1、Designation:E165905 Designation: E1659 12Standard Test Methods forCoating WeightMass and Chemical Analysis of Zinc-NickelAlloy Electrolytically Coated on Steel Sheet1This standard is issued under the fixed designation E1659; the number immediately following the designation indicates the year oforigi
2、nal adoption or, in the case of revision, 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.1. Scope1.1 These test methods cover independently the chemical analysis of
3、each surface of zinc-nickel alloy electrolytically coatedon steel sheet. The coatings have chemical compositions within the following limits:Analyte Concentration RangeCoating Weight 0.0to80g/m2Coating mass 0.0to80g/m2Nickel 7.0 to 17.0 %1.2 These test methods are in the following sections:SectionsC
4、oating Weight, by the Weigh-Strip-Weigh Method(20.0 to 45.0 g/m2)10-20Coating mass, by the Weigh-Strip-Weigh Method(20.0 to 45.0 g/m2)10-20Nickel by the Atomic Absorption Method (11.0 to 13.5 %of Coating Weight Ranging from 20 to 45 g/m2)21-31Nickel by the Atomic Absorption Method (11.0 to 13.5 %of
5、Coating mass Ranging from 20 to 45 g/m2)21-311.3 The values stated in SI units are to be regarded as standard. In some cases, exceptions allowed in Practice E380 are alsoused.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsi
6、bilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2A917 Specification for Steel Sheet, Coated by the Electrolytic Process for Applications Requiring D
7、esignation of the CoatingMass on Each Surface (General Requirements)A918 Specification for Steel Sheet, Zinc-Nickel Alloy Coated by the Electrolytic Process for Applications RequiringDesignation of the Coating Mass on Each SurfaceD1193 Specification for Reagent WaterE29 Practice for Using Significan
8、t Digits in Test Data to Determine Conformance with SpecificationsE50 Practices forApparatus, Reagents, and Safety Considerations for ChemicalAnalysis of Metals, Ores, and Related MaterialsE135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related MaterialsE173 Practice for Cond
9、ucting Interlaboratory Studies of Methods for Chemical Analysis of Metals3E380 Practice for Use of the International System of Units (SI) (the Modernized Metric System)0E663 Practice for Flame Atomic Absorption AnalysisE882 Guide for Accountability and Quality Control in the Chemical Analysis Labora
10、toryE1024 Guide for Chemical Analysis of Metals and Metal Bearing Ores by Flame Atomic Absorption SpectrophotometryE1452 Practice for Preparation of Calibration Solutions for Spectrophotometric and for Spectroscopic Atomic Analysis1These test methods are under the jurisdiction of ASTM Committee E01
11、on Analytical Chemistry for Metals, Ores, and Related Materials and are the direct responsibilityof Subcommittee E01.05 on Cu, Pb, Zn, Cd, Sn, Be, their Alloys, and Related Metals.Current edition approved Oct.April 1, 2005.2012. Published November 2005.May 2012. Originally approved in 1995. Last pre
12、vious edition approved in 20002005 asE1659 005. DOI: 10.1520/E1659-05.10.1520/E1659-12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summa
13、ry page on the ASTM website.3Withdrawn. The last approved version of this historical standard is referenced on www.astm.org.1This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becaus
14、eit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Bar
15、r Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.E1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method3. Terminology3.1 For definitions of terms used in this test method, refer to Terminology E135.4. Significance and Us
16、e4.1 These test methods for the chemical analysis of zinc-nickel alloy coating on sheet steel are primarily intended as refereemethods to test such materials for compliance with compositional specifications such as found in Specification A918, particularlythose under the jurisdiction of ASTM Committ
17、ee A05 on Metallic-Coated Iron and Steel Products. It is assumed that all who usethese test methods will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expectedthat work will be performed in a properly equipped laboratory under appropriate quality
18、 control practices such as those describedin Guide E882.4.2 These test methods must be applied twice, once to each side of the specimen if coating weightmass and composition arerequired for both sides of a coated sheet. Two separate specimens are required for this purpose.5. Apparatus, Reagents, and
19、 Instrumental Practices5.1 ApparatusSpecialized apparatus requirements are listed in the apparatus section in each individual test method.5.2 Reagents:5.2.1 Purity of ReagentsUnless otherwise indicated, all reagents used in these test methods shall conform to the ReagentGrade Specifications of the A
20、merican Chemical Society.4Other chemicals may be used, provided it is first ascertained that theyare of sufficiently high purity to permit their use without adversely affecting the expected performance of the determination, asindicated in Section 30.5.2.2 Purity of WaterReferences to water shall be
21、understood to mean reagent water as defined by Type II of SpecificationD1193.5.3 Photometric PracticePhotometric practice prescribed in these test methods shall conform to Guide E1024 and PracticeE1452.6. Safety Hazards6.1 For precautions to be observed in the use of certain reagents and equipment i
22、n these test methods, refer to Practices E50.7. Sampling7.1 Zinc-Nickel Alloy Coated SheetsSamples for determining weightmass and composition of coating shall be secured inaccordance with Specification A917, which is referred to in Specification A918. Test specimens shall be of squares with sides of
23、50 6 5 mm. One test specimen is required for each side to be analyzed. The backside which is not to be analyzed shall be marked“X.”8. Interlaboratory Studies and Rounding Calculated Values8.1 Calculated values shall be rounded to the desired number of places in accordance with the rounding method of
24、 Practice E29.9. Interlaboratory Studies9.1 These test methods have been evaluated using Practice E173, except for the update in the stripping solution, 17.1, 17.8,20.1.2, 20.2, 31.1.1, and 31.2 as well as Table 1, Table 2, Table 3, and Table 4.WEIGHTMASS OF COATING ON ZINC-NICKEL ALLOY-COATED SHEET
25、 BY WEIGH-STRIP-WEIGHMETHOD10. Scope10.1 This test method provides a procedure for determining independently the weightmass of coating on each surface ofzinc-nickel alloy-coated sheet steel, in coating masses from 20 to 45 g/m2(Note 1).NOTE 1The upper limit of the scope has been set at 45 g/m2becaus
26、e test materials with higher coating weightmass were not available for testingin accordance with Practice E173. However, recognizing the simplicity of the weigh-strip-weigh technique, materials with higher coating weights can betested following this procedure. Users of this test method are cautioned
27、 that use of it for coating weightmass determinations above 45 g/m2is not supportedby interlaboratory testing.11. Summary of Test Method11.1 The coating on the sheet steel is stripped by using hydrochloric acid solution containing an inhibitor to prevent the attack4Reagent Chemicals, American Chemic
28、al Society Specifications , American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. P
29、harmacopeial Convention, Inc. (USPC), Rockville, MD.E1659 122on the base steel. The coating weightmass is determined from the weightmass difference of the specimen before and after stripping.12. Interferences12.1 The hexamethylene tetramine inhibitor used in this test method permits the dissolution
30、of some base metal, which couldlead to higher than expected coating weightmass determinations. Since Zn/Ni coatings contain no appreciable amounts of Fe, theeffects of this bias are corrected by determining the mass of iron stripped with the coating and subtracting that value from the rawweigh-strip
31、-weigh data.13. Apparatus13.1 Analytical Balance, capable of weighing to 0.1 mg.TABLE 1 Statistical InformationComparison of StrippingSolutions on 20/20 MaterialTestMaterialOriginalStrippingSolution,g/m2ACurrentStrippingSolution,g/m2AIronStripped,g/m2BAdjustedCoatingWeight,g/m2C1 23.45 23.74 0.68 23
32、.062 23.18 24.29 0.83 23.463 23.54 24.33 1.13 23.204 23.11 23.94 0.64 23.30Average 23.320 24.075 0.820 23.2552 Standard Deviations 0.415 0.568 0.445 0.337AResults obtained following the original test method with no adjustments for ironstripped.BIron stripped from base metal from 17.8, expressed in g
33、/m2.CCoating weight mass results obtained by using the current test method,adjusting for the stripped iron.TABLE 2 Statistical InformationComparison of StrippingSolutions on 30/30 MaterialTestMaterialOriginalStrippingSolution,g/m2ACurrentStrippingSolution,g/m2AIronStripped,g/m2BAdjustedCoatingWeight
34、,g/m2C1 35.21 38.19 1.03 37.162 37.47 35.83 0.50 35.333 35.64 37.86 0.55 37.314 37.65 36.05 0.51 35.54Average 36.493 36.983 0.648 36.3432 Standard Deviations 2.494 2.429 0.512 2.074AResults obtained following the original test method with no adjustments for ironstripped.BIron stripped from base meta
35、l from 17.8, expressed in g/m2.CCoating weight mass results obtained by using the current test method,adjusting for the stripped iron.TABLE 3 Statistical InformationComparison of StrippingSolutions on 20/20 MaterialTest MaterialOriginal StrippingSolution, %NiCurrent StrippingSolution, %Ni1 11.25 11.
36、382 11.20 11.303 11.37 11.33Average 11.27 11.342 Standard Deviations 0.175 0.081TABLE 4 Statistical InformationComparison of StrippingSolutions on 30/30 MaterialTest MaterialOriginal StrippingSolution, %NiCurrent StrippingSolution, %Ni1 11.44 11.742 11.40 11.763 11.42 11.684 11.20 11.85Average 11.37
37、 11.762 Standard Deviations 0.222 0.141E1659 12313.2 Electroplaters Tape, capable of protecting one side of a coated piece of sheet steel while the other side is being strippedin a hydrochloric acid solution. It must not contaminate the acid solution or interfere with the coating weightmass determin
38、ationby gaining or losing weight. mass.13.3 Vernier Calipers, calibrated to an international standard and capable of measuring to at least 0.05 mm.14. Reagents14.1 Hexamethylene Tetramine, USP GradeUsed as an inhibitor to prevent acid attack of the base metal while stripping thecoating from the base
39、 steel.14.2 Stripping SolutionAdd 340 mL hydrochloric acid to 1660 mL of water. Add 7.0 g of hexamethylene tetramine, mix, andcool before use.15. Precautions15.1 WarningHydrogen gas, which can form explosive mixtures with air, is evolved in the stripping process. Therefore, thistest method should be
40、 performed under conditions of adequate ventilation, such as a fume hood.16. Sample Preparation16.1 Clean the specimens with acetone using a soft paper towel, then dry with oil-free compressed air.16.2 Cover the side of the specimen from which the coating is not to be stripped with electroplaters ta
41、pe.16.3 Use a roller to press the tape firmly against the sheet, making sure to remove all air bubbles or wrinkles.16.4 Trim off the excess tape.16.5 Press the tape firmly near the edge to protect the taped side from acid attack.16.6 Write the sample identification on the taped side with a marker.17
42、. Procedure17.1 Specimen AreaUsing the calipers, measure and record the length of all four sides of the test specimen.17.1.1 Check that the measuring face and reference edge of the calipers are clean. Check that the calipers read “0” when themeasuring surface is closed. If it does not, correct the p
43、roblem according to the manufacturers instructions.17.1.2 Place the calipers at the corners of the specimen and measure the length of each side to the nearest 0.005cm.17.1.3 Record the length of each side as shown in the diagram below.NOTE 2To ensure that the calculated area is accurate even if the
44、specimen does not have 90 angles, all four sides are measured. In 18.2, the averageof opposite sides is calculated and used to determine specimen area.17.2 Weigh the prepared specimen to the nearest 0.1 mg and record the weightmass as the original weightmass of the specimen.17.3 Place the sample in
45、a 600-mL beaker with the taped side down.17.4 Add 25 mL of stripping solution slowly. As the coating is stripped, the color changes from gray to black and back to gray(see Note 3).NOTE 3Stripping time will depend on the nickel composition and weightmass of the coating.17.5 After the coating is strip
46、ped, remove the sample with a poly (tetrafluoroethylene) coated magnet attached to one end ofan approximately 150-mm long flexible polyethylene tube. Holding it over the same beaker, rinse it carefully with water and policethe stripped side to remove the last traces of nickel.17.6 Dry the stripped s
47、pecimen with oil-free compressed air. Weigh it to the nearest 0.1 mg and record the weight. mass.17.7 Warm the beaker on a hotplate until all the stripped coating is dissolved. Transfer the solution to a 100-mLvolumetric flask,dilute to the mark, and mix thoroughly. Reserve this sample stock solutio
48、n for iron determination.17.8 Determination of Stripped Iron:17.8.1 Calibrate the instrument in accordance with the manufacturers instructions following the guidelines set forth in GuideE1024 and Practice E1452. Choose the appropriate wavelength and calibration solutions that provide a calibration c
49、urve thatincludes up to 2.0 mg Fe/100 mL of solution.E1659 12417.8.2 Verify the calibration curve with an iron control solution that falls in the mid-range of the calibration curve. If this controlstandard is not within 610 % of its assumed true value, identify the problem, recalibrate, and verify the curve. If the controlstandard is within 610 %, analyze the solutions from 17.7 for iron.17.8.3 After the final sample stock solution is analyzed, read the iron control standard and check that the reading is within610 % of the assumed true value. If it is not,
