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Phng php ph hp th nguyn t ngdng phn tch tch tn d kim loi nngtrong thc phm
TS: L Th Hng HoTrung tm KN-VSATTP
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QU THNH PHT TRIN PH NGUYN T
1950 1960 1970 1980 1990
ph pht x
hp th nguyn t
nguyn t hunh quang
ICPS
year
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Khong nng phn tch
ICP-MS
pht xAAS ngn
laAAS khng ngn la
1 ppt 1 ppb 1 ppm 0.1% 100%
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E2
E1e-
hn
E = E2 - E1
= hn
l = hc/ (E2 - E1 )
E2 = trng thi kch thch
E1 = trng thi c bnh = hng s Planckn = Spectral frequency
Hp th nguyn t
l = c / v
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H thngAAS
Ngun sng
gng
MONOCHROMATOR
DETECTORGhi nhn tn
hiu
Nguyn tho
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H thngAAS
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H thngAAS(1) ngun bc x (n catot rng)
Ngun sng
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Ngun pht bc x n sc
Phi l cc tia bc x nhy i vi nguyn t cn phn tch,chm tia sng phi c cng n nh, lp li c trong ccln o khc nhau trong cng iu kin v phi iu chnh c c cng cn thit trong mi php o (bng dng in lmvic ca HCL).
Ngun pht tia bc x to c chm bc x thun khit, chbao gm mt s vch nhy c trng ca nguyn t phn tch.Ph nn ca n phi khng ng k.
Chm tia pht x n sc do ngun cung cp phi c cng
cao. Nhng li phi bn vng theo thi gian v phi khng bcc yu t vt l khc nhiu lon, t b nh hng bi cc daong ca iu kin lm vic. Ngoi ra, khng qu t v khngqu phc tp khi s dng.
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n Catot rng
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N PHNG IN KHNG IN CC
Ngunbc x mnh hn n catot rnggp 10 ln
sdng cho As, Se, Te, Hg, Pb nhngnguyn t km nhyvin catot rng.
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(2) Nguyn t ho
nguyn t ho
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Nguyn t ho
L qu trnh ho hi v nguyn t ho chtphn tch thnh nguyn t t do
Dung dich
Phun kh
Son kh Nguyn
t t doNhit
Ngn la
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Cc dng nguyn t ho
(1)Ngn la
(2) Khng ngn la- L graphit AAS (GFA)
- hydride vapor generator (HVG)
- mercury vapor unit (MVU)
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Ngn la
Ngn la l s oxi ho c kt hp bi khng kh,NO2, Ar, H2, acetylene.
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Qutrnh nguyn t ho trong ngn la
Dung dch
Ho hi
Bay hi
Son kh ho
Son kh
Nguyn t hoNguyn t t do
Nguyn tc bit
Ion cbit
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Qutrnh nguyn t ho khngngn la
(1) L graphite AAS (GFA)
(2) Hydride vapor generator (HVG)
(3) Mercury vapor unit (MVU)
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L graphite AAS
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Qutrnh nguyn t ho trong l
Chuyn
Dung dch muDung dch
sy
Bt kh
Nguyen t ho
Vapor
Nguyn tc bit
Ion cbit
Free atoms
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Cc bc thay i nhit trong l
Lm kh
Tro ho
Nguyn t ho
Nhit(oC)
Thi gian (s)Outer gas (Ar)
Inner gas (Ar)
Inner gas (O2)0 20 35 50 54
Lm sch
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Cc loi cuvet nguyn t ho mu
Than ch
Pyrolytic
Platform
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Graphite Furnace Tubes
L bm mu
Cuvet graphite
L bm mu
Cuvet pyrolytic
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Cuvet Platform
im bm mu
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Qutrnh nguyn t ho khngngn la
(1) Graphite furnace
(2) Hydride vapor generator (HVG)
(3) Mercury vapor unit (MVU)
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Hydrid ho (HVG)
Se, As, Sn, Sb, Te
Bi
Ho hi Hydride
Nguyn t ho
Ngn la Nhit
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Hydrid ho (HVG)
BH4- + 3H2O + H
+ H3BO3 + 4H2
3BH4- + 3H + + 4H3AsO3 4AsH3 + 3H2O + 3H3BO3
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Hydrid ho (HVG)
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Flameless AAS
(1) Graphite furnace AAS (GFA)
(2) Hydride vapor generator (HVG)
(3) Mercury vapor unit (MVU)
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Ho hi lnh (MVU)
Ion thu ngn trong dung dch c kh
bi SnCl2to thnh nguyn tthu ngn ckhnng bay hinhit phng.
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B ho hi thu ngn (MVU)
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Mercury Vapor Unit (MVU)
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Detector - Photomultivlier
L mt loi dng c quang hc dng thu nhn v phthin tn hiu quang hc theo hiu ng quang in ca n.Trc y thu nhn ngi ta dng knh nh hay
phim nh, sau l t bo quang in. l cc dng cc in vi nhy km.
Vi s pht trin ca khoa hc v k thut, ngy nay ngita ch to ra c nhiu loi detector quang hc c thkhuch i tn hiu o c ln c triu ln. l cc ngnhn quang in.
Nhn quang in kiu ng l mt loi dng c thu nhn
tn hiu quang hc c tnh cht vn nng, n c nhy v chn lc cao. Vng ph hot ng ca cc detector kiuny thng l t 190 900 nm, c khi n 1100 nm. H skhuch i thng n 106, i khi n 107.
C t h h
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Cc yu t gy nh hng n qutrnh o hp th nguyn t
nh hng ca nng axt v loi axttrong dung dch mu:Nng axt lmthay i nht ca dung dch, do aniongc axt quyt nh. Cc axt cng kh bayhi thng cng lm gim cng vchph. Cc axt d bay hi gy nh hng t.
Axt lm gim hp th theo th t HCl
