1、Designation: C715 90 (Reapproved 2016)Standard Test Method forNickel on Steel for Porcelain Enameling by PhotometricAnalysis1This standard is issued under the fixed designation C715; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision,
2、the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.INTRODUCTIONThe test is designed to give a sufficiently accurate and rapid test of the amount of nickel depositedon sh
3、eet steel for enameling plant control work via a photometric method. However, the approxima-tions used in the method prevent its use where extremely accurate nickel determinations are required.The method is applicable to control the weight of nickel coating on the metal.1. Scope1.1 This test method
4、covers the determination of the amountof nickel deposited on sheet steel during its preparation forporcelain enameling. It is a photometric method commonlyused on production parts and is suitable for determining theheavier nickel deposits that may be obtained during theprocessing of steel for one-co
5、at enameling.NOTE 1An alternative X-ray emission spectrometry method is TestMethod C810.1.2 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
6、 and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C810 Test Method for Nickel on Steel for Porcelain Enam-eling by X-Ray Emission SpectrometryE30 Test Methods for Chemical Analysis of Steel, Cast Iron,Open-Hearth Iron, and Wrought Iro
7、n (Withdrawn 1995)3E60 Practice for Analysis of Metals, Ores, and RelatedMaterials by Spectrophotometry3. Significance and Use3.1 This test method is primarily used to control the nickeldipping operation to ensure that the desired level of nickeldeposition is attained. It is also used to prepare tes
8、t plates usedfor calibration in Test Method C810.4. Apparatus4.1 Photoelectric Photometer, conforming to Practice E60.4.2 Weighted Rubber Ring Assembly, required to confinestripping agents to a definite area, consisting of a moldedrubber ring and a metal outer ring. The rubber ring shall havean insi
9、de diameter of 1.35 in. (34.3 mm) in order to encircle anarea of 0.01 ft2(0.000929 m2), a wall configuration as shownin Fig. 1, and the lower portion beveled at a 45 angle (0.78rad) to reduce the contact area and ensure a better seal. Themetal outer ring shall weigh about 3.5 lb (1.5 kg), suitablyma
10、chined to fit over the top of the rubber ring as shown in Fig.1.4.2.1 The exact area covered by the rubber ring willgradually increase as the rubber ring itself is consumed by theacid reagent used. In the most accurate analysis, the area etchedby the rubber ring shall be calculated occasionally, fac
11、toredagainst the prescribed area, and that number applied to thereading obtained from the graph.4.3 Aspirator, consisting of a calibrated 500-mL flask,equipped with a twohole stopper, an aspirator bulb, and asuction tube formed from 0.079-in. (2-mm) inside diametercapillary glass tubing.5. Reagents
12、and Materials5.1 Reagent grade chemicals shall be used in all tests.Unless otherwise indicated, it is intended that all reagents shallconform to the specifications of the Committee of Analytical1This test method is under the jurisdiction ofASTM Committee B08 on Metallicand Inorganic Coatings and is
13、the direct responsibility of Subcommittee B08.12 onMaterials for Porcelain Enamel and Ceramic-Metal Systems.Current edition approved Nov. 1, 2016. Published November 2016. Originallyapproved in 1977. Last previous edition approved in 2011 as C715 90 (2011)1.DOI: 10.1520/C0715-90R16.2For referenced A
14、STM 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.3The last approved version of this historical standard is referenced onwww.ast
15、m.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1Reagents of the American Chemical Society.4Other gradesmay be used, provided it is first ascertained that the reagent isof sufficiently high purity to permit its use without lessen
16、ingthe accuracy of the determination.5.2 Purity of WaterUse distilled or deionized water.5.3 Ammonium Hydroxide (sp gr 0.90)Concentrated am-monium hydroxide (NH4OH).5.4 Ammonium Persulfate(NH4)2S2O8.5.5 DimethylglyoximePrepare a 1 % solution of dimethyl-glyoxime in methyl alcohol or a 2.62 % solutio
17、n of sodiumdimethylglyoximate in water (store in a polyethylene bottle).5.6 Hydrochloric Acid (1+5)Dilute 1 vol of concentratedhydrochloric acid (HCl, sp gr 1.19) with 5 vol of water.5.7 Nickel Sulfate, Standard SolutionDissolve 0.448 g ofnickel sulfate (NiSO46H2O) in water. When the material iscomp
18、letely dissolved, cautiously add 10 mL of concentratedH2SO4and transfer the solution to the 1000-mL flask. Whencool, make up to the mark with water. One millilitre of thisstandard solution is equivalent to 0.0001 g of nickel permillilitre.5.8 Nitric Acid (1+1)Dilute 1 vol of concentrated nitricacid
19、(HNO3, sp gr 1.42) with 1 vol of water.5.9 Sulfuric Acid (sp gr 1.84)Concentrated sulfuric acid(H2SO4).6. Sampling6.1 Sampling frequency shall be consistent with the objec-tive of control of the nickel dipping operation.7. Standardization of Photoelectric Photometer7.1 The photoelectric photometer s
20、hall be standardized asfollows:7.1.1 Using a buret, accurately measure out 2, 4, 8, 12, 16,and 20 mL portions of nickel sulfate standard solution. Theseamounts are equivalent to 0.2, 0.4, 0.9, 1.3, 1.7, and 2.1 g ofnickel per square metre (0.02, 0.04, 0.08, 0.12, 0.16, and 0.20g of nickel per square
21、 foot) of surface when specimens fromthe steel surface are obtained as prescribed. (Iron in solutionthat is dissolved from the steel surfaces has a negligible effecton the nickel determinations.) Using the standard analyticalprocedures described in 8.2, determine the percent transmis-sion at a wavel
22、ength of approximately 525 nm for each of thesix increments of nickel sulfate standard solution. Then plot agraph on appropriate graph paper of the percent light transmis-sion against the known nickel concentration representing 0.2 to2.1 g of nickel deposit per square metre of surface. Theresulting
23、graph, which should be a straight line, will be used toobtain nickel-coating masses from light transmission results.8. Determinations of Nickel Coating Masses8.1 Sampling a Nickel-Coated Steel Surface:8.1.1 Place the weighted, rubber ring assembly on thenickel-coated metal surface. Add 3 mL of warm
24、(approxi-mately 120F (50C) HNO3(1+1).Allow the foaming reactionto proceed for about 10 s for light nickel coatings and about 15s for heavier nickel coatings. If the warm acid does not react,scratch the steel surface or try another spot. After the acid hasfoamed for the prescribed time, add 5 mL of H
25、Cl (1+5) to stopthe foaming reaction. Withdraw the solution from the steelsurface with the aspirator into the calibrated flask. Rinse thetest area twice with water and retain the washings in the flask.8.1.2 Alternative methods for determining nickel are de-scribed in Test Methods E30, Sections 62 to
26、 70 for thegravimetric method and Sections 71 to 73 for the volumetricmethod.8.2 Analytical Procedure:8.2.1 Add chemicals in the order given below to the solutionin the flask and mix thoroughly after each addition:Additions for 23-mm OpticalPath CellAAmount inOrder of UseAmmonium hydroxide (sp gr 0.
27、90) 50 mLAmmonium persulfate 4 gDimethylglyoxime 10 mLDilute with water to 500 mLACells with other optical path lengths are available.8.2.2 Filter a portion of the solution. Discard the first 10 to20 mL from the filter and collect a sufficient amount of filtratein the absorption cell for testing. Ju
28、st before testing, set thewavelength as determined in accordance with Section 7 andadjust the instrument to 100 % transmission with a cell thatcontains only water. Place the cell containing the test solutionin the photometer and read the percent transmission.9. Calculation and Report9.1 Refer to the
29、 graph developed in Section 7. Determinethe mass of nickel that corresponds to the percent transmissionreading shown by the photometer. Report the results in gramsof nickel per square metre of steel surface.10. Precision and Bias10.1 The precision and bias of this test method is believed tobe within
30、 0.000929 g/ft2(0.1 g/m2). Exact values are difficult toobtain because of sample inhomogeneity, and the effect of theacid etch on the rubber ring diameter (see 4.2.1).4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testin
31、g of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.NOTE 1The outer ring is a steel disk approximately
32、 6 by12 in. (152by 13 mm), weighing approximately 312 lb (1.58 kg).FIG. 1 Detailed Drawing of Rubber RingC715 90 (2016)2ASTM 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 express
33、ly 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 responsible technical committee and must be reviewed every five years andif not revised,
34、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 att
35、end. 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,United States.
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