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    14 views9 pages

    Hóa Phân Tích - Luận Văn, Đồ Án, Đề Tài Tốt Nghiệp

    Uploaded by

    Thuan Van Le
    hi hehehehe

    Copyright:

    © All Rights Reserved
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    of 9
    IV. CAC CHAT CHi TH] TRONG CHUAN DQ COMPLEXON: Dé xc dinh diém dimg trong chudn d6 complexon, thudng sit dung mét sé loai chit chi thi sau day: * Cac chat chi thj mau kim loai (cdn goi 1a chat chi thi complexon, hay chat chi thi kim loai) 1a nhimg hgp chat hitu co tao duge vai ion kim loai phit 6 mau dc trung, khéc voi miu eta chat chi thi. Diém dimg duge xéc dinh dya vao sy déi mau cia phite chat cia chi thi kim loai sang mau cia chi thi hode nguge lai ‘Trong chuan 46 complexon loai chi thj nay 14 quan trong nhat, vi vay ta sé xét chi tiét & duéi day. * Cac chit chi thi li thuéc thir dic trung rigng cia kim loai: Ching han ion SCN’ a chi thj cia phép chudn 46 Fe’* bing EDTA vi Fe” tao phite véi SCN phite ¢6 mau 46 méu: Fe’ SCN FeSCN* - Chi thi duge cho vao tir ban dau nén dung dich truéc khi chudn dé cé mau hong. Qué trinh chudn d6 xay ra true hét 1d: Fe + 0 HhY™ Fey + 2H Cho dén khi xay ra phan img canh tranh: FeSCN + HY? Fey + SCN + 2H Nhu vay sé mat mau ctia phic, ta dimg chudn d6 Didu kign dé cé thé sit dung logi chi thj nay 1d hing sé bén diéu kign cla phite chat gitta kim loai voi EDTA phai lon hon so voi hing s6 bén cia phitc chat kimlogi véi chi thi, Tuy nhign hong chi thi cho vio phai vita phai. * Cée chit chi thi hujnh quang c6 kha ning tao phite véi kim logi vi do dé miu hoe cudng 9 huynh quang cia cht chi thi bj thay d4i, Vi dy, fluorexon trong dung dich kiém ‘manh duge dung lam chi thj dé chudn 49 cdc kim loai kiém thé (Ca”’, Sr’”, Ba’) bing EDTA: tai diém twong duong huynh quang bj tit do cdc kim logi 43 chuyén hoan toan thanh phite véi EDTA. * Cac chit chi thi oxi héa — khir duge ding khi kim loai chudn d6 tén tai duge 6 2 dang oxi héa va khit, Duéi day ta sé xét ky phan chi thj kim loai: 1. Phan loai chi thi (Céc chit chi thi kim loai thug diing thudc céc loai sau day: a. Céc thude nhugm triphenylmetan: vi du pirocatesin tim, xilen da cam, metalphtalein, thimolphtalein, Phitc kim logi — chi thi cé mau dé. b. Cac thude nhugm azo, vi du Eiocrom den T (ErioT hay E100), 4-(2-piriddinazo)-2- naphton (PAN), asenazo I ¢. Céc chat chi thj thuge logi khic: vi dy murexit, alizarin S, 2. Diéu kign 44i véi chi thi trong chudn 46 complexon: - Cé dé nhay cao dé cé thé quan sit sy di mau khi néng d6 chit chi thi bé (co 10° 10%) va do 46 phan kim logi lién két trong phite v6i chat chi thj 1 khéng ding ké va c6 thé jén khi tinh sai s6 chudn 46. khéng can ~ Phite kim logi— chi thi Min phai cé 46 bén trong pham vi xée dinh: phite Min phai tuong 44i bén, nhung phai kém bén hon phite kim loai — EDTA thi sy chuyén mau méi 13. ‘Thubng chon chi thi sao cho: 10° < fre < Baw - Phan ing tao phite gitta ion kim logi va chét chi thi phai nhanh va thun nghich 3. Co ché tée dung cia chi thi kim loai: it la BrioT) duge viét dang don Gia sit ta cé chi thi théng dung li Eriocrom den T (vié ‘idm la HpIn. Trong dung dich chi thi xdy ra qué trinh: Hl H+ Hin w+ In TO < pH < u Maudé mau xanh ‘miu da cam Trong dung dich truée Khi chuin d6 ta cho mt lwgng vita dit chi thi vao dung dich chifa ion kim logi (vi du chuan d3 Mg’) thi dung dich s& cé mat : Mg” va phite cita Mg” véi thi. Hau hét kim loai déu tao vi ErioT phic mau dé man, nhw vay dung dich khi chua chudn d6 cd mau dé man, Mg’ += In* Mgin’ Batein (46 man) (Qué trinh chun d6 xdy ra trade hét I: Mg + HY MgY* + 2H” Brey Sau khi ton bé Mg” da tao phite véi HY” thi xay ra phan img canh tranh: Mgin + HY? Mgy* + 2H! + In’ Nhu vay tai diém cudi chudn d6 chi thj sé tén tai trang thai khéng tao phic, trang thai nay sé 06 dang HpIn’, HIn® hay In mang mau sic khdc nhau tiy thuge vio pH cia dung dich. Gia sir phép chuin 46 Mg” bing EDTA & pH = 10 thi diém cudi chudn d6 chi thi tin tai 6 dang Hin? nén né cé mau xanh. 4, Sy chuyén mau va d6 nhay cua céc chat chi thj kim loai: 5.M6t sé chi thj kim loai théng dung: Ngay nay, ngudi ta da ting hgp duge hang chuc thudc thir hitu co lam chat chi thi mau kim loai trong chudin dé complexon. Sau day lamét sé chi thi quan trong nhat duge dung chi thj rat nhigu nén rong rai trong cdc phong thi nghigm Héa phan tich. Vi sé Iugng cdc chat tinh phd bién cia cdc phuong phip chudn 46 complexon ngay cing duge mé réng, ngudi ta néi phong phdp chudn d6 complexon 1a hat nhan cia phn tich thé tich hign dai. a, Briocrrom den T D6 1a mudi natri ca axit (J-oxi-2-naphtylazo)-6-nitro-2-naphtol-4-sunfonic, Céng thite cu tgo cita chat chi thj 1a: Vhfuigdhif’ hme -00 1a chat chi thj c6 mau khéc nhau phu thugc vio pH cia dung dich hda tan n6. Chat chi thj 18 mudi ciia da axit Hsln, NaHyIn = Nav + Hil Hain’ H+ Hin pk, =63 Hin? H + In’ pK, =11,5 Nhu vay dung dich chi thi s® 6 mau cia pH. Cu thé nw saw pH <7 chi thi tén tai dang Hyln' cé mau dé. pH > 11 chi thi t6n tai dang In* cé mau dam cam. 7< pH < 11 chi thi tn tai dang HIn™ c6 mau xanh. 2T-00 tgo phite vi nhiéu ion kim logi nhu: Mg”, Ca”, Zn’*, Cd, Hg”, AI*, Ga”. da sé céc phite c6 ty 18 1:1 va c6 miu dé min (hodc tim). ET-00 thuéng durge ding dét chuén 46 tryc tiép cdc ion trén trogn méi truéng c6 pH = 10 ( thuéng ding hén hop dém amoni). Ngoai ra né con duge ding lim chat chi thi dé dinh phan gidn ic ion kim loai khdc nh Ni’’, Pb** bang phuong phao chudn 46 nguge voi mudi Zn”* (pH = 10), chuin 46 Ca” & pH = 10 bing cach them phite Mg” vao. b. Murexit Murexit 18 mudi amoni cia axit pupuric CsHsQ,Ns.. Ctet Anion Hyln’ eta Murexit tén tai trong dung dich axit manh: NHdHIn Ni H4In- H+ + HB. pKI=9,2 H3In2- H+ + H2In-——pk2= 10,9 Hai néc axit c6n Iai v6 cing bé xem nhur khong phan i Mau céc dang cua cht chi thi phu thudc vio pH. pH <9 chi thi tn tai dang H4ln- c6 mau ds tim, pH > 11 chi thj tn tai dang H2In3-cé mau xanh tim. 9< pH <11 chi thj tén tai dang H3In2- 06 mau tim, Murexit c6 kha ning tao phite véi cdc ion kim loai sau: véi Ca”* khi pH = 12 phite miu dd; Cu?” va Ni?” khi 7 < pH <9 phite cé mau vang; véi ion Ag+ trong dung dich 4ém NH3 véi 10 10,4 chi thj e6 mau dé nhat. v. CAC PHUONG PHAP CHUAN BQ COMPLEXON: 1. Chuan 46 true tigp Day 1A phwong phdp chudn 6 don gian nhdt. Trong phuong phdp nay nguéi ta diéu chinh pH thich hgp cla dung dich chuin d6 bing mot hé dém va sau dé thém dung dich chudn tir buret, thuéng 1a complexon IIL, vio dung dich chudn 46 cho dén khi i mau ciia chat chi thi tir miu ciia phite kim logi véi chi thi sang mau cita chat chi thi 6 trang thai khng tao phtc. Phép chin d6 tryc tiép doi héi mét sé yéu cau sau: ~ Phite M-Y phai bén (B > 1077). - Toc dé phan img tao phite phai nhanh, - C6 kha ning xéc dinhj durge diém twong duong tite 1a chon durge chi thi thich hop cho phép chun 9. Dé ngdn ngtta su tao phute hidroxo kim logi & pH chudn 49 ngudi ta thudmg ding cdc hé dém ma sy c6 mit cila cdc chit trong hé dém dé khéng hode c6 sy tao phite nhung rit yéu véi ion kim loai Sai sé trong chuan 46 truc tigp duge dinh gid theo phuong trinh: { 1) cc Wud safe +C,) st ll Bw aaa 7 1) ole +[[ade+ leur] Néng 6 ion kim loai khéng bj chun 49 (M]* tai diém cudi chudn 4§ duge tinh theo phnrong trinh: 1 [var] vay Uinl* é phép chudn d6 cé thé dat téi 46 chinh xée cao nhdt nén chon chi thi c6 Ig A "9, [y+ cang gin véi pM* tai diém tuong duong ang tét 2. Chun 46 nguge Trong truéng hop khéng thé chudn 46 true tigp duoc, vi du khéng thé c6 chit chi thi thich hgp cho kim logi xéc dinh, hoc khi phan img gitta ion kim loi véi EDTA xay ra qui chim, hodc & pH chudn dé kim loai bj két tia duéi dang hidroxit kim loai, thi phdi sir dung phwong phép chudn 46 nguge. Trong truong hop nay ngudi ta thém vio dung dich EDTA ly dur va thi kign (nhigt 46, pH) dé ion kim loai M, n chudn mét Iugng chinh xéc lip xéc dinh phin tmg hoan toan v6i EDTA. Sau d6 chudn dé lugng du EDTA bing mt dung dich chudn ion kim loai Mz lay tir buret cho dén khi d6i mau ciia chat chi thj tr mau cia dang chi thi khéng tg0 phi sang mau cita phire chi thi véi ion kim loai Mz. ¥ Tir phép chudn d9 ta c6: sM1=SEDTA-SM2 (s lA sxcee) Néu kim loai M; tao phite chim véi EDTA thi phéi dun néng dung dich truée khi chudn d§ hoe phai di cho phan img xay ra hoan toan. Néu ion kim logi bj két tia & nhiing gi ti pH thich hop cho vige chudn d6 thi phai thém dir dung dich EDTA vao dung dich cdnn chudn 43 duge axit héa, sau dé méi dua pH cia dung dich dén gid tri thich hgp cho phép chun 46 ngwoc bing mét hé dém thich hgp. ‘Vi du Cr(JI]), Co(I) tao phite khé bén v6i EDTA nhung téc d6 phan img rat chim ngay ca khi dun néng, vi vay khéng thé chudn dé tryc tiép duge. Trong trudng hop nay phai thém EDTA dur, dun si 2 — 15 phit (tity theo anion c6 mat trong dung dich) dé phan img hoan toan, réi chudn 43 EDTA du bing dung dich kim loai chudn Fe, Ni, Cu hoic Mn & pH thich hop. ‘Trong truéng hgp khi phan tmg tao phite M, ~ EDTA xay ra khong chim thi phdi chon kim logi chuin dé nguge M; sao cho hing sé bén diéu kign cla phitc M;-EDTA (B’M2Y) bé ‘hon hang s6 bén diéu kién cia phirc M, EDTA (B”M1Y) nhung khéng duge bé hon 10’ BI(v Trong thye t&, ngudi ta thuéng chon Mg dé chudn 46 nguge vi phn 1én céc kim loai tg0 v6i EDTA phite bén hon phitc Mg — EDTA. Mat khéc Eriocrom den T 1a chat chi thj t6t di voi Mg. kim logi M tgo phirc bén voi EDTA ca trong méi trudng axit thi cé thé dung céc kim loai nhu Cu, Zn, Ni dé chuén 49 nguoc. 3. Chuan dé thé Khi khéng thé chudn d6 tryc tiép kim loai M, bing EDTA thi cé thé thay thé M, bing mot hong tuong durong ki loai Mz cép thé chun d6 tre tiép bing EDTA. Muén vay, nguéi ta cho m6t lrgng dir dung dich complexonat M; (MY) vio dung dich chuén d6 va sau khi phan img trao déi: Djvfiivi209/11 xay ra thi chudn d M; du bing EDTA. Dé phan img trao doi (s6) xay ra hoan tdan thi phai chon phirc MyY sao cho hang sé bén diéu kign B’M2Y<

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