1、Designation: D612 88 (Reapproved 2012)Standard Test Method forCarbonizable Substances in Paraffin Wax1This standard is issued under the fixed designation D612; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisi
2、on. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () 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 covers determination of carboni
3、zablesubstances 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 D87, between 117 and 149F (47and 65C).1.2 The values stated in inch-pound units are to be r
4、egardedas standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information onlyand are not considered 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 u
5、ser of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific warningstatements are given in Annex A1.2. Referenced Documents2.1 ASTM Standards:2D87 Test Method for Melting Point of Petroleum Wax(Cooling C
6、urve)D1193 Specification for Reagent Water3. Summary of Test Method3.1 Five millilitres of melted wax are 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
7、 the standard,the wax is reported as passing the test.4. Significance and Use4.1 This test method is a means 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-resis
8、tant glass3fitted with a well-ground glass stopper, the stopper and the tubebearing identical and indestructible 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
9、 tube withstopper inserted shall be between 13.6 and 15.6 mL. A rollededge may be provided for suspending 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
10、 provided with a coverof any suitable material, with holes approximately 16 mm indiameter through which 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
11、 comparatorare optional, but the size and shape of the apertures shallconform to the dimensions prescribed 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
12、the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.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.1This test met
13、hod is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.10.0A on Physical/Chemical Properties.Current edition approved Nov. 1, 2012. Published November 2012. Originallyapproved in 1941. Last previous edition approved
14、 in 2007 as D61288(2007). DOI:10.1520/D0612-88R12.2For 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 to the standards Document Summary page onthe ASTM website.3Borosilica
15、te 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 Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd.,
16、 Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16.2 Purity of WaterUnless otherwise indicated, re
17、ferencesto water shall be understood to mean distilled water, such asreagent water corresponding to Specification D1193, Type III,or water of equal purity.6.3 Cobaltous Chloride Solution (0.5 N)Dissolve about65 g of cobaltous chloride (CoCl26H2O) in enough dilutedhydrochloric acid (HCl, 1 + 39) (War
18、ningHydrochloric acid(concentrated) causes burns, vapor extremely irritating. SeeA1.2) to make 1000 mL of solution. Transfer exactly 5 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
19、produces aviolent reaction or eruption upon too rapid a mixture withwater. See A1.4), and 5 mL of hydrogen peroxide. Boil for 10min, cool, and add2gofpotassium iodide (KI) and 20 mL ofsulfuric acid (H2SO4, 1+4) (WarningSulfuric acid (con-centrated) causes burns, vapor irritating, strong oxidizer. Se
20、eA1.3). When the precipitate has dissolved, titrate the liberatediodine with 0.1 N sodium thiosulfate (Na2S2O3) solution usingstarch solution 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 ad
21、dition ofdiluted HCl (1 + 39) so that 1 mL contains 59.5 mg ofCoCl26H2O.6.4 Colorimetric Reference Standard SolutionPrepare areference 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
22、 mL ofthis mixture into a test tube as specified in 3.1. This pale amberreference standard shall then be overlaid with 5 mL of whitemineral oil.6.5 Cupric Sulfate Solution (0.5 N)Dissolve about 65 g ofcupric sulfate (CuSO45H2O) in enough diluted HCl (1 + 39)(WarningHydrochloric acid (concentrated) c
23、auses burns,vapor extremely irritating. See A1.2) to make 1000 mL ofsolution. Transfer exactly 10 mL of this solution to a flask, add50 mL of water, 4 mL of acetic acid (WarningAcetic acid(glacial) is corrosive, combustible, vapor irritating. See A1.5),and3gofKI.Allow the mixture to stand for 5 min,
24、 then titratethe liberated iodine with 0.1 N Na2S2O3solution, using starchsolution as an indicator. Each millilitre of 0.1 N Na2S2O3solution 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 CuSO45
25、H2O.6.6 Ferric Chloride Solution (0.5N)Dissolve about 55 gof ferric chloride (FeCl36H2O) in enough diluted HCl(WarningHydrochloric acid (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
26、 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 mLof 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
27、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 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)
28、shall benitrogen-free when analyzed in accordance with the followingprocedure: Dilute a small amount of the acid with an equalvolume 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
29、 thezone of contact within 1 h. This test detects as little as0.0002 % NO3.7. Procedure7.1 Clean a test tube with cleaning solution of sulfuric acidand Nochromix5(Warning Nochromix5is corrosive. SeeA1.1), rinse with tap water followed by distilled water, and dryin an oven at 105 C for 1 h.5Nochromix
30、 is a trademark of Godax Laboratories, Inc., P.O. Box 422, CabinJohn, MD 20818.FIG. 1 Color Comparator for Carbonizable Substances in Liquid PetrolatumD612 88 (2012)27.2 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
31、 0.2 %). Then add the melted wax, at atemperature not more than 10F (5.5C) above its meltingpoint, 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 stopp
32、er sufficiently to release any pressure andreinsert, remove the test tube from the bath quickly, 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
33、minute. Do not keep the test tube out of the bathlonger than 3 s for each shaking period.NOTE 1A 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
34、, remove the test tube, immediately place it inthe color comparator, and compare the acid layer with 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 tw
35、o layers.7.5 In some cases the acid remains trapped with the wax asan emulsion, and no lower layer 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 emu
36、lsion, andwithout waiting for the two liquids to separate.8. Interpretation of Results8.1 Paraffin 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 e
37、mulsion produced byvigorously shaking the reference standard colorimetric solutionwith white mineral 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 referenc
38、e standardcolorimetric solution and white mineral oil in equalproportions, the paraffin wax shall be reported as not passingthe 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 sin
39、ce the result only states whether thereis conformance to the criteria for success specified in theprocedure.10. Keywords10.1 carbonizable substances; petroleum wax; waxANNEX(Mandatory Information)A1. WARNING STATEMENTSA1.1 Glass Cleaning Solution (Nochromix5)A1.1.1 WarningCorrosive, potent, clear li
40、quid. Solutionis a mixture of sulfuric acid (concentrated) and Nochromix,5awhite crystalline, inorganic oxidizer.Handle carefully with special highly acid resistant glovesonly.Do not close container airtight.A1.2 Hydrochloric Acid (Concentrated)A1.2.1 WarningPoison. Corrosive. May be fatal if swal-l
41、owed. Liquid and vapor cause severe burns. Harmful ifinhaled.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 with
42、adequate ventilation.Keep container closed when not in use.Use protective clothing and goggles when handling.Wash thoroughly after handling.A1.3 Sulfuric Acid (Concentrated)A1.3.1 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
43、 in tightly closed container in approved acid storagecabinet.Keep cool.Loosen closure carefully when opening.Use with 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
44、thoroughly after handling.A1.4 Sodium HydroxideA1.4.1 Before using, secure information on procedures andprotective measures for safe handling.D612 88 (2012)3Do 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
45、 face shield,protective gloves, boots, and clothing.When mixing with water, add slowly to surface of solutionto avoid violent 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
46、 addition should cause a concentration increasegreater than 5 %.A1.5 Acetic Acid (Glacial)A1.5.1 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 away from heat and open flame.Keep in tightly closed container in approved acid st
47、oragecabinet.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.Wash thoroughly after handling.ASTM International takes no position respecting the validity of any patent rights asserted
48、 in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the 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
49、 responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your 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
