1、1 H 9999906 2042437 437 MIL-PRF-25604E O1 October 97 Superseding MIL-P-25604D 23 May 1969 PERFORMANCE SPECIFICATION PROPELLANT, uns-DIMETHYLHYDRAZINE This specification is approved for use by ali Departments and Agencies of the Department of Defense 1. SCOPE 1.1 Scope. This specification covers the
2、requirements for unsymmetrical dimethylhydrazine (CH31 2NNH2 propellant (UDMH) . 2. APPLICABLE DOCUMENTS 2.1 General. The documents listed in this section are specified in sections 3 and 4 of this specification. This section does not include documents in other sections of this specification or recom
3、mended for additional information or as examples. While every effort has been made to ensure the completeness of this list, document users are cautioned that they must meet all specified requirements documents cited in sections 3 and 4 of this specification, whether or not they are listed. 2.2 Gover
4、nment documents. 2.2.1 Specifications, standards, and handbooks. The following specifications form a part of this document to the extent specified herein. Unless otherwise specified, the issues of these documents are those listed in the issue of the Department of Defense Index of Specifications and
5、Standards (DoDISS) and supplement thereto, cited in the solicitation (see 6.2). SPECIFICATIONS FEDERAL BB-H-886 - Hydrogen BB-A-1034 - Air, Compound, for Breathing Purposes DEPARTMENT OF DEFENSE Beneficial comments (recommendations, additions, deletions) and any pertinent data.which may be of use in
6、 improving this document should be addressed to: Code (68) SA-ALC/SFSP, 1014 Billy Mitchell Blvd/STE 1, Kelly AFB TX 78241- 5603, by using the standardization Document Improvement Proposal (DD Form 1426) appearing at the end of this document or by letter. AMSC N/A FSC 9135 DISTRIBUTION STATEMENT A.
7、Approved for public release; distribution is unlimited. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-PRF-25604E MIL-PRF-27401 - Propellant Pressurizing Agent, Nitrogen MIL-PRF-27407 - Propellant Pressurizing Agent, Helium (Unless otherwise ind
8、icated, copies of the above specifications, and standards are available from the Standardization Document Order Desk, 700 Robbins Avenue, Building 4D, Philadelphia PA 19111-5094). 2.3 Non-Government publications. The following documents form a part of this document to the extent specified herein. Un
9、less otherwise specified, the issues of the documents which are DoD adopted are those listed in the issue of the DoDISS cited in the solicitation. Unless otherwise specified, the issues of documents not listed in the DoDISS are the issues of the documents cited in the solicitation (see 6.2) . AMERIC
10、AN SOCIETY FOR .TESTING AND MATERIALS (ASTM) ASTM D 1193 - Specification for Reagent Water (DoD adopted) ASTM D 1298 - Standard Practice for Density, Relative Density (Specific Gravity), or API Gravity of Crude Petroleum and Liquid Petroleum Products by Hydrometer Method (DoD adopted) ASTM D 2276 -
11、Test Method for Particulate Contaminant in Aviation . Fuel by Line Sampling (DoD adopted) ASTM E 29 - Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications (DoD adopted) (Application for copies should be addressed to the American Society for Testing and Mate
12、rials, 100 Barr Harbor Drive, West Conshohocken PA 19428-2959. 2.4 Order of preceden.ce. In the event of a conflict between the text of this document and the references cited herein, the text of this document takes precedence. Nothing in this document, however, supersedes applicable laws and regulat
13、ions unless a specific exemption has been obtained. 3. REQUIREMENTS 3.1 Chemical and physical properties. The chemical and physical properties of the propellant shall conform to those listed in Table I when tested in accordance.with the applicable test methods. 3.2 Limiting values. The following app
14、lies to all specified limits in this specification: For purposes of determining conformance with these requirements, an observed value or a calculated value shall be rounded off “to the nearest,unit“ in .the last right-hand digit used in expressing the specification limit according to the rounding-o
15、ff method of ASTM Practice E 29 for using Significant Digits in Test Data to Determine Conformance with Specifications. 2 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-II 9999906 2042439 20T MIL-PRF-25604E 3.3 Filter. A filter with a 10-micrometer
16、nominal and 40-micrometer absolute rating shall be installed between the manufacturers plant system and the container to be filled for delivery. 3.4 Qualitative. The propellant shall be colorless, homogeneous liquid when exaniined visually by transmitted light. TABLE I. Chemical and physical propert
17、ies. PROPERTIES uns-Dimethylhydrazine (Percent by weight) Water (Percent by weight) Amines (Percent by weight) N-Nitrosodimethylamine (Percent by weight) Chloride (Percent by weight) Density (g/mL) 60F Particulate (mg/L) 4. VERIFICATION LIMITS 98.0 min 0.3 max 1.5 max 0.01 max 0.003 max 0.795 to 0.7
18、97 10 max TEST PARAGRAPHS 4.3.2 4.3.2 4.3.2 4.3.6 4.3.4 4.3.5 4.3.3 4.1 Classification of inspections. The inspections shall be classified as quality conformance inspections. 4.2 Quality conformance inspection. Unless otherwise specified (6.2), each filled shipping container shall be considered a lo
19、t and shall be sampled. Each sample shall be subjected to the visual examination described in 4.3.1 for conformance to 3.4 and to the tests described in Table I for conformance to the requirements specified in Table I. 4.2.1 Sample. A sample consists of not less than 600 mL of propellant. Unless oth
20、erwise specified, quality conformance tests shall be made on the sample of propellant taken directly from the shipping container. When required, the sample shall be forwarded to a laboratory designated by the procuring activity for subjection to the quality conformance tests specified herein. The bo
21、ttle intended for sampling shall be specially cleaned and handled according to the procedure described in 4.3.3 4.2.2 Rejection. When any sample of the propellant tested in accordance with 4.3 fails to conform to the requirements specified herein, the entire lot represented by the sample shall be re
22、jected. 4.3 Test methods. 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-E 9999906 2042440 T21 m MIL-PRF-25604E 4.3.1 Examination of product. The propellant shall be visually examined while performing test specified in 4.3.3 to determine complianc
23、e with the requirement as specified herein. Examination to ensure that the material conforms to 3.4 shall be conducted after the sample has been transferred to the SOO mL calibrated cylinder. 4.3.2 Uns-Dimethylhydrazine assay, water and amines. The propellant, water, and amine content of the sample
24、shall be determined by the following method. 4.3.2.1 Gas chromatographic method. 4.3.2.1.1 Assay column preparation. Weigh 5 grams of polyethylene glycol 400 and 45 grams of 60/80 mesh Fluoropak 80 into separate beakers. Dissolve the polyethylene glycol 400 in a volume of reagent grade dichlorometha
25、ne which is approximately one-half the volume of the Fluoropak 80. Pour the Fluoropak.80 into the polyethylene glycol 400 solution with gentle stirring. Spread the resulting damp powder in a tray and dry the mixture in a vacuum oven at 100C and less than 50 x& of Hg for at least one hour. Cap one en
26、d of a 1/8 inch OD by 6-foot stainless steel tube and fill the tube with the prepared column packing by pouring through a small funnel attached to the other end. Tap or mechanically vibrate the tube to ensure uniform packing. When the tube is filled, plug both ends with a small wad of glass wool, be
27、nd the column to the configuration required by the column oven, and connect the column to the inlet fitting in the oven. Condition the column with carrier gas flowing and the oven set at -120C for one hour. After conditioning the column, connect the other end to the detector and set the carrier gas
28、flow to approximately 25 ml/min, and the column oven to 100OC. The inlet and detector temperatures, if separately heated, shall be set to 100C and 150C, respectively. The detector current should be set to a nominal sensitivity value recommended for helium by the instrument manufacturer. 4.3.2.1.2 An
29、alysis. Equilibrate the column with propellant by injection of two or more S microliter (PL) samples into the inlet. If more than 30 minutes elapse between analyses, a single 5 pL injection of propellant should re-equilibrate the column. Inject 1 - 2 pL of propellant for analysis and record the area
30、s of all peaks in the chromatogram. Each analysis should require less than 15 minutes for elution of all components. The elution order of possible sample components is as follows: Air, ammonia, methylamine, dimethylamine, formaldehyde dimethylhydrazone, UDMH, water, methylhydrazine, and hydrazine. 4
31、.3.2.1.3 Calculations. The following formula shall be used to calculate the percent by weight of each component appearing in the chromatogram. %C= - &* x100 4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-PRF-25604E where A, = The measured area
32、 of a peak multiplied by its signal attenuation factor. ZAi = The sum of all the measured areas multiplied by their respective signal attenuation factors. %C = The weight percent of the component corresponding to Ac. Assumption: The thermal conductivities of all components in the sample are equal. 4
33、.3.2.1.4 Equipment and reagents. The following equipment and reagents shall apply as test conditions of 4.3.2. a. Equipment : (1) Gas chromatograph - incorporating a thermal conductivity detector. (2) Recorder - potentiometric strip chart, O - 1 millivolt, 1 second full scale response, with integrat
34、or. (3) Tubing - stainless steel, 1/8 inch O.D. x 6 feet (4) Hypodermic syringe - 10 microliter, fixed needle (5) Regulator - helium, to fit the cylinder (6) Standard screens - 60 mesh and 80 mesh (7) Vacuum oven, capable of 100C b. Reagents : (1) Fluoropak 80, Analabs, Inc. , 80 Republic Dr. , Nort
35、h Haven CT 06473 or equivalent. (2) Polyethylene glycol 400, or equivalent (3) Dichloromethane - ACS reagent grade (4) Helium gas - conforming to MIL-P-27407 4.3.3 Particulate. The propellant sample shall be tested for contamination in accordance with ASTM D-2276, Method A, with the following except
36、ions: 4.3.3.1 Mix the sample thoroughly without exposure to air. Immediately pour 500 mL of the sample into a clean 500-ml graduated cylinder. Use this 500 mL of propellant for the particulate analysis. 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,
37、-,-m 9999906 2042442 AT4 MIL-PRF-25604E 4.3.3.2 Use a solvent resistant filter disc made from such materials as Millipore LSWP-O4700 (Mitex-Teflon), Millipore URWP 04700, (Solvinert) or Gelman VF-6, (Fluoride-Metricel), plain, white, 10t3 microns, 47 mm diameter, or equivalent. 4.3.3.3 The drying ov
38、en temperature shall be 158F (7OOC) instead of the 194OF (9OOC) specified in ASTM D-2276. 4.3.3.4 Filtered isopropyl alcohol shall be used for rinsing the sample bottle and filter holder instead of petroleum ether specified in ASTM D-2276. 4.3.4 Chloride. 4.3.4.1 Procedure. Evaporate 2.0 rnL of prop
39、ellant and 0.2 mL of 1N sodium hydroxide contained in a 25 mL volumetric flask using a steambath or hot plate located in a fume hood. Purge the flask with nitrogen gas to facilitate evaporation. Dissolve the residue with 2.0 mL of ferric ammonium sulfate reagent and 2 mL of chloride-free distilled w
40、ater. Add 1.0 mL of saturated mercuric thiocyanate reagent, mix by swirling, and dilute to the 25 mL mark with chloride-free distilled water. Mix again by inverting the flask several times and allow to stand in darkness for 15 to 30 minutes. Measure the absorbance of the reagent blank and sample sol
41、utions at 460 nm in a 5.0-cm cell, after setting distilled water to “O“ absorbance. Subtract the absorbance of the reagent blank from the sample absorbance. The chloride content is determined from the calibration curve constructed according to 4.3.4.3. 4.3.4.2 Calculation. Calculate the percent chlo
42、ride in the sample using the following formula: (mg CI- from calibration curve) 157 Cl-, weight% = x 10“ 4.3.4.3 Calibration Curve. A calibration curve shall be prepared as follows: Syringe O mL, 1 mL, 2 mL, 4 mL, and 8 mL of the dilute chloride standard solution (0.010 mg/mL) into separate 25 mL vo
43、lumetric flasks. Add 0.20 mL of 1N sodium hydroxide to each flask. Add 2.0 mL ferric ammonium sulfate and 5 mL chloride-free water and swirl. Add 1.0 mL saturated mercuric thiocyanate and mix. Add chloride-free distilled water to the 25 mL mark and mix by inverting several times. Place standards and
44、 blank in darkness for 15 to 30 minutes. Measure the absorbance of the blank and each of the four standards in a 5.00 cm cell at 460 nm after setting distilled water to O“ absorbance. Subtract the absorbance of the blank from that of each standard. Plot this difference against the corresponding mg o
45、f Cl. 4.3.4.4 Reagents and equipment. 4.3.4.4.1 Reagents. a. Sodium hydroxide solution, 1N: Dissolve 40 grams of ACS reagent grade sodium hydroxide pellets in 300 mL of chloride-free distilled water contained in a 1000 mL volumetric flask. Cool the solution to room temperature, dilute to the mark wi
46、th the chloride-free distilled water, and mix thoroughly. 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-M 9999906 2042443 730 MIL-PRF-25604E Transfer the solution to a plastic bottle and protect from prolonged exposure to the atmosphere. b. Ferri
47、c ammonium sulfate: Mix 240 mL concentrated nitric acid and 160 mL of chloride-free water. Dissolve 48.2 grams of ferric ammonium sulfate, ACS grade, in the nitric acid solution and allow the precipitate to settle out. Decant the liquid for use in the analysis. c. Saturated mercuric thiocyanate: Sat
48、urate ACS reagent grade ethyl alcohol (95%) with ACS reagent grade mercuric thiocyanate. Allow the excess to settle out and decant the supernatant liquid for use in the analysis. d. Chloride stock solution: Dissolve exactly 165 mg (0.1659) of dried, primary standard grade, sodium chloride in chlorid
49、e-free distilled water contained in a 100 mL volumetric flask and dilute to the mark (1.0 mg of C1 /mL) . e. Chloride standard solution: Syringe exactly 10.0 mL of the Chloride stock solution into a 1000 mL volumetric flask, and dilute to the mark with chloride-free water (0.010 mg C1 /mL). f. Chloride-free water: This shall be double-distilled, or distilled deionized water, which tests negative (no cloudiness) with silver nitrate. 4.3.4.4.2 Equipment. a. Syr
