Reference material was synthesised for 21 substances that are frequently present as synthetic impurities, i.e. by-products, in illicitly produced amphetamine. Each of these substances is a typical by-product for at least one of the three approaches most often used to synthesise amphetamine, namely, the Leuckart, the reductive amination of benzyl methyl ketone, and the nitrostyrene routes. A large body of data on the substances was recorded, including the following: mass spectra, ultraviolet spectra, Fourier transform infrared spectra, infrared spectra in gas phase, and 1H NMR and 13C NMR spectra. © 2004 Elsevier Ireland Ltd. All rights reserved.

Photodesorption of thin films of fulvic acid adsorbed on planar iron oxide surfaces was monitored by ellipsometry. Description was first observed at 546 nm, and additional fractions of the adsorbed acid left the surfaces at 405 and 365 nm Similar kinetics for photodesorption was observed from metallic iron films and from porous iron oxide prepared electrochemically by deposition on porous silicon substrates. Soluble photoproducts leaving the surface H ere monitored by UV absorbance spectroscopy at 200 nm Gaseous products were not detected by mass spectrometry but the results seemed to indicate that net all of the photoproducts entered the liquid phase. Of the metal films tested which adsorbed fulvic acid from aqueous solution (Fe. Cr, Ni, Al, and Pt), it was only iron which exhibited a photodesorption effect. (C) 2001 Elsevier Science B.V. All rights reserved.

The composition of water leachable organics in municipal solid waste incineration (MSWI) residues is not well known. Therefore the utilisation of ashes is restricted due to the concern about their long-term environmental impact. Previous studies have focused on some highly toxic organic compounds present only in trace amounts. It is also important to know the composition of the bulk organic matter since dissolved organic carbon can alter the leachability of metals. In order to characterise water leachable organic matter in incineration residues a fractionation procedure using polymeric adsorbents was successfully developed and applied. The technique uses XAD-8 and XAD-4 resins in tandem and has been implemented on bottom ash samples from two incineration plants in Sweden in order to characterise the bulk organic matter.

A method for analysis and comparison of mineral oil-based greases thickened with a metal soap is presented. The greases are first analyzed with Fourier-transform infrared spectroscopy (FT-IR). This analysis differentiates between greases with different main constituents. When two samples can not be differentiated with IR, a more thorough analysis has to be performed. The base oil and the soap are separated. The soap is derivatized and the two components are each analyzed with gas chromatography. The metal ions of the soap are analyzed with scanning electron microscopy with an energy dispersive X-ray detector (SEM-EDX). By the method presented, grease from a weapon may be differentiated or proven to be identical to grease collected from a suspect. As thr results indicate that the grease does not change with respect to composition when the weapon is fired, the method may be used in many cases. The application of the method to an authentic case is reported.

Retention mechanisms of an unmodified and a hydroxylated polystyrene–divinylbenzene polymer were studied by solid-phase extraction of o-phthalic acid and some of its mono- and diesters from purified water and then analysing by GC–MS. The monoesters and phthalic acid were retained only when protonated (i.e. acidified with HCl to pH 0.9). Of all elution solvents tested, ethyl acetate gave the best overall recoveries (61–89%) with both polymers. Applicability to complex matrixes (e.g. acidogenic landfill leachates) was examined by introducing a washing step with acetone in acidified water (pH 0.9) to eliminate volatile fatty acids (C₂–C₆) from the cartridge. Finally, the method was tested on real samples.

Cellulose powder and softwood sawdust were subjected to alkaline degradation under conditions representative of a cementitious environment for periods of 7 and 3 years, respectively. During the first 3 years, sampling was frequent, and data on the degradation of cellulose and production of isosaccharinic acid was used for establishing long-term prediction models. Samples after an additional period of 4 years were compared to the predicted values. The total rate of degradation was measured as the increase in total organic carbon (TOC) in corresponding solutions. A previously published theoretical model of degradation kinetics gave a good approximation of the present experimental data. Peeling-off, stopping, and alkaline hydrolysis reaction rate constants were obtained as model parameters, and the results suggested that the transformation of the glucose end group is the rate-limiting step in the cellulose peeling-off reaction and also determines the pH dependence of that reaction. After 3 years, isosaccharinic (ISA) acid represented 70-85% of all degradation products as quantified by capillary zone electrophoresis. The long-term prediction model indicated that all of the cellulose would be degraded after only 150-550 years. The control sampling after 7 years points toward a lower degradation of cellulose and production of ISA than predicted by the model, reflecting either a degradation of ISA that was faster than the production or a termination of the ISA production.

The feasibility of employing an electronic tongue to measure the growth of mold in a liquid medium was studied. We used the electronic tongue developed at Linköping University, which is based on pulsed voltammetry and consists of an array of different metal electrodes. Instead of focusing on a single parameter, this device provides information about the condition or quality of a sample or process. Accordingly, the data obtained are complex, and multivariate methods such as principal component analysis (PCA) or projection to latent structures (PLS) are required to extract relevant information. A gas chromatographic technique was developed to measure ergosterol content in mold biomass and was subsequently used as a reference method to investigate the ability of the electronic tongue to measure the growth of mold in liquid media. The result shows that the electronic tongue can monitor mold growth in liquids. In PLS analysis, the electronic tongue signals correlate well with the amount of ergosterol in the mold biomass as well as the microbially induced changes in the pH of the medium. © 2002 Elsevier Science B.V. All rights reserved.

Anabolic androgenic steroids are testosterone and its derivates. Testosterone is the most important naturally existing sex hormone for men and is used for its anabolic effects providing increased muscle mass. Testosterone is taken orally or by intramuscular injection in its ester form and are available illegally in different forms of esters. Anabolic androgenic steroids are today analyzed only in urine. To differentiate between the human natural testosterone and exogenous supply the quote natural testosterone and epitestosterone is used. Detection of testosterone esters in serum is an unmistakable proof of exogenous supply of testosterone. The aim of this thesis was to find a method for determining testosterone esters in serum and to study an extraction method possible for quantification of testosterone esters in serum.

The technique used to separate and identify the Testosterone esters was Liquid Chromatography Tandem Mass Spectrometry Electro Spray Ionisation. Parameters for chromatography and mass detection were optimized for nine testosterone esters and evaluated according to selectivity, resolution and intensity. A method that could be used for determination of testosterone esters in serum was found. The MS-method was set and at least three possible transitions for each testosterone ester were found. The best choice of column proved to be the C18 column where all the esters were separated and seven of them were base-line separated. The C18 column along with methanol and ammonium acetate buffer, 5 mM, pH 5 showed the highest sensitivity for Multiple Reaction Monitoring-detection. A gradient profile for a total runtime of 5.6 minutes was established. Two alternative extraction procedures were tested, with tert-butylmethylether or diethyl ether/ethyl acetate and both seemed to work satisfactory. Analysis of serum proved to work well and no severe interference occurred. Results from the linearity tests indicate that future quantification method in serum will be possible.

It has been shown that some of the fluorinated ethane derivatives being introduced as CFC-replacements can be transformed to TFA (trifluoroacetate) in the atmosphere. Moreover, TFA is extremely stable in the environment, and this has raised questions regarding how widespread TFA is in the environment. We found that TFA is ubiquitous in precipitation: samples of rain from Ireland and Poland and snow from Canada, Sweden, New Zealand, and East Antarctica contained 1-1100 ng/L, and, studying a firn core drilled in Antarctica, concentrations of 3-56 ng/L were measured in layers formed during the 19th century. We have confirmed the preindustrial presence of significant background concentrations of trifluoroacetate in historic precipitation samples from the analysis of firn. Extensive procedures were enforced to prevent sample contamination.It has been shown that some of the fluorinated ethane derivatives being introduced as CFC-replacements can be transformed to TFA (trifluoroacetate) in the atmosphere. Moreover, TFA is extremely stable in the environment, and this has raised questions regarding how widespread TFA is in the environment. We found that TFA is ubiquitous in precipitation: samples of rain from Ireland and Poland and snow from Canada, Sweden, New Zealand, and East Antarctica contained 1-1100 ng/L, and, studying a firn core drilled in Antarctica, concentrations of 3-56 ng/L were measured in layers formed during the 19th century. We have confirmed the preindustrial presence of significant background concentrations of trifluoroacetate in historic precipitation samples from the analysis of firn. Extensive procedures were enforced to prevent sample contamination.

A firn core was drilled in Dronning Maud Land, Antarctica, to investigate the presence of haloacetates in snow that had accumulated over the past 200 years. By employing GC-MS detection of methyl esters of haloacetic acids, we were able to measure haloacetate concentrations down to one or a few nanograms per liter. Trichloroacetate (TCA) and dibromoacetate (DBA) were found in firn at concentrations that clearly exceeded the blank level of the applied analytical procedure, with mean concentrations estimated to 12 and 6 ng/L, respectively. There were also indications that mono- and dichloroacetate (MCA and DCA) were present in firn, whereas monobromoacetate (MBA) was found only in samples of surficial snow. We concluded that there is a significant natural background level of TCA and DBA in precipitation based on the following: (i) several of samples represented snow accumulated in the 19th century, (ii) haloacetates can be expected to be immobile in Antarctic firn, (iii) extensive measures were taken to prevent sample contamination, and (iv) blank levels of the analytical procedure used were low and stable. In addition, our results suggested that MCA and DCA also occur naturally in precipitation.