Problems in the Extraction of Polycyclic Aromatic Hydrocarbons from Diesel Particulate Matter

In this work, a comparison between Soxhlet, ultrasonic, and microwave-assisted extraction (MAE) (using hexane:acetone 1:1) of polycyclic aromatic hydrocarbons (PAHs) from SRM 1650 diesel particulate matter was made. As good recoveries were not obtained for the higher molecular weight compounds, MAE with toluene and dichloromethane was also tested. Achieved recoveries were compared with the results obtained in the same assays made with SRM 1648 urban particulate matter and real atmospheric particulate samples. In order to explain the difficulty of the extraction of PAHs from SRM 1650 in comparison to SRM 1648 and real atmospheric particulate samples, elemental analysis, X-ray diffraction, and particle analysis using scanning electron microscopy coupled to an automatic computer imaging system were also made. It is important to notice that SRM 1650 shows a high percentage of carbon and differences in the morphology of the particles between SRM 1650 and SRM 1648 were observed.     

Standard Reference Materials (SRMs) for the Determination of Polycyclic Aromatic Compounds--Twenty Years of Progress

In 1981 the National Bureau of Standards, now the National Institute of Standards and Technology (NIST), issued the first natural matrix Standard Reference Material (SRM) for the determination of polycyclic aromatic compounds (PACs), SRM 1580 Organics in Shale Oil. In the next 10 years, additional natural matrix SRMs were developed including air and diesel particulate matter, petroleum crude oil, coal tar, sediment, and mussel tissue. The SRMs represented the "first generation" of natural matrix SRMs for the determination of PACs. The SRMs had "certified" values for only 5 to 12 PACs; however, their development established the foundation for the implementation of the "two or more independent analytical techniques" approach for certification of individual PACs in environmental matrices. The requirement for use of different analytical techniques spurred the development of both gas chromatography (GC) and liquid chromatography (LC) approaches for the determination of PACs. Since the mid-1990s, the "second generation" of natural matrix SRMs has been issued by NIST with certified values for over 20 PACs in each material. The greater number of certified values in these SRMs was the result of the combination of measurements using reversed-phase LC with fluorescence detection, multidimensional LC, and GC with mass spectrometric detection using two or more stationary phases with different selectivity for polycyclic aromatic hydrocarbon (PAH) separations. This article discusses the significant developments in analytical methods and chromatographic separation of PAHs during the past 20 years that have resulted in the certification of over 25 SRMs, which are now used worldwide for the validation of analytical methods for the measurement of PACs in environmental matrices.     

Recertification of Standard Reference Material (SRM) 1649, Urban Dust,for the Determination of Polycyclic Aromatic Hydrocarbons (PAHs)

The National Institute of Standards and Technology (NIST) recently issued SRM 1649a, Urban Dust, with certified and reference values for 44 polycyclic aromatic hydrocarbons (PAHs). This material is a recertification of SRM 1649 which was issued in 1982 with certified values for only five PAHs. The PAHs were determined using the following analytical techniques: (1) reversed-phase liquid chromatography with fluorescence detection (LC-FL) for analysis of the total PAH fraction, (2) reversed-phase LC-FL for analysis of isomeric PAH fractions isolated by normal-phase LC (i.e., multidimensional LC), and (3) gas chromatography/mass spectrometry (GC/MS) for analysis of the PAH fraction using three different stationary phases, each with different selectivity for PAH separations. The results from the different techniques are compared and discussed. SRM 1649a is currently the most extensively characterized environmental matrix SRM with respect to PAH constituents.     

车用汽柴油中硫成分分析标准物质的研究进展

随着世界各国对环境问题的普遍重视,以及汽柴油标准的不断升级和油品质量检测技术的逐步完善,我国对低硫含量汽柴油标准物质的需求日趋迫切。油品中硫含量过高,大大降低了催化转换器中催化剂效率,增加了车辆污染物的排放量。含硫汽柴油标准物质的研制,是制定汽柴油国家强制标准的急需,是有效控制大气污染的急需,是保障交通安全的急需,对元素分析仪器的校准、汽柴油硫含量检测和定值等方面起到极其重要的作用。旨在通过对国内外车用汽柴油质量标准硫含量现状和发展趋势的分析,拟为汽柴油中硫元素标准物质的研制及快速准确地对汽柴油中硫含量的检测,提供必要依据和借鉴。     

High-Molecular-Weight Polycyclic Aromatic Hydrocarbons in the Area and Vicinity of the Deza Chemical Plant,Czech Republic

Polycyclic aromatic hydrocarbons (PAHs) with molecular weight exceeding 278 amu were analyzed in air, water, and soils from the area and vicinity of the DEZA Chemical Plant (Vala w ské Mezi q í ) í, Czech Republic). Air and water were sampled using semipermeable membrane devices (SPMDs); grab sampling was applied for soils. Laser desorption/ionization-time-of-flight mass spectrometry (LDI-TOF MS) and liquid chromatography/ion trap mass spectrometry with atmospheric pressure chemical ionization (LC/APCI-ITMS) were employed for the quick assessment of PAH distribution and for the identification and quantification of some high-molecular-weight PAHs. Compounds with molecular mass up to 450 u were found. LDI-TOF mass spectra and selected LC/APCI-ITMS profiles (m/z 303, m/z 327, and m/z 351) were compared to identify potential source of contamination in this locality. High-molecular-weight PAHs were found in all environmental compartments in the area studied; their levels were quite high close to their source and decreased sharply with increasing distance from it.     

Liquid Chromatographic Determination of Polycyclic Aromatic Hydrocarbon Isomers of Molecular Weight 278 and 302 in Environmental Standard Reference Materials

Abstract

Polycyclic aromatic hydrocarbons (PAHs) of molecular weight (MW) 278 (dibenzanthracene isomers) and 302 (dibenzopyrene/dibenzofluoranthene isomers) are seldom measured in environmental samples. A multidimensional liquid chromatography (LC) procedure was developed for the quantification of isomers of MW278 and 302. The multidimensional LC procedure consists of normal-phase LC to isolate the PAH isomer groups followed by analysis of the isomeric groups by reversed-phase LC with fluorescence detection. Using the multidimensional LC procedure, six isomers of MW 278 and nine isomers of MW 302 were quantified in four environmental Standard Reference Materials (SRMs): coal tar (SRM 1597), air particulate matter (SRMs 1648 and 1649), and marine sediment (SRM 1941).     

中、美、欧盟压力容器标准／规范对材料规定的比较分析

从材料的选择、制造和用途等方面对我国压力容器标准／法规、ASME《锅炉和压力容器规范》和PED指令／EN标准进行了对比分析,阐述和分析了3个标准体系中相关标准时材料控制的相互对应关系和主要差别,旨在探讨如何深入理解和使用ASME《锅炉和压力容器规范》和PED指令／EN标准中有关材料控制的规定。