共查询到18条相似文献,搜索用时 78 毫秒
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建立了可同时分析饮用水中铁、铜、镍、锌、钴、镉、锰等过渡金属离子的方法。优化后的离子色谱条件:选用 Dionex IonPac CS5A色谱柱(4 mm×250 mm),以7.0 mmol/L 吡啶-2,6-二羧酸+66 mmol/L KOH+74 mmol/L HCOOH+5.6 mmol/L K2SO4为淋洗液,流速为1.2 mL/min,柱温为30 ℃;以0.5 mmol/L 4-(2-吡啶偶氮)间苯二酚+1.0 mol/L 2-二甲醇胺+0.5 mol/L氨水+0.3 mol/L NaHCO3为衍生液,流速为0.7 mL/min,紫外检测器波长为520 nm。结果表明,该离子色谱柱对以上过渡金属具有很好的保留和分离效果,衍生后的紫外检测手段具有优异的灵敏度和选择性。该方法稳定性良好,连续进样5针的相对标准偏差均小于0.79%;标准曲线线性关系良好,r≥0.998 8;方法检出限低,Fe3+为0.8 μg/L,Fe2+为4 μg/L,Cu2+为0.8 μg/L,Ni2+为3 μg/L,Zn2+为2 μg/L,Co2+为0.9 μg/L,Cd2+为16 μg/L,Mn2+为6 μg/L;检测结果准确,低、中、高3个水平的加标回收率均大于91.5%。该方法适用于环境水体中过渡金属离子的定量分析。 相似文献
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水中草甘膦和氨甲基膦酸的柱前衍生-液相色谱方法研究 总被引:1,自引:0,他引:1
建立柱前衍生-液相色谱-荧光检测法同时测定水中草甘膦和氨甲基膦酸的方法。水样经芴甲氧羰酰氯衍生化后取上清液进样,采用ODS C18柱,以水(5 mmol/L乙酸铵)-乙腈作为流动相进行梯度洗脱,采用荧光检测器进行检测。实验通过加入柠檬酸三钠,解决了实际水样中金属阳离子的干扰问题。草甘膦和氨甲基膦酸在一定范围内线性良好(r=0.997 3~0.999 0),回收率为92.2%~102%,相对标准偏差为4.3%~8.5%,方法检出限为1.29μg/L和1.84μg/L。 相似文献
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次氯酸钠衍生-气相色谱法测定水中苦味酸 总被引:1,自引:0,他引:1
采用次氯酸钠衍生、毛细管柱气相色谱电子捕获检测器测定水中苦味酸,选择正己烷为萃取剂,萃取时间5 min,衍生反应时间40 min。方法在5.00μg/L~100μg/L范围内线性良好,检出限为0.2μg/L,空白加标水样平行测定的RSD为2.2%,加标回收率为89.6%~95.0%。 相似文献
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采用邻苯二甲醛柱前衍生5种氨基酸,用反向高效液相色谱法测定衍生化产物,通过优化衍生化条件和色谱条件,使该方法在0.25μmol/L~25μmol/L范围内线性良好。方法检出限为0.08μmol/L~0.12μmol/L,标准溶液测定6次的RSD为0.1%~1.2%,空白加标样的回收率为80.3%~115%。用该方法测定实际水样,5种氨基酸测定值均低于0.514μmol/L,加标回收率在75.5%~120%之间。 相似文献
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利用2,4-二硝基苯肼(DNPH)固相萃取在线吸附衍生高效液相色谱-二极管阵列(HPLC-PDA)测定环境空气中的22种羰基化合物,通过试验优化条件,使方法在6.00μg/L~1 800μg/L范围内线性良好,方法检出限为0.025μg/m~3~0.091μg/m~3,加标回收率为93.2%~108%,平行样相对标准偏差10%。 相似文献
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In this work, the experimental compatibility between the standard DNPH-HPLC method and the gas chromatographic (GC) method (without any derivatization) was investigated for the analysis of atmospheric carbonyls. In the latter case, GC analysis was made based on adsorptive enrichment on solid sorbents followed by thermal desorption. For a comparative analysis between the two methods, we quantified the concentration levels of acetaldehyde from gaseous combustion samples of different charcoal products. The acetaldehyde concentration data, measured by the HPLC method (643 ± 1,689 ppb), were approximately 10% lower than the GC-based method (722 ± 1,788 ppb). As such, the differences in the measured concentrations were statistically insignificant. Although the percentage difference of the two methods fell within a relatively wide range, the results obtained by the GC-based method were comparable to those of the HPLC method with significantly strong correlations. The GC-based method, if tested for certain carbonyl species such as acetaldehyde, appeared to be a suitable alternative for the HPLC method. 相似文献
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氯甲基甲醚(CMME)和二氯甲基醚(BCME)属于确认人类致癌物,因此,建立精准、绿色的CMME和BCME检测分析方法十分必要。基于2,4,6-三氯苯酚+乙醇钠+乙醇衍生化体系,利用气相色谱法(电子捕获检测器)测定了固定污染源废气中的CMME和BCME,并且系统地优化了采样条件、衍生化条件,确定了衍生化产物的结构及衍生比率。结果表明:工作曲线相关系数均大于0.990;当采样量为10 L时,检出限均为0.003 mg/m3;当实际样品加标量分别为0.010、0.100、1.00 mg/m3时,测定结果的相对标准偏差分别为15%~16%、8.9%~13%、10%~11%,加标回收率分别为89.2%~90.8%、75.3%~78.6%、76.5%~77.2%。 相似文献
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Stoichev T Rodriguez Martin-Doimeadios RC Amouroux D Molenat N Donard OF 《Journal of environmental monitoring : JEM》2002,4(4):517-521
The concentration levels of mercury (Hg) species in natural water samples are usually low. Consequently, accurate analysis with low detection limits is still a major problem. In this work, a method was applied for the simultaneous direct determination of dissolved mercury species in water samples by on-line hydride generation (HG), cryogenic trapping (CT), gas chromatography (GC) and detection by atomic fluorescence spectrometry (AFS). The suitability of the method for real samples with different organic matter and chloride contents was evaluated by recovery experiments in synthetic and natural spiked water samples. The HG method was compared with other current available methods for mercury analysis with respect to the different fraction of mercury analysed, i.e. 'reactive', 'reducible' or total. HG derivatization and SnCl2 reduction (with and without previous oxidation with BrCl) were applied to synthetic and natural (spiked and non-spiked) water samples. The influence of chloride and dissolved organic matter concentrations was studied. The results suggest that the HG procedure is suitable for the simultaneous determination of Hg2+ and MeHg+ in surface water samples. Inorganic mercury analysed by HG (i.e. reducible) is close to the total inorganic mercury. 相似文献
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对测定水中乙醛和丙烯醛的3种方法——2,4-二硝基苯肼衍生化法、顶空气相色谱法和吹扫捕集一气相色谱质谱法进行概述和总结,并对各方法的试验条件、方法原理、测定影响因素以及效能验证等分析、比对,突出表现各自的优势和特点。用3种方法同时测定实际水样,结果无显著差异,精密度、准确度满足监测要求。 相似文献
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环境二■英类污染物受到广泛关注,目前常用的二■英类物质检测方法有仪器分析法(高分辨率气相色谱-高分辨率质谱法)和生物检测法。生物检测法具有便捷高效、成本低廉等优点,但其测定值普遍高于仪器分析法,关键原因是生物检测法在前处理阶段未能完全消除非二■英类物质的干扰。改进了传统7-乙氧基-3-异吩恶唑酮-脱乙基酶(EROD)生物检测法的前处理方法,并利用改进后的EROD法与仪器分析法对相同环境样品进行检测,对比分析两种方法得到的二■英毒性当量数据。结果显示,改进后的细分前处理手段结合梨形烧瓶-Mix前处理手段能有效提高二■英类物质的回收率(接近100%),并且改进后的EROD法的检测结果与仪器分析法测定的二■英当量结果相当,说明通过改进前处理方法可以将生物检测法的准确度提高到与仪器分析法一致的水平。研究结论可为生物检测法在环境样品二■英类污染物检测中的应用和推广提供有效的数据参考。 相似文献
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建立了超声波萃取-醋酸酐原位衍生化-毛细管气相色谱同时测定鳌江表层沉积物中五氯酚和六氯苯的方法,优化了试验条件。方法线性范围为5μg/L-200μg/L,五氯酚和六氯苯的检出限均为0.5ng/g,沉积物标准物质的测定值符合质控要求,基质加标的平均回收率分别为77.7%和81.8%。 相似文献
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Hamid Reza Sobhi Ali Esrafili Hadi Farahani Mitra Gholami Mohammad Mehdi Baneshi 《Environmental monitoring and assessment》2013,185(11):9055-9065
A simple and sensitive method based on a modified hollow-fiber liquid-phase microextraction followed by gas chromatography–mass spectrometry has been successfully developed for the extraction and simultaneous derivatization of some nitrophenols (NPs) in soil and rain samples. Microwave-assisted solvent extraction was used for the extraction of NPs from the soil, while the rain sample was directly applied to the previously mentioned method. Briefly, in this method, the analytes were extracted from aqueous samples into a thin layer of organic solvent (dodecane?+?10 % tri-n-octylphosphine oxide) sustained in the pores of a porous hollow fiber. Then, they were back-extracted using a small volume of organic acceptor solution (25 μl; 10 mg/L N-methyl-N-(trimethylsilyl)trifluoroacetamide, as derivatization reagent, in acetonitrile) that was located inside the lumen of the hollow fiber. Under the optimized extraction conditions, enrichment factors of 255 to 280 and limits of detection of 0.1 to 0.2 μg/L (S/N?=?3) with dynamic linear ranges of 1–100 μg/L were obtained for the analytes. The accuracy of the approach was tested by the relative recovery experiments on spiked samples, with results ranging from 93 to 113 %. The method was shown to be rapid, cost-effective, and potentially interesting for screening purposes. 相似文献