ASTM D612-1988(2004) Standard Test Method for Carbonizable Substances in Paraffin Wax《石蜡中可碳化物质的标准试验方法》.pdf

1、Designation: D 612 88 (Reapproved 2004)An American National StandardStandard Test Method forCarbonizable Substances in Paraffin Wax1This standard is issued under the fixed designation D 612; the number immediately following the designation indicates the year oforiginal adoption or, in the case of re

2、vision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test method

3、 covers determination of carbonizablesubstances in paraffin wax. The test method is applicable toparaffin wax for pharmaceutical use, as defined by the U.S.National Formulary, with a melting point as determined inaccordance with Test Method D 87, between 117 and 149F(47 and 65C).1.2 The values state

4、d in inch-pound units are to be regardedas the standard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bilit

5、y of regulatory limitations prior to use. Specific warningstatements are given in Annex A1.2. Referenced Documents2.1 ASTM Standards:2D 87 Test Method for Melting Point of Petroleum Wax(Cooling Curve)D 1193 Specification for Reagent Water3. Summary of Test Method3.1 Five millilitres of melted wax ar

6、e treated with 5 mL ofconcentrated, nitrogen-free sulfuric acid at 158F (70C). Thecolor of the acid layer is compared with that of a colorimetricreference standard. If the color is not darker than the standard,the wax is reported as passing the test.4. Significance and Use4.1 This test method is a m

7、eans for ascertaining whetherpharmaceutical paraffin wax conforms to the standards forquality prescribed by the U.S. National Formulary.5. Apparatus5.1 Test Tube, as shown in Fig. 1, of heat-resistant glass3fitted with a well-ground glass stopper, the stopper and the tubebearing identical and indest

8、ructible numbers. The tube shall be140 6 2 mm in length and between 14.5 and 15.0 mm inoutside diameter, and shall be calibrated at the 5 6 0.2-mL and10 6 0.2-mL liquid levels. The capacity of the tube withstopper inserted shall be between 13.6 and 15.6 mL. A rollededge may be provided for suspendin

9、g the tube on the cover ofthe water bath.5.2 Water Bath, suitable for immersing the test tube abovethe 10-mL line and equipped to maintain a temperature of 1586 1.0F (70 6 0.5C). The bath shall be provided with a coverof any suitable material, with holes approximately 16 mm indiameter through which

10、the test tubes may be suspended.5.3 Color Comparator, of a suitable type for observing thecolor of the acid layer in comparison with the referencestandard color solution. The size and shape of the comparatorare optional, but the size and shape of the apertures shallconform to the dimensions prescrib

11、ed in Fig. 1.6. Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are ava

12、ilable.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean distilled water, such as

13、reagent water corresponding to Specification D 1193, Type III,or water of equal purity.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.10 on Properties of Petroleum Wax.Current edition approved

14、May 1, 2004. Published June 2004. Originallyapproved in 1941. Last previous edition approved in 1999 as D 61288 (1999).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer

15、to the standards Document Summary page onthe ASTM website.3Borosilicate glass has been found satisfactory for this purpose.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chem

16、ical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428

17、-2959, United States.6.3 Cobaltous Chloride Solution (0.5 N)Dissolve about65 g of cobaltous chloride (CoCl26H2O) in enough dilutedhydrochloric acid (HCl, 1 + 39) (WarningHydrochloric acid(concentrated) causes burns, vapor extremely irritating. SeeA1.2) to make 1000 mL of solution. Transfer exactly 5

18、 mL ofthis solution to a flask; add 15 mL of sodium hydroxide(NaOH, 1 + 5) (WarningSodium hydroxide, corrosive, cancause severe burns or blindness. Evolution of heat produces aviolent reaction or eruption upon too rapid a mixture withwater. See A1.4), and 5 mL of hydrogen peroxide. Boil for 10min, c

19、ool, and add2gofpotassium iodide (KI) and 20 mL ofsulfuric acid (H2SO4, 1+4) (WarningSulfuric acid (con-centrated) causes burns, vapor irritating, strong oxidizer. SeeA1.3). When the precipitate has dissolved, titrate the liberatediodine with 0.1 N sodium thiosulfate (Na2S2O3) solution usingstarch s

20、olution as an indicator. Each millilitre of 0.1 N Na2S2O3solution consumed is equivalent to 0.023799 g of CoCl26H2O.Adjust the final volume of CoCl2solution by the addition ofdiluted HCl (1 + 39) so that 1 mL contains 59.5 mg ofCoCl26H2O.6.4 Colorimetric Reference Standard SolutionPrepare areference

21、 standard pale amber solution for color comparison bymixing together 1.5 parts of CoCl2solution, 3.0 parts of FeCl3solution, and 0.5 parts of CuSO4solution. Measure 5 mL ofthis mixture into a test tube as specified in 3.1. This pale amberreference standard shall then be overlaid with 5 mL of whitemi

22、neral oil.6.5 Cupric Sulfate Solution (0.5 N)Dissolve about 65 gof cupric sulfate (CuSO45H2O) in enough diluted HCl(1 + 39) (WarningHydrochloric acid (concentrated) causesburns, vapor extremely irritating. See A1.2) to make 1000 mLof solution. Transfer exactly 10 mL of this solution to a flask,add 5

23、0 mL of water, 4 mL of acetic acid (WarningAceticacid (glacial) is corrosive, combustible, vapor irritating. SeeA1.5), and3gofKI.Allow the mixture to stand for 5 min, thentitrate the liberated iodine with 0.1 N Na2S2O3solution, usingstarch solution as an indicator. Each millilitre of 0.1 N Na2S2O3so

24、lution is equivalent to 0.02497 g of CuSO45H2O. Adjust thefinal volume of CuSO4solution by the addition of diluted HCl(1 + 39) so that 1 mL contains 62.4 mg of CuSO45H2O.6.6 Ferric Chloride Solution (0.5N)Dissolve about 55 gof ferric chloride (FeCl36H2O) in enough diluted HCl(WarningHydrochloric aci

25、d (concentrated) causes burns,vapor extremely irritating. See A1.2) (1 + 39) to make 1000mL of solution. Transfer exactly 10 mL of the solution to aflask, add 5 mL of HCl (sp gr 1.19), 25 mL of water, and about3 g of KI. Stopper and allow the mixture to stand for 5 min.Dilute the mixture with 50 mL

26、of water, and titrate the liberatediodine with 0.1 N Na2S2O3solution, using starch solution as anindicator. Each millilitre of 0.1 N Na2S2O3solution is equiva-lent to 0.02703 g of FeCl36H2O. Adjust the final volume of theFeCl3solution by the addition of diluted HCl (1 + 39) so that1 mL contains 45.0

27、 mg of FeCl36H2O.6.7 Sulfuric Acid (94.7 6 0.2 %)The sulfuric acid(H2SO4)(WarningSulfuric acid (concentrated) causesburns, vapor irritating, strong oxidizer. See A1.3) shall benitrogen-free when analyzed in accordance with the followingprocedure: Dilute a small amount of the acid with an equalvolume

28、 of water and superimpose 10 mL of the cooled liquidupon diphenylamine solution (1 g of diphenylamine in 100 mLof concentrated H2SO4). A blue color should not appear at thezone of contact within 1 h. This test detects as little as0.0002 % NO3.7. Procedure7.1 Clean a test tube with cleaning solution5

29、(WarningNochromix5is corrosive. See A1.1), rinse with tap waterfollowed by distilled water, and dry in an oven at 105 C for 1h.7.2 Melt a representative portion of the sample on a steambath or hot water bath. Fill the test tube to the 5-mL mark withH2SO4(94.7 6 0.2 %). Then add the melted wax, at a5

30、A solution of sulfuric acid and Nochromix (a trademark of Godax Laboratories,480 Canal St., New York, NY 10013) has been found suitable for this purpose.FIG. 1 Color Comparator for Carbonizable Substances in Liquid PetrolatumD 612 88 (2004)2temperature not more than 10F (5.5C) above its meltingpoint

31、, to the 10-mL mark, insert the stopper loosely, and placethe test tube in position in the water bath at 158 6 1.0F (7060.5C).7.3 After the test tube has been in the water bath for 5 min,loosen the stopper sufficiently to release any pressure andreinsert, remove the test tube from the bath quickly,

32、hold witha finger over the stopper, and give three vigorous, verticalshakes over an amplitude of about 5 in. (127 mm), shaking thetest tube quickly and at a rate corresponding to 5 shakes/s.Repeat every minute. Do not keep the test tube out of the bathlonger than 3 s for each shaking period.NOTE 1A

33、shaking machine may be used provided that the resultsobtained agree with those obtained by the prescribed manual agitation.7.4 At the end of 10 min from the time the test tube was firstplaced in the bath, remove the test tube, immediately place it inthe color comparator, and compare the acid layer w

34、ith 5 mL ofthe standard colorimetric solution and 5 mL of white mineraloil in a test tube that has been shaken vigorously for 10 s andallowed to stand just long enough for the contents to separateinto two layers.7.5 In some cases the acid remains trapped with the wax asan emulsion, and no lower laye

35、r is obtained to compare withthe standard colorimetric solution. When this occurs, comparethe emulsion with the standard colorimetric solution and whitemineral oil shaken vigorously to give a similar emulsion, andwithout waiting for the two liquids to separate.8. Interpretation of Results8.1 Paraffi

36、n wax shall be reported as passing the test whenthe acid layer is not darker than the reference standardcolorimetric solution or, if completely emulsified, when theemulsion is not darker than a similar emulsion produced byvigorously shaking the reference standard colorimetric solutionwith white mine

37、ral oil in equal proportions.8.2 If the acid layer is darker than the reference standardcolorimetric solution, or if the emulsified paraffin wax and acidare darker than a similar emulsion of the reference standardcolorimetric solution and white mineral oil in equal propor-tions, the paraffin wax sha

38、ll be reported as not passing the test.9. Precision and Bias9.1 No statement is made about either the precision or thebias of this test method for measuring carbonizable substancesin white refined waxes since the result only states whether thereis conformance to the criteria for success specified in

39、 theprocedure.10. Keywords10.1 carbonizable substances; petroleum wax; waxANNEX(Mandatory Information)A1. WARNING STATEMENTSA1.1 Glass Cleaning Solution (Nochromix5)WarningCorrosive, potent, clear liquid. Solution is amixture of sulfuric acid (concentrated) and Nochromix,5awhite crystalline, inorgan

40、ic oxidizer.Handle carefully with special highly acid resistant glovesonly.Do not close container airtight.A1.2 Hydrochloric Acid (Concentrated)WarningPoison. Corrosive. May be fatal if swallowed.Liquid and vapor cause severe burns. Harmful if inhaled.Do not get in eyes, on skin, or on clothing.Do n

41、ot breathe vapor, spray, or mist.Dilute by addition of acid to water.Keep in tightly closed container in approved acid storagecabinet.Keep cool.Loosen closure carefully when opening.Use with adequate ventilation.Keep container closed when not in use.Use protective clothing and goggles when handling.

42、Wash thoroughly after handling.A1.3 Sulfuric Acid (Concentrated)Do not get in eyes, on skin or on clothing.Do not breathe vapor, spray, or mist.Dilute by addition of acid to water.Keep in tightly closed container in approved acid storagecabinet.Keep cool.Loosen closure carefully when opening.Use wit

43、h adequate ventilation.Do not allow water to get into container because of violentreaction.Keep container closed when not in use.Use protective clothing and goggles when handling.Wash thoroughly after handling.A1.4 Sodium HydroxideBefore using, secure information on procedures and protec-tive measur

44、es for safe handling.Do not get in eyes, on skin, or on clothing.Avoid breathing dusts or mists.Do not take internally.When handling, use chemical safety goggles or face shield,protective gloves, boots, and clothing.D 612 88 (2004)3When mixing with water, add slowly to surface of solutionto avoid vi

45、olent spattering. In the preparation of solutions donot use hot water, limit temperature rise, with agitation, to10C/min or limit solution temperature to a maximum of 90C.No single addition should cause a concentration increasegreater than 5 %.A1.5 Acetic Acid (Glacial)Do not get in eyes, on skin, o

46、r on clothing.Do not breathe vapor, spray or mist.Dilute by addition of acid to water.Keep away from heat and open flame.Keep in tightly closed container in approved acid storagecabinet.Keep cool.Loosen closure carefully when opening.Use with adequate ventilation.Keep container closed when not in us

47、e.Use protective clothing and goggles when handling.Wash thoroughly after handling.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the

48、validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your

49、comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,U