XC NH HM LNG As NGM CHIT

TRONG MU CHT THI NGUY HI

BNG PHNG PHP QUANG PH
HP THU NGUYN T
EPA Test Mothod 1311 TCLP
SMEWW 3113 B 2012

XC NH HM LNG As NGM CHIT TRONG MU CHT

THI NGUY HI BNG PHNG PHP QUANG PH HP THU
NGUYN T
1.

NGUYN TC.
Mu cht thi khi c a v phng th nghim s tin hnh phn loi v ng nht

mu. i vi thnh phn rn, cc kim loi trong mu s c chit bng dung dch pH =
4.93 0.05 hoc pH = 2.99 0.05 ty thuc vo pH ca tng mu. i vi cht lng c hm
lng cn < 0.5% th tin hnh lc qua mng lc 0.6-0.8 m. Sau cc dung dch thu c
s tin hnh xc nh kim loi bng k thut quang ph hp thu nguyn t.
2.

PHM VI P DNG.
Phng php ny c p dng nh lng hm lng ngm chit nguyn t As c

trong mu cht thi c xem l cht thi nguy hi bng phng php quang ph hp thu
nguyn t k thut nhit in (l graphite).
3.

TI LIU THAM KHO.

p dng theo EPA Test Method 1311: phng php ngm chit c tnh.
Tham kho: QCVN 07: 2009/BTNMT.
Tham kho: ASTM D5233 92.
Tham kho: SMEWW 3113B - 2012
4.

THIT B, HA CHT.

4.1. Thit b, dng c.

My quang ph hp thu nguyn t AAS AA6300, Shimadzu hiu chun.
n Cathode: As
Cn phn tch c chnh xc 0.01g.
My pH c chnh xc 0.05 25 0C.
My khuy t hoc my lc mu.
T sy c th iu chnh nhit trong khong 85115 0C.
Bp in c th iu chnh nhit 50 0C .
My nghin mu.

 Ry c ng knh l < 9.5 mm.

Bnh nh mc cc loi (Din A).
Pipet cc loi (Din A).
Bnh ngm mu l cc becher: 1 lt, 2 lt, 3 lt.
Dng c thy tinh cc loi

: Becher, Erlen, phu lc, ng ong, .

Mng lc si thy tinh c kch thc l 0.6-0.8 m.

4.2. Ha cht.
4.2.1. Ha cht thng.
Nc ct 1 ln, khng cha kim loi cn phn tch.
Acid Acetic m c 99%.
Dung dch Acid Clohydric 1N: Ha tan 83 mL HCl 37% trong 1lt nc ct.
Dung dch Acid Nitric 1N: Ha tan 70 mL HNO3 65% trong 1lt nc ct.
Dung dch NaOH 1N: Ha tan 20.20(g) NaOH vi 200 mL nc ct sau nh mc
thnh 500 mL.
Dung dch chit 1 (pH = 4.93 0.05): Ha tan 5.7 mL Acid Acetic vi 500 mL nc
ct, thm 64.3 mL NaOH 1N sau nh mc thnh 1 lt.(dng my pH iu chnh
ng pH)
Dung dch chit 2 (pH = 2.88 0.05): Ha tan 5.7 mL Acid Acetic vi 500 mL nc
ct, sau nh mc thnh 1 lt.(dng my pH iu chnh ng pH)
4.2.2. Ha cht chun.
Dung dch chun As gc: 1000 2 mg/L, Merck
Dung dch chun th cp:
Dung dch chun As 100 mg/L: Ht 10 mL dung dch chun gc 1000 mg/L vo bnh
mc 100 mL. nh mc n vch bng acid nitric 0.1N (dng pipet bu 10 mL).
Dung dch chun As 10 mg/L: Ht 10 mL dung dch chun As 100 mg/L vo bnh
nh mc 100 mL. nh mc n vch bng acid nitric 0.1N (dng pipet bu 10 mL).
Dung dch chun As 1 mg/L: Ht 10 mL dung dch chun As 10 mg/L vo bnh nh
mc 100 mL. nh mc n vch bng acid nitric 0.1N (dng pipet bu 10 mL).

 Dy chun lm vic ca As: 5, 10, 20, 40, 60 g/L: Ht 0.25, 0.5, 1.0, 2.0, 3.0 mL
chun As: 1 mg/L cho vo ln lt cc bnh nh mc 50 mL. nh mc n vch bng acid
nitric 0.1N (dng pipet vch 5 mL).
4.2.3. Bo qun
Tt c cc dung dch chun phi c bo qun trong chai thy tinh hoc nha Teflon
c np y kn v t ni thong mt, kh ro, khng c nh sng chiu trc tip vo, nhit
khng qu 300C.
Thi gian s dng ca dung dch chun gc ty thuc vo nh sn xut.
Dy chun lm vic ca cc kim loi ch pha v s dng trong ngy.
Chun th cp ch pha li khi xy dng ng chun mi.
5.

CCH TIN HNH.

5.1. CHUN B MU TH.

Mu cht thi sau khi a v phng th nghim s tin hnh phn loi v c chia lm
3 loi chnh nh sau:
Mu cht thi lng: L mu cht thi c hm lng cn kh nh hn 0.5%.
Mu cht thi va c cn rn, va c cht lng: Ta tin hnh tch ra lm 2
phn rn v lng tin hnh phn tch ring.
Mu cht thi rn: Ta tin hnh nghin mu cho qua ry c ng knh l <
9.5mm, phn mu qua ry s c gi li tin hnh phn tch.
5.2. CCH TIN HNH.
5.2.1. i vi cht thi lng: Ta tin hnh lc qua mng lc si thy tinh c kch thc l
0.6-0.8 m. Phn dung dch qua lc c gi xc nh cc kim loi bng phng
php quang ph hp thu nguyn t. Nu cha xc nh ngay th phi c bo qun
nhit < 40C.
5.2.2. i vi mu cht thi va c cn rn, va c cht lng: Tin hnh ng nht v cn
khong 100 g mu, sau tch ra lm 2 phn: rn v lng phn tch
5.2.2.1. Phn cht lng ta cho qua mng lc si thy tinh c kch thc l 0.6-0.8 m. Dung
dch sau lc (k hiu: dung dch A) c bo qun nhit < 40C, ghi li th tch V1(L).
5.2.2.2. Phn cht rn ta tin hnh lm kh, nghin mn sau cho qua ray c kch thc l <
9.5mm. Phn cht rn qua ray s c gi li v tin hnh phn tch nh sau:

 Trc tin ta phi tin hnh kim tra pH chn dung dch chit ph hp: Cn 5(g)
mu nghin nh cho vo becher 500mL, thm vo 96.5mL nc ct. Ta tin hnh lc
hoc khuy t trong khong 5 pht, sau ta th pH ca mu. Nu pH < 5 ta s dng dung
dch chit 1, nu pH > 5 ta thm vo 3.5 mL dung dch HCl 1N. t becher ln bp in v
gi 500C trong 10 pht, sau ngui n nhit phng v tin hnh kim tra pH. Nu
pH < 5 th ta cng s dng dung dch chit 1, nu pH > 5 th ta s dng dung dch chit 2.
Sau khi kim tra pH, ta tin hnh cn 1 lng mu th c nghin nh t nht
l 100(g) cho vo becher 3 lt. Sau ta thm 1 lng dung dch chit 1 hoc dung dch chit
2 ( theo phn kim tra pH trn) vi khi lng gp 20 ln khi lng mu th. Tin hnh
khuy hoc lc lin tc trong vng 18 + 2 gi, sau lng v lc ta c dung dch B, ghi
li th tch Vnc (L)
5.2.2.3. Sau khi tin hnh x l xong 2 phn rn v lng nh trn. Nu dung dch A (xem
phn 5.2.2.1) v dung dch B (xem phn 5.2.2.2) ng nht, th ta trn chung 2 dung dch li
v xem n l mt dung dch nc. Xc nh kim loi bng phng php quang ph hp thu
nguyn t. Nu dung dch A (xem phn 5.2.2.1) v dung dch B (xem phn 5.2.2.2) khng
ng nht v tnh cht, th ta xem n l 2 dung dch nc v tin hnh phn tch ring l trn
my AAS, kt qu c tnh l kt qu trung bnh ca dung dch A v dung dch B ( Xem
phn 6)
5.2.3. i vi mu cht thi l cht rn: Ta cng tin hnh lm kh v nghin mn sau
cho qua ray c kch thc l < 9.5mm. Phn cht rn qua ray s tin hnh x l ging
nh phn 5.2.2.2. Dung dch thu c dng xc nh kim loi bng phng php
quang ph hp thu nguyn t.
6.

TNH TON KT QU.

Nng ngm chit Ctc l nng (mg/L) ca mt thnh phn nguy hi trong dung

dch sau ngm chit, c thi ra t cht thi khi tin hnh chun b mu phn tch bng
phng php ngm chit.
6.1. i vi cht thi lng (phn 5.2.1), cht thi rn (phn 5.2.3): Hm lng kim loi
c trong mu cht thi l:

Ctc ( mg / L)

C0
F
1000

Trong :
Ctc (mg/L): Hm lng kim loi thi ra trong mu bn thi.

 C0 (g/L): Hm lng kim loi tnh trn ng chun.

F: H s pha long.
6.2. i vi mu cht thi va rn va lng:
6.2.1. Nu dung dch A (phn 5.2.2.1) v dung dch B (phn 5.2.2.2) ng nht, hm lng
kim loi c trong mu c tnh theo cng thc sau:
Ctc ( mg / L)

C0
F
1000

Trong :
Ctc (mg/L): Hm lng kim loi thi ra trong mu bn thi.
C0 (g/L): Hm lng kim loi tnh trn ng chun.
F: H s pha long.
6.2.2. Nu dung dch A (phn 5.2.2.1) v dung dch B (phn 5.2.2.2) khng ng nht v tnh
cht, hm lng kim loi c trong mu c tnh theo cng thc sau:
Ctc (mg / L)

C1 V1 C nc Vnc
V1 Vnc

Trong :
Ctc (mg/L): Hm lng kim loi ngm chit trung bnh trong phn rn v phn lng
ca mu bn thi.
C1 (mg/L): Hm lng kim loi c trong phn lng ca mu bn thi.
V1(L): Th tch phn cht lng tch ra t mu bn thi (phn 5.2.2.1).
Cnc (mg/L): Hm lng kim loi thi ra trong phn rn ca mu bn thi.
Vnc(L): Th tch ngm chit phn cht rn ca mu bn thi (phn 5.2.2.2).
7.

CC THNG S THM NH.

lp li ca phng php (% RSDr): 8.3 13 %

ti lp phng th nghim ca phng php (% RSDR): 19 24 %
Hiu sut thu hi ca phng php (% H): 88 108 %
Gii hn pht hin ca phng php (MDL): 0.002 mg/L