Abstract One major objective of the European project “Collaborative Harmonisation of Methods for Profiling of Amphetamine Type Stimulants” (CHAMP), funded by the sixth framework programme of the ...European Commission, consisted of the harmonisation of a gas chromatography/mass spectrometry (GC/MS) method for the analysis of organic impurities found in illicit methamphetamine (MA) samples in a drug intelligence perspective. Statistical analysis provided a selection of pertinent variables among the 43 organic impurities identified in the chromatograms. As for the 3,4-MethyleneDioxyMethAmphetamine (MDMA) study 1 , correlation coefficients were used as a discrimination tool between populations of linked samples (from the same seizure) and unlinked samples (from different seizures). It was also shown that correlation measurements based on Pearson and cosine functions applied to the data pre-treated by normalisation to the sum of peak responses followed by the square root provided excellent discrimination between the two populations. The organic impurities profiling method was proved to be relevant for the characterization of samples from different seizures and their synthesis route patterns.
The main objectives of the European project "Collaborative Harmonization of Methods for Profiling of Amphetamine Type Stimulants" (CHAMP) funded by the sixth framework programme of the European ...Commission, included the harmonization of MDMA profiling methods and the creation of a common database in a drug intelligence perspective. In the preliminary stages of this project, the participating laboratories analysed the physical characteristics, the chemical composition and the organic impurities of MDMA tablets, using the previously harmonized methods. The aim of the present work was to apply statistical treatments to the recorded data in order to evaluate their potential in the fight against drug trafficking. Comparable working procedures were applied on the different types of data. The first part of this article deals with organic impurities data, while the second part focuses on the potential of the physical characteristics. Organic impurities data were recorded by a harmonized Gas Chromatography/Mass Spectrometry (GC/MS) method previously developed. Statistical analysis provided a selection of pertinent variables among the 46 organic impurities identified in the chromatograms. Correlation coefficients were used to yield separation between populations of samples coming from the same synthesis batch and samples coming from different batches. It was shown that correlation measurements based on Pearson and cosine functions applied to the data pre-treated by normalisation to the sum of peak responses followed by the square root provided an excellent discrimination between the two populations. The statistical methods applied to organic impurities profiles proved to be excellent techniques to differentiate samples from different batches and to highlight operational links between samples.
Drug intelligence based on MDMA tablets data Weyermann, Céline; Marquis, Raymond; Delaporte, Céline ...
Forensic science international,
5/2008, Letnik:
177, Številka:
1
Journal Article
Recenzirano
Abstract The main objectives of the European project “Collaborative Harmonisation of Methods for Profiling of Amphetamine Type Stimulants” (CHAMP) funded by the sixth framework programme of the ...European Commission, included the harmonisation of MDMA profiling methods and the creation of a common database in a drug intelligence perspective. In the preliminary stages of this project, the participating laboratories analysed the physical characteristics, the chemical composition and the organic impurities of MDMA tablets, using the previously harmonised methods. The aim of the present work was to apply statistical treatments to the recorded data in order to evaluate their potential in the fight against drug trafficking. Comparable working procedures were applied on the different types of data. The first part of this article deals with organic impurities data, while the second part focuses on the potential of the physical characteristics. Organic impurities data were recorded by a harmonised Gas Chromatography/Mass Spectrometry (GC/MS) method previously developed. Statistical analysis provided a selection of pertinent variables among the 46 organic impurities identified in the chromatograms. Correlation coefficients were used to yield separation between populations of samples coming from the same synthesis batch and samples coming from different batches. It was shown that correlation measurements based on Pearson and cosine functions applied to the data pre-treated by normalisation to the sum of peak responses followed by the square root provided an excellent discrimination between the two populations. The statistical methods applied to organic impurities profiles proved to be excellent techniques to differentiate samples from different batches and to highlight operational links between samples.
As one of the important candidate of power sources for the future, the research and production of hydrogen gas has a significant importance. In this article, the emphasis is on the influence of ...impurities on hydrogen evolution reaction, i.e., the influence of an addition of decacyclene, C
12H
35C
6H
4SO
4Na, CH
3CH
2OH, chromanone, H
2SO
4, HNO
3, 4,4′-biphenediol and 1,2,3,4-tetraphenyl-1,3-cyclopentadiene was studied by electrochemical impedance technique. The adsorption structure for some organics was measured by scanning tunneling spectroscopy techniques. Superstructure of adsorbed decacyclene on Au(111) surface was captured. The ordered adsorption structure of 4,4′-biphenyldiol on Au(111) and (100) was also observed. The addition of decacyclene has shown an opposite effects on hydrogen evolution for Au(111) and (100) surface, i.e., it inhibits the reaction at Au(100) but enhances the one at Au(111). The results show that the addition of C
12H
35C
6H
4SO
4Na and HNO
3, especially the latter, can improve the hydrogen evolution. In the article the adsorption structure and hydrogen evolution reaction have been studied in order to give some useful information about the relation between the adsorption structure and the properties. The purpose of this article is to attempt to find the relation between electrochemical performance and the adsorption structure, and to explore the effect of some additives.
Abstract The profiling of MDMA tablets can be carried out using different sets of characteristics. The first type of measurements performed on MDMA tablets are physical characteristics (i.e. ...post-tabletting characteristics). They yield preliminary profiling data that may be valuable in a first stage for investigation purposes. However organic impurities (i.e. pre-tabletting characteristics) are generally considered to bring more reliable information, particularly for presentation of evidence in court. This work aimed therefore at evaluating the added value of combining pre-tabletting characteristics and post-tabletting characteristics of seized MDMA tablets. In approximately half of the investigated cases, the post-tabletting links were confirmed with organic impurities analyses. In the remaining cases, post-tabletting batches (post-TBs) were divided in several pre-tabletting batches (pre-TBs), thus supporting the hypothesis that several production batches of MDMA powder (pre-TBs) were used to produce one single post-TB (i.e. tablets having the same shape, diameter, thickness, weight and score; but different organic impurities composition). In view of the obtained results, the hypotheses were discussed through illustrating examples. In conclusion, both sets of characteristics were found relevant alone and combined together. They actually provide distinct information about MDMA illicit production and trafficking.
In recent, production of bioethanol in Indonesia is produced primarily from sugarcane molasses and cassava as the 1st generation. But related with its development, it is quite hard to be a major ...feedstock in bioethanol conversion because there is conflict in using between consumption food and energy resources. Due to abundant lignocellulose biomass resources in Indonesia, such as empty fruit bunch (EFB) of oil palm, sugarcane bagasse and other forrest residue, the research in the development of process for 2nd generation bioethanol production is being increase. This case can be a right solution to solve the problem because lignocellulose is unused material. Processing of lignocellulosic biomass into bioethanol consists of four major unit operations: pre-treatment, hydrolysis, fermentation and product separation/distillation. Although ethanol is the dominant alcohol produced in the fermentation of sugars process, there are some byproducts in bioethanol product, such as organic impurities, water and organic acid. Determination of the impurity is important to prove the quality of produced bioethanol. Some of the impurities is not allowed in the product, such as methanol and others organic, that should be limited to control the performance from bioethanol as substituted fuel. Organic impurities of the bioethanol product was analyzed by using GC-FID while the water content was analyzed by using Karl Fischer Coulometric Moisture Titrator. In this research, the lignocellulosic bioethanol analyzed for the moisture content and organic impurities was undenatured one. The water content of the bioethanol sample was analyzed in 7 replicates where the average was 0.1776%-w (% RSD 2.0460). There are eight compounds of organic impurities detected in GC-FID that are acetaldehyde (0.0217%-w), acetone (0.0102%-w), ethyl acetate (0.0368%-w), methanol (0.0224%-w), isopropyl alcohol (0.0035%-w), n-propyl alcohol (0.0188%-w), isobutanol (0.0437%-w) and isoamyl alcohol (0.0377%-w).
This study aims to utilize the manufacturing impurities found in illicit heroin to predict whether the samples had originated from a common production batch. From highly cut heroin samples, twelve ...frequently extractable neutral/acidic impurities were selected for investigation. A gas chromatographic method was optimized using three locally seized samples containing the target impurities and a control sample consisting of n-alkanes. The method optimization procedures are reported in detail. The capability of the optimized method was further assessed using five simulated links prepared from unrelated heroin seizures. With the aid of principal component analysis (PCA), it was found that the statistical data pretreatment (normalization followed by standardization, N + S) showed promising results for sample classification using profiles obtained with the optimized method. Similarly, 252 street doses of highly cut samples were analyzed and the profiles were statistically decomposed by PCA after the N + S pretreatment. The statistics suggested that the locally seized samples could have originated from more than one production batch.
The aim of this research was to select suitable activated carbon (AC) for effective removal of organic impurities from industrial aqueous hydrogen peroxide solution to produce ultra-pure hydrogen ...peroxide. The textural parameters and surface chemistry of four kinds of AC samples were measured and analyzed. Static and dynamic equilibrium adsorption experiments were carried out to compare the effect of AC on organic impurities adsorption and hydrogen peroxide decomposition. The effects of AC pore structure and surface chemistry on the adsorption of organic impurities were investigated. The fitting operation conditions, i.e., operating temperature and AC dosage, were also examined. The results showed that AC adsorption capacity on organic impurities from industrial aqueous hydrogen peroxide solution was mainly influenced by micropore structure of AC, as well as decomposition of hydrogen peroxide. The pore size of 1–3
nm is most effective for adsorption of organic impurities. It was found that the organic impurities in industrial hydrogen peroxide solution could be reduced effectively to meet the standard of ultra-pure hydrogen peroxide of SEMI-C8 level with the proposed AC and adsorption techniques.
Spent acid is produced in ever-larger quantities in the sulfuric-acid washing of naphthalene. Since 2005, its production has increased by 15%, to more than 90 m
3
per month. In addition, its content ...of organic impurities has doubled, on account of deterioration in the naphthalene fraction and the discontinuation of pyridine removal. The naphthalene content in the organic impurities has fallen by a factor of 1.5, with increase in the content of heavy pyridine bases. The removal of pyridine in polymerizational washing increased the consumption of sulfuric acid by 0.015 t/t of naphthalene. The spent acid is collected in a tank and sent for processing in the sulfate department of byproduct-capture shop 2. Analysis of the distribution of organic impurities along the supply and processing chain shows that, in comparison with 2005, the residue in the tanks after acid discharge is reduced by a factor of 1.3; the content of organic impurities remaining in the tank is reduced by 2.5. The effectiveness of partial regeneration of the spent acid in the tank is a third as much as in 2005. In all, 1.2% of the naphthalene is lost with the acid. More than 61% of the naphthalene settles in the tanks; ~9% is in the store within byproduct-capture shop 2; 28% is in the acidic tar; and 0.6% is in ammonium sulfate. Each month, >10 t of heavy pyridine bases are discharged with the spent acid: 16% remains in the tanks; >65% is in the ammonium sulfate. Since 2005, the content of pyridine bases in the ammonium sulfate has increased sevenfold. This may be attributed to increased supply of heavy pyridine bases with the spent acid and to the discontinuation of the separation of light pyridine bases from the mother liquor in the byproduct-capture shop. To reduce the output of spent acid, hydrogen peroxide is added to the concentrated sulfuric acid. The peroxymonosulfuric acid formed improves the polymerizational washing, with decrease in sulfuric-acid consumption by 15% and increase in the removal of indole from naphthalene by 18%. The consumption of hydrogen peroxide is 0.02 kg/t of naphthalene. With increase in density of the tar in the naphthalene fraction, the content of the absorbing fraction increases. Accordingly, the quality of the naphthalene fraction may be boosted by reducing the phenol content in the phenol fraction.
Effect of compounds involved in complex reagents is described using Helamin 906H reagent as an example. The working exchange capacity of KU-2-8chs cation exchanger in hydrogen form and Amberlite IRA ...900Cl anion exchanger in OH form remained almost unchanged when they were used repeatedly to purify water that contained Helamin 906H reagent; in addition, this capacity was the same upon filtration of water that did not contain this reagent. Leakage of total organic carbon was observed earlier than that of calcium ions upon filtration of the solution through the cation exchanger layer. The test results obtained in industrial conditions indicated that using H–OH filters to purify turbine condensate enables the decrease of the concentration of organic and other impurities therein.
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