非甲烷总烃样品保存时限探讨

非甲烷总烃在监测过程中,废气样品保存容器的选择和保存时间的长短对分析结果有重要影响。研究结果表明:使用玻璃注射器保存样品,应在8 h内完成分析;使用泰德拉惰性气袋保存样品,保存时间可延长至48 h,如废气中主要组分为沸点高于150℃的高沸点化合物,则应在8 h内完成非甲烷总烃的测定。     

气相色谱法检测废气中甲烷、非甲烷总烃的问题研究

气相色谱法检测废气中甲烷、非甲烷总烃的方法存在诸多问题。针对标准参考气体的选择、采样方式、样品保存、配气方式、仪器配置等方面做了重点研究。结果表明,使用甲烷作为标准参考气体最佳,根据污染源的实际状况,可选择动力采样或玻璃注射器手动采样。样品气保存在惰性气袋中比玻璃注射器更好,实验分析更推荐双柱配置的气相色谱,手工配制标准气系列、使用填充柱也可很好的满足检测的质量要求。     

采样罐和气袋保存116种挥发性有机物效果研究

为了提高挥发性有机物(VOCs)分析的准确性,笔者考察了3种采样罐和2种气袋对116种VOCs的保存效果。结果表明:VOCs在不同种类采样罐和气袋中的保存情况有一定差异,整体上Silonite采样罐的保存效果相对更稳定,罐内水分含量会对部分VOCs的保存效果造成影响(特别是对含氧有机物);保存实际样品时,能保证VOCs分析准确性的时间为12 d。     

全玻璃针筒注射器保存空气中甲烷和总烃的影响因素

采用全玻璃针筒取样/保存、双通道双毛细管柱测定非甲烷总烃分析方法,以甲烷标准气体样品、标准气体样品(TO-14、TO-15),以及3种实际环境空气样品为例,考察了全玻璃针筒注射器取样保存影响检测结果的若干因素。结果表明,样品的保存时间取决于以下因素:(1)样品性质,不同类型样品的保存时间差异大,化学反应活性强的样品,其总烃含量呈现先升高后降低趋势,甲烷则相对稳定;(2)样品浓度水平,相同条件下相同类型样品,浓度高的保存时间短于低浓度样品,如与环境空气浓度相仿的样品保存时间可超过60 h;(3)保存环境的避光程度,对于同一种VOCs标准气体样品,避光、半避光、非避光保存样品回收率迥异,趋势差别极大,对于部分样品即便是避光保存仍发现回收率变化极大;(4)全玻璃材质注射器的气密性,需对照技术规范要求,进行气密性的检查。     

便携式GC-MS法快速测定固定污染源废气中的VOCs

采用便携式GC-MS法快速测定固定污染源废气中VOCs,32种VOCs在2×10~(-7)~1×10~(-6)范围内线性良好,方法检出限为2×10~(-9)~1×10~(-8),标准气体样品6次测定结果的RSD为1.9%~19.1%,环境空气样品的加标回收率为66.2%~116%。在实际现场监测固定污染源中VOCs时,使用速查(Survey)功能可初步判断样品浓度,确定稀释倍数。比对试验结果表明,气袋和玻璃注射器采样法对VOCs测定结果无显著性差异。     

气袋采样-苏玛罐转移-GC/MS法测定废气中醛类恶臭物质

采用气袋采样-苏玛罐转移-GC/MS法测定废气中5种醛类恶臭物质,醛类同分异构体能够被完全分离、定性定量。保存时间验证试验表明,5种低浓度醛类在Tedler采样袋和PVDFs采样袋中能稳定存放12 h,高浓度醛类能较稳定地保存24 h,转移至苏玛罐中的样品能够稳定存放至少14 d。方法在4×10~(-10)～2×10~(-8)范围内线性良好,方法检出限为0.127μg/m~3～0.207μg/m~3,混合标气6次测定结果的RSD为3.4%～8.8%,加标回收率为103%～114%。     

预冷冻浓缩系统与气相色谱-质谱联用测定空气中挥发性有机物

采用预冷冻浓缩系统和气相色谱-质谱联用,建立了测定空气中39种挥发性有机物的分析方法,该法用苏玛罐或Tedlar气袋采集空气样品经-160℃液氮预冷冻浓缩后,用GC-MS检测.该方法采样简便,灵敏度、准确度高,已应用于室内空气和环境空气的测定,取得满意的结果.     

恶臭真空瓶洗脱设备的开发与应用

当前我国大部分环保部门恶臭的采样设备为真空瓶,再次使用时需要对真空瓶进行洗脱处理,传统的化学试剂处理和高温蒸煮均有各自的缺点及不便。现以蒸汽发生器为基础,开发了一套洗脱设备用于恶臭真空瓶处理,并对效果进行的验证,实验证明该法优于上述两种方法。     

挥发性有机物气体污染源监测中直接采样法的评价

挥发性有机物气体污染源监测中 ,采样与样品的保存是极其关键的环节 ,文中评价了两种材质的塑料采样袋对样品保存的影响 ,并与玻璃针筒进行比较 ,讨论了塑料袋和玻璃针筒采样中导致样品浓度衰减的主要因素     

手工静态顶空法测定水中挥发性卤代烃的操作关键

测定水中挥发性卤代烃,国家标准推荐使用的方法是手工静态顶空法,但在实际操作时,精密度和准确度不易得到保证,操作关键除了《水和废水监测分析方法》（第四版）提到的平衡温度、平衡时间和顶空瓶的密闭性外,取样注射器表面对样品有吸附,对测定结果有影响。将注射器进行脱活处理后,即能解决玻璃表面的吸附问题。     

VOCs在线监测系统与SUMMA罐采样-气质联用法的比对分析

将挥发性有机污染物在线监测系统与实验室内SUMMA罐采样气质联用法(GC-MS)的挥发性有机物分析进行了标准气体和实际空气样品的分析比对,并对偏差原因作分析,提出在线监测系统的维护建议。结果表明,挥发性有机物在线监测系统的监测结果与实验室方法有一定的可比性,可用于大气中挥发性有机污染物的在线监测。     

苏玛罐采样-GC-FID/MS同时测定环境空气中多种VOCs

采用苏玛罐采样-大气预浓缩仪结合气相冷柱箱与Deans Switch中心切割技术,将C 2~C 3组分切割至HP-PLOT/Q+PT柱,用FID检测器分析,其余组分通过DB-1柱子分离后进入质谱分析,实现1次进样同时测定环境空气中57种PAMS和65种TO-15。结果表明:108种VOCs在0.15 nmol/mol~8.0 nmol/mol范围内线性良好,检出限为0.04μg/m^3~2.8μg/m^3,相对响应因子的RSD<30%。     

Stabilities of 58 volatile organic compounds in fused-silica-lined and SUMMA polished canisters under various humidified conditions

Fused-silica-lined (FSL) canisters and SUMMA polished (SUMMA) canisters were compared for the recoveries and the stabilities of 58 volatile organic compounds (VOCs) at low ppbv (volume/volume) levels under various humidified conditions using a three-stage preconcentration method followed by GC-MS analysis. The target VOCs included non-polar VOCs (e.g. halogenated hydrocarbons and aromatic hydrocarbons) and polar VOCs (e.g. alcohols, ketones, esters, ethers, nitriles and thiols). The three-stage preconcentration method was initially optimized for simultaneous analysis of non-polar and polar VOCs because determination of canister stability is dependent on the accuracy of analytical measurements. The method showed good linearity over the concentration range from 1 to 25 ppbv for all target analytes, and the correlation coefficients were higher than 0.9974. The method detection limits ranged from 0.023 to 0.39 ppbv. The test mixtures loaded in both type of canisters (n = 3) had concentrations of 1.7-2.5 ppbv per compound at ambient pressure under various humidified conditions (%RH = 1.6, 8.0, 27, 39, 53 and >99% with excess water present). All canister samples were initially analyzed on day 0 (after 6-12 h). The effect of competitive adsorption of water vapor and polar VOCs on active sites of interior surface was remarkably observed for SUMMA canisters. Polar VOCs had a greater requirement for water vapor to be present. The RH percentages that ensured good recovery on day 0 were RH > 8% for non-polar VOCs and RH > 27% for polar VOCs (except alcohols under the condition of RH > 99%). All thiols were not recovered from SUMMA canisters under all conditions. FSL canisters showed good recoveries of more than 86% for all VOCs under all conditions on day 0 (except alcohols under the condition of RH > 99%). The recoveries of alcohols in both canisters under the condition of RH > 99% displayed relatively low recoveries in the range 25-76% because of the partitioning effect into condensed water. The canister samples under the conditions of RH 8.0, 27, 53 and > 99% were analyzed for the stability test on days 3, 7, 14 and 28 after loading. All non-polar VOCs were reasonably stable in the FSL canisters under all examined conditions over 28 days. However, several polar VOCs that have relatively lower vapor pressure, e.g. MIBK, butyl acetate and alcohols except ethanol, showed unstable characteristics under relatively dry conditions (RH 8 and 27%) during 28 days. RH > 53% was needed to ensure good stabilities of all analytes except thiols with the recoveries of > 80% over 28 days for both canisters. Although the FSL canister showed good recoveries of more than 86% for thiols on day 0, drastic degradations were observed after day 3 and they were not detected after day 14.     

静态顶空气相色谱法顶空装置的改进

水中三氯甲烷和四氯化碳的气相色谱分析,无论是检测自来水的标准方法还是环境监测统一方法,都规定为顶端空间气相色谱法.新近文献报道测定硝基苯类化合物也采用顶端空间法.在这些方法中都使用50ml比色管作为气液平衡瓶,比色管用医用反口橡皮塞封口,本改进设计了玻璃球封口比色管作为气液平衡瓶,利用乳胶管中玻璃球的滚动来达到密封针孔的目的,从而提高了分析方法的精密度和准确性.     

含锑工业废水的样品保存方法研究

选取5-Br-PADAP光度法和原子吸收法分析预处理后水样的保存效果，经检测发现利用HNO，-HC1溶液作为固定剂，调节pH〈1后在无色玻璃瓶中贮存的样品，常温下可保存31d，锑回收率达95％以上，同时前处理带入的干扰离子最少，能够满足验收废水监测中质量控制要求。     

气相色谱-质谱法快速筛查气态制冷剂产品中的热点管控类卤代烃

建立了利用气相色谱-质谱法快速筛查气态制冷剂产品中的10种热点管控类卤代烃的分析方法。采用气密性微量注射器对气态制冷剂样品进行取样,刺透瓶盖隔垫加入到顶空瓶中,自动进样;以GS-GasPro(多孔层开管,60 m×0.32 mm)为色谱柱,采用电子轰击离子源,全扫描模式采集。测试结果显示:目标物的体积分数在0.50%~100.00%范围内,相对响应因子的相对标准偏差(RSD)均小于20%;线性相关系数r均在0.999以上;检出限(3.143倍标准偏差)为0.01%~0.05%。对实际样品进行加标回收,回收率为79.5%~102%,测定值RSD为0.5%~3.1%。该方法可为快速、准确、批量筛查气态制冷剂产品中的多种热点管控类卤代烃提供技术支撑。     

抗坏血酸溶液配制方法的改进

磷钼蓝法测定水中总磷，所用的抗坏血酸溶液很不稳定，只能保存数周。为延长抗坏血酸溶液的有效使用时间，节约试剂、提高工作效率，提出改进抗坏血酸溶液的配制方法，即在配制抗坏血酸溶液时，加入适量的EDTA和冰乙酸。经实验，该溶液贮于棕色玻璃瓶，放在冰箱中可稳定3个月，使用效果符合测定要求。     

环境空气中VOC_S在线监测法与SUMMA罐采样气相色谱-质谱法比对研究

定性比较了环境空气VOCs在线监测法和SUMMA罐采样GC-MS法的基本原理、检测化合物种类和适用范围,并对标样实验、日均浓度、小时浓度从统计学角度进行了定量比对.研究表明,VOCs在线监测法监测结果与实验室方法有较好可比性,可用于相关领域VOCs的连续监控.     

A comparison of sampling and analysis methods for low-ppbC levels of volatile organic compounds in ambient air

A carefully designed study was conducted during the summer of 1998 to collect samples of ambient air by canisters and compare the analysis results to direct sorbent preconcentration results taken at the time of sample collection. Thirty-two 1 h sample sets were taken, each composed of a "near-real-time" sample analyzed by an autoGC-MS XonTech 930/Varian Saturn 2000 system, and Summa and Silco canisters. Hourly total non-methane organic carbon (TNMOC), ozone, and meteorological measurements were also made. Each canister was analyzed on the autoGC-MS system for a target list of 108 volatile organic compounds (VOCs) and on a manual cryosampling GC-FID system. Comparisons were made between the collection and analysis methods. Because of the low sample loading (150-250 ppbC TNMOC), these comparisons were a stringent test of sample collection and analysis capabilities. The following specific conclusions may be drawn from this study. Reasonable precision (within 15% mean difference of duplicate analyses from the same canister) can be obtained for analyses of target VOCs at low-ppbC concentrations. Relative accuracy between the GC-MS and GC-FID analysis methods is excellent, as demonstrated by comparisons of analyses of the same canisters, if measurements are sufficiently above the detection limits. This is especially significant as the GC-MS and GC-FID were independently calibrated. While statistically significant differences may be observed between the results from canister and near-real-time samples, the differences were generally small and there were clear correlations between the canister results and the near-real-time results. Canister cleanliness limits detection below the EPA Method TO-14 acceptance standard of 0.2 ppbv (0.2-2 ppbC for target analytes).