MC LC

Bi 1. XC NH HM LNG ST TRONG NC BNG QUANG PH UV-VIS1

Bi 1. XC NH HM LNG ST TRONG NC BNG QUANG PH UV-VIS

I. Tng quan: 1. Gii thiu chung v st: St c mt khp ni, cu to nn v tri t. Trong nc thin nhin, k c nc mt v nc ngm iu c cha st. Hm lng st v dng tn ti ca chng tu thuc vo tng loi ngun nc, iu kin mi trng, ngun gc to thnh.. Trong nc mt, st tn ti dng hp cht Fe3+, thng l Fe(OH)3 khng tan, dng keo hay huyn ph, hoc dng hp cht hu c phc tp t tan. Hm lng st thay i v t khi vt qu 1 mg/l, c bit khi nc c tnh kim v s c kh trong qu trnh lm trong nc. Do ion st hai d b oxy ha thnh hydroxyt st ba, t kt ta v lng nn st t tn ti trong ngun nc mt. i vi nc ngm, trong iu kin thiu kh, st thng tn ti dng ion Fe2+ v ho tan trong nc. Khi c lm thong, st hai s chuyn ha thnh st ba, xut hin kt ta hydroxyt st ba c mu vng, d lng. Trong trng hp ngun nc c nhiu cht hu c, st c th tn ti dng keo (phc hu c) rt kh x l. Ngoi ra, khi nc

c pH thp, s gy hin tng n mn ng ng v dng c cha, lm tng hm lng st trong nc. Trong nc ngm, do c pH thp, st tn ti dng ion. St c ho tr 2 l thnh phn ca cc mui tan nh Fe(HCO3)2, FeSO4. Hm lng st c trong cc ngun nc ngm thng cao v phn b khng iu trong cc lp trm tch di su. 2. ngha mi trng: St l nguyn t vi lng cn thit cho c th cu to hng cu. V th, st vi hm lng 0,3 mg/l l mc n nh cho php i vi nc sinh hot. Vt qu gii hn trn, s c mt ca st trong nc gy ra mt s nh hng bt li cho ngi s dng trong sinh hot gia nh, trong cng nghip v thng mi. St thng ng li trong cc ng ng cp nc lm gim p sut ca nc trong ng dn, v vy nh hng ti qu trnh phn phi nc. mc cng nghip, s xut hin st v mng gan trong nc s ph hu thc phm, ung, cng nghip giy v dt Mi tanh c trng ca st, khi tip xc vi kh tri, kt ta Fe(OH)3 hnh thnh, lm nc c mu gch to n tng khng tt cho ngi s dng. V th, nc c st khng th dng cho mt s nghnh cng nghip i hi cht lng cao nh: giy, du lch, t, si, dt, thc phm, dc phm Do cc l do trn, vic x l st cng nh phng php xc nh hamg lng st trong nc c ngha quan trng trong i sng cng nh trong sn xut cng nghip. 3. C s phng php - C ch to phc ca Fe(2+) vi thuc th 1,10-phenantroline 1,10-phenantroline hay cn gi l or-phenantroline l hp cht hu c d vng, c kh nng to phc mnh vi mt s ion kim loi

Hnh 1. Cng thc phn t 1,10-phenantroline

Cng thc phn t

C12H8N2

Khi lng phn t 180.3 g/mol Tn to dng tinh th trng Nhit nng chy - Nguyn tc : Do trong nc, st thng tn ti dng hn hp 2 ion Fe(2+) v Fe(3+). V vy mun xc nh tng hm lng st trong nc cn chuyn ton b Fe(3+) v dng Fe(2+) bng tc nhn kh Hydroxylamin hay hydroquynon, sau ion st (II) s to phc vi ba phn t 1,10-phenanthrolin, phc cht ny c mu cam, xy ra theo phn ng: Fe(OH)3 + 3 H+ 4 Fe3+ + 2 NH2OH Fe3+ + H2O 4 Fe2+ + N2O + H2O + 4 H+ 117 C Phc gia 1,10-phenantroline vi st c tn gi l ferroin c mu cam c hnh thnh trong khong pH t 3-9, ti u l 3,5.

Hnh 2. Phn ng to phc gia Fe v thuc th

- pH: 3-9, cng mu t l vi hm lng st (II) trong dung dch o. phn ng nhanh v hon ton, cn iu chnh pH = 2.9- 3.5 v dng lng tha phenanthrolin II. THC NGHIM 1. Ha cht v dng c: Ha cht: Dung dch st chun 100ppm Thuc th 1,10 phenantroline Hydroxylamine hydrochloride Sodium acetate Acid HNO3 m c Nc ct Bnh nh mc 100ml Pipet 1, 5, 10, 25ml Pipet nha Beaker 50, 250ml Cn in t My quang ph UV-Vis My nh siu m

Dng c

2. Quy trnh tin hnh Chun b dung dch st chun: Pha long st chun: Do vic o ph UV-Vis xc nh hm lng khong nng ppm, do o tap ha long dung dch st chun 100ppm xung 5ppm. Ta c: 100ppm. V= 5ppm. 100ml

Vy ta c V= 5ml Rt 5ml dung dch st 100ppm vo bnh nh mc 100ml, tin hnh nh mc bng nc ct ti vch, nh siu m sau khi nh mc. Pha dung dch Hydroxylamine hydrochloride Dng beaker 50ml cn 10g hydroxylamine hydrochloride . Ha tan vi nc, sau cho vo bnh nh mc 100ml, trng beaker v them nc ct n ng vch Pha dung dch Sodium acetate Dng beaker 50ml cn 10g Sodium acetate Ha tan vi nc, sau cho vo bnh nh mc 100ml, trng beaker v them nc ct n ng vch Pha dung dch 1,10-phenantroline Dng beaker 50ml cn 1g 1,10-phenantroline Ha tan vi nc, sau cho vo bnh nh mc 100ml, trng beaker v thm nc ct n ng vch Ch : 1,10 phenantroline hi kh tan trong nc cn nh siu m lu ha tan hon ton Pha cc dung dch xy dng ng chun: -Ty theo mu m ta c th dng ng chun theo cc nng khc nhau. - Thng th mu c nng ln ta ch cn dng mt ng chun duy nht cho tt c cc mu, sau pha long sao cho nng lt vo khong xy dng ng chun. i vi mu c nng b hn th phi xy dng ng chun c nng thp hn, Nhng xy dng cc ng chun thp khon ppb th i hi thit b phi hin i. - S dng 6 bnh nh mc 100ml, ln lt pha dy chun l 0; 0.2; 0.4; 0.6; 0.8; 1.0ppm, nh mc bng nc ct n ng vch. V(ml) dung dch st 0 (mu 4 8 12 16 20

chun 5ppm Hydroxylamine 1,10phenantroline Sodium acetate V(ml) pha long Nng sau khi pha long

trng) 1 10 10 100 0.0

1 10 10 100 0.2

1 10 10 100 0.4

1 10 10 100 0.6

1 10 10 100 0.8

1 10 10 100 1.0

Chun b mu: Mu nc thy cc Ly khong 150ml nc thy cc cho vo beaker 200ml, Ht vi git HNO3 m c vo sau em c cn nc xung cn khong 15ml. Tin hnh pha mu: Ht 10ml nc ct sau c cn( ngui) cho vsof bnh nh mc 100ml, tin hnh cho ln lt cc cht vi s lng ging nh bng trn, nh mc bng nc ct n ng vch. Mu nc sng (Tng t) Tin hnh o Sau khi m my n nh my khong 15 pht th ta c th chy my. `Bc 1: D tm bc sng hp th cc i Trc ht cn chy Baseline mu trng trc, sau chn dung dch 0.6ppm (hoc mt trong cc dy chun) o th tm bc sng.

Hnh 3. Ph ca dung dch 0.6ppm Kt qu: = 509.3 vi hp th cao nht A= 0.092 Nh vy bc sng ta chn bc sng thch hp l = 509.3 Bc 2: Lp ng chun Vo ch photometric ( nh lng) tin hnh chy dung dch chun. Ln lt chy t nng thp n cao bc sng o l 509.3.

Kt qu:

ng chun c dng: Phng trnh ng chun: Abs = K1*(Conc) + K0 Kt qu tnh ton bng Excel
ng chun
0.25 0.2 Abs 0.15 0.1 0.05 0 0.2 0.4 0.6 Nng 0.8 1 y = 0.0409x + 0.0001 R 2 = 0.9967

Hnh 4. th ng chun ca dy chun Fe

Bc 3: o mu Sau khi chy ng chun, ta chy mu Mu 1: Nc thy cc 1 2 3 Sample ID Ln 1 Ln 2 Ln 3 Conc 0.377 0.377 0.377 WL 509.4 0.077 0.077 0.077

Kt qu mu nc thy cc: 0.377mg/l Mu 2: Nc sng Long Bnh

1 2 3 4

Sample ID Ln 1 Ln 2 Ln 3 Ln 4

Conc 0.379 0.379 0.381 0.378

WL 509.4 0.077 0.077 0.078 0.077

Kt qu mu nc sng Long Bnh: 0.37925 mg/L

Bi 2. XC NH HM LNG ACETYLSALICYLIC ACID TRONG ASPIRIN S DNG QUANG PH HUNH QUANG I. Tng quan: 1. Acetyl salicylic acid Aspirin, hay acetylsalicylic acid (ASA), (acetosal) l mt dn xut ca acid salicylic, thuc nhm thuc chng vim non-steroid; c tc dng gim au, h st, chng vim.

Hnh 5. Cng thc ASA - Tnh cht Tinh th khng mu hoc bt kt tinh trng, khng mi hoc gn nh khng mi. Kh tan trong nc, d tan trong ethanol 96%, tan trong ether v

cloroform. o T trng o Nng chy o Si 1.40 g/cm 138140 C (280284 F)

140 C (284 F) (phn ly)

S tng hp aspirin c xp vo dng phn ng ester ha, nhm alcohol t salicylic acid phn ng vi dn xut ca acid(acetic anhydride) to nn mt ester. Salicylic acid c acetyl ha bng acetic anhydride cho aspirin v acetic acid nh mt sn phm ph.

Hnh 6. Phn ng tng hp ASA Aspirin c c thng c mi ging nh gim, bi v aspirin c th t phn tch thnh acid salicylic v acid acetic Tc dng o Thuc tc dng ln cc cn au nng nh, khu tr hoc lan ta nh au u, au c, au rng, au khp. c bit c tc dng tt i vi au do vim. Khng c tc dng ln cc au ni tng nh morphine. o Khng gy ng, khng gy khoi cm, khng gy nghin - c tnh * Mc d cc dn xut ca salicylic u t c, d ung, nhng dng lu c th gy hi chng salicyl (salicylisme): bun nn, nn, tai, ic, nhc u, l ln. * c ng: Ph, m ay, mn nga, hen... * Xut huyt d dy th n, hoc th nng. * Liu cht i vi ngi ln khong 20g. 2. Hin tng hunh quang

- Hunh quang l s pht quang khi phn t hp th nng lng dng nhit (phonon) hoc dng quang (photon). trng thi c bn So, phn t hp th nng lng t mi trng bn ngoi v chuyn thnh nng lng ca cc electron, nhn nng lng cc electron ny s chuyn ln mc nng lng cao hn, gi l trng thi kch thch S*, y l mt trng thi khng bn, do electron s mau chng nhng nng lng di dng nhit v trng thi kch thch mang nng lng thp hn S*o, thi gian tn ti ca electron gia mc nng lng S*->S*o vo khong 10-9 n 10-12 giy, sau khi v trng thi kch thch S*o, electron li mt ln na pht nng lng di dng photon v mc thp hn So, hin tng ny gi l hunh quang phn t. - Ph hunh quang c ng dng rng trong dc phm v y hc, Khoa hc mi trng; Ha phn tch, Nng nghip v thc phm; Sn xut v cng nghip; Quang ha; T bo sinh hc. - Ph hunh quang hot ng: do s kch thch ca ngun n c nng lng cao, photon t ngun s kch thch nhng phn t c kh nng pht hunh quang ln mc trng thi kch thch. Khi nhng e kch thch quay tr v trng thi c bn, ng thi pht ra bc x vi mc nng lng thp hn ( pht x hunh quang)

Hnh 7. Hin tng hunh quang

Hai loi thng tin thu c khi nghin cu pht x hunh quang: o S phn b cng bc sng, l mt du hiu ca cc cu trc in t ca phn t. o Cng ti bc sng bt k ni xy ra pht x, l mt du hiu ca nng ca cht pht hunh quang trong dung dch. Thng tin th hai l thng tin quan trng m chng ta ch yu s dng trong

phn tch hunh quang. Trong o hunh quang tng, cc mu c chiu x vi bc sng bit v s pht x hunh quang xy ra trn phm vi ton dy bc sng c o, Cc pht x c o gc 900 gim thiu hiu ng tn x. Lng bc x t cht hunh quang trong mu, c s dng nh mt du hiu ca nng .

Hnh 8. Pht x hunh quang gc 90o iu ny m t mt trong rt nhiu ng dng trong dc phm ca quang ph hunh quang . o hunh quang xc nh acetylsalicylic acid (ASA) trong vin thuc aspirin, c th thc hin trong 1% acetic acid trong dung mi cloroform. Trong dung mi bc sng hunh quang kch thch cho ASA khong 290nm, v dy pht x khong 300-420nm.

II. Thc nghim 1. Dng c- Ha cht: - Dng c o My o ph hunh quang RF o Bnh nh mc 250ml, 50ml, 10ml o Pipet thy tinh, pipet nha, micropipet. o Beaker 50ml o Cn in t - Ha cht: o Acetic acid o Cloroform o Acetone o Acetyl salicylic chun 2. Quy trnh - Pha dung mi acetic acid 1%/ cloroform Do acetyl salycilic rt kh tan trong nc, d tan trong ether hay cloroform nn ta khng s dng nc m dng cloroform lm dung mi. S dng pipet thy tinh 5ml ht 2.5ml acetic acid vo bnh nh mc 250ml, sau nh mc bng cloroform ti vch. em trong bng ti trnh nh sng trc tip lm phn hy cloroform. Ch : Nn s dng dng c bo h khi tip xc trc tip vi ha cht. Pha dy chun: o Cn 5mg acetyl salicylic chun vo beaker 50ml sau ha tan vi dung mi ri cho vo bnh nh mc 50ml, nh mc bng dung mi ti vch v trong bng ti. Nng : 5mg/50ml = 100ppm

o Tin hnh pha cc dy chun ht chnh xc ta s dng micro pipet ht ch l

V (ml) ASA 100ppm V (l) ASA 100ppm V sau khi nh mc (ml) Nng sau khi pha (ppm)

0.05 50 10 0.5

0.1 100 10 1.0

0.15 150 10 1.5

0.2 200 10 2.0

0.25 250 10 2.5

Pha mu:

Mu dng vin do cn c nghin nh thnh dng bt, sau ha tan bng dng mi ri cho vo bnh nh mc 50ml, lc u ri em lc. Tin hnh pha long xung 50000 ln.
-

Ht 100l mu sau lc vo bnh nh mc 10ml, tin hnh nh mc ti vch bng dung mi. ( Bnh 1) Ht 100 l mu bnh 1 ( va nh mc) cho vo bnh nh mc 10ml, tin hnh nh mc bng dung mi ti vch ( Bnh 2) Ht 50l mu va nh mc bnh 2 vo bnh nh mc 10ml, ri nh mc bng dung mi ti vch.

3. Phn tch v kt qu - Bc 1: D tm bc sng kch thch v nc sng pht x: Trc ht ta chy mu dung mi, qut 200-900nm c hai ch EX ( kch thch) v EM ( pht x). Kt qu: Kch thch EX 274 FI 11.339 Pht x EM

299 283 326

438.739 8.814 0.438

298 360 320

1015.804 54.193 32.792

Tip theo chy dung dch 0.5ppm ( hay mt trong cc dung dch chun khc) d tm bc sng. Ta chn khong bc sng thch hp l EX 282 EM 341. Bc 2: Chy dung dch chun Ln lt chy theo th t t thp n cao. Conc 1 2 3 4 Kt qu: 0.5 1.0 2.0 2.5 FI 146.31 152.32 181.49 190.51

Phng trnh ng chun : FI=K.C + B

ng chun
200 180 160 140 120 0 0.5 1 1.5 Nng (ppm) 2 FI

y = 23.515x + 132.38 R 2 = 0.9921

2.5

Hnh 9. th ng chun ca dy chun ASA

Bc 3: Chy mu FI Conc 1.1570 1.0539 1.0944

Mu sau khi x l v pha long, em o ta c kt qu Ln 1 Ln 2 Ln 3 159.590 157.167 158.119

Kt qu = 1.1018ppm. H s pha long = 5000 ln. Nng ASA ban u: 1.1018 x 5000 = 5509 mg/ L. Do ban u ta nh mc mu trong bnh nh mc 50ml, do khi lng ASA trong vin thuc l : mg ASA/ 0.05 = 5509 mg/ L mg ASA = 275.45mg. Kt lun: Trong vin thuc Aspirin, c tn ti 275.45mg Acetyl salilic.

Bi 3. XC NH HM LNG ST TRONG NC BNG PH HP TH NGUYN T- Atomic Absorption spectrocopy (AAS) I. C s l thuyt - Vi k thut tinh t, chnh xc kh cao cng trang thit b hin i, ph hp th nguy t c bit v s dng rng ri ti cc phng phn tch cng nh cc trung tm kim ngim hin nay. Bn c bit AAS c th phn tch lng rt nh cc kim loi trong cc mu khc nhau ca cc cht v c v hu c. Hin nay bng phng php ny ngi

ta c th nh lng khong 65 nguyn t kim loi v mt s kim n gii hn nng c ppm bng k thut F-AAS, v n nng ppb bng k thut ETA-AAS vi sai s khng ln hn 15%. - Nh chng ta bit, vt cht c cu to bi cc nguyn t v nguyn t l phn t c bn nh nht cn gi c tnh cht ca nguyn t ha hc. Trong iu kin bnh thng nguyn t khng thu cng khng pht ra nhng bc x. Lc ny nguyn t bn vng v ngo nng lng nht. Nhng khi nguyn t trng thi t do, ta chiu nhng chm sng c bc sng xc nh vo m hi nguyn t , th chng s hp th nhng bc x c bc sng xc nh ng vi nhng bc x m chng c th pht ra c trong qu trnh pht x ca chng. Lc nguyn t nhn nng lng t tia bc x v chuyn ln trng thi kch thch c nng lng cao hn. Qu trnh l qu trnh hp thu nng lng ca nguyn t t do trng thi hi v to ra ph hp th nguyn t ca nguyn t . Ph sinh ra trong qu trnh ny gi l ph hp th nguyn t. - Trong php o ph hp th nguyn t xc nh mt nguyn t hay mt hp cht ngi ta c th tin hnh phn tch ngay chnh cht theo ph hp th nguyn t ca n, nh phn tch cc kim loi, hay qua vic o ph hp th nguyn t ca mt cht khc, khi cht phn tch khng c tnh cht hp th nguyn t, nhng cht ny li c mt s tng tc rt nh lng v mt ha hc theo mt phn ng ha hc nht nh vi mt kim loi c ph hp th nguyn t nhy. Do xut hin hai loi phng php phn tch nh lng theo ph hp th nguyn t, l: - Cc phng php phn tch trc tip, cho cht c ph AAS v - Cc phng php phn tch gin tip, cho cht khng c ph AAS - Trong qu trnh phn tch hm lng st ta ch cp n phng php xc nh trc tip - V nguyn tc th tt c cc nguyn t v cc cht c ph hp th nguyn t chng ta u c th xc nh n mt cch trc tip theo ph hp th nguyn t ca n t dung dch mu phn tch. Ngha l cc phng php xc nh trc tip ch ph hp cho

vic xc nh cc kim loi c vch ph hp th nguyn t. V cc kim loi u c ph hp th nguyn t ca n trong nhng iu kin nht nh. Theo cch ny, ni chung trong nhiu trng hp, mu phn tch trc ht c x l theo mt cch ph hp c dung dch mu c cha cc Ion kim loi cn phn tch. Tip tin hnh nh lng n theo mt trong cc cch chun ha bit. y l cc phng php phn tch thng thng, v ang c dng rt ph bin, xc nh lng vt cc kim loi trong cc i tng mu hu c v v c khc nhau theo ph hp th nguyn t ca n. - V th ngi ta gi i tng ca cc phng php phn tch ny l phn tch kim loi trong cc loi mu v c v hu c. V d cc mu v c l qung, t, , khong liu, mui, oxit, kim loi, hp kim, xi mng, nc, khng kh v cc mu hu c l mu thc phm, ng, sa, hp, rau qu, ung, gii kht, mu, se rum, nc tiu, cc mu cy v sinh hc. - Khi phn tch cc loi mu ny th nguyn tc chung l gm hai giai on. - Giai on I: X l mu a nguyn t kim loi cn xc nh c trong mu v trng thi dung dch ca cc Cation theo mt k thut ph hp, chuyn c hon ton nguyn t cn xc nh vo dung dch o ph. - Giai on II: Phn tch nguyn t cn thit theo ph hp th nguyn t ca n theo nhng iu kin ph hp (mt quy trnh) c nghin cu v chn ra. Dng mt h thng nguyn t ha mu chuyn mu phn tch t trng thi ban u (rn hay dung dch) thnh trng thi hi ca nguyn t t do. Tip theo chiu chm tia sng bc x c trng ca nguyn t cn phn tch qua m hi nguyn t, thu ton b chm sng, phn ly v chn mt vch ph hp thu ca nguyn t cn nghin cu o cng ca n. Gi tr cng ny ph thuc tuyn tnh vo nng ca nguyn t trong mu phn tch. Tt nhin, y giai on I l cc k quan trng. V nu x l mu khng tt th c th lm mt nguyn t cn phn tch hay lm nhim bn thm vo. Ngha l vic x l mu khng ng s l mt ngun sai s rt ln cho kt qu phn tch,

mc du phng php phn tch c chn l ph hp nht. Vn ny c bit c ngha ln trong phn tch lng vt cc nguyn t. - Cc phng php phn tch trc tip ny l thch hp xc nh cc kim loi, m bn thn chng c ph hp th nguyn t. Nhng trong khong nm nm li y, nhiu phng php phn tch gin tip xut hin phn tch cc cht khng c ph hp th nguyn t, v d nh xc nh cc Anion, cc nhm phn t, cc hp cht hu c, cc dc phm. II. Thc nghim 1. Dng c v ha cht - My ph hp th nguyn t - My nh siu m - 6 bnh nh mc 50ml - 1 bnh nh mc 1lt - 5 beaker 100ml - pipet thy tinh: 1ml, 5ml, 10ml - pipet nha - HNO3 m c - Fe chun - Nc thy cc 2. Cc bc tin hnh 2.1. iu ch dung dch chun: Pha dy chun vi nng 2.00; 4.00; 6.00; 8.00; 10.00ppm T dung dch Fe chun 1000ppm pha xung 100ppm trong bnh nh mc 50ml ta ly Vml
V .1000 ppm = 100 ppm.50ml V = 5ml

T 100ppm pha thnh 2.00; 4.00; 6.00; 8.00; 10.00ppm. Ta c:

Pha dung dch 10.00ppm cn ly Vml dung dch 100ppm

V .100 ppm = 50ml.10 ppm V = 5ml

Tng t Pha dung dch 8.00ppm cn 4ml dung dch 100ppm Pha dung dch 6.00ppm cn 3ml dung dch 100ppm Pha dung dch 4.00ppm cn 2ml dung dch 100ppm Pha dung dch 2.00ppm cn 1ml dung dch 100ppm. Dng pipet ht tt c nhng lng cho vo bnh nh mc 50ml ri cho dung dch HNO3 0.5M n vch. Xong em nh siu m khong 3pht. 2.2. iu ch mu - Ht 10ml mu nc thy cc cho vo bnh nh mc 50ml - Cho HNO3 0.5M vo ti vch - Sau em nh siu m, xong dng giy lc lc mu vo mt beaker. 2.3.Tin trnh o mu Khi ng my bt qut ch my n nh. M phn mm ca my vo Worksheet new (to file mi), t tn v chn ni lu. - Ci t cc iu kin ti u cho my chy mu. Element: Fe Instrument type: Flame Conc. Units: mg/L Instrument Mode: Absorption Sampling Mode: Manual Calibration Mode: Concentration Measurement Mode: PROMT

Wavelength: 248.3 nm Lamp Current: 5.0mA Lamp position: 2(do n Fe v tr s 2) Background Correction: BC On Standard 1: 2.000mg/L Standard 2: 4.000mg/L Standard 3: 6.000mg/L Standard 4: 8.000mg/L Standard 5: 10.000mg/L Calibration Algorithm: liner Flamp Type: Air/Acetylene Air Flow: 3.50L/min Acetylene Flow: 1.50L/min Tip theo vo tab Analysis n select Chn s ln o mu M n- iu chnh cn gt cho ng v tr n(ch nng lng n ln khong trn 60% l c). M kh Bt la n start HNO30.5M o.

Lc ny mn hnh xut hin tab prepare Instrument Zero Ta s chn dung dch Tip n l chy dy chun t 1 n 5. Xong dy chun l chy mu vi 3 ln o c kt qu chnh xc. Cui cng Save li, ri vo Report chn Print ly d liu. 2.4. Kt qu o Dy chun Conc mg/L %Prec Abs

Standard 1: Standard 2: Standard 3: Standard 4: Standard 5:

2.000 4.000 6.000 8.000 10.000

0.9 1.0 0.7 0.7 0.9

0.1580 0.3150 0.4385 0.5429 0.6286

Hnh 10. th ng chun ca dy st chun Mu (Fe chun) Ln 1: Ln 2: Ln 3: 4.453 4.615 4.571 0.8 0.6 0.6 0.3122 0.3225 0.3197

Conc mg/L : nng %Prec : chnh xc, tin cy (di 30% l tt nht) Abs : hp th Nhn xt: - Nng mu khong 4.546ppm

Hnh 11. Ph ca mu Fe chun Dy chun Conc mg/L Standard 1: Standard 2: Standard 3: Standard 4: Standard 5: 2.000 4.000 6.000 8.000 10.000 %Prec 0.9 0.8 1.0 0.6 0.9 Abs 0.1286 0.2648 0.3624 0.4519 0.5423

Hnh 12. th ng chun ca dy st chun

 Mu nc thy cc Ln 1: Ln 2: Ln 3: 3.792 3.696 3.743 0.8 0.6 0.6 0.2269 0.2217 0.2242

Hnh 13. Ph ca mu nc thy cc Nhn xt: - Nng mu o c :

3.792 + 3.696 +3.743 = 3.744 ppm 3

Do lc u pha long mu xung 5 ln bng dung dch HNO3 nn Nng ca mu ban u: 3, 744 * 5 = 18.72 ppm =18.72mg/L. 2.5. Tho lun 1. Ta thy qua hai ln o kt qu khng c lp li cao, tc chnh xc khng cao, c rt nhiu nguyn nhn gy nn, ch yu l do: K thut ca ngi pha dy chun cha cao Cc nh hng v ph: Do dng kh i vo cha ph hp hoc b nhim bn lm cho ngn la chy khng tt nh hng n qu trnh nguyn t ha mu. Hay do my cha c lm sch, cn ln nhng ht rn nh li ti ca nhng mu trc cng gy nh hng n ngn la.

Cc yu t nh hng vt l: ch yu l do nht v sc cng b mt ca mu. Chnh s khc nhau v nng axit, loi axit, thnh phn cc cht c trong dung dch mu dn n s khc nhau v nht v sc cng b mt. ni chung, tc dn mu t l ngch vi nht ca mu.

Cc yu t ha hc: ch yu l do nng axit, cation, anion v loi axit c trong dung dch mu. Nu dung mi l axt, cation, anion d bay hi th cng lm tng cng ca vch ph v ngc li.

2. Dung dch mu o bng AAS thng c pha trong axit HNO3 l do: Nng axit trong dung dch mu lun lun c nh hng n cng ca vch ph ca nguyn t phn tch thng qua tc dn mu, kh nng ha hi v nguyn t ha ca cht mu. nh hng ny thng gn lin vi loi Anion ca axit. Ni chung, cc axit cng kh bay hi v bn nhit, cng lm gim nhiu cng vch ph hp th ca nguyn t phn tch, cc axit d bay hi gy nh hng nh Ni chung, cc axit lm gim cng vch ph theo th t: HClO4 < HCl: <HNO3 < H2SO4 < HaPO4 < HF, ngha l axit HClO4 < HCl v HNO3 gy nh hng nh nht trong vng nng nh. Chnh v th trong thc t phn tch ca php o ph hp th nguyn t (AAS) ngi ta thng dng mi trng l axit HCl hay HNO3 1 hay 2%. V nng nh th nh hng ca hai axit ny l khng ng k (nh hn 5%). - Cng vi cc Cation, cc Anion cng nh hng n cng vch ph ca nguyn t phn tch nh hng ny v tnh cht tng t nh nh hng ca cc loi axit. Ni chung, cc Anion ca cc axit d bay hi thng gim t cng vch ph. Cc Anion khc thng gy hiu ng nm (lm gim) theo th t Cl < NO3 < CO3 < SO 4 < F < PO34 < SIO32 . Do thc t nn trong mi php o phi gi cho nng ca cc Anion trong mu phn tch v mu chun l nh nhau v mt gi tr nht nh khng i.

Mt khc cng khng nn chn axit H2SO4 lm mi trng ca mu cho php o AAS m ch nn dng axit HCl hay HNO3 vi nng di 2%

Ti liu tham kho 1. Phm Lun, 2006, Phng php phn tch ph nguyn t, NXB HQG H Ni. 2. H Vit Qu, Cc phng php phn tch l ha tp II, NXB Gio dc 2000. 3. http://tailieu.vn/xem-tai-lieu/chuong-1-phan-tich-trac-quang.306742.htm
4. http://tailieuhay.com/chi-tiet-tai-lieu/xac-dinh-ham-luong-sat-trong-nuoc-bang-

phuong-phap-trac-quang/7303.html