Bogdan Zygmunt

Application of solid-phase microextraction for determination of organic vapours in gaseous matrices

This paper reviews the practical applications of solid-phase microextraction (SPME) in the analysis of organic vapours which are pollutants of atmospheric air, indoor air and workplace air. Applications to headspace of solids and liquids such as different waters, soils, food, etc., are also included. Problems related to calibration in SPME analysis of gaseous matrices are also dealt with. Calibration procedures and apparatus for generation of standard gaseous mixtures are described. Advantages and limitations of SPME based gas chromatographic methods of air organic pollutants are discussed.

Solid Phase Microextraction — A Convenient Tool for the Determination of Organic Pollutants in Environmental Matrices

This article reviews the application of solid phase microextraction (SPME) for determination of organic pollutants in gaseous, liquid, and solid environmental samples. Practical aspects of direct and headspace SPME sampling and combination of SPME with other techniques of sample preparation are discussed. The application range can be widened by derivatizing analytes. SPME can combined with other related techniques of sample preparation.

Role of reference materials in analysis of environmental pollutants.

This paper discusses the importance and use of reference materials for quality assurance and quality control in environmental analysis. The general classification of reference materials and categorisation of those for chemical composition are presented. The most common reference materials for pollutants in air, water, waste water, soil, sediments, sludge and some biological materials and their producers are tabulated. Definitions, practical recommendations on selection and handling, and application areas of reference materials are also presented.

Sample preparation and chromatographic analysis of acidic herbicides in soils and sediments

This article reviews sample preparation of soil and sediment samples for the chromatographic determination of acidic herbicides of phenolic and carboxylic acid classes. The common methods of acidic herbicides enrichment and isolation from soils and sediments were discussed, mainly supercritical fluid extraction, pressurized solvent extraction, subcritical water extraction, microwave-assisted extraction, and also traditional extraction with organic solvents and aqueous basic solutions. Derivatization to make herbicides analyzable by means of gas chromatography and/or to improve detectability by GC and LC—and also extraction efficiency were described.

Gas chromatographic sulphur-sensitive detectors in environmental analysis

Abstract Gas chromatographic (GC) detection systems, which are especially suited for the selective determination of sulphur compounds in various matrices, and their applications are reviewed. They include flame photometric, electron-capture, chemiluminescence, atomic emission, electrochemical and photoionization detectors. The principles of operation, characteristics and development and compatibility with capillary columns are briefly described. The possibility of coupling with supercritical fluid chromatography, liquid chromatography and some spectroscopic techniques is discussed

Selected concentration techniques for gas chromatographic analysis of environmental samples

SummaryThe paper describes the role and tasks of environmental analysis and monitoring. It emphasises the leading role played by gas chromatography, especially when coupled with suitable sample preparation. This is demonstrated by some literature evidence and mainly by the authors original work on the design of sample preparation apparatus and development of GC-based methods of determination of a wide variety of organic pollutants in environmental samples. A typical example is the physical speciation of PAHs and PCBs in river environment with the use of a home-made filtration vessel coupled with SPE cartridges to prepare samples for GC-MS analysis; thin layer head space with self-generation of aqueous concentrate to prepare humane urine samples for DAI (direct aqueous injection)-GC-ECD analysis for the content of volatile chloro-organic compounds; studies on capillary denuders in sampling organic air pollutants; passive dosimeters in indoor air quality measurements; design and application of thermal desorbers for the introduction of analytes into GC columns and modification of a speciation analyser for organometalic environmental pollutants.

Calibration procedure for solid phase microextraction-gas chromatographic analysis of organic vapours in air.

A calibration procedure for solid phase microextraction-gas chromatographic (SPME-GC) analysis of organic vapours in air was described in which GC detector (MS in this case) signal is directly related to concentration of analytes of interest sampled by SPME. Gaseous standard mixtures used for the calibration were generated by means of a home-made permeation-type apparatus described elsewhere, W. Janicki et al., Chem. Anal., 38 (1993) 423 and modified to permit easy sampling of analytes on an SPME fibre. To establish sampling parameters, times for equilibrium partitioning of five selected organic compounds (carbon tetrachloride, toluene, chlorobenzene, p-xylene, n-decane) between gaseous mixtures and the fibre (fused silica fibre coated with 100 mum polydimethylsiloxane) were determined. For 10 min sampling time, the detector response and hence amount sampled on the fibre were linear functions of analytes concentration in a gaseous sample.

Determination of trihalomethanes in aqueous samples by means of a purge-and-trap systems with on-sorbent focusing coupled to gas chromatography with electron-capture detection

Abstract A laboratory-built purge-and-trap device in which analytes desorbed from a primary trap (macrotrap) are focused in a microtrap (also with sorbent) and moisture is removed from purgue gases by a Nafion tube (walls selectively permeable to water vapour) is described. The device is compatible with capillary GC columns. Purgue parameters such as purge gas flow-rate and volume, purge temperature and ionic strength were optimized with respect to recovery efficiencies of trihalomethanes (THMs) and carbon tetrachloride (CCl4) from aqueous samples. Sorption and desorption parameters of a macrotrap-microtrap system for THMs were selected. A procedure was developed whereby THMs and CCl4 at the level of several ppt can be determined with good accuracy and precision in a variety of aqueous samples. The procedure was applied to the determination of THMs and CCl4 in real samples, i.e., tap water, orange drinks and an infusion fluid.

Volatile and semivolatile organo-halogen trace analysis in surface water by direct aqueous injection GC-ECD

A procedure for simultaneous determination of volatile and semivolatile chloroorganic compounds (from trichloromethane to di- and trichlorobenzenes to hexachlorobutadiene) in aqueous samples was developed. The procedure is based on a DAI-GC-ECD technique widely used for trihalomethanes determination in drinking water. The DAI technique application could have been extended to semivolatile chloroorganic compounds by using a Rtx-624 (60 m x 0.32 mm I.D., df 1.8 microns (6% cyanopropyl, 94% dimethyl polysiloxane). Precision (R.S.D.) and detection limits of the DAI-GC-ECD procedure with respect to 12 volatile and semivolatile chloroorganics were determined. Relative standard deviations (R.S.D.) were lower than 22% and the detection limits (concentration equivalent to a peak height three times the baseline noise) range from 0.02 microgram L-1 for trichloroethene and tetrachloroethene to 0.25 microgram L-1 for hexachlorobutadiene to 1.6 micrograms L-1 for 1,2-dichlorobenzene. The method was successfully used to determine chloroorganic pollutants in river water.

Evaluation of Pollution Degree of the Odra River Basin with Organic Compounds after the 1997 Summer Flood – General Comments

The aim of this study is a qualitative and quantitative characterisation of organic pollutants in post-flood sediments in the Odra basin and the description of their sources with indication of especially polluted sites (so called hot spots) in the most suspected places in the drainage area. It was found that maximum allowable concentration levels for PCBs (polychlorinated biphenyls), VOCs (volatile organic compounds) and pesticides were not exceeded. Among regulated compounds, the exceeding values of the permissible level of concentration were found only for PAHs (polycyclic aromatic hydrocarbons) in sediments. Sixteen investigated samples, out of 72 had very high content of total PAHs. Sampling sites in which concentration levels of PAHs were found high, were located near power plants or roads with heavy traffic.