BO GIAO DUC VA DAO TAO DAI HOC QLOC GIA HA NOI TRirdNG D.\I HOC KHOA HOC TlTNHIEN LE THI \ INK NGHIEN ClfU ST; TAO PHLfC CUA SAT (EI) Y&L 1- (S - PYRIDYI.AZO)- - NAPHTHOL TRONG DUNG DICH mJOC VA KHA NANG IfNG DUNG VAO PHAN TiCH Chuyen nganh: Hoa phan tich Ma so: 01 04 03 LUAN AN THAC SI KHOA HOC HOA HOC Giao vien huong d§n: GS.TS Lam Ngoc Thu HANOI 11-1999 MUC LUC MCfDAU PHANI TONGQUAN 1.1 Tinh chat va cac iJng dung ciia sat 1.1.1 Mot sotinh chat quan ciia sk 1.1.2 Mot so ling dung cua sSt 1.2 Cac phuang phap tach va lam giau sat 1.2.1 Phuang phapchiet 1.2.2 Phuang phap ket tua 1.3 Cac phuang phap mau de' xac dinh sat 1.3.1 Mot so loai thuoc thu thuang duac sudung 1.3.1.1 Thuoc thu thioxyanal 1.3.1.2 Thuoc thu 0-Phenanlrolin 1.3.1.3 Thuoc thuaxit sunlosalixilic 1.3.1.4 Thuoc ihu Mccaplo axetal 1.3.1.5 Thuoc thu dipyridin - glioxal - dithioscmicabazon 1.3.1.6 Thuoc thu axetyl - pyridazin 1.3.1.7 Thuoc thu bato - phenantrolin 1.3.1.8 Thuoc thuformyl desoxybenzoin 1.3.1.9 Thuoc thu - metoxynitro sophenol 10 1.3.1.10 Thuoc thuetylen-chamin-bis-sunfosalisilic - andehit 10 1.3.1.1 Thuoc thu sufn- fcnyl - - piridin- ketoxim 10 1.3.2 Mot so loai thuoc thu moi 11 1.4 Thuoc thu PAN 16 PHANIl.KV THlATTHirc N(JHIEM 19 2.1 Hoa chat can thiet 19 2.1.1 Dicu chc dung dich chuan sdt (III) 19 2.1.2 Dicu chc dung dich chuiui PAN 19 2.3 Ky ihual chict 20 PHAN III NGHIEN CUD SI T.\0 PHUC GIUA SAl (III) - PAN 21 3.1 Khao sal su tao phuc cua sfit (111) vai PAN 21 3.1.1 Khao sat ph6 cua thuoc ihu va cua phuc 21 3.1.1.1 Khao sat hap thu cua thuoc thu 21 3.1.1.2 Khao sat hap thu cua phuc Fe(lll) - PAN 21 3.1.2 Khao sat anh huang pH den sir tao phiic 22 3.1.3 Khao sat anh huang cua thai gian den su tao phuc 24 3.1.4 Xac dinh phan cua phuc 25 3.1.4.1 Phuang phapdong phan tu gam 25 3.1.4.2 Phuang phap ty so'mol 27 3.1.5 Khao sat khoang tuan theo dinh luat Beer 28 3.2 Khao sat cac ion can 30 3.3 Xac dinh sat (111) mSu gia 31 3.3.1 Chuan bi mSu gia 32 3.3.2 Xac dinh sat (III) mSu gia bang phuang phap them 32 3.3.3 Xac dinh sat (111) mau gia bang phuang phap duang chualn 34 3.3.4 Chon phuang phap xac dinh 36 3.4 Khao sat kha nang chicl cua phii'c 36 3.5 Khao sat kha nang trao doi tren nhua anion cua phuc 37 3.6 Mot so ket luan ve phuc Fe(III) - PAN 38 PHAN IV.NGHIEN ClOJ SlJ DUNG PHlTC SAT (III) - PAN VAO MUC DICH PHAN TICH 39 4.1 Xac dinh vi luang sat bang phuang phap chiet trac quang 39 4.1.1 Khao sat ciia thuoc thu va phiic tuang huu ca 39 4.1.1.1 Khao sat ph6 hap thu ciia thuoc thu tuang huu ca 39 4.1.1.2 Khao sat ciia phuc tuang huu ca 40 4.1.2 Khao sat anh huang ciia pH den qua trinh chiet 41 4.1.3 Khao sat anh huang ciia dung moi den qua trlnh chiet 42 4.1.4 Xac dinh hieu suat chiet 45 4.1.5 Xay dung duang chuan 46 4.1.6 Xac dinh ham luang l-c(IIi) irong mau gia bang phuang phap chiet trac quang 48 4.2 Xac dinh ham luang sat nuac cat Ian bang phuang phap chiet trac quang 49 4.3 Xac dinh ham luong Fc(II) va Fe(lll) nuac ngam 50 4.3.1 Cach lay m^u va xir ly mau 50 4.3.2 Xac dinh ham luong Fc(III) mau 50 4.3.3 Xac dinh ham luami Fe(II) irons mfiu 51 3.1.1.1 Khao sat ph6 hap thu cua thuoc thir 21 3.1.1.2 Khao sat ph6 hap thu ciia phuc Fe(III) - PAN 21 3.1.2 Khao sat anh huang pH den su tao phuc 22 3.1.3 Khao sat anh huang cua thai gian den su tao phuc 24 3.1.4 Xac dinh phan cua phiic 25 3.1.4.1 Phuang phap d6ng phan tirgam 25 3.1.4.2 Phuang phap ty so'mol 27 3.1.5 Khao sat khoang tuan theo dinh luat Beer 28 3.2 Khao sat cac ion can 30 3.3 Xac djnh sat (III) mau gia 31 3.3.1 Chuan bi mau gia 32 3.3.2 Xac dinh sat (III) mau gia bang phuang phap them 32 3.3.3 Xac dinh sat (III) mau gia bang phuang phap duang chuan 34 3.3.4 Chon phuang phap xac dinh 36 3.4 Khao sat kha nang chiet ciia phiic 36 3.5 Khao sat kha nang trao doi tren nhua anion ciia phuc 37 3.6 Mot so ket luan ve phiic Fe(III) - PAN 38 PHAN IV.NGHIEN CUU SlfDUNG PHlfC SAT (III) - PAN VAO MUC DICH PHAN TICH 39 4.1 Xac dinh vi luang sat bang phuong phap chiet trac quang 39 4.1.1 Khao sat ciia thuoc thii* va phii'c tuang hiiu co 39 4.1.1.1 Khao sat ph6 hap thu ciia thuoc thii* tuang huu co 39 4.1.1.2 Khao sat ph6 ciia phiic tuang huu ca 40 4.1.2 Khao sat anh huang ciia pH den qua trinh chiet 41 4.1.3 Khao sat anh huang cua dung moi den qua trinh chiet 42 4.1.4 Xac dinh hieu suat chiet 45 4.1.5 Xay dung duang chuan 46 4.1.6 Xiic dinh ham luong IxMllI) mau gia bang phuang phap chiet trac quang 48 4.2 Xac dinh ham luang sat nuoc cat Ian bang phuang phap chiet trac quang 49 4.3 Xac dinh ham luong Fc(ll) va Fe(IlI) nuac ngam 50 4.3.1 Cach lay mau xa xir ly mau 50 4.3.2 Xac dinh ham luong Fc(lII) mau 50 4.3.3 Xac dinh ham lirang Fe(Il) irone miiu 51 PHAN V NGHIEN CCX CO CHE PHAN CSG TAO PHUC GIUA ION FEdlll-PAN XAC fi^HK,, 53 5.1-Xay dung phuong trinh xac dinh cache 53 5.1.1 Cac phuang trinh tao phuc h\drox cua ion Fe(III) 53 5.1.2 Can bang phan ly cua thuoc thu PAN (HR) 54 5.1.3 Phan ung giija Fe(III) \ai PAN 54 5.2 Xay dung duang bieu dien mat quang vao pH ciia dung dich 55 5.3 Xac dinh hang so khong h6n K^^ 58 KET LUAN CHUNG 59 TAI LifiUTHAM KHAO 60 Phan tieng Viet 60 Phan tieng Anh 61 MODfia Ngay nay, khoa hoc ky thuat phat trien manh me \'a ban than cac nguyen to vi lugng giu mot vai tro quan doi voi sir phat trien ciia dong thuc vat, viec thiia hoac thieu cac nguyen to vi luong deu khong co Igi cho doi song ciia chiing Sat la m 1 10 ' r , 11 , , , pH Hinh 14 Do thi bieu dien su phu thuoc - IgB vdo pH Bien liidn: Tren hinh 14 thi phu Ihugc - IgB = l"(pHj co duong tucmg ling voi i= 0; i= 1; i= Chi co duong i= la duong thang duong na\ ung vai Ig a = 1,93 ^ - q nen n = Ket qua thu dugc tren thi hinh 14 cho phep ket luan ion trung tam di vao phirc la Fe(III) va P.AN ihani gia \ao phirc ( dang R Phuc tao khong V bi hap phu tren anionit nhinig bi hap phu yeu tren cationit dien tich ducmg ciia sat o trung tam ciia phiic Fc(P.AN)^ Do dien tich dinmg cua phuc nen 57 cac phan tu nuac co kha nang tao lien ket hidro Khi chiet phuc bang cac dung moi khac cac phan tu dung moi se thay the cac phan tu nuac tao nen cac cua phuc cac dung moi khac co dang khac (hinh 7, 9, 10, 11) Tii cac du kien thu duac tren day, chiing toi de nghi cong thuc cau tao co kha nang nhat ciia phuc nhu duai day: 5.3 Xac djnh hang so khon^ ben K^^ Tix phuang trinh (9) a moi truang co pH bien doi tii 3,75 den 6,0 thi so ion H"^ bj ion kim loai thay the phan tu thuoc thu PAN trung hoa la (n=l) Chiing toi tinh duac hang so khong ben di^u kien ciia phuc Fe(PAN)2"'la: K,K=(1-6±0,2).10 ')'} D'\iu noi len rang phiic lao bai Fe(III) vai P.AN la phuc b6n 58 KET LUAN CHUNG Lan dau tien chiing toi nghien ciiu su tao phuc cua Fe(III) vai PAN dung djch nuac da thu duoc cac ket qua sau: Phuc Fe(lll) - PAN duoc hinh tot nhat khoang pH = 6,0 - 8,0 ben vai thai gian, co phan phuc Fe(III) PAN = - , X^,, = 565 nm, he so hap thu phan tu gam la 27.375, tuan theo dinh luat Beer mot gioi han rong Phuc bi chict dinh lugng bang cac dung moi huu ca Vi \ay, sii dung phuc Fe(III) - PAN de xac djnh vi luong sat Da nghien CLTU ca chc phan ung tao phuc cua Fe(III) vai PAN Fe(III) di vao phuc a dang Fc \ PAN tham gia vao phuc a dang PAN Phuc lao khong bi hap thu tren anionit nhung bi hap thu yeu tren cationit, co phd hap thu cac clung moi huu ca khac nhau, khac vc cue dai hap thu va cuang hap ihu Da de nghj cong thiic cau lao co kha nang nhat ciia phuc tao va tmh toan hang so khong ben ciia phii'c Phuc mau ciia Fe(Ill) \c')i PAN da dugc su dung de xac dinh ham lugng Fe(III) nu6c gieng khoan \'a nuac cat lan phong thf nghiem • Ham lugng Fe(IlI) nuac gieiig khoan la (0,63 ± 0,07) |.ig/ml • Ham lugng Fe(IIl) nuac cat lan la (2,79 ± 0,03) |_ig/ml/25 ml 59 TAI LIEU THAM KHAO Phan tieng viet l.Acmetop N.C "Hoa vo ca" Nha xuat ban Dai hoc - THCN Ha noi, tap IL trang 425 - 431, 1976 Babko A.K "Phan tich trdc quang" Nha xuat ban Dai hoc - THCN Ha noi, trang 216, 1974 Nguyen Xuan Ddng, Pham Luan " Sach tra ciiu pha che dung djch" Nha xuat ban KHTN irang 23, tap II, 1987 Glinka N.L Hoa hoc dai cuoniz" Nha xuat ban Mir ^ran^ 365 - 386, 1988 Nguyen Pham Hd "Luan van thac sT khoa hgc hoa hgc" trudng Dai hoc tu nhien Khoa hoa, chuyen nganh phan tich, ma sd 01.04.03 Ha Noi 1998 Tic Vpng Nghi, Iran Tii Hieu, Hiiynh Vdn Trung "Phan tich nuoc " Nha xuat ban Khoa hoc lu nhicn Ha Noi 1986 7.Sach G "Cac phuong phap phan tfch hoa ly" Nha xucit ban DH THCN 1974