NAVY DOD-P-82670-1980 PROPANEDIOL 1 2 (METRIC)《1 2-丙二醇》.pdf

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1、I DOD-P-82b70 68 W 7797706 0323377 O m 30 July 1965 s. MILITARY SPECIFICATION i c nirs specification is approved for use by the Naval Sea Systm Cumand, Department of the Navy and is available for use by all Departments and Agencies of the Department of the Defense. 1. SOOPE 1.1 Srope. This specifica

2、tion covers one type of propanENT Uniform Freight Classification * 1. Licensed by Information Handling ServicesDOD-P-2670 b = 777770b 0123202 7 4.3.1 Visual inspection. AU sanples shai be visuay inspected to determine conformanoe to the Horknianship requirements of 3.2. 4.3.2 Test methods and proced

3、ures. 4.3.2.1 Determination of color. The color of the pmpmediol 1, 2 4.3.2.2 Determination of specific gravity. Detemine the specific shall be determined in accordance with ASIM D-1209, platinun cobalt scale. gravity at 25/25O C by any convenient niethod that is accurate to the fourth deciml place.

4、 - 4.3.2.3 Determination of acidity. Measure 100 I& of ethyl alcohol into a flask, add three drops of phenolphthalein indicator, and titrate the alcohol to a faint pink color with 0.lN sodium hydroxide solution. Add an accurately weighed 30 to 4Ggram (g) portion of the sample to the alcoholic soluti

5、on. Titrate the mixture with 0,lN sodium hydmxide. Calculate the where: V = N= G= 4.3.2.4 shall be used and km& Abbe a. percentage of acidity as acetic acid as follows: Percent acetic acid = 6.005 VN G sodium hydmxide required for titration, I& nomlity of sodium hydroxide solution weight of sanple,

6、g Detennination of refractive index. for the determination of refractive index using a Bausch refractometer or equivalent : Wipe with caution to preclude scratching the prism surface The following procedure I of the refractometer with a tissue wet with Ethanol or xylene, and then with a dry tissue.

7、velocity of the circulating fluid so that the themmeter reads 25.0 f o. 1Oc. Adjust the temperature of the water bath and the b. Rotate the body of the instrument and the mving ann away fmthe operator until the interface between the prim is horizontal. bsen the prim clan and drop the lower prim. Wit

8、h a glass stirring md, add a few drops of the sample liquid to be tested to the lower prism, bring the prim faces together, and lock the prism clamp. instrument to the nom1 viewing position. light into the telescope. Rotate the Adjust the mirror to reflect c. nclanp the index am and mve it to the fa

9、r end of the scale. Focus the telescope eyepiece sharply on the crosshairs. Bring the divided field into view by mving the index ann forward. my have a colored border, which can be achrorratized by use of the compensators rotated by a pinion. The field will be sharpest when the edge is just turning

10、blue. the crosshairs by mving the index ann. illumination of the field. to the crosshairs by means of the fine adjustnient screw. The field Bring the field alniost into mincidence with Obtain the final adjustment of the field line Adjust the mirror for the maximum 4 Licensed by Information Handling

11、ServicesY DOD-P-2670 68 m 9777906 0323203 9 DoD-P-82670( CE) d. Focus the magnifier 011 the scale and rotate it so that the scale is well illuminated. and estirnate the figure in the fourth decimal place. If the index reading does not rernain constant within one unit in the fourth decbl place for 1

12、minute, it my indicate diffusion of solvent remining on the prim or insufficient time for thermal equilibrium. Place a new -le of the fiquid to be tested on the prim, taking care that the prism is clean and dry. elapse after placement of the drop to insure that the liquid film is at the prim tenpera

13、ture. Read the scale directly to three decimal places e. Sufficient time should f. Report the reading obtained as n95 C. 4.3.2.5 Determination of distillation range. 4.3.2.5.1 Apparatus. Use the distilzation apparatus described in ASIM D-86 with the following exceptions: a. Thenmmter. Ese an AS731 P

14、artial Imnersion Thernmneter having a range of -5 to + 300“ C and conforming to the requirements for thennxneter 2C as prescribed in ASM E-1 or a thermmter having a range of 95 to 225 C and mfoming to the requirements for thermxneter 42C as prescribed in E-1. b. Cbndenser. A Liebig glass condenser 5

15、60 millimeters (mn) in length with 400 m in contact with the cooling water may be used in place of the bath-type condenser. 4.3.2.5.2 Procedure. With the receiving graduate, transfer exactly 100 mt of the sample directly into the flask, allowing none to run into the side tube and allowing the gradua

16、te to drain thoroughly. sairple contains dissolved or suspended urater it is advisable to add a few mall pieces of pumice or broken glass to pmte siiooth distillation. Insert the thermmter so that the top of the mercury bulb (or the top of contraction chanber if the Solvents Distillation Thenimneter

17、 is used) is level with the bottom of the side tube. Cbnnect the side tube to the condenser, with the bottom of the flask resting securely in the opening in the asbestos board. Apply heat cautiously and regulate it so that the first drop of condensate falls from the condenser in not less than 5 nor

18、mre than 10 minutes. when the first drop falls from the end of the condenser. distillation begins, regulate the heat so that the distillate is collected at a rate of not less than 4 nor mre than 5 mL/min (approxmtely 2 drops per second.) observe and record the temperature when 5 mL have been collect

19、ed in the receiving cylinder, and thereafter when the level of the distillate reaches each 10 mt division of the graduate, including a 95 mL reading. Discontinue the distillation when the temperature reaches that specified in the minimum percentage requirement, or whenever the temperature rise stops

20、 and the themmter reading starts to fall, and record the naxinrmterrperature reached. percentage distilled. If the Record as the initial boiling point with thernmneter reading When the Allow the condenser to drain and record the 5 , Licensed by Information Handling ServicesDoD-P-82670( OS) 4.3.2.6 D

21、eternination of carbonyl. 4.3.2.6.1 Equipment. a. J3eclaran Expandoniatic pH Meter or other pH meter capable Glass electrode (Beckmn 41263 or equivalent.) of titration in the millivolt (mV) mde. L b. c. Calomel reference electrode (Bechan 29400 or equivalent) d. 10-mL burette. e. 15-mL pipette. 4.3.

22、2.6.2 Reagents. a. Hydroxylamine hydrochloride. Recrystallize the carmercial product from a 2:l alcohol-water solution. sriall amount of alcohol and air dry. Wash the crystals with a b: Alcoholic potassium hydmxide. Add 3g of reagent potassium hydroxide to 1 liter of isopropyl alcohol. and stir unti

23、l solution is effected. Store in a container vented to the atmsphere through a guard tube containing soda lime or soda asbestos (ascarite) to protect from atmspheric carbon dioxide. solution to contact cork, rubber or saponifiable stopcock grease. Dispense in such a mer that only the clear top porti

24、on of the liquid is obtained. Bring to the boiling point Do not pennit the 4.3.2.6.3 Pmcedure. Weigh a 1OOg sanple of the propylene glycol into a 250 mL beaker. Add 3.0 g of the recrystallized hydroxylamine hydrochloride, 10 mL of ethyl alcohol and 4.5 mL of distilled water. Stir with a magnetic sti

25、rrer until the hydroxylamine hydrochloride is dissolved and let stand 1 hoUr (h) at room tenperature. Fill the 10-mt burette with the alcoholic potassium hydroxide solution. Using a Bechm expandoniatic pH meter or an equivalent, titrate the sanple potentiometrically. Equip the instrument with a glas

26、s electmde and calomel reference electrode. Prepare the electrodes in accordance with the mufacturers instructions. Blot the electrodes with tissue and lower into the reaction mixture. Depress both the expanded and + mV push buttons. Stir the solution until equilibrium is attained. Use the stanardiz

27、e knob to mve the needle to 180 mV. (In this de the full scale of the meter registers 200 mV. Beclniian, operate in accordance with the manufacturers instructions for mV titrations.) Add the potassium hydroxide solution in increments of 0.5 mL with the burette tip imnersed in the Solution and with c

28、onstant stirring. Allow time for the reading to stablize and record the mV reading after each addition. “be mV change for the entire titration should be about 100-120. me electmdes should be returned to water after each titration. Plot mL KH solution vs mV reading. the inflection point as the end po

29、int. titrating approximtely 8- potassium biphthalate to a phenolphthalein end point. fir meters other than Draw the best curve through the points and take Standardize the KH solution by 6 Licensed by Information Handling Services- DOD-P-2670 68 W 9777906 0323205 2 DobP-82670( OS) Calculations, Norma

30、lity of foMI solution carbonyl C = mL KDH X 30 X loo0 X N sample weight (g) C = ppm carbonyl in the sanple calculated as formaldehyde 4.3.2.7 Detemination of misture. TO the titration flask add 75 to 100 fi of methanol. with stabilized Kairl Fischer reagent. of propylene glycol (5 to 15 g) to the ti

31、tration flask, to a potentiometric end-point. Titrate the methanol to a potentiometric end-point Calculate the misture content as follows: Transfer an accurately weighed sarriple Titrate the sample Percent misture = 100 (KF) w where: K = Karl Fischer reagent used in titration, mL F = reagent factor

32、(g of water per mL of reagent) W = weight of propylene glycol, g 4.3.2.8 Detednat ion of dipropylene glycol. a. Equipment. 1. 2. Recorder, 0-1 mV strip chart recorder 3. Gas Chromatograph with flame ionization detector Awdliary equipnient for use in gas chromtography b. Reagents. 1. Fluoropals 80, 4

33、0-70 mesh 2. carbowax 20M 4. Dipropylene glycol, U.S.P. 3. (&lOl-OfOrm, reagent grade c. Column preparation. 1. Fluoropak 80 by dissolving the arbowax in chloroform and coating by a suitable method. Prepare a 6.4 m x 152 an stainless steel colm using a mechanical vibrator to cmpletely fill the tube.

34、 Prepare a colm packing material of 55% carbowax 20h4 on Use only the material which will pass a 40 mesh screen. Condition the colunai for 2 h at 21OoC. 7 - .-. Y Licensed by Information Handling ServicesDOD-P-2670 b 9 77777Ob 0323206 9 9 d. Gas chmmatographic conditions. i. hen temperature 210C 2.

35、3. 4. Detector - flame ionization 5. 6. Injector and manifold taperatures 21OoC mier gas-heliun at 40 &/min Swle size - 2 microliters (PL) Attenuation - to suit the substance being measured e. Preparation of standasds. 1. Prepare high purity pmpylene glycol for use as standards Distill the material

36、at a Discard the fiist 25 mt fraction and collect 200 mL. by placing about 600 I& of propylene glycol in a 1 L round bottom flask and fit with a short fractionating colm. reasonable rate. 2. Using the distilled propylene glycol fraction prepare Obtain chrorratograms of the distilled propylene glycol

37、 Since the dipropylene glycol two standards of O. 1% and O. 2% by weight added dipropylene glycol. 3. fraction and of each of the tu0 standards. can consist of three isomers, its chroniatogram should show two mjor peaks and a sraller third one. Select an attenuation for the dipropylene glycol elutio

38、n such that at least one of the peaks for the 0.2% standard is 25 MII or mre in height. Determine the relative peak areas of the dipmpylene glycol elutions by a “cut and weigh“ method including all significant peaks after that of the propylene glycol. If the distilled propylene glycol shows an appre

39、ciable munt of dipropylene glycol (mre than 0.01%) then this should be measured by a method of additions prozedure and a corresponding correction made to the 0.1% and the 0.2% standards. f. mcedure. 1. Plot the peak areas against percent dipropylene glycol. Obtain chrorratograrrs of the samples to b

40、e analyzed using the conditions in d. and the procedures in e. above. Measure the peak area for the dipropylene glycol and detemine its percent fmthe standard curve. 4.3.3 Rejection criteria. F4tilure of any sanple to meet any requirent of this specificaton shall be cause to reject the lot or batch.

41、 5. PACKAGING 5.1 Packaging. 5.1.1 &vel C. The propylene glycol shall be packaged in unifom quantities for shipment in accordance with the mufacturers ammercial practice. packages shall be of unifom size, shape, and mterial. 5.2 Packing. ._. 8 I Licensed by Information Handling Services. . . . DOD-P

42、-82670 68 m 7779706 0123207 b W 5.2.1 kvel C. The propylene glycol shall be packed in uniform quantities in such a manner as to assure carrier acceptance and afford protection against darrage during direct shipment franthe supply source to the first receiving activity for urmediate use. conply with

43、Uniform Freight Classification Rules or other carrier regulations applicable to the mde of transportation. of uniform size, shape, and naterial. antainers used shall Containers shall be 5.3 Marking. In addition to any special mrking required by the contract, unit packages and shipping containers sha

44、ll be marked in accordance with MItSi&129. 6. NOTES 6.1 Intended use. The propylene glycol covered by this specification is intended for use in the mufacture of propellant ingredients. 6.2 Ordering data. Procurenient documents should specify the following : 6.2.1 Procurant requj.renients. a. b. C. d

45、. Title, n111135er, and date of this specification. Whether tank cars or containers are to be wed for shipment. Size of containers required. Whether a certified analysis and/or test reports are required. 6.2.2 Contract data requirements. The item of deliverable data which my be required by this spec

46、ification are cited in 4.3. kta Requirement Test Report Certified Analysis Applicable DID* DI-T - 2072 - *DI& (mta Item Descriptions/DD Form 1664) for the above data requirements are documented in the applicable ADL (Authorized Data List.) Such data will be delivered as identified on corrpleted (nuh

47、ered) DI& when specified on 13D Fbm 1423 (Cbntract Data Requirements Lists) and incorporated into applicable contracts. 6.3 Batch. A batch is defined as that quantity of propylene glycol that has been subjected to the same unit chemical or physical process intended to make the final product homgeneous. custodian: NAVY-os *US. GOVERNMENT CRINTING OFFICE: lSB1-701Q23lS22 Preparing Activity: NAVY-os Project mer 6810-NA45 9 -a- -* Licensed by Information Handling Services