NAVY MIL-T-81533 A-1967 TRICHLOROETHANE 1 1 1 (METHYL CHLOROFORM) INHIBITED VAPOR DEGREASING《蒸气脱脂1 1 1三氯乙烷(甲基氯仿)的抑制》.pdf

1、_- MIL-T-BL533A h each sample filled container shall also be weighed to determine the amount of contents. Any container in the sample, having one or more defects, or under required fill, shall be rejected and if the nwnber of defective containers in any sample exceeds the acceptance number for the a

2、pplicable sampling plan of Military Standard MIL-STD-105, the lot represented by the sample shall be rejected. 4.3.2 Lot acceDtance tests - The samples selected in accordance with 4.2.3 shall be subjected separately to the tests specified in 4,4. I. either sample fails one or more o2 these tests, th

3、e lot shall be rejected 4,40 Test procedures - 4,4.1 Nonvolatile residue - This determination shall be made in accordance with ASTM Method A, D-2109-64. A stream of warm (40 - 5OoC) dry, oil-free nitrogen or compressed air may be used to accelerate evapora- tion. The results shall be reported on a w

4、eight basis. - - “ ,“. %: Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-81533A 4.4.2 Specific gravity - The specific gravity shall be determined in accordance with ASTM D-2111-64. 4,403 APHA color - Test in accordance with ASTM Method D-2108-

5、64, 4.4.4 Awearance - A portion of the well shaken sample shall be placed in a test tube and allowed to stand stoppered and undisturbed until bubbles have entirely disappeared. Examination shall be made by trmsmitted light for uniformity and freedom from particles, 4.4.5 1.1.1 Trichloroethane conten

6、t - The content of 1,1,1 trichloroethane, inhibited, shall be assayed in accordance with the following gas chromatographic procedure or one of equal or better sensi- tivity and accuracy, - 4.4,5,1 Apparatus - A gas chromatograph having the following minimum capabilities is recommended: Temperature c

7、ontrol system capable of maintaining the chromatographic column at prescribed temperature &0,5OC. Heated sample inlet. A differential katharometer (hot wire), thermistortype thermal conductivity detector or hydrogen flame detector. 4.4.5,2 Materials - The following materials are recommended: Chromat

8、opraphic column - Annealed copper or stainless steel tubing, 12 feet long?by 1/8-inch outside diameter (0.055-inch inside diameter). Column packing - Acid washed calcined-pink firebrick (Chromosorb P), 30 to 50U.S. Standard mesh, coated with 15 percent by weight of UNCON LB 1800X liquid phase. The c

9、ompleted column should be conditioned prior to initial use at 125OC, with helium gas flowing through it for 24 hours at a rate of 15 ml per minute. - 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- . MIL-T-81533A Carrier gas - Dry helium of 99.95

10、mole percent purity. Standard - Uninhibited 1,1,1 trichloroethane of .at least 98.0% purity. 4.405.3 Analysis conditions - The following analysis conditions are recommended: Column temperature - 6OoC isothermal. Detector temperature - 225OC, Sample inlet temperature - 200C. Sample size - 5 microlite

11、rs (to be injected by means of a precision 10 ul syringe via a heated inlst), Carrier gas flow - 15 ml per minute. Detector sensitivity - Sufficient to easily meet the 0.5 percent detection requirement set forth in 3.2. Bfiploying the operating conditions recommended, all constituents of methyl chlo

12、roform solvents should elute from the column in approximately 30 minutes. 4.4.5.4 Determination of 1.1.1 Trichloroethane content - Quanti- tative measurement of concentration of a constituent in a sample depends upon a determination of the peak area or peak height of the constituents chromatographic

13、 peak or area. Peak areas may be measured by any accepted method (planimeter, ball and disc integrator, electronic digital integrator, etc.) or may be approximated by multiplying the height of the peak by the width of the peak at the half-height. To obtain the percent concentra.tion of the 1,1,1 tri

14、chloroethane ina sample, a direct comparison is made of its peak area with the peak area of 1,1,1 trichloroethane in the standard, Both sample and standard must be analyzed under identical operating conditions. 4.4.6 Water content - The water content shall be determined in accordance with ASTM Metho

15、d D-1364-64, 4.4.7 Acidity (as HC1) 4.4.7.1 The acidity of the “as received“ material shall be determined by standard titration with ,O2 normal sodium hydroxide in - anhydrous methanol using bromothymol-blue as an indicator, - 6 LIj ?,-:* Provided by IHSNot for ResaleNo reproduction or networking pe

16、rmitted without license from IHS-,-,-NIL-T-BL533A h8 m 7777706 0322832 2 MIL-T-81533A 4.4.7.2 Acidity after accelerated oxidation - The general arrange- ment of the apparatus used is shown in figure 1. Two-hundred ml of the sample shall be placed in the boiling flask. One strip of steel 1/2 inch by

17、2 inches by 1/16 inch shall be suspending by means of an uncoated copper wire so it remains above the liquid level, and another strip 1/4 inch by 3/4 inch by 1/16 inch shall be placed in the bottom of the flask, The strips shall conform to S.A.E. steels within the range of 1010 to 1040 inclusive. Th

18、e oxygen delivery tube shall extend to within 1/4 inch of the bottom of the flask. The water shall be started through the condenser. The oxygen-flow shall be regulated to 18-12 bubbles per minute by adjusting the height of the water level above oxygen outlet in the pressure control cylinder. The hea

19、ting of the solution shall be started and the solvent refluxed for 48 hours. The solvent shall be cooled to ambient temperature, 25 ml shall be withdrawn and the acidity determined by the method described in 4.4.7.1, 4.4.8 - Free halogen - Transfer 10 ml of sample to a clean test tube. Add 10 ml of

20、distilled water, 5 drops of 10 percent potassium iodine solution (ACS Reagent) and one ml of starch solution (ACS Reagent). Shake for one minute. A blue color in the aqueous layer indicates the presence of free halogen. 4.4.9 Etals corrosion - Prepare 1/2 inch by 5 inch panels of each of the followi

21、ng metals: . Aluminum alloy (QQ-A-250/4C temper T-41, Steel (MIL-S-7952) Magnesium (QQ-“44) and Titanium (MIL-T-90461, Polish panels with No, 1 emery cloth until the entire panel is bright, shiny and free from any oxide film or tarnish, Do not handle the panels with bare hands after polishing. Wash

22、with soap or detergent and water and rinse with distilled water. Was with acetone and allow to air-dry. Place each panel in separate 500 ml Erlenmeyer flask which has a ground glass neck, add sufficient 1,1,1 trichloroethane to form a layer of solvent one inch deep. Attach a reflux condenser and hea

23、t over a light shielded 150 watt light bulb and reflux for 24 hours. Allow to cool to ambient tempera- ture, rinse with sample but do not wipe, and examine for corrosion 4.4.10 Distillation range - Test in accordance with ASTM Method D-1078-63, 4.4.11 Acid acceptance (as percent NaOH by weight) - 4.

24、4.11,l Reagents - Sodium hydroxide - 0,Ol Normal, standardized. - - ,. ,Y ._ . . I ,- “ . “_ .- I. I . .“ . . - Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-f 1 = Figure“i. Accelerated Oxidation Test Apparatus 1 P Provided by IHSNot for ResaleNo r

25、eproduction or networking permitted without license from IHS-,-,-MIL-T-81533A b8 a 99797Ob 0122834 b W MIL-T-81533A Hydrochlorination reagent (hydrochloric acid) - Dissolve 1.5 ml of concentrated hydrochloric acid (HC1, sp gr 1.19) in 400 ml of absolute methanol in a 500 ml glass stoppered bottle an

26、d mix thoroughly. Indicator solution - Dissolve one gram of phenolphthalein in 50 mJ. of ethanol and dilute to 100 ml with distilled water o 4.4.11.2 Procedure - Pipet 25 ml of the hydrochlorination reagent into a 250 ml ground glass stoppered Erlenmeyer flask. Add 15 ml of the solvent under test, s

27、topper and swirl the flask to mix. Let stand for a minimum of 5 minutes to allow completion of the reaction, While the reaction is taking place, pipet 25 ml of the hydrochlorination reagent to another flask, add 25 ml of distilled water and one ml of indicator solution. Titrate with 0.01N NaOH solut

28、ion to a faint pink that remains for 15 seconds. Record the ml of NaOH used as the Blank (A). At the end of the reaction period, remove the stopper from the flask containing the sample and add 25 ml of distilled water and one ml of indicator solution. Titrate with 0.01N NaOH to same end point as spe

29、cified for the blank. Record the ml of NaOH used, (B) o 4.4.11.3 Calculation - The total acid acceptance as equivalent sodium hydroxide by weight shall be calculated as follows: Equivalent NaOH percent by weight f (A - B) N x 0.040 x 100 Where W A = ml of NaOH required for titration of blank. B = ml

30、 of NaOH required for titration of sample, N = Normality of NaOH solution. W = Grams of sample used (volume in ml times its specific gravity) 4,4.12 Residue soluble in carbon tetrachloride (CC14). Three 200-ml aliquots of the sample shall be placed in separate 200-ml tall-form. glass beakers. The so

31、lvent shall be evaporated to dryness on a steam bath, The evaporation process may be aided by passing a stream of air or nitrogen across the top of .the 200-ml beaker, Dryness is indicated by the absence of the odor of the trichloroethane in the beakers. The residue in each beaker shall be taken up

32、with 1 ml of spectrographic grade CCl4, Using a 0.5 millimeter (mm) sodium chloride (NaCl) cell, the maximum 9 1 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-tlIL-T-BL533TbB W 7777906 0122835 B W MIL-T-81533A infra-red absorbance of each residue s

33、ample shall be determined between the wavelengths of 3.35 and 3,6 microns, in conjunction with a reference standard of 0.5 mm spectrographic grade CCl4. A solution of 2.13 ml iso- octane, (2, 2, 4 trimethyl pentane) 99 percent minimum purity, made up to 1,000 ml with spectrographic grade CC14 shall

34、be prepared. The maximum infra-red absorbance of the iso-octane solution between the wavelengths of 3,35 and 3.6 microns shall be determined using a 0,5 mm NaCl cell, in conjunction with a reference standard of 0.5 mm spectrographic grade Ccjl . The average maximum infra-red absorbance of the three

35、solvent rssidue samples shall be not more than that produced by the iso-octane comparison solution. (CAUTION: Utmost care must be taken to insure that all glassware used to handle the solvent and reagents is clean. The use of sulfuric acid-potassium dichromate glass cleaner, distilled water rinse, a

36、nd drying with spectrographic grade acetone is recommended for this glassware. All infra-red salt cells must be thoroughly flushed with spectrographic grade carbon tetrachloride and dried with oil-free dry nitrogen prior to use.) 5, PREPARATION FOR DELIVERY 5.1 Packaging - 5.1,1 Level A - Unless oth

37、erwise specified, the 1,1,1 trichlo- roethane shall be furnished in 5-gallon containers conforming to Class I of PPP-P-704, or in 55-gallon drums conforming to PPP-D-729, The type and size of containers shall be specified by the procuring activity, 5,1.2 Level C - Unless otherwise specified, packagi

38、ng shall be in accordance with the manufacturers commercial practice, 5,1.3 Bulk - When specified, the material shall be shipped in sealed tank trucks or tank cars. 5.2 Packing - T“2.i Levels A and B - l,l,l trichloroethane packaged in accord- ance with 5,l.l will require no overpacking, 5,2.2 - Lev

39、el C - 1,1,1 trichloroethane packaged in accordance with 5.1,2 shall be packed to afford protection against damage during direct shipment from the supply source to the first receiving activity for immediate use. Containers shall comply with Consolidated Freight Classification Rules or other common c

40、arrier regulations applicable to the mode of,transportation. - .“ Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-T-81533A 5.3 Marking - Containers shall be marked in accordance with MIL-STD-129. The shipment marking nomenclature shall be: 1,1,1

41、T:cichloroethane , Inhibited, Vapor Degreasing. 5,3.1 Additional marking - Each container shall be marked with the following use instructions : CAUTION: VAPOR MAY BE HARMFUL Use with adequate ventilation Avoid prolonged or repeated breathing of vapor Avoid prolonged or repeated contact with skin Do

42、not take internally NOTE: Keep away from flames and other ignition sources when used where vapors may become concentrated. 6. NOTES 6,l Intended use - The 1,1,1 trichloroethane covered by this specification is intended for vapor degreasing use where air pollu- tion regulations preclude the use of ot

43、her materials. ,- 6.2 Ordering data - Procurement documents should specify the following : a. Title, number and date of this specification, b, Quantity of 1,1,1 trichloroethane desired, c. Type and size of containers (see 5.1). do. Selection of applicable levels of preservation, packaging and packin

44、g (see section 5) o 6.3 Batch - A batch is defined as that quantity of material which has been manufactured by some unit chemical process and subjected to some physical mixing operation intended to make the final product substantially uniform. Custodians : Army - MU Navy - AS AF - 68 Preparing Activity: Navy - AS (Proj, No, 6810-0783) , W.S. GOVERNMENT PRINTING OFFICE: 1967-301-512/1763 _c_z_ Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-