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。     

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。     

废气样品中甲烷的保存条件研究

气相色谱法检测废气中甲烷,样品保存容器可选择玻璃注射器、惰性气袋、真空瓶、苏码罐等,实验室对此做了比较研究。结果表明:玻璃注射器气密性较差,样品须在8 h内完成分析;真空瓶携带不方便,苏码罐价格昂贵,两者使用较少;使用玻璃注射器采集,然后注入惰性气袋保存的方法最佳,样品至少可稳定保存7d。     

影响地表水中总磷测定的因素探讨

总磷是评价水质的一项重要指标,现对样品中悬浮物(泥沙)含量、加酸保存样品保存时间与调节pH值对总磷测定的影响进行研究。结果表明,随着沉降时间的延长总磷测定值逐渐降低,加酸保存的样品总磷测定值随保存时间的延长而增高,且测定时是否调回中性对测定结果基本无影响。故进行地表水中总磷的测定需严格按照标准规定的样品采样过程控制采样沉降时间,加酸保存,24 h以内进行测定,测定时无需调回中性。     

直接进样-气相色谱质谱法同时测定固定污染源排气中的含氟温室气体

建立了一种直接进样-气相色谱质谱法同时分离和测定固定污染源排气中三氟甲烷、四氟甲烷、六氟乙烷和六氟化硫等含氟温室气体的方法。使用CP-Sillica PLOT毛细管填充柱可使上述4种目标化合物实现基线分离。分别用全扫描模式和选择离子扫描模式进行定量分析,方法检出限分别为0.12,0.19,0.10,0.08 mg/m~3和2.8,3.4,1.7,3.1μg/m~3。探讨了样品保存容器与保存时间对样品浓度衰减的影响,指出Tedlar采样袋或铝塑复合膜采样袋可以较长时间保存样品,在常温下,样品可保存至少7 d。实际样品测定结果表明方法快速、简便,适用于固定污染源排气中含氟温室气体的测定。     

地表水中丁基黄原酸的保存条件研究

通过对不同基质地表水样中丁基黄原酸在p H值、温度、光照、保存时间等条件下进行保存研究,确定对其保存效果的影响为:保存时间保存温度样品中丁基黄原酸浓度光照强度p H值。建议地表水样品使用棕色玻璃瓶盛装,于4℃下避光保存原水。高浓度样品,保存时间不超过5 d;低浓度样品,保存时间不超过1 d,最好采样后立即分析。     

影响非甲烷总烃监测结果准确性的因素研究及控制

结合非甲烷总烃监测工作实际情况,对样品采集、保存与运输、分析测试与数据处理、采样容器清洗与保存等过程详细研究后发现,采样容器从样品中吸附吸收的难挥发性与高化学活性组分和其自身的本底干扰对监测结果准确性的影响最严重,且其中残留的污染物使用传统方法难以消除。为此,通过改进采样容器清洗方法、完善相关质控措施和制定采样容器合格清洗与分类管理的判断依据,以降低各影响因素对非甲烷总烃监测结果准确性的影响。     

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。     

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。     

烟气中SO_2监测质量控制的研究

本文针对烟气中ＳＯ２手工采样监测的质量控制,如采样管的温度、采样流量、样品保存等进行了研究,并对原监测方法提出改进措施,提高了方法的准确度和精密度,从而保证了监测数据的准确性和可靠性。     

Effect of imperfect detectability on adaptive and conventional sampling: simulated sampling of freshwater mussels in the upper Mississippi River

Adaptive sampling designs are recommended where, as is typical with freshwater mussels, the outcome of interest is rare and clustered. However, the performance of adaptive designs has not been investigated when outcomes are not only rare and clustered but also imperfectly detected. We address this combination of challenges using data simulated to mimic properties of freshwater mussels from a reach of the upper Mississippi River. Simulations were conducted under a range of sample sizes and detection probabilities. Under perfect detection, efficiency of the adaptive sampling design increased relative to the conventional design as sample size increased and as density decreased. Also, the probability of sampling occupied habitat was four times higher for adaptive than conventional sampling of the lowest density population examined. However, imperfect detection resulted in substantial biases in sample means and variances under both adaptive sampling and conventional designs. The efficiency of adaptive sampling declined with decreasing detectability. Also, the probability of encountering an occupied unit during adaptive sampling, relative to conventional sampling declined with decreasing detectability. Thus, the potential gains in the application of adaptive sampling to rare and clustered populations relative to conventional sampling are reduced when detection is imperfect. The results highlight the need to increase or estimate detection to improve performance of conventional and adaptive sampling designs.     

A field-based spectrophotometric flow-injection system for automatic determination of chloride in soil water

The use of chloride as a tracer for soil water investigations is discussed. Limitations with laboratory based soil core and field based sampling are considered with respect to the poor suitability of the data for rigorous assessment of mechanistic models. Investigation of water movement in soil has been restricted by limitations in spatial and temporal sampling. Fine resolution sampling generates large numbers of samples which cause problems with post sampling laboratory analysis. This paper describes a field-based system for the analysis of chloride in soil water. There are three component parts to the system, (i) a custom sampling sub-system comprising of ceramic cup suction samplers and sample traps, (ii) a sample routing sub-system to channel sample to (iii) a sample analysis sub-system utilizing a flow injection method for sample analysis using a custom built photo-diode detector. The three sub-systems were controlled by a suitably equipped personal computer. A calibration procedure is described with a third order polynomial equation derived to convert millivolt response from the detector into chloride concentration. Field and laboratory data from a tracer experiment are presented and discussed, and it is concluded that the system is well suited to field-based applications. Finally it is noted that the photo-detector is suitable for colourimetric analysis of any tracer with suitable chemical determination.     

Assessment of vehicular pollution in Kolkata, India, using CALINE 4 model

Michigan water quality standards for public bathing beaches require local health departments to collect and analyze a minimum of three water samples for Escherichia coli during each sampling event. The geometric mean number of E. coli colonies is then compared to the 300 colonies per 100 ml standard to determine compliance. This article compares the results of the currently mandated procedure to a composite sampling method, whereby the three samples are mixed in equal volumes and analyzed once. This effectively replaces the geometric mean of the individual sample results with an arithmetic mean. Although arithmetic means are more affected by outliers, this sensitivity to high concentrations is more health conservative than the geometric mean. During the 2007 sampling season, nine bathing beaches were monitored once each week. Three individual point samples and a composite sample were analyzed for each sampling event. No statistically significant differences in bacteria concentrations were found between composite sample analysis and the arithmetic mean of individual point sample analyses. No violations were detected in the 2007 sampling season, so using historical data, a retrospective analysis was performed on samples gathered at nine bathing beaches in Kalamazoo County, Michigan during the years 2001–2007. The arithmetic mean of the three samples taken at each site served as a surrogate composite sample. The benefits of compositing the three samples were investigated assuming a 2/3 reduction in analytical costs. In the traditional sampling method, three individual samples were obtained and analyzed once in every 3-week period during the summer season, whereas compositing was simulated by taking the arithmetic mean of each week’s results. The results of this retrospective cost analysis indicates that ten to 14 violations would have been missed using the less frequent traditional sampling and analysis methodology. Composite sampling is a cost-saving alternative to traditional sampling techniques that can be more protective of public health, particularly when the savings are applied to increased numbers of samples in time or space.     

砷形态水样贮存方法及稳定性研究

设计了不同试样、不同浓度、不同酸度、不同温度以及不同容器条件的贮存方案,对含砷形态化合物水样的贮存和砷形态稳定性进行了研究。认为,人为酸化水样不利于砷形态的稳定;塑料瓶作容器、低温对砷形态水样的保存有利。本研究为水质监测砷形态提供了必要依据。     

大气优化布点监测方法简化试验

将每天TSP、SO_2两种污染物各采四次样并分别进行测定,简化为每天各采一个“日混合样”进行测定,对测定结果进行数理统计检验结果表明:测定值之间不存在显著性差异、两种方法的测值波动是由偶然因素造成的,因此,简化方法即采日混合样进行分析是一种可靠的监测方法,它适用于煤质中含硫份较低的地区。     

Framework for designing sampling programs

A general framework for designing sampling programs is described. As part of the sampling program the problem of concern, or reason for sampling, needs to be clearly stated and objectives specified. The development of a conceptual model will assist the clarification of objectives and the choice of indicators to be sampled.Objectives can then be stated as testable hypotheses and decisions made about the samallest difference/changes that are to be detected/observed by the sampling.To allow the collection of representative samples, and the statistical analysis of data to be collected, the potential sources of variability in the data must be considered. Site, selection, frequency and replication must account for the expected variability.Before field collection of samples occurs, the sample collection device needs to be tested as to its efficiency to collect a representative sample. It also will usually be necessary to consider how samples are to be preserved to inhibit biological and chemical change. All sample programs require a quality assurance program to identify, measure and control errors.As well as the above the cost-effectiveness of the program should be evaluated in terms of maximizing the information obtained/cost.     

地下水采样方法比对研究

选取3种地下水采样方法开展方法比对研究。通过系统分析监测数据,指出了3种方法所采水样在基本水质参数、无机离子、金属、挥发性有机物以及感官类指标等项目监测上的显著差异,指出了各种方法的适用性并分析原因。结果表明:与贝勒管法、潜水泵法相比,低流速法有效地解决了采样操作过程中易产生的曝气问题;对井内水体扰动较小,降低了水样浊度;减小了井内水位的大幅度泄降,避免了不同层位间污染物的迁移及周边水和井内滞水的交叉污染;节约了场地操作时间和后期污水处理所需花费。因此,低流速法在采取代表性水质样品方面更具方法优势。     

Network design factors for assessing temporal variability in ground-water quality

Benchmark major ions and nutrients data were collected biweekly for about two years at 12 wells at two sites in a shallow sand and gravel aquifer in west-central Illinois. The purpose of the study was to explore the time series properties of ground-water quality data collected at a relatively high sampling frequency. A secondary purpose was to determine the relative magnitudes of natural and sampling-related sources of variance in ground-water quality time series. The absence of this kind of information has severely hindered the design of ground-water sampling programs in the past.An autocorrelation analysis showed that the median sampling frequency for which the predicted ratio of effective independent sample size to total sample size was 0.5 (50% sampling redundancy) ranged from 6 to 14 samples per year. For a predicted ratio of effective independent sample size to total sample size of 0.9 (10% sampling redundancy) the sampling frequency ranged from 3 to 6 samples per year. This suggests that, for the wells sampled, sampling frequencies much higher than monthly can result in considerable loss of information, and may not be cost effective. Care was taken in the design of the field and laboratory sampling protocol to minimize the effects of measurement error. The data analysis confirmed that this goal was accomplished. In most cases considerably less than five percent of the total variability could be attributed to sampling and analytical error. Because of the relatively short duration of the study (42 biweekly sampling occasions at most wells) it was not possible to identify the magnitude of seasonal variations reliably.     

甲醛法在测定固定污染源排放SO2浓度中的应用

对用注射器采样甲醛法测定高浓度ＳＯ２样气精密度、准确度，采样效率，样品的稳定性进行了研究，并应用于燃煤，燃油锅炉排气中ＳＯ２浓度的测定，同时与碘量法结果进行比较和评价，表明注射器采样甲醛法测定了ＳＯ２基本可行。     

What do qualitative rapid assessment collections of macroinvertebrates represent? A comparison with extensive quantitative sampling

It is a fundamental tenet of Rapid Biological Assessments (RBA) that the samples collected reflect the community from which they are drawn. As with any biological sampling, RBA collections are subject to sampling error resulting in the omission of some taxa. The aim of this study is to compare the composition of RBA samples with an estimate of community structure based on extensive quantitative sampling. We used logistic regression to explore the relationships between the frequency of a taxon being collected in an RBA sample and its biological and ecological traits, namely its abundance, distribution, body size and habit. RBA samples and quantitative estimates of community structure were made in riffles in the Kangaroo and Nepean Rivers, New South Wales, Australia. Single RBA samples may collect up to 63% of the taxa that are collected by extensive quantitative sampling at a site. The frequency of a taxon being recorded in an RBA sample was significantly and positively related to all traits tested indicating a bias in the collection methods towards large, abundant and widely distributed taxa. Accordingly, taxa missed by RBA sampling were generally small, narrowly distributed or rare. These findings enhance our understanding of what RBA samples represent, and the bias and source of errors associated with RBA sampling. This study also quantifies the utility of RBA methods for biodiversity assessment.