Phân tích hàm lượng một số kim loại trong khói bụi xe gắn máy bằng phương pháp phân tích huỳnh quang tia X

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T~V()NG BAI HQC KHOAHQC TV NHIEN

D~ Hlinghien cuukhoa hQcca'p trliong

'Phan Tich Ham
Lu'Q'ng'MQtS6'Kim"Lo~i
Trong Kh6i
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'BQi Xe , Gan May Bang Phu'dng Phap Pban.Tich
Huynh Quang Tia X
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Chu. nhi~m d~ t~li:ThS. Tr~n Phong'Dung
BQ Mon V~t Ly H~t Nhan, Khoa V~t Ly

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Ma 56 d~ tai: 2000
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Nh6m Thlfc hi~n:

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Tnlo'ng Thi Huynh Hoa
Le PhuQngThao
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N.guy~n Cong Tninh

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Nam 2004
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Ml/CLl/C

Trang
1

,

I M1)CTIEU BE TAI
II TONG QUAN

""""""""""""""""""""""""""""""""""

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2

ILl HI; THONG PHAN TICH HUYNH QUANG

2

II.1.1. NGUYEN LY HOAT BQNG

2

II.1.2 NGUON PHONG XA KICH THICH

3

11.1.3.B AU DO

3

"

11.2CAC LOAI MAU

3

11.2.1.M.A.U CHU AN
11.2.2.MA U SO SANH
11.2.3.MA U PHAN TICH

4
4
5

"
"

II.3. PHlJONG PHAP PHAN TICH BJNH U.J<;JNG

7

II.3.1. PHVONG PHAP cHUAN NGOAI TUYEN TINH

7

II.3.2. PHVONG PHAP cHUAN NOI

9

II.4. PHVONG PHAP TUYI;T BOI HIJ;U CHINH BANG THVC NGHII;M (PHVONG

PHAP H.~M KICH .THICH)
9
11.5. PHAN

MEM

AXIL

III. THVC NGHII;M

00

00

"

13

IlL 1. HO A CHAT vA DVNG CV

IIL2 BlEU KII;N THVC NGHIJ;M

00 """" 13
00

111.3.BQ LAY MAU KHI

Phl;l Ll;lC Kit Qua Phan Tich Mtiu

Tili li~u kham khao

00

13

13

IV. KET QUA
V. KET L U AN

11

14
00

00 15


p~' ~

£)2 tai nghien ctiu cap truang"

I MT)CTIED DE TAl

Tren co sd nhung tai li~u tham khao, b~ng phuong phap phan tich ph6 huynh
quang tia X, chung t6i phan tich ham lUQngmQt sO'nguyen to' h6a hQc c6 trong b1;1ikh6i xe
g~n may (vung nQi thanh Thanh Ph6 H6 Chi Minh) voi ngu6n ph6ng x(,\kich thich 55Fe
(vanh khuyen) va H3Zr (mQt phia). Ke't qua dUQCxli' 19 tren phftn m~m AXIL theo phuong
phap Regression of Count rate vs. Concentration (sli' d1;1ngcac tinh toall h6i quy d~ suy ra
ham luQng). Voi mong mu6n nhung ke't qua nghien cUu nay g6p phftn b6 sung them

phuong phap phan tich nhanh, hi~u qua d6i yoi nhung m~u m6i trudng, d6ng thdi ap d1;1ng
ma hlnh phan tich nay d~ xac dinh ham lUQng mQt s6 nguyen to' gay 6 nhi€m khac c6
trong khi thai cua xe.

Trang1


D€ tdi nghien cliu dip trrJiJng
,,?

II. TONG QUAN:
11.1.HE THONG PHAN TICH HUYNH QUANG:[1,3,6,8]
II.1.1.Nguyen 19 hoat dong:
Buc X(;lkich thich phat ra ttr mQt ngu6n d6ng vi ph6ng XC;l
khong b~n se

tv dQng

phan ra. Qua trinh phan ra c6 th~ xay ra doi vai mQt nhan hay mQt chu6i.
Cac photon mai tuong tac vai cac nguyen tti' trong m~u b~ng hi~u ung quang
di~n ho~c b~ng tan XC;l(Compton, Rayleigh), tuy thuQc VaGnang lU<;1ng
tia X va b?c so
nguyen tti' cua cac nguyen to' trong m~u. Nhfi'ng nguyen to' nay tan XC;lvoi tia X d~ tC;lo
thanh n~n phong khong mong muan va d~t ra mQt giai hC;lncho phep do huynh quang.
Khi nang lUQngkich thich tia X chi vtra IOn hon nang lUQnglien kSt cua di~n tti'
tren lOp vo nguyen tti' tuong ung thl xac swlt phat huynh quang la IOn nha't. Xac sua't nay
suy giam nhanh nSu tiSp t1,lcgia tang nang lUQngkich thich, di~u d6 cho tha'y buc XC;l
d~c
tning c6 nang lU<;1ngtha'p. VI V?y vai mQt nang lUQngdon nang chi c6 th~ nhC;ly(c6 xac
sua't huynh quang dang k~) vai mQt so' nguyen to' . Tuy nhien trong vai truong h<;1pkhi

phan tich nhfi'ng nguyen to ra't nh~ thl vi~c sti' d1,lngbuc XC;l
lien t1,lCcho dQ nhC;lytot hon
buc XC;ldon nang.
Do hi~u sua't cua ang phat XC;ltia X cao nen d~ sti' d1,lng dUQc ph6 tia X da nang

nay nguoi ta dung cac 10C;libia trung gian. Chieu buc X<;1
nay len bia d~ t<;10huynh quang
thu ca'p la nhfi'ng tia X d~c trung cua bia. Tia X nay gftn nhu don nang dUQcdung d€ kich
thich cac m~u cftn phan tich. Phuong phap nay c6 thu?n l<;1ila ta c6 th~ Iva chQn cae bia
thu ea'p b~ng thao tac co hQc.
B€ kich thich cac nguyen to' trong m~u phat tia X huynh quang d~c trling phai
ehQn ngu6n kich thich c6 nang luQng IOn hon nang lu<;1ngqnh ha'p ph1,lcua nguyen to' cftn
phan tich. Tia X huynh quang thu ca'p phat ra tll' m:1u se di den dftu do va tuong tac vai
cac nguyen tti' cl'ta V?t li~u dung lam detecror (0 day la cha't ban d:1n), hinh thanh cac
xung di~n. Cac xung di~n nay sau khi qua bQ ph~n ti~n khuech d<;1i,bQ ph?n khuech a<;1i
bien dQ dUQc tang len ma'y b?c truac khi di VaG may phan tich bien aQ sau d6 so' ]j~u aUQc

aua VaGxu ly b~ng phftn m~m chuyen dl;tng(AXIL).

i,

Trang 2


f)~ tai nghien cuu cap Wang

11.1.2 Ngu6n phong xa kich thkh:
Cac ngu6n phong x~ dU<;1c
d~t trung bdi dc thong so sau:

- HQat dQ ngu6n.
- Chu ky ban huy.
- LQaibuc x~ phat ra.
- Nang lU<;1ng
buc x~ phat ra.
Sl! °00 tri hlnh hQCcua ngu6n d6ng vi c6 3 d~ng chinh.
** Ngu6n vanh khuyen: Thich hQp cho dc dgu do c6 di~n tich nho nhu dgu do Si(Li).
Ngu6n du<;1C
t~o bdi mQt so cac ngu6n rieng bi~t, d~c bi~t d~t thanh hlnh vanh khuyen.
N6 c6 u'u di~m la truong chie'u deu theo mQi huong nen hi~u suat kich thich IOn.
** Ngu6n di~m: Thich h<;1pcho cac dgu do c6 di~n tich rQng, nhung c6 h~n che': do c6 s\!,
che ch~n vong tam nen giam hi~u suat dgu do.
** Ngu6n mot phia: Thich h<;1pcho cac dgu do c6 di~n tich trung blnh so voi ngu6n.
Trang ba d~ng ngu6n tren thl ngu6n vanh khuyen du'Qc s11 dl,mg nhieu nhat

II.1.3. D§u do:
Buc x~ so cap chie'u de'n se tuong tac voi m~u t~o ra dc 16 trong trang lOpvo
nguyen t11va sinh ra tia X d~c trung m6i nguyen to. Ngu'oi ta dung dgu do ban d~n d~
phat hi~n va do nang lu<;1ngcua chung.
Ph6 ke' detector ban d~n chuy~n d6i nang luQng cua tia X thanh chum xung ke' co
bien dQ ty 1~voi nang luQng cua tia X, sau d6 nguoi ta dung may phan tich da kenh d~ thu
nh~n ph6 bien dQ nay. BQ phan giai cua dgu do ban d~n cao nen c6 th~ phan bi~t au'<;1c

v~ch ph6 cua nhung nguyen to co b~c so nguyen t11ggn nhau. Voi tinh chat nay chung ta
phan tich du'Qcnhieu nguyen to cung mQtluc trang m~u. Di~n tich cua m6i dinh aon ling
voi tia X d~c trung cua nguyen to ty l~ voi n6ng dQ cua nguyen to do trong m~u phan
tich.

II.2 CAC LOAI MAD: [2,5,8,9]
Trong qua tdnh phan rich, ngu'oi ta chia m~u lam 3 lQai:

Trang 3


D~ tUi nghien cl1u dIp tntiJng

11.2.1. M§u chu§n: Miiu nay thuang dUQcIffy tu cac v~t lit%utv nhien d~c trung
cho lO'.limfiu phan tich va dUQccac phong thinghit%m IOn phan tich ham lUQng b~ng cac
ky thu~t phan tich c6 dQ tin c~y, dQ chinh xac cao.
.Phudng

phap chu§n bi:

- M~u dia chelt:chQnm~u qu~ng tv nhien c6 chua cac nguyen to cftn phan tich,
sau d6 dung mQt lUQngxac d!nh, nghi~n nho saG cho cac nguyen to phan bo d~u trong
mau.
- M~u sinh hoc: chQn mfiu chua cac nguyen to n~n va cac nguyen to vi IUQng
tuang duang cac nguyen to trong m~u phan tich.
- M~u day: selykho, nghi~n nho va phan b6 d~u tren giffylQc.
- M[Unffiang:hoa tan muoi hay kim lO'.licua nguyen to can lam chu~n,sau d6

. nho len giffy lQc. Boi khi cftn pha them chelt n~n tra (khong d6ng g6p VaGhffp th\l buc X'.l
kich thich so cffp) d~ ep thanh vien. Cac cheltn~n tra c6 th~ la acid ho~c muoi cua acid
huu co.

II.2.2--M§u so sanh: Bay la lO'.limiiu nhan t'.lOb~ng cach pha che' tu nhung hoa

cheltc6 chua cac nguyen to trong m~u phan tich voi ham lUQngxac d!nh, chinh xac.
Boi voi lO'.limfiu nay c6 th~ thay the'm~u chu~n trang truang hQpm~u chu~n kh6
t':lOhay m~u chu~n qua ton kern.

. Phu'dng phap chu§n hi:
L1,1'athQn hQp chfft h6a hQc c6 thanh phftn khong d6i trong qua trlnh stYdvng.
Khoi lUQngP cua hQp chfft trong miiu dUQctinh theo cong thuc sau:
WM
P = B 100 AfJ

Trang d6 :
P: Khoi lUQnghQp chtt cua nguyen to phan tich dua VaGmiiu so sanh.
B: Khoi lU'Qngm~u so sanh.
W(%): Ham lUQngnguyen to quan tam.

..

~-,

A: So khoi nguyen to can phan tich.
Trang 4


EJJ tdi nghien cuu dip trItt'",I:

~ :SOnguyen tli'cua nguyen to dn

phan tich co trang hQpcha'ttuong ung .

M: Khoi lUQngphan tli' cua hQp cha't.
Thong thudng ngudi ta chu§n bi mot lo~t cac m~u so sanh chua mot hay nhi€u
nguyen to dn xac dinh, voi dO bi€n thien cua m~u phai bao g6m ta't ca cac gia tri ham

lUQngco the co cua nguyen to dn phan tich trong m~u.

M~u so sanh thudng dUQcchu§n bi duoi d~ng bot. Khi tron l~n cac thanh ph~n khac
nhau dn chu

y d€n

st! giong nhau v€ b€ m~t hoa hQc trang h6n hQP.

NgUdi ta thUdng chuffn bi b~ng 3 phuong phap sau:

- Phl1cJngphdo 1: tu nhung hQp cha't hoa hQc cua cac nguyen to dn xac dinh ~o
cha't n~n cho m~u phan tich, them nguyen to dn xac dinh VaGduoi d~ng muoi nitrat va
dun nong tu tu de chuyen nitrat thanh oxit ho~ckim lo~i.
- Phaang ohdp 2 : tron d~u cha't n€n voi cac cha'tdn xac dinh .
-Phaang ohdo 3: them vao cha't n€n mot lUQngdung dich nitrat cua nguyen to do
xac dinh, sau do trQnd~u va lam kho b~ng cach nung nong.
Trang tht!c h~lllh, ngudi ta thuang sli'.d~lOgphuong phap thu 2 VI no don gian hon cae
phuong phap khac.

II.2.3. M§u phan tIch:
BUQcla'y tu v~t li~u dn phan tich. M~u phan rich phai bieu hi~n d~y au cae tlnh
cha't cua doi tUQngphan rich khi la'y ph6 huynh quang tia X, nghla Ia thanh ph:1n hoa hQc
cua m~u phai phu hQp voi thanh ph~n cua chat ban d~u.

. PhilO-figphap chu§n bi
Ky thu~t chuffnbi m~u phan rich phai thoa man cac yeu du v€ cuang do buc
x~..ham lUQngcac nguyen to dn xac dinh va thanh ph~n hoa hQccua m~u phan dch.

Do tinh da d~ng cua mau nen aoi hoi phai co nhung phuong phap chu§n bi m~u thich h,.',
Q. Chuiin_bLmdu bot:

Boi voi cac lo~i mau d<;lngtho nhu aa't, qu~ng, khoang,... thuang nguoi ta khao
sat chungd d'.lng bQt.
Trang 5


EJ€tiJi nghien cdu clip trilc'lng

Cae bude ehuffn bt nhu sau: sa'y kho lam s<;lehm~u (lo<;litru cae t<;lpeha't nhu r€
diy, soi da,...) nghi~n nho, ray thanh bQt vdi dQ mtn nha't dtnh va la'y mau lheo quy t~e
ehia tu.
Tuy theo ml;ledich va thie't bt phan tich ma m~u bQt ehia thanh cae d<;lngsau:
- M~u e6 b~ day bao hoa: bQt eho vao khuon, dung may nen ep thanh vien, e6 th8
trQn them eha't n~n nhu bQt than, keo lam eha't ke't dinh,...
- M~u bQt'd<;lngvien: di d~u mQt Wp bQt m~u th~t mong len khuon, d6 tie'p len mI.'>!
Wp bQt than ho~e acid oxalic sau d6 ep thanh vien. B~ m~t m~u la mQt Wp ra't mong I:hat
bQt dn phan tich.
- M~u d<;lngfilm mong: m~u mong dudi d<;lngbQt vdi kkh thude ra't nho.. Mftu d<;lng
film ra't ly tUc1ngeho phan tich huynh quang VIham lUQngnguyen t6trong miu ty l~ vdi
euang dQtia X d~e trung. Cac hi~u ung ha'p phl;lva euang dQbt lO<;libo hOclnroan.
b Chutln bi mdurdn:
M~u r~n la cae v~t li~u d<;lngkh6i don Ie thuang dUQcche' t<;lOb~ng may d~ c6 hlnh
d<;lngva kich th\l'de phu hQp. B~ m~t nhan b6ng sao cho dQ ma'p ma b~ m~t nho hon 100 II
m d6i vdi nang hlQng tia X tren 5Kev, ho~c 20-40 Ilm khi nang lUQngtia X co 2Kev. Ccfc
m~u r~n thuang dUQct<;lOdudi d<;lngm~u day vo h<;ln.
c Chutln bi mdu long:
Chu~n bi m~u long la don gian nha't. Ne'u c6 sl.fphan tan trang cha't long thl d~
dang khii' n6 b~ng each khua'y trQn. E>6ivdi dung dich co th€ phan rich ph6 huynh quang
tia X tnlc tie'p , ho~c c6 th€ dung phuong phap co d~c hay t<;lO
mang mongo

Cach don gian nha't la d6 dffy dung dich vao trong ch~u b~ng thep khong gi hay
thau nh1,1'a,
day la mang mong hii'uco c6 dQeang th~t t6t.
d Chutln'12i mdu khi:

Trong m~u khi (khi dUQcla'y tu cac ong kh6i nha may, 6ng kh6i xe...) thuang 1.0
cac h<;ltbi nhi€m bffn cac nguyen to' cffn phan tich .Cac h<;ltdl(QChung tfen gia'y lQc hay
cac ta'm film mongo

Trang 6


D€ tai nghien cU'u cdp truilng

n.3. PHUONG PHA.P PHAN TICR DINR LUONG:
II.3.!. Phlidng phap chuiin ngoai tlly~n tinh:
Tli phuong trlnh ma tel eu'dng dQ phat huynh quang thli' ea'p trong tru'dng hQp
ngu6n kieh don nang:

1- exp

Ii (Ei) = Qi f Go 10 wi

[ {
-

pT

= r](Ei)
4n

!" ki

SlI1lf11

sin 1J12

,u(Eo) +' U(Eo)
1

0

\;i

==

!" i

4nr

lJ

sin 'f/2

r](Ej)rk-l

(E ) cv f

(0)

,Ll

sin If/l

Q if

(Ei)

J.~(Eo)+

(E ) cvt i f
0

k

Trong d6
Go la h~ so' chi phlf thuQc VaGb6 tri hlnh hQc
Tru'dng hQp m~u phan tich day:

\Y. l

I;(E,) = K .,,(E,) + piE,)
SIn1Jf 2

sin !fit

K= QitGolo

D6i voi m~u so sanh:

.

Wi

1;(EJ = K ,u(Eo) ,.., ,u*(EJ
sinV/1

sinV/2

~
t.U ,-I (E
, )+

(1
\

0 day:
.LL* (E ) =

\V

,u(E) = W t

Pi

-

~) LL.11 (E )

IN I'

(E) + (1- Wi),ull (E)

Voi J.l;(E) va PI(EI) la h~ so' suy,giam kh6i Cl'tanguyen to' i dn xac dinh tl((ing ling voi
bue X? so cap va bCCcX? thCCca'p.

TI,llIg 7


LA ,," ""..";'/1

Jii(Eo)

Jin(Ej)

u"',

~"'Jl """"6

la h~ s6 suy giam kh6i cua cha't n€n tuong ung voi buc x~ SOca'p va buc

x~ thu ca'p.
L~p tll~ ta dUQc:

,u.(E,J + ,u.(EJ
Ii(EJ

Wi sin VII

l~(EJ

w; .u(Eo) + ,Lt(EJ

sin 1fI2

(I)

sin1fl1 sinll2
N€u cha'tn€n cua m~u phan tich va rn~u so sanh c6 thanh phfin h6a hQcnhu nhau, va ham
lUQngnguyen t6 thay d6i nhc>,c6 th6 xern h~ s6 suy giarn kh6i ~ khong d6i, nghia la
Ji

;:::

Ji * khi d6 phuong trlnh (I) se tra thanh (II):

W

I
= -w*

(II)

r

Bay la truang hQp don giiin nha't, chi dung rnQtm~u so sanh. Tuy nhien neu ham lUQng
nguyen to' trang cac rn~u thuang khac nhau rnQtlUQngxac dinh thl khong ap dt:IngdUQc
(II). Luc nay phiii dung nhi€u hon m~u so sanh va l~p d6 thi 1= few). Thong thuang rn6i
lien h~ la tuy€n tinh:
w= aI+ b (III)

B6 xac dinh cac h~ so' a, b ta dung phuong phap blnh phuong cttc ti8u. 86 dQ chinh
xac cao duang chugn doi khi la rnQtda thuc b~c hai hay IOnhon. Tuy nhien cac di~u ki~n
ngoai thuang thay d6i theo thai gian, do d6 d~n den hi~n tUQngtroi ph6 va duang chuffn
phiii lam thuang xuyen. 86 kh~c pht,lctlnh tr~ng nay nguai ta dung ti s6 cuang dQtU'ong
d6i IIIe. Trang d6

Ie la cuang dQ cua rnQt v~ch quy chi€u nhu v~ch coherent hay

incoherent cua ngu6n kich. Phuong trlnh (III) tra thanh:

.v
.

d phuong phap nay vi~c pha ch€

a-

T
I"

+

b

(IV)

rn~u so sanh gfin gi6ng voi m~u phan tich. Cac

rn~u c6 ham lUQngnguyen t6 dn xac dinh da bitt. 80 cuang dQbuc x~ d~c trung phat
va xay dtfng du~c;'duong cong bi6u di€n rn6i lien h~ giii'a cuang dQ va ham luQng. N~i

duang chuffn nay khi bitt dUQccuang dQ ta tinh dUQcham lUQngnguyen to' dn phan tich,
TranK <'1


D~ tdi nghien criu cOp tnldng

II.3.2. Phu'dng {>hap chuftn noi:
f)u'a vao mQt lu'Qngnguyen to' B nao d6 b~c so' nguyen tti' khac voi b~c s6 cua
nguyen to' A dn

phan tich mQt don vi. Nguyen to' c6 ham lu'Qng da biet tru'oc gQi Iii

nguyen to' chu~n nQi hay nguyen to' so sanh. Ta se so sanh cu'ong dQ d~c tru'ng cua hai
nguyen to' nay. Ta c6 bi€u thti'c lien h~ sau:
(V)

W A= ~w B.IAIIB

WB la ham lu'Qngnguyen to' c6 trong m.1u.
~ la h~ so' cu'ong dQ du'Qcxac dinh b~ng tht,tcnghi~m sau:

cp -

I
--

A

w

A

[)

\v

;0;

I

(VI)

Dung m~u so sanh c6 ham lu'Qngnguyen to' A va nguyen to' B xac dinh ta e6:

I
I '1

~

=

"

f(W

)
A

Phu'ong trlnh (V) va (VI) s11dl;mg d€ tinh WAkhi ham lu'Qng nguyen to' A cua m~u cftn
phan tich thay d5i trang khoang gioi h~n kh6ng Ion. Tru'ong hQp ngu'Qe l~i thl phai t~o bQ

m~u so sanh e6 ham lu'Qngcae nguyen

to A, B xac

dinh, trong d6 ham lu'Qngcac nguyen

to B nhu'nhau trang cac mftu so sanh. L~p d6 thi phan tich thl h~ so g6c cua duang th~ng
la h~ so' cu'ong dQ
II.4. PHUONG PHAP TUYET DOl HIEU CHINH BANG THUC NGHIEM:
(PHUONG PHAP HAM KICH THICH):
Tli phu'ong trlnh tinh cu'ang dQbti'c x~ huynh quang thti' cap:
Ii(Ei)

= Qif

Golo Wi

(1- exp[ -pT{!l(Eo).(sin\}Jlrl + !l(Ei).(sin'P2rl}])/{!l(Eo).(sin\}Jlrl +

!l(Ei).(sin\}J2r1} (VII)
Trang d6:
Qif

=ll(Ei)(

4rc)'"CkiCDkJ

'"Cki
la h~ so' hap ph1,1kh6i quang di~n cua bti'c x~ d~c tnfng nguyen to I, nen n6 Iii

mOt ham Zi' Do c16ta co th€ c1~t:

TranI{ 9


DB tiLinghien crill cap trilling

Qif GoIo = F(Zi)

- F(Zj)

gQi la ham kich thich.

Khi d6 ,phuong trlnh (VII) co th€ trlnh bay nhu' sau:
Ij(Ej)

=

F(Z)

!l(Ej).(sin'¥2rl}

Wj

(1- exp[ -pT{!l(Eo).(sin'¥lrl

+ !l(Ej).(sin'¥2rl}])/{!l(Eo).(sin'¥lr'

+

(VIII)

Thi nghi~m bo tri sao eho cae goc '¥ I, '¥2 g~n b~ng 90°.
Ta e6:
Ij(Ej)

=F(Z) Wi

(1- exp[ -pT {!l(Eo) + !l(Ej) }])/ {!l(Eo) + !l(Ej)} (IX)

Doi voi m~u mong ta eo:

Ij(Ej)

=F(ZDwj pT

(X)

sa dl,lng mQt m~u chu§'n chI eo mQt.nguyen to dllY nha't tu'ong ung voi cac gia tIi Zj
khac nhau bao quanh gia tri Zj cila nguyen to dn phan tich, b~ng thlfC nghi~m ta do
cu'CfngdQ I cila buc x~ d~e tru'ng nguyen to duy nha't trong m~u. Voi cac gia tri p, T da
bie't cila m~u mong, ta tinh du'Qccac gia tri F(Z) tu'ong ung tti' phu'ong trlnh:
F(Z)

=I/pT

Do do, voi gia tri Zj cila nguyen to dn phan tich ta dUQcgia tri F(Zj) tu'ong ung.
Doi voi m~ll phan tich (m~u m6ng), ta do cu'CfngdQIj, con gia tri p,T tinh tti'bi€u thuc :
pT =P/S

Trong d6 P la khoi lUQngm~u, S la di~n tich b~ rn~tmau.
Thay cac gia tri da do du'Qcvao phu'ongtrlnh (X) ta co:
I(Ei)

\\i

= -p

F(ZJs

Tru'CfnghQp kh6ng t~o du'Qc rn~ll mong, ta phai xac dinh cac h~ so ha'p thl,l khoi
!l(Eo), !l(Ej) b~ng cach tra bang ho~c xac dinh b~ng thlfc nghi~m. Thay cac gia tri co c1u'Qc
vao phu'ong trlnh (IX) ta tinh dUQc Wi.


D€ tJi nghien cuu c(ip trwYng

II.5. PHAN MEM AXIL:
Axilla phin m~m xtr ly ph6 huynh quang tia X va phan tich dinh lUQngcac nguyen
to' trong m~u. G6m cac chuc nang sau:
@ Trao d6i thong tin tu may phan tich da kenh.
@ Chuy~n d6i tu d;;tngdu li~u ph6, luu tru duoi d;;tngformat Axil.
@ Str dl:lllgphuong phap fit binh phuong cvc ti~u d~ phan rich ph6.
@ Tinh toan cac ke't qua phan tich dinh lUQng.
@ Ve ph6 va in du li~u.

Phin m~m Axil xtr ly so' li~u nhanh chong va co th~ phan tich dinh lU<;5ng
nguyen
theo tung dip dQkhac nhau.

. UNG DUNG PHAN MEM AXIL:
Xac dinh ham lu<;5ngcac nguyen to' trang m~u phan tich, diu tien ta din bitt thanh
phin nguyen to' co trang m~u . Sau do t<;tObQ m~u so sanh phu hQp. DiYli~u cua bQ m~u
so sanh sau khi chie'u huynh quang tia X duc;fcphan tich xtr ly b~ng phan m~m Axil. so'
li~u nh~n dUQcla di~n tich dinh cua cae nguyen to' (co ham IUQngtu'ong ling bie't truoe).
Chuong trlnh phan tich ph6 str sl,J.ngfile "*.INP" d~ luu triYdiYli~u.
Xay dvng phuong trlnh duong chuin ham lUQngva cuong dQ cua be>m§u &0sanh ta
co th~ str dl,J.ng:
- Regression

of Count rate vs. Concentration

(sa dl,J.ngcac tinh toan h6i quy di suy ra ham

IUQng).Phuong phap nay dUQcl~p thanh 4 phuong phap sau:

. phuong phap dung nguyen to'nQichu~n (Element as internal standard).
. phuong phap str dl,J.ngbue X;;tkhong ke't hc;fpnhu la ehuin nQi.
(Incoherent radiation as int.stand. )
. phuong phap sa dl,J.ngbue x<;tke't hc;p nhu Iii ehuii'n nQi.

"-'--~.

(Coherent

radiation as int.stand. )

. Phuong phap ehuii'nngQai(No internal standard).

.-.

Of.4.I
THtf \!I~N
-

000460
--

j


D€ tiii nghien ctiu dip trlldng

- Direct

comparision of count rates (so sanh tn!c tie'p cac tinh to<:inv~ cu'ong dQ dinh huynh

quang cua chutin va m~u phan tich).
- Element sensitivitives (xily dvng du'ong chutin ham lu'Qng theo cu'ong dQ dinh huynh
quang).

Tmn" I?


DB tiii nghien CzlUca'p trliifng

III. THtj C NGHltM
DIED KIEN THUC NGHIElVl:
111.1. Hoa cha't va dt}.ngCt}.:

Na2CO3, CaCO3, K2SO4, BQt selt, ZnSO4, NaF (CiCa)
Axeton, etanol (Trung Qu6c) chung ca't l(,ii.
Gia'y lQc Whatman.
Ray:

$=0,098 va 0,074 mm.

Cha y va c6i suo
Can Mettler Toledo AG245 dQ chinh xac O,lmg.
111.2Di~u ki~n thttc nghi~m:

-

Thai gian la'y m~u:30 phut

-

Ta't d cac m~u do trong cung di~u ki~n : 10 phut.

- D(,ingm~u mongo
- Ngu6n ph6ng X(,ikich thich Fe-55(vanh khuyen), H3Zr (mQt phia).
111.3. BQ la'y m~u khi:

khi <1ivan

~
r.

Cot do heu loe

~
/

r---,

~
Gil1

l
\\, (
\1

I,.
I

I

I L.

~

/

(
(

Dong

l
~

l
\

l_-

~

. i

\
~

-

--/~

M,\y hl'[

/7~

J

J
Trang J3


D€ (,Ii lIKhien cliu cifp truang

IV KET QUA

'"

A'

~

,,?

A: LAP DUONG CHUAN CHO CAC CHUAN Ca. K. Fe. Zn.
. Khoi h.t<;1ngmftu: 1O00mg.
Sau khi do cae mftu dli<;1cke't qua trlnh bay (j bang 1:
..

Banu: So'de'mva n6ng dQcua chudn Ca, K, Fe, Zn
Ten m u

Ca
56 de'm

K
N6ng

56 de'm

de)ppm

M§ul

1089 :t 54

20,00

Fe
N6na'"

56 de'm

de)ppm

6457 :t 85

208,00

423 :t 9

Zn

N6ng de) 56 de'm

N6ng

ppm

de)ppm

I
696 :t 27

70,00

80,00

I

3469:t

M§u2

84

110,00

8445 :t 100

270,00

586:t 27

120,00
I

M§u3

3851 :t 86

M§u4

5108:t 94

M§uS

M§u6

,

150,00

5228:t 85

200,00

341:t 8

160,00

613:t 27

4007:t 77

100,00

821:t31

240,00

179:t 4
43:t 4

5773 :t1O0 230,00

2563:t 68

50,00

825 :t 22

270,00

I

9882:t 123 400,00

2226:t 67

10,00

180,00

43,00
16,00
8,00

!
i

iI
!

R2

Phuong trinh h6i quy

Chun

Ca

S= 124,95 + 3,7702. C

0,9987

Chun

K

S= 276,30 + 3,8675. C

0,9957

Chun

Fe

S= 46,951 + 0,34532. C

0,9950

Chun

Zn

S= -6,8829 + 1,4438. C

0,9900

S: Di~n tich; C .n6ng dQ (ppm= mg/kg)

B: PHAN TICH MAU:

Chung T6i tie'n hanh lay m~u va phan tich ham lli<;1.ng
mQtso nguyen to Ca, K, Zn, Fe
tren hai lo:;tixe 86, xe Dream 100 (Cllva moi). Ke'tquil nhu'sau:


DJ (ili nghien ctiu cap tnti'lng

Ham luc1ng (mglkg)

Xe Dream 100

Ca

69,1 :i:0,9

Xe86 ell

n--

-----

160,1 :i: 1,7

K

195,6 :i:2,7

Fe

298,0 :i:3,3

Zn

Xe86 mOl

96,9 :i:1,5

34,8 :i:1,1
9,0 :i:0,2

Zn (dung Cl;lla'ym§:u)

N6ngdQ 26,50 mglm3

V. KET LU!N
Phan tich m§:u bl;li khi b~ng phudng phap huynh quan tia X vdi hai ngu6n ph6ng
x~ la Fe-55 va H3Zr cua mQt so nguyen to Ca, K, Fe, Zn.

Ham luc1ng (ppm)

Nguyen to'
Ca

Dream 100:

30- 80

Xe 86

100- 250
160-210

K
Fe

Xe 86 mdi: 60-120
Xe 86 cii : 200- 400

Zn

Dream 100: 10-40
Dream *:

6-11

Qua d6, chung toi nhan tha'y nhung u'u, khuy&t di~m cua phudng phap huynh quang tia X:
T-r

~

uu di em:

- Phan

uch dUQcnhi~u nguyen to.

- Thai gian phan tich nga:n

- K&t qua thu dUQcchinh
- Yon d~u nt it

xac

-Phudng phap nay c6 th~ a,p d\lng philn tich cae nguyen to kim lo~i khac nhu Pb, Cu

TranR 15


E>€ta; nghien ct/u dip tntilng

Khuye't di~m:

~M~u phai dUge ehu~n bi e~n th~n (di;iebit$t la m~u ehu~n)

- Phai

ke't h9P sa d\mg th~t nhi~u ngu6n

- Kha nang phat hit$n cae nguyen to' nh~ rit thip.
- Cae nguyen to' ham h19ng thip phai mit nhi~u thai gian d~ liy m~u.

TrunK 16

DJ fai nghien cliu cUp trt.tClng

,,'

?

"

,

:;;:

'Phl}ll}c: KET OUA PHAN TICH MAD:
A s6lieu

~han tich ham hfdnl! Ca:
** Xe 86:
Stt

Ten ma u

Din

01

F-15B86

7033:t 108

277,76:t

14,74

02

F-17B86

6729 :t 100

264,32:t

14,03

03

F-19B86

4873 :t 55

182,27 :t 9,67

04

F-20B86

4822 :t 89

180,02 :t 9,55

05

F-21B86

4162:t

82

150,84:t 8,01

06

F-22B86

4239:t

83

154,24 :t 8,19

07

F-23B86

4615:t 86

170,87 :t 9,07

08

. F-24B86

4170 :t 83

151,19 :t 8,02

09

F-25B86

6427 :t 98

250, 94 :t 13,32

10

F-26B86

3109 :t 73

104,29 :t 5,54

11

F-27B86

5936

12

F-28B86

3916 :t 82

139,96:t

13

F-29B86

4406 :t 85

161,63 :t 8,58

14

F-30B86

5930 :t 96

229,00

15

F-31B86

3687 :t 81

129,84:t

16

F-33B86

3122 :t 25

1O4,86:t 5,58

17

F-35B86

4265:t

155,39 :t 8,25

18

F-36B86

4148 :t 103

150,22 :t 7,97

19

F-37B86

2715 :t 70

86,87 :t 4,61

20

F-38B86

3631 :t 78

127,36:t 9,76

21

F-39B86

4078 :t 51

147,13 :t 7,81

22

F-40B86

4196 :t 84

152,14 :t 8,08

23

F-41B86

4105 :t 82

148,32 :t 7,87

24

F-43B86

3147:t76

105,97:t 5,62

25

F-45B86

3408 :t 77

117, 51 :t 6,24

26

F-56B86

3868:t 100

137,84 :t 7,36

tich

103

103

Ham hiqng (ppm)

229,27

:t 12,17
7,43

:t 12,15
6,89

Trang 17


EJi tai nghien ctiu dip tn/Clng

** Xe Dream 100
Stt

Ten m§u

01

F-32BlOO

2844

:t

80

92,57:t

4,91

02

F-34B 100

2177

:t

66

63,09:t

3,35

03

F-37BI00

2715

04

F-42BlOO

4144 :t

05

F-44BlOO

2769 :t 72

06

F-46B 100

2903

:t

07

F-47B 100

2387

:t

08

F-48B 100

09

Din

tfch

Ham lti«ing ( ppm)

:t 70

86,87

82

:t

4,61

15,04:t

0,80

90,45 :t

4,80

72

95,18 :t

5,05

85

72,37:t

3,84

1835 :t 79

'47,97:t

2,55

F-49B 100

2547 :t 89

79,44:t

4,22

10

F-50BlOO

1878 :t 79

49,87:t

11

F-51B 100

2402 :t 86

73,03

12

F-52B 100

2603 :t

87

81,92 :t 4,35

13

F-53B 100

2245 :t

83

66,09:t

3,51

1

F-54B 100

1499 :t 75

33,11 :t

1,76

15

F-55B 100

2309 :t

83

68,92:t

3,66

16

F-56B 100

100

137,84 :t 7,36

17

F-57BlOO

1969 :t

80

18

F-58B 100

1162:t

69

19

F-59B 100

B S6lieuphan

:t

3868

I

2,65
:t 3,88

. 53,89:t

2,86

98,21 :t 5,21

916 :t 65

7,34:t

0,39

tfch ham ltidng K:

Stt

Ten m§u

Din

01

F-09B86

5655:t

02

F-I0B86

6138:t95

03

F-15B86

5550 :t 93

167;71:t 9,82

04

F-17B86

6018 :t 98

187,88 :t 11,00

05

F-19B86

668 1 :t 102

216,44 :t 12,68

06

F-20B86
--

tfch

Ham lti«ing (ppm)

91

6043 :t 98
- -- - -

172,23 :t 10,09
193,05 :t 11,31

--.-

188,95 :t 11,07
Tran~ /8


DJ tdi nghien ctiu dfp trl/iJng ..";,,
.

Stt

Ten mu

07

F-21B86

6668 :t 104

08

F-22B86

6021 :t 99

188,00 :t 11,01

09

F-23B86

5997 :t 98

186,97 :t 10,95

10

F-24B86

6171 :t 98

194,47 :t 11,40

11

F-25B86

6491 :t 100

208,26 :t 12,20

12

F-26B86

6103 :t 102

191,54 :t 11,22

13

F-27B86

6046 :t 98

189,08 :t 11,07

14

F-28B86

6437 :t 98

F-29B86

6543 :t 104

16

F-30B86

6553

:t 105

210,93 :t 12,35

17

F-31B86

6241 :t 103

197,83 :t 11,59

15

'

Din

tich

Ham hiqng (ppm)
215,88

205,93

:t 12,64

:t 12,06

210,50:t

12,33

C. S6lieu ph:)n tich ham lu'dng Fe.

** Xe en:

Stt

Ten mu

Din

tich

01

H-18BO

912:t 14

355,39 :t 17,20

02

H-21BO

825:t 14

313,40 :t 15,17

03

H-35BO

617 :t 12

213,00 :t 10,31

04

H-36BO

1601 :t u

687,95:t

05

H-38BO

532 :t 11

06

H-39BO

737 :t 12

270,92:t

13,11

07

H-40BO

723 :t 12

264,17:t

12,78

08

H-41BO

676 :t 12

241,18:t

11,67

09

H-42BO

558 :t 28

184,53:t 8,93

10

H-43BO

463 :t 10

138,67:t 6,71

11

H-44BO

580 :t 11

195,14:t 9,44

12

H-48BO

711 :t21

258,37 :t 12,50

Ham.lu'qng (ppm)

33,29

171,98 :t 8,32

TranK /9


IN till Ilghlell clfu cap TrIlling

Stt

Ten miu

Din

13

H-50BO

543 :t 11

177,28 :t 8,58

1.+

H-5IBO

683 :t 21

244,86 :t 11,85

15

H-52BO

926 :t 37

362,15 :t 17,53

16

H-53BO

1132 :t 39

461,57 :t 22,34

17

H-54BO

1021 :t 37

408,00 :t 19,74

18

H-56BO

539 :t 11

175,36:t

19

H-57BO

1231:t 41

509,36 :t 24,65

20

H-58BO

768 :t 32

285,89 :t 13,84

21

H-59BO

876 :t 14

338;02:t

tich

Ham'lu'(tng (ppm)

8,49

16,36

** Xe moi:

Ten miu

Stt

Din

tich

Ham lu'(tng (ppm)

01

H-28BN

435:t

11

125,16 :t 6,06

02

H-32BN

457 :t 19

135,78 :t 6,57

03

H-33BN

439 :t 10

127,09:t

I

6,15

I

04

H-34BN

307:t 9

63,36 :t 3,07

05

H-37BN

365 :t 10

91,37 :t 4,42

06

H-45BN

316 :t9

67,72:t

07

H-46BN

344 :t 25

81,23 :t 3,93

08

H-47BN

296 :t 16

65,24 :t 3,16

09

H-49BN

399 :t 10

107,78 :t 5,22

10

H-55BN

392 :t 17

104,40:t

3,28

5,05

D. S6lieu phan tich ham Iu'ong Zn.
Stt

Ten miu

01

H-32B 100

02
03

Din

I

tich

Ham Iu'(tng (ppm)

103 :t 6

16,66 :t 2,80

H-33B 100

197 :t 6

27,50:t 4,62

H-34BI00

116 :t 5

18,16:t

3,50
Trang 20

f)J tili nghien cl1u cc'{ptrtliJng

Stt

Ten mau

Din tich

Ham hiitg (ppm)

04

H-35BlOO

235 :t 7

31,89:t

05

H-36BlOO

333 :t 9

43,20 :t 7,26

06

H-37BlOO

117 :t 6

21,73:t

07

H-38B 100

170 :t 6

24,39 :t 4,10

08

H-39B100

280 :t 8

37,08 :t 6,24

09

H-40BI00

299 :t 8

39,28 :t 6,60

10

H-41BlOO

219 :t 12

11

H-42BI00

194 :t 6

27,16 :t 4,57

12

H-43BlOO

242 :t 7

32,70":t

13

H-44B 100

340 :t 8

44,01 :t 7,40

14

H-45BlOO

150 :t 6

22,08 :t 3,71

15

H-46BlOO

142 :t 6

21,16 :t 3,56

16

H-47B100

402 :t 9

51,17 :t 8,60

17

H-48BlOO

303 :t 8

39,74:t

18

H-49B 100

176 :t 6

25,08:t 4,22

19

H-50BI00

250 :t 7

33,62:t 5,65

20

H-51BI00

270 :t 7

35,93:t 6,04

21

H-52BlOO

385:t

9

41,20 :t 6,93

22

H-53B 100

441 :t 10

55,67 :t 9,36

23

H-54BlOO

355 :t 10

45,74:t 7,69

24

H-55B 100

115 :t 5

17,81 :t 2,99

25

H-56BI00

225 :t 7

30,74 :t 5,17

26

H-57B1O0

548 :t 11

68,02:t

27

H-58B1O0

429 :t 10

54,28 :t 9,13

28

H-59BI00

290 :t 8

38,24 :t 6,43

30,04:t

5,36

3,65

5,05

5,50

6,68

11,44

Trang 21


De tui I/glliim cliu cup trcfilng

Dung dung eu Iffv m~u:

Stt

Ten mftu

Din

tfch

Th

Ham hiqng

tich (m3)

N6ng dQ
(mg/m3)

01

H-09B100

45:t

8

8,19 :t 0,91

0,28

29,26

.

02

.H-10B1O0

03

40

t7

7,55 :t 0,83

0,25

30,20

H -11 B 100

50 :t 9

8,84 :t 0,97

0,32

27,62

04

H-12B 100

41 :t 7

7,67 :t 0,84

0,25

30,71

05

H-13B100

41 :t7

7,67 :t 0,84

0,25

30,71

06

H-14B 100

39 :t 7

7,42 :t 0,82

0,24

30,92

07

H-15B 100

30 :t 5

6,26:t 0,69

0,20

31,30

08

H-16B1O0

29:t

5

6,13 :t 0,67

0,20

30,65

09

H-17B100

38 t 7

7,29 :t 0,80

0,24

30,38

10

H-18B 100

49 t 9

8,71 t 0,96

0,32

27,22

11

H-19B1O0

55 t 10

9,48 :t 1,04

0,36

26,34

12

H-20B100

60 :t 11

10,13 :t 1,11

0,40

25,33

13

H-21B100

65:t

12

10,77:t 1,18

0,44

24,48

14

H-22BI00

54:t

10

9,35 :t 1,03

0,36

25,98

15

H-23B1O0

57:t

10

9,74:t

1,07

0,38

25,64

16

H-24BI00

61:t

11

10,26:t 1,13

0,40

25,65

17

H-25B 100

66

:t 12

10,91 :t 1,20

0,44

24,78

18

H-26B1O0

65 t 12

10,77 :t 1,18

0,44

24,49

19

H-27B1O0

56:t

10

9,61:t

1,06

0,36

26,71

20

H-28B 100

54 :t 10

9,36:t

1,03

0,36

25,99

21

H-29B 100

60:t

11

10,13 t 1,11

0,40

25,33

22

H-30BlOO

59 :t 11

10,00 :t 1,10

0,40

25,00

23

H-31B 100

60 t 11

10,13 :t 1,11

0,40

25,33

_.

--

Tranf{ 22


D€ tei; nghien Clludip trlldng

'A

9

TAl LIf;U TIIAM KIIAO

-[I] Donaid E. Leyden, Fundamental

of X-ray spectromet~y

as applied to Em':rgyc

dispersive techniques, Tractor X-ray, USA, 1984.
[2] Dinh hii'u Hung, Kh6a lu~n t6t nghi~p, Tru'dng DHKHTN, 2000.
[3] Eugene P. Bertin, Introduction

to X-ray Spectrometry

Analysis, Plenum Press, New

York,1978
[4] Ron Jenkins,.R.W. Gould, Quantitative

X-ray Spectrometry,

New York, 1985.

[5] Le Thanh Hung, Kh6a lu~n t6t nghi~p, Tru'dng DHKHTN, 1999.

[6] Nguy~n Tac Anh, Ph6 Huynh Qyang Tia X, DHKHTN,1998.
J7] Ph<;lffi
NgQcDang, Moi Tru'ong khong khi, NxB Khoa HQcKy Thu~t, 1988.
[8] Trftn Phong Dung, Ph6 Huynh Quang Tia X, DHKHTN, 1995.
[9] T<;lMinh Tuye'n, Kh6a lu~n t6t nghi~p, Tru'dng DHKHTN, 1999.

, .
tJH.MH.Tl1' NNtfH~

THlf \11~N

Tranf.t23