NAVY DOD-P-82671-1979 PROPYLENE GLYCOL DINITRATE《二硝酸丙二酯》.pdf

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1、This specification is approved for use by the Naval Sea Systems Command, Department of the Navy, and is available for use by all Departments and Agencies of the Department of Defense. 1.1 Scope. This specification covers the requirements for one type propellants. I 2. APPLICABLE DOCUMENTS this speci

2、fication to the extent specified herein: SPECIFICATION MILITARY DOD- P- 8 2 6 7 O Propanediol, 1, 2 STANDARDS MILITARY MIL-STD- 129 MIL-STD-286 Propellants, Solid: Sampling, Marking for Shipment and Storage (Copies of specif ications, standards, drawings, and publications required by contractors in

3、connection with specific procurement functions should be obtained from the procuring activity or as directed by the contracting officer). Beneficial comments (recommendations, additions, deletions) and any pertinent data which may be of use in improving this document should be addressed to: ization/

4、Documentation Division (Sol), Indian Head, MD 20640 by using the self -addressed Standardization Document Improvement Proposal (DD Form 1426) appearing at the end of this document or by letter. Commanding Officer, Naval Ordnance Station, Standard- Provided by IHSNot for ResaleNo reproduction or netw

5、orking permitted without license from IHS-,-,-TABLE I. Physical and chemical requirements. Requirements Test Property Minimum Maximum method Nitrogen (% by wt) 16.82 16.92 4.3.2 Acidity (as sulfuric acid) (W by wt) d o. O01 4.3.3 Alkalinity (as sodium carbonate) (2 by wt) - o. O01 4.3.3 Moisture (%

6、by wt) - O. 50 4.3.4 82 OC) (minutes) 10 - 4.3.5 Stability (potassium iodide at Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-DOD-P-BZh7L 91 R 7777706 OLL0727 L R DOD-P-826 7 1 (OS) 4. QUALITY ASSURANCE PROVISIONS 4.1 Responsibility for inspection.

7、 Unless otherwise specified in the contract, the contractor is responsible for the performance of all inspection requirements as specified herein. Except as otherwise specified in the contract, the contractor may use his own or any other facilities suitable for the performance of the inspection requ

8、irements specified herein, unless disapproved by 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 supplies and services conform to specified requirements. 4,.2 Inspection provision

9、s. 4.2.1 Lot formation. A lot shall consist of the propylene glycol dinitrate offered for acceptance at one time which has been produced by one manufacturer, at one plant, during a period of time not exceeding 20 hours, from the same materials, and under essentially the same manu-, facturing conditi

10、ons provided the operation is continuous. In the event the process is a batch operation, each batch shall constitute a lot (see 6.5). 4.2.2 Sampling. Using a dipper made of rubber or an approved plastfci a sample of approximately 50 milliliters (mL) of propylene glycol dinitrate shall be removed fro

11、m each lot. transferred to a stoppered bottle made of rubber or an approved plastic. The bottle shall be labeled to show the lot number and date of manufacture. The sample shall be 4.2.2.1 After disposal of the propylene glycol dinitrate from the sample bottle, the bottle shall be cleaned as follows

12、: a. Rinse thoroughly with acetone. b. Flush generously with hot tap water (3 minutes under a c. Rinse with distilled water and dry. direct flow is considered adequate). . 4.3 Quality conformance inspection. The material shall be subjected to all the following inspections and tests for acceptance. W

13、hen specified in the contract (see 6.2), the supplier shall submit a report giving the results obtained for all inspections and tests performed and a certified statement that the lot meets all the requirements of this specification. Unless otherwise specified, all chemicals shall be ACS grade in acc

14、ordance with NIL-STD-1218 and distilled water shall be used. blank determinations shall be run and corrections applied where significant. Where applicable, 4.3.1 Visual inspection. All samples shall be visually inspected to determine conformance to the workmanship requirement of 3.3. 4.3.2 Determina

15、tion of nitrogen. Prepare the nitrometer as described by MIL-STD-286BY method 209.3.2. using 25 .TIL of glacial-acetic acid for each of two rinses. Wash the nitrometer generator Expel all air Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-DOD-P-Zb7L

16、 7L 9979906 OLL0930 from the stopcock and sidearm. Cap the sidearm. Add 2 mL of glacial acetic acid to the generator cup and draw it approximately three quarters of the way into the nitrometer, Weigh accurately to 0.1 milligram (mg) a sample containing 0.70 ? 0.05 gram (g) of PGDN and transfer quant

17、itatively to the generator cup. Draw the acid-sample mixture into the generator. Add a 2 portion of glacial acetic acid to the generator cup and draw the acid into the generator. Repeat the steps in the previous sentence using a second portion of acid. generator cup and draw the acid into the genera

18、tor. Add 25 mL of 94.5% sulfuric acid to the CAUTION: Any temperature rise should be avoided by regulating the rate of sulfuric acid addition. There is a color change from red to purple to yellow red during the addition of the acid and the subsequent steps of the procedure. Close the top stopcock an

19、d immediately open the bottom stopcock. React the sample by gently shaking the top of the generator bulb holding the bottom end of the bulb as the axis. CAUTION: The lower stopcock must be open until the gas has been generated and any temperature rise in the sample during the reaction must be avoide

20、d. must be used. Safety shields Allow the generator to stand until the mercury settles. mercury until about 50 mm of mercury remain in the bottom of the generator bulb. Close the bottom stopcock, shake the generator bulb vigorously for 3 to 5 minutes, and allow the generator to stand for an addition

21、al 5 minutes. Vent any air from the reading tube, the stopcock, and the sidearm of the reading tube. with an airtight connection. adjust the mercury level in the compensatory tube to the calibration mark. Then adjust the mercury in the reading tube so that it is level with the calibration mark. temp

22、erature, make a final adjustment of the mercury level, and read the gas volume. Drain the excess Connect the generator to the reading tube Transfer the gas to the reading tube and Allow the system to come to equilibrium at ambient Calculation: Percent nitrogen = A W Where: A = reading of the mercury

23、 level on the measuring tube W = weight of sample (on the moisture-free basis),g 4.3.3 Determination of acidity and alkalinity, Place approximately 50mL of distilled water into each of two 12% Erlenmeyer flasks and add ten drops of bromothymol blue indicator to each flask. Neutralize the contents of

24、 the flasks with either 0.OlN acid or base to bring the 4 - /- 1 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-DOD-P-82671 91 m O6 0110931 T m DOD-P-82671 (OS) water to a neutralization point (yellow pH 6.0 - blue pH 7.6). green color indicates the

25、 desired neutralization point. 20 g of raw PGDI? from a weighing bottle into one of the flasks. sample to enter along the inner sides of the flask. sample to the nearest 0.1 mg. action. Note any change in color due to the indicator change. flask containing the PGDN with the blank flask. titrate with

26、 standard acid to the neutral point. If the PGDN flask is yellow, titrate with standard base. compare the color for the end point. color. A pale Weigh approximately llow the Record weight of the Gently mix the PGDN and-water with a swirling Compare the If the PGDN flask is blue, Use the color of the

27、 blank flask to The desired end point is a pale green Calculation: Percent acidity as H2SO4 =(mL base x normality of base) x 4.9 Sample weight, g Percent alkalinity as Na2C03 = (mL acid x normality of acid) x 5.3 Sample weight, g 4.3.4 Determination of moisture content. to 100 mL of methanol. with s

28、tabilized Karl Fischer reagent. sample of propylene glycol dinitrate (5 to 15 g) to the titration fxask. Titrate the sample to a potentiometric end-point. To the titration flask add-75 _ Titrate the methanol to a potentiometric end-point Transfer an accurately weighed Calculation: Percent moisture c

29、ontent = 100 (KF) W where : K = mL of Karl Fischer reagent used in titration F = reagent factor (g of water per mL of reagent) W = Wei-ght of propylene glycol.dinitrate, g 4.3.5 Determination of stability. Filter a portion of the propylene glycol dinitrate sample through two thicknesses “S. and S.“

30、Number 604 filter paper or equivalent. by means of a pipette, to each of three test tubes which are 140 mm long, 13 mm internal diameter and 16 mm outside diameter. Care should be taken during the transfer not to leave droplets of the propylene glycol dinitrate on the sides of the test tubes. Stoppe

31、r each-tube by means of a new, tightly fitting cork through which passes a tightly fitted glass rod eqipped with a platinum holder for a strip of standard potassium iodide starch-indicator paper. Using forceps,hang a strip of standard potassium iodide starch-indicator paper on the platinum holder. T

32、he standard potassium iodide starch-indicator test paper shall normally be approximately 25 mm long and 9.5 mm wide. Moisten a horizontal section in the upper half of the standard test paper with a 50 percent by volume solution of pure glycerin in distilled water. Transfer a 2 mL portion of the filt

33、ered material This is 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-DOD-P-82671 41 W 9999906 OLL0932 L W - - conveniently accomplished by dipping a small diameter glass rod into the glycerin-water solution, and as the rod is withdrawn, making con

34、tact with the side of the container so as to minimize the volume of the solution adhering to the rod. Draw the rod across the paper strip so as to produce a level and distinct line of demarcation on the lower edge of the wet area. Prepare a blank by suspending a moistened strip of the standard test

35、paper in a clean dry tube. Adjust the temperature of the heat tube bath to 82.2 -f- 1C and insert all four test tubes into the heating solution. The depth of immersion of the test tubes into the heating solution should be approximately 50 mm. test tubes are viewed against a white background illumina

36、ted by bright diffused daylight. Note the time of insertion of the tubes into the bath. During the test, the line of demarcation on the standard test paper should be 76 mm above the level of the propylene glycol dinitrate in the test tube, The line of demarcation in the blank tube is regulated at an

37、 equivalent height in the tube. Consider the end-point ofthe test to be the first appearance of any discoloration at the line of demarcation between the wet and the dry portion of the test paper in the sample tube which is in excess of the discoloration observed at the same position on the test pape

38、r in the blank. Note the time for completion of the test to the nearest minute. Consider the minimum time for the three tubes to represent the heat test value of the sample. After the test, rinse all rods and tubes with acetone to remove the propylene glycol dinitrate. Wash with warm soapy water, ri

39、ns thoroughly with tap water, then with distilled water and dry in a steam oven at approximately 9OoC. The bath should be placed in such a position that the 4.3.6 Rejection criteria. Failure of any sample to meet any requirement of this specification shall be cause to reject the lot or batch, 5. PAC

40、KAGING 5.1 Packing. 5.1.1 Level C. Propylene glycol dinitrate is classed as a “Fokbidden Explosive“ by Section 49 of the Code of Federal Regulations (CFR) . For shipment by public highways, the appropriate section of Section 49 of the CFR shall be followed. 5.2 Marking. The marking of interior packa

41、ges and exterior shipping containers shall be in accordance with instructions contained in Section 49 of the CFR and in accordance with MIL-STD-129. 6. NOTES 6.1 Intended use. Propylene glycol dinitrate is intended for use as a propellant ingredient. 6.2 Ordering data. Procurement documents should s

42、pecify the following: 6.2.1 Procurement requirements. a. b. Title, number and date of this specification Whether a certified analysis and/or a test report is required 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-DOD-P-8267L 71 W 777770b OLL0733

43、3 = DOD-P-82671 (OS) 6.2.2 Contract data requirements. The items of deliverable data whichmay be required by this speciflcatTon are cited in 4.3. Data Requirement Test Report Certified Analysis Applicable DID* DI-T-2072 - *DIDs (Data Item Descriptions/DD Form 1664) for the above data requirements ar

44、e documented in the applicable ADL (Authorized Data List.) will be delivered as identified on completed (numbered) DIDs when specified on DD Forms 1423 (Contract Data Requirements Lists) and incorporated into applicable contracts. Such data 6.3 Safety precautions. The safety precaution requirements

45、of the “Contractors Safety Manual for Ammunition, Explosives, and Related Dangerous Material“ (DOD 4145.26M) are applicable and should be specified in the contract or order as required by the Armed Services Procurement Regulations (ASPR) 1-323. NOTE: to be accomplished by a Government activity, the

46、safety precaution requirements of “Ammunition and Explosives Ashore“ (OP 5) should be made applicable. When this specification is used as part of the description of work 6.4 Toxic effects. Toxic effects may occur from the inhalation of vapors from propylene glycol dinitrate or the absorption from di

47、rect contact with the skin. 6.5 Batch. A batch is defined as that quantity of propylene glycol dinitrate that has been subjected to the same unit chemical or physical process intended to make the final product homogeneous. Custodian: Navy - OS Preparfng Activity: Navy - OS Project Number: 9 135 -NO8 9 *US. GOVERNMENT PRINTING OFFICE: 1979-603-022/1153 7 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-

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