NAVY MIL-L-17700-1953 LEAD SALICYLATE《水杨酸化铅》.pdf

1、MIL-L-17700( Nord) 17 September 1953 MILITARY SPECIFICATION LEAD SALICYLATE 10 SCOPE 1.1 Scope. - This specification covers one grade of lead 2. APPLICABLE SPECIFICATIONS, STANDARDS, AND PUBLICATIONS 2.1 The following specifications, standards, and publications, salicylate intended for various milit

2、ary applications. of the issue in effect on date of invitation for bids, form a part of this specification: S PECIFI CATIONS FEDERAL RR-S-366 - Sieves; Standard, Testing NAVY General Specifications for Inspection of Material STANDARDS MILITARY MIL-STD-129 - Marking of Shipments (Copies of specificat

3、ions and standards required by contractors in connection with specific procurement functions should be obtained from the procuring agency or as directed by the contracting officer,) issue in effect on date of invitation for bids, forms a part of this specification: 2.2 Other publications. - The foll

4、owing publication, of the / -, .6 63 c, . THIS DOCUMENT CQNTAIMS PAGES, 6810 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-L-17700 b8 = 7797906 01L7L53 L . -Code -of.-Federal Regulation k9CFR 71.1 - Transportation, Interstate Commerce Commissio

5、n, Explosives and Other. T,.d. Washington 25, D.C. Prices may be obtained from Mie Superintendent of Documents. ) Li - . ., . . . . - _. .I _. . . -, y.-.-, 3.2.2 Total salicylate content. - Maximum, 59.0 perkent; minimum, 55.0 percent. . - . - * . 9. . i . .i . . 3.2.3 Free salicylic ac,id. content

6、 - E4axlqwn, 1.0 percent. - . . . SC. . -,-. ?.? ., , . . I :. _. . . -. 3.3 Diethylene glycol insoluble material. - Maximum, 2.5 ,. percent. . r . 3.4 Color -0 Cre.whit i t o pure- whit e. 3.5 Granulation. - Lead salicylate shall conform to . . . -,. -. following requirement using U. S. Standard si

7、eves conforming to Federal Specification RR-S-366, unless otherwise speclfied: .- . . . -,. : : - ta - , i,“ -S. I-: _. . Retained on No. 325 “.: . . * 0.5 Pei-cent; .maximiim- “ *, =* * 4f.:3,mpLN.G; . -I,.- z.spEtTio:N . . ., . C? - . ,-. - . . . .- . . . . . . . .- . . ._ :? .* . . . ._ . ! . -.-

8、 . . .* ,. ., . ._ 4.1 Lot Unless otherwise pecifikd, a“iot :shali. consist 4.2SPrnplihg.+,TiIi percent. $lit in m-.casemore than 10 or less than.3 of the contairierd sha1l.h selected :from each lot by the inspector 80 as to be representative of the ot. there are fewer than 3 containers in the lot,

9、all the containers shall be sampled. The material shall be thoroughly mixed and approximately 8 ounces of it shall be taken from each selected container. airtight container and labelled so that the container from which .- of not more than 10,000 pounds. . ._ , . - . . : ifF, ; ,.;i. . . I .- - r,- -

10、, e*? If Each of these primary samples shall be placed in an 2 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-. L _. . . 3. Nitric acid, C.P., 1ead“content not greater than ,00002.-percent. . -_._ - 5 ml. of 1:l sulfuric acid solution and heat until

11、 the solution is clear, Cool, dilute to 90 ml, with water, and adjust to a pH of 1.4 with 10 percent potassium hydroxide solution,-using a pH meter, and finally dilute to 100 ml, This solution will last indefinitely when stored in a glass stoppered flask, 5. Sodium salicylate COP, (alternatively COP

12、, salicylic acid may be used), fNH ) SO .24.H20, in 50 al, of water, - - 4.4.3.3 Standard Curve, - Prepare a standard solution of salicylate as follows: Add exactly 0,2000 grams of sodium sali- cylate to about 900 ml, water in a beaker, then regulate the pH to 2.7 by the addition of 6 percent acetic

13、 acid, Finally transfer to a 1 liter volumetric flask and dilute to the mark with distilled water, curve by withdrawing aliquots of 1 ml, 2 d., 4 ml., 5 ml, and 6 ml, Place each of the aliquots in a 25 ml, volumetric flask, add 0.25 ml0 of the ferric alum solution and dilute to the mark with the wea

14、k acetic acid (pH 2.7) solution, Albw 5 minutes for full color development. solutions against a ferric alum blank, exactly the same as the solutions above but without adding salicylate. Wave length 520 mpis used for all absorbance readings, in terms of salicylate, using the data of column 3 of the f

15、ollowing table: Establish points for the calibration Obtain absorbancereadings of these The blank is made up The concentration 8Cah is most conveniently plotted - Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-L-177UO 68 7777706 0117158 O W MIL-

16、L-17700( Nord) SUMMARY OF CALIBRATION DATA Salicylate Standard Solut ion ml 1 2, k 5 6 Theoretical Salicylate Equivalence mg per 25 ml Absorbance Values ob17 To be determined Ob34 To be determined 0,68 To be determined Ob85 To be determined 1.03 To be determined From the standard graph a table can b

17、e prepared for routine work giving percent total salicylate readings corresponding to small increments of absorbance when the prescribed weight of sample and size of aliquots have been employed. 4bkb3.k Procedure. - i, Accurately weigh a 0,3OOO gram sample and transfer it to a 1 liter volumetric fla

18、sk, Add 25 ml, of glacial acetic acid, measured with a pipet, and swirl the mixture to facilitate dissolution of the material, When the sample is in solution (it may be slightly cloudy at this point) the solution is diluted to volume with distilled water, - 2. When the solution is thoroughly mixed w

19、ithdraw 10 db aliquots and transfer to 50 ml, volumetric flasks. Add 0,50 ml, of the ferric alum solution and dilute to volume with the weak acetic acid (pH 2.7) solution, Transfer the colored solution to a 1 cm, cell of the Beckman spectrophotometer or to the cell of the photoelectric colorimeter.

20、Prepare a blank forspectrophotometric comparison by transferring Ob5O ml. of the! ferric alum solution to a 50 ml, volumetric flask and diluting to volume with the weak acetic acid (pH 2,7) solution, Make absorbance readings at 520 my on the Beckman spectrophotometer. instrument is used, the filter

21、transmitting in the 500-550 merange is seected for use. When a filter 3, The quantity of salicylate present is read from the standard graph and the percent total salicylate in the material calculated, - - - . - - f- .7 Provided by IHSNot for ResaleNo reproduction or networking permitted without lice

22、nse from IHS-,-,-. NIL-L-37700 b W 7977706 0337357 2 MIL-L-17700( Nord) 4.4.4. Free salicylic acid content. - 4.l+4.1 Apparatus. - 1, A Beckman Kode1 DU Spectrophotometer with . ultra-violet source and 1 cm. silica cells. 2. Filter paper, Whatman No. 1, 3. 60 filter funnels. 4. Volumetric flasks, 1

23、liter, 100 ml., 50 ml. 5. Beakers, low form, 250 ml. and 10 ml. pipets. 444.2 Reagents. - 1, Chloroform, C.P. CHC13. 2. Salicylic acid, C.P, 4.f+.4.3 Standard curve. - The standard curve may be made most easily by dissolving a known amount of C.P. salicylic acid in C.P. chloroform and making reading

24、s on known dilutions of this solution with C.P. chloroform in the reference cell. For example, 100 mg of salicylic acid dissolved in 1000 ml. of chloroform will serve as a strong stock solution from which the following dilutions may be prepared. Made Up mg. Sal. Acid in CHC13 per 100 ml. ml. of Stoc

25、k Solution to ml. Dilute Solution of solution (d tt n 100 100 100 100 100 50 50 100 5 2.5 2.0 1.5 1.0 Readings are all taken at 310 mp using a slit width chosen for best sensitivity (a slit width of 0.22 was used in developing the procedure). The plot should give a straight line passing through the

26、origin. 8 /,- Y t: -. 1 L Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-L-L7700 bB 7777906 OLL7160 7.W. : . :be packaged .and. .packed in substantial commercial zantainem :so- :constructed -8s .to insur.e acceptance by common .or other carri.er

27、 ;for :safe transportatLon :atl ;the lowest rate- to. 5he :.paint .of delivery,. I 5.2 Karkihg, -a In:.additianto any :special-markin-rrgs-shall. conform with the applicable regulations of the- Interstate Commerce Commission, Notice, 0 -When-Governmnt drawings, specifications, or other - data are us

28、ed .forany purpose tother than in connection with a -: definitely related Government-procurement operation, the United Statts.Government:thereby incurs no responsibility nor any obli- gation whatsoever; and the fact that the Government may have formulated, furnished, or in any way supplied the said

29、drawings, specifications, orother data is not to be regarded by implica- tion or otherwise as in any manner licensing the holder or any other person or corporation, or conveying any rights or permission to nianufacture use, or sell any patented invention that nay in any way be related thereto, 10 . Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-