handbook of x-ray spectrometry methods and techniques
TRANSCRIPT
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H andbook of
X - R a y S p e c t ro m e t ry
Methods and Techniques
edited by
Rene E Van Grieken
Department of Chemistry
University ofAntwerp
Antwerp Belgium
Andrzej A Markowicz
Institute of Physics and Nuclear Techniques
Academ y of Mining and Metallurgy
racow
Poland
Marce l Dekk er In c.
New York • Basel • H o n g Kon g
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Contents
Preface iii
Contributors xiii
1 X ray Physics
Andrzej A Markowicz 1
I. Intro duc t ion 1
I I . Histo ry 1
III.
Genera l Fea tu res 2
IV. Em ission of Co ntinu ous Radiat ion 3
V. Em ission of Ch aracteris t ic X-ray s 8
V I. Interac t ion of Pho tons with M atter 17
V II .
Intensi ty of Ch aracteris t ic X-rays 30
VIII . IU PA C No ta t ion for X-ray Spec t roscopy 33
Appendixes
I . Cri t ica l A bsor pt ion W aveleng ths and Cri t ica l Ab sorp t ion Ene rgies 35
I I . Ch aracter is t ic X-ray W avelen gths A) and En ergies keV) 37
I I I .
Rad iat ive Tran si t ion Probabi l i t ies 49
IV. W aveleng ths of K Satelli te Lin es Ä) 52
V. Flu ore scen ce Yields and Co ster-K ronig Transi t ion Probabi l i t ies 54
V I. Coeffic ients for Calcula t ing the Pho toelectr ic Abs orpt io n
Cross Sec t ions T Barns /Atom) Via LN -L N Represen ta t ion 59
vii
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Contents
VII . Coefficients for Calcu lating the In coh ere nt Collision
Cross Sec t ions
T
Barns /Atom) Via the LN -L N Represen ta t ion 65
VIII .
Coefficients for Calcula t ing the Co heren t Scat tering
Cross Sec t ions u
R
Barns /Atom) Via the LN -L N Represen ta t ion 67
IX . To tal M ass Atte nua t ion Coeffic ients for Lo w -En ergy Line s 69
X. Co rrespo nde nce Be tw een Old S iegbahn and N ew IUPA C
No ta t ion X-ray Diagram Lines 71
References 71
2 W avelength Dispersive X ray Fluorescence 75
J A H eisen and Andrzej Kuczumow
I . Intro duc t ion 75
II . Fun dam enta l s of Wav e length Dispers ion 78
III .
Lay out of a Spec t ro mete r 82
IV . Qu al i ta t ive and Qu anti ta t ive An alysis 117
V. Ch em ical Shift and Sp eciatio n 134
V I.
Instr um enta t ion 138
References 145
3 Energy Dispersive X ray Fluorescence Analysis Using X ray
Tube Excitation 151
Joseph M Jaklevic and Robert D Giauque
I.
Intro du ct ion 151
I I . Sem iconduc to r De tec to rs for X-ray Spec t rom et ry 152
I I I . Typica l X-ray Tub e Exc i ta t ion Sys tems for ED X RF 168
IV. App l ica tions of Tub e-Exc i ted ED X RF 175
V. Sum ma ry 179
References 179
4 Spectrum Evaluation 181
Pierre J M Van Espen and Koen H A Janssens
I . Intro du ct ion 181
IL Fun dam enta l Asp ec ts 182
I I I .
Spec t rum Process ing M ethods 187
IV. Backg round Es t imat ion M ethods 205
V. Simple N et Peak A rea De term inat ion 213
V I.
Le ast-S qu ares Fi t t ing Using Reference Spe ctra 217
VII . Le ast- Sq uar es Fi t t ing Using Ana lyt ical Fun ct ions 222
VIII . M ethods Based on the M onte Car lo Technique 254
IX. Leas t -Squ ares F i t ting M ethod 258
X. Co mp ute r Imp lementa t ion of Var ious Algor i thms 268
References 291
5 Qu antification by XR F An alysis of Infinitely Thick Sam ples 295
/ . L de Vries and Bruno A R Vrebos
I.
Corre la t ion Be tw een In tens i t ie s and Con cent ra t ion 295
II . Fa cto rs Influencing the Ac cura cy of the Intensi ty M easu rem ent 300
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Contents
ix
III. Rem arks on Sample Prepara t ion 308
IV . Co nvert ing Intensi t ies to Co ncen tra t ion 309
V. Co nclusion 336
References 337
Sugg est ions for Fu rth er Readin g 338
6 Quan tification in XRF Analysis of Intermediate Thickness Sam ples 339
Andrzej A Markowicz and Rene E Van G rieken
I . Intro du ct ion 339
II . Em iss ion-Transmiss ion Method 340
I I I . Abso rpt ion Correc t ion M ethods v ia Sca t te red Pr imary Radia t ion 344
IV. Quant i ta t ion for In te rmedia te -Thickn ess Granulä r Spec imen s 350
References 357
7 Radioisotope X ray Analysis 359
John S Watt
I. Intro duc t ion 359
I I . Basic Eq uat io ns 360
I I I . Rad ioisoto pe X-ray Sou rces and D etector s 367
IV . X-r ay and -y-ray Te chn iqu es 377
V. Cho ice of X-ray Tec hniq ue for a Specific App licat ion 390
V I.
Ap plicat ions 391
VII . Con c lus ions 407
References 407
8 Synchro tron Radiation Induced X ray Em ission 411
Keith W Jones
I. In t rodu c t ion 411
II . Pro pert ies of Sy nch rotro n Rad iat ion 413
I I I .
De script ion of Syn chro tron Faci l i ties 416
IV. Ap para tus for X-ray M icroscopy 418
V. Cont inuu m and M onoch rom at ic Exc i ta t ion 427
V I. Qu anti ta t ion 428
VII .
Sensi t ivi t ies and Minim um De tect ion Lim its 432
VIII . Beam -Induced Dam age 434
IX. Ap plicat ions of SR IX E 437
X. Tom ograph y 443
X I. E X A F S a nd X A N E S 4 44
XII .
Fu ture Direct ion s 448
References 449
9 Total Reflection XRF 453
Heinrich Schwenke and Joachim Knoth
I . Intro duc t ion 453
II. Ph ysics of To tal Reflection of X -rays 454
III . Design of Ins trum ents 458
IV. An alysis of Small Qu ant i t ies on Reflecting Carrier s 463
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Contents
V . Surface An alysis 474
V I. R o l e o f T X R F 488
References 488
10 Polarized Beam X ray Fluorescence 491
Richard W Ryon and John D Zahrt
I . Intro duc t ion 491
I I . Barkla Sys tem s 497
I I I .
Bragg Sy stem s 506
IV . Syn chro tron Radiat ion 510
V. Resul t s and Exa mp les 510
V I. Con clusion 511
Ap pend ix: Cry sta ls That Diffract Selected Chara cteris t ic W aveleng ths
a t2 9 = n/2 = 90° 512
References 515
11 Particle Induced X ray Emission Analysis 517
Willy Maenhaut and Klas G Malmqvist
I.
Intro duc t ion 517
I I . Inter act ion s of Charg ed Part ic les with M atter , Characteris t ic
X-ray Produ c t ion , and Cont inuous Photon Background Produc t ion 519
I I I . Ins t rum enta t ion 526
IV . Qu anti ta t ion, De tect ion Lim its , Ac cura cy, and Precision 538
V. Sam ple Collect ion and Sam ple and Specim en Preparat ion
for PIX E An alysis 548
V I.
Ap plicat ions 550
V II .
Com plemen ta ry Ion Beam Analys i s Techniques 565
VI II . Con clusions 571
References 574
12 Electron Induced X ray Emission 583
John A Small
I . Intro duc t ion 583
I I . Qu anti ta t ive An alysis 587
I I I . Qu anti ta t ive An alysis of Thin Specim ens 616
IV . Qu anti ta t ive An alysis of Part ic les and Roug h Surfaces 621
V. Spat ia lly Reso lved X-ray Analysis 635
References 652
13 Sample Preparation for XRF 657
Jasna Injuk and Rene E Van G rieken
I.
Intro duc t ion 657
I I . Solid Sam ples 658
I I I . Fus ed Spec imen s 665
IV. Liquid Sam ples 669
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V. Biological Sam ples 676
VI.
Atm ospheric Particles 682
VII. Sample Support M aterials 685
References 687
Index
693