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HOAN THEN QUY TRINH PHAN TICH MOT SO DAN XUAT PHENOL THUOC NHOM ANKYLPHENOL vA BISPHENOL A TRONG MAU NUOC RAC TAi c A c BAI RAC KHU v a c HA NOI IRAN THI Llfiu, HOANG TUE MINH, BUI THU H A , P H A M HUNG VIET Trung tdm Nghien aim Cong nghe Moi trudng vd Phdt trien ben vitng, Trudng Dai hoc KHTN, DHQGHN Tom tat Mot so cac dan xuat phenol thudc hg ankylphenol nhu nonylphenol, octylphenol va bisphenol dugc ling dung rdng rai cdng nghiep, sinh boat va cd kha nang gay rdi loan tuyen ndi tiet dd'i vdi ddng vat hiiu sinh ciing nhu ngudi Cac ankylphenol, san pham thoai bie'n ciia ankylphenoletoxylat cd tinh doe va tich luy ben mdi trudng cung nhu xam nhap vao chudi thiic an Viec nghien ciiu, danh gia va quan trac cac hgp cha't cac hgp ph^n khac cua mdi trudng tai Viet Nam da budc dau dugc quan tam vai nam gSn day Va'n de d nhilm mdi trudng tai cac khu vuc xung quanh bai chdn la'p rac, nha't la cac bai rac thai sinh boat tir cac thi Idn nhu Ha Ndi gay khdng it nhiing birc xiic dd'i vdi cac nha quan ly va anh hudng nguy hai tdi siic khoe cua ngudi dan khu vuc va cdng ddng Chung tdi da tie'n hanh khao sat, hoan thien quy trinh phan tich cac ankylphenol va bisphenol miu nude rac (trudc va sau xtr ly) va ap dung de xac dinh ham lugng cac hgp cha't mot so mlu nude va nude rac thu thap tai bai rac Nam San, Tay Md Hieu sua't thu hdi ciia cac hgp chat phan tich la 4-nonylphenoI (4-NP), 4-tertoetylphenol (4-t-OP) va 4-n-octylphenol (4-n-OP) va bisphenol A 813 (BPA) deu dat tir 84,4- 91,4% Ket qua phan tich cho thay, ham lugng cac ankylphenol va BPA cac mSu tai khu vuc bai rac Tay Md cao ban so vdi khu vuc bai rac Nam San Cac NP va nha't la BPA deu cd mat vdi ham lugng kha cao cac mSu nude rac Ham lugng sau xir ly cua BPA dugc tdi 3913,0 ng/L va cua NP dugc 2026,0 ng/1 Mac du, ham lugng NP va BPA sau xic ly tai bai rac Nam Son deu thap ban so vdi bai rac Tay Md he thd'ng xir ly tuang dd'i hien dai va thdi gian di vao boat ddng chua lau, nhung cac gia tri ham lugng deu cao ban tieu chuan ve gia tri ham lugng khdng gay bat ky anh hudng vdi ddng vat thuy sinh ciia Chau Au Cd the ndi bai rac la ngudn d nhiem tiem tang cac ankylphenol va bisphenol A tdi moi trudng va nguy ea de dga su:c khde ngudi Chiing tdi hi vgng se c6 nhiing nghien cu:u sau rdng ban de ddng gdp vao viec quan trac, danh gia su ton luu, phan bd va van chuyen ciia cac bcTp chat ankylphenol va bisphenol A mdi trudng OPTIMIZATION OF ANALYTICAL PROCEDURE FOR SOME DERIVATIVE PHENOLS AMONG ALKYLPHENOL AND BISPHENOL A FROM LANDFILL LEACHATES SAMPLES IN HANOI'S DUMPING SITES Pham Hung Viet, Tran Thi Lieu, Hoang Tue Minh Research Centre for Environmental Technology and Sustainable Development (CETASD), Hanoi University of Science, VNU Abstract Some derivative phenols of alkylphenol group as nonylphenol, octylphenol and bisphenol A are widely applied in industry, domestic activities and cause disrupting endocrine system for wildlife and human The alkylphenols, degradation products of alkylphenolethoxylates, are toxic, persistent in the environment and potential penetration into food chain Recently, studying and monitoring of these compounds in different environmental components in Vietnam have been concerned remarkably The environmental pollution problems around the dumping sites, specially industrial and municipal ones like Hanoi, caused difficulties for the local authorities and hazardous risks for health of wildlife and human We carried out studying and completing the analytical procedure for some derivative phenols of alkylphenol group and bisphenol A in groundwater, landfill waste water samples (pre-treated and treated) 814 ana appiiea mat to samples laKen in Nam Son and Tay Mo landfill areas, Hanoi The recovery values of 4-nonylphenol (4-NP), 4-tertoctylphenol (4-t-OP), 4-n-octylphenol (4-n-OP) and bisphenol A (BPA) were ranged from 84.4 to 91.4% According to the researched results, the concentrations of target alkylphenols and bisphenol A in Tay Mo samples is higher than that in Nam Son The concentrations of nonylphenol and bisphenol A are significantly high in leachates samples, with concentrations of treated ones were 3913ng/l and 2026ng/l for BPA and NP, respectively Although, the concentrations of target alkylphenols and bisphenol A in leachates samples at Nam Son (modern waste water treatment system and short time operation) is lower comparision to that one at Tay Mo but these values are higher the European values of Predicted Non-Effect Concentration for water environment It is seemed that dumpingsites are potential pollution sources of alkylphenols and bisphenol A for the environment, health of wildlife and human We hope that we will have further researches about these compounds, contribute to assessing and monitoring its accumulation, spatial distribution as well as its fate in the environment Gidi thieu Su tha'm Igc cac cha't gay d nhilm tir cac ngudn chii ye'u nhu bai chdn la'p rac cd the dan tdi su nhiem ban cua mdi trudng nude, bao gdm ca ngudn cung ca'p nude udng Qua trinh phan tich cac chat d nhiem hiiu ca nhu ankylphenol hay bisphenol A nude rac gap rat nhieu khd khan, trd ngai Nen mfiu rat phiic tap, bao gdm ham lugng cao cua cac axit humic va fulvic cung nhu cac mud'i ciia chiing, gay can trd den viec phat hien hay lam giam kha nang thu hdi ciia cac chat phan tich [1,2] Ngoai ra, cac hgp chat quan tam thi cd mat cac mlu vdi ham lugng ra't khac nhau, tao thach thiic Idn cho viec tim mot phuang phap cd the xac dinh mot khoang ndng mlu rdng Vi vay, viec chiet tach, lam sach mau rdi lira chgn phuang phap xac dinh dugc dat nghien ciiu Ky thuat chie't pha ran ket hgp vdi dan xuat hoa, xac dinh tren thiet bi sac ky khi-khdi phd dua lai hieu sua't thu hdi cao, tiet kiem dung mdi da dugc lua chgn de phan tich cac ankylphenol va bisphenol A mau nude rac 815 Cot chie't pha rdn vdi chat ha'p phu Cuj dugc lua chgn d^ tach chi^t cac hap cha't phan tich khdi nen mau cho hieu qua cao [3] Tac nhan dan xua't boa anhydrit axetic de kiem, re tien dugc dung cho phan ling dan xua't axetyl hoa cac dan xuat phenol Muc dich ciia nghien ciiu la khao sat quy trinh phan tich ddng thdi mot so ankylphenol va bisphenol A mau nude rac va nude ng&n bi d nhiem xung quanh ling dung ky thuat chie't pha ran, ke't hgp vdi ky thuat dan xuat hoa Phuong phap loai bd dugc nhiing anh hudng cua nen mSu va hieu qua viec xac dinh lugng ve't mdi trudng Thi/c nghiem Nghien ciiu bao gdm phan: khao sat va hoan thien quy trinh phan tich cac ankylphenol va bisphenol A mau nude rac, va ap dung quy trinh khao sat dugc vao xac dinh cac ankylphenol va bisphenol A mot so mlu nude rac (trudc va sau xir ly) va mSu nude mat tai khu vuc bai rac Nam San va Tay Md Thu thap mau mau nude rac va nude ngam quanh khu vuc bai rac Tay M6 va Nam San dugc thu thap vao cac chai thuy tinh 4L sam mau va dugc Igc qua giay Igc thuy tinh (GF/F, Whatman, Anh) Dich Igc dugc axit hoa vdi HCl 4M ve pH de ngan can su phan buy ciia cac vi sinh vat va dugc bao quan tai 4"C cho de'n chie't phan tich Hoa chat Cac chat chuan ankylphenol (4-t-octylphenol, 4-nonylphenol, 4-noctylphenol) va bisphenol A, dung dich chat ndi chuan naphtlen-dS va chat ddng hanh bisphenol A-dl4 (surrogate) dugc dat tii Chem Service Dung dich chuan gdc ndng lOOOmg/L ciia mdi cha't dugc chuan bi dung mdi axeton va dugc pha loang diing lam ch^t chuan them vao va lap dudng chu^n Anhydrit axetic, axit HCl dac, loai tinh khie't phan tich cua hang Merck dugc sir dung lam tac nhan axit boa va dan xua't hoa Cac dung mdi diclometan, hexan, axeton va metanol loai tinh khie't phan tich ciia Merck 816 iNuoc cat z lan ouge igc qua thie't bi khuf ion hoa Millipore (Nhat Ban) Chat ha'p phu florisil (90-100 mesh) sieu tinh khiet ciia Supelco va Na2S04 khan dang tinh khiet phan tich ciia Merck dugc nung Id qua dem tai 450°C Sir dung cot chiet pha ran vdi chat ha'p phu RP-18 500mg cua hang Merck Thiet bj Thie't bi chie't pha ran cua hang Supelco Viec xac dinh tren thie't bi dugc thuc hien tren thiet bi sdc ky khikhdi phd GC/M8-QP2010 cua hang Shimadzu Thie't bi dugc chay d che khdng chia ddng va nhiet cdng bam mSu dugc dua tdi 280°C The tich bam la 2|LI1 Cot mao quan DB5, dai 30m, dudng kinh 0,25mm, day lap phim 0,25fim Chuang trinh nhiet ciia may: nhiet ban dau 50°C giu phut Tang de'n lOO^C vdi tdc 20>hut Tie'p tue tang nhiet len 20"C vdi tdc 10°C/phut Cudi cung tang nhiet len 280°C vdi tdc 20°C/phut, giii phut Cac cha't nghien ciru dugc dinh tinh dua vao cac manh phd khdi ciia cac dan xuat axetyl boa tuang ling xac dinh trdn thiet bi phd khdi Sir dinh lugng cac chat theo phuang phap ndi chuan, vdi cha't ndi chu^n naphtalen-d8 Hoan thien quy trinh phan tich Dich Igc ciia mSu dugc chiet bdi ky thuat chiet pha ran vdi cot SPE RP-18, da dugc rira lan lugt ciing vdi 20ml n-hexan, 20ml DCM, 20ml MeOH va 10ml nude cat khii ion Cho 200ml dich Igc miu di qua cot SPE vdi tdc lOml/phiit Cac chat can tach chie't dugc rira giai vdi 20ml MeOH Dua them lOjul chat surrogate BPA-dl4 vao dich rira giai dugc de lam chat ddng hanh, tinh gia tri hieu suat thu hdi Dich rira giai dugc cd ca't quay chan khdng va cd bang nita tdi gan khd, rdi hoa tan lai 1ml hdn hgp DCM/hexan (l:3,v/v) Dung pipet Paster dua qua cot sac ky dugc nhdi 5g cha't ha'p phu florisil (da 817 boat hoa 12 gid tai 130"C) d^ tie'n hanh budc lam sach Thuc hiSn cdc phan doan rira giai vdi lin lugt cac hdn hgp dung mdi sau: 20ml hexan/DCM (l:3,v/v), 20ml hexan/DCM (2:3.v/v), lOOml 5% MeOH/DCM Phan doan chiia cac hgp cha't ankylphenol va bisphenol A quan tam Cd ca't quay chan khdng dich rura giai phan doan thu thap v6 1ml Chuyen vao Ig nhd sdc ky 1,5ml Cd bang nito ve gSn khd Thuc hien phan ling dan xuat axetyl boa bang each cho them 50^1 pyrol va 50|al anhydrit axetic vao Ig sac ky Lac manh Ig, de yen tai nhiet phdng qua dem de phan ling dan xuat boa xay hoan toan Cho 0,5ml hexan vao Ig nhd, lac manh va ly tam (tdc 1000 vdng/phiit) Tach lay Idp n-hexan Thuc hien cho trinh them 0,5ml hexan them lan niia Ldp hexan thu thap dugc lam khan qua Na2S04 Cd dac ldp hexan ve the tich
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