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Nhm B1 thc tp ngy th 3

Tn :
Trn Thanh Phng Tho MSSV: 1114184
Nguyn Trung Hi Thnh MSSV: 1114193
Phm Tn Thoi MSSV: 1114195
Bi 7: PHNG PHP QUANG PH NGUYN T - PHNG PHP PH
HP THU NGUYN T XC NH HM LNG Mn TRONG NC
I.
Nguyn tc chung
1. Khi qut v chung ph nguyn t
Da trn s hp thu hay pht x c trng bc x in t ca nguyn t trng
thi t do phng php ph nguyn t c th phn tch nh tnh hay nh lng
cc nguyn t.
S di chuyn ca in t ha tr gia cc vng nng lng khc nhau trng thi
nguyn t t do ca cc nguyn t khc nhau l c s cho c trng ca bc
sng v tn s bc x in t m nguyn t hp thu hay pht x.
iu kin tin quyt ca phng php ph nguyn t l phi cung cp nng lng
ln ct t lin kt to thnh cc nguyn t t do. Ngun nng lng dng
ct t lin kt thng l nhit nng do cc phn ng chy sinh ra, do dng
in hoc do s ion ha cht kh. Di tc dng ca ngun nng lng ny cc
cht phn tch b bay hi nng chy v phn ly thnh cc nguyn t t do.
C 3 phng php ph nguyn t thng dng l: ph hp thu nguyn t AAS (
atomic absorption spectroscopy), AES ph pht x nguyn t (atomic emission
spectroscopy), ph hunh quang nguyn t EFS ( atomic flourescence
spectroscopy)
2. Ph hp thu nguyn t.
L 1 trong 3 phng php ph nguyn t, c s dng rng ri da trn cc
nguyn tc chung ca ph nguyn t ph hp thu nguyn t trn s hp thu ca
nguyn t t do vi cc bc x in t c trng ta c th phn tch nh lng
cc cht phn tch.
Nng lng nguyn t ha trong phng php ph hp thu nguyn t l nhit
nng c cung cp bi phn ng chy, dng in hoc t s ion ha cht kh.
Bi thc tp ny tin hnh phn tch nh lng hm lng ca Mn trong nc
bng ph hp thu di tc nhn nguyn t ha l ngn la C2H2 + khng kh bng
phng php dng ng chun.

S dng vch ph hp thu nhy nht ca Mn l vch ph 279.5 nm vch ph nhy


nht trong chum vch ph cng hng ca Mn 279.5nm, 279.8nm, 280.1nm.
II.
Thc hnh
1. Pha dung dch cha kim loi chun
Nguyn tc chung pha dung dch chun.
Nn pha t kim loi hoc oxid kim loi trong dung mi thch hp.
Dung dch lu tr phi c nng ln hn 1000g/mL, cc dung dch c nng
nh hn ch nn c chun b trc khi s dng.
Dung dch c nng nh hn 1g/mL nn c s dng trong vi gi hoc t
hn.
Trc khi cn cht chun cn x l m bo chng ng trng thi vi cng
thc ha hc.
i vi kim loi cn c ra sch vi aceton hoc ether co sch lp oxid hoc
cho tc dng vi acid ri em sy kh.
i vi oxid sy 1100C trong 2 gi ui ht nc bao bc.
i vi hp cht cn gi n nh lng nc kt tinh hoc sy kh 1100C trong
2 gi ui nc.
Dung dch Mn chun trong bi thc hnh c pha theo nguyn tc trn trong
HNO3 1% t dung dch Mn chun 1000g/mL. Dy chun nng theo bn sau
S th 1
t
Mn
0
(ppm)
2.

10

0.5

1.0

2.0

3.0

4.0

5.0

6.0

8.0

10.0

Cch o AAS trn my shimadzu 6300


Bt my AAS.
Khi ng my nn kh
M van C2H2
Khi ng phn mm.
Lp n cathode Mn vo khoang n, khai bo v tr.
Khai bo tin hnh phn tch nguyn t Mn.
Chn = 279.5nm, khe o (slit) 0.2nm, dng nui n (lamp current) 15mA, s
ln o lp n = 3, qut bc sng chn li chnh xc bc sng c hp hp
thu mnh nht tropng iu kin chun b tin hnh phn tch (v trong mi trng
hp trc khi o iu kin bn ngoi, h quang hc s nh hng lm sai lch
bc sng hp thu cc i i cht so vi l thuyt).

3.

Chn ch o AAS
iu chnh lng kh C2H2 v khng kh, bt la t chy kh C2H2 v khng kh.
Phun nc ct 3 pht vo h thng n F3 ra sch h thng.
Thit lp nng cho cc standard theo nng trong bng.
Ln lt phun cc dung dch chun vo ngon la khi tnh hiu xut hin n F4.
Thc hin cc bc tng t i vi bc sng 280.1 nm.
Line search bc sng
Trc khi tin hnh o ph hp thu ca cc cht phn tch ta cn tin hnh line
search li bc sng xc nh chnh xc bc sng c hp thu cc i trong
trng hp tin hnh o ph hp thu. V bc sng hp thu cc i trn l thuyt
v bc sng hp thu trong qu trnh o ph hp thu c th khc nhau do nh
hng ca h quang hc v cc iu kin tin hnh o ph hp thu.
i vi bc sng 279.5nm ta tin hnh line search c kt qu nh sau

Ta thy bc sng hp thu cc i trn l thuyt l 279.50nm nh bc sng hp


thu cc i y l 279.43nm nguyn nhn c th l do s sai lch i cht ca
h quang hc trong my v iu kin tin hnh o.
Tng t i vi bc sng 280.1nm ta tin hnh line search c kt qu sau

Ta thy trn l tuyt bc sng hp thu trng hp ny l 280.1nm nhng khi


tin hnh line search kt qu thu c l 279.97nm nguyn nhn gy ra sai lch
y cng chnh l do s sai lch i cht ca h quang hc v iu kin tin hnh
o ph hp thu.
xc nh c chnh xc bc sng hp thu cc i trc khi tin hnh o ph
hp thu ta cn line search li. bc sng hp thu cc i ca cht phn tch trong
trng hp o ph hp thu khc vi bc sng m n pht x pht ra, bc sng
hp thu cc i ny ph thuc vo h quang hc ca tng loi my, iu kin tin
hnh o ph hp thu nn vi mi loi my khc nhau, vi mi iu kin o ph
hp thu khc nhau s c kt qu khc nhau.
III. Kt qu v x l s liu
1. Bc sng 279.5 nm
nng (g/mL) 0.5
1.0
2.0
3.0
4.0
5.0
6.0
8.0
Abs
0.0811 0.1596 0.3102 0.4762 0.6194 0.7525 0.8727 1.0784
Theo phng php bnh phng ti thiu t phng trnh tuyn tnh bc nht
(ISO 8466-1).

Trong A l hp thu C l nng tnh theo g/mL a, b l cc h s hi quy


c :

10.0
1.2400

0.1248
0.0735

Phng sai d:

0.0028

0.0059

0.0314

Bin lun khong tin cy ca h s a, b

0.0198
0.0037

T cc gi tr trn ta thit lp phng trnh tuyn tnh nh sau:


(

Ta dng th nh sau.

A
1.4000
1.2000

y = 0.1248x + 0.0735
R = 0.9846

1.0000
0.8000
0.6000
0.4000
0.2000
0.0000
0.0

2.0

4.0

6.0

8.0

10.0

12.0

C(g/mL)

biu biu din hp thu theo nng dung


dch chun
Qua th tra thy khong tuyn tnh s tt hn nu ta s dng cc dung dch c nng
t 2.0g/mL n 6.0g/mL.
Gi s ta ch s dng cc dung dch c nng t 2.0g/mL n 6.0g/mL. Ta c kt
qu sau:

0.1401

0.0457

Phng sai d:

0.0003

0.0050

0.0212

Bin lun khong tin cy ca h s a, b

0.0224

0.0053

T cc gi tr trn ta thit lp phng trnh tuyn tnh nh sau:


(

Ta c biu :
1.0000
y = 0.1401x + 0.0457
R = 0.996

0.9000
0.8000
0.7000
0.6000
0.5000
0.4000

C(g/mL)

0.3000
2.0

2.5

3.0

3.5

4.0

4.5

5.0

5.5

6.0

6.5

biu biu din hp theo nng dung dch


chun

2. Bc sng 280.1nm
Nng 0.5
(g/mL)
Abs
0.0397

1.0

2.0

3.0

4.0

5.0

6.0

8.0

10.0

0.0802

0.1573

0.2440

0.3195

0.3934

0.4614

0.5943

0.7160

Theo phng php bnh phng ti thiu t phng trnh tuyn tnh bc nht (ISO
8466-1).

Trong A l hp thu C l nng tnh theo g/mL a, b l cc h s hi quy


c :

0.0718

0.0187

Phng sai d:

0.0002

0.0016

0.0085

Bin lun khong tin cy ca h s a, b

0.0054
0.0010

T cc gi tr trn ta thit lp phng trnh tuyn tnh nh sau:


(

Ta c biu

0.8000
0.7000

y = 0.0718x + 0.0187
R = 0.996

0.6000
0.5000
0.4000
0.3000
0.2000
0.1000
0.0000
0.0

2.0

4.0

6.0

8.0

10.0

C(g/mL)
12.0

biu biu din hp thu theo nng dung


dch chun

T biu ta thy khong tuyn tnh s tt hn nu ta chn dung dch t 1.0-6.0


g/mL.
Gi s ta ch s dng cc dung dch t 1.0-6.0 g/mL v thu c kt qu ph hp thu
nh trn ta c:
c :

0.0769
0.0070

Phng sai d:

0.00004

0.0014

0.0055

Bin lun khong tin cy ca h s a, b

0.0048
0.0012

T cc gi tr trn ta thit lp phng trnh tuyn tnh nh sau:


(

Ta dng c biu sau:

A
0.5300
y = 0.0769x + 0.007
R = 0.9986

0.4800
0.4300
0.3800
0.3300
0.2800
0.2300
0.1800
0.1300

C(g/mL)

0.0800
1.0

2.0

3.0

4.0

5.0

6.0

7.0

biu bi din hp thu theo nng dung


dch chun

NHN XT:
bc sng
279.5nm

1.4000
1.2000

bc sng
280.1nm

1.0000
0.8000
0.6000
0.4000
0.2000

C(g/mL)

0.0000
0.0

2.0

4.0

6.0

8.0

10.0

12.0

biu biu din hp thu theo nng


ca dung dch chun

hp thu 2 bc sng 279.5nm v 280.1nm khc nhau. bc sng 279.5nm


c hp thu ln hn v theo l thuyt y l bc sng hp thu cc i ca Mn
trong chm vch cng hng multilet . Vi bc sng 279.5nm ta c th phn tch
Mn vi nhy cao hn so vi khi s dng bc sng 280.1nm phn tch Mn.
Mi bc sng iu c mt khong tuyn tnh nht nh vi bc sng 279.5nm ta
c khong tuyn tnh 2.0-6.0(g/mL) cn vi bc sng 279.5nm ta c khong
tuyn tnh t 1.0-6.0(g/mL) rng hn so vi bc sng 279.5nm. Khi tin hnh
phn tch nh lng vi bc sng 280.1nm c nhy km hn nhng li cho
khong tuyn tnh rng hn nn ty vo trng hp yu cu cu php phn tch
m ta nn chn bc sng phn tch cho ph hp.
Trc khi tin hnh phn tch ta cn line search xc nh li chnh xc bc
sng hp thu trong tng trng hp c th v c th bc sng hp thu cc i khi
tin hnh phn tch s sai lch i cht so vi bc sng hp thu cc i theo l
thuyt.
Khi lp n cathode vo khoang n cho n hot ng ta ta thy n c chm
ch cathode mc d bc sng pht x ca Mn nm trong vng UV l do s Mn
trong n b kch thch nng ln pht ra bc x.
Trong qu trnh tin hnh o ph hp thu tc dng ca kh C2H2+khng kh
phi c gi n nh trong gii hn cho php v tc dng ca kh s nh
hng n tc phun sng nh hng n hiu sut ly mu v lp li ca
php phn tch.
Phng php dng ng chun thun li phn tch lng ln mu c nn mu
tng t nhau v khng qu phc tp.
Ph hp thu nguyn t l phng php phn tch c chnh xc v nhy rt
cao nht l i vi cc nguyn t kim loi. v nhy rt cao nn qu trnh x l
mu i hi tht cn thn loi tr nh hng ca nn mu trnh s gy nhiu
lm sai lch kt qu phn tch. Phi hiu r thao tc tin hnh th nghim v ch
mt s xut nh trong qu trnh phn tch cng dn ti nhng hu qu nghim
trng. phng php i hi my mc k thut hin i, chnh xc cao.