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Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

XC NH HM LNG KIM LOI NNG TRONG THC PHM TNG QUAN Kim loi nng l nhng kim lai c khi lng ring ln hn 5g/cm3. Mt s kim loi nng c th cn thit cho sinh vt, chng c xem l nguyn t vi lng. Mt s khng cn thit cho s sng, khi i vo c th sinh vt c th khng gy c hi g. Kim loi nng gy c hi vi mi trng v c th sinh vt khi hm lng ca chng vt qu tiu chun cho php. X hi cng pht trin, vn nhim mi trng cng t ln hng u, nhim mi trng t nhiu ngun khc nhau y l mi nguy c e da s sng ca mun loi. Qu trnh th ha nhanh, cng nghip ha, hin i ha cc nc pht trin l nguy c gy nhim kim loi nng cho nc, t v khng kh. S nhim c bi cc kim loi nng nh Zn, Cd, Pb, Cugy ra nhng bnh m v nguy hi i vi con ngi v ng vt. Cc kim loi ny c hp th vo c th qua lng thc - thc phm, nc ung cng c th qua bt a, chi. Lng thc thc phm b nhim kim loi nng th cc kim loi ny s thc y qu trnh h hng thc phm, lm gim gi tr dinh dng cng nh gi tr cm quan ca thc phm. Thc phm c th b nhim cc kim loi nng t nhiu ngun khc nhau: Nguyn liu dng ch bin thc phm, trong qu trnh ch bin, bo qun thc phm, qu trnh chuyn ch thc phm.. Trong thi i ngy nay vic s dng ho cht a vo sn xut kh ph bin nn nguy c nhim cc kim loi nng vo thc phm ngy cng tng do tnh trng ng c do cc kim loi nng ang gia tng. V vy vic tm ra Cc phng php xc nh hm lng kim loi nng c trong thc phm l vn cn quan tm hng u bo v sc kho v mi trng.

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

Phn I: C S L THUYT CA CC PHNG PHP XC NH MT S KIM LOI Cu, Zn, Pb, Cd I. Phng php trc quang Phng php phn tch o quang l phng php phn tch cng c da trn vic o nhng tn hiu bc x in t v tng tc ca bc x in t vi cht nghin cu. Phng php ny chuyn cc cht phn tch thnh nng lng nh sng suy ra lng cht cn phn tch. Nguyn tc ca phng php l da trn kh nng to phc mu ca cht phn tch vi mt thuc th no . o hp th quang ca phc mu ta s bit c nng cht phn tch. Phng php c u im l tin hnh nhanh, thun li. C nhy cao, chnh xc c ti 10-6mol/l. Tu thuc vo hm lng cht cn xc nh m c chnh xc t 0,2 ti 20%. 1.1. nh lut Lambe-Beer Khi chiu mt chm bc x n sc (cng bc x ban u l I0) i qua mt lp dung dch c b dy l v c nng l C, th sau khi i qua dung dch cng bc x b gim i (cng ca bc i ra khi dung dch l I) do qu trnh hp th, phn x, tn x... hp th quang ca dung dch t l thun vi C v l. A = lg
I I0 = .l.C I

% truyn qua: T = I . 100 (%) A = lgT 0 Trong : A : hp th : h s hp th mol (lit.mol-1.cm-1). c trng cho kh nng hp th nh sng ca dung dch. Ph thuc vo bn cht dung dch v bc sng . l: b dy dung dch (cm) C: nng dung dch (mol/l) SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
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Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

1.2. Phng php trc quang (phng php ditizon) 1.2.1. Bn cht ca phng php ditizon. Ditizon ( Diphenyl thiocacbazon) c cng thc: NH NH C6H5 S=C N = N C6H5 Tan trong cacbon tetra clorua v clorform to thnh dung dch c mu xanh l cy. dng phn t tc l trong mi trng acid hoc trung tnh. Ditizon rt kh tan trong nc. Dung dch cng c phn ng kim th tan ca ditizon cng tng do to thnh ion Dz -. HDz Dz- + H+ Ditizon to vi ion nhiu kim loi nhng ditizon c mu, t tan trong nc nhng tan trong cacbon tetra clorua hay cloroform. Cc ditizon c th tn ti di hai dng, tu thuc vo acid ca mi trng. - Trong mi trng acid hay trung tnh th chng tn ti di dng xeton. - Trong mi trng kim chng tn ti di dng enol. NH N C6H5 N N - C6H5 S=C MI MI S C MI N = N - C6H5 N = N - C6H5 Dng enol thng t tan trong cacbon tetra clorua v cloroform. Cn bng chnh xy ra khi chit l: Mn+ + nHDz MDz + nH+ Ngoi ra cn phai k ti cn bng: H+ + Dz- = HDz pKA = 8,7 1.3. u nhc im ca phn tch trc quang a. u im - Cho php xc nh hm lng ca cc nguyn t c nng 10-2 10-6 mol/l vi gii hn pht hin c 0,1 0,01ppm.

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

- Vic thay i iu kin chit v cc thuc th, cc cht che cho php xc nh kh chn lc ion cn phn tch khi c mt c nhiu ion khc. b. Nhc im - Phng php i hi qu trnh tch chit, che ion cn tr.. phc tp do kt qu ph thuc nhiu vo kinh nghim v k nng ca ngi phn tch. 1.4. ng dng Hin nay phng php ditizon c dng rng ri xc nh cc c t kim loi trong lng thc thc phm. Phng php ny xc nh c lng nh kim loi t 0,1 ti 200 microgam (). II. Phng php nh lng bng quang ph hp th nguyn t (AAS) 2.1. Nguyn tc chung ca AAS Phng php AAS da trn nguyn tc tt c cc nguyn t khi trng thi nguyn t u c hp th bi mt bc sng nht nh, cng hp th th hin nng ca cc nguyn t c trong mu. Nu ta chiu mt chm tia sng c bc sng xc nh vo m hi nguyn t th cc nguyn t t do s hp th cc bc x c bc song ng ng vi nhng tia bc x m n c th pht ra c trong qu trnh pht x. Ph sinh ra trong qu trnh ny gi l ph hp th nguyn t. Phng php quang ph hp th nguyn t ha hi c p dng vi mt s nguyn t c kh nng nguyn t ha nh: Hg, As, Se, Zn Nguyn l ca phng php ny nh sau: Ngun sng n sc c pht t n Cathod rng ( HCl) hoc n phng in phi cc (EDL) hay n ph lin tc c bin in qua vng nguyn t ho n b cm bin ( detector) o cng bc x hay hp th. Mi kim loi c bc sng hp th c trng ring. n cathod rng (HCL) hay n phi cc (EDL) c cu to do chnh nguyn t c lm ngun pht bc x c trng. iu ny lm cho phng php n nh v t b nhiu. Cng bc x b hp th t l thun vi nng nguyn t c trong mu ( trong mt gii hn nng ). y chnh l c s phn tch nh lng. SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
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Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

Trong phn tch bng phng php ph hp thu nguyn t AAS ty thuc vo k thut nguyn t ha mu dng ngn la (F-AAS) hay khng ngn la (ETA-AAS) m nhy ca phng php s tng ln rt nhiu. K thut khng ngn la tuy ra i sau nhng c p dng rt hiu qu trong phn tch v nhy ca n cao hn. a. u im - C nhy v chn lc tng i cao. Gn 60 nguyn t ha hc c th c xc nh bng phng php ny vi nhy t 1.10-4 n 1.10-5 %. - Nu s dng k thut nguyn t ha khng ngn la th c th t n nhy n.10-7 % nn phng php phn tch ny c s dng rt rng ri trong nhiu lnh vc xc nh lng vt cc kim loi (phn tch cc nguyn t vi lng trong cc i tng mu y hc, sinh hc, nng nghip, kim tra cc ha cht c tinh khit cao). - Do c nhy cao nn trong nhiu trng hp khng phi lm giu nguyn t cn xc nh trc khi phn tch nn tn t nguyn liu mu, tn t thi gian, khng cn phi dng nhiu ha cht tinh khit cao khi lm giu mu, trnh c s nhim bn mu khi x l qua cc giai on phc tp. - Cc ng tc thc hin nh nhng. Cc kt qu phn tch li c th ghi li trn bng giy hay gin lu gi li sau ny. - Cng vi cc trang thit b hin nay ngi ta c th xc nh ng thi hay lin tip nhiu nguyn t trong mt mu. Cc kt qu phn tch li rt n nh, sai s nh (trong nhiu trng hp sai s khng qu 15% vi vng nng c 1 - 2 ppm). - Bng s ghp ni vi my tnh c nhn (PC) v cc phn mm c hp qu trnh o v x l kt qu s nhanh v d dng, lu li ng chun cho cc ln sau. b. Nhc im - H thng my o AAS tng i t tin. Do nhiu c s nh khng iu kin xy dng phng th nghim v mua sm my mc. - Do php o c nhy cao, cho nn s nhim bn rt c ngha i vi kt qu phn tch hm lng vt. V th mi trng khng kh phng th SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
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Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

nghim phi khng c bi. Cc dng c, ha cht dng trong php o phi c tinh khit cao - Cc trang thit b my mc kh tinh vi v phc tp. Do cn phi c k s c trnh cao bo dng v chm sc, cn cn b lm phn tch cng c thnh tho vn hnh my. Nhng yu t ny c th khc phc c qua cng tc chun b v o to cn b. - Nhc im chnh: ch cho ta bit thnh phn nguyn t ca cht trong mu phn tch m khng ch ra trng thi lin kt ca nguyn t trong mu. V th n ch l phng php phn tch thnh phn ha hc ca nguyn t m thi. i vi mt s nguyn t phng php hp th nguyn t c th xc nh n 0,1-0,005ppm. 2.2.ng dng Phng php ny c dng xc nh hm lng kim loi c trong cc mu qung, t, , nc khong, cc mu ca y hc, sinh hc, cc sn phm nng nghip, rau qu, thc phm, nc ung, cc nguyn t vi lng trong phn bn, trong thc n gia sc, v.v... Vi cc trang b v k thut hin nay, bng phng php phn tch ny ngi ta c th nh lng c hu ht cc kim loi (khong 65 nguyn t) v mt s kim n gii hn nng c ppm (micrgam) bng k thut FAAS, v n nng ppb (nanogam) bng k thut ETA-AAS vi sai s khng ln hn 15%. III. Phng php cc ph. Phng php Von Ampe l nhm cc phng php phn tch in ha da vo vic o dng ti in cc ch th theo th p vo, qua xc nh nng cht cn phn tch. Mt trong hai in cc c din tch b mt kh nh (b hn din tch b mt in cc kia kh nhiu ) nn rt d b phn cc v qu trnh kh hay oxi ha ca ion kim loi kho st xy ra trn chnh in cc ny. o cng dng in chy qua bnh in phn ng vi cc gi tr in th khc nhau t vo hai in cc, v I = f(E) ta s nhn c mt

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

ng cong gi l ng cong phn cc. Qua xc nh nng cht cn phn tch. Phng php Von Ampe c hai nhm chnh l phng php cc ph v phng php Von Ampe ha tan. y l nhng phng php s dng rng ri nht trong phn tch in ha. 3.1. Khi nim v phng php cc ph. Phng php cc ph cng l phng php in phn, nhng y vic xc nh nng thng qua vic nghin cu quan h gia in p t vo hai in cc (E) vi dng in (I) hnh thnh trong qu trnh phn cc. Phng php cc ph c th nh tnh v nh lng nhiu cht bng cch in phn dung dch phn tch trn in cc git thu ngn, ri sau v ng biu din Dng - Th ghi s bin i cng dng theo s bin i cng th in cc ca s thu phn. Trong phng php ny, ngi ta phn cc in cc git thy ngn bng mt in p mt chiu bin thin tuyn tnh vi thi gian nghin cu cc qu trnh kh cc ca cht phn tch trn in cc . V vy, thit b cc ph gm hai phn chnh l my cc ph v h in cc bao gm in cc git thu ngn v in cc so snh. ng cc ph biu din s ph thuc ca chiu cao cng dung vi nng cht phn tch. V nguyn tc ca phng php cc ph Phng php cc ph bao gm cc giai on: - t cc th khc nhau vo in cc kh cc ion khc nhau v mi ion c mt th kh tng ng xc nh, do qua th kh ca ion c th nh tnh c ion . - Nu tng dn th ca in cc nhng vo dung dch cht cn xc nh th cng dng s tng ln ng thi cho ti khi t c th kh ca ion trong dung dch. Trong iu kin nht nh, cng dng tng t l thun vi nng ion kh. Do s ph thuc gia cng dng v nng m nh lng c ion . S nguyn tc ca phng php cc ph SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
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Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

Tin hnh phn tch: Dung dch phn tch c np vo bnh nh phn c in cc thu ngn. Anot l lp thu ngn y bnh. Catt l git thu ngn ri lin tc t git m qun. t vo in cc th tng dn s to c dng c in cc tng dn, cng ny c iu chnh bng mt in k. Sau s thu c mt ng ph thuc Dng - Th (ng cong vn ampe) Dng khuych tn l dng c to do s kh ion trn in cc git thu ngn. Dng khuych tn c tnh theo cng thc Incovit: id = 605.Z.D1/2 .m2/3 . t1/6 Trong : id : cng dng khuych tn Z : ho tr ion b kh

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

D : h s khuych tn hoc s phn t gam ion kh khuych tn qua b mt 1 cm2 trong 1 n v thi gian cho gadian nng bng n v. C : nng ion kh miliion g/ lit. M : khi lng thu phn ri khi mao qun trong n v thi gian, tnh ra mg/giy. T : thi gian git thu phn ri khi mao qun, s. Trong thc t kh xc nh c h s khuych tn D, nn ngi ta o song song dung dch cht tiu chun v cht phn tch, ri thit lp ng cong vn ampe ca c hai dung dch v tnh nng (X) cht cn phn tch theo cng thc: x= h tc
a.hx

Trong : a: khi lng cht trong dung dch tiu chun. hx v htc : chiu cao sng ca dung dc phn tch v dung dch tiu chun. Phng php cc ph khng ch xc nh cc cation, n cn c th xc nh c cc anion v phn t c kh nng kh trn in cc git thu ngn. u im ca phng php: - nhy cao c th xc nh cc cht c nng 10-5 - 10-6 gam/lit. - C th ng thi xc nh nhiu cht khng cn tch bit chng. - Nhanh: ch tn vi pht xc nh nng cht trong dung dch. 3.2. ng dng: Trong phn tch thc phm phng php cc ph dng xc nh cc ion kim loi nng, mui n, ng fructoza, saccaroza, cc vitamin C, B1, xc nh c tnh nm men v vi c t cht hu c. 3.3. Phng php Von Ampe ha tan xung vi phn ( DDP) Qu trnh xc nh bng phng php Von ampe ha tan xung vi phn gm hai giai on: - Giai on 1: in phn lm giu kim loi trn b mt vi in cc mng thy ngn (catot): SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
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Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

M2+ + 2e = M (Pb, Cu, Zn, Cd) - Giai on 2: Ha tan kim loi kt t trn b mt in cc v ghi dng ha tan bng phng php Von ampe kt hp xung vi phn (DPP) di dng pic. L phng php ti u nht xc nh kim loi nng. Trong nhng iu kin thch hp cng dng ha tan t l thun vi lng kim loi kt ta trn b mt in cc tc l nng cht cn xc nh trong dung dch. Phng php ny c nhy, chn lc v lp li cao, thc hin nhanh v kh n gin . Trong phng php cc ph xung vi phn, in cc git thu ngn c phn cc bng mt in p mt chiu bin thin tuyn tnh vi tc chm ( 1 2 mV/s ) nhng vo cui mi chu k git ( git ri cng bc nh b g ), trn khung in p bin i mt chiu ngi ta t thm mt xung vung gc vi bin thay i trong khong 10 100 mV v di xung c 400 100 ms. Cng dng l hiu ca gi tr dng ghi 17ms trc khi np xung v 17ms sau khi ngt xung. a. u im Phng php ny l cho php xc nh hm lng vt cc ion kim loi nng, c, c nng rt thp. c bit vic s dng DDP kt hp vi Von ampe ha tan (ASV) c th xc nh nng cc ion trong khong 0,1 g/L. Phng php cc ph xung v von ampe ha tan c lp li cao, chnh xc v chn lc cao. Trong vic xc nh cc kim loi th phng php cc ph xung v von ampe ha tan vi AAS c tnh nng tng t nhau, nhng n c u vit hn l gi thnh r hn nhiu. b. Nhc im - S dng thy ngn c. - Nu dung dch phn tch cha cc tp cht hu c s gy nhiu m nguyn nhn l do cc tp cht tham gia phn ng in ha trn cc in cc. - Khng thch hp khi xc nh cc ion c th in cc rt m nh Na+, Ca2+, K+, Mg2+

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

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Xc nh Kim loi nng


E

GVHD: Th.s. Hong Vn Trung

Fei

Estep
Chu k git

tstep

Hnh 1. : Dng in p phn cc trong phng php DPP Fei : Bin xung Estep : Bc th mt xung in tstep : Thi gian np xung in
i ip = i1 i2

Hnh 2 : Dng tn hiu u ra ca phng php DPP

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

11

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

IV. Cc phng php x l mu thc phm phn tch kim loi trong thc phm C ba phng php x l chnh: Phng php v c ha kh Phng php v c ha t Phng php v c ha kh t kt hp 4.1. Phng php v c ha kh t kt hp a. Nguyn tc chung Nguyn tc ca k thut ny l mu c phn hy trong chn hay cc nung mu. Trc tin, ngi ta thc hin x l t s b trong cc, hay chn nung bng mt lng nh axit, v cht ph gia ph v s b cu trc ban u ca cc hp cht mu, v to iu kin gi mt s nguyn t c th bay hi khi nung. Sau em nung nhit thch hp. V th lng axit dng x l thng ch bng 1/4 hay 1/3 lng cn dng cho x l t.Nh th s tn t axit tinh khit cao. Sau em nung s nhanh hn v qu trnh x l s trit hn x l t v hn ch bt c s mt ca mt s kim loi khi nung. Do tn dng c u im ca hai k thut x l t v kh, nht l gim bt c cc ha cht tinh khit cao khi tro ha t, dung dch thu c l trong v sch hn tr ha t. b. Cc phng php v v d V l x l kh t kt hp l k tip nhau, trc tin x l s b, sau mi nung nn tnh cht v s din bin cng tng t nh k thut kh, k thut t. Ch c khc l sau khi x l mu khng phi ui lng axit d qu nhiu trong k thut t. V d 1: X l mu rau qu xc nh cc kim loi ( Na, K, Ca, Mg, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn.). Ly 5g mu v chn nung, thm 10ml HNO 3 65% v 5ml Mg(NO3)2, trn u ri sy kh hay un trn bp in cho mu si nh v n kh thnh than en. Sau em nung nhit , lc u 400 4500C trong 3 gi, sau 500 5300C, n khi ht than en c tro trng. SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
12

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

Sau ha tan tro tthu c trong 20ml dung dch HCl 1/1 un nng cho tan, lm bay ht axit d, n cn mui m, nh mc bng dung dch HCl 2 % thnh 25ml. y l dung dch xc nh cc nguyn t ni trn bng cc phng ph UV VIS, hay ph nguyn t ( AES, AAS). Quy trnh nh sau:

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

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Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

5g mu + 10ml HNO3 56% + 5ml Mg(NO3)2 5% Than en 400 - 4500C trong 3 gi Sau nung 500 - 5300C Tro trng + 20ml dung dch HCl 1/1, un nng Mui m nh mc bng dung dch HCl 2% thnh 25ml Dung dch phn tch

o bng AAS, AES, UV-VIS V d 2: X l mu tm, cua, c xc nh kim loi ( Na, K, Ca, Mg, Cd, Cu, Fe, Mn, Ni, Pb, Zn). Ly 5g mu vo chn thch anh, thm 15ml H2SO4 75% v 3ml Mg(NO3)2 5% trn u, x l t s b, sau sy hay un trn bp in cho mau si nh v un t t cho n kh v thnh than en. Sau SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
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Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

em nung 3 gi u nhit 400 4500C, sau nung nhit 5300C ch mu tro ha n c b khng cn en. Sau ha tan tro thu c trong 15ml HCl 1/1, un cho mu tan ht, lm bay hi ht axit d n cn mui m nh mc thnh 25ml bng HCl 2%. y l dung dch mu xc cc kim loi ni trn bng phng UV-VIS hay ph nguyn t AES, AAS. Quy trnh nh sau: 5g mu + 15ml H2SO4 75% v 3ml Mg(NO3)2 + ung hoc sy trn bp in Than en Nung 3 gi u 400 -4500C Sau nung 5300C Tro trng Ha tan trong 15ml HCl 1/1. un nong cho mu tan v ui ht axit d Mui m nh mc thnh 25ml HCl 2% Dung dch phn tch o trn ph UV-VIS hay ph (AAS, AES) c. u nhc im v phm vi s dng: Cc u im ca k thut ny l tn dng c cc u im ca k thut x l t v c x l kh, c th l: - Hn ch s mt mt ca mt s cht phn tch SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
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Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

- s tro ha l trit , sau khi ha tan tro s c dung dch mu trong . - Khng phi dng nhiu axit tinh khit cao - Thi gian x l nhanh hn tro ha t - Khng phi ui axit d lu, nn han ch s nhim bn do mi trng. - Ph hp cho nhiu loi mu khc nhau xc nh kim loi - Khng cn trang b phc tp n h l vi sng t tin Cch ny c s dng ch yu x l mu cho phn tch cc nguyn t kim loi v mt s anion v c nh: Cl- , Br- ,SO4 2-, Trong cc loi mu sinh hc, mu mi trng, mu hu c, mu v c. Khng dng c cho x l mu xc nh cc cht hu c. Trong phng th nghim bnh thng, khng trang b l vi sng th cch x l ny vn l mt phng php thch hp, n gin m vn m bo c kt qu tt. 2. Phng php kh - Dng c, ho cht Capxun dung tch 250 ml Pipet 100 ml Bnh nh mc dung tch 250 ml Cn k thut

Bp cch ct Giy lc Magie dioxyt (MgO2) Canxi acetat Ca(CH3COO)2

Phu Acid nitric c (d=1.4) Bp in, l nung iu chnh c nhit ( 600- 7000 C) - Tin hnh Dng pipet ly chnh xc 100 ml thc phm ( nu l sn phm lng) hoc ly cn 100 g thc phm ( nu l sn phm kh) cho vo capxun. Thm vo capxun 0,5g MgO2 v 0,5g Ca(CH3COO)2 tng tc v c ho v chng vic to thnh cc hp cht bay hi cha kim loi nng khi t ( v c ho). Cc cht ny nht thit khng c cha thic, ng v ch. t capxun trn bp cch ct, t cho thc phm chy hon ton thnh than. t capxun vo l nung, nung nhit 600- 7000C, n khi sn phm bin hon ton thnh tro xm, khong 3 gi. Ly capxun ra khi l nung, ngui, cho vo capxun 20 SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
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Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

ml acid nitric c ( tuyt i khng cha ng v ch) v 50 ml nc ct hai ln, nc trng cng chuyn vo bnh nh mc. Thm nc ct n vch mc, lc k. 3. Phng php t - Dng c, ho cht Capxun dung tch 250 ml Bp cch ct Pipet 100 ml Giy lc Bnh nh mc dung tch 250 ml Phu Cn k thut Bp in, l nung iu chnh c nhit ( 600- 7000 C) - Ho cht: Acid nitric c ( d = 1,4) Acid sunfuric c (d = 1,84) Amon axetat NH4(CH3COO)2 - Tin hnh Ly lng mu nh trn cho vo capxun. Thm vo capxun 3 ml acid nitric c v 50 ml acid sunfuric c. t capxun ln bp in, un si dung dch trong capxun. Tip tc un v c mi pht li nh thm 5- 20 git acid nitric c. Kh NO2 mu nu s thot ra (lm trong t ht hi). Nu thy dung dch trong capxun thm mu li th tng tc nh acid nitric c. Khi dung dch tr nn nht mu th gim tc nh acid nitric c, n khi dung dch khng mu th thi. Tip tc un cho khi trng bc i ht, ri li tip tc un si 10 pht na. Nu sau dung dch vn khng mu th vic v c ho hon ton xong. Nu dung dch en tr li th nh acid nitric. Ly capxun ra khi bp in. Cho vo capxun 0,20g amonaxetat, khuy cho tan ht. Chuyn ton b dung dch t capxun vo bnh nh mc dung tch 250 ml. Thm nc ct hai ln n vch mc, lc k. Nu dung dch capxun b c th phi lc trc khi chuyn vo bnh nh mc. Ghi ch: Phng php t kh ni trn xc nh ng v ch cng c tha nhn xc nh thic. MgO 2 tch ra oxy hot ng gip oxy ho nhanh cc cht hu c. Ca(CH3COO)2 ng vai tr ph v MgO2 lm tng oxy hot ng phng vo cht hu c, do lm tng tc t. Cng c th

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

17

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

dng Mg(CH3COO)2 v NaCl: Mg(CH3COO)2 v Ca(CH3COO)2; NH4Cl v NaCl, (NH4)2CO3 Song hn hp MgO2 v Ca(CH3COO)2 t l 1/1 lm cho tc t cht hu c nhanh nht. Nu t kh khng dng hn hp MgO2 v canxi axetat, th cc mui thic d bay hi v mt phn Sn nm di dng khng tan l acid metastanic. S mt thic trong t kh nh vy c th t 2,7 n 77%.

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

18

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

Phn III: Cc phng php xc nh mt s kim loi nng (Cu, Pb, Cd, Zn) I.Cc phng php xc nh Ch (Pb) Theo khuyn co ca t choc FAO/WHO th hm lng ch c th tip nhn qua ng thc n ti a hng ngy l 3.4 - 4g/kg c th. Tiu chun ti a cho php ca WHO nng ch trong nc ung khng vt qu 0.05 mg/l. xc nh Pb trong nc b mt, nc sinh hot thng dng phng php chit trc quang vi thuc th Dithizon l phng php cho php xc nh t 0,11,0 mg Pb/l. Pb l kim loi d xc nh bng phng php cc ph, phng php ny cho php xc nh Pb trong nc t 0,05mg n vi mg trong 1 lt nc. xc nh Pb trong nhng loi nc sch c hm lng nh hn 0,02 mg/l nn dng phng php phn tch in ho ho tan. 1.1. Phng php cc ph Ion Pb (II) l mt trong nhng ion c hot tnh cc ph b kh trn catot thu ngn thnh kim loi. Trong nn NaOH 1 M phc Pb(OH) 3 b kh thun nghch v cho sng cc ph vi th bn sng -0,76 V so vi cc calomen bo ho. Nu trong dung dch c cha Fe (III) vi hm lng khng ln lm, st s b kt ta hidroxit trong nn NaOH v khng gy tr ngi n s xc nh Pb. Nu hm lng st ln kt ta Fe(OH)3 s hp ph Pb, trong trng hp ny nn xc nh Pb bng phng php thm chun. Nu trong nc c lng tng i ln Cu (II) trong mi trng kim d, n cng b tan mt phn di dng CuO22- v sng ca ng cng nh hng n s xc nh Pb. Trong trng hp ny sau khi thm NaOH vo dung dch phn tch lng kt ta ri dng pipet ly ra 10 ml dung dch trn thm vo 0,5ml KCN 1M che ng. Lng xianua khng c d nhiu v s d nhiu s lm gim bc sng ca Pb. Tu thuc vo hm lng Pb m ta tin hnh nh sau:

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

19

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

+ Ly 25ml mu nc cho vo bnh nh mc dung tch 50ml nu cn pha long mu nc trong 25ml cha khong 0,13 mg Pb. Nu hm lng Pb trong mu ch nm trong khong 0,55 mg Pb/l th cn ly 250ml mu thm vo 1ml HNO3 c. + Lm bay hi trong bp cch thu n cn kh, ho tan b kh trong nc ct v chuyn ton b dung dch thu c vo bnh nh mc 50 ml. + Tip theo thm vo 5 ml NaOH, 1ml gielatin nh mc bng nc ct v lc u dung dch. Nu c kt ta hydroxit th cn lng v tin hnh ly phn dung dch trong v tin hnh ghi cc ph nhy thch hp t -0,4 -1,0 V so vi anot y thu ngn. + o chiu cao sng v da vo ng chun xc nh hm lng Pb. Nu hm lng mu c cha 0,051mg Pb/l th: Ly 250ml mu nc cho vo cc chu nhit thm vo 1ml HNO3 c v lm bay hi dung dch n kh. Thm vo b kh ngui 0,5ml HNO 3 c v c li ln na. Cho vo b kh ngui 5ml dung dch NaOH 10M +1ml gielatin + 44ml nc ct trn u (dung dch nn). Sau khi b kh ho tan ht tin hnh o ghi cc ph t -0,4 -1,0 V so vi y anot thu ngn. Da vo ng chun xc nh hm lng Pb. Nu mu cha lng ln cht hu c cn ph hu chng nh trong phng php dithizon trn. loi oxi khng dng Na2SO3 v ion Pb (II) s kt ta di dng PbSO4, c bit vi trng hp nng Pb ln. Cn dng khng kh tr nh N2 hoc H2 tinh khit cho chy qua dung dch trc khi ghi cc ph loi oxi. Dng gielatin loi tr cc i cc ph ca Pb. Phng php Vn-Ampe ho tan hp th (AdSV) vi thuc th 8hydroquinolin (pH= 7,88,5) Pb cho pic ti -0,54 V vi gii hn pht hin l 3.10-10M. Bng phng php Von-Ampe ho tan anot (ASV) trong nn m axetat (pH= 4,6) Pb cho pic ti -0,4 V vi gii hn pht hin ti 1.10-10M .

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

20

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

1.2. Phng php nh lng bng quang ph hp th nguyn t. Vi phng php F-AAS s dng ngn la l hn hp kh (khng khaxetilen) vi t l 5,2/1,25 L/ph (V/V) o ch bc sng = 217nm. Vi k thut ny t nhy 0,1g/ml, gii hn pht hin 0,02g/ml. C th dng thuc th APDC (amoni pyrolydin dithiocacbamat) trong MIBK (metyl isobutyl ketone) (mu c axit ho bng axit HCl n pH = 45). Vi phng php AAS khng dng ngn la th nguyn tc ca phng php l: mu c a vo l, ti y n c sy kh, tip n l tro ho v cui cng mui ca ch c phn ly di dng ch nguyn t, trong mi trng kh tr Argon. iu kin nguyn t ho l: sy nhit 120oC 200oC, trong thi gian l 30 giy; tro ho nhit 450 oC, trong thi gian 20 giy; nguyn t ho nhit 1900oC, trong thi gian 3 giy. Vng tuyn tnh l: 2 50 mg/ml. Vi k thut ny t nhy 0,05g/ml, gii hn pht hin 0,01g/ml. a. Thit b, dng c: - My quang ph hp th nguyn t c trang b n catt ch rng bc sng ci t l 283,3 nm, s dng ngn la axetilen khng kh vi chiu rng ca u t l 4 inch. - Chn s dung tch 50ml, su 5cm hoc cc thu tinh c m bng thch anh dung tch 100ml. - T sy nhit 1500C - L nung kim sot c nhit t 2500C 6000C vi sai lch khng qu 100C. - Dng c thu tinh c ra sch bng acid nitric nng 8N v trng li bng nc ct trc khi s dng. - Cn phn tch c chnh xc loi n 0,01g v loi n 0,001g. b. Ho cht v cht chun: - Dung dch HCl 1N : pha long 82ml dung dch HCl m c bng nc ct 1000ml. - Dung dch acid nitric 1N - Acid Percloric HClO4 m c 70,5% - Oxyt Lantan La2O3 SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
21

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

- Etylen dinitritetraaxetac EDTA - Dung dch m : Pha dung dch m nh sau: + Cho 163g EDTA vo trong bnh nh mc 2000ml, sau thm 200ml nc ct v mt lng va NH4OH ho tan ht EDTA. Thm 8 git ch th methyl da cam vo dung dch EDTA. + Cho 500ml nc ct vo mt cc thu tinh ri t t cho thm 60ml dung dch acid percloric m c, khuy u ri ngui. Sau , cho 50g acid lantan vo cc ri khuy u ho tan ht lng acid lantan ny. + Rt t t dung dch oxyt lantan vo dung dch EDTA pha trn, va rt va khuy mnh. Nu cn thit, thm NH4OH vo dung dch trn gi cho dung dch c tnh kim vi methyl da cam (dung dch c mu vng). - Dung dch ch chun: + Dung dch chun gc 1mg /l: ho tan 1,5985g nitrat ch chun trong khong 500ml dung dch acid nitric 1N. Sau nh mc thnh 1000ml bng dung dch HNO3 1N trong bnh nh mc. + Dung dch chun trung gian 10mg/ml: ly chnh xc 10ml dung dch chun gc cho vo bnh nh mc 1000ml, thm 82ml dung dch HCl 1N vo bnh. Sau nh mc ln bng nc ct. + Dung dch chun lm vic: Pha long dung dch chun trung gian thnh cc dung dch chun lm vic c hm lng ch ln lt l 0,1; 0,2; 0,6; 1; 3; 5 v 10mg Pb/ml bng dung dch HCl 1N trong cc bnh nh mc dung tch 50ml. c. Phng php tin hnh - Chun b mu trng Lm bay hi 4ml dung dch HNO3 m c trong chn s n kh trn bp cch thu. Ho tan cn bng 20ml dung dch HCl 1N v chuyn dung dch vo bnh nh mc 25ml. ngui bnh v nh mc ti vch bng HCl 1N. Yu cu hm lng ch trong mu trng khng c ln hn 10mg. - Chun b mu th

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

22

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

+ Cn khong 25g mu cho vo chn s ri sy kh trong t sy trong thi gian 2h nhit t 1350C 1500C. chuyn chn s vo l nung v tng dn nhit n 5000C. gi nhit l 5000C trong 16h tro ho mu. + Ly chn s ra ngui n nhit trong phng. Cho 2ml HNO 3 m c vo chn ri bay hi dung dch trong chn cho n kh trn bp cch thu. t ch s tr li vo l nung nhit thng, sau tng dn nhit n 5000C v gi nhit ny trong vng 1gi. + Ly chn ra ngui v lp li thao tc nh trn cho n khi tro c mu trng hon ton. + Cho 10ml dung dch acid clohydric nng 1N vo chn c tro ri ho tan tro bng cch nung nng. Chuyn gn dung dch vo bnh nh mc 25ml. + un nng phn tro cn li trong chn 2 ln, mi ln vi 5ml dung dch clohydric nng 1Mri rt dung dch vo bnh nh mc 25ml ni trn. ngui v nh mc ti vch bng acid clohydric nng 1N ri lc u. - Tin hnh phn tch: + Ti u ho cc iu kin lm vic ca my quang ph hp th nguyn t ti bc sng cng hng 283,3nm v t tc dng ca hn hp acetylen khng kh theo hng dn ca nh sn xut v iu kin lm vic chun vi ch. + Xy dng ng chun vi cc hm lng ca ch ln lt l 0,0; 0,2; 0,4; 1,0; 3,0; 5,0; v 10,0mg/ml da trn hp th ca chng. Trong trng hp tn hiu nhn c yu, phi iu chnh khuych i c hp th A ca dung dch chun (0,2mg/ml) khng nh hn 1%. + Khi ng chun c tuyn tnh tt, tin hnh o hp th ca dung dch mu th v mu trng c chun b nh sau: i vi dung dch mu th trong, khng c cn lng: Tin hnh xc nh hp th 3 ln theo cc bc sau: bm ln lt dung dch chun sau l dung dch mu th. nu s lng dung dch nhiu th th bm ln lt mt dung dch chun v 3 dung dch mu th cho n khi bm ht lng dung dch chun v mu th, mu trng. SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
23

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

i vi dung dch mu th c: thm 1ml dung dch m vo cc dung dch mu th, mu trng chun b trn v cc dung dch chun. Sau tin hnh xc nh hp th ca cc dung dch nh i vi dung dch mu th trong. + Tnh hm lng ch trong mu thng qua ng chun sau khi tr i mu trng. - Yu cu tin cy ca php phn tch. + hp th li ca bm 2 ln. + lch chun (CVs) tnh theo hp th ca hai ln bm lin tip ca cng mt dung dch chun phi nh hn 0,5%. + thu hi c xc nh bng cch s dng 5 mu cho vo mt lng dung dch ch chun bit chnh xc nng . thu hi tnh c phi nm trong khong t 85% - 115%, thu hi trung bnh ln hn 90%. d. Tnh kt qu Hm lng ch trong mu thu sn c tnh theo cng thc sau: + i vi dung dch mu th trong, khng c cn lng. CPb =
m Pb . 25 M Vd 25

+ i vi mu th c phi b xung thm dung dch m. CPb = mPb . V 1 . M d

Trong : CPb: hm lng ch c trong mu th (mg/g) mPb: hm lng ch c trong dung dch mu tnh c theo ng chun mg/mol. 25: th tch dung dch acid clohydric nng 1M dng ho tan mu (ml) Vd: th tch dung dch mu th b sung 1ml dung dch m phn tch (ml) M: khi lng mu th (g)

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

24

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

1.3. Phng php trc quang Pb (II) l cation kim loi c kh nng to phc vi nhiu thuc th hu c khc nhau. V vy c th p dng phng php trc quang xc nh Pb. Vic xc nh Pb bng phng php trc quang vi dithizon l phng php ph bin nht bi tnh u vit ca n. Dithizon Diphenylthiocacbazon l thuc th hu c c kh nng to phc cng cua vi hng lot ion kim loi, trong c ch. Phc ch ithizonat kh tan trong nc nhng d tan v tan nhiu trong cc dung mi hu c nh CHCl3 hoc CCl4. V vy, ngi ta thng dng phng php chit trc quang xc nh ch. Trong CCl4 th dithizonat c mu , cc i hp ph = 520nm. Ch dithizonat c chit chn lc v nh lng t dung dch nc c pH = 8 9 cha lng d xianua l cht dng che nhiu kim loi khc c th cng b chit vi ch. Trong mi trng k trn, cng b chit vi ch c c tali, bitmut v thic (II). Tali khng cn tr vic xc nh ch nhng thic v bitmut ngn cn nn cn c tch trc bng cch chit chng t mi trng axit. +Trong mi trng axit ch khng b chit, cn li trong pha nc. Thic v bitmut c tch trc nh sau: thm hidrazin vo dung dch mu nc, un nng kh Sn4+ xung Sn2+ v kh cc cht khc. + Sau khi ngui, thm dung dch natritactrat vo, a pH ca dung dch n 2,3 3 ( bng dung dch axit tactric). + Tin hnh chit nhiu ln, mi ln bng 5ml dung dch dithizon 0,1 % trong CHCl3. + Tin hnh chit cho n khi pha hu c vn gi nguyn mu xanh ca dithizon cho n khi pha hu c vn gi nguyn mu xanh ca dithizon. + Cui cng, lc pha nc vi ln vi CHCl 3 ( mi ln dng 5ml ) n khi pha khng cn mu xanh. Tin hnh chit nh vy khng nhng tch c thic m cn tch c c thy ngn, bc v ng. Nu nh trong mu nc cha lng ng k cc cht hu c cn phi v c ha chng bng cch chho vo vi ml HNO3 c v HClO4 c ri c SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
25

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

mu n kh, sau tm t b kh bng axit nitric v ha tan bng nc ct. cc cht oxi ha cn c kh trc bng hidrazin. Phng php ny cho php xc nh hm lng Pb n c 0,001mg/l. 1.4. Phng php Von Ampe ha tan xung vi phn Hin nay ngi ta s dng phng php Von Ampe ha tan kt hp xung vi phn (DPP) c th xc nh c 10-9M Pb2+ vi thi gian khng qu 3 pht. C th ni hin nay DDP l phng php cc ph hon chnh nht xc nh hm lng kim loi nng v phng php ny c nhy, chn lc cao v c tnh vn nng i vi hu ht cc i tng phn tch. II. Cc phng php xc nh Cadimium ( Cd ) Caimi v dung dch cc hp cht ca n l nhng cht cc c, thm ch vi nng rt thp chng s tch lu sinh hc trong c th cng nh trong cc h sinh thi. Cc hp cht cha caimi cng l cc hp cht gy ung th. Ngoi ra nhim c caimi cn gy nh hng n ni tit, mu, tim mchTheo tiu chun WHO quy nh, nng caimi cho nc ung 0,003 mg/l . Tu theo hm lng Cadimi trong mu v yu cu ca php phn tch m chng ta c cc phng php xc nh Cd ph hp khc nhau. Sau y l mt s phng php xc nh Cadimi. 2.1. Phng php trc quang xc nh Cd bng phng php trc quang dng dithizon, ngi ta chit bng CCl4 t mi trng kim mnh cha tactrat. Dung dch dithizonat ca dung dch Cd trong dung mi hu c c mu hp ph cc i bc sng = 515 nm. Cc cht cn tr c che bng CN - , NH2OH, tacrtrate. Nng pht hin nh nht 0,5 g trong th tch 1ml b dy cuvet 2cm. Phc dithizonate cadimi cho khong tun theo nh lut Beer n nng 0,4 g Cd/ml. Bng phng php ny c th xc nh hm lng t phn trm mg n miligam Cd.

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

26

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

Trong mi trng kim c mt s kim loi cng b chit cng cadimi nh bc, niken, coban, ng, loi tr cc nguyn t ny ngi ta chit chng trong mi trng axit trc khi xc nh cadimi. Hm lng Cadimi khong 0,01 0,5mg Cd/l c th dng phng php xc nh nh sau: + Nu nh mu phn tch c cha lng ln cht hu c th cn v c ho chng bng cch thm vo th tch nc ly phn tch 12ml H2SO4 c, 35 ml HNO3 c v lm bay hi dung dch trong t ht. + Nu dung dch cn c mu th li thm 5ml HNO3 c v li lm bay hi ln na, ng tc ny lp i lp li cho n khi thu c dung dch khng mu. Sau lm bay hi dung dch n kh thm tip vo b 1ml HCl c v lm bay hi ln na. Phn b sau khi ngui c ho tan bng nc ct 2 ln, un nng ho tan ht mui tan, lc qua phu lc kh bng giy lc v gi ly dung dch xc nh Cd. Trong mi trng kim mnh cc kim loi khc nh Ag, Cu, Ni,Co cng b chit cng vi Cd. Cc nguyn t ngn cn cn c chit trc khi xc nh Cd bng dithizon t mi trng axit. + Nu trong mu c CN- th cn ph hu xianua bng cch thm 0,5 ml H2SO4 c vo 100ml mu nc un si 10 pht trong t ht. Sau thm 0,2 ml HCl c khuy u v yn ( kt ta AgCl lng xung) trong 2 gi. Lc dung dch ra phu bng vi ml nc ct, trong nc lc cn c th cha mt lng nh Ag, Cu, Hg v mt lng nh Ag cn trong nc lc c c chit loi b bng dithizon t mi trng c pH= 2. Thm vo nc lc 5ml dung dch mui xaynhet 20% iu chnh pH n 2 bng cch khuy v thm t t dung dch NH3 hoc HCl. Cho mu vo phu chit v chit mi ln bng 5ml dithizon 0,1% trong CHCl3, chit cho n khi lng dithizon sau khi chit vn gi nguyn mu xanh ban u ca n. Sau ra mu bng 10 ml CHCl3 cho n khi dung mi ra khng mu. Cui cng ra thm 2 ln mi ln 5 ml CCl4. + Nu trong mu c cha Ni th tch bng dimetylglioxim nh sau: Ly 50 ml dung dch mu u hoc dung dch mu sau khi v c ho, cho vo 10 ml dung dch kalinatritactrat 20% (nu ly mu sau khi tch Ag, SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
27

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

Cu, Hg th ch cn thm 5 ml dung dch tactrat l ). Thm NH 3 vo cho n khi pH= 8,59, thm vo tip 5 ml dung dch dimetylglioxim 1% trong ru etylic 96%. Cho ton b hn hp vo phu chit lc u trong 30 giy. Chit phc niken dimetylglixionat vi ln, mi ln bng 10 ml CHCl 3. Cui cng ra tng nc bng 5 ml CCl4. Nu hm lng Zn gp 50 ln Cd th vic chit Cd khng hon ton v phm sai s m. Cc cht oxi ho cn c phn hu bng cch thm H2O2 vo v un si k. Cc cht hu c cn c chit tch bng 5 ml CCl4 mi ln chit. 2.2. Phng php AAS Vi phng php AAS s dng l nhit in, nguyn tc ca phng php l: Mu c a vo l, ti y n c sy kh, tip n l tro ho v cui cng mui ca cadimi c phn ly di dng cadimi nguyn t. S dng thuc th l APDC (amoni pyrolidin thiocacbonat) pH=9, mu c axit ho bng axit HNO3 (axit ho bng 100ml mu bng 1ml axit HNO3). Sau tim vo l 10g mu, loi dung mi 100oC trong 25 giy, tro ho 450oC trong 80 giy v nguyn t ho 1950oC trong 4 giy. o hp th ti bc sng = 228,8 nm. Da vo ng chun tnh kt qu. Trong trng hp ny hm lng Cadimi qu nh c th nng cao nng bng cch chit MIBK (metyl isobutyl ketone) vi thuc th APDC. + Vi phng php F-AAS s dng ngn la l hn hp khng khaxetylen vi t l 5,2/1,2 L/ph (V/V), cng dngthuc th APDC chit mu, mu cng c axit ho bng axit HNO3, thm vo dung dch axetat 40% pH= 34, thm 5ml thuc th APDC, yn trong 2 pht . Thm 10ml MIBK vo bnh lc mnh trong 30 giy, thm nc ct vo cho n khi dung mi hu c ln n vch ca bnh nh mc. Sau a mu vo ngn la ca my v phn tch mu. o hp th bc sng = 228,8 nm. V da vo ng chun tnh kt qu (mu chun c chun b trong MIBK). Phng php AAS c ng dng xc nh cadimi trong nhiu i tng khc nhau. bc sng 228,8nm th t nhy 0,01g/ml, gii hn SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
28

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

pht hin 0,004g/ml i vi k thut ngn la. i vi k thut khng ngn la th t nhy 0,008g/ml , gii hn pht hin 0,002g/ml. 2.3. Phng php cc ph Nu trong mu phn tch m hm lng Cd cao khong trn 1 mg/l th c th dng phng php cc ph xc nh. V Cd trong nn hn hp m ammoniac v nhiu nn khc cho cc sng cc ph thun nghch v nh lng. xc nh Cd bng phng php cc ph, ngi ta thng dng nn m ammoniac - amoniclorua (NH3 1M + NH4Cl 1M ). + Nu trong mu phn tch hm lng Cu khng ln hn hm lng Cd c th xc nh ng thi c 2 nguyn t v nn dng phng php thm chun. + Trong trng hp hm lng Cu qu ln so vi hm lng Cd th cn che Cu bng xianua. Cc kim loi khc nh Fe (III), Bi, Sn, Sb, s kt ta di dng hydroxit trong dung dch m. xc nh Cd ta ly phn dung dch trong trn. Nu hm lng kt ta qu ln cn xc nh theo phng php thm. Zn, Co, Ni, Mn l nhng kim loi trong nn ny cho sng cc ph nhng th m hn sng ca Cd nn khng nh hng n vic xc nh n. Nu trong nc c lng ln Pb th cn tch trc bng cch kt ta n bng axit Sunfuric long v lc b kt ta Ch sunfat. Tu theo hm lng ca Cd trong mu m chng ta thc hin pha long hay c cn bt sao cho trong 25 ml mu cha t 0,051,25 mg Cd. Thm mt git Metyl da cam v trung ho bng HCl hoc NH3 n khi cht ch th va i mu. Tip theo thm 10 ml dung dch nn, 1 ml gielatin, 1 ml m Natri sunfit v nh mc bng nc ct, lc u dung dch, cho dung dch vo bnh in phn v ghi cc ph t -0,4 V -0,8 V so vi anot y thu ngn. C th nh lng bng phng php thm chun hoc phng php ng chun. Nu mu cha 0,02 0,5 mg Cd/l th cn lm giu bng cch c nh sau: SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
29

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

+ Ly 250 ml mu, cho vo bt s hoc cc chu nhit, thm vo 1ml HCl c, lm bay hi n cn kh. + Thm vo phn b kh 5 ml dung dch c iu ch nh sau: Trn 10 ml dung dch nn + 1 ml gielatin + 1 ml Natrisunfit + 38 ml nc ct 2 ln. Cho ton b vo bnh in phn v ghi cc ph t - 0,4 V -0,8 V. Nn xc nh bng phng php thm chun. Ngy nay vi k thut tin tin nhiu phng php cc ph hin i c th xc nh Cd c nng 10-9 M trong cc nn khc nhau. c bit c th xc nh c ng thi ti 5 nguyn t cho chnh xc cao ( v d: Zn, Cd, Pb, Cu, Bi). Bng phng php Vn-Ampe ho tan hp ph (AdSV) s dng thuc th 5-hydroxy quinolin (8-HQ) trong nn m HEPES (pH= 7,8) Cd cho pic ti -0,69 V vi gii hn pht hin ti 1.10-10 M bng phng php Vn-Ampe ho tan anot (ASV), Cd trong nn m axetat pH= 4,6 V cho pic ti -0,59 V vi gii hn pht hin ti 1.10-10M. 2.4. Cc phng php in ha Cadimi c th xc nh bng phng php cc ph. Nguyn tc ca phng php ny da trn s kh ion Cd2+ trong mi trng axit, trung tnh hoc kim. Trong mt khong nng nht nh ca Cd2+ th cng dng khuch tn (hay chiu cao song cc ph) t l vi nng Cd2+ theo phng trnh Incovich: I= k.C Phng php in ha c s dng ph bin hin nay l phng php von ampe ha tan anot, l mt phng php xc nh cadimi c nhy cao. y l phng php va xc nh va lm giu cht phn tch. Trc tin cadimi c in phn lm giu ln in cc lm vic th khng i. Sau ha tan Cd bng cch phn cc ngc anot ri ghi li ng cong von ampe ha tan ca cadimi. Khi xc nh cadimi theo phng php cc ph nu trong mu nc hm lng Cu ln th cn che bng xianua.

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

30

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

III. Cc phng php xc nh ng (Cu). ng l nguyn t ha hc trong bng h thng tun hon c k hiu Cu v s nguyn t bng 29, thuc nhm IB. Lng ng trong nc ung thng thp ch vi g/l nhng ng nc v vt dng cha nc c mi hn bng ng c th lm tng nng ng. Nng ng trong nc ung c th tng ln n nhiu mn sau mt thi gian nc ng trong ng. ng l nguyn t c bn, lng ng a vo c th t thc phm vo khong 1-3 mg/ngy. Cc hp cht ca ng co c tinh khng cao so vi cac kim loai nng khac, cc mui ng gy tn thng ng tiu ha, gan, thn v nim mc. c nht l mui ng xuanua. Khi hm lng ng trong c th ngi l 10g/kg th trng gy t vong, liu lng 60 100 mg/kg gy nn ma. ng nh hng nghim trng n sc kho do thiu ht cng nh d tha. ng thit yu cho vic s dng st (Fe), bnh thiu mu do thiu ht st tr em i khi cng c kt hp vi s thiu ht ng. Vi c, khi hm lng ng l 0,002 mg/l c 50% c th nghim b cht. Vi khun lam khi hm lng ng l 0,01 mg/l lm chng cht. Vi thc vt khi hm lng ng l 0,1 mg/l gy c, khi hm lng ng l 0,17 0,20 mg/l gy c cho c ci ng, c chua, i mch. Vic tha ng cng gy ra nhng biu hin ng c m chng c th dn ti tnh trng cy cht. L do ca vic ny l do dng thuc dit nm, thuc tr su, khin cho cht liu ng b cn li trong t t nm ny qua nm khc, ngay c bn phn Sulfat Cu cng gy tc hi tng t. Nng gii hn cho php : Vi nc ung v nc mt: 0,02 1,5 mg/l tu theo tiu chun tng nc. Nc ti cy nng nghip: 0,2 mg/l ring vi t rt thiu ng c th dng nc cha ti 5 mg/l ti trong thi gian ngn.

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

31

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

3.1. Phng php trc quang s dng thuc th DDC. Ion Cu (II) to c phc vng cng vi DDC (ietyl dithiocacbamat), phc c mu nu, kh tan trong nc nhng tan nhiu trong mt s dung mi hu c nh clorofom. Trong dung mi ny phc c mu nu nh vng. Do nh lng ng bng thuc th ny ngi ta thng tin hnh chit trc quang. tng tnh chn lc ca phng php thng chit phc bng clorofom t mi trng cha ammoniac, amoni xitrat v complexon III l nhng cht dng che cc ion cn tr vic xc nh ng. Nu ng tn ti trong nc di dng phc bn xianua th trc khi phn tch cn phi ph hu phc bng cch lm bay hi mu nc sau khi thm vo 0,5 ml H2SO4 c v 5ml HNO3 c. Sau khi lm bay hi mu n kh, thm vo b 1 ml HCl c v lm bay hi ln na.Tip theo thm nc ct hai ln vo, lc v gi ly phn nc lc phn tch. Trong mi trng c cha ammoniac, xitrat, v complexon III a s cc kim loi khc khng gy cn tr cho php xc nh Cu bng phng php ny, ch c Bimut (Bi), bc (Ag), Hg vn phn ng vi DDC v c th b chit cng vi phc ca Cu. Tuy vy ch c phc ca Bi c mu vng l c nh hng cn phc ca Hg v Ag khng mu hp th nh sng trong min t ngoi, nn thc t khng nh hng n vic xc nh ng. xc nh Cu di dng phc CuDDC c th dng NaDDC lm thuc th hoc c th dng phc PbDDC v c th tin hnh chit trao i xc nh Cu. Phc ng bn hn phc ch nn y ch ra khi phc ca n v Cu c chit hon ton t tng nc sang tng hu c. CTCT ca NaDDC:

3.2 Phng php cc ph Cu (II) c hot tnh cc ph, trong nhiu nn khc nhau cho sng cc ph nh lng. Trong a s cc nn cc ph, sng ca ng nm trong khong th kh dng so vi kim loi khc, t 0 0,6 V. V vy xc nh Cu bng SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
32

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

phng php ny rt thun li v kh chn lc. Nn hn hp m ammoniac l mt trong nhng nn tt xc nh Cu. Trong nn ny cc ion kim loi b kh th m hn nh Cd(II), Co(II), Ni(II), Zn(II), Mn(II)khng gy nh hng n vic xc nh Cu. Oxi ho tan trong nc c kh bng cch thm vo lng d Natri sunfit Na2SO3. Cromat, Co(III), Tl(III) cng cho sng cc ph trong khong th c sng ng nn gy cn tr nu hm lng ca chng ng k. + Nu trong nc c hm lng ln Fe(III), Al(III), Bi, Mn l nhng kim loi kt ta hidroxit trong mi trng ammoniac, th kt ta c th hp ph mt phn ng, trong trng hp ny trnh sai s nn tin hnh nh lng ng bng phng php thm chun, khng nn dng phng php ng chun. + Nu trong nc c cha lng ng k l cht hu c th cn phi v c ho mu nh sau: thm vo th tch nc ly phn tch 1 2 ml axit H2SO4 c, 3 5 ml HNO 3 c v lm bay hi dung dch trong t ht cho n khi xut hin khi trng SO3. Nu dung dch thu c cn c mu th thm 5ml HNO3 c v lm bay hi ln na, ng tc ny c lp li cho n khi thu c dung dch khng mu. Sau lm bay hi dung dch n cn kh. Phn b sau khi ngui c ho tan trong nc ct hai ln, un nng ho tan ht cc mui tan, lc qua phu kh bng thu tinh xp v gi ly xc nh ng. loi tr cc i cc ph dng dung dch gielatin. + Nu mu cha t 2 50 mg Cu/l, th ly 25 ml dung dch mu cho vo bnh nh mc dung tch 50 ml. nu mu nc ch cha khong 0,2 3 ml Cu/l th ly 250 ml cho vo cc chu nhit sch, thm vo 1 ml HCl c v lm bay hi trn ni cch thu. Sau khi ngui tm t bng 1 ml HCl c, ho tan mui bng nc ct v chuyn ton b dung dch vo bnh nh mc 50 ml. Trung ho mu bng NH 3 n khi i mu metyl da cam, thm vo 10 ml dung dch nn, 1 ml gielatin, 1ml Na2SO3 nh mc bng nc ct hai ln v lc u. trng bnh in phn bng vi ml dung dch , mt phn dung dch trong bnh nh mc vo bnh in phn. Ghi cc ph t -0,2V n - 0,8V nhy thch hp. Sau da vo ng chun xc nh hm lng ng. SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
33

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

+ Nu mu c hm lng Cu trong khong 0,02 5ml Cu/ lit nc th ly 250 ml mu nc thm vo 1 ml axit HCl c, lm bay hi n kh, sau ngui thm vo 5ml HCl c na v li lm bay hi ln na n kh. Sau khi ngui thm vo 5 ml dung dch c ch nh sau: 10 ml dung dch nn c trn u vi 1 ml gielatin + 1 ml Na 2SO3 + 38 ml nc ct, dng a thu tinh nh khuy u cho mui trong cc tan ht. Chuyn ton b dung dch vo bnh in phn kh cha thu ngn kh v sch dng lm anot y. Ghi cc ph t -0,2 V n 0,8 V. Ri da vo ng chun tnh hm lng ca ng. Dng c, ho cht: - My cc ph LP.55.A - Dung dch nn (ho tan amon clorua vo 10ml dung dch amoniac c). - Gelatin dung dch 1%. - Dung dch ng tiu chun: (ho tan 3,9283g ng sunfit tinh th (CuSO4.5H2O) trong 1lt nc ct, 1ml dung dch ny cha 1mg ng, khi dng pha long 10 ln c 0,1mg ng trong 1ml. Tin hnh : Dng pipet ht 20ml nc lc loi I, thm 5ml dung dch nn vo mt cc, thm mt lng natri sunfit (Na2SO3)v 10 git gelatin dung dch 1% khuy k. Chuyn ton b vo bnh in phn, lm cc ph vi th 200 v t nhy in th 1/100 1/400 Sau , ly 20ml nc lc loi I, thm 10ml dung dch ng tiu chun, 4ml dung dch nn, mt lng natri sunfit v 10 git gelatin, lm cc ph nh trn. Tnh kt qu: Hm lng ng tnh thnh mg trn 1kg sn phm, tnh theo cng thc sau: x = ( H .V H V ).V .G 2 2 1 1 1 Trong : Cc: Nng dung dch tiu chun (0,1 mg/ml)
C c .Vv .H 1 .V1 .V0 .1000

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

34

Xc nh Kim loi nng Vc: H1: V1: V0: H2:

GVHD: Th.s. Hong Vn Trung

Th tch dung dch tiu chun thm vo, ml Chiu cao sng cc ph dung dch mu th, mm Th tch dung dch ly mu lm cc ph, ml Th tch ton b nc lc I, ml Chiu cao sng cc ph dung dch mu v ng tiu chun, mm V2: Th tch dung dch mu v tiu chun. G : Lng mu cn Hin nay c nhiu phng php cc ph hin i c th xc nh Cu c nng 10-9 M v c th xc nh trong nhiu nn khc nhau. Bng phng php Vn-Ampe ho tan hp ph, s dng thuc th catechol (pH = 7,8) Cu cho pc ti -0,2 V vi gii hn pht hin ti 1.10 -11 M. Vi thuc th 6-hydroxi quinolin (pH = 6 9) Cu cho pc ti -0,45 V vi gii hn pht hin l 2,4.10-10 M. Bng phng php Vn-Ampe ho tan trong nn m axetat (pH = 4,6) Cu cho pc ti - 0,0038V vi gii hn pht hin l 1.10-10 M. 3.3. Phng php Von ampe ho tan xung vi phn: Qu trnh xc nh bng phng php Von ampe ha tan xung vi phn gm hai giai on: - Giai on 1: in phn lm giu kim loi trn b mt vi in cc mng thy ngn (catot): Cu2+ + 2e = Cu - Giai on 2: Ha tan kim loi kt t trn b mt in cc v ghi dng ha tan bng phng php Von ampe kt hp xung vi phn (DPP) di dng pic. L phng php ti u nht xc nh kim loi nng. Trong nhng iu kin thch hp cng dng ha tan t l thun vi lng kim loi kt ta trn b mt in cc tc l nng cht cn xc nh trong dung dch. Phng php ny c nhy, chn lc v lp li cao, thc hin nhanh v kh n gin .

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

35

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

3.4. Phng php AAS Vi phng php F-AAS th s dng ngn la l hn hp khng khaxetilen vi t l 5,2/1,2 L/ph (V/V), o Cu bc sng = 324,76 nm. i vi k thut ny t nhy 0,03g/ml , gii hn pht hin 0,02g/ml. Vi phng php AAS khng dng ngn la, th mu c sy 120oC 200OC trong thi gian l 30 giy, tro ho nhit 450 oC 600oC trong thi gian l 20 giy, nguyn t ho nhit 2400 oC trong thi gian l 3 giy. i vi k thut khng ngn la th t nhy 0,0008g/ml , gii hn pht hin 0,015g/ml. Xc nh ng trong cc hp cht trn nn ca Fe ngi ta dng vic chit dng xalixialdocximat ng pH = 3, y ngi ta che Fe bng xitrat. S phun bi dch chit trong ngn la axetylen- oxi, xc nh bc sng = 324,7 nm v cho php xc nh n 0,5 g/ml Cu, cng pht x ca ng trong dung dch chit so vi s pht x trong dung dch nc tng ln 10 ln. lm dung mi ngi ta dng clorofom, hay amiaxetat. Xalixialdocximat ng ho tan tt trong clorofom nhng amiaxetat mc cao hn clorofom cho kh nng tng pht x quang ph. ng cng c chit di dng 8-oxiquinolat ng vi dung mi l MIBK pH ca dung dch chit l 3 5, = 324,8 nm c nhy tng 6 8 ln so vi trc quang trong dung dch nc, dng ngn la Hidro-Oxi. IV. Cc phng php xc nh Km (Zn) Km l nguyn t vi lng c tm thy trong nhiu loi thc phm v nc ung di hnh thc cc phc cht hu c. Cc mui km ha tan u c. Khi ng c km s cm thy ming c v kim loi, au bng, mch chm, co git... Ch n thng l ngun cung cp km chnh cho c th. Mc d lng km trong nc ngm thng khng vt qu 0,01 - 0,05 mg/l, nhng ring nc my c nng km cao hn nhiu o s ho tan km t ng dn nc. c tinh cua chung phu thuc vao pH, nhit va cng cua nc. - i vi cy trng: S d tha Zn gy c i vi cy trng khi Zn tch t trong t qu cao. D tha Zn cng gy ra bnh mt dip lc. S tch SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
36

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

t Zn trong cy qu nhiu gy mt s mi lin h n mc d lng Zn trong c th ngi v gp phn pht trin thm s tch t Zn trong mi trng m c bit l mi trng t. - i vi con ngi: Zn l dinh dng thit yu v n s gy ra cc chng bnh nu thiu ht cng nh d tha. Trong c th con ngi, Zn thng tch t ch yu trong gan, l b phn tch t chnh ca cc nguyn t vi lng trong c th, khong 2 g Zn c thn lc mi ngy. Zn cn c kh nng gy ung th t bin, gy ng c thn kinh, s nhy cm, s sinh sn, gy c n h min nhim. S thiu ht Zn trong c th gy ra cc triu chng nh bnh lit dng, teo tinh hon, m mu, vim da, bnh v gan v mt s triu chng khc. 4.1. Phng php trc quang Trong lng thc thc phm lng km thng rt nh nn c th xc nh c bng ditizon. Trong dung dch trung ha hoc kim yu (thch hp nht l pH= 8,3) v trong dung dch cha m xitrat Zn2+ tc dng vi ditizon to phc cht mu : Zn2++ 2H2O= Zn(HDz)2+ 2H+ Ch : phi loi b cc Ion ng, ch c trong dung dch trc khi xc nh km. Dng c, ha cht: Dng c: - Cn phn tch - Cc dung tch 250ml - Bnh ng mc dung tch 1000ml - Phu chit dung tch 100ml - Giy th PH - Buret 100ml - Amoniac dung dch 2N - Kali natri lactrat(KNaC4H4O6.4H2O) dung dch 20% - Ha tan 20g KNaC4H4O6.4H2O trong nc ct n thnh 100ml - Dung dch ditizon trong Cloroform 50 Lp 49K- Ha
37

Ha cht:

SVTH: Nguyn Th Hng Thy Trn Th Thy

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

- Natrisunfua (Na2S)trong dung dch bo ha. - Dung dch km tiu chun: cn ly 43,97mg km sunfua (ZnSO4.7H2O) tinh khit loi I Cho vo bnh nh mc dung tch 100ml, thm vo 10ml acid sunfuric dung dch 2N ri thm nc ct n vch mc, ly k 1ml dung dch ny cha 10 km. Tin hnh Ly 25ml dung dch v c ha( bng phng php kh hoc t). Cho vo phu chit . Trung ha bng amoniac dung dch 2N n PH= 7 vi giy trung ha PH. Cho vo phu chit 5ml dung dch ditizon, lc mnh phu 1-2 pht yn cho phn lp. Tch b lp di c phc ng ditizonat mu tm. Li thm ditizon, lc mnh cho ti khi khng cn mu tm phn ditizon. Trt phn ditizon vo mt cc, cho 3ml kali dung dch 20% chng kt ta hydro kim loi. Trung ha bng amoniac dung dch 2N. Chuyn ton b dung dch t cc vo phu chit, lc k dung dch s c lp mu ca km- ditizonat. Cho vo phu 10ml natrisunfua dung dch bo ha ( loi b ch v ditizon d), lc k , yn cho tch lp. Tch b lp di. Tip tc ra vi Na2S cho n khi li dui khng cn mu th thi. Chuyn dung dch km-ditizonat mu vo bnh nh mc dung tch 25ml, thm clorofom li vch mc, lc k. em dung dch dch mu ny , o mu trn my. Tnh kt qu: V d: tr s mt quang c c i vi 10ml dung dch km tiu chun l:
0,752 0,751 trung bnh 0,752 0,753

Tr s mt quang c c i vi 25ml dung dch mu l:


0,502 0,504 trung bnh 0,504 0,505

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

38

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

Ta bit trong 10ml dung dch km tiu chun cha 10.10 = 100(). vy lng km c trong 25ml l:
100.0.504 = 66,94 0.752

4.2. Phng php AAS Thc hin php o AAS i vi km bc sng 213,9 nm, nu dng k thut ngn la th t nhy 0,08g/ml, gii hn pht hin 0,04g/ml. Nu dng k thut khng ngn la th t nhy 0,07g/ml, gii hn pht hin 0,003 g/ml. 4.3. Phng php cc ph xc nh km bng phng php cc ph, ngi ta dng nn NH 3 1M + NH4Cl 1M . Trong nn ny th na sng ca km ng vi s trao i 2 electron l -1,35 V so vi cc Calomen bo ho. Phng php cc ph cho kh nng xc nh c km vi hm lng nh nht l 0,01 mg/l. Sai s ln nht khong 5 %. Nu trong mu nc cn cha ng thi ng, Cadimi v Niken vi hm lng xp x hm lng Km th dng nn ny ta c th xc nh c cc nguyn t , v sng ca chng trong trng hp ny hon ton tch khi nhau. Nu ghi cc ph t -0,2 V th cc sng thu c trn cc ph ln lt l Cu, Cd, Ni, Zn. Oxi ho tan trong dung dch c kh bng Natrisunfit. Nu cc nguyn t ng, Cadimi, Niken v Coban c trong nc vi hm lng ln hn hm lng ca Km nhiu th chng s cn tr vic xc nh Km v sng cc ph ca chng th dng hn sng Km. + Nu trong my cc ph c b phn chnh dng khuch tn ta s dng n b chnh dng cc ph ca cc kim loi cn tr . Khi hm lng ca chng khng qu cao th c th b chnh c v thu c sng ca Km khi ghi cc ph t -0,8 V. + Nu vic b chnh khng thc hin c, th cn tch Km ra khi mu bng phng php chit, gii chit Km li tng nc v xc nh n bng phng php cc ph. SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
39

Xc nh Kim loi nng

GVHD: Th.s. Hong Vn Trung

Trong trng hp khng cn phi tch Km th nn xc nh n bng phng php thm. Sau khi ghi cc ph dung dch cn phn tch, thm lng nh dung dch chun c nng thch hp vo dung dch phn tch v ghi cc ph ln na. lng Km c thm vo nh th no sng th hai c chiu cao gp ri hoc gp i ca chiu cao sng th nht. Cch tin hnh nh sau: Trong bnh nh mc dung tch 50 ml, thm vo 25ml mu nc hm lng ca km trong l 1 25 mg. + Nu trong mu c hm lng Km nh hn 0,15mg/l, th ly 250ml nc thm vo 1 ml HCl c v lm bay hi n cn kh hai ln nh nhau v ho tan b kh trong 25ml nc ct. Sau thm tip vo 5ml dung dch nn, 1ml gielatin, 1ml Na2SO3 v nh mc bng nc ct, lc u dung dch trong bnh, chuyn 25ml dung dch vo bnh in phn v ghi cc ph t -0,8 V n -1,5 V, nhy ca my sao cho sng thu c c chiu cao t nht 20 mm. Thm vo bnh in phn 0,2ml dung dch chun (loi no tu thuc vo nng Km trong dung dch mu) v ghi cc ph dung dch ny nhy c. Chn nng dung dch chun thm vo sao cho sng th hai c chiu cao gp ri hoc gp hai ln sng th nht. + Nu trong nc c ng, Cadimi, Niken vi hm lng hm lng cho php xc nh cng vi Km, th cng tin hnh nh trn v ghi cc ph t -0,2V n -1,5V. Vic xc nh cng c tin hnh theo phng php thm chun. + Nu hm lng ca cc nguyn t ngn cn qu ln th cn tch Km trc nh sau: ly mt th tch nc sao cho hm lng km trong t 0,010,5mg trong 50ml. Ly 50ml thm vo 2 git metyl v trung ho cn thn bng HCl long hoc bng NH3 long cho n khi cht ch th va i mu. Thm tip vo 20ml dung dch che. Chit km mt vi ln, mi ln bng 20ml dithizon, chit n khi ln chit cui mu xanh ca dithizon khng thay i. Gp tt c cc phn chit khc, thm vo 25ml HCl 1:5 v lc phu gii chit km tr li tng nc. Gi tng nc v lp li s gii chit hai ln na, mi ln 25ml HCl. Gp ton b dung dch nc thu c, lm bay hi trn bp cch thu n cn kh v ho tan b kh trong nc ct. SVTH: Nguyn Th Hng Thy Trn Th Thy Lp 49K- Ha
40

Xc nh Kim loi nng Tin hnh xc nh km nh trn.

GVHD: Th.s. Hong Vn Trung

4.4. Phng php Von ampe ha tan xung vi phn Thng ngi ta in phn lm giu dung dch cha Zn2+ in th -1,4V, sn phm in phn l km kim loi. Sau ha tan km trn b mt ca in cc lm vic, tn hiu phn tch thu c di dng pic. in th ng vi nh pic l c s ca php phn tch nh tnh cn chiu cao (cng dng ha tan ) hay din tch pic l c s ca php phn tch nh lng.

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

41

Xc nh Kim loi nng KT LUN

GVHD: Th.s. Hong Vn Trung

Trn y l mt s k thut v phng php xc nh mt s kim loi nng trong lng thc thc phm, trong t, ncTuy cha thc s y nhng qua gip chng ta c mt kin thc kh tng qut v cc phng php xc nh kim loi nng thng dng. Vic kim tra chnh xc hm lng kim loi nng c trong lng thc thc phm gip cn b lm cng tc thu mua c c s loi b nhng nguyn liu khng t yu cu, cn b Y T c th xc nh mt s nguyn nhn gy ng c thc phm i vi con ngi, cc cn b k thut c th kim tra cht lng thc phm ca mnh trc khi a ra tr trng. Hin nay c thm nhiu phng php mi xc nh kim loi nng, cn tm hiu c s ca cc phng php cng nh vic p dng cc loi my mc hin i phc v cho cng tc kim tra v phn tch cht lng. ng thi cn tm cc bin php ti u ha cc ha cht v thit b s dng c kt qu kim tra nhanh v chnh xc nht.

SVTH: Nguyn Th Hng Thy Trn Th Thy

Lp 49K- Ha

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