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1.1.1
..o0o..

Tiu lun
ng dng phng php
hunh quang tia X trong
khoa hc v k thut

Mc Lc
ng Dng Phng Php Hunh Quang Tia X Trong Khoa Hc V K Thut

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Mc Lc.................................................................................................................... 1
Chng 1. L Thuyt Pht X Hunh Quang Tia X..................................................3
1.1 C Ch Pht X Hunh Quang Tia X..............................................................3
1.2 u im V Nhc im...............................................................................5
1.2.1 u im.....................................................................................................5
1.2.2 Nhc im...............................................................................................5
Chng 2. Cc ng Dng Ca Phng Php Hunh................................................6
2.1 ng Dng Trong Xc nh Nguy Hi V Nguyn T Vi Lng Thit Yu
Trong Mi Trng V Vt Liu Sinh Hc.............................................................6
2.1.1 Gii thiu..................................................................................................6
2.1.2 Cc loi my s dng v iu kin o.......................................................7
2.1.2.a Ph k EDXRF vi bia th cp...........................................................8
2.1.2.b Quang ph k TXRF...........................................................................8
2.1.2.c Quang ph k PXRF...........................................................................9
2.1.2.d Quang ph k XRF/CT.................................................................11
2.1.3 Chun b mu..........................................................................................11
2.1.3.a Mu sinh hc.....................................................................................13
2.1.3.b Mu mi trng................................................................................13
2.1.4 Kt qu....................................................................................................14
2.1.4.a .Mu go...........................................................................................14
2.1.4.b Mu xng........................................................................................14
2.1.4.c Mu mi trng................................................................................15
2.1.4.d Mu kh ht nhn ngng t...............................................................16
2.1.4.e Mu t nhim Uranium...................................................................17
2.2 ng Dng S2 Picofox Phn Tch Du Vt Nguyn T, Xc nh Tnh Xc
Thc V Kim Tra Tinh Khit Ca Cc Mu Dc Phm.............................19
2.2.1 Gii thiu................................................................................................19
2.2.2 Nhng thng s o lng........................................................................21
2.2.3 Chun b mu..........................................................................................21
2.2.4 Kt qu....................................................................................................23
2.2.4.a Kim tra tnh xc thc ca ASA........................................................23
2.2.4.b Kim tra tinh khit ca Natri clorua.............................................24
2.2.5 Kt lun...................................................................................................25
2.3 Mt S ng Dng Khc................................................................................26
2.3.1 Trong phn tch hnh nh.........................................................................26
2.3.2 Trong php y...........................................................................................27
Ti Liu Tham Kho................................................................................................28

ng Dng Phng Php Hunh Quang Tia X Trong Khoa Hc V K Thut

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Chng 2. L Thuyt Pht X Hunh Quang Tia X

2.1 C Ch Pht X Hunh Quang Tia X
Khi mt ngun kch thch tia X s cp t mt ng tia X hoc t ngun ng v
phng x chiu vo mu, tia X c th c hp th bi cc nguyn t hay phn tn
thng qua vt liu. Qu trnh trong mt tia X c hp th bi cc nguyn t
bng cch chuyn ton b nng lng ca n cho mt electron trong cng c gi
l " hiu ng quang in ". Khi electron cc lp K, L, M. thot ra ngoi, nguyn
t trng thi kch thch v cc l trng c lp y bi s dch chuyn electron
cc lp ngoi c mc nng lng ln hn, mi s chuyn mc u c nng lng
km theo v nng lng ny c s dng theo mt trong hai cch:

Dng cho photon tia X ngha l bc x hunh quang tia X

Quang electron

Bc x pht ra t
ng tia X hoc
ngun ng v
phng x

ng Dng Phng Php Hunh Quang Tia X Trong Khoa Hc V K Thut

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Dng cho electron Auger ngha l nng lng tia X hon ton b
mt do hp th trong phm vi nguyn t vi kt qu l electron mc cao hn
( lp ngoi) s thot ra ngoi.

ng Dng Phng Php Hunh Quang Tia X Trong Khoa Hc V K Thut

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2.2 u im V Nhc im
2.2.1 u im
Hunh quang tia X thch hp cho vic phn tch c lin quan n:
- Phn tch c s lng ln cc nguyn t ha hc chnh (Si, Ti, Al, Fe, Mn,
Mg, Ca, Na, K, P) trong v trm tch.
- Phn tch c s lng ln cc nguyn t vi lng (> 1 ppm; Ba, Ce, Co,
Cr, Cu, Ga, La, Nb, Ni, Rb, Sc, Sr, Rh, U, V, Y, Zr, Zn) trong v trm tch.

2.2.2 Nhc im
Trong l thuyt XRF c kh nng pht hin tia X pht ra t hu ht tt c cc
yu t, ty thuc vo bc sng v cng ca tia X. Tuy nhin :
- Trong thc t, cc ph k thng mi rt hn ch trong kh nng o chnh
xc cc nguyn t c Z <11 hu ht cc vt liu t t nhin.
- XRF phn tch khng th phn bit cc bin th trong s cc ng v ca
mt nguyn t, do , cc phn tch ny thng xuyn c thc hin vi
cc dng c khc.
- XRF phn tch khng th phn bit cc ion ca cng mt nguyn t trong
nhng trng thi ha tr khc nhau, do , nhng phn tch ca v khong
sn c thc hin vi k thut nh phn tch ha hc t hoc ph
Mossbauer.

ng Dng Phng Php Hunh Quang Tia X Trong Khoa Hc V K Thut

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Chng 3. Cc ng Dng Ca Phng Php Hunh

Quang Tia X
3.1 ng Dng Trong Xc nh Nguy Hi V Nguyn T Vi Lng Thit
Yu Trong Mi Trng V Vt Liu Sinh Hc
3.1.1 Gii thiu
S nhim mi trng do thin nhin hoc do hot ng ca con ngi gy
ra, kt qu lm nhim bu kh quyn, nc, tDo nghin cu s nhim
mi trng, cn tip cn mt cch ton din, mt lot cc mu i din cn phi
c phn tch y trong phm vi rng cc thng s. iu ny s bao gm vic
o lng s lng ln cc mu c bn cht khc nhau. Thng tin y thu c t
vic kim tra cp nhim theo di mt cch ton din cc c trng ca cht
gy nhim, thng tin s cho bit cc con ng gy nhim v phc v cho vic
qun l, kim sot chng. T nhng l do trn, cc yu cu t ra l phi phn tch
nhanh, khng ph hy mu v phn tch ng thi nhiu nguyn t. Ph hunh
quang tia X phn tn nng lng ( EDXRF) v k thut lin quan p ng nhu cu
ny. Trong 20 nm qua my EDXRF c pht trin mnh m. Gn y, s tin
b trong detector s dng cht bn dn, trong x l tn hiu s v trong h thng
my tnh iu khin d liu m rng ng dng ca k thut ny vi chi ph thp,
xc nh nhanh nng cc nguyn t trong mu. Li th chnh ca k thut
EDXRF hn cc phng php khc l n c kh nng phn tch c nhiu nguyn
t, phng php chun b mu d dng v pht hin tt gii hn cc nguyn t. Mt
li th khc l chi ph bo tr thp cho php EDXRF c s dng rng ri trong
cc phng th nghim trn th gii. Cc b phn ca EDXRF c sn trn th trng,
cc phng th nghim ph k tia X c th lp t d dng v c lp. IAEA thng
qua cc d n hp tc h tr cc phng th nghim XRF, cung cp phn mm
phn tch v gip bo tr trang thit b. C quan ny cng tham gia o to i
ng nhn vin chuyn nghip. h tr cc hot ng IAEA thnh lp mt
phng th nghim XRF ti Seibersdorf, c.

ng Dng Phng Php Hunh Quang Tia X Trong Khoa Hc V K Thut

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Tt c cc cng vic th nghim c tin hnh v kt qu thu c ti

phng th nghim XRF ca IAEA. Phng th nghim c trang b mt h thng
XRF thng mi dng cho cc cng tc phn tch thng xuyn, v mt vi nhm
lm vic vi quang ph k EDXRF. Cc k thut phn tch c th bao gm EDXRF
vi bia th cp, tng phn x hunh quang tia X (TXRF), chm vi m XRF (XRF)
v ph k XRF xch tay phn tch trc tip ti ch ng v phng x ( PXRF). Cc
ph k XRF cng c s dng chp ct lp tia X (CT). S dng nhng k
thut ny, xc nh nguy hi v nguyn t vi lng thit yu trong mi trng, mu
sinh hc v c tnh ca mu hn tp c thc hin.
Mu

EDXRF
sec.target

Mu
Sinh hc
Go
Xng ngi

TXRF

PXRF

XRF

CT

Mu
Mi trng
t
Kh ht nhn
ngng t
t b nhim
uranium

Bng 1: Mu v cc k thut quang ph c s dng

3.1.2 Cc loi my s dng v iu kin o

Cc phn tch XRF thc hin s dng mt vi phng php XRF v quang
ph k. N ty thuc vo ph s dng, cc mu phn tch c chun b dng
vin nn, ht c gi trn b lc polycarbonate ( EDXRF), cht lng - sau khi ha
tan trong h thng l vi sng axit ha tan ( TXRF) hoc lc ht c gi sau mt
chu trnh trc c c ha hc ( EDXRF v TXRF), bt lng ( PXRF), ht ring l

ng Dng Phng Php Hunh Quang Tia X Trong Khoa Hc V K Thut

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c gi trn l Mylar ( XRF) v mu pht gn kt nhng ht ring l (CT). Cu

to ca cc ph k v iu kin o lng c m t di y

3.1.2.a Ph k EDXRF vi bia th cp

Hai quang ph k c s dng. H thng th nht l mt b my thng mi
bao gm mt cc dng bng Pd, ng tia X (300W), nm bia th cp (
Al2O3 , Co, Mo, Pd , nhit phn than ch nh hng cao (HOPG)), mt detector Si(Li)

( FWHM =150eV / 5.9keV, vng kch hot 20mm 2, ca s Be 8m ) . Vic o lng

c thc hin trong chn khng, thi gian phn tch mi mu l 1800s
( bao gm thi gian o vi tt c nm bia) v ng HV c ci t ty thuc vo bia
th cp, l mt trong cc thng s sau: 52,5kV/Al 2O3 , 30kV/Co , 30kV/Mo ,
44kV/Pd v 15kV/HOPG. Phn tch c iu khin bi h thng my tnh thu thp
d liu. Cc mu phn tch c chun b dng vin nn vi ng knh bng 32
mm. S phn tch nh lng c s dng trong quang ph k thng mi da
trn cch tip cn thng s tn x c bn. Vi mc ch phn tch trc tip khng
kh ht nhn ngng t trn b lc polycarbonate , h thng th hai l quang ph k
EDXRF sec.target c s dng. Quang ph k ny bao gm cc dng l Mo,
ng tia X (3000W), bia th cp l Mo, mt detector Si(Li) ( FWHM=170eV /
5.9keV, vng kch hot 30mm2, ca s Be 8m) i km vi in t NIM, kt ni vi
h thng my phn tch bin a knh (MCA) da trn my tnh. Cc php o
c thc hin trong chn khng, thi gian o mi mu l 10000s. iu kin hot
ng ca ng l 45kV/40mA.

3.1.2.b Quang ph k TXRF

Quang ph k TXRF bao gm mt bung chn khng gn vi ng tia X
(3000W), cc dng l Mo. Bung c trang b ng c gii hn phn x v c
gii ha giai on mu cho php iu khin t xa gc lt qua. Ph tia X c thu
nhn bi detector Si(Li) ( FWHM = 170eV / 5.9keV, vng kch hot 30mm 2 , ca s
Be 8m). S iu khin gc ti hn v thu thp d liu c thc hin di s iu

ng Dng Phng Php Hunh Quang Tia X Trong Khoa Hc V K Thut

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khin ca my tnh chy phn mm SPECTOR. ng tia X hot ng ti

45kV/40mA v thi gian o mi mu trong khong 100-500s.

Mt h thng c thit k v lp rp ti phng th nghim IAEA

Hnh 1: Quang ph k TXRF

3.1.2.c Quang ph k PXRF

Quang ph k c th s dng trc tip trn mu t v cng c th phn tch
mu bt lng ng trong ly nha. Ti a ba ngun ( Fe-55, Cd-109, Am-241) c th
c lp t trn mt bnh xe quay vng cho mu lin tc b kch thch. Cc kt qu
thu c bng cch s dng ngun ng v phng x Cd-109 c hot 925MBq
kch thch bc x hunh quang tia X. Ph tia X c thu nhn bi detector
photodiode Si-PIN c cung cp bi acquy hot ng tch hp nng lng/ b
khuch i gn vi acquy hot ng. D liu thu thp c kim sot bi mt my
tnh. Hiu sut ca quang ph k c xc nhn bng cch phn tch ph rng

ng Dng Phng Php Hunh Quang Tia X Trong Khoa Hc V K Thut

Trang 10

ca cc vt liu lin quan di dng bt v thc hin ti ch xc nh nguyn t

trong mt t.

Ph k cm tay da trn ng v phng x c thit k v lp rp ti phng

th nghim IAEA
Hp ng ngun c
th quay

L chn
bng ch

Hp ng mu
bng nha

Ngun Cd-109 hnh

vnh khuyn
Ngun Fe-56
hnh vnh khuyn
Khung detector v
bn tn nhit

Ngun cung
cp

ng Dng Phng Php Hunh Quang Tia X Trong Khoa Hc V K Thut

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Hnh 2: Ph k cm tay XRF

3.1.2.d Quang ph k XRF/CT

Mt quang ph k qut chm vi m bao gm mt ng tia X nng lng cao
gn vi mao mch quang hc pht ra mt chm tia X chun trc tt. Cc chm ti
ch c kch thc ng cho nh, FWHM nh l o lng trn b mt mu, th
bng khong 12m. Cc ng anode khc c th d dng ci t cho php ti u ha
iu kin kch thch. Cc mu c gn pha trc chm trn mt giai on c gii
ha mu. chnh xc ca v tr mu vo khong 1-2m. H thng c trang b
hai detector, detector Si(Li) ( FWHM = 160eV / 5.9keV, vng kch hot 80mm 2 ,
ca s Be 8m) v detector SD ( FWHM = 170eV / 5,9 keV, vng hot ng
2mm2, ca s Be 8m ). S qut v thu thp d liu th c iu khin bi my
tnh chy phn mm SPECTOR. Cc tnh nng thun li ca h thng ny so vi
cc ng tia X khc l n da trn quang ph k chm vi m, n c hai detector c
th hot ng ng thi. Detector Si(Li) ghi nhn ph hunh quang tia X ca mu
v detector SD hot ng ti thi gian hnh thnh nh 0,25s, o lng trc tip
chm chuyn i thng qua mu phn tch. Cng vi cng khuch i tch hp v
ADC nhanh, cc detector SD c th hot ng vi tc m 10 5cps. H thng

ng Dng Phng Php Hunh Quang Tia X Trong Khoa Hc V K Thut

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cng c s dng kim tra s c mt ca Uranium giu trong mu t b

nhim v cho hnh nh 3D ca mt mnh xng.

3.1.3 Chun b mu
Cc mu c chun b bng nhiu cch khc nhau ty thuc vo cc loi
mu, s lng c sn, v la chn cc quang ph k thch hp thc hin cc
phn tch .

Mu

Khng c bt k

Cc dng

s chun b no

(PXRF,XRF,

(PXRF, EDXRF)

CT )

Dng vin
( EDXRF)

Ha tan
( TXRF )

Mu sinh
hc
Go

Vin, khng
c cht kt
dnh

Xng

ng kh

ngi
Mu mi
trng
t

Trc tip, ti ch

Bt

Vin, c hoc
khng c cht
kt dnh

Khng

Trc tip trn b

Ha tan

kh ht

lc

vo dung

ng Dng Phng Php Hunh Quang Tia X Trong Khoa Hc V K Thut

Trang 13

nhn

dch c

ngng t

cha
Cobalt

t b

Gi trn l

nhim
Uranium
Bng 2: Bng tm tt cc dng mu

3.1.3.a Mu sinh hc
Mu sinh hc c phn tch bao gm go v mnh xng. Go c nghin
thnh bt mn, sau ly 7g, nm thnh vin c ng knh 32mm, khng c cht
kt dnh. Mu go c phn tch bi EDXRF v ph k thng mi.
Mu xng ca mt ngi b long xng c chun b thc hin cc
hnh nh 3D CT ( cu trc xng). Mnh xng c ng kh. Mu xng c
t trn khung graphite 0.5mm v sau c qut trong ph k CT.

3.1.3.b Mu mi trng
Mu mi trng bao gm t, khng kh ht nhn ngng t v t b nhim
uranium.
Mu t c chun b dng vin bng cch nn bt ng nht to thnh
vin dy, hoc thm vo cht kt dnh to thnh dng axit boric hoc cellulose.
Sau , mu c o bi ph k EDXRF. Nhng mu ny dng bt c phn
tch bi ph k PXRF v b mt t c th phn tch trc tip ti ch.
Mu khng kh ht nhn ngng t ban u c phn tch bi ph k EDXRF
m khng c bt k s chun b no. Sau khi EDXRF phn tch, b lc c nhng
vo dung dch c cha cobalt trong mt h thng l vi sng . Sau , mt phn 2L
c ht vo trong mu thch anh v c o bng ph k TXRF
t b nhim uranium c tri u trn b mt mt l Mylar dy 2.5m c
lp vo mt khung nha. ng knh ca mu t trn l Mylar khong 1cm. Mu

ng Dng Phng Php Hunh Quang Tia X Trong Khoa Hc V K Thut

Trang 14

ny c gn vo ph k XRF v c tri ra trong vng 5mm x 5mm ( 51 im

nh x 51 im nh). Thi gian o lng mi im nh l 1s i vi detector Si(Li)
v 0.3s i vi detector SD. Bng cch kim tra tn hiu truyn v tn hiu hunh
quang trong mt vng nh ( 1.5mm x 2.5mm) cha ht nhn nng, ht Uranium
giu c la chn v qut bng cch s dng phn gii cao ( 251 im nh x
251 im nh) v thi gian o di hn ( 5s trn mi im nh i vi hunh quang
v 2s trn mi im nh i vi tn hiu truyn).

3.1.4 Kt qu
3.1.4.a .Mu go
Trong hai mi mu go, bao gm 2 mu go thng mi, c phn tch bi
EDXRF sec.target. Xc nh c cc nguyn t: P, K, Ca, Mn, Fe, Zn, Br, Rb. S

Dy nng ( g.g-1 )

thay i nng cc nguyn t trong phn tch mu go c trnh by hnh 3

Nguyn t

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Hnh 3 : S thay i nng cc nguyn t trong mu go

3.1.4.b Mu xng
H XRF c s dng qut hnh nh 3D ca mu xng ngi b long
xng. Ph k CT qut c hnh nh 3D trnh by hnh 4

Hnh 4: Hnh nh mu xng ngi b bnh long xng c qut bi CT.

3.1.4.c Mu mi trng
Ph k EDXRF thng mi cng c s dng xc nh s c mt ca cc
nguyn t trong t, bin v trm tch. Nng ca nhm nguyn t c xc nh
l: Mg, Al, Si, P, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, As, Br, Rb, Sr, Y,
Zr, Nb, Mo, Cd, Sn, Cs, I, Ba, La, Ce, Pb, Th, U. Mu mi trng c phn tch

ng Dng Phng Php Hunh Quang Tia X Trong Khoa Hc V K Thut

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bng ph k EDXRF. Mi tng quan gia nng xc nh v nng cho c

trnh by hnh 5. Kt qu trnh by hnh 5 thu c t vic o cc mu IAEA-

Nng xc nh c ( g.g-1 )

Soil-7, CERAMIC-1 SARM 69 v mu Penrhyn Slate.

___ ng lm khp, dc = 1.06

.. ng l tng, dc = 1

Nng cho ( g.g-1 )

Hnh 5: S tng quan gia nng xc nh v nng cho ca cc nguyn t
da trn s o ba mu IAEA-Soil-7, CERAMIC-1 SARM 69 , Penrhyn Slate.

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3.1.4.d Mu kh ht nhn ngng t

Nng trong khng kh ( ngm-3 )

Hnh 6: Ph tia X ca kh ht nhn ngng t thu c vi ph k EDXRF

( phn tch trc tip) v ph k TXRF ( sau khi ha tan)

Nguyn t

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Hnh 7: Nng nguyn t trong khng kh thu c bi ph k TXRF v

ph k EDXRF. Kh ht nhn ngng t c chn trong mu khng kh lng phn

3.1.4.e Mu t nhim Uranium

K thut XRF c ng dng xc nh ht Uranium giu trong t b
nhim. Cc kt qu ca mt khu vc qut ( 2.5mm x 1.5mm/ 251 bc x 251 bc;
kch thc bc: dx = 10 m, dy = 6m, thi gian o mi im nh t = 5s i vi
tn hiu hunh quang, t = 2s i vi tn hiu truyn) c trnh by. Biu phn
b nguyn t Uranium giu v cc ht khc c trnh by trn hnh 8. Hnh 9 cho
thy s trng hp gia U v As.

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Hnh 8: S phn b ca cc ht, trnh by bi tn hiu Mo-K, cc ht U

giu/ As giu, K giu, Fe giu, Ca giu c nhn bit bi ph hunh quang tia X.

ng Dng Phng Php Hunh Quang Tia X Trong Khoa Hc V K Thut

Cng

Trang 20

Nng lng ( KeV)

Hnh 9: Ph hunh quang tia X ca cc loi ht c nhn bit trong mu t
nhim Uranium

3.2 ng Dng S2 Picofox Phn Tch Du Vt Nguyn T, Xc nh Tnh

Xc Thc V Kim Tra Tinh Khit Ca Cc Mu Dc Phm
3.2.1 Gii thiu
S m t c im ca nhng nhn hiu thuc c tn thng mi v khng c
tn thng mi l mt nhim v cn thit trong phn tch dc phm. Mt vi k
thut phn tch th thch hp cho vic xc nh s phn b kch thc ht, hnh thi
hc v trng thi phn b. n nay, vic xc nh thnh phn ha hc ca thuc
khng t c s tha ng do cc yu cu chun b mu. Ngoi ra, thnh phn
cc nguyn t ca nguyn liu th v sn phm cui cng phi c phn tch
thng xuyn tun theo ni quy nh.

ng Dng Phng Php Hunh Quang Tia X Trong Khoa Hc V K Thut

Trang 21

ng dng ca k thut hunh quang tia X (XRF) thng thng cho nhng
nhim v phn tch th b hn ch do i hi cao v nhy, trong nhiu trng hp
s lng mu nh sn c v thiu tiu chun nh c thch hp. S dng cc
phng php khc phn tch du vt nguyn t ging nh quang ph hp th
nguyn t (AAS) hoc quy np- cng vi plasma pht x quang ph (ICP-OES) th
thng b gii hn bi s lng mu, s cn thit cho vic ha tan mu v nhng
hn hp lin quan th gp kh khn.
Vi ph tng phn x hunh quang tia X (TXRF), s lng mu dng nh hn
milligram c th c phn tch theo di s phn b nguyn t. l phng
php da trn cc ni tiu chun. Hn na, ph k TXRF S2 PICOFOX khng i
hi s ph hy mu, kh hoc phng tin lm lnh.
Trong phn ny p dng quang ph TXRF phn tch tnh xc thc ca cc
mu dc phm. S khc nhau v phng din thng mi ca acid acetylsalicylic
l da vo cc loi thuc c kim tra bng cch phn tch TXRF nh tnh v
nh lng
Vi mc ch ny cc loi thuc sau y c phn tch:
- Aspirin 500mg, Bayer AG,c
- Aspirin + C(vin si bt), Bayer AG, c
- ASA 100mg, Hexal AG , c
- ASA, Ratiopharm GmbH , c
- Aspirin, khng tn, M
xc nhn s ph hp ca cc PICOFOX S2 kim tra tinh khit ca
mt nguyn liu th in hnh, natri clorua (NaCl) c trn vi hm lng As
khc nhau xc nh gii hn pht hin ca cht gy nhim ny.

ng Dng Phng Php Hunh Quang Tia X Trong Khoa Hc V K Thut

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3.2.2 Nhng thng s o lng

Ph k c trang b mt ng Mo (37W) v mt detector Xflash Silicon Drift
30mm2. Mu c o mt in p cao 50 kV, 750 A cho 1000 s.

Hnh 10: Hnh nh v Acetylsalicylic acid ( ASA) v

cc thit b s dng

3.2.3 Chun b mu
Tt c cc mu c nghin bng tay trong mt ci m no c c cc
ht c kch thc nh hn 75m.
Mt phn tch nh tnh c thc hin bng cch cn lng mu bt
khong 60 mg v t mu vo trong chn nha. i vi s chun b bn than, 2,5
ml c 1% nc dung dch Triton X100 c thm vo. Triton X100 l mt cht ty
ra thng thng iu chnh nht ca cc dung dch. ng dng ca s chun
b bn than trong phn tch TXRF, n gip tng cng cht lng ca cc mu. Sau
khi ng nht trit , 10 ml bn than c t trn mu knh thch anh, mu c
sy kh trong mt bnh kh m v sau em i o.
nh lng v d liu o TXRF c thc hin bng phng php chun ha
bn trong. V mc ch ny, bn than cng c chun b ging nh trong phn tch

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nh tnh. Nh l mt ni tiu chun khong 30 ml ca 100mg /l dung dch Se

c thm vo.
Sau khi ng nht, 10l bn than c chit sut bng pi-pt ln trn mu
knh thch anh , mu c sy kh trong bnh kh m v o cng iu kin vi
mu nh tnh.
i vi kim tra nhim, khong 60mg NaCl (p.A, As <0,4 mg/Kg) c
ha tan trong 1ml nc siu tinh khit v trn vi dung dch As t c nng
cui cng trong khong t 0 n 4mg/Kg.

Hnh 11: Ph TXRF in hnh ca ba loi thuc ASA khc nhau:

Aspirin Bayer (mu xanh l cy), Apirin Hexal (mu xanh da tri) v ASA
(mu ), khng tn

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Tt c cc gi tr trong mg/kg
Bng 3: Nng cc nguyn t trong thuc Aspirin

Hnh 12: S phn tch tng ng v thnh phn nguyn t ca 5 loi thuc
Aspirin khc nhau

3.2.4 Kt qu
3.2.4.a Kim tra tnh xc thc ca ASA
Hnh 11 cho thy quang ph ca cc mu ASA khc nhau. P, Ni, Cu v Sr c
mt trong Aspirin khng tn ; V, Cr, As v Se c mt trong mu Hexal. Cc
nguyn t nh Cl, K, Ca, Fe, Zn v Pb cho thy s khc bit ln trn tt c 5 loi

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thuc. Nh mt s nguyn t i din (Cl, Zn, Pb) khc nhau trong nng c
th hin trong bng 3.
S khc bit ca cc loi thuc ASA c th c so snh sau khi d liu
chuyn i v nhng thnh phn nguyn t c trng. Php phn tch tng ng
ny c biu din bi php phn tch Biplot, a ra mt s gii thch v hnh nh
ca cc thnh phn ha hc (Hnh 12). Kch thc ca mi im d liu i din
cho cc li ca php phn tch TXRF .R rng, tt c cc loi thuc c th c
phn tch mt cch ng tin cy.
S lp li ca cc php o c chng minh bng mi ln s chun b v
phn tch mu Aspirin ,khng tn, USA. Bng 4 cho thy cc gi tr trung bnh
ca cc nguyn t quan trng nht. lch tiu chun vt qu mt phm vi chp
nhn c ch trong trng hp nng gn vi gii hn pht hin.

Bng 4: Gi tr trung bnh ca cc nguyn t quan trng trong mu "Aspirin,

khng tn, M", trung bnh ca 10 php o.

3.2.4.b Kim tra tinh khit ca Natri clorua

Vic o nng NaCl cho thy s tng quan tt vi nng As trn vo (R 2
= 0,9972 , hnh 13). Hn na, cc php o ch ra s c mt ca khong 0,2 mg/kg
As trong cc thuc th cng ph hp vi gi tr quy nh < 0,4 mg / kg.

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Nhng gii hn pht hin cho tt c cc php o c th hin trong bng 5.

Trong tt c cc dung dch kim tra th gii hn pht hin As l ng k di 0,1 mg

Nng As trong NaCl ( mg/kg)

/ kg.

Nng ca As trn vo ( mg/kg)

Hnh 13: S tng quan ca cc php o tinh khit NaCl vi s nhim bn As

trn vo
Nng As thm vo
0
1
2
4
Trung bnh

Gii hn pht hin

0.089
0.067
0.066
0.054
0.069

Bng 5:Gii hn pht hin ca As trong NaCl

3.2.5 Kt lun
S khc bit trong thnh phn nguyn t, c bit l P, S, Cl, Ca, Fe, Zn, Sr,
Pb ca nm loi thuc aspirin khc nhau c xc nh chnh xc bng ph k S2
PICOFOX TXRF.
Kt qu l tnh xc thc ca thuc th nghim c biu din bng mt
th phn tch tng ng. Php phn tch nh lng cung cp thng tin c gi tr, c
th dn n mt s xc nh r rng ca cc nhn hiu sn phm.
Ngoi ra, S2 PICOFOX c chng minh kim tra tinh khit ca
nguyn liu, cht rn ha hc. N thng c dng trong sn xut nhng dc

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phm. S nhim As ca NaCl c o mt cch chnh xc bng cch pht hin gii
xung n 70 14ppb. Li ch c th ca TXRF phn tch cc dc phm so vi
nhng phng php phn tch khc l:
+ Lng mu cn thit l cc k thp (di mg )
+ Vic chun b mu l nhanh chng v n gin cho nhng ng dng thng thng
+ Dng c nh c v vic s dng nh c tiu chun l khng cn thit
+ Tt c cc nguyn t c th pht hin c phn tch cng mt lc

3.3 Mt S ng Dng Khc

3.3.1 Trong phn tch hnh nh
Ph k XRF phn tch hnh nh ca mt bn vit tay c i Nepal xc
nh c bt mu bao gm: son (HgS), diachlon (Pb 3O4), l ng cacbonat v
vng. Bn cht ca X-quang cho php xc nh c im khng th nhn thy bng
mt c nghin cu, trn bn tho ny c mt lp vng m crm (PbCrO 4)

Hnh 14: Thnh phn ca bn vit tay c i Nepal

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3.3.2 Trong php y

Cc nh khoa hc t phng th nghim quc gia Los Alamos s dng mt
chm tia X mng ri sng cc du vn tay - k thut c tn gi hunh quang vi
tia X (XRF). Cc nguyn t nh natri, kali, clo c mt trong m hi ngi s hp
th tia X v pht ra nh sng, hay "hunh quang", dng tn s thp. K thut ny
nhm pht hin ra mui trong m hi ngi - vn to nn ng vin ca du vn
tay. Nu du vn tay lu li lng mui, my s nhn dng c n m khng
cn can thip vo mu.
K thut trn cng c th xc nh c nhng cht ny khi ngn tay b ph
bi m phm, t, nc bt hoc kem chng nng - l nhng cht nhim lm mt
s chnh xc ca phng php iu tra ti phm truyn thng.
Phng php c th thu du vn tay trn nhng cht liu khc nhau, nh giy,
g, da thuc, plastic v thm ch trn da ngi. N cng c ch trong vic nhn dng
vn tay tr em, l i tng c t du trn da. Ngoi ra, cc chuyn gia cn c th
thu c nhiu thng tin t vn tay. Chng hn, mu thc n cui cng ca nghi
phm git ngi. y l mt cng c mi ca cc nh iu tra php y, cho php h
pht hin du vn tay bng phng php khng ph hu, m theo k thut truyn
thng c th b b qua. Hn ch ca n l i khi lng vt liu c th pht hin
c qu nh. Cc tia X khng nhn ra nhng nguyn t nh hn (v ph bin hn)
nh carbon, nit v xy.

Hnh 15: Hnh nh du vn tay

s dng k thut XRF

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Ti Liu Tham Kho

1. www.ichtj.waw.pl/ichtj/nukleon/back/full/.../v49n3p087f.pdf
2. www.bruker-axs.de/.../LR_XRF_92_S2_PICOFOX_Authenticity_test_low_res.pdf
3. www.springerlink.com/index/j32rux7335641653.pdf
4. en.wikipedia.org/.../Xray_fluorescence
5. www.bruker-axs.de/.../sec3_1.html

ng Dng Phng Php Hunh Quang Tia X Trong Khoa Hc V K Thut