Namiesnik Jacek VN

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p dng k thut chun b mu xanh c lp,

lm giu v phn tch sc k cc nhim hu


c trong mi trng
Marcinkowski ukasz1, Spietelun Agata1,
Kloskowski Adam1, Namienik Jacek2
1Department

of Physical Chemistry, Chemical Faculty


of Analytical Chemistry, Chemical Faculty
Gdask University of Technology,
80-233 Gdansk, 11/12 G. Narutowicza St., Poland
*chemanal@pg.gda.pl

2Department

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

VAI TR CA HA PHN TCH TRONG


LNH VC KHOA HC MI TRNG
Kho st hin trng mi trng v cc qu trnh xy ra
trong mi trng
Xc nh kh nhiu nhim, thng tn ti lng vt
hay siu vt trong cc mu nn c thnh phn phc tp
v bin i.
Cn phi a vo thc nghim phn tch cc phng
php v thit b phn tch mi p ng nguyn tc pht
trin bn vng v ha hc xanh.

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

HA HC XANH

(LCH S PHT TRIN)

Vin HA HC XANH (EPA) ra i USA.


Vin thc y s hp tc gia cc c quan
nh nc v cc tp on cng nghip, s
phi hp gia cc trng v vin nghin cu,

Nhm hot ng Ha hc xanh ca IUPAC


(IUPAC Working Party on Green Chemistry)
c thnh lp.

2003

Hi ngh quc gia u tin v HA HC


XANH c t chc Balan
EkoChemTech03

1997

Hi tho quc t u tin v HA HC


XANH

1996
1995

Chng trnh Ha hc xanh c US EPA


khi xng
Hi ng Th gii v Mi trng v Pht
trin ca lin hip quc (World Commission on
Environment and Development - WCED) xut bn
Tng lai chung ca chng ta, cn c bit
vi tn Bo co Brundtland,

Gii thng hng nm cho cc thnh tu


trong lnh vc p dng cc nguyn tc ca
HA HC XANH

1991

C quan kim sot Cht c v ngn nga


nhim a ra chng trnh h tr nghin
cu c tn Tng hp thay th ngn nga
nhim

1987

Paul Anastas a ra thut ng HA HC


XANH

1993

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

11. Phn tch thi gian


thc ngn nga
nhim
10. Thit k ha cht v
sn phm c th phn
hy sau s dng

12. Gim thiu nguy c


xy ra s c

1. Trnh pht thi


2. Tng hiu sut nguyn t
trong cc qu trnh ha hc
(atom economy )
3. t tng hp ha
nguy hi

GREEN
CHEMISTRY

9. Dng xc tc

4. Ha cht v sn phm
an ton hn.
8. Trnh cc dn xut
ha hc

7. Dng nguyn
liu ti to

5. Dung mi v iu kin
phn ng an ton
6. Tng hiu qu nng
lng

Nguyn tc ca HA HC XANH
(P.T. Anastas, J. Warner, Green Chemistry.Theory and Practice,
Oxford University Press,New York, 1998, p. 30)
PRINCIPLES of GREEN CHEMICAL TECHNOLOGY
(N. Winterton, Green Chem., 3 (2001) G73)
PRINCIPLES of GREEN CHEMICAL ENGINEERING
(P.T. Anastas, J.B. Zimmerman, Environ. Sci.Technol., 37 (2003) 94A-101A.)
Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

HA HC XANH
Ha hc xanh, l s sng to, thit k v ng dng cc sn phm v
qu trnh ha hc nhm hn ch v loi b vic s dng hay to ra cc
cht nguy hi
P. T. Anastas, J. C. Warner, Green Chemistry: Theory and Praktice. Oxford Science Publications, Oxford (1998)

HA PHN TCH XANH-GAC


S dng cc k thut phn tch ha hc v cc phng php lun
nhm gim hay loi tr dung mi, thuc th, cht bo qun v cc
ha cht nguy hi cho sc khe hay mi trng, ng thi cho php
phn tch nhanh hn, tit kim nng lng hn m khng lm gim
cc tiu ch hiu nng
H. K. Lawrence, Green Analytical Methodology Curriculum
http://www.chemistshelpingchemists.org/GreenAnalyticalMethodologyCurriculum.ppt#257,2,Curriculum
Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

THE COMPONENTS OF GREEN ANALYSIS

D vn hnh, an ton

Gn nh, tn t nng lng

A. Gauszka, Z.M. Migaszewski, J. Namienik Twelve principles of green analytical chemistry


SIGNIFICANCE of green analytical practices. Trends Anal. Chem. Submitted.
Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

THE PRINCIPLES OF GAC EXPRESSED AS


TM QUAN TRNG NG GHI NHN

Chn phng php trc tip


Tch hp qu trnh phn tch v iu khin
t thi hn, nu c th th x l cn thn
Khng hao ph nng lng
T ng ha v lm phng php gn li
u tin thuc th t cc ngun c kh nng ti to
Tng tnh an ton cho ngi thc hin
Thc hin cc php o in-situ
Trnh bin tnh
S mu v lng mu cng t v nh cng tt
Chn cc phng php phn tch a cht, a bin
Thay th v loi b cc tc cht c hi
A. Gauszka, Z.M. Migaszewski, J. Namienik Twelve principles of green analytical chemistry
SIGNIFICANCE of green analytical practices. Trends Anal. Chem. Submitted.
Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

A KHI NIM PHT TRIN BN


VNG VO CC PTN PHN TCH

HA PHN TCH XANH

Tm k thut phn tch mi


Tm k thut chun b mu khng cn dungmi
Mi trng ly trch mi
Dng cht lng iontrong giai on chun b mu trc khi phn tch.
Dng nc siu ti hn lm mi trng ly trch

Cc tc ng gin tip ln cc cht


p dng visng.
p dng siu m.
p dng tia UV.

Tch hp v nhha thit b phn tch


nh gi tc ng mi trng ca cc phng th nghim v cc quy trnh
phn tch ng dng k thut nh gi vng i.
Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

CC MC NG NH TRONG HA PHN TCH XANH


1974

Pht trin pp phn tch tim dng - FIA

1974

Pht trin k thut gii - hp th (purge-and-trap) - PT

1976

Pht trin pp. chit pha rn - SPE

1978

Pht trin pp ly trch im sng (cloud point extraction CPE)

1985

Pht trin pp ly trch bng vi sng (microwave-assisted extraction MAE)


Pht trin pp ly trch cht lng siu ti hn (supercritical fluid extraction SFE)

1987

Khi nim ha hc sinh thi (H. Malissa)


Khi nim pht trin bn vng

1990

Pht trin pp vi chit pha rn (solid-phase microextraction SPME)


Pht trin H phn tch tng vi lng (micro total analysis system - TAS)

1993

Pht trin pp chit pha rn ng du phn t (molecularly imprinted solid-phase extraction- MIMSPE

1995

Khi nim ha phn tch thn thin vi mi trng (M. de la Guardia, J. Ruzicka)

1996

Pht trin pp chit p sut cao (presurized solvent extraction PSE)


Pht trin pp chit pha lng vi lng (liquid phase micro extraction LPME)
Pht trin pp chit vi lng n git (single drop microextration SDME)

1999

Khi nim ha hc xanh (P.T. Anastas)


Khi nim ha phn tch sch ( M. de la Guardia)
Khi nim ha phn tch xanh ( J. Namienik)
Pht trin pp chit hp th trn thanh khuy (stir bar sorptive extraction- SBSE)
Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

MI TRNG LY TRCH
DUNG MI XANH
Thng s

CO2 Siu ti hn

H2O Siu nng

tan ca cht c th thay i

10-100 ln

50-1000000 ln

Cc cht c th chit c

Cht phn cc

Cht khng phn cc

Cc cht c th chit d dng

Cht khng phn cc

Cht phn cc

Hot tnh ca cht cn phn tch

Thp

Thp trung bnh

Lm giu sau ly trch

usually easy

kh thay i

Ly trch chn lc cc cht vi


phn cc khc nhau

Trung bnh

tt

ly trch chn lc t cc mu vi
thnh phn mu nn cho trc
( t)

tt

Km

Khong bin thin phn cc


ca cc cht c phn tch ()

1-2

10-80

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

10

MI TRNG LY TRCH MI
DUNG MI XANH
CHT LNG ION DUNG MI CA TH K 21ST
NHNG TNH CHT HP DN V
HA HN CA CHT LNG ION
Nhng mui ny dng lng nhit phng.
Ha tan cc hp cht hu c v v c.
Bn nhit;
nht cao;
a nc/ k nc;
khng bay hi (p sut hi 25C rt thp);
dn in cao.

TNG S KT HP CATION V
ANION THEO L THUYT C TH
12
TI 10
Cho n nay bit khong 1500 CHT
LNG ION.
Mi c 500 c thng mi ha.

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

11

MI TRNG LY TRCH MI
DUNG MI XANH
Chun b mu giai on quan trng nht trong quy trnh phn tch tng th

KHNG TiN X L TRC PHN TCH GiI PHP HON HO


TUY NHIN c rt t k thut phn tch nh vy
Lm giu cht ch (cc cht cn phn tch ) v nng cao
hn gii hn pht hin ca my o/my quan trc.
C lp cht CH khi nn mu ban u hay n gin ha nn
Loi tr cc cht c nh hng v loi tr nhng thnh phn
hp ph bn ln ct sc k lm ct nhanh hng.

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

12

K THUT CHUN B MU KHNG DUNGMI


Dng dng kh tr lm mi
trng ly trch

K thut chit pha rn


kt hp vi gii hp
nhit

K thut chit bng


mng

Phn tch Ha hi tnh (S-HS)


Phn tch Ha hi ng (D-HS)
By lnh (CT)

Headspace (Ha hi)

Lm sch v by (Purge and Trap PT)


Phn tch gii loi trong ng (CLSA)
Ly trch trn gm (GPE)
Chit ng trong kim (INDEX)
By hp ph trong mao qun kim (INCAT)
Ly trch hp thu Ha hi (HHSE)
By ng h (OTT)
Chit vi lng mao qun ph (CCME)

By ng mng dy h (TFOT)
By mao qun mng dy (TFCT)
Chit hp th trn thanh khuy (SBSE)
Chit trn pha rn vi lng (SPE)
Chit vi lng trn pha rn (SPME)
Chit nano lng pha rn (SPNE)
Thit b chit pha rn quay

Khi ph mng u vo (MMS)


Chit trn mng vi b mt hp ph (MESI)
Phn tch ly mu si rng (HFSA)
Vi by cho chit mng trong dng (OLMEM)
By v gii loi trn mng (MPT)

Chit xung trn mng (PIME)


Thit b bn thm mng (SPMD)
ng dng gii hp nhit mng (TMDA)
Gii hp nhit lng k thm th ng

Chit bng cht lng


siu ti hn
K thut chit gn
nh khng dung mi

Chit pha lng vi lng dy rng (HF-LPME)


Tch / Chit mng in (EMI/EME)
Chit vi lng n git (SDME)

Rn ha git hu c tri (SFOD)


Chit vi lng Lng-Lng phn tn (DLLME)
Thit b chit pha rn quay

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

13

CHIT VI LNG N GiT


(SDME)
EXTRACTING
FORSDME
SDME
DUNG MI LYSOLVENTS
TRCH TRONG
DI-SDME

HS-SDME

IL-SDME

n -Hexane
n -Octane
iso-Octane
Cyclohexane
n -Hexadecane
Butylacetate
Diisopropyl ether

n -Octane
n -Decane
Tetradecane
Ethylene glycol
Toluene
o -Xylene
1-Octanol

BMIM PF 6
HMIM PF 6
OMIM PF6
HMIM NTf 2

Dung lng git

1 8L

chn lc cao

Gii hn pht hin thp


n gin, nhanh, d
Chun b mu nhanh gn
T ng ha nh tr gip ca cc thit b c thng mi
C kh nng p dng cho phn tch vt trong nc
G. Liu, P.K. Dasgupta, Anal. Chem. 68 (1996) 1817
Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

DI-SDME: direct immersion


HS-SDME: headspace
IL-SDME:ionic liquid-base
14

Cc ch chit SDME

CONTINOUS
FLOW
DNG LIN
TC
W. Liu, H.K. Lee, Anal. Chem., 72 (2000), 4462

LLLME
CHT

NHNG TRC TiP

HA HC

L. Xu, C. Basheer, H.K. Lee. J. Chromatog. A, 1152 (2007), 184

DROP-TO-DROP
GiT TRONG GiT

DMD-LPME

LNG
ION

Git = Mng Git - LPME

M. Ma, F.F. Cantwell, Anal. Chem.,


70 (1998), p. 3912

H.F. Wu, J.H. Yen, C.C. Chin, Anal. Chem.,


78 (2006) 1707

T. Sikanen, S. Pedersen-Bjergaard, H. Jensen, R.


Kostiainen, K. E. Rasmussen, T. Kotiaho,
Anal. Chim. Acta 658 (2010) 133

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

15

CHIT VI LNG NG C GiT HU C


TRI (SFOD/SFOME)

Tnh cht ha l ca dung mi dng


trong SFOME:
Khng trn ln vi nc
bay hi thp
T trng thp
C kh nng ly trch cht cn phn tch

Dung
mi solvents
thng dng
Common
used
in SFOME
1-Undecanol

o
Melting
point
Nhit
si( C)
13-15

1-Dodecanol

22-24

2-Dodecanol

17-18

n-Hexadecane

18

1,10-Dichlorodecane

14-16

Organic solvent

M.R.K. Zanjani, Y. Yamini, S. Shariati, J. . Jnsson, Anal. Chim.Acta, 585 (2007) 286
Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

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CHIT VI LNG PHA LNG DY


RNG (HF-LPME)
R, n gin, sch
C th t ng ha
Thch hp cho phn tch GC, HPLC, CE
chn lc v linh hot cao
Ch Ha hi/nhng
Kh nng bin tnh in-situ

HF-LPME c th c:
Ch ba pha (a)
Ch hai pha (b)

TIN B TRONG K THUT HF-LPME :


Chit vi lng Lng-Lng-Lng Mng trn
dy rng (HFM-LLLME)
Chit vi lng pha lng dy rng ng HFLPME
Fig. D. Han, K. H. Row, Microchim. Acta,176 (2012) 1

Chit vi lng pha lng dy rng ng dung


mi lnh HF-LPME (SC-DHF-LPME)

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

17

C LP MNG iN HA (EMI)
CHIT MNG iN HA (EME)

EME trn chip

S. Pedersen-Bjergaard, K.E. Rasmussen, J. Chromatogr., A 1109 (2006) 183.

M. D. Ramos Payn, H. Jensen, N. J. Petersen, S. H. Hansen, S. Pedersen-Bjergaard, Anal. Chim. Acta, 735 (2012) 46

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

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CHIT VI LNG PHN TN LNG


LNG (DLLME)

Fig. A. V. Herrera-Herrera, M. Asensio-Ramos, J. Hernndez-Borges,


M. . Rodrguez-Delgado, Trends Anal. Chem., 29 (2010) 728

R, n gin, nhanh
D thc hin
C th t ng ha
Din tch tip xc gia mu v pha nhn ln
Thch hp cho phn tch bng GC, HPLC, CE v UV-vis
ng hc ly trch nhanh
H s lm giu mu cao
M. Rezaee, Y. Assadi, M.R.M. Hosseini, E. Aghaee, F. Ahmadi, S. Berijani, J. Chromatogr., A 1116 (2006) 1.
Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

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Tin b trong chit vi lng phn tn Lng-lng


DLLME tr gip bng vi sng

DLLME tr gip bng lc xoy

DLLME tr gip bng cht hot ng b mt

DLLME gii nh tng ha bng dung mi


DLLME kt thc bng dung mi
DLLME gii nh tng ha vi dung mi t trng thp
DLLME tim tun t
Dung mi ly trch mi
DUNG MI LY TRCH NHE HN NC
THIT B LY TRCH CHUYN DNG T CH TO

DLLME GiT HU C TRI RN


CHT LNG ION
CHIT VI LNG DA TRN KT TP LNH (CIAME)
CHIT VI LNG TO DUNG MI IN SITU (ISFME)

DLLME CHT LNG ION KiM SOT NHIT (TILDLME)


GiT T V MIXEN O

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

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THIT B CHIT PHA LNG QUAY

Hollow Fiber Solid-Liquid Phase Microextraction (HFSLPME)

Stir Membrane liquidliquid microextraction


(SM-LLME)

Z. Eshaghi, M. A.-K. Khooni, T. Heidari,


Spectrochim. Acta Part A, 79 (2011) 603

M. C. Alcudia-Len, R. Lucena, S. Crdenas, M. Valcrcel,


Anal. Chem., 81 (2009) 8957

Dual Solvent Stir Bars Microextraction


(DSSBME)
C. Yu, Q. Liu, L. Lan, B. Hu, J. Chromatogr. A, 1188 (2008) 124

Solvent Bar Microextraction


(SBME)
X. Jiang, H. K. Lee, Anal. Chem., 76 (2004) 5591

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

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THIT B CHIT PHA LNG QUAY

Modes:
bar adsorptive - extraction (BaE)
multi-spheres adsorptive -extraction (MSAE)

Stir cake sorptive extraction (SCSE)


X. Huang, L. Chen, F Lin, D. Yuan, J. Sep. Sci., 34 (2011) 2145

Adsorptive -extraction (AE)


N.R. Neng, A.R.M. Silva, J.M.F. Nogueira, J.Chromatogr. A, 1217 (2010) 7303

Rotating disk sorbent extraction (RDSE)


P. Richter, C. Leiva, C. Choque, A. Giordano, B. Sepulveda,
J. Chromatogr. A, 1216 (2009) 8598

Stir rod sorptive extraction (SRSE)


Y. B. Luo, Q. Ma, Y. Q. Feng, J. Chromatogr. A, 1217 (2010) 3583.

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

22

CHIT HP THU THANH KHUY


(SBSE)
Nhanh, n gin, khng dung mi

Ly trch nhy v hiu qu


Thch hp cho phn tch bng GC, HPLC, CE
Ch Ha hi v Nhng trc tip
Nhit v ha hc ca lp ph thanh khuy n nh
Tin b trong k thut SBSE:
p dng mt xp poliurethane, PPESK, alkyl-diolsilica
RAM, vt liu silica, lp ph phn t ng du, k thut
monoliths (nguyn khi) v sol-gel ch to lp ph
thanh khuy.
Lp ph thanh khuy nh pha
E. Baltussen, H. G. Janssen, P. Sandra, C. A. Cramers, J. High. Resolut. Chromatogr., 20 (1997) 385
Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

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Chit pha rn vi lng (SPE)


R, n gin, sch
D p dng
D thao tc
Thch hp cho phn tch GC, HPLC
Ch Ha hi v Nhng
nhy m bo
lp li tt
lm giu tuyt vi

Tin b trong k thut (SPE) :


ng dng ti giy gn, si composite polyaniline-nylon-6
(PANI-N6) v si polypyrrole-polyamide (PP-PA) iu ch
bng phng php spin in ha ch to tm hp thu.

C. Basheer, A. A. Alnedhary,B. S. M. Rao, S. Valliyaveettil, H. K. Lee, Anal. Chem., 78 (2006) 2853


Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

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ng dng ht nano trong k thut ly trch quy


m nano
THY TINH KCH THC
MICRO VI HT NANO Au

MU NC

LC V LYTM

THUKT TA

THM DUNGMI

LC V LYTM

LY TH NI TRN MT

HPLC

LETRESS

PHNG N I
H. Wang, A. D. Campiglia, Anal. Chem., 80 (2008) 8202

PHNG N II
Y. Zhu, S. Zhang, Y. Tang, M. Guo, C. Jin, T. Qi,
J Solid State Electrochem, 14 (2010) 1609.

ChiT nano pha rn (SPNE)


H. Wang, A. D. Campiglia, Anal. Chem., 80 (2008) 8202
Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

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CHIT VI LNG PHA RN


(SPME)
Thao tc n gin
Thi gian ly trch v gii hp ngn
Hon ton khng dung mi
Kch thc rt nh (tin thit k thit b bn)
C th hon ton t ng ha
Kt ni trc tip vi GC
Kh nng ly mu in-situ v in-vivo
Ch Nhng trc tip hay Ha hi
1.
2.
3.
4.
5.

u trn
ng rng
Bao kim
Kim trong
Dy silica ph nng

C. L. Arthur, J. Pawliszyn, Anal. Chem., 62 (1990) 2145


Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

26

CC MC PHT TRIN
PHNG PHP SPME
SPME Ha hi
(HS-SPME)

SPME MNG
(M-SPME)

SPME LNH TRN SI PH


(CCF-SPME)

SPME DY TRONG NG
SPME SI TRONG NG

SPME TRONG NG

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

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TiN B TRONG K THUT


SPME
T NG
PHA LY TRCH MI
CHT LNG ION
CARBON NANOTUBES V GRAPHEN
SILICA CU TRC MICRO
THIT B MI V CC CI TiN
SPME MNG
CHIT VI LNG LNG-LNG-RN
SPME GIA TC BNG iN HP PH
Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

28

SI CHO SPME TRN TH TRNG


HP TH

t la chn

C th c s phn hy

Gii hp khng hon ton


Tng tc xc tc gia cht hp th v
cht b bt gi

chn lc km cho
cht phn cc
kh nng cnh tranh chim cc tm hp ph
gia cc cht nn v cht ch

HP PH

Cn nhit cao gii hp cc cht kh bay


hi

Nhit gii hp thp

S phn hy cht cn phn tch


Xc tin, xc tc s phn r cc cht ch
c bt gi

Cht b bt ha tan trong pha hp phu


Cht b bt gi khng b phn hy
Khng c tng tc c bit gia cht
b bt gi v pha hp ph
analyte and sorbent

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

29

CHIT VI LNG LNG-LNG-RN

n gin
chi ph thp rt hp dn
thn thin vi mi trng
lng dung mi khng ng k
hiu nng cao
x l chn lc v nhy
Y. Hu, Y. Wang, Y. Hu, G. Li, J. Chromatogr. A, 1216 (2009) 8304
Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

30

SPME HP PH iN HA GIA TNG


(EE-SPME)

n gin, nhanh, nhy


Hiu sut tt
Thi gian hp ph ngn
Khong tuyn tnh ln
LOD thp
phc hi cao

Q. Li, Y. Ding, D. Yuan, Talanta 85 (2011) 1148

Phng php ly trch vi in cc lm vic ph ht nano c


bit vi tn:
LY TRCH NANO PHA RN iN HA
X. Chai, Y. He, D. Ying, J. Jia, T. Sun, J. Chromatogr. A, 1165 (2007) 26 Y. Zhu, S. Zhang, Y. Tang, M. Guo, C. Jin, T. Qi, J. Solid State Electrochem, 14 (2010) 1609.

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

31

SPME TRN MNG (M-SPME)

1) Dy silica
2) Lp ph polyethylene glycol (PEG)
3) Lp ph polydimethylsiloxane (PDMS)
Vt liu hp ph
B dy trung bnh ca lp ph
Chiu di lp ph
Vai tr ca lp ph cht hp ph

Lp ph trong
PEG
40-50m
1cm
Mi trng bt gi
cht rt phn cc

Lp ph ngoi
PDMS
100-110m
1,2 cm
K nc, mng khng
phn cc

A. Kloskowski, M. Pilarczyk, J. Namienik, Anal. Chem., 81 (2009) 7363.


Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

32

U iM CA SPME TRN MNG


Chi ph cho dy rt thp
bn nhit cao (PDMS bn cho n 300oC)
thi gian ly trch v gii hp ngn
nc khng b hp thu (nh lp mng k nc)
i lc cao vi hp cht phn cc
nhit ly trch, PEG phn t lng thp hot ng nh l
cht lng b c nh (polymer lng nht)

Cht cn phn tch b bt gi nh ha tan vo lp hp ph


Bn cht hp ph ca s bt gi
C ch phn tch ca qu trnh gii hp
Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

33

Xc nh phenols
Bng SPME mng v GC
Khong
tuyn tnh
(g/L)

R2

15-1500

2-Chlorophenol

Hp cht

LOD (g/L)
M-SPME

PA

0.9953

50

3-300

0.9936

43

530

2,4-Dichlorophenol

3-300

0.9987

15

120

2,4-Dimethylphenol

3-300

0.9921

110

2,4-Dinitrophenol

10-1000

0.9963

110

950

2-Methyl-4,6-dinitrophenol

15-1500

0.9898

81

680

2-Nitrophenol

3-300

0.9945

60

4-Nitrophenol

15-1500

0.9937

150

1800

Pentachlorophenol

15-1500

0.9914

83

740

2,4,6-Trichlorophenol

10-1000

0.9932

61

440

4-Chloro-3-methylphenol

A. Kloskowski, M. Pilarczyk, J. Namienik, Anal. Chem., 81 (2009) 7363

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

34

Xc nh VOCs
Bng SPME mng v GC
R2
Compound
chlorobenzene
p-xylene
o-xylene
isopropylbenzene
n-propylbenzene
2-chlorotoluene
4-chlorotoluene
t-butylbenzene
sec-butylbenzene
1,3-dichlorobenzene
1,4-dichlorobenzene
1,2-dichlorobenzene

LOD (mg/L)

RSD (%)

M-SPME

DVB/CAR
/PDMS

M-SPME

DVB/CAR
/PDMS

M-SPME

DVB/CAR
/PDMS

0.997
0.992
0.986
0.994
0.998
0.997
0.995
0.997
0.987
0.989
0.994
0.986

0.994
0.986
0.994
0.995
0.997
0.993
0.995
0.985
0.992
0.998
0.987
0.988

0.031
0.022
0.018
0.015
0.013
0.016
0.017
0.011
0.011
0.017
0.017
0.016

0.016
0.015
0.014
0.018
0.017
0.019
0.018
0.021
0.021
0.017
0.023
0.028

11
9
12
12
14
8
10
12
11
14
13
13

9
6
7
8
10
6
6
8
8
10
7
7

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

35

Kt lun v SPME mng


C ch phn tch ca qu trnh chit c trng bi khong tuyn tnh ln hn so vi cc
si ly trch trn th trng.
Cho php dng cc cht hp ph phn cc mnh m khng c nguy c tan vo nn mu
phn cc
Cho c hi ng dng cc vt liu hon ton mi m cho n nay khng c ch ti do
c nhit nng chy thp hay tan trong nc
Hiu sut ly trch cao phenols v VOCs bng ly trch vi lng pha rn mng trn dy,
bng v cao hn so vi dng dy c trn th trng

M-SPME kt hp vi GC c th tr thnh cng c hu


hiu v thn thin vi mi trng ly mu, c lp v
lm giu cc nhim hu c.
c th p dng trong giai on chun b mu c nng
ppb trc bc nh lng cui cng.

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

36

NH GI TC NG MI TRNG CA CC
QUY TRNH PHN TCH
CNG C:
nh gi vng i (LCA)1
Quy m sinh thi 2
Phm vi sinh thi 3
Consoli, F., D. Allen, R. Weston, I. Boustead, J. Fava, W. Franklin, A. Jensen, N. de Oude, R.
Parrish, R. Perriman, D. Postlethwaite, B. Quay, J. Sguin and B. Vigon., Guidelines for life cycle
assessment: A Code of practice. SETAC, Brussels and Pensacola, 1993.
1

Aken K., L. Strekowski, L. Patiny, EcoScale, a semi-quantitative tool to select an organic


preparation based on economical and ecological parameters, Beilstein J. Org. Chem. 2, 3, 2006.

3 Home

Sustainability Assessment, http://www.ecocompass.com.au/

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

37

QUY M SINH THI CA


PHNG PHP PHN TCH
Cng c mi nh gi xanh ca ca phng php phn tch
Quy m sinh thi = 100 tng s im pht
Kt qu c nh gi nh sau:
>75 phn tch xanh tt
>50 phn tch xanh chp nhn c
<50 khng t phn tch xanh
im pht c cho da trn lng cht, ri ro (vt l, mi trng, sc khe v ngh
nghip), nng lng tiu hao v cht thi trong mt qu trnh phn tch.

Gauszka A., Konieczka P., Migaszewski Z.M., Namienik J. 2012. Analytical Eco-Scale for assessing the greenness of analytical procedures.
Trends in Analytical Chemistry 37, 6172.

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

38

IM PHT (PPS) TRONG TNH QUY M SINH THI


TC CHT

Lng
Ri ro (vt l, mi trng,
sc khe v ngh nghip)

im pht con
1
2
3
0
1
2

<10 mL (g)
10-100 mL (g)
>100 mL (g)
Khng
t ri ro
Ri ro

im pht tng
Amount
PPHazard
PP

THIT B
Nng lng

Ri ro ngh nghip

Cht thi

0.1 kWh / mu

1.5 kWh kWh / mu

>1.5 kWh kWh / mu

H thng phn tch kn

Thi hi v kh vo khng kh

Khng

<1 mL (g)

1-10 mL (g)

>10 mL (g)

Ti ch
Phn hy
Th ng ha
Khng x l

0
1
2
3

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

39

B MN HA PHN TCH
KHOA HA
I HC CNG NGH GDANSK
Department of
Analytical Chemistry

C th tm bi ging ny a ch
http://www.pg.gda.pl/chem/Katedry/Analityczna/analit.html

Analytica Vietnam , 17-19.04.2013, Ho Chi Minh City

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EUROPEAN MASTER IN QUALITY


IN ANALYTICAL LABORATORIES- EMQAL

http://eacea.ec.europa.eu/erasmus_mundus/
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MODAS
Sn xut v chng thc cc vt liu mi quan trng c
bit cc phng th nghim ca Balan t chng
nhn ca chu u MODAS

http://www.pg.gda.pl/chem/modas/

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43
43

MEMBERS OF MY RESEARCH GROUP

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THANK YOU FOR YOUR ATTENTION!

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