1、Designation: D565 99 (Reapproved 2013)Standard Test Method forCarbonizable Substances in White Mineral Oil1This standard is issued under the fixed designation D565; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last r
2、evision. 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 white mineral oil (
3、Mineral OilUSP and Light Mineral Oil NF) to determine whether itconforms to the standard of quality required for pharmaceuticaluse as defined by the United States Pharmacopeia and theNational Formulary, or the Food and Drug Administration.1.2 The values stated in SI units are to be regarded asstanda
4、rd. No other units of measurement are included in thisstandard.1.2.1 ExceptionDimension requirements for the colorcomparator in Fig. 1 are in SI and inch-pound units.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of t
5、he user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specific hazardstatements, see Section 6.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent Water2.2 Offcial Compendia:3
6、United States PharmacopeiaCurrent EditionMonograph on Mineral OilNational FormularyCurrent EditionMonograph on Light Mineral Oil2.3 Government Document:421CFR 172.878 Food and Drug Administration Title3. Summary of Test Method3.1 The mineral oil is treated with concentrated sulfuric acid(H2SO4) unde
7、r prescribed conditions and the resulting color iscompared with a reference standard to determine whether itpasses or fails the test.4. Significance and Use4.1 This test method is a means for ascertaining whetherpharmaceutical mineral oil conforms to the standards of theUnited States Pharmacopeia, t
8、he National Formulary, and theFood and Drug Administration.5. Apparatus5.1 Test Tube, as shown in Fig. 1, of heat-resistant glassfitted 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 1
9、5.0 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 can be provided for suspending the tube on the cover ofthe water bath.5.2 Water Bath, suitable for immersin
10、g the test tube abovethe 10 mL line equipped to maintain a temperature of 100 60.5C. The bath shall be provided with a cover of any suitablematerial with holes approximately 16 mm in diameter throughwhich the test tubes can be suspended.5.3 Color Comparator, of a suitable type for observing thecolor
11、 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 prescribed in Fig. 1.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Prod
12、ucts, Liquid Fuels, and Lubricantsand is the direct responsibility ofSubcommittee D02.06 on Analysis of Lubricants.Current edition approved Oct. 1, 2013. Published October 2013. Originallyapproved in 1940. Last previous edition approved in 2009 as D565 99 (2009)1.DOI: 10.1520/D0565-99R13.2For refere
13、nced 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.3Available from U.S. Pharmacopeial Convention, 12601 Twinbrook Parkway,R
14、ockville, MD 20852.4Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16. Reagents6.1 Purity of ReagentsReagent
15、 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 available.5Other grades may beused, provided it is first
16、 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 or water ofequal purity conforming to Type III of Specificati
17、on D1193.6.3 Cobaltous Chloride Solution (0.25 M)Prepare a solu-tion of hydrochloric acid (HCl) (WarningCauses burns.Vapor extremely irritating.) by mixing 30 mL of concentratedHCl with 1170 mL of water. Slowly add the acid to the water.Dissolve 65 6 1 g of cobaltous chloride hexahydrate(CoCl26H2O)
18、in the HCl solution to make 1000 mL ofsolution. Using a pipet, transfer 5 mL of this solution to a 250mL iodine flask. Prepare a solution of sodium hydroxide(NaOH) ( WarningCorrosive. Can cause severe burns orblindness. Evolution of heat produces a violent reaction oreruption upon too rapid a mixtur
19、e with water.) by mixing 5 gof NaOH with 20 mL of water. Add 15 mL of this NaOHsolution to the iodine flask. Add 5 mL of hydrogen peroxide(H2O2) (3 % v/v). Boil for 10 6 1 min, cool, and add2gofpotassium iodide (KI). Prepare a solution of H2SO4(WarningCauses burns. Vapor extremely irritating. Strong
20、oxidizer.) by mixing 6 mL of H2SO4with 18 mL of water.Slowly add the acid to the water (see Note 1). Add 20 mL ofthis H2SO4solution to the flask.) When the precipitate hasdissolved, titrate the liberated iodine with 0.100 M sodiumthiosulfate (Na2S2O3) solution, using starch solution as anindicator.
21、Each millilitre of Na2S2O3solution is equivalent to0.0238 g of CoCl26H2O. Adjust the final volume of CoCl2solution by the addition of HCl solution so that 1 mL contains59.5 mg of CoCl26H2O.NOTE 1This freshly prepared H2SO4solution will be hot. Allow tocool before continuing.6.4 Cupric Sulfate Soluti
22、on (0.25 M)Prepare a solution ofHCl (Warningsee 6.3) by mixing 30 mL of concentratedHCl with 1170 mL of water. Slowly add the acid to the water.Dissolve 65 6 1 g of cupric sulfate pentahydrate(CuSO45H2O) in enough HCl solution to make 1000 mL ofsolution. Using a pipet, transfer 10 mL of the solution
23、 to a250-mL iodine flask, add 40 mL of water. Prepare a 6M aceticacid (CH3COOH) (WarningCorrosive. Combustible. Vaporirritating.) solution by mixing 353 mL of concentratedCH3COOH with 1000 mL of water. Slowly add the acid to thewater.Add 4 mL of 6M CH3COOH,3gofKland5mLofHClto the flask. Titrate the
24、liberated iodine with 0.100 M Na2S2O3solution, using starch solution as an indicator. Each millilitre ofNa2S2O3solution is equivalent to 0.0250 g of CuSO45H2O.Adjust the final volume of the CuSO4solution by the additionof diluted HCl solution so that 1 mL contains 62.4 mgCuSO45H2O.6.5 Ferric Chlorid
25、e Solution (0.166 M)Prepare a solutionof HCl (Warningsee 6.3) by mixing 30 mL of concentratedHCl with 1170 mL of water. Dissolve 55 6 1 g of ferricchloride hexahydrate (FeCl36H2O) in enough HCl to make1000 mL of solution. Using a pipet, transfer 10 mL of thissolution into a 250-mL iodine flask, add
26、15 mL water,3gKIand 5 mL HCl, and allow the mixture to stand for 15 6 1 min.Dilute with 100 mL of water and titrate the liberated iodinewith 0.100 M Na2S2O3solution, using starch solution as anindicator. Each millilitre of Na2S2O3solution is equivalent to0.0270 g of FeCl36H2O. Adjust the final volum
27、e of FeCl3solution by the addition of the HCl solution so that 1 mLcontains 45.0 mg of FeCl36H2O.5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual S
28、tandards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.FIG. 1 Color Comparator for Carbonizable Substances in Liquid PetrolatumD565 99 (2013)26.6 The solutions prepared in 6.3
29、 6.5 may be prepared indifferent quantities, provided the ratios of components areequivalent.6.7 Colorimetric Reference Standard SolutionPrepare areference standard pale amber solution for color comparison bymixing together 1.5 parts of CoCl2solution, 3.0 parts of theFeCl3solution, and 0.5 parts of
30、the CuSO4solution. Measure5 mL of this mixture into a test tube as specified in 5.1. Thispale amber reference standard shall then be overlaid with 5 mLof white mineral oil.6.8 Sulfuric Acid (94.7 6 0.2 %)The H2SO4shall benitrogen-free when analyzed in accordance with the followingprocedure: Dilute a
31、 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 thezone of contact within 1 h. This test detects as little as0.0002 % nitric acid (HNO
32、3).7. Procedure7.1 Clean a test tube with a chromic acid (H2CrO4) cleaningsolution (WarningCauses severe burns. A recognized car-cinogen. Strong oxidizer.), or use a nonchromium containing,strongly oxidizing cleaning solution.7.2 Fill the test tube to the 5 mL mark with H2SO4(94.7 60.2 %). Then add
33、the oil to be tested to the 10-mL mark, insertthe stopper loosely, and place the test tube in position in thewater bath at 100 6 0.5C.7.3 After the test tube has been in the water bath for 30 s,loosen the stopper sufficiently to release any pressure andreinsert, remove the test tube from the bath qu
34、ickly, hold witha finger over the stopper, and give three vigorous, verticalshakes over an amplitude of about 127 mm, shaking the testtube quickly and at a rate corresponding to 5 shakes/s. (Ashaking machine may be employed provided the results thatcan be obtained agree with those obtained by the pr
35、escribedmanual agitation.) Repeat every 30 s. Do not keep the test tubeout of the bath longer than 3 s for each shaking period.7.4 At the end of 10 min from the time the test tube was firstplaced in the bath, remove the test tube and allow to stand inthe room for not less than 10 min nor more than 3
36、0 min.Observe and record any discoloration of the oil layer. Place thetest tube in the color comparator, and compare the acid layerwith 5 mL of the standard colorimetric solution and 5 mL ofwhite mineral oil in a test tube that has been shaken vigorouslyfor 10 s and allowed to stand just long enough
37、 for the contentsto separate into two layers.8. Interpretation of Results8.1 White mineral oil shall be reported as passing the testonly when the oil layer shows no change in color (see Note 2)and when the acid layer is not darker than the referencestandard colorimetric solution.NOTE 2A bluish haze
38、or a slight pink or yellow color in the oil layershould not be interpreted as a change in color.8.2 If the oil layer is discolored or if the acid layer is darkerthan the reference standard colorimetric solution, white min-eral oil shall be reported as not passing the test.9. Precision and Bias9.1 No
39、 statement is made about either the precision or biasof this test method since the result merely states whether thereis conformance to the criteria for success specified in theprocedure.10. Keywords10.1 carbonizable substances; mineral oilASTM International takes no position respecting the validity
40、of any patent rights asserted 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 t
41、o revision at any time by the 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.
42、 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
43、copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D565 99 (2013)3
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