1、MIL-D-SLLILO 68 W 9999906 0121897 3 = - /Y- kS-17 MIL-D-51410 (EA) 22 October 1974 -(See section 6) MILITARY SPECIFICATION DYE , GREEW , ETHYL-BIS( 2,4-DINITROPHENYL) ACETATE This specification is approved for use by all Departments and Agencies of the Department of Defense. 1. SCOPE 1.1 This specif
2、ication covers one type of ethyl-bis(2,b-dinitrophenyl) acetate (DA). - 2. APPLICABLE WCUMENTS 2.1 Government documents. The following documents 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. SPECIFICA!L
3、IONS FEDERAL RR-S-366 - Sieve, Test. STANDARDS MILITARY MIL-STD-105 - Sampling Procedures and Tables for Inspection by Attributes. (Copies of specifications , standards , drawings, and publications required by suppliers in connection with specific procurement functions should be obtained from the pr
4、ocuring activity or as directed by the contracting officer. ) Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MILD-51410 (EA) 2.2 ther publications. The following documents fora a part of this specification to the extent Specified herein. Unless othe
5、rwise indicated, the issue in effect on date of invitation for bids or request for proposal shall apply. AMERICAN SOCIETY FOR TESTING AND MATERIALS (ASTM) STANDARDS DlSg3-72 - Reagent Water, (Application for copies should be addressed to the American Society for Testing and Wterials , 1916 Race Stre
6、et , Philadelphia, Pennsylvania 19103. (Technical society and technical association specifications and stand- ards are generdly available for reference from libraries. distributed among technical groups and using Federal agencies. ) They are also Munsell wok of Color (The Munsell Book of Color may b
7、e obtained from the Munsell Color Company, Inc *, 2441 N. Calvert Street Baltimore, Maryland 21218. ) Pharmacopeia of the United States of America, Eighteenth Revision (Copies may be obtained from the Mack Publishing Company, Easton, Pennsylvania 18042 . ) 3. FEQUIREMENTS 3.1 Chemical and physical c
8、haracteristics. The dye shall conform to the chemical and physical characteristics of table 1 when tested as specified therein. Table I, Chemical and physical characteristics Requi r emen? : Test : . Characteristic : Minimum : Maximum : paragraph: . : Molar absorptivity at 242 5 2 : nanometers (nm)
9、: Melting point, OC : Volatile matter at lSo C, percent : by weight : Particle size, percent by weight : retained on: * 149-micron (No. 100) sieve 74-micron (NO. 200) sieve . 44-micron (No. 325) sieve . : 4.2.4,l : : 4.2.4.2 : : 4.2.4.3 : : 4.2.4.4 : Provided by IHSNot for ResaleNo reproduction or n
10、etworking permitted without license from IHS-,-,-MIL-D-5L410 68 7797706 OL2L897 7 MIL-D-51410 (U) 3.2 Characteristics of paper containing dye. A paper approximately 6 mils thick and containing 1.0 2 0.3 percent by weight of the dye shall be prepared from strong-bleached sulfite or sulfate pulp (see
11、6.5). The dye cgntent of the paper shall be verified by testing the paper as specified in 4.2.4.5. 3.2.1 Color. The color of the paper shall match one ofthe Musell colors listed in table II when tested as specified in 4.2.4.6. Table II. Munsell colors for paper containing dye Hue Value : Chroma 1 1
12、1 5. OGY 9 : 1O.OY 9 5.OY 9 N 9.5 N 9 3.2.2 Color stain produced by test reagent. When one drop of test reagent is applied to the paper as specified in 4.2.4.7, a visible color stain shall be produced within 40 seconds. the MusePl colors listed in table III. The color of the stain shall match one of
13、 Table III. Munsell colors for stain produced by test reagent 1 Hue Value : Chroma : 10,OB 3 2. SB 3 4 3 7. 5B 7.5B , * 4 . 4 4 4 4. QUALITY ASSURANCE PROVISIONS 4.1 Responsibility for inspection. Unless otherwise specified in the contract or purchase order, the supplier is responsible for the perfo
14、rm- ance of all inspection requirements as specified herein. wise specified in the contract or order, the supplier may use his own or any other facilities suitable for the performance of the inspection require- ments specified herein, unless disapproved by the Government. The Government reserves the
15、 right to perform any of the inspections set forth in the spec- ification where such inspections are deemed necessary to assure supplies and services conform to specified requirements. Except as other- 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-
16、,-. A lot shall consist of the dye produced by one manu- facturer, at one plant, fromthe same materials, and under essentially the Bame manufacturing conditions provided the operation is continuous. In the event the process is a batch operation, each batch shall constitute a lot (see 63) . 4.2 . 2 S
17、ampling. 4,2,2.1 For examination of preparation for delivery. Sampling for examination of preparation for delivery shall be conducted in accordance with MIL-STD-105, inspection level S-4, using an AQL of 2.5 percent defective. 4.2.2.2 For test, Sampling for test shall be conducted in accordance with
18、 table IV, shall be removed from each sample container and placed in a suitable clean, dry container labeled to identi* the lot and container from which it was taken, A representative specimen of approximately 50 gram (g) Table IV. Sampling for test : Number of containers in batch or lot : Number of
19、jample containers : I . 2 to 25 I 26 to 150 151 to 1,200 . 1,201 to 7,000 : 7,001 to 20,000 * Over 20,000 . 2 3 5 10 20 a 4,2,3 Inspection procedure. 4.2 . 3.1 For examination of preparation for delivery. The sample unit shall be one filled container, ready for shipment. and the preparation for deli
20、very thereof shall be examined for the follow- ing defects using an AQL of 2,5 percent defective: Sample containers (a) (b) Container not as specified (c) (a) Container damaged or leaking (e) Contents per container not as specified Container closure not as specified Marking incorrect, missing, or il
21、legible 4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-D-51410 (EA) 4.2.3.2 For test. as specified.4. for rejection of the lot represented. Each sample specimen taken in 4.2.2,2 shall be tested Failure of any test by any specimen shall be caus
22、e 4.2.4 - Tests. Water ir, accordance with ASTM D1193-72 and reagent grade chemicals shall be used throughout the tests. Where applicabe, blank determinations shall be run and corrections applied where significant. Tests shall be conducted as follows: 4.2.4.1 Molar absorptivity. Weigh to the nearest
23、 0.1 milligram (mg) approximately 0.40 g of specimen into a 500-milliliter (mi) volumetric flask. Add 250 mi of chloroform and stir to solution using a magnetic stirrer, if required. Remove the stirring bar, dilute to the volume mark with chloroform, and shake thoroughly to mix. Pipet 5 ml of the so
24、lution into a 500-mi volumetric flask, dilute to the volume mark with chloroform, and mix thoroughly. recording spectrophotometer , 10-millimeter silica cells , and chloroform in the reference cell, run an absorbance curve of the solution from 200 to 300 nm. Run zero line in the same range using chl
25、oroform in both cells. Read the absorbance at 242 5 2 nm. Calculate the molar absorptivity as follows: Using an ultraviolet lamp on a suitable double-beam Molar absorptivity = “7 420A BC where: A = Blank-corrected absorbance at 242 2 2 nm, B = Cell path length in centimeters, and C = Effective speci
26、men concentration in grams per liter, 4.2.4.2 Melting point. Determine the melting point of the specimen in accordance with the Melting Range or Temperature test, Procedure for Class I contained in the Pharmacopeia of the United States of America , Eighteenth Revis ion. 4.2.4.3 Volatile matter. Weig
27、ht to the nearest 0.01 g approximately 1 a of the specimen into a suitable moisture dish and weigh to the nearest miiligram. in a desiccator, and weigh to the nearest milligram. by weight volatile matter as follows: Heat to constant weight at 115O + 5O C, cool to room temFerature Calculate the perce
28、nt Percent volatile matter = 100(A - B) W where: A = Weight of dish and specimen before heating in grams, B = Weight of dish and specimen after heating in grams, and W = Weight of specimen in grams. 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-M
29、IL-D-51410 (EA) 4.2.4.Q Particle si,ze-. Use sieves conforming to RR-S-366. Nest the sieves specified in table I in order of decreasing mesh size (with the largest mesh sieve on top) on a receiving pan. approximately 10 g ofthe specimen. in a beaker by stirring with a glass rod to produce a smooth p
30、aste. Carefully vaeh the thoroughly wetted specimen through the sieves. of a wetting agent is permitted) , cool to room temperature, and weigh the material retained on each sieve. Calculate the percent by weight material retained on each sieve. Weigh to the nearest 0.1 g Mx the specimen with suffici
31、ent water (The use Dry the sieves in an oven at 70 to 75 C, 4.2.4.5 Dye content of paper. (a) Standard solution. Prepare a standard solution of the dye used to make the paper in accordance with the procedure used for the colu- tion tested in 4.2,4,1 (b) Specimen solution. Cut a piece of the paper we
32、ighing approximately 1,O g and weigh to the nearest 0.1 mg. Extract the &ye with six 20- to 30-ml porbions of chloroform. extract to a 250-ml volumetric flask. Dilute the combined extracts to the volume mark with chloroform and mix thoroughly. into a LOO-ml voluaeb5.c flask, dilute to the volume mar
33、k with chloroform, and mix thoroughly. of the specimen solution using the spectrophotometric procedure specified fn 4.2.4.1* solution at 242 2 2 nm. follows : Quantitatively transfer each Pipet 25 mi. of the solution (c) Procedw.e. Run absorbruice cures of the standard solution and Rea the absorbanc
34、e of the standard solution and specimen Calculate the percent by weight dye in the paper as Percent dye = 2AE - BD where: A = Blank-corrected absorbance of specimen solution at 242 2 2 nm, B Blank-corrected absorbance of standard solution at 242 2 2 nm, D = Weight of paper in grams, and E = Weight o
35、f specimen usedto make standard solution in grams. 4.2.4.6 Color of .paper containing ye Determine the Munsell color of the paper by comparison with a Munsell Book of Color. 4.2,4.7 Color stain produced by test reagent. (a) Test reagent. Prepare a solution of 14.7 percent by weight tetrahydrofurfury
36、l alcohol, 3.4 percent by weight N-methylglucamine , and 81.9 percent by weight diethylene glycol. Stir for at least 30 minutes and allow to stand overnight. reagent Centrifuge and use the clear liquid as test 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license fro
37、m IHS-,-,-MIL-D-SLLILO 68 W 7777706 01123703 5 m MILD-51410 (EA) (b) Procedure. Place one drop (0.2 ml) of the test reagent on the paper containing the dye and measure the time required for the develop- ment of a stain. stain by comparison with a Munsell Book of Color. After 40 seconds, determine th
38、e Munsell color of the 5. PREPARATION FOR DELIVERY 5.1 Packing, level C. be packed in a nominal 5-gallon capacity steel pail furnished with a gasketed, fully-removable lug cover. alteration of contents and to assure safe delivery to destination without damage or leakage. The dye shall be packed to m
39、eet carrier acceptance at the lowest rates in compliance with requirements of carrier rules and regulations applicable ta the mode of transportation. A quantity of 40.0 (+0.2 or 4) pounds of dye shall The dye shall be packed in a manner to prevent 5.2 Marking. Each pail shall be marked by any means
40、which provides legibility as follows : (a) Instructions on side of pail: FOR COVERED STORAGE ONLY (b) be applied to the cover and side of each -pail (c) (fi) (e) Net weight of contents (f) (g) Contractors name (h) (i) Appropriate address markings Nomenclature as cited in the contract or purchase ord
41、er shall National Stock Number (NSN) or part number when NSN is not given Government eontract Or purchase order number Lot number, date of manufacture, and date of pack. Additional markings as may be required by the contract and the contractors policies and procedures 6. MOTE3 6.1 Intended use. The
42、dye covered by this specification in intended for use in the manufacture of M8 chemical agent detector paper. 6.2 Ordering data. Procurement documents should specify the title, number, md date of this specification. 6.3 - Batch. A batch is defined as that quantity of material which has been manufact
43、ured by some unit chedcai. process or subjected to some physical mixing operation intended to make the final product substantially uniform. - 6.4 Significant places. For the purpose of determining conformance with this specification, an observed or calculated value should be rounded off “to the near
44、est unit“ in the last right-hand place of figures used in expressing the limiting value, in accordance trith the rounding-off method of the Recommended Practices for Designating Significant Places in Specified Limiting Values (ASTM E29). . Provided by IHSNot for ResaleNo reproduction or networking p
45、ermitted without license from IHS-,-,-, 6.5 Manufacture of paper containing dye. A method of making paper hand sheets containing dye is described in “Production Engineering Study for 148 Paper Byes )I Report No a 11 August, i969 available from Edgewood Arsenal. However, the Government makes no warra
46、nty that paper made in this manner will meet the requirements of this specification. 6.6 Supersession data. This specification supersedes and includes the requirements of Edgewood Arsenal Purchase Description 197-54-840, dated 4 October 1963. Custodian: Am - EA .k U. 5. GOVERNMENT PRINTING OFFICE: 1974.603-1 12/31 13 8 Preparing activity: Project No. 6820-AO65 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-
