thuc hanh ky thuat duong chuan

8/7/2019 thuc hanh ky thuat duong chuan

1/31

Nhm thc hin : Nhm 01

GVHD : Th.s Trn Nguyn An Sa


2/31

Ni dung

1. Tng quan k thut ng chun

2. 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


3/31

K thut ng chun


4/31

1. u im

- Vi mt ng chun cho php phn tch hng lot munn nhanh v hiu qu kinh t.

2. 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.

u v nhc im


5/31

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

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 ttcho 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 dntrong 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.


6/31

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

Phc [Fe(Phen)3]2+ bn c max 508nm, cng mukhng 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+

Nguyn tc


7/31

- Nhng cht oxi ha mnh: CN-, NO2-, PO43-

- Zinc vi hm lng ln hn st 10 ln

- Copper ln hn 5ppm

- Niken ln hn 2ppm

- Bitmut,thy ngn, molybdate, bc kt ta viphenanthroline (thm mt lng tha phenanthroline)

- Cht hu c (un si mu nhiu gi vi HCl 1:1trong ccs, khi mu cn, t nh, phn tro cn li ha tan bngaxit).

Cc cht gy cn nhiu


8/31

Ho cht

1. Dung dch chun gc 1000 ppm Fe2+.

2. Dung dch chun Fe2+ 50ppm

3. Dung dch Fe2+ 15ppm

g10p

100

M

MCVm 6

i

Mppm

ml vvvv!

Ht 2.5 ml du g dchchu gc Fe2+ 1000ppmV b h h mc 50ml

h mc b gc ct 50ml

Ht 0.75 ml du g dchchu gc Fe2+ 1000ppmV b h h mc 50ml

h mc b gc ct

50ml


9/31

4. Dung dch Fe3+ 15ppm

5. Dung dch NH2OH 10% pha trong nc.

6. m axetat pH = 5.

7. Dung dch 1,10 phenanthroline 0.5% pha trong nc.

Ho cht

Ht 0.75 ml dung dchchun gc Fe3+ 1000ppmVo bnh nh mc 50ml

nh mc bngnc ct

50ml


10/31

Bnh nh mc 50ml 10

Pipet 10ml 02

Cuvet nha 01

My quang ph 01

Bnh tia 01

Bp cao su 01

Beaker 100ml 01

Dng c - thit b

My quang ph Genesye 10UV scanning


11/31

Cch tin hnh

1. Qut ph v xy dng ng chun.

2. Hiu sut thu hi ca phng php.

3. Kim tra mu th.

4. Vn hnh thit b.


12/31

Bnh s 1 2 3 4 5 6

VFe 50ppm (ml) 0 1.0 2.0 3.0 4.0 5.0

Hydroxylamin (ml) 2.0

Dung dch m pH = 5 (ml) 10.0

1,10- phenanthroline 2.0

nh mc bng nc ct n vch 50ml

Qut ph v xy dng ng chun


13/31

Qut ph v xy dng ng chun


14/31

Bnh s 1 2 3 4 5 6 7

V_dd B 10 10 10

V_ dd C 10 10 10

Hydroxylamin 2.0 0.0 2.0

yn 10 pht


1,10- phenanthroline (ml) 2.0


Hiu sut thu hi ca phng php


15/31

Bnh s 1 2 3 4 5 6 7

V_ddA (ml) 10 10 10 10 10 10

Hydroxylamin (ml) 2.0 0.0 2.0

yn 10 pht


1,10- phenanthroline (ml) 2.0


Kim tra mu


16/31

Vn hnh my


17/31

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 - Kinetics

- Standard curve - Scanning

- Absorbance Ratio - 3-point Net

- Absorbance Difference - Mulatiwavelength- Performance Validation

Vn hnh my


18/31

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


19/31

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 ccbc sau:

Vn hnh my


20/31

Phn mm gm 4 module:

Scan : Ghi nhn ph.

Rate :

Fixed : Ghi nhn s hp thca mu ti mt im ca

mt bc sng.

Quant : nh lng theo nhlut Lambert Beer.

Scan .msc

Rate .mra

Fixed .mfx

Quant .mqa

Vn hnh my


21/31

Scan


22/31

Rate


23/31

Fixed


24/31

Quant


25/31

Vn hnh my

Nhp cc thng s ca ch qut


26/31

- Qut mu trng bng nc ct hoc bnh Blank, ta cho mutrng 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 hincc bc sau:

Vn hnh my


27/31

Vn hnh my

- Nhp cc thng s xy dng ng chun


28/31

- 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 viui 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. Saukhi o mu trng (my bo 100%), ta ln lt t mu tht,

nhp thng tin mu, nhn Measure o mu tht.

Vn hnh my


29/31

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.


30/31

Ti liu tham kho

1. Gio trnh thc hnh phn tch ha l.2. Trn T Hiu(2003), Phn tch trc quang ( Ph hp th UV

Vis), NXB i hc quc gia H Ni, H Ni.

3. Http://www.google.com.vn/search

4. Http://www. Bioblock.com


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