KS D ISO 16592-2011 Microbeam analysis－Electron probe microanalysis－Guidelines for determining the carbon content of steels using a calibration curve method《微光束分析 电子探针显微分析 用校准曲线法测定.pdf

1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS D ISO 16592 KS D ISO 16592:2011 2011 11 28 http:/www.kats.go.krKS D ISO 16592:2011 : ( ) ( ) ( ) : () () : (http:/www.standard.go.kr) ： ：2011 11 28 2011-0525 ： ： ( 02-509-7274) (http:/www.kats.go.kr). 10 5 , . KS D ISO 16592:2011 i . ii 1 1 2 1 2.1 .1 2.2

2、 .1 2.3 2 2.4 K X 2 2.5 (background subtraction)3 2.6 4 3 .5 4 .6 A( ) 7 B( ) 9 10 KS D ISO 16592:2011 ii 2006 1 ISO 16592, Microbeam analysis Electron probe microanalysisGuidelines for determining the carbon content of steels using a calibration curve method , . KS D ISO 16592:2011 Microbeam analys

3、is Electron probe microanalysis Guidelines for determining the carbon content of steels using a calibration curve method 1 ( 1 % 2 % ) . , X , , . 1.0 % . . X X . 2 2.1 . . . C K , , , , (point counting mode), , . 2.2 . . (austenite) Fe-C . . Fe-C Fe3C1KS D ISO 16592:2011 2 C K . 2.3 2.3.1 . . ( , ,

4、 ) . 2.3.2 . . , , . , (smearing) . 2.3.3 , , . , . . . 2.4 K X 2.4.1 X , C K . C K X . X X ( 1 ). X . 6 keV2 , C K X 10 keV 15 keV . X . . . (normalization) . KS D ISO 16592:2011 3 X (keV) Y C K (cps/nA) 1 C K ( 2 ) 2.4.2 (counting time) EPMA . ( .) . 1 , . . 2 , , , . 2 . 2.4.3 (PHA) PHA C K . Fe3

5、C PHA . 2.4.4 (crystal) C K . , d( )- , . 2.5 (background subtraction) KS D ISO 16592:2011 4 . . , C K 2 5 X . 5 , (A), (B), X (C), (D) . C K . X Y C K 1 2 3 (B) 4 (A) 5 (D) 6 X (C) 2 C K X (C) . (A) (B) , . (A) (B) C K . C K 0 X . , . 2.6 KS D ISO 16592:2011 5 3 C K . 0 1.0 % C K , (1) . iiCbbI10+=

6、(1) Ii ： X Ci ： b0 ： b1 ： b0 b1 ( A ) . , 0 0 . . X (%) Y C K (cps/nA) 1 C K 2 X C K 3 C K b1 3 3 KS D ISO 16592:2011 6 . . , . . . , , , , . . . . . . (CRM) . . . A3, 4 . / . B . 4 KS Q ISO/IEC 17025 5.10 . a) b) , c) , d) e) f) (take-off angle) g) , h) i) j) k) l) (crystal) m) PHA n) C K o) p) q)

7、, , (： ) r) s) KS D ISO 16592:2011 7 A ( ) . C K . EPMA X . . iiCbbI10+=(A.1) Ii ： X Ci ： b0 ： b1 ： uc(y) ( y x1, x2,.xn )( 3 4 ). ),()()(2)(),(),(11122111212c jijijNiNijiiNjijijNiNjixxrxuxuxyxyxuxyxxuxyxyxxyu+=+=L(A.2) )jixxr ,( . u(CS) . 10SSbbIC)( = (A.3)() () () () ()()( )+=210S1010122210S021S21

8、S2,211bbIbbrbubububbIbubIubCu22() () () ()()( )+=21S10101221S0221S221,211bCbbrbubububCbubIub() () () ()()( )1010S122S02S221,21bbrbubuCbuCbuIub+= (A.4)()( )10120210,),(, bbr bubu b b 5. KS D ISO 16592:2011 8 =niniiiiiiniiiniiiCCICID1b11221222-10=niniiiiiniiiiniiCICI1D1b112212121- 212122121=niiiniiini

9、iCCD - () =niiiCDbu122021() =niiDbu121211()=niniiiiniiiCCbbr1122212101, - b0 ： b1 ： n ： CS ： IS ： X i2 ： Ii Ii ： X Ci ： KS D ISO 16592:2011 9 B ( ) . 0.089 %, 0.188 %, 0.281 %, 0.460 %, 0.680 % 5 . 5 C K 5 , B.1 . B.1 C K ： % 1 2 3 4 5 0.089 7 842 7 908 7 806 7 956 7 896 7 882 58.6 0.188 9 360 9 168

10、 9 240 9 396 9 342 9 301 94.3 0.281 10 158 10 230 10 380 10 182 10 218 10 234 86.7 0.460 12 612 12 552 12 546 12 930 12 480 12 624 177.3 0.680 14 730 15 012 14 868 14 736 14 562 14 782 168.5 12 372 12 006 12 180 12 186 183.1 A . b0 6 882 b1 11 948 u(b0) 66.87 u(b1) 260.46 r(b0, b1) 0.794 X (IS) 12 1

11、86 , . % 0.44 948 11882) 6 186 (12S=-C u(CS) . ),()()(2)()()(1)(1010S122S02S221S2bbrbubuCbuCbuIubCu += 0.794)(260.4666.870.442260.460.4466.87183.1)948111( 22222-+= 273 0.000 = u2(IS) 183.12 ( X ) u(CS) 0.017 % KS D ISO 16592:2011 10 1 SAUNDERS, S.R.J., KARDUCK, P. and SLOOF, W.G. Certified reference

12、 Materials for Micro-Analysis of Carbon and Nitrogen, Microchimica Acta, 145, 2004, pp. 209-213 2 BASTIN, G.F. and HEIJLINGERS, H.J.M. Quantitative Electron Probe Microanalysis of Carbon in Binary Carbides. University of Eindhoven, The Netherlands, 1990 3 ELLISON, S.L.R., ROSSLEIN, M. and Williams,

13、A. Quantifying Uncertainty in Analytical Measurement, 2nd edn, EURACHE/CITAC Guide, 2000 4 Guide to the Expression of Uncertainty in Measurement, BIPM, IEC, IFCC, ISO, IUPAC, IUPAP, OIML, 1993 (corrected and reprinted 1995) 5 TAYLOR, J.R. An Introduction to Error Analysis, University Science Books,

14、1982 6 SCOTT, V.D., LOVE, G. and REED, S.J.B. Quantitative Electron Probe Microanalysis,. 2nd edn, Ellis Horwood, London, 1995 7 DUERR, J.S. and OGILVIE, R.E. Electron Probe Microdetermination of Carbon in Ferrous Alloys. Analytical Chemistry, 1972, 44, No.14, pp. 2361-2367 8 KS A ISO 5725 6, ( ) 6：

15、 9 KS D ISO 14594, 10 KS D ISO 14595, 11 ISO 17470, Microbeam analysis Electron probe microanalysis Guidelines for qualitative point analysis by wavelength dispersive X-ray spectrometry 12 ISO 22309, Microbeam analysis Quantitative analysis using energy-dispersive spectrometry (EDS) 13 KS D ISO 2383

16、3, 14 KS Q ISO/IEC 17025, 153787 1 92 3(13) (02)26240114 (02)262401489 http:/ Korean Agency for Technology and Standards http:/www.kats.go.kr KS D ISO 16592:2011 KSKSKS SKSKS KSKS SKS KS SKS KSKS SKSKS KSKSKS Microbeam analysisElectron probe microanalysisGuidelines for determining the carbon content of steels using a calibration curve method ICS 71.040.50