Lecture 1-Safety Proc in X-Ray

8/13/2019 Lecture 1-Safety Proc in X-Ray

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Safety Procedures in Irradiating Apparatus

(X-Ray Analyser)

Radiation Protection Course for Officers

Bangi Ray Services Sdn. Bhd.,

No. 24A Jalan 4!2A,

4"2## BAN$AR BAR% BAN&', Selangor


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Overview

Introduction

Basic principle of X-ray analyser

Components of X-ray analyser XRF: EDXRF and WDXRF

Eamples of XRF applications

XRD

Eamples of XRD applications

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"istory of X-ray

# 1895:Wil$elm Conrad

R%nt&endiscovers X-

rays' Receives first(o)el pri*e in +$ysics

for $is discovery

,./0'

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X-Ray

Ioni*in& radiation

In t$e form of electroma&netic waves

2end to travel t$rou&$ air and mostmedia

+enetrative t$rou&$ tissue and resulted

to eternal $a*ard

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()ray()ray

X-ray li4es &amma ray5 no c$ar&e5 no mass and also

electroma&netic radiation'

6enerated )y ener&etic electron processes

- 2$e )asic production of -ray is )y acceleratin& electrons in order to collide wit$ a metal tar&et ,tun&sten0'

- "ere t$e electrons suddenly de-accelerateupon collidin&

wit$ t$e metal tar&et5 and if enou&$ ener&y is contained

wit$in t$e electron5 it is a)le to 4noc4 out an electron from t$e inner s$ellof t$e metal atom and as a result electrons

from $i&$er ener&y levels t$en fill up t$e vacancyand -ray

p$oton are emitted'

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8

Production of X-ray

C$aracteristic -ray


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X-ray spectru

2$e X-rays produced w$en $i&$

velocity electrons stri4e t$e

tar&et material consist of:

9 2$e continuous or

Bremsstra$lun& spectrum9produced w$en electron

approac$es t$e nucleus

9 2$e c$aracteristic spectrum

9 produced as a result ofmovement of electrons from

t$e different s$ells


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X-ray spectrum as a function of applied voltage

!"# $ullity and S"R"Stoc%

5 kV

10 kV

15 kV

20 kV

25 kV

SWL Wavelength

X-rayintensity

$ontinuous spectru

&'

&

$aracteristic

spectru

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Basic +rinciples < 2ec$ni=ues

Interaction of X-ray wit$ >aterials:

+rocesses

?catterin&@)sorption

Diffraction

Ioni*ation

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!asic principles and tecni*ues:

W$en X-rays interact wit$ a material5 t$ey will

)e scattered5 a)sor)ed or diffracted' 2$e scattered X-rays can lose or c$an&e t$eir

ener&y after t$e interaction'

Diffraction is usually caused )y crystal latticeand it5 t$erefore5 occurs if t$e material involved

is of crystalline nature'

X-Ray Analy+ers

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saple

- soller slit

- analyser crystal

- detector

Scattering processes: scattering of te

X-ray tu,e spectru on te saple

Rayleig scattering

(elastic)

$opton scattering

(inelastic)


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@)sorption

&-Auant

-Auant

&-Auant

&

.-sell

/issionpoton/0citation

/lectron

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@)sorption

@)sorption $appens w$en electron in t$e inners$ell is eected and t$e empty position isreplaced )y electron from t$e outer s$ells

C$aracteristic ener&iesare released durin& t$isprocess

2$e c$aracteristic ener&y is used to identify t$eelement ,fin&er print0

@)sorption process is t$e )asic principle )e$indt$e XRF tec$ni=ue

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Diffraction

Diffractionis also a form ofscattered X-ray and it is caused

)y crystal lattice'

2$is occur w$en if t$e material

to )e analy*ed is crystalline in

nature

Diffraction can )e represented

)y Bra&&s aw

sin n 2d 2$is is t$e )asic principle of

XRD

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X-rays will )e diffracted )y t$e materials only if t$ey

satisfy t$e followin& relations$ip:

sin n sin - an&le of incident to t$e

!d tar&et material

d - inter-atom spacin& of t$e lattice

- -rays wavelen&t$and

n - an inte&er

2$e scattered X-rays are t$en measured to indicate t$elattice pattern of t$e material and t$is form t$e )asic

principle of X-rays diffraction ,XRD0'

X-Ray Analy+ers

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Basic Components of X-ray @nalyser

X-ray source

?ource $ousin&

X-ray detector

Electronic si&nal processor

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2ypes of X-ray ?ources

Coolid&e ,X-ray0 2u)e

Radioisotopes


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X-ray tu,es:Sceatic of old side-3indo3 tu,e

(e&ative $i&$ volta&e on t$e cat$ode

4 1//m Beryllium window

@node Coolin& water for anode

Electron )eam

cat$ode

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2$e X-Ray 2u)e

X-ray 6u,es9 7oltage deterines

3ic eleents can ,e

e0cited"9 .ore po3er lo3er

detection liits

9 $urrent deterines teintensity (ore counts,etter precision)

9 Anode selectiondeterines optialsource e0citation(application specific)

Introduction to XR

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X-ray ?ources: Radioisotopes

Isotope "alf-life Emission +refered element ran&e

-lines -lines

Fe-77 !' years >n X-rays ?i - G () - Ce

Cm-!33 '; years +u X-rays 2i 9 ?e a - +)

Cd-/. '1 years @& X-rays Cr 9 >o 2) - H

@m-!3 311 years 6ammarays

n - (d "f - H

!/


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Comparison )etween X-ray tu)e and

Radioisotope source

X-Ray 2u)e Radioisotope

Htility Re=uirements Electricity (one

@pplications XRF and XRD XRF only

Element ran&e Be 9 H

,at' no' 3 - .!0

imited dependin&on isotope

X-ray imitation ?$elf-life "alf-life

?afety Easily disposed Re=uires properdisposal procedure

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2u)e $ousin&

2$e -ray source is enclosed in a tu)e $ousin&

2$e tu)e $ousin& is used for minimi*in&radiation lea4a&e and to protect t$e source from

p$ysical dama&e For most -ray analysers5 tu)e $ousin& is

inte&rated wit$ detector and electronic si&nalprocessor

It is usually w$olly or partially enclosed ininterloc4ed )arriers or s$ield to provide furt$erprotection

!!


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X-ray detector

Detector converts t$e emitted ener&y into

series of electronic si&nal

2ype of detector depends on type of -rayanalyser e'&' ?emiconductor ,silicon0

detector5 proportional counter5 scintillation

counter5 etc'

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C$aracteristics of &ood detector

6ood sta)ility

Ru&&edness

Ener&y independence

"i&$ efficiency of detection

"i&$ resolvin& power ow cost

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Electronic si&nal processor:9 Consists of:

# "i&$ volta&e

# +reamplifier

# >ain amplifier

# Discriminator ,selector0

# ?caler J ratemeter

9 It is re=uired for:

# ?upplyin& $i&$ volta&e to t$e detector'# @mplifyin& t$e detectors si&nals to a suita)le level'

# Re&isterin&5 analy*in& and presentin& t$e detectors si&nals'


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Electronic components to support analyser or

detector system

Components includesK

"i&$ volta&e 9 supply volta&e to X-ray tu)e and

detector

+reamplifier and @mplifier 9 amplify si&nal detected

)y detector

Discriminator 9 select ri&$t pulse si*e of detector

output

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Components of X-ray analyser

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X-ray analysisis anot$er tec$ni=ue used in modern industryand researc$ for analy*in& materials or products'

It wor4s )ased on -rays produced )y an irradiatin&apparatus or a sealed radioactive source'

2$ey are availa)le eit$er in t$e form of: Enclosed devices +artly enclosed devices or Devices wit$out any enclosure

Enclosed or partly enclosed devices ensure no possi)ility ofinadvertent eposure to t$e -ray )eams'

Devices wit$out enclosure s$ould )e operated in a speciallydesi&ned and s$ielded eposure room'

X-Ray Analy+ers

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X-Ray Analyser (Irradiating Apparatus)

2$e XRF < XRD are t$e common -rayanalyser in industry and la)oratory

Hsed as testin& e=uipments for researc$ and

routine analysis Bot$ uses -ray as t$eir met$od of analysis

2$e -rays used are $a*ardous to wor4ers and

mem)ers of pu)lic

@ safety procedure is re=uired w$en usin&t$ese instruments

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@pplication of X-ray analy*er:

2$ere are two types of X-ray analy*er:

9X-ray fluorescence ,XRF0

9X-ray diffraction ,XRD0

X-Ray Analy+ers

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X-Ray Fluorescence ,XRF0

XRF is widely used in electronicindustry5 petroleum industry5 cementfactory5 tin smelters5 aircraftmaintenance and researc$ la)oratories

It is used to determine c$emical content

,=ualitative0 and composition,=uantitative0' @lso used to determineplatin& or coatin& t$ic4ness

?amples analysed include roc45mineral5 powder5 metal5 paper5 plastic5t$in film etc'

Basically t$ere are ! different types ofXRF: Ener&y-dispersive XRF andWavelen&t$-dispersive XRF

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Instrumentation XRF

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9 2wo types of XRF:

Ener&y-dispersive:

In ener&y-dispersive XRF5 identification of anelement is )y means of its ener&y line'

Wavelen&t$-dispersive: In t$e wavelen&t$-dispersive5 t$e element is

identified from its wavelen&t$ property'

X-Ray luorescence

11

I t d ti t XR


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2ypes of XRF: Ener&y-dispersive XRF

Introduction to XR

13


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Wavelen&t$-dispersive XRF

acuuseal

;5 3indo3

up to onoc$romator

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Comparison EDXRF < WDXRF/#XR =#XR

X-ray source andpower X-ray tu)e 7/5/// 9R>8//5///

R>//5/// 9R>5///5///

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@dvanta&es of XRF over conventional

tec$ni=ue

(on-destructive

>inimum sample preparation

Fast analysis Device is easy to use < user friendly

@vaila)le in porta)le form

It $as ecellent accuracy < precision

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Disadvanta&es of XRF

(ot suita)le for t$e analysis of very li&$telement ,e'&' "5 "e and i0

(ot as sensitive as some ot$er

tec$ni=ues e'&' Inductive Couple +lasma,IC+0 and (eutron activation analysis,(@@0 9 detection limit varies to t$eelements ,depends on atomic no'0

2$e device is 4nown to suffered frommatri effect

1;


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Eample of XRF @pplication : +recious >etals @nalysis

1.


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W$ic$ is t$e real &oldN

3/


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6old Reference ?tandards Hsed at

(uclear >alaysia

# ... ,..'.M @u0

# .7/ ,.7'/M @u0

# .8 ,.'8M @u0# ;7 ,;'7M @u0

# ;17 ,;1'7M @u0

# 7/ ,7'/M @u0

3!


43/77

Different 6old +urity )y EDXRF

# ?pectrum s$ows &old and

copper pea4s of t$e

different &old standards

# 2$e overlay Cu pea4ss$ow it increases as purity

of &old is lowers

# 6old pea4 increases wit$

increase in &old purity

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Cali)ration 6rap$ for 6old wit$ >atri

Correction 2ec$ni=ue

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@ccuracy of EDXRF @nalysis

Sample ire !ssay"ppt#

$%X&"ppt#

%ifference

'old (50 ()(*+ (),*, 0*05

'old (1 (15*+ (15*, 0*05

'old &ing1

(20*1 (1(*2 0*0(

'old &ing

2

(1,* (1,*) 0*02

'old.ecklace

(1/* (1/*+ 0*0+

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+recious >etal ?amples

# Fa4e 6old )ar

# >ade from copper5

*inc and nic4el

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Eample of XRF @pplication !: Coatin&

2$ic4ness >easurement

3.


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7/


51/77

Real ?ample

>ulian ?old @ec%lace

Pone $onnector

Pasar .ala ?old

@ec%lace

7

R lt f R l ? l


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Results for Real ?amples

?old @ec%lace fro Pasar .ala

?old @ec%lace >ulian

Pone $onnector

&eading 1 2 3 4 5 !verage hickness"m#

ntensity 10.3 17.7 12.2 12.2 17.7 1)*02 0*0)2,+/


ntensity 29.00 28.20 28.30 28.10 29.90 2,*/0 0*0,/(


ntensity 14.400 13.600 14.400 13.800 14.000 1)*0)0 0*0)2,(,

7!


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EDXRF ? t


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EDXRF ?pectrum

+t

+t

Fe

Fe

?pectrum:i&$t )lue /nm

coatin&

Red nm coatin&

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Recent development:

- >icrofocus XRF ,PXRF0

77

e'&' 9 to inspect inte&rated circuit < +CB

9 to inspect $i&$ =uality coatin& and welded material

A


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@pplication: Auality control

# Red-(i Blue-Cl 6reen - +)

78

ICXRI!//! 9 XRD Wor4s$op


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X-Ray Diffraction ,XRD0


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X-ray diffraction ,XRD0:

9 Hsed in t$e analysis to identify and =uantifycrystalline materials and crystallite si*e of t$ematerials'

9 It provides means to &at$er information on p$ysicalproperties of metals5 polymeric materials5 naturalproducts and ot$er solids'

9 Hsed in industry to analyse ceramic materials andores and in researc$ la)oratories for studies in&eolo&y5 p$ysics5 environment5 mineralo&y5metallur&y and c$emistry'

X-Ray Analy+ers

7;

XRD Instrument


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XRD Instrument

7.


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XRD: Instrumentation

8/


61/77

>atter in solid state

CrystallineAmorphous

Single crystal Polycrystalline

8

@tom arran&ed in re&ular form

@tom arran&ed in random

form e'&' &lass


62/77

Crystals

Ionic >olecular

8!

H i C ll


63/77

Hnit Cell

et us t$in4 of a very smallcrystal ,top0 of roc4salt,(aCl05 w$ic$ consists of/// unit cells'

Every unit cell ,)ottom0 $as

identical si*e and is formedin t$e same manner )yatoms'

It contains (aQ-cations , 0

and Cl-

-anions , 0' Eac$ ed&e is of t$e len&t$ a

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W$at information can )e derived from XRD

@n&ular pea4 position+osition S!2$etaT-/ -7 !/ !7 1/

Counts

/

7////

-/////

@lp$a-'RD

Peak position StructureIntensity (Height) QuantityFWHM Crystallite size !attice strain

FWHM

PEAKH

EIGHT

Integrate" peakIntensity

83

Determination of ?tressJ?train in sport rim


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Determination of ?tressJ?train in sport rim

and automotive components

Colla#oration $ith %r& %iana !a"os' Worcester PolytechnicInstitute 87


66/77

Position AB26)etaC15 25 45

$ountsDs

5

1555

2555

XRD of c$ocolate

#ar% $ocolate

Scan tie:

15 inutes

!y understanding te

structure of cocolateE it is

possi,le to#iproe te production

process

#preent ageing of

cocolate

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Identification @nalysis usin& searc$-matc$


68/77

Identification @nalysis usin& searc$-matc$

met$od wit$ ICDD +owder Diffraction File

Crystalline

6i))site5 @l,O"01

@morp$ous&amma alumina5

U-@l!O1

8;


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Auantitative analysis

@anosi+ed

particles

arge

particles

+$otocatalytic properties must )e suppressed5

to prevent dama&e of t$e or&anic matri V

use RH2IE p$ase

+articles must )e nano-si*ed and nota&&lomerate in t$e product to ensure

transparency

a

ar

a a

aa

a5 r

a5 r

r

a anatase 2iO!r rutile 2iO!

8.


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X-ray tu,es

2$e -ray tu)e is a vacuum tu)e in w$ic$ electronsare accelerated to a $i&$ velocity )y means ofelectrostatic field and t$en suddenly stopped )ycollision wit$ a tar&et'

Result of t$is collision5 -rays are emitted'

2o prevent -rays from )ecomin& a $a*ard andcreate scattered radiation5 t$e -ray tu)e is s$ieldedwit$ lead,t$e window remains uns$ielded0'

!

X t ,


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X-ray tu,es

2$e )asic components of a -ray tu)e are: a sealed &lass tu)e envelope5

a cat$ode5

an anode

-ray tu)e window

6arget (Anode)ilaent ($atode)

?lass tu,e enelopeX-ray tu,e 3indo3

1

X t ,


74/77

A sealed glass tu,e enelope:

>ade of &lass or metal-ceramic $avin& $i&$ meltin&point to wit$stand t$e intense $eat &enerated at t$eanode'

"i&$ vacuum environment: 2o prevent oidation of t$e electrode materialsK

2o permit ready passa&e of t$e electron )eam wit$outionisation of &as wit$in t$e tu)eK and

2o provide electrical insulation )etween t$e electrodes'

X-ray tu,es

3

X t ,


75/77

A catode: Cat$ode incorporates focusin& cup and filament'

Focusin& cup acts as a lens to direct t$e electrons in a )eamtowards t$e anode'

Filament is $eated )y @C current from a separately controlledtransformer'

@ c$an&e in t$e volta&e ,4G0 applied to t$e filament varies t$efilament current ,in @0 and t$e num)er of electrons emitted'

Current passin& )etween t$e cat$ode and anode )y means oft$e $i&$-speed electrons5 called tu)e current ,in m@0'

X-ray tu,es

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0-ray tu,e 3indo3:

2$e tu)e $as a window desi&ned for escape of t$e&enerated X-ray p$otons

X-ray tu,es

Documents

Lecture 1-Safety Proc in X-Ray