土壤中有机化合物（SVOCs）检测方案(快速溶剂萃取)

智能文字提取功能测试中

Application NotePage 1 of 3ap0107Extraction of Semi-Volatile Organic Compounds from Soil in Accordance with EPA 3545 Extraction of Semi-Volatile Organic Compounds from Soil inAccordance with EPA 3545 Semi-Volatile Organic Compounds (SVOCs) are a subgroup ofVolatile Organic Compounds (VOCs) that have a high molecularweight and high boiling points. They are primarily composedof pesticides and herbacides. Prolonged exposure to thesecompounds， especially indoors， raises a public health concern.For example， many of these compounds have been listed by theUS EPA as hazardous air pollutants (HAPs). This classificationapplies to pollutants that can cause serious health effectssuch as： allergies， asthma， endocrine and thyroid disruption，reproductive toxicity， fetal and child development delays，andeven cancer. Soil is one of the most common matrices in which thesecompounds are present and the extraction of these compoundsfrom soil can be a lengthy and tedious process. The CEMEDGETM is a revolutionarily simple system for the rapidextraction of semi-volatile organic compounds (SVOCs) fromsoil that is more than six times faster than other automatedtechniques. With its patent pending Q-Cup TechnologyTM theEDGETM makes the extraction process fast and simple andmeets the requirements of EPA 3545. Semi-volatile organic compounds consist of substances with abroad set of chemical properties and structural features. Thesedifferences make it challenging to efficiently extract all analytesof interest with one method. Furthermore， the soil matrix fromwhich the SVOCs are to be extracted is often complex withmultiple components adding to the complexity of extraction. TheCEM EDGE with Q-Cup TechnologyTM can effectively extract adifficult set of analytes from complex matrices with one simplemethod. Traditional methods， such as soxhlet， are very time consumingand use a large amount of solvent. Automated methods oftenrequire tedious sample preparation with complex sampleholders. EDGE is the fastest exaction system available anduses a minimal amount of solvent. The Q-Cup sample holder iscomprised of two easy-to-assemble pieces allowing the sampleto be prepared in seconds. Due to their persistent nature， SVOCs continue to accumulateand concentrate in our environment. To ensure our safety，thesecompounds need to be extracted，identified，and quantified.The accuracy of SVOC analysis is dependent on an efficientextraction. EDGE yields an efficient extract that is filtered，cooled， and ready for analysis in under 5 minutes. EPA 3545 isa method for the extraction of water-insoluble or slightly water- soluble volatile and semi-volatile compounds in soils， clays， sediments， sludges， and waste solids. EDGE is meets the requirements ofEPA 3545 and is preprogrammed with the methodology. nstrumentation The EDGE uses Q-Cup Technology that combines the process of Pressurized Fluid Extraction and Dispersive Solid Phase Extraction in oneinstrument that yields rapid and efficient extraction. The easy-to-assemble Q-Cup sample holder offers a unique open cell concept thatcreates a dispersive effect and promotes rapid extraction and filtration. The result is fast， simple and efficient extractions. Sample preparation in the EDGE could not be easier. Simply place a Q-DiscTM into the Q-Cup base and screw the two parts together.Soil samples from 1 g to 30 g can be extracted and NaSO can be added to dry the sample if needed. The EDGE will use only 40 mL ofsolvent per extraction which includes solvent for diffusive extraction， sample rinse， and cleaning of the system. The rapid heating of theextraction chamber in combination with diffusive action allows a temperature of up to 180°℃ to be achieved in less than 2 minutes. Sample is Loaded The Q-Cup is automatically loaded into the chamber by the autosampler. The pressure cap then creates a pressurized seal onthe top of the Q-Cup. Solvent is Added Solvent is first added through the bottom to fill the gap betweenthe chamber and Q-Cup， this aids in heat transfer. Then， solventis added through the top of the Q-Cup to wet the sample. Chamber is Heated As the chamber walls are heated， the pressure in the gapincreases. This overcomes the pressure inside the Q-Cup，forcing the solvent to disperse into the sample. Extract is Collected Once the sample reaches temperature， the solvent isdispensed through the Q-Disc， the cooling coil， and into acollection vial. Procedure and Method 10 g of sand， loam， or clay spiked with 250 pl of spike solutionwas weighed into an assembled Q-Cup containing a Q-Disc. 10g of CRM 110-100 from Sigma Aldrich was also prepared. TheQ-Cups were placed in the EDGE removable rack each with acollection vial and the rack was slid into place on the EDGE.The One Touch MethodTM for EPA 3545 was used. The extractswere injected into the Agilent 7890A with a 5975C MSD foranalysis adhering to EPA 8270. A Phenomenex ZB-5MSplus 30m， 0.25 mm column was used. Sand，loam and clay purchased from Sigma Aldrich were spikedwith SPEX CertiPrep TCLP Base/Neutral/Acid Extractable SpikeSolution in Methylene Chloride， Part#：TCLP-BNA. CRM 110-110was purchased from Sigma Aldrich. CRM and Spiked sampleswere extracted via the EDGE and soxhlet. A 50/50 mixture ofacetone/hexane was used as the extraction and rinse solvent.The system was washed with hexane and acetone. Results and Discussion The EDGE extracted sand， loam and clay samples in under5 minutes， including： filtration， cooling， and system washing.No post clean up， solvent exchange or concentration wasnecessary. The extracts were directly injected into the GCMS foranalysis. The recoveries for all three types of spiked soil werecomparable to soxhlet. Table 1 is a table of the % recoveriesas compared to soxhlet from spiked soil of some difficult toextract semi-volatile organic compounds. The extraction of CRM110-100 via EDGE was also comparable to soxhlet as seen inTable 2. Table 1： % recovery data as compared to soxhlet for spikedsand， loam， and clay Analyte Sand (% Soxhlet) Clay (%Soxhlet) Soil (% Soxhlet) 1，4 dichlorobenzene 94 98 93 hexachloroethane 91 94 88 4-methylphenol 82 91 85 nitrobenzene 86 101 95 hexachlorobutadiene 94 97 89 2，4，5-trichlorophenol 87 76 81 2，4，6-trichlorophenol 92 73 86 2，4-dinitrotoluene 85 85 86 hexachlorobenzene 86 84 82 Table 2： % recovery data as compared to soxhlet forCRM 110-100 Compound % Soxhlet 2-nitroanaline 94 2，4-dinitrotoluene 114 dibenzofuran 92 fluorene 105 United States France Germany， Austria， Ireland (Headquarters) 33(01) 69 35 57 80 Switzerland +353 (0)1885 1752 800-726-3331 Fax： 33 (01)60 19 6491 (49) 2842-9644-0 Fax： +353(0) 1885 1601 704-821-7015 info.fr@cem.com Fax： (49) 2842-9644-11 info.ireland@cem.com Fax： 704-821-7894 info@cem.de info@cem.com Italy Japan United Kingdom WWw.cem.com (39) 35-896224 +81-3-5793-8542 (44)1280-822873 C2017 CEM Corporation All rights reserved. This may not be Fax： (39) 35-891661 Fax： +81-3-5793-8543 Fax： (44) 1280-822873 reproduced or published without info.srl@cem.com info@cemjapan.co.jp info.uk@cem.com written permission from CEM. C CEM Corporation 摘要    半挥发性有机化合物（SVOCs）具有较高的分子量和沸点 , 且 SVOCs 不易挥发， 主要由农药和除草剂组成。这些化合物日积月累暴露在外，和室内环境中，会留下很大的环境隐患， 导致公众卫生健康危害。所以被US EPA 列为有害空气污染物（HAPs），可导致过敏、哮喘、内分泌和甲状腺破坏、生殖毒性、胎儿和儿童发育迟缓、甚至是癌症。土壤是这些化合物最主要的基质，如何从土壤中将这些化合物萃取出来，是一个繁杂的过程。 CEM 公司革命性的 EDGE ™萃取系统，可从土壤中快速萃取出 SVOCs，其速度约是其他自动化技术的 6倍。专利 Q-Cup 技术™可简单、快捷、 有效地从复杂样品中萃取出待测物，EDGE 内置符合 EPA 3545 实验方法的标准程序。 简介土壤基质是含有多种组分的复杂样品， SVOCs 包括具有广泛化学特性和结构特性的多样化合物，其多样性将增加萃取过程的难度， 对于萃取技术是一巨大挑战。传统的方法如索氏提取，非常耗时且需要使用大量的溶剂。自动化方法往往需要繁琐的样品制备过程。EDGE 是目前可达到的最快的样品萃取系统，使用少量的溶剂即可实现样品萃取。Q-Cup 样品架由两个容易组装的部件构成，在几秒钟内即可准备好样品。半挥发性有机化合物（SVOCs）不易挥发， 这些化合物日积月累暴露在外，会留下很大的环境隐患，为了确保人类的安全，需要提取、识别、量化处理这些有害化合物，而 SVOCs 的精准分析完全取决于高效的萃取前处理技术。专利 Q-Cup 技术™可简单、快捷、 有效地从复杂样品中萃取出待测物，在 5min 内即可完成过滤、冷却和萃取产物的分析准备，EDGE 内置符合 EPA 3545 实验方法的标准程序，可在土壤、粘土、沉积物、污泥、固体废物中迅速有效萃取非水溶性 / 略水溶性挥发性化合物和半挥发性化合物。 仪器使用美国 CEM 公司发明了 EDGE 革命性萃取技术 , 完美结合了加压流体萃取法和固相离散萃取技术， 全自动过程包括试剂添加、萃取、过滤、冷却和分离过程， 萃取效率高， 重复性好。Q-Cup TM 独特的开放单元设计，在压力流动萃取基础上同时产生固相离散萃取的双效应，过程中动态压力振荡迫使试剂上下双向循环，增进了化合物析出效率，实现大量样品的快速萃取和过滤。 EDGE 使样品制备非常容易，Q-Disc ™滤膜置于 Q-Cup 底部，并将底盖旋好。可以迅速提取 1-30g 的土壤样品，如需要可以通过加入 NaSO4进行样品干燥。EDGE 仅使用 40mL 溶剂即可萃取反应，进行包括动态压力振荡离散萃取、样品浸润和系统清洗。工作腔快速加热，2min 内温度即可达到 180℃。过程与方法    向10 g的沙子，壤土和粘土中分别加入250µl配料溶液，并置于含有Q-Disc滤膜的Q-Cup中。准备10g的CRM110-100（西格玛Sigma Aldrich）。将Q-Cups放在EDGE移动支架上，支架置于EDGE的旁，每个支架旁都配有收集瓶。实验遵循EPA 3545一键式操作方法。将萃取液注入到安捷伦7890 A - 5975C MSD中，分析方法符合EPA 8270。色谱柱选择菲罗门ZB-5MSplus，30m/0.25mm。 样品沙子、壤土和粘土中分别加入SPEX CertiPrep TCLP碱/中性/酸可萃取的配料溶液，然后再将其加入到二氯甲烷中，其中沙子、壤土和粘土均从西格玛Sigma Aldrich 购买；SPEX CertiPrep TCLP溶液货号为TCLP-BNA。CRM110 - 100从西格玛Sigma Aldrich 购买。CRM和配料样品是通过EDGE和索氏提取得到的。50/50的丙酮/己烷混合物被用来萃取和清洗溶剂。丙酮和己烷也用来清洗反应系统。 结果与讨论EDGE 在5min内即可完成沙子、壤土和粘土样品的萃取，其中包括过滤、冷却和系统清洗过程。萃取液直接注入到GC-MS中进行分析。三种配料土壤样品的平均回收率与通过索氏提取所得到的结果相差无几。