NAVY MIL-L-82661-1977 LECITHIN TECHNICAL《技术用卵磷脂》.pdf

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1、MIL-L-82bhl bw 777770b 0123078 5 w J Beneficial comments (recommendations, additions deletions) and any pertinent data which may be of use in improving this document should be addressed to: Commanding Officer, Naval Ordnance Station, Standardization Division (611) , Indian Head, Maryland 20640 by us

2、ing the self-addressed Standardi- zation Document Improvement Proposal (DD Form 1426) appearing at the end of this document or by letter. MIL-L-82 66 1 (OS) 31 January 1977 Superseding (see section 6) MILITARY SPECIFICATION LECITHIN, TECHNICAL This specification is approved for use by the Naval Sea

3、Systems Command, Department of the Navy and is available for use by all Departments and Agencies of the Department of Defense. 1. SCOPE 1.1 Scope. This specification covers one type of lecithin referred to herein as “the material“. 2. APPLICABLE DOCUMENTS 2.1 Issues of documents. The following docum

4、ents of the issue in effect on date of invitation for bids or request for proposal, form a part of this specification to the extent specified herein. STANDARDS Mi lit ary MIL-STD-105 Sampling Procedures and Tables for Inspection by Attributes MIL-STD-129 Marking for Shipping and Storage MIL-STD-1218

5、 ACS Chemicals (Copies of specifications, standards, drawings, and publications required by suppliers in connection with specific procurement functions should be obtained from the procuring activity or as directed by the contracting officer.) 2.2 Other publications. The following documents form a pa

6、rt of this specification to the extent specified herein. indicated, the issue in effect on the date of the invitation for bids or the request for proposal- shall apply. Unless otherwise Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- MIL-L-82663 68

7、W 7797706 0323077 7 W _ MIL-L- 66 i( s ) . ._ A$RICAN.SOCIETY FOR TESTING AND MATERIALS (ASTM) -, ASTM D 70-72 . Specific Gravity of Semi-solid Bituminous Materials (Application for copies should be ddressed to the American Society for Testing *- and.Materials, 1916 Race Street, Philadelphia, PA 191

8、03.) ,- _.L.% - INTERNAL -REVENUE SERVICE - .L -1RSP No. 368 Formulas for Denatured Alcohol and Rum (Application for copies should be addressed to the Superintendent of Documents, Government Printing Office, Washington, DC 20402.) NATIONAL MOTOR FREIGHT TRAFFIC ASSOCIATION, INC., AGENT National Moto

9、r Freight Classification (Applications for copies should be addressed to American Trucking Associations, Attn: Tarriff Order Section, 1616 P Street, Washington, DC 20036.) UNIFORM CLASSIFICATION COMMITTEE, AGENT Uniform Freight Classification (Applications for copies should be addressed to the Unifo

10、rm Classi- fication Committee, Room 1106, 222 South Riverside Plaza, Chicago, IL 60606. ) standards are generally available for reference from libraries. are distributed among technical groups and using Federal agencies,) (Technical society and technical association specif ications and They 3. REQUI

11、REMENTS 3.1 Material. The material shall be vegetable lecithin amber to reddish colored in a viscous liquid form. 3.2 Chemical and physical properties. The chemical and physical properties shall be in accordance with TABLE I. 3.3 Workmanship. The material shall be uniform, free from contamil nation,

12、 foreign material, or any other defect that would prevent its use for the purpose intended. 4. QUALITY ASSURANCE PROVISIONS I 2 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-L-826b1 68 = 777770b 0123100 T W I Viscosity at 25“C, poise - Specific

13、 gravity, 25“/25“C 1.02 Water content, wt% - Acid value, mg KOH/g - MIL-L-82661 (OS) 15 O 1.04 1.0 32 TABLE I. Chemical and physical properties. . Beneene insoluble, wt% Acetone insoluble, wt% I I i - 0.2 62 .O - I Property Values Minimum Maximum 4.1- Responsibility for inspection. Unless otherwise

14、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 requirements specified

15、 herein, unless disapproved by 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 prescribed requirements. The Government 4.2 Inspection conditions. Unless otherwis

16、e specified (see 6.2), all inspections shall be performed under the following conditions: a. Temperature: Room ambient 18 to 35C (65 to 95F) b. Altitude: Normal ground c. Vibration: None d. Humidity: Room ambient to 95 percent relative, maximum 4.3 Sampling. 4.3.1 - Lot Unless otherwise specified in

17、 the contract (see 6.2), a lot shall consist of all material manufactured,in one continuous production run or in one batch, under essentially identical conditions, from the same raw materials, and to be offered for acceptance at one time. Several batches, manufactured from the same raw materials, ma

18、y be blended to form a uniform larger batch which shall then constitute a lot for inspection purposes. 4.3.2 Sampling. Sampling for quality conformance inspection shall be in accordancewith inspection level I of MIL-STD-105. The sample unit Shall be one unit package or container of material. shall c

19、onsist of sufficient material to perform the quality conformance tests as specified-in 4.4. Each sample 3 . Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- MIL-L-82bbL 68 7777906 0123101 1 MIL-L-8 26 6.1 (OS) 4.4 Quality conformance inspection. Each

20、 sample obtained in accordance with 4.3.2 shall be subjected to the tests and examination of 4.5. When specified in the contract (see 6.2), the contractor shall furnish test reports showing quantitative results for all quality .conformance tests specified for each lot of material. The acceptable qua

21、lity level (AQL) shall be 2.5% defective. 4.5 Tests. Unless otherwise specified herein, all chemicals shall be ACS grade .in accordance with MIL-STD-1218. 4.5.1 Visual examination. All samples shall be visually examined to verify conformance to the workmanship requirements. 4.5.2 Viscosity determina

22、tion at 25OC. “he apparatus and procedures for the determination of viscosity at 25OC shall-be in accordance with the following: a. Apparatus: 1. Brookfield Viscometer, Model RVF, Brookfield Engineering Laboratories, Stoughton, Massachusetts, or equivalent. 2. Constant temperature water baths, maint

23、ained at 25OC. b . Procedure: 1. Remove the wood handle and mount the viscometer on a ring stand. Carefully attach the Brookfield No. 7 spindle. 2. Pour the sample into a 600 ml beaker, place in the water bath at 25OC and stir with a thermometer until the sample comes to the test temperature. air bu

24、bbles into the sample. Lower the viscometer on the ring stand until the surface of the sample is in the narrow section of the spindle. Level the viscometer, and operate at 20 RFM for determina- tions in the 100 to 2000 poise range, maintain the spindle depth in the sample so that the polymer level c

25、limbs midway up the narrowest section of the spindle. Obtain a series of readings until the value is constant. Use care to avoid stirring 3. During operation 4. c. Calculations: -. . 1. Using the No. 7 spindle at 20 rpm, and reading the O to 100 scale, calculate the viscosities as follows: Viscosity

26、 at 25OC, poise = (20) (scale reading) If a different spindle or speed is used, consult the chart accompanying the instrument for the proper multi- plying factor. poise by dividing by 100. Convert the resulting centipoise to 4 Provided by IHSNot for ResaleNo reproduction or networking permitted with

27、out license from IHS-,-,-NIL-L-2bbl b 7779906 0323302 3 MIL-L-82661 (OS) 4.5.3 Specific gravity (25/25OC). Specific gravity shall be determined at 25.0 ? 0.1OC in accordance with ASTM D 70-72. 4.5.4 Water content. The water content shall be determined in accordance with the following: a. b. C. d. e.

28、 - - Reagents : 1. Methanol 2. Carrier solution - 3:lmixture by volume of pyridine and methanol 3. Stabilized Karl Fischer reagent, diluted to a water equivalent of 2.5 to 3.0 milligram/milliliter (mg/ml) with Karl Fischer Diluent. 4. Sodium tartrate Apparatus: Standardization of Karl Fischer reagen

29、t: methanol to the reaction vessel. Neutralize the znethanol with dilute Karl Fischer reagent by automatically titrating to a 30 second end point using the Aquameter. to 0.11 g of sodium tartrate weighed to the nearest 0.1 mg, to the neutralized methanol. Dissolve the sodium tartrate in the methanol

30、 by setting the stirring action to the highest speed which will not cause splashing or bubble.formation. Automatically titrate with dilute Karl Fischer Reagent to a 30 second end point. Reagent. determinations agree within 0.05 mg/ml. Calculate the water equivalent of the dilute Karl Fischer reagent

31、 as follows: Aquameter, Beckman Model KF-4, or equivalent. Add 100 ml of Carefully add 0.09 Record the volume of dilute Karl Fischer Repeat the standardization procedure until three A= 156.6B C where : A= B= C= 156.6 = water equivalent of the dilute Karl Fischer reagent, mg/ml weight of sodium tartr

32、ate, g volume of dilute Karl Fischer reagent used to titrate the standard, ml factor for sodium tartrate Procedure: Add 100 ml of the carrier solution to the reaction vessel. Purge with dry air, Neutralize the carrier solution with dilute Karl Fischer reagent by automatically titrating to a 30 secon

33、d end point using the Aquameter. Add 6 to 10 g of sample weighed to the nearest 0.01 g to the carrier solution in the reaction vessel. same as that used in the standardization. Dissolve the sample and automatically titrate with standardized dilute Karl Fischer reagent to a 30 second end point. Karl

34、Fischer reagent. Set the stirring action action the Record volume of dilute 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-L-82663 68 W 999990b 0323303 5 MIL-L-82661 (OS) f. Calculate the water content as follows: c -4 water content, wt% =I AD

35、 x 100 1000E where: A = water equivalent of the dilute Karl Fischer D = volume of standardized dilute Karl Fischer E = sample weight, g reagent (from d. above), mg/ml reagent used to titrate sample, ml 1000 = multiplication factor to convert g to mg g. Report the results of -a minimum of 2 determina

36、tions and their average. 4.5.5 Acid value. Acid value shall be determined in accordance with the following: a. Reagents: 1. Standardized 0.1 normal (N) sodium hydroxide (NaOH) 2. Ethyl alcohol, 95 percent denatured, Formula D-30 conforming to IRSP No. 368 (neutralized to phenolphthalein just prior t

37、o use). 3. Petroleum ether. 4. Phenolphthalein indicator, 1 percent in ethanol. b. Apparatus: 1. Erlenmeyer flask, 250 ml. 2. Microburet, -. 10 ml. c. Procedure: Warm (not over 60C) the sample, if necessary, to soften the material and then mix thoroughly, of sample, to the nearest 0.1 mg, into a 250

38、 rnl Erlenmeyer flask. Then add 50 ml of neutral ethyl alcohol and shake to mix, four drops of phenolphthalein indicator and titrate while shaking with 0.1 N NaOH to the first pink color which persists for approximately 5 seconds. tained by adding the bulk of the NaOH solution rapidly until near the

39、 end point, and then slowly down to four, then two drops at a time. During the early addition of the NaOH, the mixture will become clear. As additional NaOH is added, two phases will occur. the NaOH should begin and the lower phase observed for the end point Weigh 1.8 to 2.0 8 Dissolve in 50 ml of p

40、etroleum ether by shakinR gently. Add The end point is fairly easily ascer- At this point, slow incremental addition of Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-L-82661 (OS) d. Calculation: Acid value, mg f(OH = 56.1VN W g where: V = volum

41、e of standardized NaOH, ml N = normality of standardized NaOH W = weight of sample, g 56.1 = molecular weight of potassium hydroxide (KOH) e. Report the results of a minimum of 2 determinations and their results. .4.5.6 Benzene insolubles. The benezene insolubles shall be deter- mined in accordance

42、with the following: a. Apparatus: Filtering crucible, Selas, 30 ml, fine porosity, or equivalent. b. Reagent: Benzene. c. Procedure: Weigh 10 to 11 g of sample, to the nearest 0.1 mg, into a 250 ml beaker. Add 100 ml of benzene and stir until dissolved. crucible and wash the remaining insoluble matt

43、er into the crucible using two 25 ml portions of benzene. Maintain suction for approximately 5 minutes until the sample is free of benzene. Dry the sample at 105“ f 5“ C for a minimum of 1 hour, cool and weigh. Filter the sample quantitatively through a Selas (A-B ) W d. Calculation: Benzene insolub

44、les, wt% = -.X 100 where: A = weight of crucible and insoluble matter, g B = weight of crucible, g W = weight of sample, g e. Report the results of a minimuro of 2 determinations and their average; 4.5.7 Acetone insolubles. Acetone insolubles shall be determined in accordance with the following: a.

45、Reagent: Acetone, presaturated with purified acetone insoluble material (phosphatides) 1. . Purification of phosphatides - Purify phosphatides from previous acetone insoluble determination by dissolving approximately 5 g in 10 ml of petroleum ether and reprecipi- tating with 25 ml of acetone. is fre

46、e from conglomerates before further processing. Transfer the precipitate to two centrifuge tubes using additional acetone to facilitate the transfer. Stir thoroughly and make to volume of 45 mi, stir, chill for a minimum of 15 minutes in ice bath at 0 to SOC, stir again and centrifuge for a minimum

47、of 5 minutes. Decant acetone soluble, break up solids with stirring rod, refill tubes Ascertain the precipitate 7 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-L-82661 b8 m 777790b 0323105 7 m MIL-L-82661 (OS) with acetone; stir, chill, centrif

48、uge and decant as before. The solids, after the second centrifugation, require no further processing and may be used, as is, for presaturating acetone. L - 2. Saturation of acetone - add purified phosphatides to acetone at O“ to 5C. 5.0g of the phosphatides are sufficient for about 16 liters of acet

49、one. Maintain at O“ to 5C for about 2 hours, shaking vigorously at approximately 15 minute intervals. Decant through a rapid filter paper avoiding transfer of any of the solids to the paper and conducting the filtration under refriger- ated conditions (Oo to 5C) in order to maintain the same conditions for saturation as described under the procedure. b. Apparatus : 1. Centrifuge, motor driven with head to