TIU CHUN VIT NAM

TCVN 7245 : 2003

L T CHT THI RN Y T - PHNG PHP XC NH NNG NIT OXIT (NO X) TRONG KH
THI
Health care solid waste incinerator - Determination method of nitrogen oxides (NO x) concentration in
fluegas
Li ni u
TCVN 7245 : 2003 do Tiu Ban k thut Tiu chun TCVN/TC 146/SC 2 "Cc phng php phn tch
thng s nhim trong kh thi L t rc y t" bin son, Tng cc Tiu chun o lng Cht lng
ngh, B Khoa hc v Cng ngh ban hnh.

L T CHT THI RN Y T - PHNG PHP XC NH NNG NIT OXIT (NO X) TRONG

KH THI
Health care solid waste incinerator - Determination method of nitrogen oxides (NO x) concentration
in fluegas
1. Phm vi p dng
Tiu chun ny qui nh phng php xc nh nng khi lng ca nit oxyt NO x trong khi ng khi
l t cht thi rn y t, quy v iu kin nhit v p sut tiu chun.
Ch thch
- Nit (NOx) c nh ngha l tng NO v NO2. Nng khi lng NOx l nng tng ng NO2
biu th bng miligam trn mt khi.
- Nhit v p sut tiu chun l nhit 0oC v p sut 101,3 kPa.
Tiu chun ny p dng cho khong nng t 5 mg/m 3 n 1000 mg/m3 tnh theo NO2 vi th tch mu
1000 ml.
Gii hn pht hin di ca phng php c th t l 2 mg/m 3 (NO2) khi dng cuvet c b dy 5 cm.
Tiu chun ny khng dng xc nh dinit monoxyt (N 2O).
Cn tr
- Phn ng gia SO2 vi NO v NO2 trong pha kh trc khi thm dung dch hp th l o c. Nhng
dung dch hp th c cha H2O2 s oxy ha nhanh SO2 thnh SO42, khng phn ng vi NO v NO2.
- Nu nng HCl trong khi ng khi di 365 mg/m 3 s khng gy nh hng n phn tch (nng
cao hn cha c nghin cu nhng hy vng rng n khng gy cn tr). HCl khng gy cn tr tr
khi lng HCl trong mu kh lm gim pH ca dung dch hp th xung thp hn 12. Nu pH ca dung
dch hp th gim xung thp hn 12 do b sung axit th NO3 s c sinh ra.

- ion ng (Cu2+) nng cao lm gim s to thnh phm mu azo. Lng Cu 2+ c dng lm cht
xc tc phi lun khng i k c trong dung dch mu trng.
- CO v CO2 trong kh thi khng gy cn tr.
- N2O (n 100 mg/m3) l bn v khng cn tr, (nng cao hn cha c nghin cu)
- NH3 (n 20 mg/m3) khng cn tr, (nng cao hn cha c nghin cu)
- SO3 (n 100 mg/m3) v HF (n 10 mg/m3) khng cn tr, (nng cao hn cha c nghin cu).
2. Tiu chun vin dn
TCVN 4851 : 1989 (ISO 3696 : 1987), Nc dng phn tch trong phng th nghim. Yu cu k thut
v phng php th.
TCVN 7242 : 2003 L t cht thi rn y t - Phng php xc nh nng cacbon monoxit (CO) trong
kh thi.
3. Nguyn tc
Phng php ny c dng xc nh nng khi lng ca nit oxyt trong kh thi, sau khi ra
ui, loi nit bng kh v/hoc loi nit xc tc, trc khi thi vo kh quyn.
Nit oxyt trong kh thi c hp th vo dung dch hydro peroxyt kim (NaOH 1,2 mol/l, H 2O2 0,6 %) khi
c mt ion ng (Cu2+) lm cht xc tc nit oxyt b oxy ha to thnh ion nitrit (NO 2)
nhng nng trn, ion nitrat khng sinh ra trong dung dch hp th.
Hydro peroxyt d trong dung dch hp th cn tr vic to mu. Do , hydro peroxyt c phn hy
nh xc tc ca Cu2+ khi un nng dung dch 30 min trn bp cch thy 80oC.
Nng nitrit c xc nh bng cch dng my o quang o hp th cc i ca dung dch mu
hng t phn ng ca sunfanilamit vi naphtyletylendiamin (NEDA) bc sng 545 nm.
Nng khi lng ca nit dioxyt c xc nh bng cch so snh hp th thu c vi ng
chun c chun b t dung dch tiu chun natri nitrit tinh khit.
4. Thuc th
Trong phn tch, tr khi c nhng qui nh khc, ch s dng thuc th c tinh khit c tha nhn,
nc ct hoc nc loi khong hoc nc c tinh khit tng ng theo TCVN 4851 : 1989
(ISO 3696).
4.1 Dung dch hp th (NaOH 1,2 mol/l; H2O2 0,6% : Na2CO3 4,0%; NaCOOH 0,0005 %).
Ha tan 48g natri hydroxyt, 40,0 g natri cacbonat v 5 mg natri format trong khong 800 ml nc, thm
20 ml hydro peroxyt (30%) v pha long bng nc n 1000 ml.
Ch thch: Dung dch hydroxyt hp th c th bo qun trong bnh y kn, ch lnh, ti trong mt tun
l. Lc lm cho hydro peroxyt d b phn hy.

4.2 Dung dch ng sunphat (0,0004 mol/l)

Ha tan 0,1g ng sunphat (CuSO4.5H2O) bng nc trong bnh nh mc 1000 ml v thm nc n
vch. Pha long 10 ml dung dch ny bng nc thnh 100 ml trong bnh nh mc.
4.3 Dung dch sunfanilamit/axit clohydric (sufanilamit 0,5%, axit clohydric 20%)
Ha tan 1,0g sunfanilamit trong khong 50 ml nc, thm 112 ml axit clohydric (37%) trong bnh nh
mc 200ml. Thm nc n vch.
4.4 Dung dch naphtyletylendiamin(NEDA) (0,1%)
Ha tan 0,1 g NEDA diclorua ngm 2 HCl trong 100 ml nc.
4.5 Dung dch nitrit gc (250 mg/l, tnh theoNO-2)
Ha tan 375 mg natri nitrit kh (NaNO2) v 0,2 g natri hydroxyt (NaOH) bng nc trong bnh nh mc
1000 ml. Thm nc n vch v lc u.
Ch thch: Dung dch ny bn t nht trong 3 thng nu trong bnh y kn.
4.6 Dung dch chun nitrit cng tc (20 mg/l tnh theoNO-2)
Ly 40,0 ml dung dch nitrit (4.5) vo bnh nh mc 500 ml. Thm nc n vch v lc u; 1 ml dung
dch ny cha 20 g NO2.
Chun b dung dch ngay trc khi dng.
5. Thit b, dng c
Trong phn tch, s dng cc thit b dng c quy nh trong TCVN 7242 : 2003 v cc thit b dng c
sau:
5.1 My o quang ph, c kh nng o bc sng 545 nm v c b dy cuvet t 1,0 cm n 5,0 cm.
6. K thut ly mu
6.1 Nguyn tc chung
Ty thuc vo nhim v o v thit b c sn, mt h thng thit b ly mu ph hp vi mt trong cc s
(xem hnh 4 ca TCVN 7242 : 2003) s c lp t.
S h thng thit b ly mu hnh 4 TCVN 7242 : 2003 ch c dng nu bit lng NO 2 l rt
nh. Ni chung, kh thi ca l t cht thi c lng NO 2 nh hn so vi lng nit oxyt tng (tng NO
+ NO2 = NOx). Nu lng NO2 thp hn 10% NOx s mt NO2 do ngng t l khng ng k.
Phi m bo khng c r r trong h thng thit b ly mu.
Thi gian ly mu t 5 min n 12 min. Thi gian xc nh NO x khong 60 min.
6.2 Ly mu kh bng phng php th ch th tch

Ni bnh ly mu kh (6) vi thit b ly mu nh hnh 4 TCVN 7242 : 2003. Khi ng bm ht (5),

thi sch ng ly mu v bnh n khi th tch kh i qua bng 10 ln th tch bnh ly mu.Sau
ng hai kha ca bnh ly mu. Khi nhit cn bng (thng trong 3 min) bnh c di nc, o
nhit v p sut khng kh bn ngoi v a dung dch hp th vo bng bm tim.
6.3 Tho bnh
ng kha ca bnh ly mu.Tho bnh (6) ra khi thit b ly mu.
6.4 a dung dch hp th vo bnh
Dng ng cao su silicon ni u kha ca bnh ly mu vi bm tim cha sn 50 ml dung dch hp
th (4.1) v 5 ml dung dch ng sunfat (4.2) c lc trn k trc. Sau m kha v a dung
dch hn hp vo bnh. ng kha bnh v tho bm tim ra khi bnh.
6.5 Lc bnh
Lc mnh bnh, thnh thong ngng trong vng 3 min hoc sau khi lc mnh bnh 1 min ri t bnh vo
my lc v lc thm 2 min.
6.6 Chuyn dung dch sang bnh nh mc
Chuyn dung dch mu t bnh ly mu sang bnh nh mc c dung tch 100 ml (th tch V 1). Trng bnh
ly mu hai ln bng 15 ml nc v nhp nc ra ny vo dung dch mu trong bnh nh mc.
Ch thch - Nu bnh nh mc c y kn kh th dung dch c th bo qun c ti 36h trc khi
tin hnh bc tip theo ca qui trnh ny (6.7).
6.7 Phn hy hydro peroxyt
t bnh nh mc vo ni cch thy 80oC trong 30 min. Ly ra v lc.Lm ngui bnh n nhit
phng bng dng nc chy.
6.8 Chun b dung dch mu phn tch
Thm nc vo bnh nh mc 100 ml n vch v lc.Dng dung dch ny lm dung dch mu phn
tch.
Ch thch - Nu bnh nh mc c y kn kh th dung dch c th bo qun c ti 48h trc khi
tin hnh bc tip theo ca qui trnh ny.
Nu nng NOx ln (t 1000 mg/m3 n 5000 mg/m3) th pha long mu hoc ly mt phn mu
phn tch
7. Cch tin hnh
7.1 Chun b dy dung dch chun
Ly su bnh nh mc, dung tch 100 ml ngm v ra bng dung dch sunfo cromic, trng k bng
nc v nh s t 0 n 5. Cho ln lt dung dch chun NaNO 2 (4.6) 0,0 ml; 1,0 ml; 2,0 ml; 3,0 ml; 4,0
ml; 5,0 ml. Theo qui trnh t 6.4 n 6.8 [thm 50 ml dung dch hp th (4.1) v 5 ml dung dch ng

sunfat (4.2) vo bnh ly mu (6.4), lc trong 2 min (6.5), chuyn dung dch vo bnh nh mc (6.6), ph
hy H2O2 (6.7) v chun b dung dch mu phn tch (6.8)].
Bng 1 - Nng khi lng NO2 tng ng trong cc bnh
Bnh s

0,0

1,0

2,0

3,0

4,0

5,0

0,2

0,4

0,6

0,8

1,0

Dung dch chun (ml)

Dung dch chun cng tc NO2 20 mg/l
(4.6)
Nng khi lng NO2 (mg/l)
7.2 Chun b dy dung dch trng
Chun b dung dch trng nh sau:
a) Ly 50 ml dung dch hp th (4.1) v 5 ml dung dch ng sunfat (4.2) cho vo bnh nh mc dung
tch 100 ml.
b) Phn hy hydro peroxyt nh m t 6.7 ri thm nc n vch v lc u.
c) Theo qui trnh t 7.4 a) n 7.4 c); sau yn dung dch ny 15 oC n 30oC trong 15 min. Dng
dung dch ny l dung dch trng.
7.3 Xy dng ng chun
phn tch cc dung dch chun, tin hnh theo qui trnh 7.3.
V ng chun theo hp th ca cc dung dch chun vi nng khi lng ca nit dioxyt (xem
hnh 1).
dc ca ng chun c tnh theo cng thc:
=

(1)

trong
A l hp th:
c l nng khi lng ca ion nitrit, tnh bng miligam trn lt;
f l h s hiu chun (tng ng vi b dy cuvet 1 cm), tnh bng miligam trn lt;
Gi tr in hnh ca f l 0,9 mg/l (vi b dy cuvet 1 cm).
7.4 Phn tch

a) Ht bng pipet 20,0 ml (V) dung dch mu vo bnh nh mc 100 ml;

b) Thm 10 ml dung dch axit sufanyamit/axit clohydric (4.3);
c) Thm 5 ml dung dch NEDA (4.4), thm nc n vch v lc u;
d) yn dung dch trong 15 min 15oC n 30oC v o hp th bng my o quang ph bc
sng 545 nm, so snh vi dung dch trng. Phn tch trc quang cn c tin hnh trong 2 h k t khi
chun b dung dch.

Hnh 1 - Th d v ng chun cho nit oxyt

Ch thch - Nu nng khi lng NO trong dung dch mu ln hn 1,2 mg/l th ng chun s khng
thng. Trng hp ny, dung dch phi c pha long bng dung dch trng n nng thp hn gi
tr gii hn trn (1,2 mg/l).
8. Tnh kt qu
8.1 Tnh lng mu khi ly
Tnh lng mu khi ly, quy v iu kin kh quyn tiu chun (0 oC v 101,3 kPa) bng cng thc (2):

(2)
trong
Vs l lng mu kh ly, tnh bng lt;
Va l dung tch bnh ly mu, tnh bng lt;

p0 l p sut trong bnh trc khi ly mu, tnh bng kilopascan;

p1 l p sut trong bnh sau khi ly mu, tnh bng kilopascan;
t0 nhit trong bnh trc khi ly mu, tnh bng Celsius ( C);
t1 nhit trong bnh sau khi ly mu, tnh bng Celsius ( C);
pw1 l p sut hi nc t1, (bng 0 nu kh kh), tnh bng kilopascan.
t1 = t0 l cng thc (2) c gin lc thnh cng thc (3)

(3)
Cc k hiu nh cng thc (2).
8.2 Tnh nng khi lng nit oxyt
Tnh nng khi lng nit oxyt trong mu kh theo nit dioxyt bng cng thc (4):
c=

(4)

trong
c l nng khi lng nit oxyt (tnh theo NO2) trong mu kh, tnh bng miligam trn mt khi;
fl h s hiu chun, tnh bng miligam trn lt dung dch;
Ch thch - Gi tr ca f phi ph hp vi b y cuvet, nu thay cuvet phi dng li ng chun.
A l hp th;
n l t ph pha long ca dung dch mu: (0,1/0,02 = 5);
V1 l th tch ca dung dch mu tng (0,1 l); tnh bng lt;
Vs l th tch ca mu kh iu kin tiu chun nh tnh 8.1, tnh bng lt.
9. chnh xc ca phng php
lp li ca phng php l trong khong 3% ti mc nng khi lng ca nit oxyt trong khong
t 50 mg/m3 n 1000 mg/m3.
10. Bo co kt qu
Bo co kt qu gm nhng ni dung sau:

a) Nhn bit y mu kh;

b) Lu lng kh thi
c) Kt qu th;
d) Nhng bt thng trong khi xc nh;
e) Tt c s liu cn thit ca l t trong thi gian tin hnh o;
f) Mi thao tc ngoi cc thao tc qui nh trong tiu chun ny hoc tiu chun khc c vin dn.