the sample graph stacking the sample spectrum onto the reference spectrum for visual comparison. Annotate all spectra before print out. Print the stack spectra (sample plus reference spectra) for visual comparison. Visually compare the

30、 spectrum of the sample with the reference spectrum for identification of the sample material. (NOTE: Sample spectrum that has been determined through comparison and analysis to be an exact match of the spectra in Figure 1 can be stored in the library of the FTlR computer for use as a standard refer

31、ence.) 4.3.2 Purity assay of DMDNB by HPLC. The DMDNB shall be analyzed by a reversed phase HPLC method using UV detection at 220 nm. The HPLC system used should be comprised of a column, mobile phase, pumping system, sample injection system, detection system and data integrator system. (1) The foll

32、owing apparatus and devices or their equivalents shall be used to perform the HPLC assay analysis: (a). Analytical column: Supelco Supelcosil LC-8-DB 4.6 mm (b) Isocratic pump: Waters 2690 Alliance. (c) Detector: Waters Photo Diode Array 996 or Waters UV 484 (d) Integrator: Hewlett Packard 3395 x 25

33、 cm ph 5-8354 (2) Chemical reagents used in the test shall be HPLC grade acetonitrile, deionized or HPLC grade water. DMDNB used to prepare the standard solutions shall have a minimum purity of 99.9%. The purity of the standards used shall be independently confirmed by a reputable chemical laborator

34、y. If a standard with a purity of 99.9% or above is not available, a less pure standard can be used and the analysis result shall be corrected by multiplying the obtained purity by the fiactional purity of the less pure standard. Whenever a sample which is purer than the certified standard is found,

35、 this purer sample can be and should be used as the new standard provided its assay purity is documented, and is traceable to an independently certified standard. Mobile phase used: 400 mls of HPLC grade acetonitrile in solution with 600 mls of deionized or HPLC grade water. Diluent used: 400 mls of

36、 HPLC grade acetonitrile in solution with 600 mls of deionized water. 5 Licensed by Information Handling Services4.3.2.1 HPLC procedure. (1) Preparation of standard and sample. (a) Standards: Primary standard solution - Accurately weigh and record O. 1 O00 gram of DMDNB standard to the nearest 0.000

37、1 gram, and transfer the weighed sample to a 100 ml volumetric flask. Dilute to volume with acetonitrile and mix the contents well. Secondary standard solution- Pipette 10 ml of primary standard solution into a 100 ml volumetric flask. Dilute to volume with acetonitrile and mix thoroughly. Injection

38、 standards - Pipette 5, 10, 15, and 20 mls of the above secondary standard solution respectively into four 50 ml volumetric flasks. Dilute to volume with Diluent and mix well. (b) Samples Primary sample solution: Accurately weigh and record 3 grams of sample to the nearest 0.0001 gram, and transfer

39、the weighed sample to a 100 ml volumetric flask. Dilute to volume with acetonitrile and a small amount of deionized water if necessary, and mix well. Secondary sample solution - Pipette 5 mls of the primary sample solution to a 1 O0 mls volumetric flask, dilute to volume with Diluent. Mix thoroughly

40、. Injection sample - Pipette 2 ml of the secondary sample solution to a 100 ml volumetric flask. Dilute to volume with Diluent. Mix thoroughly. (2) HPLC system setting. The HPLC and its accessories shall be set to the following operating parameters: UV detector: Wavelength -220 m; AUFS - O. 1; Filte

41、r - 1 .O Autosampler injector: Injection volume - 20 uL; Run time - 15 min. Integrator: Attention - 6; Thresh - 5 Isocratic pump: Flow rate - 1.5 mVmin Cht spd - 0.5; Pk wd - 0.04; AR REJ - O (3) Analysis: Put an aliquot of each standard and sample in vials and put them into the autosampler in the f

42、ollowing sequence: 6 Licensed by Information Handling ServicesA-A-594 1 O Vial 1 - 5 mL/50 mL Standard. Vial 2 - 10 mL/50 mL Standard Vial 3 - 15 mL/50 mL Standard Vial 4 - 20 a. Title, number, and date of this CID. b. Issue of Department of Defense Index of Standards and Specifications (DODISS) to

43、be cited in the solicitation, and if required, the specific issue of the individual documents referenced. c. Quantity required. d. Packaging and marking requirements. 7 Licensed by Information Handling ServicesA-A-54410 BI 7038054 00047Lb T70 B A-A-594 1 O 6.2 Source of supply. DMDNB (2,3-dimethyl-2

44、,3-dinitrobutane) has been previously procured from Hampshire Chemical Corporation, 5529 US 60 East, Owensboro, Kentucky 42303, and found to be acceptable with regard to its chemical and physical properties, punty of the material, etc. for general laboratory applications. DMDNB from a new supplier i

45、ntended for a particular application should be evaluated (qualified) for the specific application. 6.3 Equivalent test method. Prior approval of the Contracting Officer is required for use of equivalent test methods. A description of the proposed method should be submitted through the Contracting Of

46、fcer to: Commander, ATTN: AMSTA-AR-QAT- P, ARDEC, Picatinny Arsenal, NJ 07806-5000. This description should include, but not be limited to, the procedures used, the accuracy and precision of the method, test data to demonstrate the accuracy and precision and drawings of any special equipment require

47、d. 6.4 Source of documents. 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. 6.5 Technical agency. ARDEC, Picatinny Arsenal, (AMSTA-AR-QAT-P), is the technical agency that is responsible

48、for the preparation and revision of this Commercial Item Description. This CID should not be revised without the expressed concurrence and approval from the Technical Agency. All correspondence to the Technical Agency should be submitted through the contracting officer to: Commander, TACOM-ARDEC, ATTN: AMSTA-AR-QAT-P, Picatinny Arsenal, NJ 07806-5000. Custodian: Preparing Activity: Army-AR Review Interest: Army - AMSSB-REN-SS Army - AR (Project 68 10- 1643) Licensed by Information Handling Services