Nhm thc hin GVHD

: Nhm 01 : Th.s Trn Nguyn An Sa

Ni dung
1. 2. Tng quan k thut ng chun ng dng xc nh hm lng Fe(II) v tng Fe Nguyn tc Cc cht gy nhiu Ho cht Dng c - thit b Cch tin hnh

K thut ng chun

u v nhc im
1. 2. u im Vi mt ng chun cho php phn tch hng lot mu nn nhanh v hiu qu kinh t. Nhc im Cn c my, my cng chnh xc th kt qu cng tin cy.

S hp thu nh sng ca dung dch phi tun theo nh lut Bughe- Lambe- Beer.
Khng loi c nh hng ca nn mu.

ng dng xc nh hm lng Fe(II) v tng Fe

St l nguyn t vi lng cn thit cho c th. V th, st vi hm

lng 0,3 mg/l l mc cho php i vi nc sinh hot. Vt qu gii

hn trn, st c th gy ra nhng tr ngi: Mi tanh c trng ca st, lm nc c mu to n tng khng tt cho ngi s dng. Nc c st khng th dng cho mt s nghnh cng nghip nh: giy, si, dt, thc phm, dc phm Kt ta st lng ng thu hp dn tit din hu dng ca ng dn trong mng li phn phi nc. Do cc l do trn, vic xc nh hm lng st trong nc c ngha quan trng trong i sng cng nh trong sn xut cng nghip.

Nguyn tc
Fe2+ to phc bn c mu cam vi 1,10 phenanthroline.

Phc [Fe(Phen)3]2+ bn c max 508nm, cng mu khng thay i trong khong pH t 2 9.

Tng hm lng St: dng hidroxylamine kh Fe3+ v Fe2+. Hm lng Fe3+ = tng hm lng Fe - hm lng Fe2+

Cc cht gy cn nhiu
Nhng cht oxi ha mnh: CN-, NO2-, PO43Zinc vi hm lng ln hn st 10 ln Copper ln hn 5ppm Niken ln hn 2ppm Bitmut,thy ngn, molybdate, bc kt ta vi phenanthroline (thm mt lng tha phenanthroline) Cht hu c (un si mu nhiu gi vi HCl 1:1trong cc s, khi mu cn, t nh, phn tro cn li ha tan bng axit).

Ho cht
m V ml Cppm MM 100 10 6 Mion p

Ht 2.5 ml dung dch chun gc Fe2+ 1000ppm Vo bnh nh mc 50ml

nh mc bng nc ct

50ml

Ht 0.75 ml dung dch chun gc Fe2+ 1000ppm Vo bnh nh mc 50ml

nh mc bng nc ct
50ml

Ho cht
4. Dung dch Fe3+ 15ppm
Ht 0.75 ml dung dch chun gc Fe3+ 1000ppm Vo bnh nh mc 50ml nh mc bng nc ct
50ml

5. Dung dch NH2OH 10% pha trong nc.

6. m axetat pH = 5. 7. Dung dch 1,10 phenanthroline 0.5% pha trong nc.

Dng c - thit b
Bnh nh mc 1L Pipet vch 10ml Cuvet My pH k Cn phn tch Bp cao su Beaker 250ml Beaker 100ml My khuy t a thy tinh Pipet bu 5ml C t My so mu 01 01 01 01 01 01 03 02 01 01 My quang ph Genesye 10UV scanning 02 01 01

Cch tin hnh

1. 2. 3. 4. Qut ph v xy dng ng chun. Hiu sut thu hi ca phng php. Kim tra mu th. Vn hnh thit b.

Qut ph v xy dng ng chun

Bnh s VFe 50ppm (ml) Hydroxylamin (ml) Dung dch m pH = 5 (ml) 1,10- phenanthroline 1 0 2 1.0 3 2.0 2.0 10.0 2.0 4 3.0 5 4.0 6 5.0

nh mc bng nc ct n vch 50ml

Qut ph v xy dng ng chun

Hiu sut thu hi ca phng php

Bnh s V_dd B 1 2 10 3 10 4 10 5 6 7

V_ dd C
Hydroxylamin 2.0 0.0

10

10
2.0

10

yn 10 pht Dung dch m pH = 5 (ml) 1,10- phenanthroline (ml) 10.0 2.0

nh mc bng nc ct n vch 50ml

Kim tra mu
Bnh s V_ddA (ml) Hydroxylamin (ml) 2.0 yn 10 pht 1 2 10 3 10 0.0 4 10 5 10 6 10 2.0 7 10

Dung dch m pH = 5 (ml) 1,10- phenanthroline (ml)

10.0 2.0

nh mc bng nc ct n vch 50ml

Vn hnh my

Vn hnh my
1. Trng hp my khng kt ni vi phn mm Visionlite

Nhn cng tc ngun ON/OFF trn my, ch n nh. Nhn phm Test mn hnh hin th: - Advanced A; %T; C - Standard curve - Absorbance Ratio - Absorbance Difference - Performance Validation - Kinetics - Scanning - 3-point Net - Mulatiwavelength

Vn hnh my
Nu qut bc sng, nhn phm hoc chn Scanning; sau Enter. Chn khong bc sng cn qut v chn lnh qut bc sng. - Chy nn bng cch qut vi mu trng. - Chy mu bng cch chn mt mu bt k qut. Nu o mu ring bit nhn phm hoc chn ch o Advanced A ; %T; C. Nu xy dng ng chun ta nhn phm hoc

chn Standard curve.

Vn hnh my
2. Trng hp my o quang kt ni vi phn mm Visionlite Nhn cng tc ngun ON/OFF trn my, ch n nh. Khi ng my vi tnh, m phn mm Visionlite

Nu qut bc sng ta chn ch Scan v thc hin cc bc sau:

Vn hnh my
Phn mm gm 4 module: Scan : Ghi nhn ph. Rate : Fixed : Ghi nhn s hp th ca mu ti mt im ca mt bc sng. Quant : nh lng theo nh lut Lambert Beer.

Scan Rate Fixed Quant

.msc .mra .mfx .mqa

Scan

Rate

Fixed

Quant

Vn hnh my
Nhp cc thng s ca ch qut

Vn hnh my
- Qut mu trng bng nc ct hoc bnh Blank, ta cho mu trng vo my quang, nhn Baseline hoc Measure samples

v sau check vo mc Measure blank v nhn

Measure qut mu trng.

- Sau khi qut mu trng (my bo 100%), ta t mu tht vo v nhn Measure qut mu tht, v lu file vi ui msc. Nu xy dng ng chun, ta chn ch Quant, v thc hin cc bc sau:

Vn hnh my
- Nhp cc thng s xy dng ng chun

Vn hnh my
- Sau khi nhp cc thng s xy dng ng chun, ta nhn Measure standards v sau check vo mc Measure blank v nhn Measure o mu trng. Sau khi o mu trng (my bo 100%) , ta ln lt t cc chun t thp n cao v nhn Measure o chun, lu file vi ui mqa. o mu, ta m li file ng chun lu, t mu trng v nhn Measure sample v sau check vo mc Measure blank v nhn Measure o mu trng. Sau khi o mu trng (my bo 100%), ta ln lt t mu tht, nhp thng tin mu, nhn Measure o mu tht.

Kt lun

Nm r kin thc v k thut ng chun.

ng dng xc nh hm lng Fe2+ v Fe tng. Cch kho st bc sng cc i, xy dng ng chun. Vn hnh my o quang ph Genesye 10UV scanning v phn mm Visionlite.

Ti liu tham kho

1. 2. 3. 4. Gio trnh thc hnh phn tch ha l. Trn T Hiu(2003), Phn tch trc quang ( Ph hp th UV Vis), NXB i hc quc gia H Ni, H Ni. Http://www.google.com.vn/search Http://www. Bioblock.com