COD工业废水样的保存及结果准确度的探讨

根据《环境监测分析方法》规定:测COD的水样保存为加硫酸使pH<2,此时样品可保存七天。鉴于各行业工厂排放的废水性质差异很大,组分极其复杂,必然给样品的保存带来不同的影响。为找出各种废水合适的保存条件及保存效果。我们分别对纺织、印染、制药、食品、化工、农药等23个工厂的水样进行了保存试验。同时对样品进行了加标回收试验,对方法的准确度进行了验证。     

碱化保存淡水及海水样品测定甲基汞和总汞

本文研究了水样保存条件对汞分析物稳定性的影响。常规总汞分析酸化水样保存法只适用于保存寒冷冬季水样测定甲基汞,而夏季水样在酸化保存过程中甲基汞会转化为无机汞。碱化（ｐＨ＞１２）保存天然水样可以防止甲基汞无机化,并且同时适用于长期室温保存冬季和夏季水样测定甲基汞和总汞。聚氟塑料瓶、聚丙烯塑料瓶、聚乙烯塑料瓶和硼玻璃瓶均可用于保存碱化水样测定甲基汞,但只有前两种容器同时适用于总汞分析水样保存。本文认为天然水样中的微生物是水样保存过程中导致甲基汞无机化的主要因素。     

《地表水和污水监测技术规范》(HJ/T 91-2002)的相关技术说明

文章从概念名称、采样方式、样品保存、质量管理等多方面阐述了《地表水和污水监测技术规范》(HJT91-2002)的相关技术,对于贯彻执行该规范具有很强的指导性和操作性。     

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。     

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。     

土壤环境样品库建设及样品信息数据库管理

土壤样品携载丰富的环境特征信息,对于掌握不同历史阶段土壤环境状况及变化趋势有着不可替代的作用。环境保护部国家土壤环境样品库于2010年建成,是中国环境保护重要基础设施,具有储存专业化、管理集中化、信息系统化、质控标准化等特点,创新性地集合了土壤样品保存和应用的现代技术,已成为中国最大的土壤环境资源和信息平台。通过开展国家土壤样品库建设和样品信息数据库管理研究,集成国家土壤样品库建设技术和土壤样品数据库信息管理成果,为各地建立省级土壤样品库提供借鉴,对于规范和指导全国土壤环境样品库建设和样品保存、数据库信息管理和应用等具有重要意义。     

不同保存条件对化学需氧量测定的影响

化学需氧量(COD)是表示水中还原性物质多少的一个指标,也是评价水质好坏的重要指标之一。不同的保存条件对COD值的影响是非常大的。通过本次实验验证了不同的保存方式对COD值的具体影响情况,从而在实际工作中采取合适的保存方式以确保COD值的准确性。     

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。     

气体样品的保存及其成分的变化

介绍了气体样品的各种保存方法及其在保存过程中成分变化的特点，以降低气体保存过程中的损失，提高监测管理水平。     

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。     

Air quality impact assessment

Air quality impact assessment (AQIA) is an important technique for determining the relative contribution to ground level pollutant concentrations of specific current or future source emissions at receptor sites. The principal activities in AQIA are air quality modelling and monitoring techniques. The choice of techniques which are applicable to a particular situation is intimately related to the problem to be assessed. A review of relevant modelling techniques has been presented, with emphasis placed on Gaussian plume models because of their ease of use and broad applicability. Alternative modelling techniques have been suggested when departures from the Gaussian form in the atmosphere occurs or when more detailed information on atmospheric chemistry, deposition or long range transport is required. The objectives and techniques of ambient air quality monitoring have been examined and the siting of instruments, duration and frequency of sampling, choice of monitoring rationale (fixed or mobile), minimization of sampling errors, data storage and analysis are discussed. Modelling and monitoring are essential to successful AQIA. An orderly approach to the principles and procedures involved in performing AQIA studies, using these two techniques in conjunction, has been presented.     

A comparison of techniques to sample salamander assemblages along highland streams of Maryland

Amphibians may be useful indicators of biological condition in small streams so determining which sampling technique maximizes encounters at the least cost and at the optimal time of year is important. Area constrained surveys (ACS), used by the Maryland Biological Stream Survey, were tested against cover board surveys, drift fences with pitfall and funnel traps, quadrat leaf litter searches, and leaf litter bags. Sixteen, 100 m-long sites were established in headwater streams in the Savage River State Forest in Garrett County, Maryland. Each technique was randomly assigned to a 25 m stream section within each overall sampling site, and sites were sampled once each month from May to October (2005) with additional sampling in March and April (2006). Area constrained surveys yielded means of 2.7 taxa and 14.9 total individuals per sampling visit, which was significantly higher than the yield of all other methods in all months except October and March, when yields were low for all techniques. Area constrained surveys were also significantly more cost-effective per taxon and per individual compared to all other methods. September produced the most taxa and individuals, October and March produced the least, and yields for April through August were similar to September. We employed removal sampling at four sites in April 2006, but abundance could not be estimated because a significant linear decrease in the accumulated catch versus catch per unit effort did not occur for three of the sites.     

Utilization of the solid sorbent media in monitoring of airborne cyclophosphamide concentrations and the implications for occupational hygiene

The main objective of the study was to evaluate the applicability of two solid sorbent media (Anasorb 708 and Strata X), the impinger filled with distilled water and PTFE filters for determination of airborne cyclophosphamide (CP) in the hospital working environment. For this purpose, air contamination of Masaryk Memorial Cancer Institute (Czech Republic) was monitored using the sampling apparatus containing the samplers described above. In addition, the surface contamination was also determined using the wipe sampling technique. During the monitoring, contamination of three different workplaces (storage room, preparation room and outpatient clinic) was studied. Using Strata X solid sorbent tubes, airborne CP was determined in all (n = 5) samples collected at the outpatient clinic over a 5 day monitoring period (concentration range: 0.3-4.3 ng m(-3)). Other samplers (including PTFE filters) did not collect any detectable amount of CP (the limit of detection, LOD ≤ 0.1 ng m(-3)). Negative results detected at filter samples indicate that CP determined at Strata X samples was most probably of gaseous origin. Surface contamination ranged from <2 to 19, <8 to 418 and 133-15,500 pg cm(-2) at the storage room, preparation room and outpatient clinic, respectively. The study showed that evaporation of antineoplastic drugs should not be neglected, albeit the concentrations determined in our study are relatively low. Therefore, proper monitoring of airborne contamination should involve simultaneous sampling of both particle-bonded and gaseous phases. In this way, Strata X sorbent tubes seem to be an effective tool for the sampling of gaseous CP in the indoor air.     

An evaluation of a fast sampling procedure for the trace analysis of volatile organic compounds in ambient air

This study deals with the evaluation of a fast method for sampling of volatile organic compounds in ambient air. Special bags made of an inert material are used together with a large handpump which allows a sampling of one liter per second. After the sampling, the pollutants are concentrated by adsorption on Tenax and transfered by heat desorption, to a small capillary precolumn cooled with liquid nitrogen, or directly trapped on the precolumn. The suitability of this technique was evaluated by sampling complex synthetic mixtures of known concentration and composition, after which the samples were submitted to a series of operations such as transport, aging, changing of the humidity, heating and cooling, irradiation, etc. Changes in the original mixtures, caused by adsorption, diffusion, chemical or photochemical reactions were investigated by GC-MS analysis. The results of the study show that under certain conditions the samples can be preserved for a rather long period of time without noticeable changes in composition. However for certain compounds, severe quantitative losses occur after one day storage. Finally a practical application of this method is described in a recent case of strong odour annoyance by a chemical plant in the north of Belgium.     

Field cryofocussing hydride generation applied to the simultaneous multi-elemental determination of alkyl-metal(loid) species in natural waters using ICP-MS detection

Two hydride generation manifold systems, utilizing flow injection and cryotrapping techniques for alkyl-metal(loid) speciation analysis in natural waters, are described in this paper. They provide shipboard capacity for simultaneous derivatization of analytes with NaBH4 and cryotrapping of the generated products in a field packed column at -196 degrees C. The first system is a large-volume hydride generator, using a reagent-injection flow technique as a flow batch type, that has been fully optimized and applied to the simultaneous detection of alkylated species in estuarine waters. The technique permits the analysis of a large volume sample (0.5-11) at a sampling rate of 3 h-1. The second is an online continuous flow hydride generator. A sampling rate of 3-12 h-1 can be achieved with samples of 0.1-0.51. In addition, shipboard operation eliminates major problems related to sample pretreatment, transport and storage. Ultra-trace multi-element determination is finally performed in the laboratory by cryogenic GC hyphenated with ICP-MS. Routine detection limits of 0.5-10 pg (as metal) for 0.51 water samples were achieved for the selected alkyl-metal(loid) species of arsenic, germanium, mercury and tin. Concentrations of various species, obtained from water samples taken from the Rhine estuary, are also presented. These species include alkylated arsenic compounds, other than methyl derivatives, that have been tentatively identified and are reported here for the first time.     

Influence of Relative Humidity and Ozone on the Sampling of Volatile Organic Compounds on Carbotrap/Carbosieve Adsorbents

By using a dynamic dilution system, the atmospheric measurement of 11 selected toxics VOCs (ethylene, acetylene, propene, 1-butene, 1,3-butadiene, 1-pentene, 1-hexene, benzene, toluene, ethylbenzene, m+p-xylene) from the list WHO of 1996 and TO-14 method of US EPA by preconcentration by thermal desorption (TD), analysis by gas chromatography (GC), identification and quantification with a flame ionisation detector (FID) was developed and validated in term of metrology, especially the techniques of sampling of these VOCs with adsorbents cartridges "Air Toxics" when used with an "UMEG sampler" equipped in the inlet with a nafion membrane. In particular the influence of climatic conditions (temperature and relative humidity) and the influence of chemical factors like ozone, on the representativity of sampling were studied. Experiments made with various humidities showed that the addition of a nafion membrane in the inlet of the sampling system was required. Without this membrane, losses of compounds were observed for RH >50%. With this membrane, storage for 2 weeks in a refrigerator, as for canisters, did not induce a loss of compounds. No significative decrease of concentrations of the studied VOCs after 14 days storage, which are known to react with ozone, were observed with an ozone concentrations of 55 ppb. One explanation is that nafion membrane, placed in the inlet of the sampler, will neutralize ozone before entering the sampling tubes. This observation is in accordance with literature which states that the sampling of VOCs on Carbotrap cartridges without ozone scrubber induce a loss of compounds.     

样品量对河流沉积物组分分析结果的影响

在完全相同的实验条件下 ,将 GSD-9水系沉积物作为监控样品 ,对河流表层沉积物 (<63 μm粒级部分 )取不同重量进行消化并用 ICP-AES法分析测定主要元素 K、Na、Ca、Mg、Al、Fe、Mn、Ti,分析的准确度大于 94% ,分析结果相对标准偏差小于 5 % ,说明消化过程和分析结果是可信的。通过对四条不同河流黄河、赣江、汾河和辽河沉积物样品量与元素分析结果之间的关系图发现 ,在样品量小于 2 0 mg的情况下 ,总体会造成分析结果较大的波动 ,实验数据很难保证 ,而当样品量达到 2 0 mg以上 ,测定结果逐渐趋于平稳基本呈水平线 ,在 5 0～ 2 5 0 mg之间分析结果最为稳定。因此为了保证测定结果的准确性 ,河流表层沉积物的样品量至少应保证大于 2 0 mg。     

Towards a sampling strategy for the assessment of forest condition at European level: combining country estimates

A correct characterization of the status and trend of forest condition is essential to support reporting processes at national and international level. An international forest condition monitoring has been implemented in Europe since 1987 under the auspices of the International Co-operative Programme on Assessment and Monitoring of Air Pollution Effects on Forests (ICP Forests). The monitoring is based on harmonized methodologies, with individual countries being responsible for its implementation. Due to inconsistencies and problems in sampling design, however, the ICP Forests network is not able to produce reliable quantitative estimates of forest condition at European and sometimes at country level. This paper proposes (1) a set of requirements for status and change assessment and (2) a harmonized sampling strategy able to provide unbiased and consistent estimators of forest condition parameters and of their changes at both country and European level. Under the assumption that a common definition of forest holds among European countries, monitoring objectives, parameters of concern and accuracy indexes are stated. On the basis of fixed-area plot sampling performed independently in each country, an unbiased and consistent estimator of forest defoliation indexes is obtained at both country and European level, together with conservative estimators of their sampling variance and power in the detection of changes. The strategy adopts a probabilistic sampling scheme based on fixed-area plots selected by means of systematic or stratified schemes. Operative guidelines for its application are provided.     

Volatile Organic Compounds: Sampling Methods and Their Worldwide Profile in Ambient Air

The atmosphere is a particularly difficult analytical system because of the very low levels of substances to be analysed, sharp variations in pollutant levels with time and location, differences in wind, temperature and humidity. This makes the selection of an efficient sampling technique for air analysis a key step to reliable results. Generally, methods for volatile organic compounds sampling include collection of the whole air or preconcentration of samples on adsorbents. All the methods vary from each other according to the sampling technique, type of sorbent, method of extraction and identification technique. In this review paper we discuss various important aspects for sampling of volatile organic compounds by the widely used and advanced sampling methods. Characteristics of various adsorbents used for VOCs sampling are also described. Furthermore, this paper makes an effort to comprehensively review the concentration levels of volatile organic compounds along with the methodology used for analysis, in major cities of the world.     

被动采样在水体中有机污染监测的应用:以PAHs为例

半透膜采样技术是一种可原位、连续、动态监测水环境中非极性、弱极性有机污染物的被动采样技术,已在国内外发展20余年,但在环境监测中使用很少。从半透膜被动采样特点、采样器构造入手,着重对应用该技术的环节进行剖析,同时涉及被动采样结果及其评价方法。最后以多环芳烃（PAHs）为例,综述了近年来SPMD技术监控水体中非极性、弱极性有机污染物的常用分析技术及其发展。