1、I INCH-POUND I MIL-E-82756(OS) AMENDMENT 1 14March 1995 MILITARY SPECIFICATION EXPLOSIVE, PLASTIC-BONDED, CAST PBXN-103 This Amendment forms a part of MIL-E-82756(OS), dated 4 April 1994, and is approved for use by the Department of the Navy and is available for use by ail Departments and Agencies o
2、f the Department of Defense. PAGE 13 After paragraph 4.6.2.6 and before 4.6.3 add: “4.6.2.7 Alternate test method for cured PBXN-103 mixed plasticizer analysis using High Performance Liquid Chromatography (HPLC). 4.6.2.7.1 Equipment. The following equipment or equivalent shall be used: a. High perfo
3、rmance liquid chromatograph equipped with ultraviolet (UV) detector, auto sampler, column oven and data handling system b. HPLC C-18 reverse phase column, 25 cm long, 4.6 mm inner diameter C. Volumetric flasks; 25 and 100 mL d. Pipets, volumetric, Class A, 1 and 100 mL e. Auto sampler vials with cap
4、 and PTFE faced septa f. Disposable syringe filters, 25 mm diameter, PTFE membrane, 0.45 micron porosity. 4.6.2.7.2 Reagents. The following reagents shall be used: a. Tetrahydrofuran (THF), HPLC grade b. Acetonitrile (ACN), HPLC grade C. Water, suitable for HPLC d. Resorcinol, analytical grade e. Tr
5、imethylol Ethane Trinitrate (TMETN), production grade f. Triethylene Glycol Dinitrate (TEGDN), production grade AMSC NIA i of3 FSC 1376 DISTRIBUTION STATEMENT A. Approved for public release; distribution is unlimited. Provided by IHSNot for ResaleNo reproduction or networking permitted without licen
6、se from IHS-,-,-9999906 i1984440 i22 MIL-E-82756(OS) AMENDMENT 1 g. Ethyl centralite (EC), analytical grade h. 2, 6-Diethylaniline, analytical grade, 99.5 percent purity. 4.6.2.7.3 Standard preparation. Prepare standard solutions as follows: a. Resorcinol stock solution: accurately weigh 0.3 grams o
7、f resorcinol to f 0.1 mg into a 100-mL volumetric flask. Bring to volume with ACN and mix well. b. Internal standard stock solution: accurately weigh 5.0 grams of 2, 6- diethylaniline to to volume with ACN, and mix well. 0.1 mg into a 100-mL volumetric flask. Dissolve, bring C. Mixed plasticizer sto
8、ck solution: accurately weigh 0.025 grams TEGDN, 0.23 grams TMETN and 0.015 grams EC to k 0.1 mg into a 100 mL volumetric flask. Pipet 1 mL of the resorcinol stock solution into this flask. Bring to volume with ACN and mix well. Accurately pipet 1 mL of the internal standard stock solution into the
9、100-mL volumetric flask containing the mixed plasticizer ingredients. Total volume should be 101 mL. d. Analysis standard: accurately pipet 1 mL of the mixed plasticizer stock solution into a 25-mL volumetric flask and bring to volume with ACN. 4.6.2.7.4 Sample preparation. Prepare sample as follows
10、. Samples should be prepared in duplicate. a. Cut the sample into small pieces. b. Accurately weigh a 1-gram sample to k 0.1 mg into a 100-mL stoppered flask. C. Accurately pipet 100 mL of tetrahydrofuran (THF) into the flask. Accurately pipet 1 mL of the internal standard solution into the same fla
11、sk and stopper flask tightly. Allow the mixed plasticizer and nitrocellulose ingredients to dissolve. Shake the sample to thoroughly mix the dissolved ingredients. d. Accurately pipet 1 mL of this solution into a 25-mL volumetric flask and bring to volume with ACN. e. Filter sample solution through
12、a 0.45 micron syringe filter before analysis. 4.6.2.7.5 Instrument set up. Set up the instrument in accordance with the manufacturers manual and as follows: a. Instrument linearity should be checked by using three different standard concentration levels to cover the expected sample concentration ran
13、ge. 2 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-9999906 3984443 669 MIL-E-82756(OS) AMENDMENT 1 b. The mobile phase composition should be 65% ACN and 35% water. Degas mobile phase before use. The mobile phase composition may be adjusted by the
14、operator to optimize chromatographic system and to insure baseline separation of all peaks. C. The UV detector is set at 215 nm. d. Column oven temperature recommended setting is 40C. The oven temperature setting may be changed by the operator in accordance with instrument instructions. The selected
15、 temperature shall be constant throughout the analysis to insure baseline separation of all peaks. e. Mobile phase flow rate is 1.0 mL/min. f. All injections are 10 microliters. g. Obtain a chromatograph of the standard at the beginning of the analysis and another after all samples are tested. The t
16、wo results shall be within 2 percent. No more than five samples are to be chromatographed between standard injections. h. Perform duplicate runs on all standards and samples. Ensure that the duplicate runs agree within 2 percent. 4.6.2.7.6 Calculations. Calculate weight percent of each analyte in sa
17、mple as follows: where: W, = Weight of analyte, g, from 4.6.2.7.3 (a) for resorcinol and 4.6.2.7.3 (c) for TMETN, TEGDN, and EC W, = Sample weight, g, from 4.6.2.7.4 A, = Average area of 2, 6-diethylaniline peak in standard A? = Average area of 2, 6-diethylaniline peak in sample A, = Average area of
18、 analyte peak in standard A, = Average area of analyte peak in sample D = Dilution factor for each analyte (D = 1 for resorcinol: D = 100 for EC, TMETN and TEGDN)“ Preparing Activity: (Project 1376-0004) Navy - OS 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-
