1、MIL-H-22868 b 3939906 OLLBLLS b W MIL-H-22868 (Wep) 21 March 1961 MILITARY SPECIFICATION KYDROGEIJ PEROXIDE, E-STABILIZED, 76 AND 9C$ FOR ToRpE;1no USE-) TMs specirlcatiti been approved by the Bureau of Naval WeapPn.6. Department of TENa-i, 1. SCOPE 1.1 This specification covers aqueous solutions of
2、 hydrogen peroxide in which additives have been dissolved to impart a low decomposition rate, to repress the effects of accidental catalytic contamination and to prevent corrosion of aluminum containers. hydrogen peroxide solutions are designated as “Ew stabilized. the following grades as specified
3、(see 6.2) Such 1.2 Classification - E-stabilized hydrogen peroxide shall be of Grade 7OE- 7 hydrogen peroxide by weight Grade 9OE- 96 hydrogen peroxide by weight 2. APPLICABU DOCUMENTS 2.1 The following specification and standards, of the issue in ef,tct on date of invitation for bids, form a part o
4、f this specication: SPECIFICATION Military ) ._-, . MIL-A-799 - Aluminum, High-Purity, Wrought MILSTD-O MIL-STD-12g - Sampling Procedures and Table for Inspection by Attributes - Marking for Shipment and Storage (Copies of specifications, 8 tandards, drawings, and publications, required by contracto
5、rs in connection with specific procurement functions should be obtained from the procuring agency or as directed by the contracting officer . ) 2.2 Other Publications - The following publication forms a part of this specification. on date of invitation for bids shall apply. Unless otherwise indicate
6、d, the issue in effect NAVY DEPAHTMENT, BUREAU OF NAVAL WEAPONS NAVORD Report 543 - Navol Loading Depot IVLVORD Report 5216 - Introduction to Hydrogen Peroxide THIS DOCUMfPX CO“!A#8 u PAGES, Ir Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-1-22868
7、(Wep 1 (Copies of these reports required by contractors in connection with specific procurement functions should be obtained from the procuring agency or as directed by the contracting officer.) Regulations for Tramportation of Explosives and other Dangerous Articles, eta. (Application for copiei eh
8、ould be addressed t0 the Superintendent of Documente, Government printing Office, Washington 25, D. a.) 3. m- 3.1 Material - The E-stabillred hydrogen peroxide shall be clear, colorless solution of hydrogen peroxide and additives in water. 3.2 Concentration - The aoncentration (7% or 9) shall be spe
9、cified by the bureau or agency concerned, and shall be designated as the percent hydrogen peroxide by weight contained in the solution. Unless otherwise specified, this concentration shall not vary by more than plus 1.0 or minus 0.5 percent. 3.3 Additives - E-stabilized hydrogen peroxide solutions s
10、hall contain the following constituents: Tin (Sn) Phosphate (PO4-) Nitrate (NO3-1 respectively introduced in 7C$ or 96 hydrogen peroxide by use of the following additives: . 32 / 4 milligrams per liter 29 7 4 milligrams per liter i10 ;i 20 milligrams per liter - Sodium stannate (NanO3.3?) Sodium pho
11、sphate, Dibasic, Dodecahydrate Bodium nitrate (?03) and Nitric acid (?03) for pH adjustment (Na2m4.mg) 3.4 Objectionable inrpurtiee - One liter of E-Stabilized hydrogen peroxide solution shall contain no more than i milligram of Chloride (ci?) an 10 miUigrams of Suifate (SO4?) when tested in accorda
12、nce with 4.5.6 and 4.5.7 respectively . 3.5 Evaporation Residue - The evaporation residue, when tested a8 specified in 4.5.8 shall not exceed 325 milligrams per liter. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-I 3.6 Stability - E-stabilized hyd
13、rogen peroxide solutions shall not lose more than 2.0 peruent (maximum) of its original active oxygen when tested according to 4.5.9. 3.7 Acidity, pH - Unless otherwise requested by the contractor and agreed to by the purchasing activity, the apparent pH of E-stabilized hydrogen peroxide solutions,
14、determined as specified in 4.5.10 shall be: 1.4 0.2 0.2 for Grade 70 E 0.2 for Grade 90 E - - If necessary, pi? adjustment is made by the use of either pure nitric acid, or pure sodium hydroxide solutions in pure water. 3.8 Surface Tension - Unless otherwise requested by the contractor and agreed to
15、 by the purchasing activity, the surface tension of E-stabilized hydrogen peroxide solutione when determined by the method of 4.5.11 shall be no less than the following values: Grade 70 E Grade 90 E 4. QUALITY ASSURANCE PROVISIONS Minimum Surface Tension (dynes/centimeter ) 72 at 2Ooc 74 at 200 4.1
16、The supplier is responsible for the performance of all inspection requirements as specified herein. Except as otherwise specified, the supplier may utilize his own or any other inspection facilities and services acceptable to the Government. inspection records of the examinations and tests shall be
17、kept complete and available to the Government as specified in the contract or order. The Government reserves the right to perform any of the inspections set forth in the specification where such inspections axe deemed necessary to assure supplies and services conform to prescribed requirements. 4.2
18、Swingl 4.2.1 Lot - For purposes of sampling, a lot shall consist of all material of the same type offered for delivery at the same time in drums filled from one storage tank at one time. 4.2.1.1 When offered in tank car or storage tank - For purposes of sampling, a lot shall consist of all material
19、of the same type, stored in one storage tank, and offered for delivery at the same time. Ali glassware and equipment for purposes of sampling shall be properly cleaned and passivated prior to use. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-H
20、-22868 68 m 7797706 OLL8122 b m 4.2.1.2 Time of Sampling - Sunpling shall be acconrplirhed not earlier than three weeks prior to shipping date. 4.2.2 Sampling for Inspection of filled Containers - A rriitnain sample of filled containers shallbe relected from each lot by the inspector in accordance w
21、ith Standard MIL-STD-105 at Inspection kvel I and acceptable quality level (AU) equal 2.5 percent defective to verify compliance with this specification regarding fill, olosure, marking, and other requirements mt involving tests. 4.2.3 Sampling for each sample filled container shu also be weighed to
22、 determine the amount of the contente. furnished by the manufacturer shall be accepted an tare weights shall not be verified unless the inspctor has evidence that these may not be correct. to detect any unusual temperature; and his ear to detect any sound of activity within the drum; these are signs
23、 of decomposition of the hydrogen peroxide, and any drum showing either is defective. sample having one or more defects, or under required fill, shall be rejected and if the number of defective containers in any sample exceeds the acceptance number for the appropriate sampling plan of Standard MILST
24、D-105, the lot represented by the ample shall be rejected. The tare weights The inspector shall place his hand on each of the sample drums Any container in the 4.4 Lot Acceptance Tests - Samples selected in accordance with 4.2.3 shall be subjected to the tests specified in 4.5. Lots shall be accepte
25、d or rejected on the basis of the laboratory test results of these samples. weeks after the sampling date. is found to be not in conformance with this specification, the lot which it represents shall be rejected. 4.4.1 Time of Testing - Testing shall be performed not later than four 4.4.2 Action in
26、case of failure - If any one of the samples tested Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-4.4.3 Reports on Inspection end Tests - Two copies of each lot acceptance iaspection and test report shall be forwarded to the procuring activity and t
27、he Bureau of Ordnance by the inspector. The inspection and test report shall certify the results of the required Geternination, the dates of sampling, test and shipment, and shall include a brief description of the test methods employed, in case any deviation from these epecified under 4.5 have been
28、 adopted. 4.5 Test Procedures1 4.5.1 Visual Inspection - Twenty-five milliliter (mi) specimens shall be taken from each of the samples and shall be placed in separate 8 inch by 1 inch test tubes. Each separate test tube shall be visually inspected across the diameter of the tube and compared with a
29、similar tube of distilled water by the inspector to verify conformance with this specification as to clarity and color. 4.5.2 Concentration 4.5.2.1 Reagent - standard Mn4 solution. - Make up an approximately O.5N solution of KMn4 and age in the dark for at least one week. Filter the solution through
30、 pure asbestos (free from organic matter), or through a medium-porosity sintered glass crucible before standardizing against Bureau of Standards sodium oxalate. sample of sodium oxalate which has been dried for 1 hour at 10pto =Oo C. Dissolve the oxalate in 250 ml of l:3 sulfuric acid, previously bo
31、iled for 10 to 15 minutes and then cooled. Add from the calibrated burette 90 to 95 percent of the necessary KMn4, (25O C.), ana let stand until the pink color disappears. adding the permanganate dropwise, allowing each drop to become decolorized before the next is added. The end point shall be take
32、n at the point where the pink color persists for 30 seconds. Determine the reagent blank by titrating the same volume of boiled and cooled sulfuric acid with the permanganate. Subtract the volume required for the blank from the original titration. Weigh an approximately 1.5 gram Heat to 55O to 6OOc
33、and complete the titration by Calculation% Note: A 1.5. gram sample of sodium oxalate (if the Bureau of Standards oxalate sanrple has a purity of 99.95 percent) requi-res 44.75 ml of 0.5N i(Mno4. he to decomposition caused by contamination, ment for purposes of testing shall be properly prior to use
34、. 3 6 all glassware and equip- cleaned and passivated Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-H-22868 68 777770b OLL8125 L = - 1-2-22868 (Wep) 4.5.2.2 Concentration Determination - Accurately weigh by difference 6 to 8 drops (approximatel
35、y 0.4 gram) of hydrogen peroxide sample into a clean, glass stoppered I25-ml Erlenmeyer flask, being careful not to allow the H202 to wet the ground glass joint. acid. Titrate with the standardized WO4 solution until a pink color persists for 30 seconds. the temperature of the KMnO4 is different tha
36、n 25OC, blank by titrating 35mi of 1:l sulfuric acid to the same end point. the milliliters of WO4 used in the sample titration by subtracting the blank titration* results of a minimum of three titrations. The three results should fall within a range of 0.5 percent. Add 35 mi of 1:l sulfuric Utilize
37、 temperature correction factor if Determine the reagent Correct Determine the concentration of H202 by averaging the Calculation: Ml WO4 (corrected) x = normality KMnO4 x 1.701 Weight H202 sample Percent H202 4.5.3 Determination of Tin content. Reagents : 2N Sodium hydroxide 3546 Hydrochloric acid A
38、mmonium chloride gelatin solution - dilute I2 mi of a 1% gelatin solution to one liter with saturated aqueous ammonium chloride solution. Stock tin solution - dissolve pure tin in the minimum quantity of 3596 HC1 then make up to 200 mi with i HC1. 0500 g Standard tin solution: - Dilute 10 ml of stoc
39、k tin solution to 100 mi with distilled water. This solution contains 0.25 mg of Sn per ILL. Note; The stock tin solution will keep indefinitely, but the standard solution should be made up fresh on the day it is to be used. PROCEDURE: Measure 50 ml of hydrogen peroxide and pour into a 500 mi. tall
40、form beaker. Add an equal volume of distilled water and 5 mi of 2N NaOH. Cover with a watch glass and warm gently until the hydrogen peroxide begins to decompose vigorously. When decomposition has nearly ceased, bring to boiling and reduce the volume to approximately 10 ml, Provided by IHSNot for Re
41、saleNo reproduction or networking permitted without license from IHS-,-,-MIL-H-22868 68 9779706 OLL8226 3 m Run 7.5 ml of 35$ HC1 from a burette into a 50 mi volumetric flask and measure 30 ml of ammonium chloride gelatin solution in a graduated cylinder. When the decomposed hydrogen peroxide soluti
42、on has been reduced to a volume of about 10 mi, cool and pour into the HC1 in the 50 ml volumetric flask, washing the beaker into the flask with the ammonium chloride gelatin solution. Make up to volwne with distilled water . Transfer to a polarographic cell and bubble nitrogen for i5 minutes. Measu
43、re on the polarograph from to -0.9 volts versus a saturated calomel electrode. Plot a polarogram. -0.3 volts Make up standards containing 0,2,5,7, and 10 ml portions of the standard tin solution in distilled water and add the reagents as above. Polmograph these standards exactly as above. Note: Unid
44、entified impurities in hydrogen peroxide may result in an ambiguous polarogram. as follows: In such case the procedure should be modified Measure 50 ml of hydrogen peroxide and pour into a 500 ml tall form beaker. Add an equal volume of distilled water and 5 ml of 2N NaOH. Cover with a watch glass a
45、nd warm gently until the hydrogen peroxide begins to decompose vigorously. bring to boiling, evaporate to dryness and subject the residue for two hours to a temperature of 325 to 35OoC. water and 7.5 ml of 3546 HC1. of tin. the flask with 30 ml of ammonium chloride gelatin solution. volume with dist
46、illed water. proceed as described above. When decomposition has nearly ceased, Cool, add 5 to 10 ml of Allow sufficient time for the dissolution Make up to Transfer to a 50 ml volumetric flask, washing the beaker into Transfer to a polarographic cell and 4.5.4 Determination of phosphate content - Ev
47、aporate 10 ml of Cool, take-up the residue in 5 ml of hydrogen peroxide to dryness on the steam bath. to 325-35OoC for two hours. approximately W sulfuric acid, and digest on a steam bath for at least 30 minutes. rinsing with distilled water. solution (in IN sulfuric acid) and 2 ml of 0.2 percent p-
48、methyl amlnophenol sulfate solution containing 20 percent sodium bisulfite. with distilled water, and allow to stand at room temperature for one half hour. concentrations under identical conditions. Subject the dry residue Cool and transfer solution into a 50 ml volumetric flask, Add 5 ml of a 546 a
49、mmonium molybdate Make up to 50 ml Measure the optical density of the solution and determine Po4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-. . ., - . . - . h MIL-H-22868 (Wep) 4.5.5 Determination of nitrate content - Add 10 ml of distilled water and 1ml of a one percent sodium carbonate solution to 5 ml of hybogen peroxide. Wash down the inside of the con
