You are on page 1of 7

tCvn

Tiu chun Vit Nam

tcvn 6134 : 1996

Cht lng t - Xc nh d lng trong t 2,4- D trong t - Phng php sc kh lng hiu sut cao
Soil quality - Determination of 2.4 - D residue in soil - High - Performence liquid chromatographic method (HPLC)

H ni - 1996

TCVN 6134:1996

Li ni u TCVN 6134:1996 do Ban k thut Tiu chun TCVN/TC 190 Cht lng t bin son, Tng cc Tiu chun - o lng - Cht lng ngh, B Khoa hc, Cng ngh v Mi trng ban hnh.

TCVN 6134:1996

Tiu chun Vit Nam

TCVN 6134:1996

Cht lng t - Xc nh d lng trong t 2,4- D trong t - Phng php sc kh lng hiu sut cao
Soil quality - Determination of 2.4 - D residue in soilHigh - Performence liquid chromatographic method (HPLC)

1. Phm vi p dng Tiu chun ny quy nh phng php xc nh lng d lng 2.4-D trong t. Phng php ny c th p dng xc nh mc nhim t do s dng cht ny cng nh cc loi ho cht tr c thuc nhm phenoxyaxetic axit khc bo v cy trng, hay do r r khi vn chuyn, bo qun. Gii hn xc nh ca phng php : 0.01 r r m. 2. Tiu chun trch dn Tiu chun ny s dng cng vi: - TCVN 5297 : 1995 Cht lng t - Ly mu - Yu cu chung - TCVN 5941 : 1995 Cht lng t - Gii hn ti a cho php d lng ho cht bo v thc vt trong t. 3. nh ngha Tiu chun ny dng cc nh ngha sau: 3.1 D lng cht tr sinh vt hi trong t: lng cht tr sinh vt hi cn st li trong t cha b phn hu hoc cha b bin i thnh cc dng khc. 3.2 Gii hn pht hin ca my: Kh nng pht hin cao nht ca thit b phn tch i vi i tng phn tch. Khi thit b phn tch l my sc l lng, gii hn pht hin l lng hot

TCVN 6134:1996
cht nh nht a vo my thu c pc sc k c chiu cao gp ba ln nhiu ng nn nhy ti a c th c khi vn hnh. 3.3 Gii hn xc nh ca phng php: nng thp nht xc nh c trong i tng cn phn tch vi cc iu kin c la chn. 3.4 pht hin (recovery): kh nng xc nh c (tnh theo phn trm) Lng cht cn phn tch so vi lng cht chun a vo i tng phn tch khi tin hnh nghin cu xy dng phng php. 4. Nguyn tc 2.4 Dtrong t c chit soxhlet bng dung mi axeton. Thu phn dch chit bng kim. Axit ho dung dch thu phn chuyn v dng axit. Chit dng axit sang pha hu c. Lm sch pha hu c bng ct sc k cha silicagen, natri sunphat. Xc nh hm lng 2.4- D bng sc k lng hiu sut cao dng detector cc tm. Phng php ny dng phn tch d lng ho cht tr c thuc nhm phenoxyaxetic nh 2.4 D (bao gm 2.4 -D dng mui natri, dng este, dng amin...) MCPA, 2, 4, 5-T... trong t. 5. Thuc th - Axeton loi tinh khit; - Etyl axetat loi tinh khit; - Metanol loi tinh khit dung cho sc k; - Natri sunphat loi tinh khit phn tch; - Axit sunfuric loi tinh khit phn tch, nng loi 18 N; - Kali hidroxit loi tinh khit phn tch; - 2.4-D chun (99%) - Nc ct 2 ln. 6. Thit b, dng c Cc dng c thng thng trong phng th nghim v cc thit b dng c sau: - B chit Soxhlet loi 150 ml.

TCVN 6134:1996
- Bnh cu nt mi loi 100, 250 ml. - Phu cjit loi 100 ml. - Mng siu lc kch thc l 0.45 m m. - My dung siu m. - My chng ct quay. - H thng sc k lng c vng bm mu 20m l, trang b detector cc tm. - Ry kch thc l 2 mm. 7. Ly mu Mu t c ly theo TCVN 5297 :1995. Cn xc nh thm thnh phn c l, ho hc ca t c c s nhn nh b sung v tnh trng din bin, kh nng lu gi v lan truyn cht nhim. 8. Tin hnh th 8.1 Xy dng ng chun Pha dy dung dch hiu chun c nng 0.5; 1.0; 2.0; 5.0; 8.0; v 10 m g/ml 2.4-D trong metanol. Bm chnh xc 20 m l mi dung dch trn vo h thng sc k lng iu kin phn tch nh iu 8.4 ca tiu chun ny xy dng ng chun v xc nh gii hn pht hin ca my. 8.2 Chit tch Ry mu t qua ry c kch thc l 2 mm loi b cc tp cht c hc. Cn 25 g t vo ti ng mu v t vo ng Soxhlet. Cho 100 ml dung mi axeton vo bnh cu loi 250 ml. lp bnh cu vo b chit Soxhlet. Lp bnh cu vo my chng ct quay.Lm bay hi dung mi 400C trong my chng ct quay vi p sut gim n cn. Tho bnh cu, cho thm 50 ml nc ct, 3 g KOH v mt t ht si. un hi lu trong 2 gi trn bp cch thu. ngui n nhit phng v chuyn vo phu chit loi 100 ml. Thm 25 ml axit sunfuric 18 N, lc 2 pht, yn 10 pht. Chit 2.4-D sang pha pha hu c bng etyl axetat, ln th nht s dng 20 ml, hai ln sau mi ln 10 ml. Tp hp pha hu c v cho chy qua phu lc c cha 10 g natri sunphat khan. Ra lp natri sunphat 2 ln, mi ln bng 10 ml etyl axetat tinh khit. Tp hp ton b pha hu c vo bnh cu loi 100 ml. Lp bnh cu vo my chng ct quay, cho bay hi dung mi 600C, p sut gim xung cn khong 5 ml.

TCVN 6134:1996
8.3 Lm sch Lt mt t bng thm nc vo y ct sc k bng thu tinh ng knh trong 1.2 cm. Chuyn 5gnatri sunphat vo ct. Cho tip 5g silicagen hot ho loi dng cho sc k c kch thc ht 60 mesh (0.250 mm). Cho tip 5g natri sunphat khan. G nh ct ln cht cc cht nhi. tmt lp bng thm nc ln mt ct. Tm t ct bng 10 mldung mi axeton c thnh phn t l 1: 9 (v/v). Hng dung dch chy qua ct vo bnh cu c nt mi loi 100 ml. Lp bnh cu vo my chng ct quay. Lm bay hi dung mi di p sut gim nhit 400C cn khong 10 ml. Chuyn dung dch cn li vo bnh qu l loi 25 ml. Lp bnh qu l vo my chng ct quay, tip tc lm bay hi n cn khong 1 ml iu kin trn. Tho bnh qu l ra khi my chng ct quay. Tip tc lm bay hi ngoi khng kh n dung mi bng dng kh kh. 8.4 Phn tch Ho tan cn trong bnh qu l bng0.5 ml metanol. Lc dch chit qua mng siu lc. Thu dch lc, bm 20 m l vo my sc k lng iu kin phn tch nh sau: Ct pha o cha cht nhi C-18, kch thc 150 x 4.6 mm. Pha ng: metanol-nc axit axetic 55.0-44.5-0.5 (v/v) c ui ht bt kh bng my dung siu m. Bc sng phn tch: 230 nm. Tc dng: 1.0 ml/pht. 9. Biu th kt qu 9.1 Tnh ton Da vo thi gian lu(tR) ca chun v mu nhn bit 2.4-D v t din tch hoc chiu cao pic, tnh ton nng 2.4-D c trong t theo cng thc sau:

N=
trong :

Am C c V Ac m

N l nng 2.4-D trong t, tnh bng r r m; Am l din tch hoc chiu cao pic mu, tnh bng milimet vung hoc milimet;

TCVN 6134:1996
Ac l din tch hoc chiu cao pic chun, tnh bng milimet vung hoc milimet; C0 l nng dung dch chun, tnh bng microgam trn microlit; m l khi lng mu dng chit sut, tnh bng gam; V l th tch dung dch mu dng phn tch, tnh bng mililit. 9.2 chnh xc chnh xc ca phng php nh sau: Gii hn pht hin ca my iu kin phn tch nu:0.5 m g/ml. Gii hn xc nh ca phng php: 0,01 r r m. pht hin : 90 - 96%. lch chun s (n = 5) = 7.6% mc 0.1 r r m v 6.0% mc 1 r r m. 10. Bo co kt qu Bo co kt qu phi bao gm cc thng tin sau: a) tham kho tiu chun ny; b) c im nhn dng xut x ca mu t; c) tnh cht ring ca mu t (s c mt ca st, ct, si, c, rc vn ...); d) kt qu xc nh d lng 2,4-D; e) cc yu t t chn v nhng yu t khc c th nh hng n kt qa. __________________________________

You might also like