1.

Phm vi p dung, quy nh chung:

Hng dn ny quy nh phng php ly mu cc kim loi nng trong bi v kh thi
ca l t cht thi rn nguy hi hoc cc qu trnh t tng t, quy v iu kin nhit v
p sut tiu chun.
Nhit v p sut tiu chun l nhit 25 0C v p sut 101,3 kPa.
Bng 3.1 Gii hn pht hin (IDL) cc kim loi nng
Kim loi

ICP-AES
g/l

AA ngn la
g/l

AA cuvet
graphitc
g/l

Antimoan/Stibi
(Sb)

40 e

200 e

3e

Asen (As)

60

2f

Bari (Ba)

100

Beri (Be)

0,3

0,2

Cadmi (Cd)

0,1

Crom (Cr) tng

50

Coban (Co)

50

ng (Cu)

20

Ch (Pb)

50

100

Mangan (Mn)

10

AA ha hia
lnh
g/l

Thy ngn (Hg)

0,2

Niken (Ni)

20

40

Phospho (P)

60

Selen (Se)

80

2f

Bc (Ag)

10

Tali (TI)

40

100

Km (Zn)

CH THCH:
KTPT03-KT-Phn tch kim loi nng

Trang 1

a Gii hn pht hin bng quang ph pht x nguyn t (ICP-AES).

b Gii hn pht hin bng quang ph hp th nguyn t ngn la (F-AAS).
c Gii hn pht hin bng quang ph hp th nguyn t khng ngn la (cuvet graphit) (GFAAS).
d Gii hn pht hin bng quang ph hp th nguyn t k thut ha hi lnh (CV-AAS).
e Gii hn pht hin vi Sb c th cao hn ph thuc vo cch ph mu.
f Gii hn pht hin As bng quang ph hp th nguyn t k thut hydrua ha.
Phng php phn tch c nu trong Bng 1 v cc php phn tch tng t th php
phn tch ph pht x nguyn t plasma (ICP-AES) c khong tuyn tnh rng hn c. Nhng
mu cha kim loi c nng t hng g/l n hng mg/l u c th phn tch c bng k
thut ny. Mu cha crm, ch hoc asen cao hn 50 mg/l cn c pha long n khong trn
hoc thp hn phn tch. Mu cha cadmi ln hn 20 mg/l cn pha long trc khi phn
tch.
Gii hn pht hin ca phng php ph thuc vo mu v c th thay i theo thnh
phn mu. Gii hn pht hin i vi antimoan/stibi cng ph thuc vo cch ph mu c
dng v c th cao hn s liu nu trong Bng 1. Gii hn pht hin cho cc kim loi c th
khc bit vi s liu nu trong bng khi ph mu bng HF.
S phc tp ca hng dn ny l nhm thu c nhng kt qu tin cy. Cc nh phn
tch cn c kinh nghim tt c cc bc t khi ly mu, x l, chun b thuc th n tun
th y cc bin php an ton v s dng cc phng tin bo v c nhn.
2. Nguyn tc ca phng php:
Mu c ly ng tc t ngun. i vi mu bi th ly bng u ly mu cha ci lc
c lm nng, i vi mu kh th ly mu trong dy bnh c lm lnh, hai bnh trng,
hai bnh cha dung dch axit nitric long v hydro peroxyt, hai bnh khc cha dung dch
KMnO4 v axit sunfuric, bnh cui cng cha cht lm kh.
Cc thnh phn trong h thng ly mu c thu hi v ph mu ring theo na trc
v na sau ca h thng ly mu. Kim loi thu c trong h thng ly mu c ha tan
trong axit cc cht v c tan ht cn cc cht hu c c th cn tr vic phn tch b loi i.
Dung dch axit nitric v hydro peroxyt, dung dch HCl dng trng, dung dch
KMnO4 trong mi trng axit v dung dch trng u ly mu v dung dch ph mu trn ci
KTPT03-KT-Phn tch kim loi nng

Trang 2

lc cng c dng phn tch thy ngn bng phng php ph hp th nguyn t ha hi
lnh. Ton b by trong h thng ly mu, tr dung dch kali permanganat, dung dch trng
HCl v nc thu thy ngn, c th dng phn tch cc kim loi cho trong Bng 1 bng
quang ph hp th nguyn t ngn la, quang ph hp th nguyn t vi cuvet graphit.
thun tin, phn ht ca phn 1A v phn 2A c th kt hp li phn tch. Phn
1A thng c pha long n 300ml trc khi phn tch v phn 2A c pha long n 150
ml trc khi phn tch. Vic kt hp cn tun theo t l gia phn 1A v 2A.
Hiu qu ca phng php phn tch c nh gi qua mu kim tra hoc o cht
lng ca phng php ny gm c kim tra hiu ng nn.
3. Cc yu t cn tr:
St (Fe) c th l mt s can thip quang ph trong phn tch ca As, Cr, v Cd
Nhm (Al) c th l mt s can thip quang ph trong phn tch ca As v Pb
4. Ti liu tham kho:
USEPA Method 29: Determination of Metal Emissions from Stationary Sources.
TCVN 7557:2005: L t Cht Thi Rn Y T - Xc nh Kim Loi Nng Trong Kh
Thi Phn 1: Quy nh Chung.
Hng dn s dng my quang ph hp thu nguyn t AAS.
5. Thit b, ha cht:
Disclaimer. Phng php ny c th lin quan n vt liu nguy him, hot ng v
trang thit b. iu ny phng php th nghim c th khng gii quyt tt c cc vn an
ton lin quan n vic s dng n. N l trch nhim ca ngi s dng cc phng php th
nghim ny thit lp thc hnh an ton v sc khe ph hp v xc nh kh nng p
dng cc gii hn quy nh trc khi thc hin phng php th nghim ny.
Thuc th n mn. Cc thuc th sau l nguy him. Thit b bo v c nhn v th tc
an ton l hu ch trong vic ngn nga hin tng bn te ha hc. Nu tip xc xy ra, ngay
lp tc tun ra vi tht nhiu nc t nht 15 pht. Ci qun o di vi sen v
kh trng. iu tr bng ha hc cn st li nh bng nhit.
5.1.

Ha cht

KTPT03-KT-Phn tch kim loi nng

Trang 3

Trong phn tch, tr khi c nhng quy nh khc, ch s dng thuc th c tinh khit
c tha nhn.
V nng axit nh hng ti vic o hp th ca cc kim loi nn cc dung dch
, k c dung dch tiu chun v dung dch trng u phi c cng nng axit.
5.1.1. Nc ct: hoc nc loi khong hoc nc c tinh khit tng ng
Theo TCVN 4851 : 1989 (ISO 3696).
5.1.2. Axit clohydric c (HCl) p = 1,16 g/ml (37%)
5.1.3. Axit nitric c (HNO3) p = 1,42 g/ml
5.1.4. Axit nitric (0,1 M): Va thm va khuy 6,3 ml axit nitric c vo bnh cha khong
900 ml nc. Pha long n 1000 ml bng nc. Trn u. Dung dch phi t hn 2 g/l
i vi mi kim loi.
5.1.5. Axit nitric 10 % (th tch): Va thm va khuy 500 ml HNO3 c vo bnh cha
khong 4000 ml nc. Pha long n 5000 ml bng nc. Trn u. Dung dch phi t
hn 2 g/l i vi mi kim loi.
5.1.6. Axit nitric 5 % (th tch): Va thm va khuy 50 ml HNO3 c vo 800 ml nc.
Pha long n 1000 ml bng nc. Dung dch phi t hn 2 g/l i vi mi kim loi.
5.1.7. Axit nitric 50 % (th tch): Va thm va khuy 125 ml HNO3 c vo bnh cha
khong 100 ml nc. Pha long n 250 ml bng nc. Trn u. Dung dch phi t hn
2 g/l i vi mi kim loi.
5.1.8. Dung dch hp th HNO3 5 % (th tch)/ H2O2 10 % (th tch): Va thm cn thn
va khuy 50 ml HNO3 c vo bnh nh mc 1000 ml c cha 500 ml nc. Thm
cn thn 333 ml H2O2 30 % vo bnh. Thm nc n vch. Dung dch phi t hn 2
g/l i vi mi kim loi.
5.1.9. Axit HCl 8 M: Thm cn thn, va thm va khuy 690 ml HCl c vo bnh cha 250
ml nc. Pha long n 1000 ml bng nc. Trn u. Dung dch phi t hn 2 g/l Hg.
5.1.10.Hydro peroxyt c 30 % (th tch).
5.1.11.Kali permanganat 5 % (khi lng trn th tch).
5.1.12.Dung dch hp thu KMnO4 4 % (khi lng trn th tch) + H2SO4 10 % (th tch):
Trn cn thn 100 ml H2SO4 c vo 800 ml nc. Va thm nc n 1000 ml va
KTPT03-KT-Phn tch kim loi nng

Trang 4

khuy. Dung dch ny l H2SO4 10 % (th tch). Ha tan khi khuy 40 g KMnO 4 vo
dung dch H2SO4 10 %. Thm nc n 1 lt. Pha v gi trong bnh thy tinh trnh
phn hy. Dung dch phi t hn 2 g Hg/l.
Chun b dung dch hng ngy.
Ch Thch: gim s t phn hy ca dung dch permanganat, lc dung dch qua giy
lc What - man 541. Do phn ng ca KMnO 4 vi axit sinh kh trong bnh cha nn cc bnh
ny khng c y v cn thng hi trnh n. Thng hi l cn nhng trnh dung
dch b nhim bn. Nn dng np c khoan l 70 - 72 v ng dn bng teflon.
5.1.13.Axit sunfuric (H2SO4) c p = 1,84 g/ml (98%)
5.1.14.Silicagen v nc : theo TCVN 7557-2 : 2005.
5.1.15.Axit flohydric HF c.
5.1.16.Dung dch chun
Hg chun (AAS Grade), 1000 mg /ml.
Pb chun (AAS Grade), 1000 mg /ml.
Kh chun (AAS Grade), 1000 mg /ml.
Cd tiu chun (AAS Grade), 1000 mg /ml.
Cr chun (AAS Grade), 1000 mg /ml.
Sb chun (AAS Grade), 1000 mg /ml.
Co Standard (AAS Grade), 1000 mg /ml.
Cu chun (AAS Grade), 1000 mg /ml.
Mn chun (AAS Grade), 1000 mg /ml.
Ni tiu chun (AAS Grade), 1000 mg /ml.
Se chun (AAS Grade), 1000 mg /ml.
Ag chun (AAS Grade), 1000 mg /ml.
Zn chun (AAS Grade), 1000 mg /ml.
Fe tiu chun (AAS Grade), 1000 mg /ml

KTPT03-KT-Phn tch kim loi nng

Trang 5

5.2.

Thit b:
H thng my quang ph hp thu nguyn t AAS.
-

H thng AA - Hydride (quang ph pht x nguyn t ICP-AES).

H thng AA - cuvet graphit.

H thng AA Flame (AA-Ngn la).

Cc loi bnh nh mc, pipet cc loi.

Cc loi dng c th nghim khc trong phng th nghim.
6. Tin hnh phn tch:
6.1.

Chun b mu th
Kim vin sau khi tip nhn mu t on quan trc tn hnh kim tra i chiu cc vch

th tch trn cc bnh mu c ging vi khi chp trong bin ban khng.
6.1.1. Bnh cha s 1 (mu Filter-ci lc):
Nu cn xc nh pht thi bi th lm kh ci lc v ci by lc n khi lng khng
i. phn tch kim loi th chia ci lc v by lc thnh nhiu phn, mi phn khong 0,5g
t vo bnh chu p lc hoc bnh ph mu chu p lc. Thm vo mi bnh 6ml HNO 3 c v
4 ml HF c. Ph mu bng vi sng, hoc t vo bnh ph mu chu p lc 140 0C (2850F)
trong 6 h. ngui mu n nhit phng v trn vi phn trng u ly mu ph theo
6.1.3.
HF l rt c nn cn phi cn thn khi thao tc s dng.
6.1.2. Bnh cha s 2 (axeton trng):
o cht lng trong bnh cha ny theo th tch chnh xc n 1 ml hoc khi lng
n 0,5 g. Chuyn sang cc 250 ml trng axit v cn trc ri cho bay hi n kh
nhit v p sut thng. Nu cn phn tch bi th lm kh bng cht lm kh trong 24 h
(khng dng nhit) n khi lng khng i theo phng php xc nh thy ngn v cng
b kt qu chnh xc n 0,1mg. Ha tan cn bng 10 ml HNO 3 c v nhp ton b cht lng
v rn vo bnh cha s 3 va lm va khuy v bt u lm theo iu 6.1.3.

KTPT03-KT-Phn tch kim loi nng

Trang 6

6.1.3. Bnh cha s 3 (trng u ly mu):

pH ca mu phi l 2 hoc thp hn. Nu pH ln hn 2 phi thm HNO 3 mt cch cn
thn, khi khuy, n pH = 2. Mu c chuyn vo cc cha nc v c y bng np knh
ng h. Th tch mu c c trn bp nhit thp hn nhit si n khi cn 20 ml v
ph mu bng mt trong cch sau:
- Ph mu bng vi sng hoc bnh ph mu chu c p lc 140 0C (2850F) n khi
mu cn 20ml.
Trn mu va ph xong vi mu ph mc 6.1.1. Mu kt hp l Phn 1
Lc dung dch kt hp gia dung dch ph mu ci lc v dung dch trng u ly mu
qua giy lc Whatman 541. Pha long n 300 ml (hoc th tch thch hp ty theo nng
kim loi) bng nc. Dung dch sau khi pha long l Phn 1. o v ghi th tch ca Phn 1
chnh xc n 0,1ml.
- Ly chnh xc 50 ml v gi l Phn 1B.
- nh du 250ml cn li l Phn 1A. Phn 1A c dng cho phn tch ph pht x
nguyn t plasma, khi ph plasma hoc quang ph hp th nguyn t cho tt c cc kim loi,
tr Hg. Phn 1B dng xc nh Hg na trc ca h thng ly mu.
6.1.4. Bnh cha s 4 (Bnh 1 n 3, bnh HNO3/H2O2 v bnh o m nu c, v dung dch
trng):
o v ghi th tch tng ca mu (Phn 2) chnh xc n 0,5ml. Ly 75ml n 100ml
phn tch Hg, gi l Phn 2B.
nh du phn cn li l Phn 2A. Ton b Phn 2A c ph mu v c cn, phn c
ny dng phn tch cc kim loi tr Hg. Phn 2A c pH = 2 hoc nh hn, nu cn, iu
chnh bng HNO3 n pH = 2. Chuyn vo cc cha nc v y bng np knh ng h. C
trn bp nhit thp hn nhit si n th tch 20ml. Ph mu bng axit theo phng
php m t trong iu ny hoc theo mt trong cc phng php c m t trong Ph lc E,
F, G ca TCVN 7557-2: 2005.
Ph mu phn 2A:Thm 30ml HNO 3 50% vo, V c trn mt tm nng ngay di
si trong 30min. Thm 10ml H2O2 30% v ung thm trong 10pht. Thm 50ml nc nng,
lm nng mu trn thm 20 pht. Lm lnh mu v nhit phng, lcmu, v pha long n
KTPT03-KT-Phn tch kim loi nng

Trang 7

150 ml (hoc khi lng thch hp cho cc kim loi d kin nng ) vi nc. Pha long ny
to ra phn tch Phn s 2A. o lng v ghi li th tch chnh xc n 0,1ml
6.1.5. Bnh cha s 5A, 5B v 5C (bnh 4, 5 v 6). ring cc mu ny:
o v ghi th tch 5A v 5B chnh xc n 0,5 ml. Pha long 5C n 500 ml bng nc.
Nh vy c Phn 3A, 3B v 3C.
V dung dch trng kali pecmanganat trong mi trng axit v nc cha lng ln Hg
t bnh permanganat, lng Hg trong dung dch trng HCl (Phn 3C) c th rt nh. Tuy
nhin, nh ni phn u ca phng php ny, cng phn Hg Phn 3C vo Phn 1B,
2B, 3A v 3B tnh Hg tng s.
6.1.6. Bnh cha s 6 (Silicagen): Cn silicagen dng (hoc silicagen cng vi bnh) chnh
xc n 0,5g bng cn. (Giai on ny c th lm ti hin trng).
6.2.

Phn tch mu:

6.2.1 Vi mi h thng ly mu cn phn tch by bnh ring. Mt s nhn mu, chun b

v phn tch c m t Hnh 3.3. Hai mu u, gi l Phn 1A v 1B, gm cc mu
ha tan na trc h thng.
- Phn 1A dng phn tch quang ph pht x nguyn t plasma v quang ph hp th
nguyn t.
- Phn 1B dng phn tch Hg na trc.
6.2.2 Na sau ca h thng dng bnh th by chun b mu th ba. Mu th ba v bn,
dn nhn 2A v 2B, cha mu nc do m v HNO 3/H2O2 t bnh 1 n bnh 3. Phn
2A dng cho phn tch quang ph pht x nguyn t plasma v quang ph hp th
nguyn t. Phn 2B dng phn tch Hg.
6.2.3 Mu 5A, 5B v 5C c dn nhn Phn 3A, 3B v 3C. Chng cha cht v dung dch
trng ca bnh trng 4 v kali pecmanganat trong mi trng axit bnh 5 v 6. Cc
mu ny dng phn tch Hg. Thy ngn tng s na sau ca h thng l tng s t
cc phn 2B, Phn 3A, 3B v 3C.
6.2.4 u tin phn tch tt c cc mu cho cc kim loi tr Hg. Nu c st v nhm th cc
mu cn c pha long nng Fe, Al nh hn 50 ppm gim cn tr i vi
asen, cadmi, crom v ch.
KTPT03-KT-Phn tch kim loi nng

Trang 8

Ch Thch: Khi phn tch mu trong HF cn dng n Al. Cc mu na trc h thng

u cha HF cn dng n Al.
6.2.5 Phn tch trn h thng AAS:
AA (quang ph hp th nguyn t) ht trc tip hoc dng cuvet graphit. Nu phn tch
Phn 1A v 2A dng cuvet graphit hoc ht trc tip th cn xem bng A-2 bit nhng cn
tr c th c v k thut gim thiu.
AA phn tch Hg bng nguyn t ha hi lnh. Phn 1B, 2B, 3A, 3B v 3C dng phn
tch ring r Hg bng quang ph hp th nguyn t k thut ha hi lnh.
Nu khng bit trc khong nng Hg th pha long 1ml n 10ml mu u thnh
100ml. Ghi r s mililit dng pha long thnh 100ml.
xc nh Hg trong pht thi, lng mu cn ly pha long ph thuc nng Hg:
lng mu cn ly pha long v phn tch phi di 1g Hg v nm trong ng chun (t
0 ng n 1000 ng).
Cc thao tc vn hnh trn my AAS u do cn b c chuyn mn vn hnh.
7. Tnh ton:
Kt qu phn tch c phn mm ca my AAS tnh ton v cho ra kt qu, kt qu ny
c lu li v ghi vo phiu bo co kt qu.
Cng thc tnh tay da trn ng chun:
Th tch kh kh. Dng s liu t php th ny tnh Vm(std), th tch mu kh kh iu
kin tiu chun nh cho 6.3 phng php xc nh thy ngn.
Th tch hi nc v m. Dng cc d liu thu c php th ny tnh th tch
hi nc Vw(std) v m Bws ca ng khi. Dng phng trnh 5-2 v 5-3 phng php xc
nh thy ngn.
Tc kh trong ng khi. Dng s liu ca php th ny v phng trnh 2-9 ca
phng php 2 tnh tc kh trung bnh trong ng khi.
Kim loi (tr Hg) trong mu
7.1.

Phn 1A, na trc, kim loi (tr Hg). Tnh ton lng tng kim loi trong Phn 1 ca
h thng ly mu theo phng trnh:

KTPT03-KT-Phn tch kim loi nng

Trang 9

M fh=C a 1 F d V soln1 (1)

Trong :
Mfh l khi lng tng ca mi kim loi (tr Hg) thu c na trc ca h thng
(Phn 1), tnh bng microgram.
Ca1 l nng ca kim loi trong Phn 1A, tra t ng chun, tnh bng microgram trn
mililit.
Fd l h s pha long (Fd = nghch o ca phn s dung dch c v dung dch thc dng
khi c c nng C a1, th d, khi pha long 2 ml dung dch phn 1A thnh 10 ml th F d =
5).
Vsol.1 l th tch tng ca dung dch mu c ph (Phn 1), tnh bng mililit.
7.2.

Phn 2A, na sau, kim loi (tr Hg). Tnh ton lng mi kim loi trong phn 2 theo
phng trnh:
M bh=C a2 F a V soln 2 (2)

Trong :
Mbh l khi lng tng tng kim loi (tr Hg) thu c na sau ca h thng ly mu
(Phn 2), tnh bng microgam;
Ca2 l nng ca kim loi mu cha pha long Phn 2A, tra t ng chun tnh bng
microgram trn mililit;
Fa l h s phn ht, th tch Phn 2 chia cho th tch phn ht Phn 2A. Xem 6.1.4;
Va l th tch tng s ca dung dch mu c ph (Phn 2A c), tnh bng mililit. Xem
6.1.4.
7.3.

Tng s kim loi (tr Hg). Tnh tng lng kim loi trong h thng ly mu nh sau:
Mt = (Mfh - Mfhb) + (Mbh - Mbnb) (3)
Trong :
Mt l khi lng tng cc kim loi thu c trong h thng ly mu, tnh bng

microgam;

KTPT03-KT-Phn tch kim loi nng

Trang 10

Mfhb l gi tr hiu chnh trng ca kim loi na trc, tnh bng microgam;
Mbhb l gi tr hiu chnh trng ca kim loi na sau, tnh bng microgam.
7.4.

Thy ngn trong mu

7.4.1 Phn 1B, na trc, Hg. Tnh ton lng thy ngn thu c na trc, Phn 1, ca
h thng ly mu theo phng trnh:
Hgth = x Vso ln.1

(4)

trong :
Hggh l khi lng tng ca Hg na trc ca h thng ly mu (Phn 1), g;
Qth l lng Hg trong mu phn tch, tnh bng microgam;
Vsoln.1 l th tch tng ca mu c ph (Phn 1), tnh bng mililit;
Vf1B l th tch Phn 1B em phn tch, tnh bng mililit. Xem ch thch.
Ch Thch: Vf1B l th tch Phn 1B c phn tch. Nu 1 ml ca phn 1B c pha
long n 100 ml ph hp vi khong o th Vf1B s l 1/100 = 0,01.
7.4.2 Cc phn 2B, 3A, 3B v 3C, na sau, Hg. Tnh ton lng Hg Phn 2 bng phng
trnh 5 v Phn 3A, 3B v 3C bng phng trnh 6. Tnh lng Hg tng s na sau
ca h thng ly mu bng phng trnh 7.
Hgbh2 = x Vso ln.2 (5)
Trong :
Hgbh2 l tng lng Hg thu c Phn 2, tnh bng microgam;
Qbh2 l lng Hg trong mu phn tch, tnh bng microgam;
Vsoln.2 l th tch tng ca Phn 2, tnh bng mililit;
Vf2b l th tch Phn 2B c phn tch, tnh bng mililit (xem ch thch).
Ch Thch: Vf2b l lng thc t ca phn 2B c phn tch. Th d, nu 1 ml ca
Phn 2B c pha long thnh 10 ml m bo nm trong khong phn tch v ly 5 ml
phn tch, Vf2b s l 0,5. Dng phng trnh 6 tnh lng Hg na sau ca Phn 3A, 3B v
3C.
Hgbh3(A,B,C) = x Vso ln,3(A, B, C) (6)
KTPT03-KT-Phn tch kim loi nng

Trang 11

Trong :
Hgbh3

(A, B, C)

l tng lng Hg thu c tng Phn 3A, 3B hoc 3C, tnh bng

microgam;
Qbh(A, B, C) l lng Hg phn tch c, tnh bng microgam;
Vf3(A, B, C) l th tch Phn 3A, 3B, 3C em phn tch, tnh bng mililit. (xem cch tnh
ging trn);
Vsoln,3(A, B, C) l th tch tng Phn 3A, 3B, hoc 3C, ml.
Hgbh = Hggh2 + Hgbh3A + Hgbh3B + Hbh3C (7)
trong :
Hgbh l tng lng Hg thu c na sau ca h thng ly mu, tnh bng microgam.
7.4.3 Tng lng Hg trong h thng ly mu. Tnh lng tng s ca Hg trong h thng ly
mu bng phng trnh 8.
Hgt = (Hgfh - Hgfhb) + (Hgbh - Hgbhb) (8)
Trong :
Hgt l tng lng Hg thu c trong h thng ly mu, tnh bng microgam;
Hgfhb l gi tr hiu chnh mu trng ca Hg thu c na trc, tnh bng microgam;
Hgbhb l gi tr hiu chnh mu trng ca Hg thu c na sau, tnh bng microgam.
Ch Thch: Nu tng gi tr hiu chnh (Hg fhb + Hgbhb) nm trong khong t 0 n 6 g
th tng ny c th dng hiu chnh mu (Hg fh + Hgbh); nu tng vt qu 6 g th dng s
ln hn trong hai s: 6 g hoc 5 % ca gi tr mu (Hgfg + Hgbh).
7.4.4 Nng kim loi trong kh ng khi. Tnh ring nng kim loi Cd, Cr, As, Ni, Mn,
Be, Co, Cu, Pb, P, TI, Ag, Ba, Zn, Se, Sb v Hg trong kh ng khi (khng iu kin
chun) nh sau:
Cs = K4 (Mt / Vm (std))
Trong :
Cs l nng mi kim loi trong kh ng khi, tnh bng miligam trn mt khi;
K4 l 10-3 tnh bng miligam trn microgam;
KTPT03-KT-Phn tch kim loi nng

Trang 12

Mt l tng lng mi kim loi thu c trong h thng ly mu, g (dng Hg t, tnh ton
thay cho Mt);
Vm(std) l th tch kh kh chuyn v iu kin chun, tnh bng mt khi.
7.4.5 Bin thin ng tc v kt qu chp nhn c Kt qu: 90% I 110%, kt qu chp
nhn c..

KTPT03-KT-Phn tch kim loi nng

Trang 13

8. Kim sot cht lng

8.1.
-

Mu trng.

Khi phn tch, cc mu trng Bnh s 7 n bnh s 12 c ph v phn tch nh sau: Ph

mu ci lc ca bnh cha 12 theo 6.1.1, 100 ml ca bnh cha s 7 theo 6.1.2, 100 ml ca
bnh cha s 8 theo 6.1.3. iu sinh ra phn mu trng 1A v phn mu trng 1B t phn
mu trng 1. (C th ph hai ci lc ring r theo 6.1.1, pha long ring n 300 ml v phn
tch ring, sinh ra hai gi tr trng cho phn mu trng 1A v phn mu trng 1B. Ba gi tr
phn mu trng 1A s c tnh nh ba gi tr ca M fhb trong phng trnh 3, sau ba gi tr
c cng li v chia 3 c gi tr M fhb dng tnh Mt theo phng trnh 3. Tng t, ba
gi tr ca Phn mu trng 1B c tnh ring r, cng li, ly trung bnh v c dng nh
gi tr Hgfhb trong phng trnh 8.

Phn tch hai ci lc khc l ty chn v phng php ny khng yu cu nhng nu phn tch
th kt qu c xem nh trn). Kt hp 100 ml ca bnh cha 8A vi 200 ml ca bnh cha
9 ri ph theo 6.1.4. iu sinh ra phn mu trng 2A v phn mu trng 2B t phn mu
trng 2. 100ml ca bnh cha s 8A l phn mu trng 3A. Kt hp 100ml ca bnh cha s10
vi 33ml ca bnh cha 8B c phn mu trng 3B. (Dng 400 ml phn mu trng 3B khi
tnh gi tr trng. Dng th tch hin ti khi tnh ton cc gi tr trng khc). Pha long 225 ml
ca bnh cha 11 n 500 ml bng nc c phn mu trng 3C. Phn tch 1A cho gi tr
hiu chnh trng na trc ca h thng, tr Hg, phn tch phn mu trng 1B cho gi tr hiu
chnh trng cho Hg na trc ca h thng. Phn tch phn mu trng 2A cho gi tr hiu
chnh cho cc kim loi t Hg ca na sau h thng. Phn tch ring phn mu trng 2B v 3
cho ta gi tr hiu chnh cho Hg na sau ca h thng.
8.2.

Mu kim sot cht lng. Cc mu sau dng phn tch kim sot cht lng.

8.2.1 Phn tch AA ht trc tip hoc dng cuvet graphit Sb, As, Ba, Be, Cd, Cr, Co, Cu, Pb,
Ni, Mn, Hg, P, Se, Ag, Tl v Zn. Tt c cc mu u c phn tch kp. Phn tch li
mt mu bt k t ph mu ca na trc v mt ca na sau. Nu kt qu nm ngoi
khong 75 % v 125 % th cn phn tch tng mu bng phng php thm chun.
8.2.2 Phn tch Hg bng AA dng k thut ha hi lnh. Tt c cc mu u phn tch kp.
Phn tch li mt mu ca bnh axit nitric k t cng on ph dng phng php
ng chun. Kt qu phi nm trong khong 25 %, nu khng th cc mu cn c
lm theo phng php thm chun.
KTPT03-KT-Phn tch kim loi nng

Trang 14

9. Hiu qu ca phng php

9.1.

m bo nhy cc php o, nng kim loi nn cao hn t nht 10 ln gii

hn pht hin. Trong mt s trng hp v khi ht sc ch trong phng php phn
tch nng c th khong ba ln gii hn pht hin. Trong mi trng hp nn
phn tch t nht mt mu kp cho cc kim loi, dng phng php thm (MSA), pha
long hng lot, hoc thm cht nn m bo cht lng cc s liu.

9.2.

Phng php xc nh gii hn pht hin da trn cc thng s ngun mu v cc kt

qu phn tch. Nu cn th gii hn pht hin c th nhy hn l ch ra Bng 3.2 bng
cch:
Ly mu kh 1 h vi th tch khong 1,25 m 3. Nu thi gian tng v ly n 5 m 3 th

gii hn pht hin s l 1/4 gi tr ca Bng 2 (ngha l phng php nhy hn 4 ln so vi ly

mu 1 h).
Gii hn pht hin c lm vi gi thit l tt c cc mu u c ph (tr phn ht
ca Hg) v th tch cht lng cui cng l 300 ml i vi na trc (phn 1) v 150 ml vi
na sau (phn 2A). Nu th tch ca na trc c c t 300 ml xung cn 30 ml, gii hn
pht hin s l 1/10 ca gi tr trn (nhy hn 10 ln). Nu th tch na sau c t 150 ml xung
cn 25 ml, gii hn pht hin l 1/6 gi tr trn. Hiu ng nn rt quan trng nht l khi mu
c c c hn bnh thng. Gim th tch xung di 25 ml lm kh cho vic ha tan cn
v tng cn tr do cc hp cht khc.
Khi c hai ci tin trn c p dng ng thi cho mt mu th kt qu ci tin c
nhn ln. Th d, khi th tch mu tng 5 ln v th tch ph mu ca na trc v na sau
gim 6 ln th gii hn pht hin s gim 30 ln (phng php nhy hn 30 ln).
Ngc li, gim th tch mu kh v tng th tch cht lng s lm tng gii hn pht
hin (ngha l phng php s km nhy hn). Mu na trc v na sau (phn 1A v 2A) c
th kt hp theo t l trc khi phn tch. Ghi th tch cht lng to ra (tr ca Hg, n cn
c phn tch ring). Kt hp mu nh vy khng cho php xc nh (k c na trc v na
sau) mu c ly u trong h thng.
Gii hn pht hin nh vy tr nn gi tr n cho cc kim loi tr Hg, tuy vn phi ch
ti phn ng gp ca Hg.
Nhng tho lun trn khng bn n hiu chnh trng.
KTPT03-KT-Phn tch kim loi nng

Trang 15

Bng 3.2 - Gii hn pht hin (g/m 3) i vi phn mu ca h thng ly mu s dng

phng php ICP-AES v AAS

Kim loi

Na trc ca
h thng ly
mu Phn 1
u ly mu &
ci lc

Na sau ca h
thng ly mu
Phn 2
Bnh hp thu
(impinger) 1 - 3

Na sau ca h
thng ly mu
Phn 3
Bnh hp thu
(impinger) 4 - 5

Antimoan/Stibi
(Sb)

7,7 (0,7) *

3,8 (0,4) *

11,5 (1,1) *

Asen (As)

12,7 (0,3) *

6,4 (0,1) *

19,1 (0,4) *

Bari (Ba)

0,5

0,3

0,8

Beri (Be)

0,07 (0,05) *

0,04 (0,03) *

0,11 (0,08) *

Cadmi (Cd)

1,0 (0,02) *

0,5 (0,01) *

1,5 (0,03) *

Crom (Cr) tng

1,7 (0,2) *

0,8 (0,1) *

2,5 (0,3) *

Coban (Co)

1,7 (0,2) *

0,8 (0,1) *

2,5 (0,3) *

ng (Cu)

1,4

0,7

2,1

Ch (Pb)

10,1 (0,2) *

5,0 (0,1) *

15,1 (0,3) *

Mangan (Mn)

0,5 (0,2) *

0,2 (0,1) *

0,7 (0,3) *

Thy ngn (Hg)

0,6**

3,0**

Niken (Ni)

3,6

1,8

5,4

Phospho (P)

18,0

9,0

27,0

Selen (Se)

18,0 (0,5) *

9,0 (0,3) *

27 (0,8) *

Bc (Ag)

1,7

0,9

2,6

Tali (TI)

9,6 (0,2) *

4,8 (0,1) *

14,4 (0,3) *

Km (Zn)

0,5

0,3

0,8

2,0**

Ton b h
thng ly mu

5,6**

Ch thch 1:
()*: Gii hn pht hin khi phn tch bng GF-AAS.
**: Gii hn pht hin khi phn tch bng CV- AAS, c tnh i vi na sau v ton
b h thng ly mu.
KTPT03-KT-Phn tch kim loi nng

Trang 16

Ch Thch 2:
Thng thng, gii hn pht hin c xc nh da vo cc thng s thc t v kt
qu phn tch c m t iu bn trn iu ny.
9.3.

Dng (1) cch tin hnh ca phng php, (2) gii hn pht hin trnh by iu 1, (3)
th tch 300 ml vi na trc v 150ml vi na sau v (4) mu kh 1,25 m 3, gii hn
pht hin nh trn Bng 2, c tnh nh sau:

=D
Trong :
A l gii hn pht hin phn tch, tnh bng microgam trn mililit;
B l th tch mu dng cho phn tch, tnh bng mililit;
C l th tch mu kh, dscm (dsm3);
D l gii hn pht hin trong ng khi, tnh bng microgam trn mt khi.
Gi tr Bng 3.2 c tnh cho na trc, na sau v ton b h thng.
10. An ton trong qu trnh quan trc:
Trang b y cc trang thit b bo h lao ng cho cc thnh vin trong nhm quan
trc khi lm vic.
Lun m bo tnh an ton khi thao tc vi acid, v cc ha cht khc.
Lun tun th cc quy nh v an ton lao ng, quy nh v PCCC trong sut qu trnh
t lc bt u n kt thc t quan trc.
ng Nai, Ngy 30 thng 07 nm 2016
Ngi bin son

Trng PTN

Qun l cht lng

V Th H

V Th H

Phm Th Hi Yn

KTPT03-KT-Phn tch kim loi nng

Trang 17