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Application of green sample preparation techniques for the isolation, preconcentration

and gas chromatographic determination of organic environmental pollutants

Spietelun Agata 1 , Marcinkowski Łukasz 1 , Kloskowski Adam 1 , Namieśnik Jacek 2

1

Department of Physical Chemistry, Chemical Faculty

2

Department of Analytical Chemistry, Chemical Faculty Gdańsk University of Technology,

80-233 Gdansk, 11/12 G. Narutowicza St., Poland

*chemanal@pg.gda.pl

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accurately monitoring the state of the environment and the processes taking place in it

determining an wide range of analytes, often present in trace and ultratrace amounts in sample matrices with complex or variable compositions

need to introduce to analytical practice new

methodologies and equipment in order to comply with the principles of sustainable development and green chemistry

FURTHER CHALLENGES

OF ANALYTICAL CHEMISTRY

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2003

1997

1996

1995

1993 1991 1987

Office of Pollution Prevention and Toxics launched a research grants program called Alternative Synthetic Pathways for Pollution Prevention

Paul Anastas coined the term GREEN CHEMISTRY

an annual award was established for

achievements in the application of GREEN CHEMISTRY principles

IUPAC Working Party on Green Chemistry founded

the GREEN CHEMISTRY INSTITUTE (EPA) came into being in the USA. It fosters contacts between governmental agencies and industrial corporations on the one hand, and university research centres on the other

the first international GREEN CHEMISTRY symposium took place

the first national conference devoted to GREEN CHEMISTRY took place in Poland – EkoChemTech’03

GREEN CHEMISTRY (SHORT HISTORY)

Our Common Future, also known as the Brundtland Report, from the United Nations World Commission on Environment and Development (WCED) was published

Green Chemistry Program was inaugurated

by the US EPA

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PRINCIPLES of GREEN CHEMISTRY (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.)

GREEN CHEMISTRY

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GREEN CHEMISTRY

GREEN ANALYTICAL CHEMISTRY-GAC

‘The use of analytical chemistry techniques and methodologies that reduce or eliminate solvents, reagents, preservatives, and other chemicals that are hazardous to human health or the environment and

that also may enable faster and more energy efficient analyses without compromising required performance criteria’

H. K. Lawrence, Green Analytical Methodology Curriculum

http://www.chemistshelpingchemists.org/GreenAnalyticalMethodologyCurriculum.ppt#257,2,Curriculum

‘Green chemistry, is the invention, design and application of chemical products and processes to reduce or to eliminate the use and

generation of hazardous substances’

P. T. Anastas, J. C. Warner, Green Chemistry: Theory and Praktice. Oxford Science Publications, Oxford (1998)

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 Potentiometric techniques (ion-selective electrodes- ISE)

 Flameless atomic absorption spectrometry (FAAS)

 Inductively coupled plasma emission spectrometry (ICP)

 Neutron activation analysis (NAA)

 X-ray fluorescence spectrometry (XRF)

 Surface analysis techniques (AES, ESCA, SIMS, ISS)

 Immunoassay (IMA)

KNOWN TYPES OF DIRECT

TECHNIQUES OF MEASUREMENT

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1974 Development of flow injection analysis - FIA 1974 Development of purge-and-trap technique - PT 1976 Development of solid phase extraction - SPE 1978 Development of cloud point extraction - CPE

1985 Development of microwave-assisted extraction - MAE Development of supercritical fluid extraction - SFE 1987 The concept of ecological chemistry (H. Malissa)

The concept of sustainable development

1990 Development of solid-phase microextraction - SPME Development of micro total analysis system - µTAS

1993 Development of molecularly imprinted solid-phase extraction - MIMSPE

1995 The concept of environmentally friendly analytical chemistry (M. de la Guardia, J. Ruzicka) 1996 Development of presurized solvent extraction - PSE

Development of liquid phase micro extraction - LPME Development of single drop microextration -SDME 1999 The concept of green chemistry (P.T. Anastas)

The concept of clean analytical method ( M. de la Guardia) The concept of green analytical chemistry ( J. Namieśnik)

Development of stir bar sorptive extraction- SBSE

MILESTONES IN GREEN ANALYTICAL CHEMISTRY

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NEW EXTRACTION MEDIA GREEN SOLVENTS

Parameter Supercritical CO

2

Supercritical H

2

O Analyte solubility can be changed 10-100 times 50-1000000 times

Extractable analytes polar constituents non-polar constituents Easily extractable analytes non-polar constituents polar constituents

Analyte reactivity low low-average

Analyte preconcentration

(after extraction) usually easy variable level of difficulty Selectivity of extraction of analytes

of different polarity average good

Selectivity of extraction from samples with a given matrix composition

(e.g. soils)

good poor

Range of analyte polarity(ε) 1-2 10-80

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NEW EXTRACTION MEDIA GREEN SOLVENTS

IONIC LIQUIDS – SOLVENTS OF THE 21 ST CENTURY

IS are salts containing:

• an organic cation

• an anion (usually inorganic) Terminology

• Room-temperature ionic liquid

• Task specific ionic liquid

• Neoteric solvents

• Non-aqueous ionic liquid

• Molten organic salt

• Fused salt

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at room temperature these salts are liquids

• dissolve organic and inorganic compounds

• thermally stable

• high viscosity

• usually immiscible with water

• non-volatile (very low vapour pressure at 25°C)

• high electrical conductance, wide electrochemical windows

• dissolve catalysts, especially complexes of transition metals without damaging the walls of glass or steel reactors

INTERESTING AND PROMISING

PROPERTIES OF IONIC LIQUIDS

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SOLVENT-FREE SAMPLE PREPARATION TECHNIQUES

preconcentration of the analytes to a level above

the limit of detection of the measuring/monitoring instrument isolating the analytes from the original sample matrix

and/or matrix simplification

removal of interferents and elimination of sample constituents being strongly adsorbed in the chromatographic column

and thus accelerating its consumption

Sample preparation - most critical step of the whole analytical protocole

NO SAMPLE PRETREATMENT BEFORE ANALYSIS NECESSARY AN IDEAL SOLUTION

BUT only a limited number of such techniques!

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CLASSIFICATION OF SOLVENT-FREE SAMPLE PREPARATION TECHNIQUES

Application of stream of inert gas as extractant

Static Headspace analysis (S-HS) Dynamic Headspace (D-HS) Cryotrapping (CT)

Solid phase extraction techniques with thermal desorption:

Purge and Trap (PT)

Closed Loop Stripping Analysis (CLSA) Gum-Phase Extraction (GPE)

Inside Needle Dynamic Extraction (INDEX) Inside Needle Capillary Absorption Trap (INCAT) Stir Bar Sorptive Extraction (SBSE)

Headspace Sorptive Extraction (HHSE) Open-Tubular Trapping (OTT)

Coated Capillary Microextraction (CCME) Thick Film Open Tabular Trap (TFOT) Thick Film Capillary Trap (TFCT) Solid-Phase Microextraction (SPME

)

Membrane extraction techniques

Membrane Inlet Mass Spectrometry (MMS)

Membrane Extraction with Sorbent Interface (MESI) Hollow Fibre Sampling Analysis (HFSA)

On-line Membrane Extraction Microtrap (OLMEM) Membrane Purge and Trap (MPT)

Pulse Introduction Membrane Extraction (PIME) Semi Permeable Membrane Devices (SPMD) Thermal Membrane Desorption Application (TMDA) Passive permeation dosimeters+thermal desorption

Supercritical Fluid Extraction

SOLVENT-FREE SAMPLE PREPARATION TECHNIQUES

C. W. Huie, Anal. Bioanal. Chem. 373, (2002), 23.

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Liquid phase microextraction techniques:

• SDME (Single Drop Microextraction)

• HF-LPME (Hollow Fibre Liquid-Phase Microextraction)

• DLLME (Dispersive Liquid-Liquid Microextraction)

• SM-LLME (Stir Membrane Liquid–Liquid Microextraction) Solid phase microextraction techniques:

• SBSE (Stir Bar Sorptive Extraction)

• μSPE (Micro Solid-Phase Extraction)

• AμE (Adsorptive μ-Extraction)

• SCSE (Stir Cake Sorptive Extraction)

• SPNE (Solid-Phase Nano-Extraction)

• SPME (Solid-Phase Microextraction)

MICROEXTRACTION TECHNIQUES

C. W. Huie, Anal. Bioanal. Chem. 373, (2002), 23.

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SINGLE DROP MICROEXTRACTION (SDME)

• High selectivity

• Low detection limits

• Simple, fast, and easy

• Minimal sample preparation

• Can be automated with commercially available equipment

• Possible application for trace water analysis

HMIM PF

6

OMIM PF

6

HMIM NTf

2

DI-SDME HS-SDME

n -Hexane n -Octane

EXTRACTING SOLVENTS FOR SDME IL-SDME BMIM PF

6

n -Octane iso-Octane Cyclohexane n -Hexadecane

n -Decane Tetradecane Ethylene glycol

Butylacetate Diisopropyl ether

Toluene o -Xylene 1-Octanol

Drop volume 1 – 8L

G. Liu, P.K. Dasgupta, Anal. Chem. 68 (1996) 1817

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Fig. D. Han, K. H. Row, Microchim. Acta,176 (2012) 1

HF-LPME may be accomplished in:

• three-phase mode (a)

• two-phase mode (b)

HOLLOW FIBER LIQUD-PHASE MICROEXTRACTION

(HF-LPME)

Inexpensive, simple, clean-up

Possibility of automation

Compatible with GC, HPLC, CE

High versatility and selectivity

Headspace/immersion mode

Possibility of n-situ derivatization

S. Pedersen-Bjergaard, K.E. Rasmussen, Anal. Chem. 71 (1999) 2650.

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ADVANCES IN HF-LPME TECHNIQUE

 Hollow Fiber-Protected Ionic Liquid supported three-phase (Liquid–Liquid–Liquid) Microextraction (HFM-LLLME)

 Hollow Fiber Solid–Liquid Phase Microextraction (HF-SLPME)

 Solvent Stir Bar Microextraction (SSBME)

 dynamic-HF-LPME

 Solvent Cooling Assisted Dynamic HF-LPME (SC-DHF-LPME)

 Electro Membrane Extraction (EME)

 on-chip EME

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CONTINOUS FLOW

LLLME DROP-TO-DROP

DI-SDME HS-SDME

SDME MODES

W. Liu, H.K. Lee, Anal. Chem., 72 (2000), 4462 L. Xu, C. Basheer, H.K. Lee. J. Chromatog. A, 1152 (2007), 184

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DROPLET-MEMBRANE-DROPLET-LPME (DMD-LPME)

• Reasonably high selectivity

• Cheap (commercial propylene membrane)

• No gluing or clamping process

• Simple and easy

• Minimal sample preparation

T. Sikanen, S. Pedersen-Bjergaard, H. Jensen, R. Kostiainen, K. E. Rasmussen, T. Kotiaho, Anal. Chim. Acta 658 (2010) 133

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SOLIDIFICATION OF FLOATING ORGANIC DROP MICROEXTRACTION

(SFOD/SFOME)

Physical and chemical properties of solvents for SFOME:

• immiscible with water

• low volatility

• low density

• able to extract analytes

1,10-Dichlorodecane

13-15 22-24 17-18 18 14-16 1-Undecanol

1-Dodecanol 2-Dodecanol n-Hexadecane

Common used solvents in SFOME

Organic solvent Melting point (oC)

M.R.K. Zanjani, Y. Yamini, S. Shariati, J.Å . Jönsson, Anal. Chim.Acta, 585 (2007) 286

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ELECTRO MEMBRANE ISOLATION (EMI)

ELECTRO MEMBRANE EXTRACTION (EME)

On chip- EME

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

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

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DISPERSIVE LIQUD-LIQUID MICROEXTRACTION

(DLLME)

Fig. A. V. Herrera-Herrera, M. Asensio-Ramos, J. Hernández-Borges, M. Á. Rodríguez-Delgado, Trends Anal. Chem., 29 (2010) 728

Inexpensive, simple, fast

Easy to operate

Possibility of automation

Enormous contact area between acceptor phase and sample

Compatible with GC, HPLC, CE, UV-vis spectrometry

Fast extraction kinetics

High enrichment factor obtained

M. Rezaee, Y. Assadi, M.R.M. Hosseini, E. Aghaee, F. Ahmadi, S. Berijani, J. Chromatogr., A 1116 (2006) 1.

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ADVANCES IN DLLME TECHNIQUE

SOLVENT DEMULSIFICATION DLLME

NEW EXTRACTION SOLVENTS

SOLVENT TERMINATED- DLLME

EXTRACTION SOLVENT LIGHTER THAN WATER

IONIC LIQUID

SPECIAL HOME-MADE EXTRACTION DEVICES

DLLME BASED ON THE SOLIDIFICATION OF A FLOATING ORGANIC DROP

COLD- INDUCED AGGREGATION MICROEXTRACTION (CIAME) IN SITU SOLVENT-FORMATION

MICROEXTRACTION (ISFME) TEMPERATURE-CONTROLLED IONIC LIQUID

EXHAUSTIVELY DLLME (TILDLME) SEQUENTIAL INJECTION–DLLME

LOW-DENSITY SOLVENT-BASED SOLVENT DEMULSIFICATION-DLLME

SURFACTANT-ASSISTED DLLME

COACERVATES AND REVERSE MICELLES ULTRASOUND ASSISTED DLLME

VORTEX-ASSISTED DLLME

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STIR BAR SORTPIVE EXTRACTION (SBSE)

Advances in SBSE technique:

 Application of poliurethane foams, PPESK, alkyl-diolsilica RAM, silica materials,

molecularly imprinted coatings, monoliths

and sol-gel technique to prepare of stir bar coatings

 Double-phase stir bar coatings

 Rapid, simple, solvent-free

Sensitive and effective extraction

Compatible with GC, HPLC, CE

Headspace and immersion modes

High thermal and chemical stability of stir bar coatings

E. Baltussen, H. G. Janssen, P. Sandra, C. A. Cramers, J. High. Resolut. Chromatogr., 20 (1997) 385

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STIR „CAKE” SORPTIVE EXTRACTION (SCSE)

Combines the advantages of stirring with the high absorption capacity of the monolithic material

high availability

preparation simplicity

low cost

excellent longevity of monolithic cakes (lifetime more than 1000h)

very versatile approach, broad applicability

good extraction results

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

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MICRO SOLID-PHASE EXTRACTION (µSPE)

Advances in (µSPE) technique:

 Application of mulberry paper bag, electrospun composite of polyaniline-nylon-6 (PANI-N6)

and electrospun composite of polypyrrole-polyamide (PP-PA) as sorbent sheet

 Inexpensive, simple, clean-up

Conveniently applicable

Easy to be manipulated

Compatible with GC, HPLC

Headspace and immersion modes

Sufficient sensitivity,

Good reproducibility

Excellent enrichment

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

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ADSORPTIVE μ-EXTRACTION (AμE)

Modes:

•bar adsorptive μ- extraction (BaμE)

•multi-spheres adsorptive μ-extraction (MSAμE)

cost-effective

easy to work-up

devices are easy to prepare

robustness and good μ-extraction efficiency

demonstrating to be a remarkable analytical tool for trace analysis

presents the advantage to tune the most suitable sorbent to each specific type of application

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

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APPLICATION OF NANOPARTICLES IN NANOEXTRACTION TECHNIQUES

VARIANT I VARIANT II

WATER SAMPLE MICRO-PLANE GLASS

WITH Au NPs

SHAKING AND CENTRIFUGATION

COLLECT PRECIPITATE

SOLVENT ADDITION

SHAKING AND CENTRIFUGATION

SUPERNATANT COLLECTION

HPLC LETRESS

H. Wang, A. D. Campiglia, Anal. Chem., 80 (2008) 8202 Y. Zhu, S. Zhang, Y. Tang, M. Guo, C. Jin, T. Qi, J Solid State Electrochem, 14 (2010) 1609.

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SOLID PHASE MICROEXTRACTION (SPME)

1. Plunger 2. Barrel

3. Injection needle 4. Inner needle

5. Coated fused silica fiber

 simplicity of operation

 short extraction and desorption time

solvent-free operation

 small size (convenient for designing portable devices)

 possibility of full automation

 direct linkup with a GC

possibility to in-situ and in-vivo sampling

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

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1. direct-immersion SPME 2. headspace-SPME

PRINCIPLES OF SPME

Operation steps:

1. Immersion of the needle in the sample 2. Exposition of the fiber

3. Extraction of an analytes 4. Retraction of the fiber

5. Introduction of the fiber to injection port

6. Desorption of analytes

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MILESTONES IN THE DEVELOPMENT OF SPME

SOLID PHASE MICROEXTRACTION (SPME) first paper on concept of SPME 1990 HEADSPACE SPME (HS-SPME) - Analytes are sampled from headspace above the sample,

particularly useful for analysing the composition of solid samples or samples containing matrix constituents and in the extraction of very volatile analytes

1993

COOLED COATED FIBRE SPME (CCF-SPME) - approach improving extraction efficiency by heating the sample and simultaneously cooling the SPME fiber. The temperature is easily controlled by cooling the fibre coating from the inside with a coolant and by altering the core diameter of the arrangement

1995

IN-TUBE SPME - the extraction phase is immobilized as the inner coating of the needle or part of the chromatographic column. Analytes are retained in the extraction medium during a few draw/eject cycles of the sample, or extraction takes place following a one-off filling of the needle

1997

FIBRE-IN-TUBE SPME - polymer core is inserted into the capillary of the in-tube SPME

arrangement. The core reduces the capillary volume, but the surface area of the sorbent is not reduced

2000

SOLID-PHASE AROMA CONCENTRATE EXTRACTION (SPACE) - the SPACE rod is fabricated from stainless steel coated with an adsorbent mixture (mainly of graphite carbon) fixed on the head of a closed flask, where it adsorbs the aroma for a given time

2004

MEMBRANE-SPME (M-SPME) - physical separation of the two phases with a membrane impermeable to both of them or by immobilization of the extracting agent in the

membrane pores

2009

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ADVANCES IN SPME TECHNIQUE

AUTOMATION

NEW EXTRACTION PHASE

NEW DEVICES AND MODIFICATIONS

IONIC LIQUIDS

CARBON NANOTUBES AND GRAPHEN

SILICA MICROSTRUCTURES

MEMBRANE-SPME LIQUID-LIQUID-SOLID

MICROEXTRACTION

ELECTROSORPTION ENHANCED-SPME

(33)

COMMERCIAL SPME FIBERS

 limited choice

 high cost

 poor selectivity for polar analytes

 some fiber coating have active adsorption centers- possibility of competing of the matrix compounds with the analytes for available adsorbent sites

 need to high temperatures to be used to desorb the less

volatile compounds- can lead to degradation of the analytes,

adsorbent materials and promote catalytic breakdown of the

trapped analytes

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ABSORPTION VS ADSORPTION

ADSORPTION

artefact formation

incomplete desorption

strong catalytic interactions

of trapped analytes with adsorbents

ABSORTION

analytes are retained by dissolution

analytes can be desorbed at moderate temperatures

analyte decomposition can be ruled out

non-specific interactions between analyte and sorbent

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LIQUID–LIQUID–SOLID MICROEXTRACTION (LLSME)

simple

exciting low-cost

environment-friendly

negligible organic solvent consumption

enhanced efficiency

high selective and sensitive pretreatment

Y. Hu, Y. Wang, Y. Hu, G. Li, J. Chromatogr. A, 1216 (2009) 8304

(36)

ELECTROSORPTION ENHANCED SPME (EE-SPME)

simple, fast, sensitive

good performance

short adsorption time

wide linear range

low detection limit

high recoveries

(37)

MEMBRANE-SPME (M-SPME)

1) silica fiber

2) coating of polyethylene glycol (PEG) 3) coating of polydimethylsiloxane (PDMS)

Inner coating Outer coating

Absorbent material PEG PDMS

Average thickness of coating 40-50μm 100-110μm

Length of sorbent coating 1cm 1,2 cm

The role of sorbent coating very polar retaining medium

hydrophobic, nonpolar membrane

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

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M-SPME ADVANTAGES

 low cost of fiber preparation

 high thermal stability (PDMS is stable up to 300

o

C)

 short extraction and desorption time

 lack of water sorption (due to the presence of hydrophobic membrane)

 high affinity to polar analytes

At the extraction temperature PEG of low molecular weight behaves as an immobilised liquid (viscous liquid polymer)

Analytes are retained by dissolution in the sorbent layer absorption nature of the retention

partitioning mechanism of the extraction

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

Determination of phenols using M-SPME and GC

Compound Linearity

range (µg/L) R

2

LOD (µg/L)

M-SPME PA

4-Chloro-3-methylphenol 15-1500 0.9953 7 50

2-Chlorophenol 3-300 0.9936 43 530

2,4-Dichlorophenol 3-300 0.9987 15 120

2,4-Dimethylphenol 3-300 0.9921 9 110

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 9 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

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Compound

R2 LOD (mg/L) RSD (%)

M-SPME DVB/CAR

/PDMS M-SPME DVB/CAR

/PDMS M-SPME

DVB/CA R /PDMS

chlorobenzene 0.997 0.994 0.031 0.016 11 9

p-xylene 0.992 0.986 0.022 0.015 9 6

o-xylene 0.986 0.994 0.018 0.014 12 7

isopropylbenzene 0.994 0.995 0.015 0.018 12 8

n-propylbenzene 0.998 0.997 0.013 0.017 14 10

2-chlorotoluene 0.997 0.993 0.016 0.019 8 6

4-chlorotoluene 0.995 0.995 0.017 0.018 10 6

t-butylbenzene 0.997 0.985 0.011 0.021 12 8

sec-butylbenzene 0.987 0.992 0.011 0.021 11 8

1,3-dichlorobenzene 0.989 0.998 0.017 0.017 14 10

1,4-dichlorobenzene 0.994 0.987 0.017 0.023 13 7

1,2-dichlorobenzene 0.986 0.988 0.016 0.028 13 7

Determination of VOCs

using M-SPME and GC

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M-SPME conclusion

partitioning mechanism of the extraction, which is characterized by significantly higher linearity range when compared to commercial fibre enabling highly polar sorbents to be used without the risk of dissolving in polar sample matrix

povides opportunity of application of quite new kinds of materials,

which due to low melting temperatures or solubility in water have not been taken into consideration so far in this kind of applications

high extraction efficiency of phenols and VOCs obtainable with M-SPME fibres, comparable and better than the extraction efficiency using

commercially available fibres

M-SPME combined with determination by GC may become a powerful, environmentally friendly tool for sampling, isolation and preconcentration of organic pollutants

• applicable on the sample preparation step prior to the final

quantitative determination of analytes on the ppb level

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TOOLS:

Life Cycle Assessment (LCA) 1 Eco- Scale 2

Eco-Compass 3

1Consoli, 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. Séguin and B. Vigon., ‘Guidelines for life cycle assessment: A ‘Code of practice’, SETAC, Brussels and Pensacola, 1993.

2Aken 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/

EVALUATION OF ENVIRONMENTAL

IMPACT OF ANALYTICAL PROCEDURES

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A new tool for evaluation of the greenness of analytical methodology

Eco-Scale = 100 – total penalty points

The result is ranked on the following scale:

>75 – excellent green analysis

>50 – acceptable green analysis

<50 – inadequate green analysis

Penalty points are assigned for amount of reagents, hazards

(physical, environmental, health and occupational), energy used and waste generated in the analytical procedure

Gałuszka A., Konieczka P., Migaszewski Z.M., Namieśnik J. 2012. Analytical Eco-Scale for assessing the greenness of analytical procedures.

Trends in Analytical Chemistry 37, 61–72.

A NALYTICAL E CO -S CALE

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REAGENTS

Subtotal PP Total PP

Amount <10 mL (g) 1

Amount PPHazard

PP

10-100 mL (g) 2

>100 mL (g) 3

Hazard (physical, environmental, health)

None 0

Less severe hazard 1

More severe hazard 2

INSTRUMENTS Energy

≤0.1 kWh per sample 0

≤1.5 kWh per sample 1

>1.5 kWh per sample 2

Occupational hazard

Analytical process hermetization 0

Emission of vapors and gases to the air 3

Waste

None 0

<1 mL (g) 1

1-10 mL (g) 3

>10 mL (g) 5

Recycling Degradation Passivation No treatment

0 1 2 3

T HE PENALTY POINTS (PP S ) TO CALCULATE ANALYTICAL E CO -S CALE

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DEPARTMENT OF ANALYTICAL CHEMISTRY CHEMICAL FACULTY

GDANSK UNIVERSITY OF TECHNOLOGY

Department of Analytical Chemistry

This lecture can also be found on the homepage of the Department of Analytical Chemistry

http://www.pg.gda.pl/chem/Katedry/Analityczna/analit.html

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EUROPEAN MASTER IN QUALITY

IN ANALYTICAL LABORATORIES- EMQAL

http://eacea.ec.europa.eu/erasmus_mundus/

(47)

MODAS

„Production and attestation of new types of reference materials crucial for achieving European accreditation for polish industrial

laboratories ‐ MODAS”

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

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48

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MEMBERS OF MY RESEARCH GROUP

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THANK YOU FOR YOUR ATTENTION!

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