1、INCH-POUNDA-A-59342September 30, 1998SUPERSEDINGMIL-E-463B14 May 1962COMMERCIAL ITEM DESCRIPTIONETHYL ALCOHOL (FOR ORDNANCE USE)The General Services Administration has authorized theuse of this commercial item description, for allfederal agencies.1. SCOPE. This commercial item description (CID) cove
2、rs the requirements forsix grades of ethyl alcohol intended for ordnance use.2. CLASSIFICATION. Ethyl alcohol shall be of the following grades asspecified (see 7.4).Grade 1 - 95.0 percent by volume without denaturant.Grade 2 - 94.9 percent by volume with denaturant.Grade 3 - 99.0 percent by volume (
3、anhydrous), with toluene denaturantGrade 4 - 95.0 percent by volume, denatured with tertiary-butyl alcoholand benzyldiethyl(2.6 xylycarbamoyl) ammonium benzoate.Grade 5 - 95.0 percent by volume.Grade 6 - 88.3 percent by volume.3. SALIENT CHARACTERISTICS.3.1 Material . Ethyl alcohol, prior to the add
4、ition of dye or denaturant, shallbe a clear, transparent, colorless liquid having a characteristic odor, andshall not contain visible insoluble material. The quantity and grade shall beas specified in the contract or order (see 7.2 and 7.4).3.1.1 Grade 1 ethyl alcohol shall contain neither dye nor d
5、enaturant andconform to Table I when tested as specified therein.3.1.2 Grade 2 ethyl alcohol shall be produced by the addition of toluene toGrade 1, ethyl alcohol and shall conform to Table I when tested as specifiedtherein.AMSC N/A FSC 6810DISTRIBUTION STATEMENT A . Approved for public release; dis
6、tribution isunlimited.Beneficial comments (recommendations, additions, deletions) and any pertinentdata which may be of use in improving this document should be addressed to:Commander, US Army TACOM-ARDEC, Attn.: AMSTA-AR-QAW-E, Bldg 12, PicatinnyArsenal, NJ 07806-5000 by using the Standardization D
7、ocument ImprovementProposal (DD Form 1426) appearing at the end of this document or by letter.Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-A-A-5934223.1.3 Grade 3 ethyl alcohol shall be produced by the addition of toluene toan anhydrous grade of a
8、lcohol that complies with the requirements of Grade 1ethyl alcohol when tested as specified therein.3.1.4 Grade 4 ethyl alcohol shall be produced by the addition of 1/8 gallonof tert-butyl alcohol and 1/4 avoirdupois ounce of benzyldiethyl (2.6xylylcarbamoyl) ammonium benzoate to 100 gallons of Grad
9、e 1 ethyl alcohol, andshall be dyed with one part by weight of fuchsin dye to 500,000 parts, byweight, of ethyl alcohol. Grade 4 ethyl alcohol shall conform to Table I whentested as specified therein.3.1.5 Grade 5 shall be produced by mixing 100 gallons of anhydrous ethylalcohol with 5 gallons of an
10、hydrous methyl alcohol and shall conform to TableI when tested as specified in the contract or order (see 7.2).3.1.6 Grade 6 shall be produced by mixing 100 gallons of either anhydrousSD3A Alcohol or Grade 5 alcohol with 5 gallons of ethyl acetate and 1 gallonof methyl isobutyl ketone and shall conf
11、orm to Table I when tested asspecified in the contract or order (see 7.2).TABLE I. Chemical and physical propertiesProperties Grades1 2 3 4 5 6TestMethodEthyl alcohol by volume,minimum (min.) percent 95.0 94.9 99.0 94.9 95.0 88.3see 5.3.1Toluene by volume,maximum (max.) percent 0.01 0.75 0.75 - - -s
12、ee 5.3.2Acidity, grams(gm.) per100 milliliters (mL) (asacetic acid, max.)0.005 0.01 - - 0.01 0.01see 5.3.3Aldehydes, max. milligram(mg.) per 100 mL 20.0 - - - - -see 5.3.4Non-volatile matter, max.percent0.004 0.006 - - - - see 5.3.5Organic impurities, max.,percent0.1 - - - - - see 5.3.6Water, percen
13、t by weight,max.- - - - 0.3 0.3 see 5.3.7Methyl alcohol, percentby volume, max. - - - - 5.0 4.5see 3.1.5,5.3.8, and7.2Ethyl acetate, percent byvolume, max - - - - - 5.4see 3.1.6,5.3.9,and7.2Methyl isobutyl ketone,percent by volume, max. - - - - - 1.5see 3.1.6,5.3.10 and7.2Specific Gravity, max. .815
14、8 .8162 .7987 .8162 .8158 .8387 see 5.3.1Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-A-A-5934233.2 Chemical and Physical Properties . The chemical contents and physicalproperties of each grade shall comply with the requirements shown in Table Iwh
15、en tested as specified herein.3.3 Taste . (Grade 4 only). Grade 4 ethyl alcohol shall be distinctly bitter.4. REGULATORY REQUIREMENTS. The offeror/contractor is encouraged to userecovered materials to the maximum extent practicable, in accordance withparagraph 23.403 of the Federal Acquisition Regul
16、ation (FAR).5. QUALITY ASSURANCE PROVISIONS.5.1 Product Conformance . The products provided shall meet the salientcharacteristics of this commercial item description, conform to the producersown drawings, specifications, standards, and quality assurance practices, andbe the same product offered for
17、sale in the commercial market. The governmentreserves the right to require proof of such conformance.5.2 Testing .5.2.1 Sampling .5.2.1.1 Containers . From each inspection lot, two containers shall be selectedat random. A composite sample shall be prepared by taking a 16 ounce specimenfrom each of t
18、he selected containers. Transfer the specimen to a 32 ounce airtight glass bottle having a glass topper or a cap containing a cork orcardboard liner covered with metal foil, and labeled to show the name of thematerial, grade, manufacturer, plant contract or purchase number and lot size.If the sample
19、s fail to comply with any of the requirements, the lot shall berejected.5.2.1.2 Tank cars . By means of a clean, weighted, small-neck, glass bottleapproximately 1 quart of the material shall be removed from the tank car. Theunstoppered bottle shall be rinsed with the material being sampled, andlower
20、ed to the bottom of the tank by means of a cord, chain, or rod. Thebottle shall be immediately withdrawn to the surface. In order to obtain arepresentative cross-section of the material, the speed of lowering andraising the bottle shall be uniform, and so regulated that the bottle, is justfilled as
21、it reaches the surface of the liquid. This sample shall be placed inan airtight glass bottle, having a glass stopper or a cap containing a cork orcardboard liner covered with metal foil, and labeled to show the name of thematerial, manufacturer, plant, contract or order number, lot number, and a lot
22、size. If the sample fails to comply with any of the requirements, the lotshall be rejected.5.3 Test methods and procedures .5.3.1 Ethyl alcohol content . The specific gravity shall be determined at15.6 O C/15.6 O C (60 O F/60 O F) by means of a calibrated hydrometer, pycnometer orother standard meth
23、od. The percentage of alcohol by volume shall be obtainedby reference to Table II.5.3.2 Toluene . The test for toluene in Grade 1 ethyl alcohol shall be made inaccordance with the colormetric method described in 5.3.2.1 and the tests fortoluene in Grades 2 and 3 ethyl alcohol shall be made in accord
24、ance with thespectrophotometric method described in 5.3.2.2 or 5.3.2.3.5.3.2.1 Colormetric method . A 10 mL portion of nitrating mixture, made bymixing equal parts, by volume, of sulfuric acid (specific gravity 1.84) andfuming nitric acid, free of brown oxides of nitrogen, shall be placed in a 50Pro
25、vided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-A-A-593424mL beaker. Precautions shall be taken to prevent rise of temperature above25 O C (and subsequent evolution of brown fumes) by use of a buret to permitslow dropwise addition of the sample, and a m
26、echanical stirrer to effect rapidand thorough mixing. Then, 0.5 mL of the sample shall be added. With vigorousstirring, the resultant mixture shall be slowly poured into 40 mL of water.The mixture shall be transferred, at a temperature of not more than 25 O C to a125 mL separatory funnel, and extrac
27、ted once with 20 mL of ethyl ether byshaking for approximately 1 minute. The lower layer shall be discarded. A 20mL portion of water shall be added, and shaken vigorously for approximately 1minute. The wash water (lower layer) shall be discarded. A 20 mL solution,made by diluting 5 mL of saturated s
28、odium, bicarbonate solution with 15 mL ofwater, shall be added. The alkaline wash solution, which should have a yellowto brownish-yellow color, shall be slowly removed and tested for alkalinitywith a universal indicator test paper. If the solution is acid, the otherportion shall again be treated wit
29、h dilute sodium bicarbonate solution. Thewash solution shall be discarded. The ether layer shall be transferred throughthe mouth of a separatory funnel to a dry 50 mL beaker and almost, but notcompletely, evaporated to dryness on a steam bath. The contents shall bewashed into a dry test tube (approx
30、imately 16 by 150 millimeter (mm) with 10mL of toluene free 95 percent ethyl alcohol. Then 1 mL of butanone(methylethyl-ketone) shall be added, and the solution shaken. A 0.5 mL portionof alcoholic NaOH solution, made by dilution of 1 volume of aqueous NaOHsolution (40g NaOH per 100 mL of aqueous so
31、lution) to 10 volumes with toluene-free 95 percent ethyl alcohol shall be added. The solution shall be thoroughlymixed, and allowed to stand for 5 minutes. A blank shall be run simultaneouslywith the sample, using toluene-free 95 percent ethyl alcohol. In the absenceof toluene, the solution has a ye
32、llow to yellow-orange color. The presence oftoluene is indicated by a reddish color, having a greater intensity than thatobtained when a synthetic mixture of 0.01 percent toluene has been tested intoluene-free alcohol.5.3.2.2 Spectrophotometric method . This method is based on the fact thattoluene h
33、as a characteristic absorption curve in the ultra-violet region.5.3.2.2.1 Apparatus . Absorbance measurements shall be made using aspectrophotometer with ultra-violet accessories, matched 1 centimeter silicacells and a blue sensitive phototube in position. (A Beckman Model DUspectrophotometer (see 7
34、.8) has been found to be satisfactory.)5.3.2.2.2 Standard curve . Standard solutions of toluene in ethyl alcoholshall be prepared by pipetting 0.2, 0.5 and 0.8 mL of reagent grade toluenerespectively into labelled 100 mL volumetric flasks. The toluene in the flasksshall be diluted to the mark with t
35、oluene free reagent grade ethyl alcohol (95percent or absolute). Ten mL of each standard shall be pipetted to suitablylabelled 100 mL volumetric flasks, diluted to volume with reagent grademethanol and mixed thoroughly. The absorbance readings of these solutionsshall be taken at a wave-length of 261
36、 millimicrons using a methanol blank.The absorbance readings shall be plotted against the concentration. Thisshould be a straight line passing through the origin. All pertinent data shallbe recorded. The graph for a particular instrument may be retained and usedfor future routine work by checking tw
37、o points on the curve.5.3.2.2.3 Procedure . A 10 mL portion of the sample shall be transferred,quantitatively, to a 100 mL volumetric flask and diluted to a volume withreagent grade methanol. The solution shall be mixed thoroughly and one of thesilica cells of the apparatus shall be filled with the
38、sample solution and theother cell filled with methanol. The cells shall be inserted in the cellholder and the optical density at 261 millimicrons shall be recorded, afterproper adjustment of the instrument. (Use of a slit width chosen for the bestProvided by IHSNot for ResaleNo reproduction or netwo
39、rking permitted without license from IHS-,-,-A-A-593425sensitivity). The quantity of toluene present shall be read from the standardgraph (5.3.2.2.2).5.3.2.3 Alternate method . A 0.10 mL portion of the sample shall betransferred, by means of a pipette, to a dry test tube. Then 5 mL ofconcentrated su
40、lfuric acid, containing 0.5 percent of formaldehyde solution(not less than 37 percent formaldehyde), shall be added by means of a pipette.The test tube and contents shall be agitated. The color developed shall be nodarker than that of a 0.75 percent solution of toluene in 95 percent alcohol,by volum
41、e, when treated in the same manner as the sample. In case of question,doubt, or dispute, the spectrophotometric method specified in 5.3.2.2 shall bemandatory.5.3.3 Acidity . Mix 100 mL of sample with 100 mL of carbon-dioxide freedistilled water. Add two drops of bromothymol blue indicator prepared b
42、ydissolving 0.1 g bromothymol blue in 100 mL 50 % ethyl alcohol and titratewith 0.01 Normal Sodium Hydroxide to a blue endpoint. Calculate acidity asacetic acid as follows:Acetic acid (g per 100 mL) = 0.06 VNwhere:V = mL of alkali usedN = Normality alkali5.3.4 Aldehydes . 120 mL of sample shall be t
43、ransferred to a 250 mL flask, addapproximately 20 mL. of distilled water and a few granules of carborundum.Distill slowly into a 100 mL volumetric flask, to the mark, and mix.5.3.4.1 Procedure . The 100 mL of freshly distilled ethyl alcohol shall beplaced in a 500 mL flask and approximately 100 mL o
44、f distilled water andexcess of .05 normal sodium bisulfite shall be added and allowed to standapproximately 30 minutes shaking occasionally (excess sodium bisulfite shouldbe equivalent of approximately 25 mL of .05 normal iodine). Excess iodine .05normal solution shall be added and this excess titra
45、ted with .05 normal sodiumthiosulfate. A blank shall be run using the same quantities of .05 normaliodine and sodium bisulfite as used in the sample.Aldehydes in mg. per 100 mL = A x 1.1where:A = difference in mL between the two titration of sodiumthiosulfate used.5.3.5 Non-volatile matter . Evapora
46、te 100 mL of the sample on a steam bath ina tared platinum or other suitable dish. Dry the dish and residue to constantweight in an oven at 105 O C to 110 O C. The increase in weight of dish shall becalculated as percentage non-volatile residue. Calculate the increase asfollows:Non-volatile matter i
47、n g per100 mL = B - Awhere:A = tare weight of dishB = weight of dish plus residue5.3.6 Organic impurities . A 0.1 mL portion of reagent grade, isoamyl alcohol(isobutyl-carbinol) shall be transferred to a volumetric flask, and made up to100 mL with reagent grade absolute ethyl alcohol (standard solut
48、ion). Both ofthe following tests, on this standard solution, and on the sample, shall beProvided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-A-A-593426conducted using test tubes of uniform size. These tests are especiallyintended for the detection of an e
49、xcessive percentage of fuse oil.5.3.6.1 Sulfuric acid method . To 10 mL of the sample, in a large test tube,10 mL of sulfuric acid (specific gravity 1.84) shall be cautiously added downthe side of the test tube. During this addition, the test tube shall be gentlyswirled to obtain thorough mixing of the acid with sample. The temperature ofthe mixture will rise to approximately 90 O C. This proc
