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
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

!
"istory of X-ray
#
1895: Wil$elm Conrad
R%nt&en discovers X-
rays' Receives first
(o)el pri*e in +$ysics
for $is discovery
,-./-0'
1
X-Ray

Ioni*in& radiation

In t$e form of electroma&netic waves

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

media

+enetrative t$rou&$ tissue and resulted

to eternal $a*ard
3
()ray
()ray
X-ray li4es &amma ray5 no c$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$e electrons suddenly de-accelerate upon collidin&
wit$ 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$e inner s$ell of t$e metal atom and as a result electrons
from $i&$er ener&y levels t$en fill up t$e vacancy and -ray
p$oton are emitted'
7
8
Production of X-ray
C$aracteristic -ray
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$lun& spectrum 9
produced w$en electron
approac$es t$e nucleus
9
2$e c$aracteristic spectrum
9 produced as a result of
movement of electrons from
t$e different s$ells
:
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
-
r
a
y

i
n
t
e
n
s
i
t
y
$ontinuous spectru
&
'
&
(
$)aracteristic
spectru
;
Basic +rinciples < 2ec$ni=ues
Interaction of X-ray wit$ >aterials:
+rocesses
O
?catterin&
O
@)sorption
O
Diffraction
O
Ioni*ation
.
+
!asic principles and tec)ni*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 lattice

and it5 t$erefore5 occurs if t$e material involved
is of crystalline nature'
X-Ray Analy+ers
X-Ray Analy+ers
-/
saple
- soller slit
- analyser crystal
- detector
Scattering processes: scattering of t)e
X-ray tu,e spectru on t)e saple
Rayleig) scattering
(elastic)
$opton scattering
(inelastic)
--
@)sorption
&-Auant
--Auant
&-Auant
&
-
.-s)ell
/ission
p)oton
/0citation
/lectron
-!
@)sorption

@)sorption $appens w$en electron in t$e inner

s$ell is eBected and t$e empty position is
replaced )y electron from t$e outer s$ells

C$aracteristic ener&ies are released durin& t$is

process

2$e c$aracteristic ener&y is used to identify t$e

element ,fin&er print0

@)sorption process is t$e )asic principle )e$ind

t$e XRF tec$ni=ue
-1
Diffraction

Diffraction is also a form of

scattered 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&&Cs Daw
sin = n1
2d

2$is is t$e )asic principle of

XRD
-3

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

satisfy t$e followin& relations$ip:
sin E 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$e

lattice pattern of t$e material and t$is form t$e )asic
principle of X-rays diffraction ,XRD0'
X-Ray Analy+ers
X-Ray Analy+ers
-7
Basic Components of X-ray @nalyser

X-ray source

?ource $ousin&

X-ray detector

Electronic si&nal processor

-8
2ypes of X-ray ?ources

Coolid&e ,X-ray0 2u)e

Radioisotopes
-:
X-ray tu,es:
Sc)eatic of old side-3indo3 tu,e
(e&ative $i&$ volta&e on t$e cat$ode
455
1//m Beryllium window
@node
Coolin& water for anode
Electron )eam
cat$ode
-;
2$e X-Ray 2u)e

X-ray 6u,es
9 7oltage deterines
3)ic) eleents can ,e
e0cited"
9 .ore po3er 8 lo3er
detection liits
9 $urrent deterines t)e
intensity (ore counts
,etter precision)
9 Anode selection
deterines optial
source e0citation
(application specific)
Introduction to XR9
-.
X-ray ?ources: Radioisotopes
Isotope "alf-life Emission +refered element ran&e
F-lines D-lines
Fe-77 !': years >n F X-
rays
?i - G () - Ce
Cm-!33 -:'; years +u D X-rays 2i 9 ?e Da - +)
Cd--/. -'1 years @& F X-rays Cr 9 >o 2) - H
@m-!3- 311 years 6amma
rays
In - (d "f - H
!/
Comparison )etween X-ray tu)e and
Radioisotope source
X-Ray 2u)e Radioisotope
Htility Re=uirements Electricity (one
@pplications XRF and XRD XRF only
Element ran&e Be 9 H
,at' no' 3 - .!0
Dimited dependin&
on isotope
X-ray Dimitation ?$elf-life "alf-life
?afety Easily disposed Re=uires proper
disposal procedure
!-
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&nal
processor

It is usually w$olly or partially enclosed in

interloc4ed )arriers or s$ield to provide furt$er
protection
!!
X-ray detector

Detector converts t$e emitted ener&y into

series of electronic si&nal

2ype of detector depends on type of -ray

analyser e'&' ?emiconductor ,silicon0
detector5 proportional counter5 scintillation
counter5 etc'
!1
C$aracteristics of &ood detector

6ood sta)ility

Ru&&edness

Ener&y independence

"i&$ efficiency of detection

"i&$ resolvin& power

Dow cost
!3

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 detectorCs si&nals to a suita)le level'
# Re&isterin&5 analy*in& and presentin& t$e detectorCs si&nals'
Electronic si&nal processor
Electronic si&nal processor
!7

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
!8
Electronic si&nal processor
Electronic si&nal processor
Components of X-ray analyser
!:
+
X-ray analysis is anot$er tec$ni=ue used in modern industry
and 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 of
inadvertent eposure to t$e -ray )eams'
+
Devices wit$out enclosure s$ould )e operated in a specially
desi&ned and s$ielded eposure room'
X-Ray Analy+ers
X-Ray Analy+ers
!;
X-Ray Analyser (Irradiating Apparatus)

2$e XRF < XRD are t$e common -ray

analyser 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
!.
+
@pplication of X-ray analy*er:

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

9
X-ray fluorescence ,XRF0
9
X-ray diffraction ,XRD0
X-Ray Analy+ers
X-Ray Analy+ers
1/
X-Ray Fluorescence ,XRF0

XRF is widely used in electronic

industry5 petroleum industry5 cement
factory5 tin smelters5 aircraft
maintenance and researc$ la)oratories

It is used to determine c$emical content

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

?amples analysed include roc45

mineral5 powder5 metal5 paper5 plastic5
t$in film etc'

Basically t$ere are ! different types of

XRF: Ener&y-dispersive XRF and
Wavelen&t$-dispersive XRF
1-
Instrumentation XRF
1!
9
2wo types of XRF:

Ener&y-dispersive:
In ener&y-dispersive XRF5 identification of an
element 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 9luorescence
X-Ray 9luorescence
11
2ypes of XRF: Ener&y-dispersive XRF
Introduction to XR9
13
Wavelen&t$-dispersive XRF
:acuu
seal
;5
3indo3
up to <
colliators
S$
FC
?ample in measurin& position (et sample waitin&
>onoc$romator
17
Comparison EDXRF < WDXRF
/#XR9 =#XR9
X-ray source and
power
X-ray tu)e <
radioisotope5 low power
X-ray tu)e5 $i&$ power
Element identification
scale
Ener&y ,FeG0 Wavelen&t$ ,!L0
Concentration ran&e -/ppm--//M -ppm--//M
Di&$t element detection
,B5 C5 (5 O5 F0
Bad 6ood
?i*e of instrument ?mall and porta)le Dar&e mainly as Da)
instrument
@pplications Industry and researc$ 6eolo&ical5 researc$
and industry
Cost R>-7/5/// 9
R>8//5///
R>://5/// 9
R>-5///5///
18
@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

1:
Disadvanta&es of XRF

(ot suita)le for t$e analysis of very li&$t

element ,e'&' "5 "e and Di0

(ot as sensitive as some ot$er

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

2$e device is 4nown to suffered from

matri effect
1;
Eample of XRF @pplication -: +recious >etals @nalysis
1.
W$ic$ is t$e real &oldN
3/
3-
6old Reference ?tandards Hsed at
(uclear >alaysia
# ... ,..'.M @u0
# .7/ ,.7'/M @u0
# .-8 ,.-'8M @u0
# ;:7 ,;:'7M @u0
# ;17 ,;1'7M @u0
# :7/ ,:7'/M @u0
3!
Different 6old +urity )y EDXRF
#
?pectrum s$ows &old and
copper pea4s of t$e
different &old standards
#
2$e overlay Cu pea4s
s$ow it increases as purity
of &old is lowers
#
6old pea4 increases wit$
increase in &old purity
31
Cali)ration 6rap$ for 6old wit$ >atri
Correction 2ec$ni=ue
33
@ccuracy of EDXRF @nalysis
Sample ire !ssay
"ppt#
$%X&
"ppt#
%ifference
'old (50 ()(*+ (),*, 0*05
'old (1- (15*+ (15*, 0*05
'old &ing
1
(20*1 (1(*2 0*0(
'old &ing
2
(1,*- (1,*) 0*02
'old
.ecklace
(1/*- (1/*+ 0*0+
37
C+recious >etalC ?amples
#
Fa4e 6old )ar
#
>ade from copper5
*inc and nic4el
38
+latinum
#
..'..M +latinum )ar sold in t$e
local mar4et at discounted price
#
+latinum mar4eted as product
of Oo$son >attey5 ?oe4arno
platinum and also ?wiss Ban4
3:
#
@nalysis of t$ese platinum samples
s$ows t$at it is a 1-8 stainless steel wit$
no platinum
+latinum spectrum ?tainless steel 1-8 spectrum
3;
Eample of XRF @pplication !: Coatin&
2$ic4ness >easurement

3.
7/
Real ?ample
>)ulian ?old @ec%lace
P)one $onnector
Pasar .ala ?old
@ec%lace
7-
Results for Real ?amples
?old @ec%lace fro Pasar .ala
?old @ec%lace >ulian
P)one $onnector
&eading 1 2 3 4 5 !verage 0hickness
"1m#
2ntensity 10.3 17.7 12.2 12.2 17.7 1)*02 0*0)2,+/
&eading 1 2 3 4 5 !verage 0hickness
"1m#
2ntensity 29.00 28.20 28.30 28.10 29.90 2,*/0 0*0,/-(
&eading 1 2 3 4 5 !verage 0hickness
"1m#
2ntensity 14.400 13.600 14.400 13.800 14.000 1)*0)0 0*0)2,(,
7!
Can EDXRF determine (ano Coatin& N
+t-Fe coated on &lass
- Coatin& t$ic4ness measured )y ?E>
71
EDXRF ?pectrum
+t
+t
Fe
Fe
?pectrum:
Di&$t )lue E :/nm
coatin&
Red E -:nm coatin&
73
Recent development:
- >icrofocus XRF ,PXRF0
77
e'&' 9 to inspect inte&rated circuit < +CB
9 to inspect $i&$ =uality coatin& and welded material
@pplication: Auality control
# Red-(i Blue-Cl 6reen - +)
78
ICXRI!//! 9 XRD Wor4s$op
X-Ray Diffraction ,XRD0

X-ray diffraction ,XRD0:

9
Hsed in t$e analysis to identify and =uantify
crystalline materials and crystallite si*e of t$e
materials'
9
It provides means to &at$er information on p$ysical
properties of metals5 polymeric materials5 natural
products and ot$er solids'
9
Hsed in industry to analyse ceramic materials and
ores and in researc$ la)oratories for studies in
&eolo&y5 p$ysics5 environment5 mineralo&y5
metallur&y and c$emistry'
X-Ray Analy+ers
X-Ray Analy+ers
7;
XRD Instrument
7.
XRD: Instrumentation
8/
>atter in solid state
Crystalline
Amorphous
Single crystal
Polycrystalline
8-
@tom arran&ed in re&ular form
@tom arran&ed in random
form e'&' &lass
Crystals
Ionic >olecular
8!
Hnit Cell

Det us t$in4 of a very small

crystal ,top0 of roc4salt
,(aCl05 w$ic$ consists of
-/-/-/ unit cells'

Every unit cell ,)ottom0 $as

identical si*e and is formed
in t$e same manner )y
atoms'

It contains (a
Q
-cations , 0
and Cl
-
-anions , 0'

Eac$ ed&e is of t$e len&t$ a

81
W$at information can )e derived from XRD
@n&ular pea4 position
+osition RS!2$etaT
-/ -7 !/ !7 1/
Counts
/
7////
-/////
@lp$a-'RD
Peak position Structure
Intensity (Height) Quantity
FWHM Crystallite size
!attice strain
FWHM
P
E
A
K

H
E
I
G
H
T
Integrate" peak
Intensity
83
Determination of ?tressJ?train in sport rim
and automotive components
Colla#oration $ith %r& %iana !a"os' Worcester Polytechnic
Institute
87
Position AB26)etaC
15 25 45
$ountsDs
5
1555
2555
XRD of c$ocolate
#ar% $)ocolate
Scan tie:
15 inutes
!y understanding t)e
structure of c)ocolateE it is
possi,le to
#ipro:e t)e production
process
#pre:ent ageing of
c)ocolate
88
ICXRI!//! 9 XRD Wor4s$op
+$ase Identification 9
?earc$J>atc$ @nalysis wit$ t$e
ICDD +owder Diffraction File
Identification @nalysis usin& searc$-matc$
met$od wit$ ICDD +owder Diffraction File
Crystalline
6i))site5 @l,O"0
1
@morp$ous
&amma alumina5
U-@l!O1
8;
Auantitative analysis
@anosi+ed
particles
-arge
particles
-
+$otocatalytic properties must )e suppressed5
to prevent dama&e of t$e or&anic matri V
use RH2IDE p$ase
-
+articles must )e nano-si*ed and not
a&&lomerate in t$e product to ensure
transparency
a
a
r
a a
a a
a5 r
a5 r
r
a E anatase 2iO
!
r E rutile 2iO
!
8.
@pplications of XRD in industry

Identification and verification of in-comin& powder5

minerals5 metals samples

Auality control of products

>easurement of stressJstrain in components ,e&' )ra4e

pad and ot$er car components0

2$in film coatin& of semiconductor materials

Dru& and p$armaceutical products

Crystal si*e of (anomaterial

:/
6)an% Fou
6)an% Fou
for your attention
X-ray tu,es
X-ray tu,es
E
2$e -ray tu)e is a vacuum tu)e in w$ic$ electrons
are accelerated to a $i&$ velocity )y means of
electrostatic field and t$en suddenly stopped )y
collision wit$ a tar&et'
E
Result of t$is collision5 -rays are emitted'
E
2o prevent -rays from )ecomin& a $a*ard and
create scattered radiation5 t$e -ray tu)e is s$ielded
wit$ lead ,t$e window remains uns$ielded0'
:!
X-ray tu,es
X-ray tu,es
2$e )asic components of a -ray tu)e are:
E
a sealed &lass tu)e envelope5
E
a cat$ode5
E
an anode
E
-ray tu)e window
6arget (Anode) 9ilaent ($at)ode)
?lass tu,e en:elope
X-ray tu,e 3indo3
:1
A sealed glass tu,e en:elope:
E
>ade of &lass or metal-ceramic $avin& $i&$ meltin&
point to wit$stand t$e intense $eat &enerated at t$e
anode'
E
"i&$ vacuum environment:
E
2o prevent oidation of t$e electrode materialsK
E
2o permit ready passa&e of t$e electron )eam wit$out
ionisation of &as wit$in t$e tu)eK and
E
2o provide electrical insulation )etween t$e electrodes'
X-ray tu,es
X-ray tu,es
:3
A cat)ode:
E
Cat$ode incorporates focusin& cup and filament'
E
Focusin& cup acts as a lens to direct t$e electrons in a )eam
towards t$e anode'
E
Filament is $eated )y @C current from a separately controlled
transformer'
E
@ c$an&e in t$e volta&e ,4G0 applied to t$e filament varies t$e
filament current ,in @0 and t$e num)er of electrons emitted'
E
Current passin& )etween t$e cat$ode and anode )y means of
t$e $i&$-speed electrons5 called tu)e current ,in m@0'
X-ray tu,es
X-ray tu,es
:7
An anode:
E
@node - metallic electrode of $i&$ electrical and t$ermal
conductivity'
E
2ar&et materials - tun&sten5 &old or platinum'
E
2un&sten - most common anode material )ecause it $as a
$i&$ atomic num)er5 $i&$ meltin& point and $i&$ t$ermal
conductivity'
E
6eneration of $eat if not controlled would =uic4ly cause t$e
surface of t$e tar&et to erode'
E
2o avoid over$eatin& t$e tar&et5 t$e tun&sten is em)edded in
a mass of material wit$ $i&$ t$ermal conductivity5 suc$ as
copper'
X-ray tu,es
X-ray tu,es
:8
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
X-ray tu,es
::