TIU CHUN VIT NAM

TCVN 7557-3 : 2005

L T CHT THI RN Y T - XC NH KIM LOI NNG TRONG KH THI PHN 3: PHNG PHP XC NH NNG CADMI V CH BNG QUANG PH
HP TH NGUYN T NGN LA V KHNG NGN LA
Health care solid waste incinerators - Determination of heavy metals in fluegas Part 3: Determination of cadmium and lead concentrations by flame and electrothermal atomic
absorption spectrometric method
Li ni u
TCVN 7557-3 : 2005 hon ton tng ng MDHS 10 v MDHS 6 - Vng quc Anh v k
thut nhng c thay i v bin tp.
TCVN 7557 - 3 : 2005 do Tiu ban k thut Tiu chun TCVN/TC146/ SC2 "L t cht thi
rn y t" bin son trn c s d tho ngh ca Vin Y hc lao ng v V sinh mi trng B Y t, Tng cc Tiu chun o lng Cht lng xt duyt, B Khoa hc v Cng ngh ban
hnh.
TCVN 7557 gm cc tiu chun sau, vi tn chung L t cht thi rn y t - Xc nh kim loi
nng trong kh thi.
TCVN 7557-1 : 2005, Phn 1: Quy nh chung.
TCVN 7557-2 : 2005, Phn 2: Phng php xc nh nng thy ngn bng phng php
quang ph hp th nguyn t k thut ha hi lnh.
TCVN 7557-3 : 2005, Phn 3: Phng php xc nh nng cadmi v ch bng quang ph hp
th nguyn t ngn la v khng ngn la.

L T CHT THI RN Y T - XC NH KIM LOI NNG TRONG KH THI

PHN 3: PHNG PHP XC NH NNG CADMI V CH BNG QUANG PH
HP TH NGUYN T NGN LA V KHNG NGN LA
Health care solid waste incinerators - Determination of heavy metals in fluegas Part 3: Determination of cadmium and lead concentrations in fluegas by flame and
electrothermal atomic absorption spectrometric method
Cnh bo:

- Cc nh ha hc hoc k thut vin p dng tiu chun ny phi c o to, hun

luyn v c kinh nghim.
- Cn ch c bit n c tnh ca cc kim loi nng, cc dung dch ca chng v cc
thuc th dng trong phn tch. Cn cn trng khi s dng v thi b cc dung dch sau
khi phn tch. Cc ha cht c bay hi phi thao tc trong t ht c v khng c ht
cc thuc th bng mm khi dng pipet. Phng nga cc phn ng gia cht oxy ha vi
cht kh nh kali permanganat v H2O2 to hn hp n.
- Khi lm vic phi s dng y cc phng tin bo v c nhn nh gng tay, khu
trang, co chong, tp d cao su, mt n phng c
1. Phm vi p dng
1.1. Tiu chun ny quy nh phng php quang ph hp th nguyn t ngn la (F-AAS) v
khng ngn la (GF-AAS) xc nh nng 2 kim loi nng l cadmi (Cd) v ch (Pb) trong
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.
CH THCH: Nhit v p sut tiu chun l nhit 0 0C v p dng 101,3 kPa.
Phng php ny thch hp xc nh cadmin v ch trong kh thi (bi v khi):
a. Cadmi:
- Gii hn pht hin: 0,0015 mg/m3 (c tnh bng 10 ln lch chun).
- chnh xc ca phng php > 10 % trong khong nng t 0,025 mg/m3 n 0,1 mg/m3.
- Cn tr: khng pht hin c cht cn tr.
b) Ch:
- Gii hn pht hin: 0,01 mg/m3 (c tnh bng 10 ln lch chun).
- chnh xc ca phng php > 10 % trong khong nng t 0,075 mg/m3 n 0,03 mg/m3.
- Cn tr: Khi phn tch ch bng AAS dng ngn la khng kh - axetylen di bc sng
217,0 nm, nu c antimoan s b cn tr v antimoan hp th bc sng 217,6 nm, khi ch
cn c o bc sng 283,3 nm. Mt s anion gy cn tr nh phosphat, cacbonat, iodua,
florua v axetat. Cc anion ny lm gim hp th ca ch khi nng ca chng gp 10 ln
nng ch. Cn tr ny c th gim ng k khi thm dung dch axit etylendiamin tetraaxetic.
C th xc nh cadmi v ch bng 2 phng php:
Phng php A - Phng php quang ph hp th nguyn t khng ngn la (AAS-GF).

Phng php B - Phng php quang ph hp th nguyn t ngn la (F-AAS).

Gii hn pht hin ca cc phng php ph thuc vo mu v c th thay i thnh phn mu.
Gii hn pht hin cho cc kim loi c th khc bit vi s liu nu trong bng khi ph mu bng
HF.
Cc phng php trn cng c th dng cho nhng nng cadmi v ch cao hn bng cch pha
long mu hoc cng c th xc nh c nhng nng thp hn bng cch axit ha v c
cn thn mu (lm giu mu).
Nhiu bc tin hnh trong quy trnh xc nh v thuc th c dng cho c phng php v
cho cc nguyn t khc nhau trong mt phng php. V vy ngi s dng tiu chun cn c
cn thn ton b tiu chun trc khi thc hin bt k bc tin hnh no trong tiu chun ny.
2. Ti liu vin dn
Cc ti liu vin dn sau l rt cn thit cho vic p dng tiu chun. i vi cc ti liu vin dn
ghi nm ban hnh th p dng bn c nu. i vi cc ti liu vin dn khng ghi nm ban
hnh th p dng phin bn mi nht.
TCVN 4851 : 1989 (ISO 3696). Nc dng phn tch trong phng th nghim - Yu cu k
thut v phng php th.
TCVN 5977, S pht thi ca ngun tnh - Xc nh nng v lu ng bi trong cc ng dn
kh - Phng php khi lng th cng.
TCVN 7557-1 : 2005, L t cht thi rn y t - Phng php ly mu cc kim loi trong kh
thi.
TCVN 7557-2 : 2005, L t cht thi rn y t - Phng php xc nh nng thy ngn trong
kh thi bng phng php quang ph hp th nguyn t k thut ha hi lnh.
4. Thit b dng c
Dng c thng thng phng th nghim v cc thit b sau:
4.1. H thng ly mu
Theo 4.1 TCVN 7557-1 : 2005
4.2. My quang ph hp th nguyn t
4.2.1. i vi phng php A - Quang ph thp th nguyn t khng ngn la (GF-AAS)

My quang ph hp th nguyn t c trang b b phn nguyn t ha nhit in ngun n

sc, n catot rng hoc n phng in khng in cc tng ng vi nguyn t cn xc nh
v hot ng theo hng dn ca nh sn xut, c hiu chnh nn, my tnh hoc my ghi tc
cao. Vic hiu chnh nn c s dng vi my quang ph hp th nguyn t c th l n D2
hoc hiu ng Zeeman.
CH THCH: Hiu chnh nn dteri thch hp vi cadmi v ch nu gii hn hiu chnh nn
i vi mt s thit b khng vt qu 0,6 n 0,8 hp th. Cn phi hiu chnh nn Zeeman
hoc Smith Hieftje i vi c hai nguyn t nu tn hiu nn cao. nng cao t s tn hiu phn
tch trn tn hiu nn, nn s dng cuvet graphit hot ha cng vi vic bin i nn mu, th
d bng amoni hydro phosphat (NH4)2HPO4, paladi kh hoc cht khc.
4.2.1.1. My quang ph hp th nguyn t dng cho xc nh cadmi:
Cn c trang b n catot lm cadmi, dng ngun sng lin tc nh n deuteri hoc vi
ngun sng lin tc khc. My c th hiu chnh (hoc b chnh) nn 228,8 nm dng ngun
sng lin tc nh n deuteri hoc dng hiu chnh nn Zeeman.
4.2.1.2. My quang ph hp th nguyn t dng cho xc nh ch:
Cn c trang b n catot rng ch, n t khng kh - axetylen. My c th hiu chnh (hoc
b chnh) nn 217,0 nm v 283,3 nm dng ngun sng lin tc nh n deuteri hoc dng hiu
chnh nn Zeeman.
4.2.2. i vi phng php B - Quang ph hp th nguyn t ngn la (F-AAS)
My quang ph hp th nguyn t phi c trang b: mt n catot rng hoc n phng in
khng in cc tng ng vi cadmin v ch cn xc nh (theo khuyn ngh v n ca nh sn
xut), mt h thng hiu chnh nn, mt n t thch hp vi ngn la khng kh/axetylen hoc
nit oxyt/axetylen (theo hng dn ca nh sn xut). Vic hiu chnh nn bng n dteri l k
thut ti thiu c chp nhn cho hiu chnh nn o bc sng thp hn 350 nm v mt n
halogen o bc sng trn 350 nm. Nhng h khc (nh phn cc Zeeman, Smith-Hieftje)
cng c chp nhn l bng nhau v trong nhng tnh hung nht nh c th tt hn.
Cnh bo: Phi tun th nghim ngt cc khuyn co v an ton ca hng sn xut thit b
khi s dng nhng ngn la .
4.3. H thng ly mu t ng
5. Thuc th
Trong phn tch, tr khi c nhng quy nh khc, ch s dng thuc th c tinh khit c
tha nhn,
CH THCH: V nng axit nh hng ti vic o hp th ca cc kim loi nn cc dung
dch o, k c chung dch tiu chun v dung dch trng phi c cng nng axit.

5.1. Nc ct hoc nc loi khong hoc nc c tinh khit tng ng

Nc ct hoc nc loi khng hoc nc c tinh khit tng ng theo TCVN
4851:1989 (ISO 3696).
Nc phi c in tr ln hn 0,5 mega om/cm, dn in nh hn 2m ho/cm.
Nc dng xc nh mu trng v chun b mu th, cc dung dch chun phi c nng
nguyn t cn xc nh khng ng k so vi nng thp nht ca nguyn t ny trong dung
dch mu.
5.2. Axit clohydric c (HCl) = 1,18 g/ml, (37%)
Phi s dng axit clohydric cng loi trong sut qu trnh th nghim.
5.3. Axit nitric c (HNO3) = 1,42 g/ml
Phi s dng axit nitric cng loi trong sut qu trnh th nghim.
5.4. Axit nitric (0,1 M): Thm khi 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 cha t hn 2 l/l i vi
mi kim loi.
5.5. Axit nitric 10 % (th tch): Thm khi khuy 500 ml HNO3 c vo bnh cha khong 4000
ml nc. Pha long n 5000 ml bng nc. Trn u. Dung dch phi cha t hn 2 l/l i vi
mi kim loi.
5.6. Axit nitric 5% (th tch): Thm khi khuy 50 ml HNO3 c vo 800 ml nc. Pha long
n 1000 ml bng nc. Dung dch phi cha t hn 2 l/l i vi mi kim loi.
5.7. Axit nitric 50 % (th tch): Thm khi khuy 125 ml HNO3 c vo bnh cha khong 100
ml nc. Pha long n 250 ml bng nc. Trn u dung dch phi cha t hn 2 g/l i vi
mi kim loi.
5.8. Dung dch hp th axit nitric (HNO3)/hydro peroxyt (H2O2) HNO3 5 %/H2O210%:
Thm cn thn khi 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 cha di 2
l/l mi kim loi.
5.9. Axit HCl 8 M: Thm cn thn khi khuy 690 ml HCl c vo bnh cha 250 ml nc. Pha
long n 1000 ml bng nc. Trn u. Dung dch phi cha t hn 2 g/l Hg.
5.10. Hydro peroxyt 30 % (th tch).
5.11. Kali permanganat 5 % (khi lng trn th tch)).

5.12. 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. Thm nc khi khuy n 1000 ml. Dung
dch ny l H2SO4 10% (th tch). Ha tan khi khuy 40 g KMnO4 vo dung dch H2SO4 10%.
Thm nc n 1 lt. Pha v gi trong bnh thy tinh trnh phn hy. Dung dch phi cha t
hn 2 g/l Hg.
Chun b dung dch trong 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 KMnO4, 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.
5.13. Axit sunfuric (H2SO4) c = 1,84 g/ml (98%)
Phi s dng axit sunfuric cng loi trong sut qu trnh th nghim.
5.14. Silicagen v nc : Xem TCVN 7557-2:2005.
5.14. Axit flohydric HF c.
Phi s dng axit flohydric cng loi trong sut qu trnh th nghim.
5.16. Dung dch trng/dung dch nn amoni axetat 10%
Dung dch ny nhm gim thiu cht cn tr v tng nhy phn tch.
5.17. Dung dch chun cadmi
5.17.1. Dung dch chun gc cadmi 1000 g/ml
Ha tan 1000 g/ml cadmi kim loi trong 50 ml HNO3 50% (th tch) trong mt bnh nh mc
1000 ml, thm nc va n vch mc.
5.17.2. Dung dch cadmi chun lm vic 20 g/ml
Dng pipet ht 2 ml dung dch chun gc niken 1000 g/ml cho vo bnh nh mc 100 ml, thm
5 ml HNO3 c phi t hn 2 g cadmi/l ri pha long n vch mc bng nc.
5.17.3. Axit nitric c = 1,4 g/ml, khong 65 %, phi t hn 2 g cadmi/l.
5.17.4. Axit nitric 5 %: Pha long axit nitric c ( = 1,42 g/ml) phi t hn 2 g cadmi/l vo
1000 ml nc. Lc u.

5.18. Dung dch chun ch

5.18.1. Dung dch ch chun gc 1000 g/ml
Ha tan 1,598 g ch nitrat (Pb/NO3)2) trong mt bnh nh mc 1000 ml vi mt lng nh (1
H2O + 1 HNO3), thm 10 ml HNO3 c v thm nc n vch mc.
5.18.2. Dung dch ch chun lm vic 50 g/ml
Thm 5ml dung dch Pb gc (4.1.4.1) vo 5ml axit nitric c phi t hn 2 g ch/l (d:1,4 g/ml).
nh mc n vch bnh nh mc 100 ml bng nc ct. Dung dch bn trong 1 nm.
6. Ly mu v x l mu
6.1. Ly mu
Theo 6.1 TCVN 7557 - 1 : 2005, v:
Th tch mu kh cn ly l 30 lt, thi gian ly mu t 15 min n 8h vi tc l 2 lt/min.
Cn chun ha bm ly mu, u ly mu v ci lc bng dng c o dng bn ngoi trc v
sau khi ly mu t nht 2 h/ln. Cn m bo thit b hot ng tt bng theo di tc dng trn
bm.
6.2. X l mu
Dng kp t ci lc vo cc 100 ml, thm 5 ml HNO3 50 % c H2O2 v y cc bng np knh
ng h. c cc ln bp v un 15 min. ngui v lc qua giy lc celulose. Thu nc lc
vo bnh nh mc 10 ml. Nu hm lng cadmi hoc ch ln hn, c th dng bnh nh mc 25
ml hoc 50 ml. Trng cc bng mt lng nh HNO3 5 % (th tch), lc qua giy lc v gp vo
phn nc lc trn. Thm HNO3 5 % (th tch) n vch mc.
7. Cch tin hnh
7.1. Phng php A: Xc nh cadmi v ch bng phng php quang ph hp th nguyn
t khng ngn la
7.1.1. Nguyn tc chung
Kim loi trong kh ng khi c thu trn ci lc, sau x l ci lc bng axit nitric (HNO3)
trong hydro peroxyt (H2O2). Dung dch thu c em phn tch bng phng php quang ph
hp th nguyn t khng ngn la. Cc iu kin phn tch chung c quy nh trong Bng 1.
CH THCH: Cn cn thn trnh nhim bn mangan ca mi trng v mangan trong mi
trng thng nng tng i ln.

Bng 1 - Cc iu kin phn tch chung cho phng php phn tch ph hp th khng
ngn la
Nguyn t

Bc sng

iu kin
nguyn t ha

nm

Cng
dng ca n
(mA)

K thut hiu
chnh nn nn
dng

Cadmi

228,8

Nn dng gi

Zeeman, Dteri

Ch

217,0

Nn dng gi

Zeeman, Dteri

7.1.2. Nguyn tc xy dng ng chun v xc nh

Thit lp cc thng s thit b v lp t b phn nguyn t ha nhit in theo hng dn ca
nh sn xut tn dng ti a h thng hiu chnh nn.
i vi loi mu cha bit, xc nh nng tng nguyn t bng phng php thm chun.
Nu kt qu thu c theo phng php thm chun v phng php ng chun bng nhau th
c th s dng phng php ng chun.
CH THCH 1: nh ngha v khong chp nhn khng phi l ni dung ca tiu chun ny.
Tuy vy, ngi s dng cng cn ghi nh v quy trnh kim sot cht lng. Cc quy trnh ny
trong phng th nghim cng phi ph hp vi phng php nh da trn th kim tra, tm
gii hn tin cy v s phn b thng k chun v khng chun.
CH THCH 2: lp li ca cc s c do my cung cp c biu th bng sai s tuyt i,
h s dao ng hoc lch chun ph thuc vo nng ca nguyn t trong mu th.
- V ng chun: V th c nng nguyn t ca cc dung dch chun (bao gm c s liu
chun trng) tnh bng miligam trn lt t trn trc honh v cc gi tr tng ng ca chiu cao
nh (hoc din tch nh) t trn trc tung.
7.1.3. Thuc th
7.1.3.1. Thuc th xc nh cadmi
Theo iu 5 (t 5.1 n 5.17)
7.1.3.2. Thuc th xc nh ch
Theo iu 5 (t 5.1 n 5.16 v 5.18).

7.1.4. Cch tin hnh

7.1.4.1. Xy dng ng chun v xc nh cadmi
7.1.4.1.1. Xy dng ng chun cadmi
Ly by bnh nh mc dung tch 50 ml, dng pipet ht: 0 ml; 0,5 ml; 1 ml; 2 ml; 3 ml; 4 v 5 ml
dung dch Cd chun lm vic (20 g/ml) vo cc bnh. Thm ln lt thuc th theo Bng 2.
Thm HNO3 5 % n vch mc, y nt v lc u. Xy dng ng chun tng quan gia
hp th v nng Cd.
o hp th bc sng 228,8 nm vi hiu chun (b chnh) ng nn, di bc sng
ny, nhy ca cadmin khong 0,01 g/ml, ng chun tuyn tnh trong khong t 0 n 2
g/ml v nhy ca thang khong 0,001 n v.
Sau mi ln o mt dung dch chun, cn kim tra li im "0" vi dung dch dng t im
"0"
Xy dng ng chun tng quan gia hp th v nng Cd.
Bng 2 - Hm lng Cd tng ng trong cc bnh
Bnh s

0,5

1,0

1,5

2,0

3,0

4,0

60

80

Thuc th (ml)
Dung dch chun Cd 20
g/ml (5.17.2)

Thm 10 l/ 10 l dung dch mu

Dung dch nn amoni

axetat 10 % (5.16)
Dung dch HNO3 5 % (5.6)
Hm lng Cd (g)

Thm va n vch mc
0

10

20

30

40

7.1.4.1.2. Xc nh cadmi
Ht mu th v xc nh hp th ca mu v xc nh nng Cd t th ng chun.
Nu nng Cd trong mu ln hn 2 g / ml th pha long dung dch bng HNO3 5 %.

7.1.4.2. Xy dng ng chun v xc nh Pb

7.1.4.2.1. Xy dng ng chun Pb
Phng php ny thch hp cho vic xc nh Pb 0,075 mg/m3 - 0,3 mg/m3 vi sai s thp hn
10%. chnh xc khi c hp th khong 0,001 n v v thang chun tuyn tnh t 0 n
5 g Pb.
Ly su bnh nh mc dung tch 50 ml, dng pipet ht: 0 ml; 1 l; 2 ml; 3 ml; 4 v 5 ml dung
dch Pb chun lm vic (50 g Pb/ml) vo cc bnh. Thm ln lt thuc th theo Bng 3. Thm
HNO3 5% n vch, y nt v lc u. Xy dng ng chun tng quan gia hp th v
nng Pb.
o hp th bc sng 217,0 nm vi hiu chun (b chnh) ng nn. Sb cn tr xc nh
vi hp th 217,6 nm nn khi c mt Sb th phi o Pb bc sng 283,3 nm.
Cc dung dch cha t 0 - 5 g Pb/ml trong HNO3 5% v nn chun b cc dung dch ny hng
tun.
Sau mi ln o mt dung dch chun, cn kim tra li im "0" vi dung dch dng t im
"0"
Xy dng ng chun tng quan gia hp th v nng Pb.
Bng 3 - Hm lng Pb tng ng trong cc bnh
Bnh s

1,0

2,0

3,0

4,0

5,0

Thuc th (ml)
Dung dch chun Pb 50 g/ml
(5.18.2)

Thm 10 l/ 10 l dung dch mu

Dung dch nn amoni axetat 10

% (5.16)
Dung dch HNO3 5 % (5.7)
Hm lng Pb (g)
7.1.4.2.2. Xc nh ch

Thm va n vch mc
0

50

100

150

200

250

Ht mu th v xc nh hp th ca mu v xc nh nng Pb t th ng chun.
Nu nng Pb trong mu ln hn 5 g/ml th pha long dung dch bng HNO3 5%.
7.2. Phng php B: Xc nh cadmi (Cd) v ch (Pb) bng phng php quang ph hp
th nguyn t ngn la
7.2.1. Nguyn tc chung
Kim loi trong kh ng khi thu trn ci lc, sau x l ci lc bng axit nitric (HNO3) trong
hydro peroxyt (H2O2). Dung dch thu c em phn tch, trong phng php quang ph hp th
nguyn t ngn la, mt phn mu ring bit c a vo ngn la v o hp th ca
nguyn t .
Cc iu kin phn tch chung c quy nh trong bng 1.
Bng 4 - Cc iu kin phn tch chung cho phng php phn tch quang ph hp th
ngn la
Nguyn t

Bc sng

Loi ngn la

nm

Lanta
n
clorua

Cht cn
tr
chnh

Hiu
chnh nn

Fe

Dteri

Cadmi

228,8

Khng kh oxy
ha/axetylen

Khng

Ch

217,0

Khng kh oxy
ha/axetylen

Khng

Dteri

CH THCH: Bc sng cho l nhy nht. Ngi s dng cn bit rng nhng bin i nh
v t s th tch kh cng c th nh hng ng k n cng tn hiu phn tch v cn c
th lm bin i tuyn tnh ca kt qu do thit b cung cp. C s khc nhau v nng axit
trong khi ph mu cng c th nh hng n mt s nguyn t vi mt s my o, c bit l
khi khng hiu chnh nn. V vy, ngi s dng phi lm quen vi tnh nng k thut thit b.
7.2.2. Nguyn tc xy dng ng chun v xc nh
- Thit lp cc thng s thit b v lp t b phn nguyn t ha mu theo ch ngn la theo
hng dn ca nh sn xut tn dng ti a h thng hiu chnh nn. Lp t tng t b
phn t ng ly mu.
7.2.3. Thuc th
7.2.3.1. Thuc th xc nh cadmi

Theo iu 5 (t 5.1 n 5.17)

7.2.3.2. Thuc th xc nh ch
Theo iu 5 (t 5.1 n 5.16 v 5.18).
7.2.4. Cch tin hnh
7.2.4.1. Xy dng ng chun v xc nh cadmi
7.2.4.1.1. Xy dng ng chun cadmi
- Ht cc dung dch chun cadmi 20 g/ml (5.17.2) thm ln lt thuc th theo Bng 5 v ti
u ha cc iu kin ht, chiu cao ca gi t v cc iu kin ngn la. iu chnh tn hiu
ca my n im "0" ca thang hp th ang ht nc.
- Ht dung dch chun trng coi nh "0" (5.16).
- Sau khi dng 10 s, c hp th ca mi dung dch t nht 2 ln v cc gi tr ri vo mt dy
chp nhn c th gi tr trung bnh. Cn m bo chc chn rng khi dng dung dch chun
m c hn c hp th < 1, thch hp nht l khng ln hn 0,7.
CH THCH: nh ngha v dy c chp nhn khng phi l ni dung ca tiu chun ny.
Tuy vy, ngi s dng cn thc hin quy trnh kim sot cht lng, th d nh th kim tra,
tm gii hn tin cy v s phn b thng k chun v khng chun.
7.2.4.1.2. Xc nh cadmi
Dng h thng bm mu t ng bm dung dch trng (5.16) v cc dungd ch chun cadmi 20
g/ml (5.17.2) hoc ring bit vo ngn la v o hp th ca cc nguyn t . c s o
ca cc dung dch t nht hai ln. Nu cc gi tr nm trong khong chp nhn c th ly gi tr
trung bnh. Sau mi php o, ht nc v iu chnh v "0" nu cn. Nu nng ca nguyn t
trong mu th ln hn ng chun th pha long dung dch th bng dung dch trng (5.16).
CH THCH 1: Nhit ca cc dung dch chun v dung dch th ch c khc nhau trong
phm vi 1 0C ti thi im o.
CH THCH 2: lp li ca cc s c do my cung cp c biu th bng sai s tuyt i,
h s dao ng hoc lch chun ph thuc vo nng ca nguyn t trong mu th.
Bng 5 - Hm lng Cd tng ng trong cc bnh
Bnh s

Thuc th (ml)
Dung dch chun Cd 20
g/ml (5.17.2)

0,5

1,0

1,5

2,0

3,0

4,0

Thm 10 l/ 10 l dung dch mu

Dung dch nn amoni

axetat 10 % (5.16)
Dung dch HNO3 5 % (5.6)

Thm va n vch mc
0

Hm lng Cd (g)

10

20

30

40

60

80

7.2.4.2. Xy dng ng chun v xc nh ch

7.2.4.2.1. Xy dng ng chun ch
- Ht cc dung dch chun 50 g/ml (5.17.2) thm ln lt thuc th theo bng 6 v ti u ha
cc iu kin ht, chiu cao ca gi t v cc iu kin ngn la, iu chnh tn hiu ca my
n im "0" ca thang hp th ang ht nc.
- Ht dung dch chun trng coi nh "0" (5.16).
- Sau khi dng 10 s, c hp th ca mi dung dch t nht 2 ln v nu cc gi tr ri vo mt
dy chp nhn c th ly gi tr trung bnh. Cn m bo chc chn rng khi dng dung dch
chun m c hn c hp th < 1, thch hp nht l khng ln hn 0,7.
CH THCH: nh ngha v dy c chp nhn khng phi l ni dung ca tiu chn ny. Tuy
vy, ngi s dng cn thc hin quy trnh kim sot cht lng, th d nh th kim tra, tm
gii hn tin cy v s phn b thng k chun v khng chun.
Bng 6 - Hm lng Pb tng ng trong cc bnh
Bnh s

Dung dch chun Pb 50 g/ml

(5.18.2)

1,0

2,0

3,0

4,0

5,0

Thuc th (ml)

Dung dch nn amoni axetat

10 % (5.16)

Thm 10 l/ 10 l dung dch mu

Dung dch HNO3 50 % (5.7)

Thm va n vch mc

Hm lng Pb (g)

50

100

150

200

250

- V ng chun: V th c nng nguyn t ca cc dung dch chun tnh bng miligam

trn lt t trn trc honh v cc gi tr tng ng ca chiu cao nh (hoc din tch nh) t
trn trc tung.
7.2.4.2.2. Xc nh ch
Dng h thng bm mu t ng bm dung dch trng (5.16) v cc dung dch chun ch 50
g/ml (5.18.2) ring bit vo ngn la v o hp th ca cc nguyn t . c s o ca cc
dung dch t nht hai ln. Nu cc gi tr nm trong khong chp nhn c th ly gi tr trung
bnh. Sau mi php o, ht nc v iu chnh v "0" nu cn. Nu nng ca nguyn t trong
mu th ln hn ng chun th pha long dung dch th bng dung dch trng (5.16).
CH THCH 1: Nhit ca cc dung dch chun v dung dch th ch c khc nhau trong
phm vi 1 0C ti thi im o.
CH THCH 2: lp li ca cc s c do my cung cp c biu th bng sai s tuyt i,
h s dao ng hoc lch chun ph thuc vo nng ca nguyn t trong mu th.
8. Tnh kt qu
Nng kim loi nng trong kh ng khi c tnh theo cng thc:

(1)
Trong :
C l nng kim loi nng trong kh thi, tnh bng miliham trn mt khi;
Cs l nng kim loi nng trong dung dch mu, tnh bng microgam trn mililit;
Cb l nng kim loi nng trong dung dch trng, tnh bng microgam trn mililit;
Vs l th tch dung dch mu, tnh bng mililit;
Va l th tch mu kh ly, tnh bng lt;

d l h s pha long.
9. Bo co kt qu
Trong bo co kt qu, cn thit phi c cc thng tin sau:
a) Vin dn tiu chun ny;
b) Nhn bit mu;
c) M t nh my v qu trnh hot ng (cng ngh);
d) iu kin vn hnh ca nh my;
e) V tr mt phng o;
f) V tr o trong mt phng o;
g) Nhng thay i trong hot ng ca nh my, chng hn nhng thay i b phn t nhin
liu;
h) Nu bt k thao tc ny khng c quy nh trong tiu chun ny hoc coi l thao tc ty ;
i) Kt qu phn tch;
j) Ngy thng v thi gian nhn mu.