Handbook of X-Ray Spectrometry Methods and Techniques

8/18/2019 Handbook of X-Ray Spectrometry Methods and Techniques

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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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VIII

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


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 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 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

Documents

Handbook of X-Ray Spectrometry Methods and Techniques