TIU CHUN QUC GIA

TCVN 8742:2011
CY TRNG- XC NH NITRAT V NITRIT
BNG PHNG PHP SO MU
Plant - Determination of nitrate and nitrite by colorimetric method
Li ni u
TCVN 8742:2011 c chuyn i t 10 TCN 452- 2001 theo qui nh ti khon 1 iu 69 ca Lut Tiu chun
v Quy chun k thut v im a khon 1 iu 6 Ngh nh s 127/2007/N-CP ngy 1/8/2007 ca Chnh ph qui
nh chi tit thi hnh mt s iu ca Lut Tiu chun v Quy chun k thut.
TCVN 8742:2011 do Vin Th nhng Nng ho bin son, B Nng nghip v Pht trin Nng thn ngh,
Tng cc Tiu chun o lng Cht lng thm nh, B Khoa hc v Cng ngh cng b.

TCVN 8742:2011
CY TRNG XC NH NITRAT V NITRIT BNG PHNG PHP SO MU
Plant Determination of nitrate and nitrite by colorimetric method
1 Phm vi p dng
Tiu chun ny quy nh phng php xc nh hm lng nitrat v nitrit tng s trong mu thc vt ti bng
phng php quang ph.
2 Ti liu vin dn
Cc ti liu vin dn sau y l cn thit p dng tiu chun ny. i vi cc ti liu vin dn ghi nm cng b
th p dng bn c nu. i vi cc ti liu vin dn khng ghi nm cng b th p dng phin bn mi nht,
bao gm c cc sa i, b sung (nu c).
TCVN 4851:1989 (ISO 3696 - 1987), Nc dng cho phn tch trong phng th nghim- Yu cu k thut v phng
php th.
TCVN 8551:2010, Cy trng - Nguyn tc chung v ly mu v chun b mu xc nh mt s nguyn t.
3 Nguyn tc
Ha tan (chit xut) nhanh NO3- v NO2- trong mu cy trng ti trong mi trng nc bng nng lng vi
sng.
o mu vng c trng ca dung dch c hp th quang cc i bc sng 410 nm, hnh thnh bi dung
dch NO3- tc dng vi thuc th axit phenoldisulfonic to thnh nitrophenoldisulfonic trong mi trng kim.
o mu hng ca dung dch c hp th quang cc i bc sng 520 nm, hnh thnh bi dung dch NO 2tc dng vi thuc th axit sulfanilic v - naphtylamin trong mi trng axit.
4 Ha cht v thuc th
Ho cht s dng pha cc cht chun t loi tinh khit ho hc, ho cht s dng phn tch t loi tinh
khit phn tch.
4.1 Ha cht
4.1.1 Nc ct, TCVN 4851:1989.
4.1.2 Phenol (C6H5OH).
4.1.3 Axit sunfuric (H2SO4) d= 1,84.
4.1.4 Axit axetic (CH3COOH), 10 % theo th tch (V:V), ha tan trong nc ct.
4.1.5 Axit sulfanilic (C6H7NO3S).
4.1.6 Naphthynlamin (C10H7N2.NH2).
4.1.7 Sulfanilamit (C6H8N2O2S).
4.1.8 N (1-naphthyl) etylen diamin dihydroclorua (NED) C12H14N2.2HCl.
4.1.9 Amoni hydroxit (NH4OH).
4.1.10 Natri Hydroxit (NaOH).
4.2 Thuc th

4.2.1 Dung dch axit phenoldisulfonic (C6H6O7S2): Ho tan 25 g phenol tinh khit vo 150 ml H 2SO4 c (d=
1,84), thm 75 ml axit H2SO4 bc khi. un nng 2 h trong nc si, bo qun trong l mu ti.
4.2.2 Dung dch thuc th Griss:
4.2.2.1 Dung dch thuc th Griss kiu c, gm 2 dung dch:
Dung dch axit sulfanilic: Ha tan 0,5 g axit sulfanilic trong 150 ml axit axetic 10 %.
Dung dch naphthynlamin: Ha tan 0,1 g - naphthynlamin vo 20 ml nc ct, khuy u, un si dung dch,
lng trong, lc ly phn trong v thm vo 150 ml axit axetic 10 %, lc u, bo qun trong l mu ti.
4.2.2.2 Thuc th Griss ci tin, gm 2 dung dch:
Dung dch sulfanilamit: Cn 5 g sulfanilamit ha tan trong bnh nh mc 500 ml bng nc ct, lc k. Dung
dch n nh trong 2 n 3 thng.
Dung dch N (1-naphtyl) etylen diamin dihydroclorua (NED): cn 0,5 g NED ha tan trong 500 ml nc ct,
bo qun trong bnh ti mu. Dung dch khng bn, thay th hng thng hoc thay khi dung dch chuyn sang
mu nu.
4.2.3 Dung dch tiu chun nitrat, nng 10 mg/l
Cn chnh xc 0,1631 g KNO3 kh tinh khit, ha tan bng nc v thm nc n 1000 ml trong bnh nh mc.
Trn u dung dch, thu c dung dch tiu chun c nng 100 mg/l, ha long tip 10 ln c dung dch tiu
chun nng 10 mg/l.
4.2.4 Dung dch tiu chun nitrit, nng 5 mg/l
Cn chnh xc 0,375 g NaNO2 kh tinh khit, ha tan bng nc ct thnh 1 lt dung dch, thu c dung dch
tiu chun nng 250 mg NO2-/l. Pha long 50 ln c dung dch tiu chun 5 mg NO 2-/l.
4.2.5 Dung dch NH4OH, pha trong nc ct t l 1:1 tnh theo th tch.
4.2.6 Dung dch NaOH, pha trong nc ct t l 10 % tnh theo khi lng trn th tch.
5 Thit b, dng c
S dng cc thit b, dng c thng thng trong phng th nghim v cc thit b, dng c nh sau:
5.1 My quang ph.
5.2 My nghin mu thc vt ti.
5.3 Cn phn tch, chnh xc 0,0002 g.
5.4 L vi sng, cng sut 850 W, tn s 2450 MHz.
5.5. Ni cch thy, nhit 100 0C.
5.6 Cc chu nhit, dung tch 250 ml.
5.7 Bnh nh mc, dung tch 50; 100; 200; 250; 500; 1000 ml.
5.8 Pipet, dung tch t 1 ml n 5 ml.
6 Cch tin hnh
6.1. Ly mu v chun b mu: Phng php ly mu v chun b mu xc nh NO 3- v NO2- theo TCVN
8551:2010.
6.2 Phng php chit nitrat v nitrit bng l vi sng:
NO3- v NO2- trong mu cy trng c ha tan bng l vi sng. Phng php chit ny c th loi tr c hu
ht cc nh hng xu ti kt qu phn tch nitrat v nitrit. Cch lm nh sau:
6.2.1 Thi nh, trn u mu, cn khong 10 g mu vi chnh xc 0,2 mg, nghin nh bng my nghin thc
vt ti v cho vo cc 250 ml, thm nc ct n khong 200 ml.
6.2.2 Cho cc vo l vi sng v tin hnh un vi sng mc nng lng cao 100 % trong thi gian 7 min (cng
c th un mc nng lng 70 % trong thi gian 12 min).
6.2.3 Ly ra ngui, lc b b v nh mc dch lc bng nc ct n 200 ml. Ly 10 ml xc nh NO 3- v
10 ml xc nh NO2-.
6.3 Xc nh nitrat
6.3.1 Xy dng th chun NO3-, dy tiu chun 0 mg NO3-/l n 1 mg NO3-/l
6.3.1.1 Chun b dy cc 250 ml, thm vo mi cc mt lng dung dch nitrat tiu chun 10 mg/l theo th t ln
lt 0,0; 0,5; 1,0; 2,0; 3,0; 4,0; 5,0 ml.
6.3.1.2. un cch thy cho bay hi n cn (khng chy) v ngui.

GHI CH 1: C th c cn bng l vi sng mc nng lng thp 30 % cng sut, trong thi gian khong 5 min
n 10 min.
6.3.1.3 Thm vo mi cc 1 ml dung dch axit phenoldisulfonic v lc mnh cho phn ng xy ra nhanh chng.
6.3.1.4 yn 10 min, sau thm mi cc khong 20 ml nc ct.
6.3.1.5 Cn thn thm vo mi cc 8 ml dung dch NH 4OH t l 1:1 theo th tch pH nm trong khong t 10
n 11.
GHI CH 2: C th trung ha dung dch bng cch nh tng git dung dch NaOH 10 %, th bng qu tm, cho
n khi dung dch chuyn mu vng (d mt t NaOH khng nh hng n mu ca dung dch).
6.3.1.6 Chuyn dung dch trong cc vo bnh nh mc dung tch 50 ml, nh mc bng nc ct n vch v lc
k.
6.3.1.7 Sau 20 min, o hp th quang bc sng 410 nm. Sau khi biu din ln th ta c ng chun
c nng NO3- t 0 mg/l n 1 mg/l.
6.3.2 o mu
6.3.2.1 Chun b dy cc 250 ml, ly vo mi cc 10 ml dch chit bng l vi sng.
6.3.2.2 Tip tc cc bc t 6.3.1.2 n 6.3.1.6.
6.3.2.3 o hp th quang ca dung dch mu bc sng 410 nm.
6.3.2.4 ng thi tin hnh mu trng vi 10 ml nc nh vi dung dch mu.
6.3.2.5 o dung dch mu ng nht iu kin nh o dung dch tiu chun.
6.3.2.6 Cn c vo th chun v s o mu trn my xc nh c nng mg NO 3-/l trong dung dch o, t
suy ra hm lng NO3- trong mu.
6.3.3 Tnh kt qu
Hm lng nitrat tnh theo miligam/kg mu ti (mg NO3-/kg mu ti) c tnh theo cng thc:
mg NO3-/kg mu ti =

a x V x 1000
V x m

Trong :
a Hm lng NO3- tnh bng miligam trong th tch trch (mg);
V Th tch dung dch mu sau khi chit tnh bng mililit (ml);
V Th tch dung dch chch ra xc nh tnh bng mililit (ml);
m Khi lng mu ti tnh bng gam (g);
1000 H s qui i t gam (g) sang kilogam (kg).
6.4 Xc nh nitrit
6.4.1 Xy dng th chun NO2-, dy tiu chun t 0 mg NO 2-/l n 0,5 mg NO2-/l, s dng thuc th Griss kiu
c
6.4.1.1 Chun b dy bnh nh mc dung tch 50 ml, thm vo mi cc mt lng dung dch nitrit tiu chun 5
mg/l theo th t ln lt 0,0; 0,5; 1,0; 2,0; 3,0; 4,0; 5,0 ml.
6.4.1.2 Thm vo mi bnh 1 ml thuc th dung dch sulfanilic v 1 ml thuc th - naphthinlamin (5.5.1).
6.4.1.3 Ln nh mc bng nc ct n vch v lc k.
6.4.1.4 Sau 20 min, o hp th quang ca dung dch bc sng 520 nm, thi gian o khng qu 1 h k t
khi phn ng mu. Sau biu din trn th ta c ng chun c nng NO2- trong dung dch t 0 mg/l
n 0,5 mg/l.
GHI CH 4: C th dng thuc th Griss ci tin (5.6.2) bng cch cho vo bnh nh mc 1 ml thuc th
Sulfanillamit v 1 ml thuc th N (1-naphtyl) etylen diamin dihydroclorua (NED) bc 7.4.1.2. Cc bc tip
theo nh 6.4.1.3 v 6.4.1.4.
6.4.2 o mu
6.4.2.1 Chun b dy bnh nh mc dung tch 50 ml, ly vo mi bnh 10 ml dch mu chit bng l vi sng.
6.4.2.2 Tip tc cc bc t 6.4.1.2 n 6.4.1.3.
6.4.2.3 o hp th quang ca dung dch mu bc sng 520 nm
ng thi tin hnh mu trng vi 10 ml nc nh vi dung dch mu.
o dung dch mu ng nht ng nht iu kin nh o dung dch tiu chun.

Cn c vo th chun v s o mu trn my xc nh c nng mg NO 2-/l trong dung dch o, t suy

ra hm lng NO2- trong mu.
6.4.3 Tnh kt qu
Hm lng nitrit tnh theo miligam/kg mu ti (mg NO2-/kg mu ti) c tnh theo cng thc:
mg NO2-/kg mu ti=

a x V x 1000
V x m

Trong :
a Hm lng NO2- tnh bng miligam trong th tch trch (mg);
V Th tch dung dch mu sau khi chit tnh bng mililit (ml);
V Th tch dung dch chch ra xc nh tnh bng mililit (ml);
m Khi lng mu ti tnh bng gam (g);
1000 H s qui i t gam (g) sang kilogam (kg).
7 Bo co th nghim
Bo co th nghim cn bao gm nhng thng tin sau:
a) Vin dn tiu chun ny;
b) c im nhn dng mu;
c) Kt qu xc nh nitrat v nitrit;
d) Nhng chi tit khng quy nh trong tiu chun ny hoc nhng iu c coi l ty chn v cc yu t c th
nh hng n kt qu th nghim.