tCvn

Tiu chun Vit Nam

tcvn 6132 : 1996

Cht lng t Xc nh d lng lindan trong t Phng php sc k lng

Soil quality - Determination of lindant residue in soilGas liquid chromatographic method (GLC)

H ni - 1996

TCVN 6132:1996

Li ni u
TCVN 6132: 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 6132:1996

Tiu chun Vit Nam

TCVN 6132:1996

Cht lng t - Xc nh d lng lindan trong tPhng php sc k lng

Soil quality - Determination of lindant residue in soilGas liquid chromatographic method (GLC)

1. Phm vi p dng Tiu chun ny qui nh phng php phn tch d lng lindan trong t. Phng php ny cng c th p dng xc nh mc nhim t do do s dng cht ny tr su bo v cy trng hay r r khi vn chuyn bo qun. Gii hn xc nh ca phng php: 0.005mg/kg. 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 li trong t cha b phn hu hoc cha 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 s k lng, gii hn pht hin l lng hot cht nh nht a vo my thu c pc sc kh c chiu cao gp ba ln nhiu ng nn nhy ti a c th c khi vn hnh.

TCVN 6132:1996
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 chn a vo i tng phn tch khi tin hnh nghin cu xy dng phng php. 4. Nguyn tc Dng dung dch nc - axeton tch lindan t mu t, sau chit lindan t dung dch trn vo hexan, tinh ch tip bng axit sunfuric,sc k ct silicagen v nh lng bng phng php sc k lng dng detector bt electron (GLC/ECD). Phng php ny dng phn tch d lng lindan trong t khi c mt cc cht hu c khc nh DDT. 5. Thuc th - n- hexan loi tinh khit ho hc. - axeton loi tinh khit. - Diclometan loi tinh khit ho hc. - axit sunfuric c (d = 1.84), tinh khit ho hc; - Natri sunfat khan loi tinh khit ho hc; - Cc dung dch chun lindan trong hecxan 0.2 v 0.02 chun gc 100 g/ml lindan trong hecxan; - Kieselgen 60, 70 - 230 mesh, art.7734 (ca hng Merck hoc tng ng); - Nc ct. 6. Thit b dng c Cc dng c thng thng trong phng th nghim v cc thit b dng c sau: - Bnh nn nt mi dung tch 250, 500 ml; - Bnh ct nhm q l dung tch 10, 50, 100 ml; - Phu chit dung tch 50, 250, 1000 ml; g/ml c iu ch t dung dch

TCVN 6132:1996
- Phu lc thu tinh ng knh 4 - 8 cm; - Bom kh ar -CH4 (95:5). - Ci chy s; - Ry kch thcl 0.5 mm. - Ct sc k (nhi silicagen) c kho vn; - B ct quay di p sut gim; - My sc k kh detector bt eletron (Packard H lan hoc cng loi); - ng tim Hamilton chia vch ti 0.2 - T sy; - My lc; - Bng thu tinh. 7. Ly mu Mu t c ly theo TCVN 5297 : 1995. Nn 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. Cch tin hnh 8.1 Xy dng ng chun Pha dy dung dch hiu chun c nng 0.01; 0.02; 0.05; 0.1; 0.2; 0.3; trong hexan. Bm chnh xc 1 g/ml lindan l.

l mi loi 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 05 mm loi b cc tp cht c hc. Cn 30-40 g t vo bnh nn nt mi loi 500 ml (ng thi cn mt mu t khc vo cc, sy 1050C trong mt gi xc nh m ca mu).Thm vo 50 ml nc ct lc vi hexan, y nt, lc, i 30 pht cho t ngm nc ri thm 150 ml axeton v lc 1 gi

TCVN 6132:1996
trn my lc. 1 gi cho lng trong ri gn sang ng ong loi 250 ml (ly ti a). Thm 100 ml axeton vo mu t v lc tip 1 gi chit ln th hai. lng trong v gn lp axeton vo ng ong trc y, o th tch tng cng. T th tch ny v th tch tng cng nc - axeton ly (50 ml + 150 ml +100 ml = 300 ml) bit c lng nc -axeton cn li trong t hiu chnh khi tnh ton. Sau chuyn phn chit c t ng ong sang phu chit loi 1000 ml c sn 100 ml hexan v 200 ml nc lc sn vi hecxan. Trng k ng ong bng mt ln nc, hai ln axeton (mi ln 5 ml), tt c vo phu chit. Lc trn my lc t 10 n 15 pht cho cc cht hu c chuyn vo lp hexan. i 20 -30 pht cho phn lp hon ton, tch lp nc axeton di vo mt phu chit khc, thm 50 ml hexan, lc 5 pht ri yn cho phn lp, tch b lp nc -axeton, nhp phn hexan ny cng vi lng hexan ra li phu (5 ml) vo phn hexan phu chit u. Thm 200 ml nc lc vi hexan vo phu v lc 10 - 15 pht, yn 20-30 pht cho phn lp hon ton, tch b lp nc, lp li nh vy mt hai ln na loi ht axeton v cc cht phn cc khc. Lm khan phn hexan cn li trong phu bng Na2SO4 khan v ct loi hexan trong my ct quay di p sut gim 40-500C n cn 2-3 ml. 8.3 Lm sch Chuyn 2-3 ml dung dch va ct loi hexan trn cng lng hexan trng bnh (0.5-1 ml) vo phu chit nt mi c 50 ml v lc vi axit sunfuric 98% (2-3 ml) cho n khi mt mu honton. Sau khi kh mu, ra phn hexan 3-4 ln bng nc cho n ht axit. Lp hexan ny cng vi lp hexan trng ra phu chit c lm khan bng Na2SO4 khan v c tinh ch tip trn ct silicagen. Cn 5.1 g klgel 60, hot ho trong t sy 15 gi 2000C. Cho t t hexan vo cc cha kieselgel va ly trong t sy ra cn nng, trn u nhanh vo ct. Dng ng nh git ht thm hexan trng ra, chuyn ht kieselgen bm trn thnh ct xung di to thnh lp kieselgen c b mt phng. Tho bt lp dung mi cho chy xung bnh hg ch lilp hexan khong 1 cm trn b mt kieselgen. Dng ng nh git sch a cht c x l phn trn cng hexan trng ra bnh ng cho vo ct. Lp phu chit cha dung mi vo u ct v iu chnh cc kho vn sao cho tc dung mi chy t phu chit xung ct sc k v t ct sc k xung bnh hng tng phn on bng nhau, khong 60 git/pht. Thu ly 3 phn on sau: Phn on 1 l 40 ml hexan cha DDT Phn on 2 l 60 ml hexan cha polyclobiphennyl

TCVN 6132:1996
Phn on 3 l 40 hn hp diclometan: hexan= 1:4 theo th tch, cha lindan. Ly phn on 3 cha lindan em ct quay di p sut gim 40-500C loi dung mi n va kh. Dng ng nh git ht mt t hexan ho tan cht cn li v trng ra bnh ct. Chuyn cc phn ho tan, ra, trng vo bnh nh mc 1 ml, thm hexan n vch mc. 8.4 Phn tch Bm chnh xc 1 nh sau: My sc k kh Ct sc k: 0V- 101, di 25 m, ng knh 0.25 mm. Nhit detector : 3000C, nhit nector 2500C; nhit ct: 700C, 15 pht, 50C/pht, 2000C/10 pht (chy theo chng trnh nhit ). Kh mang Ar + CH4 (5%), p sut ct 1,2 .105 Pa (1.2 kg/cm2). Thi gian lu v khong tuyn tnh ca detector i vi. Cht Lindan 9. Biu th kt qu 9.1 Tnh ton Hm lng lindan (X), tnh bng miligam trn kilogam, tnh theo cng thc: Thi gian lu (pht) 26 - 179 Khong tuyn tnh (ng) 0.01 - 0.3 l dung dch thu c trn y vo my sc k lng iu kin phn tch

X =
trong

AVH 2V 2 H !V1 P

A l nng cht chun, tnh bng miligam trn microlit; V l th tch cht chun bm vo my,tnh bng micrrolit; H2 l chiu cao ca pic mu,tnh bng milimet (hoc s m);

TCVN 6132:1996
V2 l th tich cui cng ca mu, tnh bng microlit; H1 l chiu cao ca pic chun, tnh bng milimet (hoc s m); V1 l th tch mu bm vo my, tnh bng microlit; P l lng cn mu t, tnh bng kilogam. 9.2 chnh xc chnh xc ca phng php nh sau : Gii hn pht hin ca my iu kin phn tch nu : 0.004 ng. Gii hn xc nh ca phng php: 0.005 mg/kg. pht hin: 65 - 85%. lch chun s(n = 4) = 18.7% mc 0.01 ppm. 10. Bo co kt qu Bn bo co kt qu phi bao gm cc thng tin sau: a) tham kho tiu chun ny; b) c im nhn dng xut s ca mu t; c) tnh cht ring ca mu t (v d s cmt ca set, si ct hay c, rc vn...) d) kt qu xc nh lindan; e) cc yu t t chn v nhng yu t khc c th nh hng n kt qu. -----------------------------------------------