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51503926 XAC ĐỊNH HAM LƯỢNG SẮT TRONG NƯỚC BẰNG PHƯƠNG PHAP TRẮC QUANG PDF
51503926 XAC ĐỊNH HAM LƯỢNG SẮT TRONG NƯỚC BẰNG PHƯƠNG PHAP TRẮC QUANG PDF
Tng quan:
1. Gii thiu chung v st:
2. ngha mi trng:
-
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
-
C12H8N2
117 C
- Nguyn tc :
-
3 H+
2 NH2OH
Fe3+
H2O
Hydroxylamine hydrochloride
Sodium acetate
Acid HNO3 m c
Nc ct
Dng c
-
Bnh nh mc 100ml
Pipet nha
Cn in t
My quang ph UV-Vis
My nh siu m
Ta c:
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.
-
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.
0 (mu
12
16
20
chun 5ppm
Hydroxylamine
1,10phenantroline
Sodium acetate
V(ml) pha long
Nng sau khi
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
pha long
Chun b mu:
-
Mu nc thy cc
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
Kt qu:
ng chun c dng:
Phng trnh ng chun: Abs = K1*(Conc) + K0
Kt qu tnh ton bng Excel
ng chun
0.25
Abs
0.2
0.15
y = 0.0409x + 0.0001
R 2 = 0.9967
0.1
0.05
0
0.2
0.4
0.6
0.8
Nng
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
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
Tng quan:
1. Acetyl salicylic acid
cloroform.
o T trng
1.40 g/cm
o Nng chy
138140 C (280284 F)
o Si
-
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)
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
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
0.05
0.1
0.15
0.2
0.25
50
100
150
200
250
10
10
10
10
10
0.5
1.0
1.5
2.0
2.5
Pha mu:
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
Pht x EM
FI
11.339
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.
-
FI
0.5
146.31
1.0
152.32
2.0
181.49
2.5
190.51
Kt qu:
ng chun
y = 23.515x + 132.38
R 2 = 0.9921
200
FI
180
160
140
120
0
0.5
1.5
Nng (ppm)
2.5
Bc 3: Chy mu
Conc
Ln 1
159.590
1.1570
Ln 2
157.167
1.0539
Ln 3
158.119
1.0944
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.
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
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.
-
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
M kh Bt la n start
Lc ny mn hnh xut hin tab prepare Instrument Zero Ta s chn dung dch
HNO30.5M o.
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:
2.000
0.9
0.1580
Standard 2:
4.000
1.0
0.3150
Standard 3:
6.000
0.7
0.4385
Standard 4:
8.000
0.7
0.5429
Standard 5:
10.000
0.9
0.6286
4.453
0.8
0.3122
Ln 2:
4.615
0.6
0.3225
Ln 3:
4.571
0.6
0.3197
%Prec
Abs
Standard 1:
2.000
0.9
0.1286
Standard 2:
4.000
0.8
0.2648
Standard 3:
6.000
1.0
0.3624
Standard 4:
8.000
0.6
0.4519
Standard 5:
10.000
0.9
0.5423
Mu nc thy cc
Ln 1:
3.792
0.8
0.2269
Ln 2:
3.696
0.6
0.2217
Ln 3:
3.743
0.6
0.2242
2. Dung dch mu o bng AAS thng c pha trong axit HNO3 l do:
phuong-phap-trac-quang/7303.html