COD_(Mn)二次取样体积的确定

标准分析方法中规定,锰法测定COD,所取水样体积,应使最终回滴过量的草酸钠标准溶液所消耗的高锰酸钾溶液的体积(以下简称耗量)在4～6ml之间。由于其范围较窄,在实际工作中,特别是对于污染较严重的地面水,要达到这一要求往往需要多次反复。在第一次耗量超出范围后,一般凭经验估计第二次取样体积。这种估计存在着较大的盲目性,可能还会超出范围,以致再行三次、四次取样,既费时,又耗试剂。为此,本文总结出COD_(Mn)二次取样体积的经验公式,据此二次取样一般都能成功。     

环境样品稀释方法的原则

文中从环境样品稀释步骤的选择，量器的选择及取样体积的确定3个方面来论述如何减少环境样品稀释的误差。     

冷原子荧光法测汞操作方法的改进

通过监测实验,对冷原子荧光法测定汞的操作方法进行了改进,采用密闭进样,先加还原剂和多次通气使仪器读数回零的操作方法,其数据的重复性和再现性均可满足实验室允许差的要求,同时采用校准曲线点进样体积中汞含量与峰值读数关系绘制校准曲线,避免了试样制备取样体积,还原瓶进样体积和稀释进行体积而引起计算上的混乱。     

水中放射性核素锶-90测量不确定度的评估

阐述了分析放射性核素产生不确定度因素比一般化学分析多的原因，通过采用鱼骨图法分析放射性核素锶-90测量实验中的不确定度和分析计算公式中的有关参数，了解到分析水中放射性核素锶-90时，主要受到样品测量、仪器探测效率、样品化学回收率和样品取样体积等4个方面的不确定度因素影响。     

工业废水BOD5测定中取样体积的探讨

对于工业废水和生活污水,在BOD_5测定中,由于可被生物降解的有机物含量较高,而溶解氧却很少,不能满足五天生化过程所消耗的氧量,必须用稀释水(或接种稀释水)稀释后培养测定,现行标准分析方法[1]要求,稀释程度应使五天培养中所消耗的溶解氧大于 2mg/L,剩余溶解氧大于1mg/ L。可见,在 BOD_5测定中确定取样体积是一个很关键的技术问题。目前,关于计算取样体积(或稀释倍     

气相色谱法测定水中吡虫啉和氟虫腈

采用液液萃取、气相色谱氮磷检测器同时测定水中吡虫啉和氟虫腈,以二氯甲烷为提取溶剂,考察了提取酸碱条件的影响.吡虫啉和氟虫腈分别在1.00 mg/L ～ 20.0 mg/L和0.500 mg/L-10.0 mg/L范围内线性良好,检出限分别为0.018 mg/L和0.004 mg/L(按取样体积200 mL,定容体积5 ...     

石墨炉原子吸收光谱法测定土壤中银

建立了土壤样品中痕量银的石墨炉原子吸收光谱测定方法,优化了试验条件,标准曲线线性关系良好,当取样质量为0.25 g,定容体积为25 mL时,方法检出限为0.01 mg/kg.经标准样品验证,方法准确度符合土壤样品分析要求.     

微波消解石墨炉原子吸收法测定土壤和沉积物中的铍

以氯化钯为基体改进剂，采用微波消解石墨炉原子吸收法测定土壤和沉积物中的铍，优化了微波消解条件，考察了共存元素对测定的干扰。方法在0μg／L～4．00μg／L范围内线性良好，检出限为0．01μg／g（以取样质量0．2000g、定容体积50mL计），标准样品平行测定的RSD为3．5％～6．7％，实际样品的加标回收率为84．0％-113％。     

硬质聚氨酯泡沫和组合聚醚中消耗臭氧层物质的便携式GC-MS测定方法

建立了便携式顶空/气相色谱-质谱法测定硬质聚氨酯泡沫和组合聚醚中一氟三氯甲烷（CFC-11）、二氟二氯甲烷（CFC-12）、二氟一氯甲烷（HCFC-22）及一氟二氯乙烷（HCFC-141b）的定性分析方法，系统考察了色谱柱、顶空体系、顶空温度和顶空时间对测定结果的影响。结果表明，DB-WAX色谱柱对目标物质的分离效果最好，顶空温度为50℃、顶空时间为10 min条件下，目标物质的检测灵敏度最高。在优化条件下，硬质聚氨酯泡沫取样体积为1 cm³时，4种目标物的方法检出限为0.6~0.8 μg；组合聚醚取样量为10 mg时，4种目标物的方法检出限为0.5~0.6 μg。该方法具有较高的灵敏度，定性准确，适用于实际样品的现场快速定性分析。     

生化需氧量测试方法稀释比的改良

由污水常规监测及实验室内质控样的分析结果,进行比较分析,获取经验常数,确立BOD_5与CODcr存在线性关系,可由CODcr计算BOD_5的近似值,引用经验公式,直接确定取样体积,对BOD_5常规测试方法进行了改良,以达到降低工作强度,提高监测人员工作效率的目的。     

取样量与烘干时间对总悬浮物测定结果的影响

就取样量和烘干时间两个因素的变化对总悬浮物测定结果的影响程度进行了探讨。结果表明 ,取样量是造成悬浮物测定结果准确与否的主要因素 ,而不同的烘干时间对测定结果的精密度不会造成明显的影响。随着取样量的逐步减少 (从 2 0 0 0 ml减至 50 ml) ,平行样的相对偏差则从 2 7%上升到 4 5 5%。为了使相对偏差≤ 1 5% ,取水量必须满足其中的总不可滤残渣达到 6 2 mg以上。     

环境空气采样流量标定方法误差分析及校正换算

由于压力和温度的变化,使得校正态下标定的流量与采样态实际流量不符,会给采样体积计算带来偏差。通过转子流量计流量计算公式和理想气体状态方程推导出了采样态体积与校正态体积之间的换算公式,并结合实例进行了计算,分析了采用和不采用公式计算两者之间的误差。     

DNPH衍生化采样-溶剂解析-高效液相色谱法同时测定木制品中25种醛酮化合物

建立了DNPH衍生化采样-溶剂解析-高效液相色谱测定木制品中醛酮化合物的方法。采样时需在2,4-二硝基苯肼吸附管前串联一只SEP-PAK脱臭氧小柱;采样体积应≤10 L,流量≤400 m L/min。该法对25种醛(酮)化合物对应的衍生物分离效果良好,在0.005~3 mg/L范围内线性良好,相关系数R2≥0.999 6,回收率为85.3%~113.5%,精密度为2.67%~4.56%。采样量为10 L时,25种醛(酮)化合物的检出限和定量限分别≤0.16和0.50μg/m3。     

浮游动物DNA宏条形码多样性监测采样方法研究

浮游动物是水生生态系统的重要组成部分,对环境因子敏感,是水生生态健康状况的重要指示生物.基于传统形态学的浮游动物调查方法无法鉴定桡足类幼体,难以准确了解浮游动物群落组成.DNA宏条形码技术基于DNA序列差异识别物种,为浮游动物群落组成的准确解析提供了新方法.比较了不同浮游动物采样方法(直接过滤法和网富集法)对浮游动物D...     

Performance of semipermeable membrane devices for sampling of organic contaminants in groundwater

Lipid-filled semipermeable membrane devices (SPMDs) are receiving increasing attention as passive, in situ samplers for the assessment of environmental pollutant exposure. Although SPMDs have been successfully used in a variety of field studies in surface waters, only a few studies have addressed their characteristics as groundwater samplers. In this study, the performance of the SPMDs for monitoring organic contaminants in groundwater was evaluated in a pilot field application in an area severely contaminated by chemical waste, especially by chlorinated hydrocarbons. The spatial distribution of hydrophobic groundwater contaminants was assessed using a combination of passive sampling with SPMDs and non-target semiquantitative GC-MS analysis. More than 100 contaminants were identified and semiquantitatively determined in SPMD samples. Along the 6 field sites under investigation, a large concentration gradient was observed, which confirms a very limited mobility of hydrophobic substances in dissolved form in the aquifer. The in situ extraction potential of the SPMD is limited by groundwater flow, when the exchange volume of well water during an exposure is lower than the SPMD clearance volume for the analytes. This study demonstrates that SPMDs present a useful tool for sampling and analyzing of groundwater polluted with complex mixtures of hydrophobic chemicals and provides guidance for further development of passive sampling technology for groundwater.     

TSP-PM10-PM2.5-2型中流量大气颗粒物采集系统的开发和应用

自行开发并研制了TSP-PM10-PM2.5-2型中流量TSP、PM10、PM2.5大气颗粒物采集系统,是目前中国唯一可以采集TSP、PM10、PM2.5样品并提供足够的样品量进行大气颗粒物化学成分分析的中流量大气颗粒物采集器.该系统精心设计和加工的限流孔可以保持完全固定的流量,保证切割粒径的稳定,减小采样的误差并方便操作.该系统已经成功地应用于20多个城市和地区大气颗粒物的监测和研究中,为研究大气颗粒物的污染状况和来源提供了有效的技术手段和支持.     

Performance optimisation of a passive sampler for monitoring hydrophobic organic pollutants in water

The performance of an integrative passive sampler that consists of a C18 Empore disk sorbent receiving phase fitted with low density polyethylene membrane was optimised for the measurement of time-weighted average concentrations of hydrophobic micropollutants in water. A substantial improvement of sampling characteristics including the rate of sampling and the sampling precision was achieved by decreasing the internal sampler resistance to mass transfer of hydrophobic organic chemicals. This was achieved by adding a small volume of n-octanol, a solvent with high permeability (solubility [times] diffusivity) for target analytes, to the interstial space between the receiving sorbent phase and the polyethylene diffusion-limiting membrane.     

Integration of high volume portable aerosol-to-hydrosol sampling and qPCR in monitoring bioaerosols

In this study, the integration of a high volume, portable aerosol-to-hydrosol sampling technique and quantitative polymerase chain reaction (qPCR) was investigated for bioaerosol monitoring by adapting the RCS High Flow to sample air with mineral-oil-strips. Bacillus subtilis var niger and Pseudomonas fluorescens were aerosolized and collected by the RCS High Flow loaded with mineral-oil-strips for 1, 2 and 5 min. In addition, the adapted aerosol-to-hydrosol sampler was also tested for sampling environmental bacterial aerosols in four different environments (a back yard, a student dorm, a dining hall, and a play ground). The performances of the RCS High Flow with mineral-oil-strips were compared with the use of agar strips under similar conditions in all experiments. Air samples collected by the RCS High Flow were cultured, and in addition those collected with mineral-oil-strips were also quantified using qPCR. When sampling B. subtilis var niger aerosols, the use of mineral-oil-strips was shown to report significantly higher culturable concentrations than those obtained by agar strips regardless of the sampling time tested (p-value = 0.04). In contrast, the differences between the two methods when sampling P. fluorescens aerosols were not statistically significant (p-value = 0.5). When coupled with qPCR, the RCS High Flow loaded with mineral-oil-strips obtained significantly higher bacterial aerosol concentrations than those detected by the culturing method. The sampling time was observed to have negligible effects on the efficiency of the technology developed here. When sampling in different environments, the use of mineral-oil-strip was observed to yield significantly higher, about 4-12 times, culturable bacterial aerosol concentration levels compared to the use of agar. This study demonstrated a high volume (100 L min?1) portable aerosol-to-hydrosol sampling technique, holding broad promise in monitoring airborne biological threats when coupled with qPCR technology. Yet, caution should be taken in relating the bioaerosol concentrations to health risks as qPCR detects both culturable and non-culturable cells including inactivated ones.     

Long-term measurement of volatile organic compounds in ambient air by canister-based one-week sampling method

A canister-based 1 week sampling method using a mechanical flow controller and a 6 L fused-silica-lined canister was evaluated for the long-term measurement of 47 VOCs in ambient air at pptv (volume/volume) to ppbv levels by use of a three-stage preconcentation method followed by GC-MS analysis. The GC conditions were initially optimized for complete separations of several pptv-level VOCs (e.g. vinyl chloride, 1,3-butadiene, acrylonitrile, 1,2-dichloroethane and chloroform) in ambient air because the selected ions are easily interfered with by coexisting C4-, C5-hydrocarbons and analytes presented at ppbv levels. Thirty-four VOCs determined by the 1 week and 24 h sampling method in December 16-22 (2002) had concentrations of 6.0-15000 pptv per compound. Concentrations of 28 VOCs (including polar VOCs (e.g. methyl isobutyl ketone and butyl acetate)) obtained by the method were approximately equal to the mean values calculated from 24 h sampling (< +/- 10% deviation). Six VOCs that had low concentrations of 6.0-43 pptv showed more than +/- 10% deviation. Thirteen VOCs were not detected during the entire sampling period. The effect of relative humidity or ozone for the specific VOCs (e.g. MIBK, butyl acetate, vinyl chloride, 1,3-butadiene and styrene) was negligible.     

离子色谱法测定空气中氟化氢氯化氢和硫酸

以多孔玻板吸收管采样,采用离子色谱法同时测定作业场所空气中的氟化氢、氯化氢和硫酸,采样效率>92%。氟化氢在0 mg/L～2.00 mg/L、氯化氢在0 mg/L～2.50 mg/L、硫酸在0 mg/L～4.00 mg/L范围内线性良好,检出限分别为0.003 mg/m3、0.02 mg/m3、0.023 mg/m3(按采样体积60 L计),标准溶液平行测定的RSD≤8.0%,两个质量浓度水平加标的平均回收率为92.6%～106%。