AAS法测定土壤中铜的新型进样装置

研制了一种新的进样装置，装置既可常规进样又可以脉冲进样，可用于土壤中铜元素的测定。并对两种进样的方法的分析性能进行了对比。     

用同轴表面波激励器和微波等离子体炬获得的微波等离子体的…

同轴表面波激励器和微波等离子体炬是两种获得微波等离子体的装置，本文比较了用这两种装置获得的ＭＷＰ作原子发射光谱法光源时的分析性能，结果表明这两种装置各有优点，但微波等离子体炬效果更好。     

JEE—4x型真空镀膜仪功能扩展

报道了对ＪＥＥ－４ｘ型真空镀膜仪蒸发装置的改进以及建立蒸发材料回收装置的具体方法，并介绍了改进后该仪器在高分辨扫描电镜样品制备上的应用实例．实验证明，上述改进不但扩展了ＪＥＥ—４ｘ型真空镀膜仪的制样功能又节省了蒸发材料，集中了离子溅射法及常规高真空镀膜法的优点，完全满足ＳＥＭ样品的分析要求，该方法简单易操作．     

AAS法测定土壤中铜的新型进样装置

研制了一种新的进样装置,该装置既可常规进样又可以脉冲进样,可用于土壤中铜元素的测定。并对两种进样方法的分析性能进行了对比。     

参数法和非参数法估计组合样中被测组分含量的置信区间

本文以散装生铁块的随机样本分析结果为基础,应用Ｍｏｎｔｅ Ｃａｒｌｏ模拟法考察了组合样本中Ｓｉ、Ｍｎ,Ｃ,Ｓ,Ｐ含量（或份样平均值）的分布情况,研究了组分含量的置信区间,对参数法和非参数法的结果进行了比较。结果表明,对近似符合正态分布的原始总体或当组合样中的份样数目较多时,两种方法所估计的置信区间相近。但对偏离正态分布（或ｔ－分布）的总体且组合样中的份样数目较少时,非参数法较参数法的结果更符合实际     

气动雾化进样时微波等离子体炬作为激发光源的性能研究

以气动雾化进样研究了微波等离子体炬（ＭＰＴ）放电作原子发射光谱法激发光源的性能，包括ＭＰＴ的获得、操作参数的影响、样品引入及其分析性能，并与微波诱导等离子体进行了比较，证明ＭＰＴ放电作激发光源有良好的分析性能．     

气动雾化进样时微波等离子体炬作为激光发源的性能研究

以气动雾化进样研究了微波等离子体矩（ＭＰＴ）放电作原子发射光谱法激光发源的性能，包括ＭＰＴ的获得、操作参数的影响、样品引入及其分析性能，并与微波诱导等离子体进行了比较，证明了ＭＰＴ放电作激发光源有良好的分析性能。     

在火焰原子吸收分光光度计上进行无火焰原子化法测定

介绍了在常规火焰原子吸收分光光度计上采用特制高温陶瓷管进行无火焰原子化测定的方法，该方法即具有常规火焰原子化法的装置简单，操作方便，稳定性好的特点，又具有无火焰原子化法高灵敏度的优点。采用此方法对铜、锌两种元素进行了测定，灵敏度比常规火焰原子化法提高了30～50倍，检出限及回收率等指标均优于常规火焰原子化光谱法，是一种高效、简便、经济、实用的原子化方法。     

多波长线性回归法校正火焰原子吸收光谱干扰

用多波长线性回归法校正了火焰原子吸收分析中Ｇａ４０３．２９８ｎｍ对Ｍｎ４０３．３０７ｎｍ的吸收线重叠干扰，对合成样中Ｍｎ和Ｇａ含量的测定，结果令人满意。     

高效液相色谱讲座Ⅲ高效液相色谱仪器系统（下）

§3-2进样系统 进样系统是将待分析样品引入色谱柱的装置。对于液相色谱的进样装置,要求重复性好,死体积小,保证中心进样,进样时对色谱柱系统流量波动要小,便于实现自动化等。 进样系统包括取样、进样两个功能。而实现这两个功能又有手动和自动两种方式。     

提高碘量法测定天然气中硫化氢效率的方法

碘量法是测定管道输送天然气中硫化氢的一种经典方法,而管道输送天然气中硫化氢含量较低,按照GB/T11060.1–2010方法测定,取样量较大,取样时间长,影响工作效率。针对此问题,从两方面对碘量法进行改进:减小天然气取样量进行试验,并与国标规定取样量时的实验结果进行比对,确定最佳取样量;增大取样流量进行试验,并与国标规定取样流量时的实验结果进行比对,确定最佳取样流量。对硫化氢质量浓度为7.2~14.3,14.3~28.7 mg/m~3的天然气样品进行试验测定,结果表明,将天然气取样量减少为20 L,取样时间分别由200,100 min缩短为40 min;将天然气取样流量设定为750 m L/min,取样时间分别由200,100 min缩短为133,67 min。减少取样量或者提高取样流量,均能缩短管输天然气的取样时间,提高检测效率。     

SSTS-Ajax for analysis on-line by gas chromatography

A switching system of triplet samples (SSTS-Ajax) is introduced to the analysis on-line by gas chromatography. The triplet samples (i.e., a sample and its two duplicates) can be obtained at the same time and then analyzed in turn by using this system. During a reaction, if the analysis of one sample is unsuccessful or the result is abnormal, a duplicate can be kept for a second analysis in the sampling tube without the following on-line analyses interrupted. Alternatively, the triplet samples can be respectively analyzed under different operating conditions, and thus offer more information about the sample. Furthermore, the triplet samples from different points on-line can be obtained alternately or even at the same time with the aforementioned advantages maintained. In addition, six samples from one point on-line can also be obtained at the same time or even at six different times and then analyzed one by one, which is very helpful when the duration of an analysis is much longer than the interval of two continuous sampling operations. The principle and usage of SSTS-Ajax is discussed in detail.     

Identification and quantification of sources of variation in the analysis of steel

In steel industries a need exists for the reduction of variation in the element concentrations. This need is triggered by an increasing demand for high quality steel products by clients. The results of a large-scale experiment concerning the identification and quantification of sources of variation in the production, sampling and analysis of steel are presented. The results are obtained by means of a strategic approach that consists of six steps. By means of this strategic approach, insight is obtained in the build-up of the total variation. This knowledge can be used to reduce the influence of those factors that have a major impact on the total variation. Attention is focused on estimating the magnitude of sources of variation apparent in sampling of certain stages of the steel making process and in analysis of steel samples by means of spark emission spectrometry.     

Development of the performance reference compound approach for the calibration of “polar organic chemical integrative sampler” (POCIS)

The purpose of the Water Framework Directive is to ensure the quality of the natural water across Europe. In this context, passive samplers have shown interesting capacities for the monitoring of contaminants in aqueous ecosystems. They allow the measurement of time-weighted average concentrations, overcoming many drawbacks of the spot-sampling techniques known to be expensive and time consuming. However, application of passive samplers such as polar organic chemical integrative samplers (POCIS) for the monitoring of hydrophilic contaminants requires calibration to define compound sampling rates; key parameters to deduce the pollutant water concentrations from the amounts of pollutants accumulated by the device. Unfortunately, sampling rates are influenced by a range of environmental factors; in that respect, a question remains: is it not evident to know to what extent the sampling rates obtained in laboratory experiments can be used in field conditions? The problem can be solved for hydrophobic samplers by using performance reference compounds (PRCs), and an ongoing challenge for POCIS is focused on the improvement of the quantitative aspect of this family of samplers. In this study, potential PRCs have been selected during a specific experiment and their performance was tested in the laboratory under two hydrodynamic conditions. Results revealed a good proportionality between elimination rates of PRCs and sampling rates of chemicals. Afterwards, the application of the approach under environmental conditions was assessed by deploying POCIS in the Arcachon Bay (France) where POCIS–PRC-derived water concentrations appear to be close to the simultaneous grab-sampling results.

Identification and quantification of sources of variation in the analysis of steel

In steel industries a need exists for the reduction of variation in the element concentrations. This need is triggered by an increasing demand for high quality steel products by clients. The results of a large-scale experiment concerning the identification and quantification of sources of variation in the production, sampling and analysis of steel are presented. The results are obtained by means of a strategic approach that consists of six steps. By means of this strategic approach, insight is obtained in the build-up of the total variation. This knowledge can be used to reduce the influence of those factors that have a major impact on the total variation. Attention is focused on estimating the magnitude of sources of variation apparent in sampling of certain stages of the steel making process and in analysis of steel samples by means of spark emission spectrometry. Received: 6 November 1999 / Revised: 10 February 2000 / Accepted: 19 March 2000     

Development and validation of a new direct sampling method for coarse mono- and mixed waste fractions bound in bales

Sampling of coarse waste materials is considered to be a particularly challenging task and is at the same time the most crucial step in the overall data acquisition process. Despite this fact, research work on new sampling methods or new scientific approaches to sampling has been rather limited over the last decades. This paper focuses on a completely new sampling procedure for coarse two-dimensional materials similar to municipal solid waste or packaging plastics. The developed method is especially suitable for materials with particle sizes >100 mm and is based on the ‘press-and-drill method’ introduced by researchers from Fachhochschule Nordhausen. The basic idea is to sample the material in its compressed form (e.g. as bales) with a drilling tool in order to gain increments. The study presented in this paper shows the results of two extensive test series applying this new sampling technique to a middle-calorific fraction produced from packaging material (mainly plastics, textiles and paper). In parallel, the state-of-the-art approach was also applied on the same materials to gain valuable reference data. Results from both approaches are used for the extensive validation of the new sampling method. The verification of accuracy was realised by doping the material with defined pieces of foil containing molybdenum sulphide (MoS₂) which acted as a tracer in the bale. The results obtained by the new direct bale sampling showed not only good accordance with the actual tracer content in each bale but also with results derived from the state-of-the-art approach. In this study, homogeneously distributed parameters (e.g. loss of ignition) were included just as inhomogeneously distributed elements (i.e. Cu). It is shown that sufficient representativeness for coarse materials (d₉₅ > 300 mm) is obtained despite relatively small sample amounts and without previous comminution of the material.     

Polycyclic aromatic hydrocarbons in the atmosphere: monitoring, sources, sinks and fate. I: Monitoring and sources

This is the first of a series of two papers intended to review the state-of-the-art knowledge on atmospheric PAHs, concerning their monitoring, sources and transformation processes in the atmosphere. The monitoring section briefly introduces this class of compounds, mainly focusing on the 16 PAHs indicated by the US-EPA as priority pollutants. These compounds undergo partitioning between the gas phase and particulate, which has to be considered in the choice of the sampling methodology. Furthermore, sampling artifacts may arise from further phase transfers inside the sampling device. After sampling, extraction, clean up and detection/quantification procedures will follow. They are closely related since the choice of the extraction technique will heavily condition the clean-up step, and both procedures will place demands on the performance of the detection technique (usually GC-MS or HPLC). This is particularly true in the case of complex samples such as those arising from atmospheric sampling. The sources of atmospheric PAHs are then discussed with a particular focus on receptor models, which can allow the apportionment of PAH sources based on concentration data that can be routinely obtained by pollution control networks.     

Headspace SPME followed by GC/PFPD for the analysis of malodorous sulfur compounds in liquid industrial effluents

Headspace SPME was used to analyse malodorous sulfur compounds in liquid industrial effluents. A pulsed flame photometric detector (PFPD) was selected for a specific and sensitive analysis. Two fibres, PDMS/Dvb and PDMS/Carboxen, which are particularly convenient for extracting small and volatile molecules were tested. To compare these fibres, both sensitivity and artefact formation were considered. The PDMS/Carboxen fibre showed the lower limits of detection and moreover the least artefact formation yields. It was therefore selected and headspace SPME extraction conditions were optimised. Limits of detection of the target compounds evaluated were 12–31 ng L^–1 and repeatability was around 7%. Due to the adsorption mechanism involved, extraction is strongly influenced by the sample matrix and the low affinity compounds can suffer displacement effects. To investigate the occurrence of this phenomenon, two sampling times corresponding to non-equilibrium (5 min) and equilibrium conditions (60 min) were investigated. An external calibration was carried out by using standard solutions for both sampling times. The developed procedure was then compared to the standard addition method on a real industrial effluent. The results obtained from the two methods and for the two extraction times were in good agreement, demonstrating that even a long sampling time can be used. Therefore, the simple and timesaving external calibration was defined as relevant for an accurate quantification of sulfur compounds by headspace SPME.     

Comparative analysis of bias in the collection of airborne pollutants: Tests on major aromatic VOC using three types of sorbent-based methods

This study was undertaken to establish one of the most reliable sampling methods and to precisely evaluate the bias involved in the collection of airborne pollutant samples. For the purpose of our study, we investigated the performance of three different types of sampling techniques by measuring major aromatic volatile organic compounds (VOC) in outdoor air; the target analytes specifically include benzene, toluene, ethylbenzene, and xylene (commonly called BTEX). As the first step of our approach, we designed and developed a multi-channel sampling system consisting of a six-port mass flow controller (SJU-MFC) system. Because this system allowed the collection of up to six replicate samples, our measurement results were analyzed and screened statistically for the derivation of high-quality BTEX data. The feasibility of this sampling system was further tested through a comparison with concurrent measurement data sets obtained by two additional, but independent, sampling techniques: (1) automatic continuous sampler (ACS) and (2) on-line GC (O-GC) system. Based on the data sets collected concurrently by three different sampling methods, we attempted to evaluate the compatibility of sampling techniques. Although the results obtained by SJU-MFC system were not statistically different from those of the O-GC system, they were moderately distinguishable from those of ACS. Such patterns were seen consistently, when examined by correlation analysis. The overall results of our study thus generally point out that the compatibility of data sets, when the proper caution is taken, improve significantly among different sampling methodologies.