1、14- 2 o - 6 3 DOD-B-2669 68 W 9999906 0123192 W DOD-B-82669 (OS) 19 January 1979 SUPERSEDING ws 2101 30 July 1965 MILITARY SPECIFICATION BUTYL SEBACATE, DI-NORMAL This specification is approved for use by the Naval Sea Systems Command, Department of the Navy, and is available for use by all Departme
2、nts and Agencies of the Department of Defense. 1. SCOPE 1.1 Scope. This specification covers the requirements for one type of di-n-butyl sebacate suitable for use in the manufacture of propellants. 2. APPLICABLE DOCUMENTS 2.1 Government documents. The following documents of the issue in effect on da
3、te of invitation for bids or request for proposal form a part of this specification to the extent specified herein. STANDARDS MIL I TAY MIL-STD-105 MIL-STD- 129 MIL-STD- 1218 PUBLICATIONS Sampling Procedures and Tables for Inspection by Attributes Marking for Shipment and Storage ACS Chemicals NAVAL
4、 SEA SYSTFMS CCMMAND (CODE IDENT 10001) OD 43852 Determination of Sodium in Propylene Glycol Dinitrate by the Atomic Absorption Method (Copies of specifications, standards, drawings, and publications required by contractors in connection with specific procurement functions should be obtained from th
5、e 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/Documentation Division (Sol), Indian Head, MD 20640, by using the self-ad
6、dressed 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 networking permitted without license from IHS-,-,-2.2 Other publications. The
7、 following documents form a part of this specification to the extent specified herein. indicated, the issue in effect on date of invitation for bids or requests for proposals shall apply. Unless otherwise NATIONAL MOTOR FREIW TRAFFIC ASSOCIATION, INC., AGENT National Motor Freight Classif ication (A
8、pplication for copies should be addressed to the American Trucking Associations, Attn: Traffic Department, 1616 P Street, Washington, DC 20 36). Uniform Classification Committee, Agent Uniform Freight Classification (Application for copies should be addressed to the Uniform Classifi- cation Committe
9、e, Room 1106, 222 South Riverside Plaza, Chicago, IL 60606). AMERICAN SOCIETY FOR TESTING AND MATERIALS (2,2 Saponification number 350 360 4.392.3 Refractive index (n25OC) 1,4385 1,4405 4,3*2*4 r Moisture (% by wt) 0.15 4,3,2,5 Sodium (ppm) 1.0 4,3.2,6 - .2 Provided by IHSNot for ResaleNo reproducti
10、on or networking permitted without license from IHS-,-,-DOD-B-82669 68 7799906 032339LI 3 W DOD-B- 82669 (OS) 3.2 Worhanship. The di-n-butyl sebacate shall be a water white, homogeneous liquid, free from dirt, sediment, and other suspended foreign matter when examined visually by transmitted light,
11、4. QUALITY ASSURANCE PROVISIONS 4.1 Responsibility for inspection. Unless otherwise specified in the contract, the contractor is responsible for the performance of all inspection requirements as specified herein. in the contract, the contractor may use his own or any other facilities suitable for th
12、e performance of the inspection requirements specified herein, unless disapproved by the Government. 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 prescribed requirements. Except as ot
13、herwise specified The Government reserves 4.2 Inspection provisions. 4.2.1 Lot formation, batch shall be a lot (see 6.3). continuous process, a lot shall cansist of material produced by one plant of one manufacturer, with no change in the process, materials or conditions and offered for acceptance a
14、t one time. 4.2.2 Sam ling. Sampling from tank cars shall be conducted in accordance wit + ASTM D-270. Sampling from smaller containers shall be conducted as follows: A random sample shall be taken from each lot, in accordance with MIL-STD-105, Inspection Level S-2, acceptance number zero. If there
15、are fewer than three containers in a lot, each container shall be sampled. selected. A 500 milliliter (mL) specimen shall be removed from each container in the sample and placed in a clean, dry container (nonreactive with di-n-butyl sebacate) with a tight fitting closure. shall be labeled to identif
16、y the lot and container from which it was taken. If the process is a batch operation, each If the butyl sebacate is produced in a In all other cases, no fewer than three containers shall be The container 4.2.3 Test specimens. A composite specimen shall be made with equal portions from each specimen
17、and the composite shall be tested as specified in 4.3. be tested as specified in 4.3. If there are fewer than three specimens, each one shall 4.3 Qualtiy conformance inspection, The material shall be subjected Iilhen specified to all the following inspections and tests for acceptance, in the contrac
18、t see 6.21 , 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 accordance with MIL-STD-1218 an
19、d distilled water shall be used. blank determinations shall be run and corrections applied where significant, Where applicable, 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-4,3.1 Visual inspection. All samples shall be visually inspected to dete
20、rmine conformance to the workmanship requirements of 3.2, 4.3.2 Test methds and procedures 4.3.2.1 Determination of color. The color of di-n-butyl sebacate shall be determined in accordance with ASTM Lk1209, platinum cobalt scale. 4.3.2.2 Determination of acidity. Measure 100 mL of ethyl alcohol int
21、o a flask, add three drops of phenolphthalein indicator, and titrate the alcohol to a faint pink color with 0.i.N sodium hydroxide solution. to the alcoholic solution, Calculate the percentage of acidity as acetic acid as follows: Add an accurately weighed 30 to 40 gram .(g) portion of the sample Ti
22、trate the mixture with 0.lbJ sodium hydroxide. Precent by wt acetic acid = 6.005 VN G where : v = sodium hydroxide required for titration of sample, mL N = norinality of sodium hydroxide solution G = weight of sample, g 4.3.2.3 Determination of saponification number. Transfer 0.8 g weighed to $: O.
23、1 milligram (mg)- of the sample to an appropriate size flask, and add 50 mL of O. 5N alcoholic. potassium hydroxide by means of a -calibrated burette or pipette. (0.a alcoholic potassium hydroxide is prepared by adding 28 g of potassium hydroxide to 1 liter of 95-percent ethyl alcohol), the flask to
24、 a reflux condenser by means of ground joints and heat .on a water bath until the precipitation appears to be cmplete. Add approximately 15 mL of water to dissolve the potassium sebacate and reflux on a water bathfor not less than 60 minutes with occasional whirling of the flask. Wash down the sides
25、 of the reflux condenser and the gound joints with approximtely 25 mL of the water. titrate with standard 0.31 hydrochloric acid using phenelphthalein indicator. Protect sample solution from carbon dioxide during heating and cooling with an ascarite guard tube. on 50 mL of alcoholic potassium hydrox
26、ide which has been carried through the complete process. Saponification ntunber (mg potassium hydroxide per g) Fit Cool the solution to 25OC and At the same time, conduct a blank determination Calculate the saponification number as follows: = (Vi - V?.)X N x 56.1 W where : VI = volume of hydrochlori
27、c acid solution required for blank titration, (fi) V2 = volwne of hydrochloric acid solution required for the sample titration, (mL) N = nomlity of the hydrochloric acid solution W = weight of sarrple, (g) 4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IH
28、S-,-,-DOD-B-82669( CE) 4.3.2.4 Detemination of refractive index. The following procedure shall be used for the determination of refractive index using a Bausch and mb Abbe refractometer or equivalent: a. refractometer with a tissue wet with methanol or xylene, and then with a dry tissue. circulating
29、 fluid so that the themmeter reads 25.0“+ 0.1“C. Wipe with caution to preclude scratching the prism surface of the Adjust the temperature of the water bath and the velocity of the b. Rotate the body of the instrument and the mving am amy from the operator until the interface between the prim is hori
30、zontal. prism clamp anddrop the lower prism. drops of the sample liquid to be tested to the lower prism. faces together and lock the prism clamp. normal viewing position. telescope, msen the With a glass stirring rod, add a few Rotate the instrument to the Bring the prism Adjust the mirror to reflec
31、t light into the c. Unclamp the index arm and Move it to the far end of the scale. The field my have a Focus the telescope eyepiece sharply on the crosshairs. field into view by mving the index arm forward. colored border, which can be achromatized by use of the compensators rotated by a pinion. The
32、 field will be sharpest when the edge is just turning blue. Bring the field almost into coincidence with the crosshairs by mving the index m. Adjust the mirror for the maximum illumination of the field. Obtain the final adjustment of the field line to the crosshairs by means of the fine adjustment s
33、crew. Bring the divided d. Focus the magnifier on the scale and rotate it so that the scale Read the scale directly to three decimal places and is well illuminated. -estimate the figure in the fourth dechal place. e. If the index reading does not remain constant within one unit in Place the fourth d
34、ecimal place for lminute, it may indicate diffusion of solvent remaining on the prim or insufficient time for thermal equilibrium. a new sample of the liquid to be tested on the prism taking care that the prism is clean and dry. Sufficient tim should elapse after placement of the drop to insure that
35、 the liquid film is at the prism temperature. f. Report the reading obtained as n25“C. 4.3.2.5 Detemination of misture. To the titration flask add 75 to 100 mL of methanol. Titrate- the methanol to a potentiometric end point with stabilized Karl Fischer reagent. sample of di-n-butyl sebacate (5 to 1
36、5 g) to the titration flask. the sample to a potentiometric end point. as follows: Tr&sfer an accurately weighed Titrate Calculate the misture content Percent misture = l(KF) w where : K = Xarl Fischer reagent used- in titration, mL W = weight of di-n-butyl sebacate,? g F = reagent factor, g of wate
37、r per mL of . - - reagent - - - - . . -. . _. 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-DOD-B-82669 68 M 9999906 OL23L97 7 M DoD-B-82669( OS) . 4.3.2.6 Determination of sodium. The sodium shall be determined in accordance with OD 43852 except
38、 that a factor of 1.17 shall be used. 4.3.3 Rejection criteria, Failure of any sample to meet any require- ment of this specification shall . cause for rejecting _. . . the lot or batch. 5. PACKAGING 5.1 Packaging. 5.1.1 Level C. The di-n-butyl sebacate shall be packaged in uniform quantities for sh
39、ipmnt in accordance with the manufacturers comnercial practice. Packages shall be of uniform size, shape, and mterial. 5.2 Packing. 5.2.1 Level C. The di-n-butyl sebacate shall be packed in unifonn Containers used shall comply with the Uniform quantities in such a mer as to assure carrier acceptance
40、 and afford pro- tection against damage during direct shipment fran the supply source to the first receiving activity. Freight Classification, National Motor Freight Classification, or other carrier regulations applicable to the mode of transportation. shall he of unifonn size, shape, and material.
41、Containers 5.3 Marking. In addition to any special marking required by the contract, unit packages and shipping containers shall be mked in accordance with MIGSTD-129. 6. 6.1 Intended use. The di-n-butyl sebacate covered by this specification 6.2 Ordering data. Procurement documents should specify t
42、he following: 6.2.1 Procurement requirements. is intended for use in the manufacture of propellant. a. b. c. Size of containers required d. Title, number, and date of this specification Whether tank cars or containers are to be used for shipment Whether a certified analysis and/or test report is req
43、uired 6.2.2 Contract data requirements. The items of deliverable data which may be required by this specification are cited in 4.3, Data Requirement Test Report Certified Analysis Applicable DID* DI-T-2072 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-Preparing Activity : NAVY - Project Number: 6810-NA44 QU.9. GOVERNMENT PRINTING OFFICE: 1979-603-022/1152 7 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-
