Interlaboratory trial on the analysis of alkylphenols, alkylphenol ethoxylates, and bisphenol A in water samples according to ISO/CD 18857-2.

ISO/CD 18857-2 (International Organization for Standardization, Geneva) describes a new international standard method for the determination of octylphenol, nonylphenol, their mono- and diethyoxylates, and bisphenol A in nonfiltered samples of drinking, ground, surface, and wastewater. The method is based on the extraction of the analytes from an acidified water sample by solid phase extraction, solvent elution, derivatization, and determination by gas chromatography with mass spectrometric detection. For validation of this method, 14 laboratories from 4 different countries in Europe and Canada participated in an interlaboratory trial to determine the performance characteristics of the method, which are intended for publication in the corresponding standard. The interlaboratory trial was evaluated according to ISO 5725-2 and included two duplicate nonfiltered water samples: surface water containing the target compounds in an analyte concentration range from 0.05 to 0.4 microg/L and wastewater containing the target compounds in a concentration ranged from 0.1 to 5 microg/L. The repeatability variation coefficients (within-laboratory precision) varied for all samples and compounds between 1.9 and 7.8%, showing a sufficiently high repeatability of the method. The reproducibility variation coefficients (between-laboratory precision) were found to vary within a satisfactory range of 10.0-29.5% for surface water and 10.8-22.5% for wastewater. The recoveries as a measure of accuracy varied from 98.0 to 144.1% for surface water and from 95.4 to 108.6% for wastewater. The determined concentrations of the samples compared well to the "true" values, thus showing very satisfactory accuracy of the method. In the chromatogram of the surface water sample, a high unresolved background made up of coextractable matrix compounds was apparent. It is conceivable that compounds from this background may be responsible for enhanced recoveries of 144.1% for 4-nonylphenol (mixture of isomers) and of 123.4% for 4-nonylphenol monoethoxylate (mixture of isomers) in the surface water samples. The isotope-marked standard compounds developed in this context proved to be reliable internal standards that allow a precise and accurate quantitation of all compounds specified in ISO/CD 18857-2. The results of the interlaboratory trial confirmed that the analytical method is robust and reliable and can be used as a standard method to analyze the target compounds in water samples.

Mathematical algorithm for qualitative and semiquantitative analysis of petroleum hydrocarbons in solid wastes using on-line gas chromatography.

Non-degradated mineral-oils like gasoline, solvent naphtha, diesel fuel, fuel and lubricating oils provide a characteristic fingerprint gas chromatogram. This visual classification, e.g. in solid wastes, is complicated due to the simultaneous presence of several mineral-oils. Therefore, a mathematical algorithm for the separation of gas chromatographic fingerprint of "single mixtures" of aliphatic hydrocarbons is developed. The technique is essential for analysis of time-overlapping "single mixtures" of petroleum hydrocarbons (so-called "complex mixtures") and it relies on the concentration-varying hydrocarbons during evaporation. It is possible to separate the data from the gas chromatogram of a "complex mixture" of hydrocarbons into the chromatograms of the pure "single mixtures" and to give their respective concentrations. A synthetic "complex mixture" of kerosene, diesel fuel and lubricating oil is used to illustrate the method.