1、 MIL-S-322C 68 7777906 0233745 b m- MI LYS 73 2 2C 5 February i968 Superseding 20 September 1962 MIL-S-322B MILITARY SPECIFICATION SODIUM NITRATE This specification is mandatory for use by all Depart- ments and Agencies of the Department of Defense. 1. SCOPE 1.1 for use in the manufacture (see 6.1).
2、 Scope - This specification covers sodium nitrate of pyrotechnics, and other ordnance applications A 1.2 Classification - Sodium nitrate shall be of ehe follow- ing grades and classes as specified (see 6.2): Grade A (see Table I) Grade B (see Table I) Grade C (see Table I) Class 1 (see Table 11) Cla
3、ss 2 (see Table 11) Class 3 (see Table II 2. APP.LICABLE DOCUMENTS “ 2.1 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: J. SPECIFICATIONS Federal RR- S- 36 6 PPP-D- 705 Militar
4、y MIL-STD-105 Sieve, Test Drum: Metal Shipping, Steel (Over 12 and Under 55 Gallon). Sampling Procedures and Tables for Inspection by Attributes. TH18 DOCUMENT CONTAINS /ulfates(as Na2S04) !hlorides(as NaCl) ./ The percentages i Max. Min. Max. Min. Max. Min. 0.75 . 0.5 . 0.75 . 0.5 . 0.1 . 0.5 . b 0
5、.05 . None . 0.06 . . 97.0 . 99.5 . 97.0 I I I I I 0.06 . None . 0.06 . I 0.3 . 0.1 . 0.3 0.15 . 0.06 e 0.15 . 0.5 . 0.2 . 0.45 . . . 0.15 . 0.15 . I dicated, except the percent of moisture,are to be obtained in the-sodium nitrate after the sample has been dried to constant weight at 302t - 5OF(150
6、- t 3OC). ii 3.3 Granulation - The sodium nitrate shall conform to the granulation requirements of Table II, when determined in accordance with 4.4.11,unless otherwise specified in the contract or order. 3 Licensed by Information Handling ServicesMI L-.S - 3 2 2C TABLE II-Granulation requirements -1
7、 r Class I Class 2 Class 3 Sieve number i/ Percent through Percent through Percent retained on - Minimum Minimum Minimum 20 . . 80.0 60 98.0 . . 10 o . 98 .O o 200 . . . 325 . . . - - i/ Use U. S, Standard sieves conformxg to Specification RR-S-366, 3.4 Average particle diameter - (applicable to Cla
8、ss 2 only) In addition to conforming to the granulation reauirements SDecified in Table II, the average particle diameter of Class 2 sodium nitrate shall be 30i - 15 microns, when determined in accordance with 4.4.12. 3.5 Workmanship - The sodium nitrate shall be processed in a manner that will prod
9、uce the high quality product necessary to meet the requirements of this specification (see 4.4.1). 4. QUALITY ASSURANCE PROVISIONS * 4.1 Responsibility for inspection - Unless otherwise specified in the contract or purchase order, the supplier is responsible for the performance of all inspection req
10、uirements as specified herein. Except as otherwise specified, the supplier may utilize his own facilities or any commercial laboratory acceptable to the Government. ment reserves the right to perform any of the inspections set forth in the specification when such inspections are deemed necessary to
11、assure supplies and cervices conform to The Govern- prescribed requirements. $i 4.2 Classification of inspection - The examinaticm and testing of the sodium nitrate shali be entirely by quality conformance inspection. ,- - 4 Licensed by Information Handling ServicesMIL-S-322C fi 4.3 Quality conforma
12、nce inspection - The quality conformance inspection shall consist of an examination for acceptability of quality control methods used by the manufacturer, an examination of Billed containers for conformance to packaging, packing, and marking require- ments, and examinations and tests of samples (4.3
13、.3) for all the require- ments of this specification. defined in MIL-STD-109. The inspection terms used herein are fi 4.3.1 - Quality conformance samples - Quality conformance samples shall consist of a samDle for tests (4.3.3) and samDles for examination of filled containers (4.3.4). information id
14、entifying the purpose of the sample, name of product, specification number, lot and batch number, date of sampling, and contract number. Samples shall be labLled completely with 2? 4.3.2 a lot shall consist of sodium nitrate from one batch offered for delivery at one time, but not to exceed 24 conse
15、cutive hours under essentially the same manufacturing conditions and with no change in materials, providing the operation is continuous. A batch is that quantity of material which has been subjected to some unit chemical or physical mixing process intended to make the final product substantially uni
16、form. the process is a batch operation, each batch shall constitute a lot. Lot and batch - For the purpose of sampling and inspection, In the event sc 4.3.3 weight, 25 grams each, shall be randomly selected from each lot of Sample for tests - Ten (10) primary samples of equal material and thoroughly
17、 mixed to form a composite sample representative of the lot. The container shall belabeled to identify the sample with t.he lot represented. If there are less than 10 containers in a lot, a sample shall be taken from each container. subjected to the conformance inspection specified herein. A lot sha
18、ll be inacceptable if a sample fails to meet any of the test requirements specified. The composite sample shall be 4.3.4 . Sample for examination of filled containers - A random sample of filled oontainers shall be selected from each lot of sodium nitrate in accordance with MIL-STD-105 at inspection
19、 level I and accept- able quality level (AQL) = 2.5 percent defective. 4.4 Inspection methods - Unless otherwise specified, the physical and chemical values specified in Section 3 shall apply to the average of the determinations made on the unit of product. 4.4.1 Conformance of the sodium nitrate to
20、 the requirements for material (3.1) and workmanship (3.5 ) shall be -determined by appropriate examination and testing in accordance with Section 3. 4.4.1.1 Reagent water conforming to D1193 and reagent chemicals conforming to American Chemical Society (A.C.S.) specifications (see 2.2) shall be use
21、d throughout the tests. nearest 0.0001 gram (gm). shall be made up on a weight basis. Weighings shall be made to the Unless otherwise specified herein, solutions , 5 Licensed by Information Handling ServicesMIL-S-322C 4.4.2 Moisture - Transfer a weighed 10 gm portion of the sodium nitrate to a previ
22、ously tared shallow weighing bottle, heat in an air bath for 2 hours at 302 t 5OF. (150 + 3OC.), cover, cool in a desiccator and weigh. in the .sample. Calculate th; loss in weTght as the percentage of moisture 100 (A-B) Percent moisture = w Where : A Weight of bottle plus sample before drying in gr
23、ams. B = Weight of bottle plus sample after drying in grams. W = Weight of sample in grams. 4.4.3 Insoluble matter - Transfer a weighed 25 gm portion of sodium nitrate to a beaker. Heat to boiling with 200 ml of water and decant the solution through a filtering crucible of fine porosity (a nominal m
24、aximum pore diameter of 4.5 to 5.0 microns) which has been dried at 212 + 5OF. (100 t 3OC.I and weighed. Rinse the beaker with boiling distilled water and transfer any adhering insoluble matter to the filter. Decant the wash waters from the beaker through the filter. Catch the filtrate and wash wate
25、rs in a 500-mL volumetric flask and retain for the determination of alkalinity (see 4.4.4). filtering crucible shall be dried in an oven at 221 t.9OF. (105 t 5OC.) for 3 hours, cooled in a desiccator, and weighed. The increase Tn weight shall be calculated to percent insoluble matter as follows: The
26、 Percent insoluble matter = loo (A-B) W Where : A = Weight of crucible plus residue in grams. B = Weight of crucible in grams. W - Weight of sample in grams. Licensed by Information Handling ServicesMIL-Sl322C 4.4.4 Alkalinitv - Using freshly boiled distilled.wa-ter, make up the filtrate hTained as
27、specified in 4.4.3 to 500-ml andmix thoroughly. Pipet 100 ml of this solution into a flask, add 3 to 5 drops of phenolphthalein indicator and if the solution is alkaline, titrate with 0.1N acid. A blank determination shall be made on the distilled water and a correction applied if necessary. Calcula
28、te to percentage Na20 in the sample as follows: Percent Na20 = 3.1 VN Where : V = ml acid.used in the titration. N = Normality of acid used. W = Weight in grams of sample represented by the aliquot. 4.4.5 Nitrates 4.4.5.1 Standardization of the nitrometer 4.4.5.1.1 Absolute method - Assemble the nit
29、rometer (DuPont or equiv- alent) after thoroughly cleaning and drying all parts. with the exception of the reservoir bulbs, are completely filled with mercury. bulb. by lgwering the mercury reservoir and opening both stopcocks, both stopcocks and shake vigorously for 3 minutes. Connect the gener- at
30、ing bulb into the compensating tube by adjustment of the two mercury reservoirs, keeping open the stopcock of the measuring tube. Continue the introduction of the air until the mercury in the reading tube is nearly at the 12.50 mark. small blowpipe flame. another portion of air and transfer this to
31、the reading tube until the mercury in the reding tube, compensating tube, and their mercury reser- voirs are at the same level, the mercury in the reading tube being approx- imately at the 12.50 mark. be exact or equal. and attach to the reading tube. temperature and then adjust the mercury levels i
32、n the reading tube, comp- ensating tube, and their mercury.reservoirs so that the air in the reading tube is under atmospheric pressure, as shown by the acid levels in the arms of the manometer tube. Take the reading on the graduated scale of the calibrated reading tube, and at the same time note th
33、e temperature and barometric pressure. From these readings calculate the volume of air at 20OC. and 760 mm. pressure in the reading tube by means of the following formula: The various parts, Place 25 ml of 94.5 f 0.5 percent sulfuric acid in the generating Draw air into the bulb 70 nearly the level
34、of the lower shoulder Close Seal the compensating tube by means of a Desiccate simil-arly in the generating bulb It is not necessary that these gas volumes Fill a small U-tube manometer with sulfuric acid Allow the apparatus to come to constant / d E. I _I; 7 Licensed by Information Handling Service
35、sMIL-S-322C - O 38692 PR( 1, O. 00018t) V=R P x 293(1-0.00018t) - 760(273 I- T) (1-0.00018 x 20 ) 273 trT Where : V = ml air at 20OC. and 760 mm. , barometer at 20OC. R = ml air at the observed temperature (TOC.) and at the observed pressure (Pmm). t = Temperature (OC.) of the barometer, The factor
36、0.00018 represents the correction to be applied for the coefficient of expansion of mercury in the barometer. When P has been calculated, adjust the heights of the reading tube, compensating tube, and their reservoirs so that, with the mercury in the reading and comp- ensating tubes on a level, the
37、mercury in the reading tube marks the calculated volume of the air. Paste a strip of paper on the tube so as to mark the height of the mercury in the compensating tube. Take this as the standard volume of air with which every volume of gas to be measured is compared. Note. The use of dry air tends t
38、o form a scum around the reading level of the compensating tube, thus requiring frequent restandardization of the nitrometer. wi+h mercury op by impurities- Dry nitrogen eliminates this condition and should be used, if available. prevent this smm. 4.4.5.1.2 95 percent alcohol a sample of chemically
39、pure grade of potassium nitrate, and grind this to pass through a U. S. Standard No. 100 sieve. After drying at 275 to 302OF. (135 to 15OOC.1 for 2 or 3 hours, weigh a portion of exactly 1 gm into a small weighing bottle and transfer this portion to the cup of the generating bulb. generating bulb by
40、 means of 8 to 10 portions of 94.5 + 0.5 percent nitrogen-free sulfuric acid cooled to approximately 4F, (5OC. ) using a total volume of 25 ml of the acid. With the lower stopcock of the generating bulb open and the mercury reservoir low enough to maintain a slightly reduced pressure in the generati
41、ng bulb,shake the sample until most of the gas has been generated. Adjust the mercury reservoir until the mercury drops nearly to the lower shoulder of the generating bulb. Close the lower stopcock and shake the bulb vigorously for 3 minutes. Replace the bulb on the rack, open the lower stopcock,and
42、 allow the tube to stand for 5 minutes, the levels in the generating bulb and reservoir being approximately the same. i/ Close the lower stopcock, and shake the generating bulb for 1 additional minute. This scum is caused by reaction of oxygen in the air A half drop of sulfuric acid will also Potass
43、ium nitrate method - Recrystallize three times from Wash the potassium nitrate into the Transfer the gas to the reading Having previously introduced desiccated air into the compensating i/ tubeas described under the absolute method, Licensed by Information Handling ServicesMIL-S-322C tube, and adjus
44、t the levels of the mercury in the reading and comp- ensating tubes to approximately the same height. stand for about 20 minutes to permit equalization of the temperature. With a sulfuric acid U-tube leveling device, make careful adjustment, so that the mercury in both tubes are at the same level an
45、d that in the reading tube it is at the 13.85 mark (the percentage of nitrogen in poassium nitrate). volume occupied by the air equivalent to the volume of nitric oxide gas liberated from exactly 1 gm of potassium nitrate. This mark is usually made on a strip of gummed paper attached to the compensa
46、ting tube. Allow the gas to Make a mark in the compensating tube to show the Note 1: In order to avoid any doubt regarding the purity of the potassium nitrate, it is desirable to check the standardization obtained by the use of potassium nitrate by means of the absolute method. If the agreement is w
47、ithin one-or two-hundreths of 1 percent, the potassium nitrate can be considered as of satisfactory quality and used in subsequent periodic standardizations. experimentation that the solubility of nitric oxide in sulfuric acid of the strength prescribed is so small that no correction need be applied
48、 to bring the value in agreement with the mark set by the absolute method. It has been found by actual Note 2: If the nitrometer is standardized by both the absolute and potassium nitrate methods, the results may not be in agreement by 0.01 to 0.04 percent nitrogen due to expansion of the brass baro
49、meter scale. Such difference may be removed by.applying the brass scale correction corresponding to the temperature. 4.4.5.2 Procedure - Crush a portion of about 3 gm of the sodium nitrate so that it will pass through a U. S. Standard Na. 100 sieve and dry for 2 hours at 302 t 5OF. (150 t 3OC.). imately 0.85 gm of the dried sampleand transfer it to the cup of a standardized five-part nitrometer (DuPont or equivalent). a smallgraduate 25 ml of nitrogen-free 94.5 t 05 percent sulfuric acid cooled to approximately 41OF. (5OC. ) . bottle into the nitrometer cup with 5 ml of t
