1、 1 ASTM :D 7039 04 1 D 7039;,.().1.1.1 ,2/500/(MWDXRF).,1.1 1.2.(PLOQ)4/.1 ,-.1.2 ,1.,(5).1.3 500/(.5.2).(15).1.4 ,5.1.5,.,.1.6 ,.1 D02 ASTM D02.03 .01 2004.2004.2 2.2.1 ASTM2:D 4057 .D 4177 .D 6299 .D 6300 .3.3.1 ,-,(.1).0.5373 (5.373)().()(/).,/,(WDXRF)3.(.,.,).1 (MWDXRF)2 ASTM ASTM www.astm.org s
2、erviceastm.org.ASTM ASTM .3 Bertin,E.P.,Principles and Practices of X-ray Spectrometric Analysis,Plenum Press,New York,1975,pp.115-118(.Plenum Press,-,1975,.115-118).3 4.4.1 .4.2 ,.4.3 ,.5.,5.1 .,-,.();1.,0.98 1.04.,2002,.,0.98 1.04.,.2 86%14%,C/H 5.4 8.5.2.3%(12%MTBE)/.5.2 ,.,.5.2.1 2.2.4-(),.5.2.2
3、,.4 /,%.2 /6.6.1 (MWDXRF)4,0.5373 (5.373).,15.6.1.1 ;.25,Rh L,Pd L,Ag L,Ti K,Sc K Cr K.6.1.2 ;.6.1.3 ;.2.7 (20).,.6.1.4 ;.6.1.5;.6.1.6 ;.4 ,X-ray Optical Systems,Inc.,15 Tech Valley Drive,East Greenbush,NY 12061.,ASTM International.,./,5 6.1.7 ;,(MWDXRF),(.6.1.8)5.6.1.8 ;(.6.1.7),.,.,.7.7.1 .,5.,.7.
4、2 ;.,.7.3-,.7.4 (),(.10.4,11.1 12.1).,.(RSD)1%(.1).2 .,.3 .7.4.1 ,.5,American Chemical Society,Washington,DC.,.,BDH Ltd.,Poole,Dorset,U.K.,U.S.Pharmaceutical Convention,Inc.(USPC),Rockville,MD.6 7.5 (QC),(.14).,.4 (QC).5 (QC).7.6 ,.7.7,99.9%,.8.8.1 ,D 4057 D 4177.8.2 ,.0 4.,.8.3 .,(,).,.(.7.2).-.8.4
5、 ,(.7.2).9.9.1 ,(MWDXRF).7 9.1.1 (T).9.1.2,1.9.2 :9.2.1 .5,.,.9.2.2 .,(,).,.9.2.3 ,.9.2.4 .,.10.10.1 ,(500/)-(.5.2).,.(/).10.2 11.2 ().(RS)()()()(.9.1.1 9.1.2).10.3 :10.3.1 ,10.3.2 .:RS=Y+(E x S)(1):RS=,.10.2,;Y=y ,;E=,-1-1;S=,/.10.4 ,.RS 8 .RS,2 12.1.10.5 (.7.2).,.,.11.11.1 ,.,RS;RS 2 12.1 11.2 :11
6、.2.1 9.2.11.2.2 ,.11.2.3 RS.11.3 RS ,.,.,11.2 .11.4 12.12.12.1 (F),2.,F 1.F=A/B(2):A=RS ,(10.4);B=RS ,(11.1).12.2 (Rcor):Rcor=F x RS(3):F=,2;RS=.9 12.3 (S),(Rcor)RS 1 10.3.12.4 ,.(So):So=Sd x(Mo+Mb)/Mo Sb x(Mb/Mo)(4):Sd =(12.3),/;Mo=,;Mb=,;Sb =,/.13.13.1 12 /,0.1/100/1/100/.,D 7039.14.14.1 (.7.5).14
7、.2 /(QC/QA),.14.3 QC/QA ,2.15.6 15.1 ,(.6)D 6300,:15.1.1 ,:(r)=0.555 X0.5 :(r)=0.54 X0.496 /.1 .15.1.2 .6 2002 .().6 ,RR:D02-1552 ASTM International.10 .1 2 0.8 0.8 5 1.2 1.2 10 1.8 1.7 20 2.5 2.4 50 3.9 3.8 100 5.6 5.3 200 7.8 7.5 500 12.4 11.8 15.2 .16.16.1;(MWDXRF);,;.()1 1.1 7(),1.1.,1.cal ,test
8、 .C=0test+StestG/0cal+ScalG(1.1):0=0XC+0OXO+0HXH(A1.2)S=198.3XC+468.3XO+0.58XH(A1.3)G=,.G ;(.1)G=0.87;0=(2/)(0);S=(2/)=0.5373;7 Goldstein,J.I.,et al.,Scanning Electron Microscopy and X-ray Microanalysis,Plenum Press,New York,1992,pp.743-777(.,Plenum Press,-,1992,.743-777).11 0=(2/)(=14.8 Cr K)0O=(2/
9、)(=37.7 Cr K)0H=(2/)(=0.34 Cr K)XC=;XO=;XH=.1.2 (RC):RC=C x RS(1.4):RC=;=,1.1;RS=.1.3 (S),(1.4)1(.10.3).1.4.2 .C/H 5 10 0 3.0%.1.1 /=6.2,.()1.1.1 8,().1.0%(%RSD),(.1.3).1.2 (RSD)=100 RS RB.(RSD):%RSD=100T-0.5(RS+RB)0.5/(RS RB)(1.1):RS=,;RB=,(.1.2.2).1.2.1 RS,.y(Y)(.10.3.2)RB 1.1.8 Bertin,E.P.,Princi
10、ples and Practices of X-ray Spectrometric Analysis,Plenum Press,New York,1975,pp.472-500(.Plenum Press,-,1975,.472-500).12 1.2.2 ,.1.2.3 ,RB ,.,RB ,y RB 1.1.1.3 ,.,.2.2.1 (QC).2.1.1 (QC).(QC).2.1.2 (QC),.(QC).(QC),.,(QC).2.2 (QC).D 6299 MNL-7A9 (QC).2.2.1 (QC)15 ,.2.2.2 ,().2.2.3 ,(QC).,.,.9 ,ASTM MNL 7A,ASTM International.13,.,.(ASTM).,.,.ASTM International.100 Barr Harbor Drive,West Conshohocken,PA 19428-2959,United States.()ASTM 610-832-9585 610-832-9555 :serviceastm.org ASTM(http:/www.astm.org).