No description available.

Analytical procedures have been developed for the quantitative analysis of phenols in crude oils and sedimentary rock pyrolysates and extracts. The procedures involve isolation of the phenolic components of the sedimentary organic matter by extraction with alkaline aqueous methanol, followed by the removal of carboxylic acids using a back extraction step. Co-extracted non-polar components are removed from the alkaline extract by liquid chromatography or by extracting it with hexane. The phenol isolates thus obtained were analysed by capillary GC, GC-MS and GC-FTIR. Recoveries of 70-95% were measured for C(subscript)0-C(subscript)3 alkylphenol compounds using these procedures.Crude oil samples (45) representing a range of locations, ages, depositional environments, maturities, source types, and biodegradation levels have been analysed for their phenol contents. A range of C(subscript)0-C(subscript)5 alkylphenols (approximately 40) were identified in crude oils using co-chromatography on up to three different stationary phases and by comparison of their retention times, mass spectral and infrared spectral properties with reference compounds. Isopropylmethylphenols (six) and sec-butylmethylphenols (nine) were synthesised for use in the identification of these compounds. A range of C(subscript)0-C(subscript)4 alkylphenols (24) were quantified using a dimethyl siloxane column (BP 1 or DB 1) and found to occur at concentrations ranging from 190x10(subscript)3 ng/g down to the limit of detection of 10 ng/g (ppb).The crude oil samples were classified into six groups based on their C(subscript)0-C(subscript)5 alkylphenol compositions. Group 1 crude oils have at least one isomer class in which the relative proportions of the alkylphenol isomers reflect their relative thermodynamic stabilities. The vast majority of samples, however, do not contain relative proportions of ++ / phenols which reflect their stabilities, and these differences have been used to group the remaining crude oils. Group 2 crude oils contain predominantly alkylphenols derived from natural product precursors. This group has been further subdivided into Group 2A in which samples have isopropylmethylphenol distributions dominated by carvacrol and thymol; and Group 2B which is comprised of crude oils that contain high relative abundances of methylphenols which can be derived from tocopherols. Group 3 crude oils have C(subscript)2-C(subscript)5 alkylphenol compositions dominated by ortho and para substituted phenols which are proposed to be formed from geosynthetic processes. Group 4 crude oils contain alkylphenol compositions in which the relative abundances of meta substituted compounds in six isomer classes are much greater than those expected from chemical equilibration. Group 5 comprises of samples which are biodegraded and as a consequence contain alkylphenols below the limit of detection. Group 6 crude oils contain very low concentrations of alkylphenols and comprises samples which are derived from source rocks that pre-date the widespread occurrence of land plants or contain negligible land plant input.Some alkylphenols in crude oil are structurally related to natural product precursors and therefore appear to be biomarkers. The monoterpenoid natural products carvacrol and thymol, or its rearrangement product 3-isopropyl-5-methylphenol, which occur in high relative abundances in Group 2A samples are such compounds. Because carvacrol and thymol occur widely in extant conifers and angiosperms, their presence in crude oils derived from source rocks deposited when these plant types were widespread suggests they also originate from these plants. A range of trimethylphenols and tetramethylphenols which occur in high relative abundances in Group 2B samples, are also ++ / reaction products obtained from heating alpha-tocopherol with aluminium smectite. This, together with the reported widespread occurrence of tocopherols in plant photosynthetic tissue and in sedimentary rocks, leads to the conclusion that tocopherols are likely precursors to these petroleum methylphenols.The lignin components of terrestrial plants also appear to be important precursors to petroleum alkylphenols. Strong evidence for this is provided by the observation that crude oils derived from source rocks which contain negligible higher plant input contain very low concentrations of kylphenols (Group 6). In order to determine the likelihood of lignins as precursors of petroleum alkylphenols, the phenol contents of coals of lignitic through to bituminous rank were examined. The unbound phenolic components of the lignite samples were analysed by isolating the phenols from their dichloromethane extracts, and the bound phenolic components were analysed by pyrolysis GC-MS. At lignitic rank the unbound methoxyphenols allowed taxonomical classification of the samples and the bound hydroxyphenols bore structural similarities to lignin moieties. The bound C(subscript)0-C(subscript)4 alkylphenol components of lignitic, subbituminous and bituminous coals in a sedimentary sequence were quantitatively analysed by isolating the phenols from their hydrous pyrolysates. In the coals of subbituminous and bituminous rank, the bound alkylphenol components could not easily be related to lignin precursors because molecular transformations of lignins are very severe at these ranks. The increases in the individual concentrations and relative proportions of alkylphenols with methyl and/or isopropyl substituent(s) in the ortho and para positions in the subbituminous coal pyrolysate were attributed to electrophilic methylation and isopropylation reactions occurring to lignin structures in ++ / coals during coalification. The dominance of ortho and para substituted methylphenols in coaly Group 3A crude oils which were also observed in the hydrous pyrolysates of coals suggests that the altered lignin structures in coals may be precursors of some of these petroleum methylphenols.Methylation, isopropylation and sec-butylation, are proposed as geosynthetic processes to account for the alkylphenol compositions of crude oils with phenol distributions dominated by ortho and para alkyl-substituted compounds (Group 3). Many crude oils show high relative abundances of ortho and para substituted C(subscript)1-C(subscript)5 alkylphenol isomers and some were also enriched in C(subscript)3-C(subscript)5 alkylphenols compared to kerogen pyrolysates. Because the alkylphenol products obtained from the laboratory alkylation of cresols have distributions which closely resemble those in these crude oils, it is proposed that similar alkylation processes occur in source rocks. Alkylation ratios reflecting the degree of methylation, isopropylation and sec-butylation, which were based on the relative abundance of the dominant alkylation products compared to their likely precursor ortho cresol, indicate that high levels of methylation occurred in crude oils over a wide range of maturities. In contrast, high levels of isopropylation and sec-butylation were observed only in mature samples. Selective dissolution of phenol isomers in crude oils by water contact was discounted as an explanation for the observed phenol distributions based on the relative distribution coefficients of phenols between isooctane and water.The alkylphenol compositions of the remaining crude oils appear to be produced from alteration processes occurring in the subsurface; these include oxidation and biodegradation processes. Oxidation of alkylphenols is proposed to account for the alkylphenol compositions of ++ / Group 4 crude oils. Because ortho and para substituted alkylphenols are more susceptible to oxidation than their meta substituted counterparts, the selective removal of these compounds via an oxidation process is suggested as an explanation for the high relative abundances of meta substituted isomers observed in these crude oils. A natural product origin for these compounds appears unlikely due to the lack of known natural products which could give rise to meta substituted alkylphenols with isopropyl substituents, and the diverse range of organisms required to give rise to the meta substituted phenols with n-alkyl substituents observed in Group 4 samples.Crude oils from two Australian basins which have undergone various levels of biodegradation were analysed to assess biodegradation effects on petroleum alkylphenol compositions. Alkylphenols could not be detected in the moderately to severely biodegraded crude oils (Group 5) whereas related non-biodegraded samples contained relatively higher levels of alkylphenols. The very low levels of phenols in the biodegraded samples (< 10 ppb) suggests that phenols are depleted via processes that occur during biodegradation. Because water washing often co-occurs with biodegradation, the very low levels of alkylphenols in these samples may also be due in part to the removal of these polar components via water dissolution.

No description available.

No description available.

Ce travail s'est focalisé sur le devenir des polybromodiphényléthers (PBDE) et des alkylphénols (AP) dans les filières de traitement des eaux usées des stations d'épuration Seine-Centre et Seine-Amont, en agglomération parisienne. Des prélèvements effectués par temps sec et par temps de pluie ont permis de déterminer la qualité des eaux brutes vis-à-vis des paramètres globaux, des PBDE et des AP, ainsi que l'efficacité des ouvrages de traitement primaire et secondaire. Par temps sec, les concentrations dans les eaux brutes de Seine-Amont sont en moyenne 6 et 2 fois plus élevées pour ∑6AP et ∑4PBDE respectivement. Un bassin-versant plus industrialisé sur Seine-Amont et une forte dilution dans le réseau de Seine-Centre expliquent ces différences. Par temps de pluie, la pollution est diluée sur Seine-Amont. A l'inverse, la pollution particulaire augmente sur Seine-Centre, à cause de l'érosion des dépôts présents dans le réseau. En traitement primaire, la décantation physico-chimique lamellaire sur Seine-Centre favorise nettement l'abattement des pollutions particulaires et organiques. Ses performances sont stables et bien plus élevées que la décantation classique sur Seine-Amont. Par temps de pluie, les performances des deux ouvrages sont conservées, voire améliorées, malgré une hausse des charges polluantes et des vitesses ascensionnelles. Aucun de ces ouvrages n'est adapté au traitement de la pollution dissoute. En traitement secondaire, des abattements élevés pour la biofiltration et les boues activées ont été obtenus. Les traitements des deux stations étudiées conduisent à des effluents secondaires de qualité globalement similaire, même si les concentrations en pollution particulaire et en PBDE restent plus élevées sur Seine-Amont. Par temps de pluie, le 3ème étage de la biofiltration est dérivé et aéré sur Seine-Centre. Cette configuration impacte principalement les nitrates et le BDE-209. Sur Seine-Amont, les performances des boues activées sont légèrement affectées mais restent généralement supérieures à 80 %. Ceci conduit à des concentrations dans les effluents secondaires par temps de pluie 1,4 à 3 fois plus élevées en moyenne pour la pollution particulaire et les PBDE / This study investigates the fate of polybromodiphenylethers (PBDE) and alkylphenols (AP) within two sewage treatment plants, Seine-Centre and Seine-Amont, located in Paris conurbation. Samplings were performed under dry and wet-weather flows to determine the raw water quality and the performances of the primary and secondary treatment. During dry-weather periods, mean concentrations of ∑6AP and ∑4PBDE in Seine-Amont raw sewage were respectively 6 times and twice higher. This is due to a highly industrialized watershed for Seine-Amont, and a strong dilution in Seine-Centre sewer network. Under wet-weather flows, the particulate pollution increases markedly in Seine-Centre raw sewage, due to the erosion of in-sewer deposits. As a primary treatment, the physico-chemical lamella settler in Seine-Centre clearly improves the removal of particulate and organic pollutions. Its performances are constant and much higher than normal settling in Seine-Amont. Under wet-weather flows, the performances of both techniques are maintained or improved, despite higher pollutant loads and ascensional velocity. The dissolved pollution is not removed in the primary treatment, whatever the process. In the secondary treatment, high removal is obtained for both biofiltres and activated sludge processes. Seine-Centre and Seine-Amont secondary effluents reach a similar quality, although particulate pollution and PBDE concentrations remain slightly higher in Seine-Amont. Under wet-weather flows, one stage of Seine-Centre biofiltration unit is derived and aerated. In these specific conditions, nitrates and BDE-209 removal is impacted. For activated sludge in Seine-Amont, performances are slightly decreased but remains over 80 % for most parameters. Hence, in Seine-Amont secondary effluents, PBDE pollution is from 1.4 to 3 times higher under wet-weather flows

Les phtalates et les alkylphénols sont des composés organiques générés par l'industrie chimique, qui entrent dans la composition des matières plastiques, pour les phtalates, et des détergents, pour les alkylphénols. Leurs productions mondiales avoisinent les 6 millions de tonnes pour les phtalates et 500 000 tonnes pour les alkylphénols. Ces composés sont considérés comme ubiquitaires dans l'environnement, c'est-à-dire qu'ils sont retrouvés dans tous les compartiments environnementaux (de l'atmosphère au milieu naturel). Par ailleurs, ils sont considérés comme des perturbateurs endocriniens et peuvent donc causer des dommages aux faunes et flores présentes dans le milieu naturel. Ce travail de thèse a permis de déterminer les niveaux de contamination des eaux usées en phtalates et alkylphénols dans plusieurs compartiments environnementaux situés en zone urbaine. Ainsi, des prélèvements effectués, par temps sec, ont permis de déterminer la qualité des eaux brutes vis-à-vis des paramètres globaux, des phtalates et des alkylphénols dans les rejets industriels, domestiques, les émissaires parisiens ainsi que dans les eaux usées transitant au sein d'une station d'épuration majeure d'Ile-de-France (Seine Centre, Colombes, 92). Ces résultats reflètent certaines spécificités et disparités du réseau d'assainissement, notamment marqués par la forte variabilité qui entoure, à la fois, le prélèvement et les niveaux de contamination par ces micropolluants. Au niveau des rejets industriels, de forts contrastes ont été observés entre les différents secteurs répertoriés (traitement des textiles, traitement de surface, métallurgie, industries pharmaceutiques, etc.). Globalement, les résultats des flux par équivalent-habitant soulignent que les apports domestiques sont la première source de contamination pour ces polluants en région parisienne. En effet, la contribution des apports industriels est inférieure à 5 %, pour tous les composés, quelque soit le secteur industriel considéré. L'étude des émissaires parisiens a permis de montrer une certaine stabilité temporelle de la qualité des effluents dans la partie avale du réseau d'assainissement. En revanche, cette étude a également mis en exergue des divergences et des similitudes entre les sous-bassins versants drainés par les différents émissaires. Ainsi, une étude statistique a montré que les émissaires Saint Denis Achères et Clichy Achères Argenteuil apparaissent significativement plus contaminés que les émissaires Sèvres Achères Reuil et Clichy Achères Bezons. Au niveau de l'efficacité des ouvrages de traitement, les résultats obtenus pour la station d'épuration de Seine Centre ont confirmé son efficacité pour les paramètres globaux communément utilisés pour déterminer la qualité des eaux usées. D'autre part, les résultats obtenus sur l'abattement des phtalates et des alkylphénols (rendements supérieurs à 83 % pour tous les composés) soulignent que même si les stations d'épuration ne sont, initialement, pas construites pour réduire et/ou éliminer les micropolluants, elles y parviennent de façon significative. A l'échelle des ouvrages, le traitement primaire par décantation physico-chimique lamellaire a permis de mettre en évidence l'élimination des polluants hydrophobes tels que le DEHP, le NP, le DnBP et le BBP. Le traitement secondaire par biofiltration a mis en exergue son efficacité à abattre significativement tous les polluants, aussi bien les composés légers (DEP) que les autres composés / Phthalates and alkylphenols are organic molecules generated by the chemical industry, entering the composition of plastics, for phthalates, and detergents for alkylphenols. Their worldwide productions are around 6 million tons and 500,000 tons, respectively. It is now obvious from the concentrations and contents measured in the various environmental compartments that phthalates and alkylphenols are ubiquitous environmental contaminants. Indeed, they are found in all environmental compartments (from the atmosphere to the natural environment) at significant levels. These contaminants are also recognized as endocrine disrupting compounds and can cause damages to fauna and flora present in the natural environment. This work has identified levels of wastewater contamination of phthalates and alkylphenols in various environmental compartments in urban areas. Thus, samples taken, during dry weather periods, were used to determine the quality of raw water for global parameters, phthalates and alkylphenols within industrial and domestical discharges as well as the sewer network and a major Parisian sewage treatment plant (Seine Centre, Colombes, 92). These results reflect certain characteristics and disparities of the sewer network, including both high variability of the sampling and the contamination levels by these micropollutants. For industrial discharges, significant disparities have been observed between the different sectors listed (textile manufacturing, surface treatment, metallurgy, pharmaceutical industries, etc.). Overall, the results confirm that household inputs correspond to the first source of contamination in Parisian conurbation. Indeed, the contribution of industrial inputs is less than 5%, for all compounds, whatever the industrial sector. The study of the Parisian sewer network showed some temporal stability of wastewaters in the downstream part. This work however also highlighted disparities and similarities between the sub-watersheds drained by the sewer network. Thus, the northern part of the Parisian network (SDA and CAA) appears to be more contaminated than the Southern part (CAB and SAR).The results obtained for Seine Centre wastewater treatment plant (WWTP) confirms the effectiveness of the treatment processes on the removal on the routine water quality parameters. Additionally, the results on the elimination of phthalates and alkylphenols in sewage treatment plant (yields above 83% for all compounds) confirm that even if WWTP are initially not designed for reducing and/or eliminating micropollutants, they proceed significantly. During primary treatment, physicochemical lamellar clarification underlined the removal of hydrophobic pollutants such as DEHP, NP, DnBP and BBP. During the secondary treatment, biofiltration highlighted its effectiveness in eliminating all pollutants, as well as volatile compounds (DEP) and other contaminants

La Directive Cadre sur l'Eau (DCE) (2000/60) a mis en place une liste de 33 substances prioritaires, avec des normes qualité de l'environnement (NQE) pour chaque substance, et leur concentration dans les milieux aquatiques qui ne doivent pas dépasser c es NQE. De plus, elle exige des performances analytiques spécifiques pour ces méthodes: la limite de quantification doit être au moins aussi basse que 30% des NQE et l'incertitude de la méthode au niveau de la NQE doit être inférieure à 50%, pour k = 2. Par conséquent, le défi analytique actuel est de mesurer de faibles concentrations de ces polluants dans les matrices parfois difficiles. Ceci peut être réalisé en améliorant la technique d'extraction utilisée pour obtenir un extrait de l'échantillon plus concentré et plus propre. Dans ce contexte, les trois méthodes d'analyse ont été mises au point pour déterminer les composés musqués, alkylphénoliques et organométalliques dans les matrices environnementales. Ces techniques d'extraction et de pré-concentration innovantes ont ensuite été appliquées pour l’évaluation de la présence de ces composés dans les stations d'épuration locales et dans les cours d'eau récepteurs. Enfin, les niveaux de concentrations de fond au niveau national ont été mises à jour pour les composés organométalliques. / The ambitious Water Framework Directive (WFD) (2000/60) set up a list of 33 priority substances, with Environmental Quality Standards (EQS) for each substance, and their concentration in aquatic environments should not go beyond the EQS. Additionally, it requires specific analytical method performances: the limit of quantification must be at least as low as 30 % of the EQS and the uncertainty of the method at the EQS level must be inferior to 50 %, for k=2. Therefore, the current analytical challenge is to measure low concentrations of these pollutants in sometimes difficult matrices. This can be achieved by improving the extraction technique used to obtain a more concentrated and cleaner sample extract. In this context, 3 analytical methods were developed to determine musk, alkylphenols and organometallic compounds in environmental matrices. Recent extraction and pre-concentration techniques were applied and later the occurrence of these compounds in the local WWTPs and in the receiving water bodies where they are discharged was evaluated. Additionally, updated French background concentrations were established for organometallic compounds.

<p>  This dissertation focuses on the examination of the influence of sample storage conditions on the accuracy and precision of hydrocarbon composition measurements of Jet A made with GC×GC/FID and the accuracy and precision of flash point measurements of Jet A made with a Tag closed cup flash point tester. Areas of focus also include the influence of the column load value used, the S/N threshold value used, and the number of measurements made for a single sample vial on the accuracy and precision of the GC×GC/FID results. This dissertation also describes the development of an analytical method for the identification and quantitation of alkylphenols in Jet A (which are the most abundant heteroatom containing compounds in jet fuel) by using preparative high-performance liquid chromatography (prep-HPLC) and two-dimensional gas chromatography with electron ionization time-of-flight mass spectrometry (GC×GC/(+)EI TOF MS).</p>

Dans le cadre de la protection de l’environnement et du consommateur, CTC effectue des tests enchimie analytique sur de nombreux paramètres en matrices aqueuses, cuir et textile. Les nouvelles substancesmises sur le marché ainsi que les réglementations évoluant sans cesse, le développement de nouvellesméthodes d’analyses est donc nécessaire.Plusieurs méthodes analytiques ont ainsi été développées. Pour l’analyse des rejets d’effluents industriels desinstallations classées et pour l’analyse d’innocuité de produits utilisant le cuir ou le textile (chaussures,maroquinerie, prêt-à-porter…).Les chloroalcanes ont été dosés en chromatographie gazeuse (GC) associée à la spectrométrie de masse (MS)utilisant l’ionisation chimique, à la fois en matrices aqueuses (limite de quantification, LQ, à 0,6 μg/l) et sur lescuirs (LQ à 2 mg/kg).Une analyse des alkylphénols et alkylphénols ethoxylates a été développée pour les matrices aqueuses parGC/MS (LQ à 0,05 μg/l).Plusieurs familles de retardateurs de flammes ont ensuite été étudiées. Les polybromodiphénylethers peuventêtre dosés dans les eaux (LQ<0,05 µl) et le cuir (LQ <= µg/kg), par GC/MS en ionisationchimique.L’hexabromocyclododécane et des organophosphates, par chromatographie liquide et spectrométrie de masseen tandem pour des matrices textiles (LQ à 6 mg/kg). Des hydrocarbures aromatiques polycycliques dans le cuir ont ensuite été analysés par GC/MS-MS (LQ à 250 μg/kg).Enfin, une méthode multirésidus portant sur plusieurs familles de micropolluants organiques a été mise aupoint en GC/MS pour les rejets d’effluents (LQ <0,1 µg/l) / Taking in account the increasing needs and demands in environmental and consumer protection, CTCis always seeking improvement in analytical methods and development of new ones dealing with leather,fabrics and aqueous samples. In this thesis, several new methods were developed to be able to handleanalytical requests dealing with leather and textile materials being parts of shoes, clothes and other leathergoods.A GC/MS method using chemical ionization was developed to detect short polychlorinated alkanes down to aconcentration of 0.6 μg/L in aqueous sample and 2 mg/kg in leather samples. Alkylphenols and theirethoxylates were similarly determined by GC/MS down to 0.05 μg/L.Flame retardants are another large class of chemicals becoming suspicious. Polybromodiphenylethers weredetermined in aqueous samples and leathers. The respective GC/MS highest limits of quantification (LOQ)were0.05 µg/l and 80 μg/kg. Other members of this class are hexabromocyclododecane andorganophosphates. Both were determined by LC/MS-MS with LOQ of about 6 mg/kg.Carcinogenic polyaromatic hydrocarbons were also determined in leather samples using GC/MS-MS down to250 μg/kg.The last improved GC/MS analytical method was handling sewage sludge seeking multi residues of organicpolluants down to the 0.1 µg/l level or below. The analytical performances developed or improved allowedfor an efficient and useful control of the various sample received from the CTC customers and followinginternational quality rules

Auf Basis moderner unabhängiger Analysenmethoden wurden selektive und spezifische Analysenverfahren für die Analytik von Phenolen, unter besonderer Berücksichtigung der Alkylphenole entwickelt, optimiert und teilweise validiert. Es wurden Verfahren für die Hochleistungs-Flüssigchromatographie - Massenspektrometrie (HPLC-MS), Hochleistungs-Flüssigchromatographie - Kernmagnetische Resonanzspektrometrie (HPLC-NMR), Gaschromatographie - Massenspektrometrie (GC-MS) und Kapillarelektrophorese (CE) entwickelt. Die HPLC-MS wurde mit den Atmosphärendrucktechniken "Electrospray Ionization" (HPLC-ESI-MS) und "Atmospheric Pressure Chemical Ionization" (HPLC-APCI-MS) eingesetzt. Die Gaschromatographie wurde in Kopplung zu einem hochauflösenden Massenspektrometer (GC-HRMS) und in Kopplung zu einem niederauflösenden Quadrupol-Spektrometer (GC-LRMS) verwendet. Mit der Kapillarelektrophorese wurden Verfahren in den Modi "Kapillar-Zonen-Elektrophorese (CZE) und "Micellare Electrokinetische Chromatographie (MEKC) mit verschiedenen internen Anreicherungstechniken ("Stacking") entwickelt. Für die Validierung des MEKC-Verfahrens mit interner Anreicherung ("Direktes-MEKC-Stacking") wurde ein Ringversuch organisiert und durchgeführt. Anhand von representativen Modellgemischen wurden die Verfahren geprüft und miteinander verglichen. Die Modellgemische sind reproduzierbar herstellbar; ihre Stabilität und Homogenität wurde abgesichert, so daß sie als synthetische Referenzmaterialien zur laborinternen Qualitätssicherung, zur Methodenbewertung und zum Laboratoriumsvergleich eingesetzt werden können. Anhand von charakteristischen Kenngrößen wie Bestimmungsgrenzen, Selektivität, Zeitaufwand, Kosten und Meßunsicherheiten wurden die Verfahren auf ihre Eignung als Standard- bzw. Referenzverfahren bewertet. Die Verfahren der HPLC-NMR, HPLC-ESI-MS, HPLC-APCI-MS und GC-HRMS können mit unterschiedlichem Einsatzbereich als Referenzverfahren für die Analytik von Phenolen eingesetzt werden. Die GC-HRMS ist dabei das leistungsstärkste Referenzverfahren. Die Verfahren der GC-LRMS und CE ("Direktes-MEKC-Stacking") sind als Standardverfahren geeignet und besitzen alle Voraussetzungen um auch als Normverfahren für die Analytik von Phenolen eingeführt zu werden. / Different selective and specific analysis procedures were developed for the determination of phenol derivatives, in particular alkylphenols, in environmental relevant matrices using High-Performance Liquid Chromatography - Mass Spectrometry (HPLC-MS), High-Performance Liquid Chromatography- Nuclear-Magnetic Resonance Spectrometry (HPLC-NMR), Gas Chromatography- Mass Spectrometry (GC-MS) and Capillary Electrophoresis (CE). HPLC-MS was used with atmospheric pressure ionization techniques, Electrospray Ionization (HPLC-ESI-MS) and Atmospheric Pressure Chemical Ionization (HPLC-APCI-MS). Analysis procedures for GC-MS were developed for a high resolution mass spectrometer (GC-HRMS) and a low resolution benchtop quadrupole mass spectrometer (GC-LRMS). CE was used in the Capillary Zone Electrophoresis (CZE) and Micellar Electrokinetic Chromatography (MEKC) mode with different internal stacking techniques. The MEKC procedure with internal stacking (called "Direct-MEKC-Stacking") was validated by an interlaboratory comparison test. These procedures were tested and optimized using representative model mixtures and the most efficient then validated. The model mixtures were produced reproducably and their stability and homogeneity were demonstrated for the application as synthetic reference materials, e.g. for internal laboratory control, quality assurance or method development. The different analysis procedures were categorized as standard- or reference procedures on the basis of characteristic properties, e.g. detection limits, selectivity, analysis time, cost and uncertainty. HPLC-NMR, HPLC-ESI-MS, HPLC-APCI-MS, GC-HRMS can be used as reference procedures for different fields of use. Best performance can be reached with GC-HRMS. GC-LRMS and "Direct-MEKC-Stacking" can be used as standard procedures for the analysis of phenol derivatives and they fulfill all conditions for their implementation in standardization.