环境样品稀释方法的探讨

环境样品分析中，特别是污染源样品分析经常遇到样品浓度高于方法的检出范围。为此，根据不同分析项目的分析方法和质量控制的要求，研究和探讨了样品稀释可采用原始样品、中间样品和分析后样品进行稀释。稀释倍数可根据日常积累的基础资料推算、肉眼观察和简单试验的方法确定。探讨了稀释误差的来源及降低稀释误差的方法。     

环境样品稀释方法的探讨

环境样品，特别是污染源样品，在监测分析中经常要对污染物含量较高的样品进行稀释，使稀释后详品中污染物的浓度量分析方法测定浓度范围内。采取科学的稀释方法，确定适当的稀释份数，不仅可减轻分析工作量，节约分析成本，而且可降低样品中干扰物质的浓度，降低稀释误差，提高监测结果的可靠性。1样品稀释方法及其选择样品的稀释方法很多，本文便讨论根据样品稀释时使用的样品预处理程度分类。如原始样品稀释法，中同样品稀释法，分析后样品稀释法等．1．1原始样品稀释法需要稀释的环境样品中，均可采用原始样品稀释法。原始样品稀释法根…     

新形式下工业废水BOD_5稀释倍数的计算

推导了 BOD5稀释系数的量值关系 ,得出 BOD5稀释系数与样品的可生化性成正比 ,与稀释后水样的耗氧量成反比 ,并据此进一步分析了如何对样品的可生化性和稀释后水样的耗氧量进行预期。在此基础上从实际出发 ,根据工作经验简化和优化了稀释倍数的计算 ,达到提高测定准确度 ,降低劳动强度的目的     

关于如何降低稀释样品浓度最大相对误差问题的探讨

关于如何降低稀释样品浓度最大相对误差问题的探讨陈云，丁咏梅（江苏金坛县环境监测站，２１３２００）在监测分析中，分析人员经常要对污染物含量较高的样品进行稀释，以使稀释后样品中污染物的浓度置于分析方法最佳测定浓度范围之内。然而，由于稀释样品所用量器存在容...     

三点比较式臭袋法测定污染源臭气的改进建议

提出采用三点比较式臭袋法测定污染源臭气样品时,可能出现因初始稀释倍数设定过高而无法准确计算结果的情况,单一的初始稀释倍数无法适用于同一批样品和低浓度样品.建议取消判定师的初步嗅辨试验环节,直接从第一级稀释倍数开始嗅辨试验,低浓度样品转为环境空气样品分析,同时实行嗅辨员分级制度.     

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。     

BOD5样品分析中稀释倍数的确定

首衔正确估计出样品ＢＯＤ５浓度范围，并测定稀释水的溶解氧，然后根据稀释倍数公式计算三个适当的稀释倍数，本方法省时，可靠，适用性强，能够确保ＢＯＤ５样品分析一次成功。在ＢＯＤ５样品中分析中具有广泛的应用价值。     

工业废水BOD_5测定接种条件初探

稀释法测定BOD时,稀释倍数和接种条件是两个关键问题。对不同类型工业废水BOD测定中,接种条件的研究在国内较少具体报道。我们从82年6月至84年底共分析研究了26种工业废水。分析废水、接种液等样品总计约150个,由于稀释倍数不合适和接种量不合适等原因,只选取94个基本合格的样品(包括标准样品)数据进行统计计算並报告结果。     

五日生化需氧量测定中稀释倍数的估算

假定样品经过培养后耗氧率达５５％；推导出ＢＯＤ５稀释倍数Ｋ＝ＢＯＤ５／４．４，由稀释程度规定推导出ＢＯＤ５稀释倍数Ｋ＝（ＢＯＤ５－１）／４．０两种方法Ｋ基本相同，标准样品，工业废水经上述方法稀释后，测定结果比较满意，尤其对工业废水测定，既缩短了分析时间，又降低了测定误差。     

BOD5样品稀释度对测定结果的影响

1选取合适的样品稀释度是提高 BOD5分析结果准确度的关键。实验结果表明 ,最合适的样品稀释度所对应的培养液耗氧率为 43%～ 67%。 2根据环境监测的特点 ,建议采用下述 BOD5分析数据处理及结果表述方法 :选取耗氧率为 30 %～70 %的培养水样作为 BOD5测定结果 ,若有几种稀释度均在所要求区间 ,取其平均值 ;如果培养水样均不在所要求区间 ,则取其与 30 %或 70 %相差较小的水样作为 BOD5测定结果。 BOD分析报告 ,应同时报告样品稀释度和培养液溶解氧消耗率BOD_5样品稀释度对测定结果的影响@唐文天$荆州市环境监测站!湖北沙市434000 …     

超声辅助离子液体-分散液液微萃取-高效液相色谱法测定水中苯胺类化合物

本研究建立了超声辅助离子液体-分散液液微萃取-高效液相色谱测定环境水样中苯胺(AN)、对氟苯胺(4-FA)、对硝基苯胺(4-NA)、对氯苯胺(4-CA)四种苯胺化合物的方法。以最常用的烷基咪唑六氟磷酸盐类离子液体为萃取剂,通过超声加速萃取剂的分散程度,提高了萃取效率。该方法的检测限达到0.1~73 ng/ml,对黄河水和自来水中的加标回收率均在90.5%~113%之间,回收效果良好。与传统的液液萃取相比,该萃取方法具有绿色、快速、富集效果好、有机溶剂消耗小的优点,可以满足环境水体中苯胺类化合物的测定。     

气相色谱法中液体样品的进样技术

阐述了气相色谱中液体样品的4种进样技术。     

固相膜萃取-高效液相色谱法测定地下水中的多环芳烃

采用C18固相膜萃取对地下水中15种多环芳烃进行富集净化，以二氯甲烷作洗脱溶剂，高效液相色谱法，荧光检测器测定。对萃取、浓缩和色谱条件进行优化，在1．ooixg／L～40．0μg／L范围内测定标准系列溶液并绘制标准曲线，相关系数R2〉0．999；15种多环芳烃的仪器检出限为0．4ng／L～3．0ng／L；对地下水样品加标，平均回收率在75．7％～96．7％之间；标准溶液平行测定7次的RSD为3．1％～11．9％。     

Preconcentration and determination of lead and cadmium levels in blood samples of adolescent workers consuming smokeless tobacco products in Pakistan

The present study was aimed to evaluate the cadmium (Cd) and lead (Pb) levels in the blood samples of adolescent boys, chewing different smokeless tobacco (SLT) products in Pakistan. For comparative purpose, boys of the same age group (12–15 years), not consumed any SLT products were selected as referents. To determine trace levels of Cd and Pb in blood samples, a preconcentration method, vortex-assisted liquid–liquid microextraction (VLLME) has been developed, prior to analysis by flame atomic absorption spectrometry. The hydrophobic chelates of Cd and Pb with ammonium pyrrolidinedithiocarbamate were extracted into the fine droplets of ionic liquid (IL) 1-butyl-3-methylimidazolium hexafluorophosphate, while nonionic surfactant, Triton X-114 was used as a dispersing medium. The main factors affecting the recoveries of Cd and Pb, such as concentration of APDC, centrifugation time, volume of IL and TX-114, were investigated in detail. It was also observed that adolescent boys who consumed different SLT products have 2- to 3-fold higher levels of Cd and Pb in their blood samples as compared to referent boys (p?<?0.001).     

Quantification of Polycyclic Aromatic Hydrocarbons in Tea and Coffee Samples of Mumbai City (India) by High Performance Liquid Chromatography

This paper describes a method for quantification of sixteen polycyclic aromatic hydrocarbons (PAHs) in tea and coffee samples of Mumbai City with the help of reversed phase high performance liquid chromatography with UV-VIS detector. This method is based on liquid–liquid extraction followed by clean up with C-18 cartridge. Concentration of total PAHs in different brands of tea and coffee samples varied from 18.79 to 31.37 μg/L and from 16.47 to 18.24 μg/L, respectively. Mean concentration of total PAHs was 27.56 μg/L in tea and 17.20 μg/L in coffee. Recoveries at different concentration levels were higher than 68% in samples of tea and coffee. Detection limit was found to be low (0.0006 ng) for anthracene and highest (0.174 ng) for naphthalene with relative standard deviation between 0.4%–7%.     

A rapid and sensitive analytical method for the quantification of residues of endosulfan in blood

A new sensitive analytical procedure has been developed for the determination of residues of endosulfan in human blood samples. The method involves the extraction of residues of endosulfan from blood samples by the addition of 60% sulfuric acid at 10 degrees C, liquid/liquid partitioning by using hexane and acetone mixture (9:1) and quantification by using GC-ECD. Residues of endosulfan in blood samples were quantified as the sum of alpha-endosulfan, beta-endosulfan, endosulfan sulfate and endosulfandiol. The influence of temperature during the extraction has been studied. Recovery experiments were conducted over the concentration range 1.0-50 ng ml(-1) and the relative standard deviation calculated. The method was found to be sufficiently sensitive to quantify the residue of total endosulfan up to the 1.0 ng ml(-1) level. The recovery was 92% with a calculated relative standard deviation of 1.96%. Conversion of endosulfan to endosulfandiol is found to be less than 0.5% under the defined conditions. The method was applied to the analysis of residue contents of endosulfan and its metabolites in blood samples collected from the exposed population. The data obtained has been confirmed by GC-MS-EI in selective ion monitoring (SIM) mode.     

底质中硫化物样品预处理分析方法的改进

通过对底质中的硫化物预处理方法的改进 ,证明在盐酸或硫酸介质中气化 ,以 Na OH-EDTA为吸收液的预处理方法 ,具有准确度高、精密度好 ,测定周期短等优点。     

The simultaneous stripping of arsenic and selenium from wastewaters using hollow-fibre supported liquid membranes

The extraction of total arsenic and selenium using hollow-fibre supported liquid membranes (HFSLMs), with specific interest in the optimal conditions for the extraction in wastewater, is reported. The extraction time, type of liquid membrane, sample and donor pH and stirring rate were optimised, and thereafter, the developed method was tested in real wastewater samples. The optimal HFSLMs adopted, after optimisation tests, comprised of Aliquat 336, 0.8 M NaOH, 200 rpm and 80 min as the extractant, stripping phase, stirring rate and reaction time, respectively. The developed method had reasonable-to-high extraction efficiencies in real wastewater samples with the final effluent recording as high as 73 and 78 % removal efficiencies for Se and As, respectively. Considering the initial concentrations found in the samples, use of this developed method could bring down the concentrations to levels admissible by the United States Environmental Protection Agency (US-EPA) and World Health Organisation (WHO).     

煤化工厂烟气中苯并(a)芘现状监测分析

通过试验建立了煤化工厂烟气中苯并(a)芘的液相色谱监测分析方法.通过条件优化,用配有荧光检测器的高效液相色谱仪分析烟气样品中苯并(a)芘的含量,该方法以乙腈、水梯度比例混合作为流动相;流速为1.0 ml/min;激发波长为255nm、发射波长为420nm;保留时间为27.38 min,测定检出限为2×10-3μg/m3...     

土壤和沉积物中多氯联苯单体测定的净化方法研究

对浓硫酸净化、铜粉脱硫、氟罗里硅土柱、硅胶柱、石墨碳柱等净化方法在土壤和沉积物多氮联苯单体测定中的应用进行了研究.浓硫酸对多氯联苯单体的净化回收率达92.4％～109％;氟罗里硅土柱用正己烷/丙酮混合溶液淋洗,净化洗脱液体积为8 mL～10 mL时,回收率达85.7％ ～ 108％;硅胶柱用正己烷淋洗,净化洗脱液体积为...