TP CH KHOA HC V CNG NGH, I HC NNG - S 4(33).

2009

XY DNG PHNG PHP XC NH TNG ASEN TRONG MT S NGUN NC B MT THNH PH NNG BNG PHNG PHP QUANG PH HP TH PHN T UV-VIS
AN ANALYTICAL METHOD DEVELOPMENT FOR THE DETERMINATION OF TOTAL ARSENIC IN SOME SURFACE WATER SOURCES IN DANANG CITY WITH THE UV-VIS SPECTROPHOTOMETER ABSORBANCE MOLECULE METHOD L Th Mi

Trng i hc S phm, i hc Nng

TM TT Nc b mt l mt h phc tp bao gm nhiu cht v c v hu c tn ti nhiu trng thi khc nhau, trong phi k n hm lng kim loi nng c hi c bit l Arsen (As) - mt cht kch c. Kt qu ca vic xy dng phng php phn tch hm lng As trong nc b mt bng phng php quang ph hp th phn t UV-VIS v p d ng xc nh, nh gi hm lng As trong mt s ngun nc mt cho thy As c mt trong hu ht cc ngun nc mt (t 0,0027mg/lt n 0,0123mg/lt) trn a bn thuc thnh ph Nng tuy nhin mc an ton vn nm trong gii hn cho php ca TCVN (0,05mg/lt). ABSTRACT Surface water is a complex system containing many organic and inorganic compounds in different forms. Great attention is being paid to heavy metals because of their toxicities. Especially, among them is Arsenic (As) an extremely toxic metal. The protocol for total Arsenic determination in water by means of the UV-VIS spectroscopy method has been set up. The results of quantative analysis in some surface water sources in Danang city shows that Arsen can be found in all the water samples (from 0,0027mg/lit to 0,0123mg/lit) but the arsen content is below the permissible limit in accordance with the Vietnamese standard (0,05mg/lit).

1. t vn Nc b mt ng vai tr ht sc quan trng i vi s pht trin kinh t v x hi ca con ngi, ch yu tp trung cc ao, h, m... Hin nay trn a bn thnh ph Nng c khong 30 h, m thc hin cc chc nng chnh l iu tit nc, iu ha vi kh hu, to cnh quan p v x l nc thi th. V vy s nhim bn bi cc cht c hi v kim loi nng trong nc b mt l iu khng th trnh khi . c bit As l cht kch c, c th gy cht ngi khi b nhim c cp tnh v khi b nhim c mn tnh c th gy ra 19 loi bnh khc nhau, trong c cc bnh nan y nh ung th da, phi... Bnh nhim c mn tnh asen l mt tai ha mi trng i vi sc khe con ngi [1,3,5.6]. V vy phn tch nh gi hm lng As trong cc ngun nc l vic lm cp bch v l vn quan tm hng u ca cc nh khoa hc. Trong ti ny chng ti trnh by quy trnh xy dng phng php phn tch hm lng As trong nc b mt bng phng php quang ph hp th phn t UV-VIS. Trn c s
104

TP CH KHOA HC V CNG NGH, I HC NNG - S 4(33).2009

phng php xy dng p dng phn tch As trong mt s ngun nc mt trn a bn thuc thnh ph Nng . 2. Vt liu v phng php thc nghim 2.1. Thit b, dng c, ha cht. 2.1.1. Thit b, dng c: - My quang ph hp th phn t UV -VIS Jasca V-530 ca Nht Bn vi cuvt thch anh - B ct As. Pipt chia n 0,02ml; 0,1ml, bnh nh mc cc loi... 2.1.2. Ha cht. Cc ha cht thuc lo i tinh khit ha hc ca Cng ha Php, Cng ha c: Dung dch gc asen 1000ppm, H 2 O 2 30%. Mui: Natri Dietylditiocacbamat (Na-DDC), AgNO 3 , KI, Pb(CH 3 COO) 2 , Na 2 S, SbCl 3 . Axit: HCl c, HNO 3 c, H 2 SO 4 c. Thic ht, km ht. Nc ct hai ln. 2.2. Ly mu v x l mu: Mu nc b mt c ly cc ao, h, m trn a bn thnh ph Nng theo quy trnh ca TCVN trong thng 5 v thng 6/2009. Mu nc ng trong chai nha polyetylen v c x l s b bng HNO 3 c. 2.3. Phng php phn tch ha hc. phn tch hm lng As trong nc b mt, chng ti s dng phng php quang ph hp th phn t UV-VIS. 3. Kt qu v tho lun Cc phng php xc As rt a dng, tuy nhin ph hp vi iu kin nh ca phng th nghim hin nay, chng ti chn phng php quang ph hp th phn t UV-VIS vi thuc th bc dietylditiocacbamat (AgDDC) trong cloroform. Nguyn tc ca phng php ny l ton b lng asen c trong m s chuyn v asenat bng u dung dch KI hoc NaI, sau di tc dng ca dng hiro mi sinh do phn ng ca Zn vi axit HCl asenat b kh thnh asin (AsH 3 ). Kh asin to thnh i qua ng hp th cha bc dietylditiocacbamat trong dung d ch piridin (hoc cloroform) to thnh mt phc cht mu . 3.1. Lp dng phng php phn tch. xy dng phng php phn tch hm lng As trong nc chng ti tin hnh kho st mt s iu kin ti u nh chn th tch dung dch hp th AgDDC trong cloroform, chn thi gian phn ng to phc mu, s thay i cng mu ca phc theo thi gian,nh hng ca s c mt cc cht khc n s xc nh As nh S2-, Sb3+ v a ra phng php loi tr. kho st th tch dung dch hp th ti u, chng ti chn cc th tch l 4, 5, 6, 7, 8 ml, kt qu cho thy khi th tch dung dch hp th l 6 ml th mt quang ca
105

TP CH KHOA HC V CNG NGH, I HC NNG - S 4(33).2009

phc mu l ln nht. Qua vic tham kho ti liu [2,4,7] cho thy cng mu ca phc AsDDC gim dn theo thi gian, do chng ti tin hnh kho st tm thi gian phn ng ti u m mt quang l ln nht. Thi gian phn ng kho st ln lt l 20 pht, 25 ph, 30 ph, 40 ph, 50 ph v 60 ph. K qu kho st cho thy sau 30 pht kh asin t c hp th hon ton bi dung dch hp th v mt quang t gi tr cao nht. Cng mu ca phc AsDDC gim dn theo thi gian nn chng ti kho st s thay i mt quang theo thi gian v kt qu cho thy dung dch c bn mu trong khong 5 pht. Phn ng gia AsH 3 vi AgDDC b cn tr bi H 2 S v SbH 3 . H 2 S phn ng vi thuc th to thnh hp cht c mu tng t, SbH 3 cng c kh nng phn ng tng t nh AsH 3 to hp cht mu hng nht. Do vy chng ti tin hnh kho st nh hng ca s c mt S2- v Sb3+ n qu trnh xc nh asen v kt qu cho thy S2nh hng mnh n mt quang ca dung dch. loi tr H 2 S chng ti dng bng thy tinh tm Pb(CH 3 COO) 2 ri sy kh. Cn SbH 3 ch to mu hng nht khi hm lng ca Sb3+ cao hn 0.1mg/l m trong nc thng th nng Sb3+ ch lng vt nn khng cn phi loi tr. Nh vy qua kt qu kho st chng ti chn c iu kin ti u cho qu trnh phn tch hm lng As nh sau: Th tch dd hp th Thi gian to phc Thi gian n nh mu 6ml 30 pht 5 pht Loi tr S2Pb(CH 3 COO) 2

Da trn cc iu kin ti u chn chng ti xc nh gii hn nng pht hin As3+ l 0,002mg/l tc 10 -4 mg asen v khong nng tuyn tnh ca asen l 0.001-0.015mg. Trn c s cc iu kin ti u chn, chng ti tin hnh xc nh hiu sut thu hi v sai s thng k ca phng php trn 2 mu gi qua nm ln th nghim. Kt qu phn tch cho thy hiu sut thu hi ca phng php t 90.53%, sai s nh, chnh xc cao v h s bin ng nh, chng t lp li tt (bng 3.1)
Bng 3.1. Mt s gi tr nh gi sai s thng k ca phng php

Cc i lng c trng Phng sai S2 lch chun S H s bin ng C v (%) sai chun S x Bin gii tin cy Sai s tng i %
106

As3+ 0,08 ppm 3,48.10-7 5,89.10-4 0,81 2,63. 10-4

7,32.10-4 1,01

As3+ 0,12 ppm 8,48.10-7 9,21.10-4 0,85 4,12. 10-4

1,15.10-3 1,06

TP CH KHOA HC V CNG NGH, I HC NNG - S 4(33).2009

Ly 250ml mu nc x l s b C trn bp cch ct Cn li khong 50ml Thm: - 5ml HNO3 c - 2ml H2SO4 c - 0,5ml H2O2 3% C cn n bc khi trng Cn kh - ngui - Ha tan bng nc ct 2 ln - nh mc ln 50ml Dung dch phn tch Chuyn vo bnh phn ng. Thm vo 10ml HCl, 6ml KI 15%, 1ml SnCl2. yn 15

Dung dch phn ng Thm 5g Zn t. phn ng xy ra h trong 30 o mt quang phc mu

Hnh 3.1. Quy trnh phn tch mu nc b mt

Da trn kt qu kho st trn, chng ti xy dng quy trnh phn tch hm lng As trong nc b mt, s c trnh by trn hnh 3.1. 3.2. Kt qu phn tch mu nc thc t p dng quy trnh c xy dng trn, chng ti tin hnh xc nh hm lng asen trong m s mu nc b mt thuc a bn Thnh ph Nng trong t thng 5 v thng 6. Kt qu phn tch c th hin trong bng 3.2 v 3.3.
Bng 3.2. Nng asen trung bnh trong mt s mu nc thuc a bn Thnh ph Nng trong thng 5.

Ngy ly mu 02/05/2009 02/05/2009

a im ly mu Pha Bc H Bu Trm Pha Nam H Bu Trm

Nng asen (mg/l) 0.00426 0,00702

107

TP CH KHOA HC V CNG NGH, I HC NNG - S 4(33).2009

02/05/2009 05/05/2009 05/05/2009 07/05/2009 07/05/2009 07/05/2009 09/05/2009

H iu Tit (P. Thanh Kh Ty) H Thc Gin Vnh Trung H Cng Vin 29/3 H m Rong (ly mu gia h pha bn phi ngn dng) H m Rong (ly mu gia h pha bn tri ngn dng) H Xun H A H Xu TCVN 5942- 1995

Khng pht hin 0,00685 0,00325 0,00916 0,00856 0.00650 0.00270 0,05

Bng 3.3. Nng asen trung bnh trong mt s mu nc thuc a bn Thnh ph Nng trong thng 6.

Ngy ly mu 20/06/2009 20/06/2009 20/06/2009 22/06/2009 22/06/2009 24/06/2009 24/06/2009 25/06/2009 25/06/2009

a im ly mu Pha Bc H Bu Trm Pha Nam H Bu Trm H iu Tit (P. Thanh Kh Ty) H Thc Gin Vnh Trung H Cng Vin 29/3 H m Rong (ly mu gia h pha bn phi ngn dng) H m Rong (ly mu gia h pha bn tri ngn dng) H Xun H A H Xu TCVN 5942- 1995

Nng asen (mg/l) 0.00457 0,00744 Khng pht hin 0,00705 0,00402 0,00975 0,01230 0.00820 0.00380 0,05

Kt qu phn tch mu nc, cho thy: Asen c mt trong hu ht cc ngun nc mt trn a bn Thnh ph nng. Tuy nhin mc an ton vn nm trong gii hn cho php ca TCVN. H m Rong c hm lng asen kh cao nguyn nhn do ngoi chc nng iu tit ma, iu ha kh hu h cn tip nhn nc thi sinh hot ca khu vc dn c trn mt lu vc rng 205 hecta. H iu Tit Phng Thanh Kh Ty khng pht hin c s c mt ca asen. H ny chc nng chnh l iu tit ma, gp phn to cnh quan v iu ha kh hu cho khu vc dn c xung quanh.

108

TP CH KHOA HC V CNG NGH, I HC NNG - S 4(33).2009

4. Kt lun Kt qu nghin cu qu trnh xy dng phng php phn tch hm lng As trong nc b mt cho php a ra nhng kt lun sau: 1. Kho st c cc iu kin ti u cho quy trnh phn tch tng hm lng asen trong nc: th tch dung dch hp th (AgDDC trong CHCl 3 ) l 6ml, thi gian phn ng l 30 pht, cng mu ca phc bn trong 5 pht. 2. Xc nh c yu t nh hng n qu trnh xc nh asen l S2- v a ra phng php loi tr bng Pb(CH 3 COO) 2 . 3. Xc nh c gii hn pht hin nng asen bng phng php trc quang phn t UV-VIS l 0.002 mg/l v khong nng tuyn tnh ca As khi xc nh bng thuc th AgDDC l 0.001-0.015 mg. nh gi sai s thng k cho quy trnh phn tch cho thy c mc chnh xc ca phng php. 4. Nghin cu xy dng thnh cng quy trnh phn tch asen trong nc bng thuc th AgDDC trong CHCl 3. 5. p dng quy trnh xy dng phn tch m s mu n c tro ng cc h bu ln t , thuc a bn Thnh ph Nng nh gi mc nhim nc bi asen. Kt qu cho thy hm lng asen trong cc mu nc u nm trong gii hn cho php theo tiu chun mi trng ca Vit Nam. TI LIU THAM KHO [1] L Huy B, c hc mi trng, NXB i hc Quc gia TP. H Ch Minh (2000). [2] B Y t, Thng quy k thut nh lng asen trong thc phm, Ban hnh theo quy nh s 2129/ Q - BYT ngy 04/06/2002 ca B trng b y t (2002). [3] Trn Hng Cn, ng Kim Loan, Chu Th Thu Hin, Kim loi nng trong mi trng nc. Mt s kt qu phn tch v nh gi ti khu vc H Ni, Hi ngh khoa hc phn tch ha l v sinh hc Vit Nam ln th nht (2000). [4] T Vng Nghi, Hunh Vn Trung, Trn T Hiu, Phn tch nc, NXB Khoa hc v k thut H Ni (1986). [5] http://vietnamnet.vn/khoahoc/trongnuoc/2006/09/615483 [6] http://www.toquoc.gov.vn/Thongtin/O-Nhiem-Asen-Da-Co-Thuoc-Dac-Tri88306e7a9698481a83414fca68f432c7.html [7] Arnold E. Greenberg, R. Rhodes, Lenore S.Clescerl, Standard Methods for the Examination of Water and Wastewater, 16th Edition (1995).

109