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TRNG I HC KHOA HC T NHIN I HC QUC GIA H NI

Mn:

CC PHNG PHP PHN TCH C CHT

TI: PHNG PHP PHN TCH DDT TRONG T


GVHD : Trn Vn Sn Sinh Vin : Nng Vn Huynh Lp : K54 c hc mi trng

[Type text]

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Phng php phn tch DDT trong t


Mt s nt chung v DDT
DDT (Dichloro - Trichloroethane Diphenyl) l mt trong nhng thuc tr su tng hp c bit n nhiu nht. DDT c tng hp u tin vo nm 1874, nhng thuc tnh thuc tr su ca DDT th cho n 1939 mi c khm ph. Vo nhng nm u ca Chin tranh Th gii th II, DDT c s dng vi lng ln kim sot mui truyn bnh st rt, bnh st pht ban, v cc bnh do cn trng khc trong c qun i ln dn c. DDT tr thnh loi thuc tr su ph bin s dng trong nng nghip. Chng c mt khp mi ni, trong khng kh, t, nc do mt lng ln c gii phng ra khi phun trn cc cnh ng v rng dit mui v cn trng.

Trong qu trnh d ng v pht trin t nc, khng ch it am m trn c th giivic s dng khoa hc cng ngh hin i mt phn th c nn kinh t pht trin song mt khc li l m cho cuc sng con ng i ng c ng nh hng i nhi m mi tr ng. ng dng rng ri cc loi ha cht v o qu trnh sn ut tr th nh s lm dng. Tu n c li v trc mt song li c nh hng rt ln vlu d i, n c th tn ti cc loi th c ph m ca con ng i, trong khng kh, t, nc Trong c DDT v mt s hp cht o v th c v t nhm c clo. g na DDT cm s dng do tnh c ca n nh c kh nng g ung th tim t ng, g t bin v gy nhi m mi tr ng nghim trng. bo v mi tr ng v sc khe con ng i, cn phi x l kh c DDT trong mi tr ng t cng nh trong cc mi tr ng khc. DDT trong t c th gim i do s a hi, s i mn t, s hp thu ca ng v t, th c v t v s phn hy sinh hc ca cc vi sinh v t c sn trong t nhng vi th i gian tng i lu.

Phn I Tng quan ti liu


1. C IM CU TRC V TNH CHT L HA CA DDT
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1.1.khi nim v mt s nt v DDT


Tn th ng: Dichloro Diphen l Trichloroethane.(DDT) Tn ha hc: 1,1,1-trichloro-2,2-bis(p-chlorophenyl) ethane Cng thc ha hc: C14H9Cl5 Trng lng phn t: 354,51 vC mt thuc o v th c v t rt n vng do n c kh nng tr vi cc phn ngquang phn, vi i trong khng kh. Trong mi tr ng kim n d deh droclorua ha hoc polime ha th nh sn ph m dng nh a c m u

1.2.cu trc ca DDT


DDT l mt trong cc thuc dit cn trng, chng l mt nhm cc hp cht hu c c hai vng thm v c cha Clo, bao gm 14 hp cht hu c,trong : 71% l p,p,DDT, 14.9% l o,p,- DDT, 0.3%p,p,- DDD, 0.1% l o,p,-DDD, 4% l p,p,- DDE, 0.1% l o,p,-DDE, sn ph m khc l 3.5%

1.3. Tnh cht l ha ca DDT


Tt c cc ng phn ca DDT u l dng tinh th mu trng, khng mi, khng v , c cng thc tng qut l C14H9Cl5, khi lng phn t l 354.5. Nhit nng chy khong 108.5 - 1090C, p sut a hi l 2.53 x10 -5 Pa (1.9 x10 -7mmHg) ti 200C. DDT tan t trong nc (1mg/l) nhng c kh nng gi nc, tan tt trong cc hp cht hu c c bit l m ng v t. Kh nng ho tan ca DDT trong nc l thp (h s hp ph cao) nn DDT c xu hng b hp ph trong cn n, t , trm tch. iu n c vai tr c bit trong phn hy sinh hc DDT DDT l mt organochlorine, l mt loi t tinh khit c m u trng, mi thm d u n ph m thng mi cm u t trng n m sm rt t tan trong nc nhng khi ha tan DDT trong nc th ch ng to th nh hu n ph. hit nng ch : 108,5 C - 109 C, p sut hi 20 C l 1,5.10 mm g T trng: 1,55 Tan nhiu trong cc dung mi hu c nh kh nng ha tan trong m rt n do DDT c tch l qua chui thc n

2. Cng thc cu to mt s ng phn ca DDT

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P-P DDT P-P DDE : P-P DDD :

O-P DDT :

O-P DDE :

O-P DDD : 3. ngun gc pht sinh DDT


DDT [ 1,1,1-trichloro-2,2-bis-(p-chlorophen l)ethane] c tng hp v o nm 1874, nhng mi n 1930, Bc s Paul uller (Th ) mi xc nh n DDT l mt ha cht hu hiu trong vic tr su ry v t c xem nh l mt thn dc v khng bit c nh hng nguy hi n con ng i. Khm ph trn mang li cho ng gii Nobel v khoa nm 1948 v DDT c s dng rng ri khp th gii cho vic kh trng v kim sot mm mng gy bnh st rt. hng ch hai th p nin sau , mt s chuyn gia th gii khm ph ra tc hi ca DDT trn mi tr ng v sc khe ng i dn. Do , ti Hoa K t nm 1972 DDT cm s dng hn. DDT b nhi m v o mi tr ng khng kh, nc, t trong sut qu trnh s dng, DDT c mt nhiu v tr nhi m khc nhau, sau c th tip tc b lan truyn v gy nhi m mi tr ng. DDT c hiu qu chng li r n, b cht, v mui mang cc mm bnh st pht ban, d ch hch, st rt, v st v ng .v.v. DDT c dng rt rng ri hn 20 nm v
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c xem l nhn t chnh trong vic gia tng sn lng lng th c th gii v ngn chn bnh t t t cn trng. DDT thot ra t cc nh m sn ut t hn 30 nm trc, theo dng nc v trm tch di in su Cht DDT sau n c tm th trong ngun nc sinh hot vng ng ng song Cu ong vi h m lng l 0,11 Trong nng nghip dng o v c trng, trong t dit mui v su . DDT l loi thuc ha hc dit cn trng c s dng rng ri t chin tranh th gii ln th II trn khp th gii v hng triu tn c sn xut, s dng trc hin ang cn lu gi trong t v s tip tc phn tn trong mi tr ng. Mt lng ln DDT c gii phng vo khng kh, t v nc khi s dng dit cn trng, mui cc a im nhy cm nh ca sng

4.tnh trng nhim DDT trn th gii


Do tc hi ca DDT trn mi tr ng v sc khe ng i dn ti Hoa K t nm 1972 DDT cm s dng hn. Tu nhin, n nay ha cht ny vn cn gy tc hi nhng vng nng nghip s dng v nhng vng quanh ni sn xut ra DDT trc . in ti DDT vn cn ngng t ni thm lc a vng Palos Verdas (ngo i khi vng in Los Angeles) v nh my sn xut ra DDT Montrose Chemical.co ti Torrance thi DDT vo h thng cng rnh thnh ph v o nm 1971. Vic x l nhi m DDT cho vng n c tnh vo khong 300 triu USD Cho n nay M do li ch v kinh t nn vn sn xut DDT xut cng qua Phi chu v cc nc chu trong c it Nam. DDT l mt loi thuc st trng cng hiu mnh, c bit quan trng trong vic kim sot bnh st rt nn vn c s dng rng ri cc nc ang pht trin bt chp ngu c g hi tim tng v lu di ca n. S tch t nhiu nht ca DDT v cc hp cht c lin quan bin pha Ty ca Trung Quc. cc b bin khc, lng tch t ca DDT cng rt ln nh: v nh Bengal, bin Arabian, bin bc Trung Quc v.v Canada, tng lng DDT lng ng trn b mt trm tch 8 h khc dc ngang lc a vo khong 9.7ug/kg Nhiu nghin cu cng cho thy s c mt ca DDT trong cc mu trm tch vi nng cao do DDT c v n chuyn t khu v c b nhi m n Bc c c v Nam c c

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Lng DDT cao nht c tm thy gn khu v c ni m DDT vn c s dng, v d b bin Arabian ca n . Cc khu v c m lng DDT trong khng kh cao l eo bin Malacca, b bin pha nam Trung Quc, v nh Mexico.

5. Tnh trng nhim DDT Vit Nam


DDT c dng ln u tin Vit am v o nm 1949 phng nga bnh st rt. Tuy nhin, s lng thuc DDT c dng ch c 315 tn trong nm 1961 v gim xung cn 22 tn trong nm 1974. T nm 1957 n 1990, tng s lng thuc DDT nh p cng ch c 240.422 tn. Mc d vic s dng thuc DDT cng ng quc t ngn cm t nm 1992, vic nh p cng v s dng DDT Vit Nam vn tip tc cho n nm 1994. Trong khong t nm 1992 n nm 1994, s lng thuc DDT nh p cng t ga ln n 423.358 tn Tuy khng c s liu chnh xc v s lng DDT ang c s dng Vit Nam, nhng tin tc trong nc cho bit thuc ny vn cn ang c s dng rng ri c bit vng chu th sng Cu Long v l vng c nhiu sng rch v nhiu mui mng Ti mt kho d chin cha DDT nhng nm 1967 1968 Tnh vn cn mt lng tn d ln ha cht ny. Khi lng thuc DDT kho n c tnh khong 45 tn. Hin nay s thuc DDT n m phi l trn mt t, mt phn thuc c th b phn hy song phn ln vn cn , ch ng c th khuch tn vo khng kh gy nhi m mi tr ng v phn r ngm vo t v cc mch nc ngm gy nhi m t v nc trong khu v c Ngh An l mt trong nhng t nh cn tn lu mt lng tng i ln ha cht bo v th c v t, hin ti t nh c 25 im tn lu ha cht cht bo v th c, trong mi c 5 im c x l. Phn ln nhng im tn lu ha cht cht bo v th c u n m gn, hoc nguy him hn l n m lt trong khu dn c. Mt kt qu iu tra khc t nh Ngh An cho thy, DDT vn cn trong mt nh kho t nm 1965 n nm 1985. Nng ca DDT tha i t 3.38 n 960.6 mg/kg trong cc mu t v t 0.00012 n 0.00168 mg/l trong cc mu nc. Trong nhiu nm lin tip, mi thuc DDT nng nc a a n 600 mt. c 25 ng i cht v ung th, v 22 tr ng hp d thai c ghi nh n

6. tc hi ca DDT i vi mi trng t nhin


Cc cht thi sinh ra t qu trnh s dng ha cht trong nng nghip nh phn n,thuc tr su, thuc dit c l m cho mi tr ng t nhi m do s tn d ca ch ng trong t qu cao v tch l trong c trng Do thuc tn ng lu khng phn h nn n c th theo nc v gi pht tn ti cc vng khc, theo cc lo i sinh v t i khp mi ni
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DDT cth i gian n phn h l 5 15 nm, khi i v o c thth c v t, ch ng ctch l v t c o thi ra ngo i hi pht thi ra kh qu n, DDT s c kh nng di chu n h ng nghn dm trong kh qu n n cc khu v c lnh hn th kt ta li ri tr li ung mt t, tch t trong mng i v cc lo i ng v t. Do DDT c th nh phn tng i n nh nn kh phn gii trong mi tr ng t nhin v thm nh p v o c th cc lo i chim theo h thng nc, th c v t ph du, ng v t ph du, tm c nh DDT l m gim s pht trin ca to nc ngt chlorella, gim kh nng quang hpca cc lo i to in Thuc DDT trong khng kh phi sau 10 nm mi gim nng ung t l an u l 1/10, DDT tan trong in cn phi mt th i gian lu hn na mi phn h ht. DDT l hp cht cha clo g h u qu rt c i vi sinh v t khi c thi ra trong mi tr ng, DDT tn ti lu d i trong mi tr ng nc, khng phn h sinh hc v kh nng khuch i sinh hc cao. in na vn cn tm th DDT Bc C c trong nhng tng ng hoc trong mt s lo i chim di c

7. tc hi ca DDT i vi con ngi v ng vt


Trc ht ng v phng din cp tnh, nu n nh m th c ph m cha v i gram ha cht trong mt th i gian ngn c th nh hng tr c tip ln h thn kinh: kch thch, v t v, run, th gp, co gi t, c th dn ti t vong g i nhi m c s run r , co gi t mnh ko theo tnh trng i ma, m hi, nhc u v chng mt tn thng th n v thiu mu phng din mn tnh, khi nhi m c vi liu lng nh trong mt th i gian d i, chc nng ca gan tha i: to gan, vim gan, lng c t (em im) ca gan trong mu c th tng ln v DDT tch t trong cc m m, sa m v c kh nng gy v sinh cho ng v t c v v chim. u nhi m c v o khong 20 50mg/ng /kg c th, iu n c th nh hng n vic sinh sn, n cc tu n ni tit nh tu n gip trng, nang thng th n. u nhi m lu hn na c th a n ung th LC 50 (LC 50 l liu gy cht 50% mu sinh v t th nghim) mt s lo i ng v t thnghim l: LD50 ln khong 1.000mg DDT/kg, LD50 th l 300mg DDT/kg v 4.000-5.000 mg DDT/kg. DDT trong t cng c th c hp th bi mt s th c v t hoctrong c th con ng i khi n cc th c v t

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ng tng DDT (mg/kg) trn trng lng t v m t trong 6 c quan khcnhau ca c th c heo t cng in cotland; 1967 Cc ch tiu Tng DDT (trng lng t) % m Tng DDT ( trng lng m) M c voi 3.8 Gan c C bp 0.56 L lch 0.12 Thn

0.58

0.22

0.04

67 5.6

13.2 4.8

8.3 0.27

6.1 9.2

5.1 2.4

1.4 2.9

T kt qu ta nh n th r ng mc nhi m DDT ph thuc v o lng m, ring mc nhi m DDT trong c l thp nht mc d lng m ca c khng thp i vi cn trng: DDT tc ng ln h thn kinh trung ng v n chu n ion ( a , ) qua m ng t o to ra mt th hot ng l cha kha lan tru n ung thn kinh dc theo si trc (a on) DDT ha tan trong cc m m, tch l trong m ng cht o quanh t o thn kinh cn tr s v n chu n ion qua m ng t o cn tr lan tru n ung thn kinh trn si trc t o thn kinh ri lon chc nng thn kinh v n ng, cm gic => co gi t, t lit thn kinh v dn n cht

Phn II : Cht lng t- xc nh lng d DDT trong t- phng php sc k kh lng


1. Phm vi p dng
Tiu chu n n qu nh phng php c nh d lng ddt trong t Phng php p dng c nh mc nhi m t do s dng ddt bo v cy trng hay r r do bo qun v n chuyn Gii hn c nh ca phng php : 0.07mg/kg

2. Tiu chun trch dn


o Tiu chu n ny s dng cng vi :
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o QCVN 15:2008/ BTNMT D lng ha cht B T trong t o TC 5297 : 1995 cht lng t- l mu- u cu chung

3.nh ngha
Tiu chu n n dng cc nh ngha sau : 3.1 d lng cht tr sinh v t hi trong t : d lng cht tr sinh v t hi cn st li li trong t cha phn h hoc cha in i th nh cc dng khc 3.2 gii hn pht hin ca m : kh nng pht hin cao nht ca thit phn tch i vi i tng phn tch. hi thit phn tch l m sc k lng, gii hn pht hin l lng hot cht nh nht a v o m thu c pic sc k c chiu cao gp a ln nhi u ng nn nh ti a c th c khi v n h nh 3.3 gii hn c nh ca phng php : nng thp nht c nh c trong i tng cn phn tch vi cc iu kin c l a chn 3.4 pht hin ( recover ) : kh nng c nh c ( tnh theo % ) lng cht cn phn tch so vi lng cht chu n a v o i tng phn tch khi tin h nh nghin cu d ng phng php

4. Nguyn tc
Dng dung d ch nc- a eton tch DDT t mu t, sau chit DDT t dung d ch trn v o he an, tinh ch tip theo ng a it sunfuric, ct silicagen v nh lng ng phng php sc k kh lng dng detector t electron ( C/ECD) Phng php n dng c nh d lng DDT khi c mt cc cht clo hu c khc nh inDan, DDE, Adrin

5. thuc th
Axeton, tinh khit phn tch n- e an tinh khit ha hc Diclometan tinh khit ha hc A it sunfuric c (d 1.84) tinh khit ha hc atri sunfat khan tinh khit ha hc Cc dung d ch chu n DDT trong he an 0.2 v 0.02 ug/ml c iu ch t dung d ch chu n gc 100ug/ml DDT trong he an Kieselgen 60,70- 230 mesh, Art.7734 ( ca hng merck hoc c tinh nng tng ng ) c ct

6. thit b, dng c
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Cc dng c thng th ng trong phng th nghim v cc thit Bnh nn nt mi dung tch 250ml, 500 ml Bnh ct nhm qu l dung tch 10, 50, 100ml Ph u chit dung tch 50, 250, 1000 ml Ph u lc th tinh ng knh 4-8 cm Ci ch s Ct sc k (silicagen) c kha vn B ct qua di p sut gim Bom kh Ar- CH4 sc k dng detector t electron ng tim amilton chia vch ti 0.2ul t s m lc ng th tinh

dng c sau:

7. ly mu
u t l theo TC 5297 : 1995 n c nh th nh phn c l, ha hc ca t c c s nh n nh sung v tnh trng di n in, kh nng lu gi v lan tru n cht nhi m

8. cch tin hnh


8.1 xy dng ng chun
Pha d dung d ch hiu chu n c nng 0.1, 0.2, 0.5, 1, 2, 3 ug/ml DDT trong he an m chnh c 1 ul mi dung d ch trn v o m sc k iu kin phn tch ca tiu chu n d ng ng chu n v c nh gii hn pht hin ca m

8.2 chit tch


R mu t qua d c kch thc l 0.5 mm loi cc tp cht c hc. cn 3040 g t v o nh nn n t m i loi 500 ml (ng th i cn mt mu khc v o cc s 150 0c trong mt gi c nh m ca mu ), thm v o 50 ml nc ct lc vi he an, n t, lc, i 30 ph t cho t ngm nc ri thm 150 ml axeton v lc 1 gi trn m lc. 1 gi cho lng trong ri gn sang ng ong loi 250 ml (l ti a). Thm 100 ml a eton v o mu t v lc 1 gi chit ln th 2. lng trong v gn lp a eton v o ng ong trc , o th tch tng cng. t th tch ny v th tch tng cng nc-a eton l (50 ml+ 150 ml + 100 ml 300 ml) it c lng nc a eton cn li trong t hiu ch nh khi tnh ton. au chu n phn chit c t ng ong sang ph u chit loi 1000 ml c sn 100 ml he an v 200 ml nc lc vi he an. Trng k ng ong ng mt ln nc, hai ln axeton
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(mi ln 5 ml), tt c v o ph u chitDng dung d ch nc- a eton tch DDT t mu t, sau chit DDT t dung d ch trn v o he an, tinh ch tip theo ng a it sunfuric, ct silicagen v nh lng ng phng php sc k kh lng dng detector t electron ( C/ECD) Phng php n dng c nh d lng DDT khi c mt cc cht clo hu c khc nh inDan, DDE, Adrin Pha d dung d ch hiu chu n c nng 0.1, 0.2, 0.5, 1, 2, 3 ug/ml DDT trong he an m chnh c 1 ul mi dung d ch trn v o m sc k iu kin phn tch ca tiu chu n d ng ng chu n v c nh gii hn pht hin ca m . lc trn m lc 10-15 ph t cho cc cht hu c chu n v o lp he an. i 20-30 ph t cho phn lp ho n to n, tch lp nc- a eton di v o mt ph u chit khc, thm 50 ml hexan, lc 5 ph t ri n cho phn lp ho n to n, tch lp nca eton nh p phn he an n cng vi lng he an ra li ph u (5ml) v o phn he an ph u chit u. thm 200 ml nc lc vi he an v o ph u v lc 10-15 ph t, yn 20-30 ph t cho phn lp ho n to n, tch lp nc. lp li nh v 1-2 ln na loi ht a eton v cc cht phn c c khc. m khan phn he an cn li trong ph u ng a2 4 khan v ct loi he an trong m ct qua di p sut gim 40-50 0c n cn 2-3 ml.

8.3 lm sch
Chu n 2-3 ml dung d ch va ct loi he an trn cng lng he an trng nh (0.51 ml) vo ph u chit n t m i c 50 ml v lc vi a it sunfuric 98% (2-3 ml) cho n khi mt m u ho n to n. au khi kh m u, ra phn he an 3-4 ln ng nc cho n ht a it. p he an n cng vi lp he an trng ra ph u chit c l m kh ng a2 4 khan v c tinh ch tip trn ct silicagen Cn 5.1g kieselgel 60, hot ha trong t s 15 gi 200 0c. cho t t he an v o cc cha kieselgel va l trong t s ra cn nng, trn u nhanh v o ct. dng ng nh git h t thm he an trng ra, chu n ht kieselgel m trn th nh ct ung di to th nh lp kieselgel c mt phng. tho t lp dung mi cho ch ung bnh hng ch li lp he an khon 1 cm trn mt kieselgel. Dng ng nh git sch a cht c l phn trn cng he an trng ra nh ng cho v o ct. lp ph u chit cha dung mi v o u ct v iu ch nh cc kha vn sao cho tc dung mi ch t ph u chit ung ct sc k v t ct sc k ung nh hng tng phn on ng nhau, khong 60 git/ph t Thu l 3 phn on sau : Phn on 1 la 40 ml he an cha DDT
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Phn on 2 l 60 ml he an cha pol clo iphen l Phn on 3 l hn hp diclometan : he an 1 : 4 theo th tch cha indan phn on 1 cha DDT em ct qua 40-50 0c di p sut gim loi dung mi gn kh (cn 1-2 git cht lng) Dng ng nh git h t mt t he an ha tan cht cn li v trng ra nh ct. chu n cc phn ha tan, ra, trng, v o nh nh mc 1 ml, thm he an n vch mc

8.4 phn tch


Bm chnh c 1 ul dung d ch thu c trn v o m sc k kh cc iu kin phn tch nh sau : sc k kh Ct sc k : 0v -101,d i 25 m, ng knh 0.25 mm hit detector : 300 0c, nhit injector : 250 0c, nhit ct : 70 0c, 15 pht, 5 0c/ph t, 200 0c/10 ph t, (ch theo chng trnh nhit ) Kh mang Ar- C 4 (5%), p sut ct 1.2 .10 5pa (1.2 kg/cm2) Th i gian lu v khong tu n tnh ca detector i vi :

Cht DDT

Thi gian lu (pht) 36-487

Khong tuyn tnh (ng) 0.1-3

9. biu th kt qu
9.1 tnh ton
m lng DDT (X), tnh ng miligam theo cng thc :

Trong : A : nng cht chu n tnh ng mg/ul : th tch cht chu n m v o m (ul) 2 : chiu cao pic ca mu (mm)
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2 : th tch cui cng ca mu (ul) 1 : chiu cao ca pic chu n (mm) 1 : th tich m mu v o m (ul) P : lng cn mu t (kg)

9.2 chnh xc
chnh c ca phng php nh sau : ii hn pht hin ca m iu kin phn tch nu : 0.06 ng ii hn c nh ca phng php : 0.07 mg/kg pht hin : 90-95% lch chu n (n 4) 2.7% mc 0.1 ppm

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