I HC HU TRNG I HC KHOA HC KHOA VT L _B MN QUANG - QUANG PH

BI TIU LUN
TI: PHNG PHP O PH HP TH NGUYN T AAS Nhm thc hin: Nhm I

Hu, ngy 01 thng 12 nm 2011

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Tiu

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I. M U ................................................................................................. 2 II. C S L THUYT CA PHNG PHP AAS .......................... 3 2.1 Hin tng hp th nguyn t ...................................................... 3 2.2 PPPT AAS nh tnh v nh lng.............................................. 3 2.2.1 Phng php phn tch AAS nh tnh ............................... 3 2.2.2 Phng php phn tch AAS nh lng ............................ 4 2.3 u v nhc im ca phng php phn tch AAS ................. 6 III . K THUT THC NGHIM .......................................................... 7 3.1 Cu to, hot ng ca h o AAS ............................................... 7 3.2 Cch thc hin php phn tch AAS hon chnh ........................ 9 IV . V D P DNG PHNG PHP PHN TCH AAS ................ 11 V. NHN XT, NH GI PHNG PHP AAS ............................. 15 TI LIU THAM KHO ......................................................................... 16

I. M U

Phng php AAS c vit tt t phng php ph hp th nguyn t (Atomic Absorptional Spectroscopy). Phng php ph hp th nguyn t l mt trong nhng phng php tt nht xc nh cc nguyn t kim loi, vi nhy ln v chnh xc cao. Phng php da trn s hp th cc bc x c trng bi m hi nguyn t. Hin tng hp th nguyn t c ghi nhn u tin bi Wollaston v Praunhofh, c gii thch bi Bussen v Kirchhoff.

II. C S L THUYT CA PHNG PHP AAS

2.1 Hin tng hp th nguyn t:

+ Trong iu kin bnh thng nguyn t khng thu hay pht ra nng lng di dng bc x. Lc ny nguyn t tn ti trng thi c bn. Nu nguyn t nhn nng lng di dng nhit th nguyn t s chuyn ln trng thi c nng lng cao hn, gi l trng thi kch thch, trng thi kch thch ny khng bn, ch khong 10-8 10-9 s, sau nguyn t c xu hng tr v trng thi c mc nng lung thp hn, khi ny nguyn t s gii phng nng lng di dng bc x in t c bc sng khc nhau nm trong di ph quang hc. + Trong trng hp c bit, khi nguyn t tn ti trng thi hi t do nu ta chiu mt tia sng c nhng bc sng xc nh vo m hi nguyn t , th cc nguyn t s hp th cc bc x c bc sng nht nh ng vi nhng tia bc x m n c th pht ra. Lc ny nguyn t nhn nng lng ca cc tia bc x chiu vo n v n chuyn ln trng thi kch thch. + Qu trnh gi l qu trnh hp th nng lng ca nguyn t t do trng thi hi. + Ph sinh ra trong qu trnh ny gi l ph hp th nguyn t.

2.2 Phng php phn tch ph hp th nguyn t nh tnh v nh lng:

2.2.1 Phng php phn tch AAS nh tnh: + Do mi mt nguyn t hay mt tp hp cc nguyn t c du hiu ph ring bit, c quyt nh bi chnh bn thn cu trc v trng thi vt l ca chng nn cn c vo quang ph thu c chng ta c th on nhn khi qut v thnh phn cu to ca mu phn tch. + Da trn c s l cc nguyn t to ra trong b nguyn t ha mu hp th hay khng hp th tia cng hng pht ra t n catt rng lm bng mt nguyn t no nhn bit trong mu phn tch c hay khng nguyn t .

2.2.2 Phng php phn tch AAS nh lng: + xc nh nng (hm lng) ca mt nguyn t trong mu phn tch theo php o ph hp th nguyn t ngi ta thng thc hin theo cc phng php sau y: + Da theo phng trnh nh lng c bn ca php o ny qua vic o cng ca vch ph hp th ca nguyn t phn tch v xc nh (hay pht hin) nng ca cht phn tch trong mu o ph theo mt trong cc phng php chun ha sau: -Phng php ng chun. -Phng php thm tiu chun. * Phng php ng chun: Nguyn tc ca phng php ny l chn mt dy mu u (t nht l ba mu) xy dng nn mt ng chun, v sau nh ng chun ny v gi tr Ix xc nh nng Cx ca nguyn t cn phn tch trong mu o ph, ri t tnh c nng ca n trong mu phn tch. V d: ta chn dy mu u gm 5 mu C1, C2, C3, C4, C5, mu cn phn tch l Cx. Chn iu kin ph hp ri ta tin hnh o cng ph hp th c trng ca nguyn t trong mu ca mu u v mu cn phn tch, ta thu c I1, I2, I3, I4, I5 v Ix ( cng ph hp th c trng ca mu cn phn tch).

T th chun trn v t cng Ix ta i chiu v xc nh c nng Cx. Phng php ny n gin, d thc hin, c hiu sut cao trong vic phn tch hng lot mu cha cng mt i tng phn tch. Tuy nhin phng php ny c nhc im l khi mu phn tch c thnh phn phc tp v cha bit r ta khng th chun b chnh xc ba mu u c ng chun ng n. * phng php thm tiu chun: Nguyn tc ca phng php ny l ngi ta dng ngay mu phn tch lm nn chun b mt dy mu u, bng cch ly mt lng mu nht nh v gia thm vo nhng lng nht nh ca nguyn t cn xc nh theo tng bc nng (theo cp s cng). V d: Nng yu t cn phn tch l Cx=Co v lng thm vo l C1, C2, C3, C4, C5 ta c lot mu u c nng yu t cn phn tch l: Co = Cx C2 = Cx + C2 C4= Cx + C4 C1 = Cx + C1 C3 = Cx + C3 C5 = Cx + C5

Tip ta xc nh cng ph c trng ca mu u v dng ln ng chun I-C.

ng chun ny ct trc tung ti im (Io ,O). xc nh nng cha bit chng ta lm nh sau: Cch I: ko di ng chun v pha tri n ct trc honh ti im Cx , t ta c c Cx =|-Cx|. Cch II: t O v ng // vi ng chun, t Io k ng // trc honh, hai ng ct nhau ti M, t M h ng vung gc ct trc honh ti im Cx . Nh vy ta tm c gi tr Cx. Phng php thm tiu chun c nhng u im l: Qu trnh chun b mu d dng, khng cn nhiu ha cht tinh khit cao chun b dy mu u, Loi tr hon ton nh hng v thnh phn ca mu cng nh cu trc vt l ca cc cht to thnh mu.

2.3 u v nhc im ca phng php phn tch AAS:

* u im: Php o ph nguyn t c nhy v chn lc cao, tn t mu phn tch, thi gian phn tch nhanh. Cc ng tc thc hnh thc hin nh nhng, nhanh chng. Bng phng php ny ta c th xc nh ng thi hay lin tip nhiu nguyn t trong cng mt mu. Kt qu phn tch n nh, sai s nh. * Nhc im: Mun o ph hp th nguyn t cn phi c mt h thng my mc tng i t tin. Do cn c nhy cao nn s nhim bn c ngha ln i vi kt qu phn tch hm lng. Mi trng khng kh phng th nghim phi khng c bi. Cc dng c v ha cht dng trong php o phi c tinh khit cao. V c nhy cao nn cc trang b my mc l kh tinh vi v phc tp, do cn phi c k s lnh ngh bo dng v chm sc. Nhc im chnh l ch cho ta bit thnh phn nguyn t ca cht phn tch c trong mu phn tch, m khng ch ra c trng thi lin kt, cu trc ca nguyn t c trong mu.

III. K THUT THC NGHIM 3.1Cu to, hot ng ca h o ph hp th nguyn t: * Cu to ca h o ph hp th nguyn t:

Mun thc hin php o ph hp th th h o ph hp th nguyn t phi bao gm cc b phn chnh sau: + Ngun pht tia bc x cng hng ca nguyn t cn phn tch: Dng chiu vo mi trng hp th cha cc nguyn t t do ca nguyn t. l cc n catt rng (HCL), cc n phng in khng in cc (EDL), hay ngun pht bc x lin tc c bin iu. + H thng nguyn t ha mu phn tch: H thng ny c ch to theo hai loi k thut nguyn t ha mu. l k thut nguyn t ha bng ngn la v k thut nguyn t ha khng ngn la.

Trong k thut nguyn t ha bng ngn la, h thng ny bao gm: B phn dn mu vo bung aerosol ha v thc hin qu trnh aerosol ha mu (to th sol kh) v u t nguyn t ha mu, t chy hn hp kh c cha mu th huyn ph sol kh nh hnh sau:

Ngc li, khi nguyn t ha mu bng k thut khng ngn la, ngi ta thng dng mt l nung nh bng graphit (cuvet graphit) hay thuyn Tangtan (Ta) nguyn t ha mu nh ngun nng lng in c th thp (nh hn 12 V) nhng n c dng rt cao (50-800 A). + H thng my quang ph hp th hay l b n sc: B n sc, c nhim v lc, phn li v chn tia sng (vch ph) cn o, nh hng tia sng vo nhn quang in pht hin, bin i tn hiu quang thu c. + B phn bin i quang in: l b phn bin i tn hiu quang thnh tn hiu in, d khuch i v lu tr tn hiu. + B phn ghi nhn, x l tn hiu: B phn ny c th l cc trang b sau: n gin nht l mt in k ch nng lng hp th E ca vch ph; Mt my t ghi lc ca vch ph; B hin s digital; B my tnh v my in; Vi cc my hin i cn c thm mt microcomputer v h thng phn mm iu khin qu trnh o v x l tn hiu thu c.

3.2 Cch thc hin php phn tch AAS hon chnh:
tin hnh o ta tin hnh cc bc sau y: *Chun b thit b AAS: Xem xt tnh trng ca my, cc ng in, kh axetylen, N2O. Bt my vo ch lm vic. Chn cc iu kin ti u (t l kh t N2O+ axetylen dng in ). Ci t cc iu kin phn tch theo hng dn ca tng my. n nh my, n nh nhit trong vng 15 pht. *Trnh t phn tch: Dng ng chun. Pha ch dung dch cht chun cha cc nguyn t cn xc nh t cht chun phc tng ng vi nng khc nhau trong dung mi, dng ng chun cho tng nguyn t phn tch trn my AAS iu kin ti u tham kho trong cc hng dn. o ph AAS ca mu phn tch pha trong dung mi vi t l tng ng nh i vi cht chun. Ghi chp kt qu th hin trn my tnh. Sau khi kt thc cc php o a my v trng thi ban u, sau kha cc ng kh v tt my. *Tnh ton kt qu: Sau khi nhn c cc s liu kt qu trn my. Nng cc nguyn t cn xc nh c tnh ton theo cng thc sau: +Cng thc tnh cho mu lng (mg/l):
Me = A(C + B) (mg / l ) C

Trong :

-A: nng kim loi c xc nh theo ng chun mg/l. -B: lng dung mi pha long (ml). -C: nh mc mu phn tch (ml).

+cng thc sau cho mu rn (mg/kg):

Me = A.V W

Trong : -V: nh mc mu (ml). -W: khi lng mu (g).

-A: nng cht phn tch theo ng chun (mg/l).

+Tnh ton nng nguyn t trong mu phn tch bng phng php l Grafit theo cng thc sau:
Z (C + B) (mg / L) C

Trong :

-C: nh mc mu phn tch (ml). -B: th tch dung mi pha long (ml). -Z: nng nguyn t theo ng chun (mg/L).

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IV. V D P DNG PHNG PHP PHN TCH AAS p dng phng php phn tch ph hp th nguyn t xc nh hm lng thy ngn trong thy sn. 1. Nguyn tc: Mu thy sn c v c ha bng axit HNO3 m c trong bnh ph mu c np vn kn (bnh Kendal). Sau ta thu c hp cht v c c cha Hg, ta tin hnh Hydrit ha hp cht bng dng kh Hydro cho ta Hydrit thy ngn (HgH2) d bay hi. K thut c s dng phn tch Hg l k thut CV-AAS (phng php o ph hp th nguyn t bng k thut ha hi lnh). nhit phng th Hg tn ti th lng, trng thi hi th Hg tn ti trng thi n nguyn t. Cho nn thay v s dng nhit cao nguyn t ha Hg t cc hp cht ca Hg, ngi ta s dng cc cht kh mnh kh trc tip hp cht Hg2+ v Hg0 d bay hi. V d: Kh Hg2+ v Hg0 bng qu trnh Hydrit ha bng dng kh Hydro: 4H + HgCl2 = HgH2 + 2HCl HgH2 Hg + H2 2. Phng php tin hnh: (Phng php phn tch nh lng c s dng l phng php ng chun) 2.1 chun b mu: * Dung dch mu chun: - dung dch gc: ha tan 1g thy ngn trong 1000ml axit H2SO4 nng 1N. - dung dch trung gian: pha long 1ml dung dch gc thnh 1000ml bng dung dch axit H2SO4 nng 1N. - dung dch chun lm vic: pha long dung dch trung gian thnh dung dch chun lm vic c hm lng thy ngn ln lt l 2, 4, 6, 8 ,10 mg/l bng dung dch axit HNO3 nng 1N.

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* Dung dch mu phn tch: Cho 1g mu kh vo bnh Kendal, thm 5ml axit HNO3 m c ri vn cht np y kn bnh li yn t 20-30 pht. Sau , un nng chm trn bp in cho n khi thu c dung dch trong sut. Chuyn dung dch mu vo bnh chu nhit v un nng trn bp in n cn kh, ha tan cn bng 1ml nc ct ta thu c dung dch mu tin hnh phn tch. 2.2 Tin hnh phn tch: +Ghp ni hon chnh cc thit b ca h o ph hp th nguyn t . +Ti u ha cc iu kin lm vic trn my quang ph hp th nguyn t, s dng bc x kch thch c bc sng 253,7nm, nhy l 0,1ppm, ch o l CV-AAS. +Tin hnh o ph hp th ca cc mu chun c hm lng thu ngn ln lt l 2, 4, 6, 8 ,10 mg/l. T xc nh hp th A tng ng thng qua cc nh hp th trong ph hp th nguyn t va o ca cc mu chun.

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+T ta dng c ng chun A C. c minh ha nh hnh 2. di y:

+Khi ng chun c tuyn tnh tt ri th ta tin hnh o xc nh hp th Ax ca mu cn phn tch thng qua ph hp th ca n. Ph hp th ca mu cn phn tch c minh ha hnh 3.

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T kt qu Ax v ng chun ta tm c nng Cx thy ngn trong mu cn phn tch. 3. Tnh ton kt qu: Hm lng thy ngn trong mu c tnh theo cng thc sau: h
h

Trong :

+ CHg l hm lng thy ngn c trong mu (mg/g). + mHg l hm lng thy ngn c trong dung dch mu tnh c theo ng chun (mg/l). + V l th tch dung dch ha tan mu phn tch. + M l khi lng mu phn tch.

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V. NHN XT, NH GI PHNG PHP PHN TCH PH HP TH NGUYN T + Php o ph hp th nguyn t c nhy v chn lc cao. c bit hiu qu trong phn tch cc nguyn t vi lng + T nhiu ng dng ta nhn thy phng php AAS l mt k thut phn tch ha-l, ang pht trin mnh m v rng ri. + Hin nay phng php AAS tr thnh mt phng php tiu chun phn tch lng vt kim loi trong nhiu i tng khc nhau nh: t, nc, khng kh, thc phm + Hin nay trong lnh vc bo v mi trng, phng php ny l mt trong nhng cng c c lc xc nh hm lng cc kim loi nng v nhng nguyn t c hi trong t nhin v trong cc sn phm khc nhau.

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TI LIU THAM KHO

1. Cc phng php phn tch theo ph hp th nguyn t_Phm Lun, Trng i hc tng hp H ni 1987. 2. Phn tch hp cht bng phng php o ph http://www.scribd.com/doc/37407162/Phan-Tich-Hop-Chat-Bang-QuangPho-VinaEbookChemistryHere 3. Cc phng php phn tch Vt l v Ha l, Nh xut bn Khoa hc K thut. 4.http://vi.wikipedia.org/wiki/Ph%C3%A2n_t%C3%ADch_As_b%E1%BA %B1ng_ph%C6%B0%C6%A1ng_ph%C3%A1p_AAS

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