1、Designation: C 810 90 (Reapproved 2006)Standard Test Method forNickel on Steel for Porcelain Enameling by X-Ray EmissionSpectrometry1This standard is issued under the fixed designation C 810; the number immediately following the designation indicates the year oforiginal adoption or, in the case of r
2、evision, 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.1. Scope1.1 This test method covers the measurement of the amountof nickel deposited on sheet steel during i
3、ts preparation forporcelain enameling. It is an X-ray emission method used fortesting sample panels or certain commercial parts.NOTE 1An alternative wet chemical method is Test Method C 715.1.2 The values stated in inch-pound units are to be regardedas the standard. The values given in parentheses a
4、re forinformation only.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-bility of regulatory limitations prior
5、 to use. For a specifichazards statement, see Section 7.2. Referenced Documents2.1 ASTM Standards:2C 715 Test Method for Nickel on Steel for Porcelain Enam-eling by Photometric Analysis3. Summary of Test Method3.1 Steel samples coated with a light nickel deposit areinserted in the sample position of
6、 an X-ray spectrometer. Thecount rate for nickel is measured and converted by means of acalibration curve to g/m2(g/f2).NOTE 21 m2= 10.75 ft2. Industry usage is typically in mixed units,grams per square foot. For example, 0.10 g/ft2equals a little more than 1g/m2.4. Significance and Use4.1 This test
7、 method is an accurate and rapid means formeasuring nickel deposits on steel sample plates and such partsthat can be fitted into the X-ray spectrometer. Its accuracyextends over a wide range of nickel deposits.5. Interferences5.1 There are no interferences from other elements present.However, low va
8、lues can result from absorption of the X raysby overlaying material. Grease on the sample or rust due tostorage in humid areas are examples of such material. Lowresults are also obtained on de-enameled samples because thenickel deposit is converted to a nickel iron alloy at enamelingtemperatures. Th
9、e presence of the iron in the alloy layerabsorbs some of the X radiation and accounts for the lowerresult.6. Apparatus6.1 Suitable X-Ray Emission Spectrometer complete with50-kV power supply goniometer, detector with pressure-regulated gas flow attachments, scaler-counter, lithium fluorideanalyzing
10、crystal, and 0.02 Soller slit collimator is required.3About a 1-in. (25.4-mm) diameter area of the sample isirradiated.6.2 Special Sample Holder (Fig. 1), to permit insertion of a2 by 2-in. (51 by 51-mm) flat corner of a large flat sample.Alternatively, the standard sample holder supplied with theeq
11、uipment may be used, but the sample must be cut to 1.5 by1.25 in. (38 by 32-mm).6.3 Steel Sheets with various amounts of nickel deposits arerequired for calibration and standardization.6.4 Nickel-Base Alloy Sample, such as 18-8 stainless steel,for routine calibration.7. Hazards7.1 Equipment should b
12、e periodically checked for radiationleaks to ensure against exposure to X radiation.8. Calibration and Standardization8.1 Prepare approximately 18 standard plates by cleaningand pickling 4 by 6 in. (102 by 152 mm) commercial1This test method is under the jurisdiction ofASTM Committee B08 on Metallic
13、and Inorganic Coatings and is the direct responsibility of Subcommittee B08.12 onMaterials for Porcelain Enamel and Ceramic-Metal Systems.Current edition approved April 1, 2006. Published May 2006. Originallyapproved in 1975. Last previous edition approved in 2000 as C 810 90 (2000).2For referenced
14、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 the following: (1) Philips Electronic Instruments, 750 S. Ful
15、tonAve., Mount Vernon, NY 10550; (2) Siemens Corp., Medical Industrial Div., 186Wood Ave., South, Iselin, NJ 08831; and (3) Diano Corp., X-ray Div., 2 LowellAve., Winchester, MA 01890.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.e
16、nameling iron stock (any steel used in commercial enamelingoperations may be used) and applying nickel in the conven-tional manner for varying treatment times to give a range ofnickel deposition from 0 to 3 g/m2(0 to 0.4 g/ft2).8.2 Prepare a parer mask which, when placed over eachplate, will show th
17、e areas measured by the X-ray spectrometer.The mask is used later to indicate the same areas for wetdetermination of nickel deposition by Test Method C 715.Inthis way, comparative data are obtainable by both measurementmethods on the same areas of the standard plates.8.3 The spectrometer is set to t
18、he K-alpha line of nickel at1.66 A and the X-ray intensity in counts/s is scaled for eachmeasurement. A reference plate of Type 321 stainless steel (Cr18, Ni 10) is measured before and after each measurement onthe standard plates. The two counts on the reference plate areaveraged.8.4 The numbered st
19、andard plates are measured on one sideat two areas, top and bottom, and are corrected for instrumentdrift by relating the count rates on the standard plates to a fixedaverage count rate on the reference plate.8.5 On the basis of X-ray count data, ten standard plates areselected for the best distribu
20、tion of counts covering the fullrange of nickel on the plates. Nickel deposition on the tenselected plates is then determined at one area on each plate byFIG. 1 Special Sample Holder for X-Ray Beam ExposureFIG. 2 Example of Conversion of X-Ray Intensity to Nickel DepositC 810 90 (2006)2Test Method C
21、 715. The wet results are then plotted versusX-ray count rate on linear graph paper and a smooth curvedrawn through the plotted points. The curve may be used toprepare a chart which lists count ranges for each increment of0.1 g/m2(0.01 g/ft2) nickel.9. Procedure9.1 Standardization of EquipmentInsert
22、 the referencestandard (6.4) which has a known X-ray count determinedwhen equipment was standardized, in the special sampleholder. After the equipment is warm, set the voltage to obtainX-ray counts characteristic of the reference standard.9.2 Nickel Determination:9.2.1 Inserta4by6-in. (10 by 152-mm)
23、 sample in thespecial sample holder (or cut a piece to fit a regular holder).9.2.2 Using an X-ray tube with suitable target, adjust thepower supply to provide 50 kV at 25 mA and set the scaler fora 10-s count. Align the spectrogoniometer to 48.65, 2-u anglefor nickel determination using a lithium fl
24、uoride crystal. Startthe apparatus and record the count from the counter scales.9.2.3 Repeat the determination on a minimum of two areason each side of each sample. Average the counts so recordedand read the nickel concentration from the standard plot.9.2.4 Specific details of operation of the X-ray
25、 apparatus arenot included herein due to the complexity of such equipmentand the slight variations in procedure between different typesof apparatus. These details can be provided by the manufac-turer.9.3 Verification of Standard Equipment After completingdeterminations of unknown samples, recheck th
26、e machinecalibration by reinserting the reference standard and checkingthe reading.10. Report10.1 Convert X-ray counts to grams per square metre byusing the calibration curve.NOTE 3The result in grams per square metre can be converted tograms per square foot by dividing by 11.11. Precision and Bias1
27、1.1 The precision and bias of this test method is beingestablished.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 validity of any
28、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 comments are inv
29、ited 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
30、 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. 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).C 810 90 (2006)3
