Bi 3.

XC DJNH HM LUNG SAT TRONG NUC BANG PHO HP THJ

NGUYN TU- Atomic Absorption spectrocopy (AAS)
I. Co so l thuyt
- Voi ki thut tinh t, d chinh xac kha cao cung trang thit bi hin dai, ph hp thu
nguyn tu d duoc bit va su dung rng ri tai cac phong phn tich cng nhu cac trung
tm kim nghim hin nay. Ban co bit AAS co th phn tich luong rt nho cac kim loai
trong cac mu khac nhau cua cac cht v co va huu co. Hin nay bng phuong phap nay
nguoi ta co th dinh luong khoang 65 nguyn t kim loai va mt s a kim dn gioi han
nng d co ppm bng ki thut F-AAS, va dn nng d ppb bng ki thut ETA-AAS voi
sai s khng lon hon 15.
- Nhu chung ta d bit, vt cht duoc cu tao boi cac nguyn tu va nguyn tu la
phn tu co ban nho nht con giu duoc tinh cht cua nguyn t hoa hoc. Trong diu kin
binh thuong nguyn tu khng thu cng khng phat ra nhung buc xa. Luc nay nguyn tu
bn vung va ngeo nng luong nht. Nhung khi nguyn tu o trang thai tu do, ta chiu
nhung chum sang co buoc song xac dinh vao dam hoi nguyn tu do, thi chung s hp thu
nhung buc xa co buoc song xac dinh ung voi nhung buc xa ma chung co th phat ra duoc
trong qua trinh phat xa cua chung. Luc do nguyn tu d nhn nng luong tu tia buc xa va
chuyn ln trang thai kich thich co nng luong cao hon. Qua trinh do la qua trinh hp thu
nng luong cua nguyn tu tu do o trang thai hoi va tao ra ph hp thu nguyn tu cua
nguyn t do. Ph sinh ra trong qua trinh nay goi la ph hp thu nguyn tu.
- Trong phep do ph hp thu nguyn tu d xac dinh mt nguyn t hay mt hop
cht nguoi ta co th tin hanh phn tich ngay chinh cht do theo ph hp thu nguyn tu
cua no, nhu phn tich cac kim loai, hay qua vic do ph hp thu nguyn tu cua mt cht
khac, khi cht phn tich khng co tinh cht hp thu nguyn tu, nhung cht nay lai co mt
su tuong tac rt dinh luong v mt hoa hoc theo mt phan ung hoa hoc nht dinh voi mt
kim loai co ph hp thu nguyn tu nhay. Do do xut hin hai loai phuong phap phn tich
dinh luong theo ph hp thu nguyn tu, do la:
- Cac phuong phap phn tich truc tip, cho cht co ph AAS va
- Cac phuong phap phn tich gian tip, cho cht khng co ph AAS
- Trong qua trinh phn tich ham luong st ta chi d cp dn phuong phap xac dinh
truc tip
- V nguyn tc thi tt ca cac nguyn t va cac cht co ph hp thu nguyn tu
chung ta du co th xac dinh no mt cach truc tip theo ph hp thu nguyn tu cua no tu
dung dich mu phn tich. Nghia la cac phuong phap xac dinh truc tip chi phu hop cho
vic xac dinh cac kim loai co vach ph hp thu nguyn tu. Vi cac kim loai du co ph hp
thu nguyn tu cua no trong nhung diu kin nht dinh. Theo cach nay, noi chung trong
nhiu truong hop, mu phn tich truoc ht duoc xu li theo mt cach phu hop d duoc
dung dich mu co chua cac Ion kim loai cn phn tich. Tip do tin hanh dinh luong no
theo mt trong cac cach chun hoa d bit. Dy la cac phuong phap phn tich thng
thuong, d va dang duoc dung rt ph bin, d xac dinh luong vt cac kim loai trong cac
di tuong mu huu co va v co khac nhau theo ph hp thu nguyn tu cua no.
- Vi th nguoi ta goi di tuong cua cac phuong phap phn tich nay la phn tich kim
loai trong cac loai mu v co va huu co. Vi du cac mu v co la qung, dt, da, khoang
liu, mui, oxit, kim loai, hop kim, xi mng, nuoc, khng khi va cac mu huu co la mu
thuc phm, duong, sua, d hp, rau qua, d ung, giai khat, mau, se rum, nuoc tiu, cac
mu cy va sinh hoc.
- Khi phn tich cac loai mu nay thi nguyn tc chung la gm hai giai doan.
- Giai doan I: Xu li mu d dua nguyn t kim loai cn xac dinh co trong
mu v trang thai dung dich cua cac Cation theo mt ki thut phu hop, d chuyn
duoc hoan toan nguyn t cn xac dinh vao dung dich do ph.
- Giai doan II: Phn tich nguyn t cn thit theo ph hp thu nguyn tu cua
no theo nhung diu kin phu hop (mt quy trinh) d duoc nghin cuu va chon ra.
Dung mt h thng nguyn tu hoa mu d chuyn mu phn tich tu trang thai ban
du (rn hay dung dich) thanh trang thai hoi cua nguyn tu tu do. Tip theo chiu
chum tia sang buc xa dc trung cua nguyn t cn phn tich qua dam hoi nguyn
tu, thu toan b chum sang, phn ly va chon mt vach ph hp thu cua nguyn t
cn nghin cuu d do cuong d cua no. Gia tri cuong d nay phu thuc tuyn tinh
vao nng d cua nguyn t trong mu phn tich.
Tt nhin, o dy giai doan I la cuc ky quan trong. Vi nu xu li mu khng
tt thi co th lam mt nguyn t cn phn tich hay lam nhim bn thm vao. Nghia
la vic xu li mu khng dung s la mt ngun sai s rt lon cho kt qua phn tich,
mc du phuong phap phn tich d duoc chon la phu hop nht. Vn d nay dc bit
co y nghia lon trong phn tich luong vt cac nguyn t.
- Cac phuong phap phn tich truc tip nay la thich hop d xac dinh cac kim loai,
ma ban thn chung co ph hp thu nguyn tu. Nhung trong khoang nm nm lai dy,
nhiu phuong phap phn tich gian tip d xut hin d phn tich cac cht khng co ph
hp thu nguyn tu, vi du nhu xac dinh cac Anion, cac nhom phn tu, cac hop cht huu co,
cac duoc phm.
II. Thc nghim
1. Dng c v ha cht
- May ph hp thu nguyn tu
- May danh siu m
- 6 binh dinh muc 50ml
- 1 binh dinh muc 1lit
- 5 beaker 100ml
- pipet thuy tinh: 1ml, 5ml, 10ml
- pipet nhua
- HNO
3
dm dc
- Fe chun
- Nuoc thuy cuc
2. Cc buc tin hnh
2.1. Diu ch dung d|ch chun:
Pha dy chun voi nng d 2.00; 4.00; 6.00; 8.00; 10.00ppm
- Tu dung dich Fe chun 1000ppm pha xung 100ppm trong binh dinh muc 50ml ta
ly Vml
.1000 100 .50
5
' 552 552 2
' 2

- Tu 100ppm pha thanh 2.00; 4.00; 6.00; 8.00; 10.00ppm. Ta co:
Pha dung dich 10.00ppm cn ly Vml dung dich 100ppm
.100 50 .10
5
' 552 2 552
' 2

Tuong t
Pha dung dich 8.00ppm cn 4ml dung dich 100ppm
Pha dung dich 6.00ppm cn 3ml dung dich 100ppm
Pha dung dich 4.00ppm cn 2ml dung dich 100ppm
Pha dung dich 2.00ppm cn 1ml dung dich 100ppm.
- Dung pipet hut tt ca nhung luong do cho vao binh dinh muc 50ml ri cho dung
dich HNO
3
0.5M dn vach. Xong dem danh siu m khoang 3phut.
2.2. Diu ch mu
- Hut 10ml mu nuoc thuy cuc cho vao binh dinh muc 50ml
- Cho HNO
3
0.5M vao toi vach
- Sau do dem danh siu m, xong dung giy loc loc mu vao mt beaker.
2.3.Tin trnh do mu
Khoi dng may F bt quat F cho may n dinh.
Mo phn mm cua may vao Worksheet F new (tao Iile moi), dt tn va chon noi
luu.
- Cai dt cac diu kin ti uu cho may d chay mu.
O Element: Fe
O Instrument type: Flame
O Conc. Units: mg/L
O Instrument Mode: Absorption
O Sampling Mode: Manual
O Calibration Mode: Concentration
O Measurement Mode: PROMT
O Wavelength: 248.3 nm
O Lamp Current: 5.0mA
O Lamp position: 2(do den Fe o vi tri s 2)
O Background Correction: BC On
O Standard 1: 2.000mg/L
O Standard 2: 4.000mg/L
O Standard 3: 6.000mg/L
O Standard 4: 8.000mg/L
O Standard 5: 10.000mg/L
O Calibration Algorithm: liner
O Flamp Type: Air/Acetylene
O Air Flow: 3.50L/min
O Acetylene Flow: 1.50L/min
- Tip theo vao tab Analysis Fn select FChon s ln do mu
- Mo den- diu chinh cn gat cho dung vi tri den(cho nng luong den ln khoang
trn 60 la duoc).
- Mo khi F Bt lua Fn start
Luc nay man hinh xut hin tab prepare Instrument Zero FTa s chon dung dich
HNO
3
0.5M d do.
Tip dn la chay dy chun tu 1 dn 5.
Xong dy chun la chay mu voi 3 ln do d co kt qua chinh xac.
Cui cung Save lai, ri vao Report chon Print d ly du liu.
2.4. Kt qua do
Dy chun
Conc mg/L Prec Abs
O Standard 1: 2.000 0.9 0.1580
O Standard 2: 4.000 1.0 0.3150
O Standard 3: 6.000 0.7 0.4385
O Standard 4: 8.000 0.7 0.5429
O Standard 5: 10.000 0.9 0.6286

Knh 10. D thi duong chun cua dy st chun
Mu (Fe chun)
O Ln 1: 4.453 0.8 0.3122
O Ln 2: 4.615 0.6 0.3225
O Ln 3: 4.571 0.6 0.3197
Conc mg/L : nng d
Prec : d chinh xac, d tin cy (duoi 30 la tt nht)
Abs : d hp thu
Nhn xet:
- Nng d mu o khoang 4.546ppm


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

Hinh 12. D thi duong chun cua dy st chun
Mu nuoc thuy cuc
O Ln 1: 3.792 0.8 0.2269
O Ln 2: 3.696 0.6 0.2217
O Ln 3: 3.743 0.6 0.2242

Hinh 13. Ph cua mu nuoc thuy cuc
Nhn xet:
- Nng d mu do duoc :
3.792 3.696 3.743
3.744
3
552


Do luc du pha long mu xung 5 ln bng dung dich HNO
3
nn
Nng d cua mu ban du: 3, 744*5 18.72552 18.72mg/L.
2.5. Thao lun
1. Ta thy qua hai ln do kt qua khng co d lp lai cao, tuc d chinh xac khng cao,
co rt nhiu nguyn nhn gy nn, chu yu la do:
- Ki thut cua nguoi pha dy chun chua cao
- Cac anh huong v ph: Do dong khi di vao chua phu hop hoc bi nhim bn lam
cho ngon lua chay khng tt F anh huong dn qua trinh nguyn tu hoa mu. Hay
do may chua duoc lam sach, con ln nhung hat rn nho li ti cua nhung mu truoc
cng gy anh huong dn ngon lua.
- Cac yu t anh huong vt li: chu yu la do d nhot va suc cng b mt cua mu.
Chinh su khac nhau v nng d axit, loai axit, thanh phn cac cht co trong dung
dich mu d dn dn su khac nhau v d nhot va suc cng b mt. noi chung, tc
d dn mu ti l ngich voi d nhot cua mu.
- Cac yu t hoa hoc: chu yu la do nng d axit, cation, anion va loai axit co trong
dung dich mu. Nu dung mi la axit, cation, anion d bay hoi thi cang lam tng
cuong d cua vach ph va nguoc lai.
2. Dung dich mu do bng AAS thuong duoc pha trong axit HNO
3
la do:
Nng d axit trong dung dich mu lun lun co anh huong dn cuong d cua
vach ph cua nguyn t phn tich thng qua tc d dn mu, kha nng hoa hoi va
nguyn tu hoa cua cht mu. anh huong nay thuong gn lin voi loai Anion cua axit.
Noi chung, cac axit cang kho bay hoi va bn nhit, cang lam giam nhiu cuong d
vach ph hp thu cua nguyn t phn tich, cac axit d bay hoi gy anh huong nho
Noi chung, cac axit lam giam cuong d vach ph theo thu tu: HClO4 HCl:
HNO3 H2SO4 HaPO4 HF, nghia la axit HClO4 HCl va HNO3 gy anh
huong nho nht trong vung nng d nho. Chinh vi th trong thuc t phn tich cua
phep do ph hp thu nguyn tu (AAS) nguoi ta thuong dung mi truong la axit HCl
hay HNO3 1 hay 2. Vi o nng d nhu th anh huong cua hai axit nay la khng
dang k (nho hon 5).
- Cung voi cac Cation, cac Anion cng anh huong dn cuong d vach ph cua
nguyn t phn tich anh huong nay v tinh cht tuong tu nhu anh huong cua cac loai
axit. Noi chung, cac Anion cua cac axit d bay hoi thuong giam it cuong d vach ph.
Cac Anion khac thuong gy hiu ung nm (lam giam) theo thu tu Cl

NO
3

CO
3

SO
4
F PO
3
4
SIO
3
2
.
Do thuc t do nn trong mi phep do phai giu cho nng d cua cac Anion trong mu
phn tich va mu chun la nhu nhau va o mt gia tri nht dinh khng di.
Mt khac cng khng nn chon axit H2SO4 lam mi truong cua mu cho phep do
AAS ma chi nn dung axit HCl hay HNO3 voi nng d duoi 2

















Ti liu tham khao
1. Pham Lun, 006, Phuong php phn tich ph nguyn t, NXB DHQG Ha Ni.
2. H Vit Quy, c phuong php phn tich l ha tp II, NXB Giao duc 000.
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