杂多配合物催化合成羧酸异戊酯的研究

杂多配合物催化合成羧酸异戊酯的研究王玉和，周百斌，关良智，王晓光，单永奎，李萍，周宏立（哈尔滨师范大学化学系哈尔滨１５００８０）关键词杂多酸，酯化作用，异戊酯，催化羧酸异戊酯广泛用于调制各种香型的食品香料，用作溶剂、萃取剂、制革、人造丝、涂料、化妆品...     

梯度淋洗离子色谱-安培检测测定苯胺类化合物

以乙腈和硫酸的混合溶液为流动相，梯度淋洗，阳离子交换分离，直流安培检测，一次进样分离2，6-甲苯二胺（2，6-TDA），2，4-甲苯二胺（2，4-TDA）、苯胺、邻甲苯胺、对氯苯胺、4，4‘-二氯基二苯甲烷（4，4‘-DADPM）、间硝基苯胺、甲萘胺等9种苯胺类化合物。方法对2，6-TDA、2，4-TDA、苯胺、邻甲苯胺、联苯胺、对氯苯胺、4、4‘-DADPM、间硝基苯胺、甲奈胺的检测限分别为3.46、7.25、4.99、7.43、21.21、16.3、2.60、201.47和22.60μg/L。     

微波加热快速测定腐植酸总量

利用微波加热技术，在密闭容器内通过压力浸提、消解试样、能大大加快分析速度，本实验测定了不同煤样中的腐植酸总量，讨论了功率、时间、酸度等因素对分析结果的影响，并与标准方法相对照，用ｔ－检验法及Ｆ－检验法检验，没有明显差异，结果令人满意，该法具有省时、省力、经济、不污染环境，宜于批量分析，便于普及推广等优点。     

仙人掌果汁红色素含量测定与微量元素分析

用可见分光光度法与等离子体发射光谱法对仙人掌果汁色素及其微量元素的含量进行了测定，仙人掌果汁色素含量达２．１％￣３．３％，成熟果的果汁色素含量比预成熟果大。在２７种被测定的元素中，除Ａｓ、Ｂｅ、Ｃｄ、Ｃｏ、Ｍｏ、Ｐｂ，Ｓｂ，Ｔｌ等未被检出外，其余Ａｇ，Ａｌ，Ｂ，Ｂａ，Ｃａ，Ｃｒ，Ｃｕ，Ｆｅ，Ｍｇ，Ｍｎ，Ｎａ，Ｎｉ，Ｓｅ，Ｖ，Ｚｎ，Ｋ，Ｐ，Ｓ等均有准确测定值。成熟果与预成熟果的果汁微量元素含量无明显     

肺癌患者头发中的微量元素分析

分析了30例肺癌患者头发的19种微量元素，即：锌、铁、铜、钙、锰、镍，铬，钼、镉、铅，年纪最小的33岁，最大的89岁，平均年龄53．3岁，其中男22例，女8例，检测结果：肺癌患者头发微量元素锌、锰明显减低，男性肺癌病人发镍、发铬明显增高，提示肺癌的发生与人体内锌、锰的降低和镍、铬的增高有一定关系。     

环境监测现状

目前，全国已形成了国家、省、市、县四级环境监测网络，共有专业、行业监测站4800多个，其中环保系统监测站2200多个，行业监测站2600多个，国控的空气质量监测网站103个，酸雨监测网站113个，水质监测网站135个。同时，还建有噪声监测网、辐射监测网和区域监测网等。到2005年，国控环境监测网络调整为：环境空气监测网站226个，测点数793个；酸雨监测网站239个，测点数472个；水质监测网站197个；监测断面1074个；生态监测网站15个。目前，我国已制定各类国家环境标准410项，覆盖了大气、水质、土壤、噪声、辐射、农药等领域。开展了环境质量监测，     

HGZ—Ⅱ型自动辉光放电光源的研制

在仔细研辉光放电光源工作过程的基础上，在国内首先设计，制成了ＨＧＺ－Ⅱ型自动辉光放电光源。该光源除换样品外，实现抽空、进气、对光、预燃、曝光、充气、复位等摄谱全过程的自动控制。有水压、真空度、短路保护措施施和醒铃线路。设计合理，性能良好，操作简便，工作安全，可靠。程控部分的编排包括顺序控制。时序控制和条件控制。由于使用通用执行元、器件，降低了成本，提高了耐用性。为满足表层，逐层分析的需要，还专门设     

超临界二氧化碳脱附固体吸附剂上卤代烃污染物研究

本文使用自制超临界流体萃取仪，考查了从活性炭、Ｃｈｒｏｍｏｓｏｒｂ １０２、Ｃｈｒｏｍｏｓｏｒｂ１０５、Ｔｅｎａｘ－ＴＡ四种吸附剂上脱附１，２，３－三氯丙烷、１，３二溴丙烷、１，４－二溴丁烷、１，２，４－三氯化苯、间－二溴苯五种组分的性能。证明使用甲醇改性后ＣＯ２萃取，比单纯使用ＣＯ２萃取的效率高得多，萃取活性炭时，组分的回收率可达５０％，萃取另３种吸附剂时，组分的回收率超过８０％，这表明利用某些     

负离子对紫精光还原和电氧化还原性能的影响

负离子对紫精光还原和电氧化还原性能的影响冯敏辉，刘伟区，梁兆熙（中山大学高分子研究所，广州，５１０２７５）关键词紫精化合物，负离子，电氧化还原，光还原，化学还原合成了不同负离子（Ｆ－、Ｃｌ－、Ｂｒ－、Ｉ－、ＳＣＮ－、ＣｌＯ４－）的芳基紫精聚合物，并研...     

平顶山学院化学化工学院

平顶山学院化学化工学院始建于1978年，现有化学（师范类）、化学工程与工艺两个本科专业，化学教育、应用化工技术、环境监测与治理技术三个专科专业。现有教师35人，其中教授2人，副教授及高级实验师12人，教师队伍中有博士1人，在读博士7人，硕士21人，省、校级中青年骨干教师7人，师资队伍强大：有1人获得曾宪梓教育基金奖，1人获得李政道奖学金，5人获得省、校课堂教学优秀奖，     

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。     

Grab vs. composite sampling of particulate materials with significant spatial heterogeneity—A simulation study of “correct sampling errors”

Sampling errors can be divided into two classes, incorrect sampling and correct sampling errors. Incorrect sampling errors arise from incorrectly designed sampling equipment or procedures. Correct sampling errors are due to the heterogeneity of the material in sampling targets. Excluding the incorrect sampling errors, which can all be eliminated in practice although informed and diligent work is often needed, five factors dominate sampling variance: two factors related to material heterogeneity (analyte concentration; distributional heterogeneity) and three factors related to the sampling process itself (sample type, sample size, sampling modus). Due to highly significant interactions, a comprehensive appreciation of their combined effects is far from trivial and has in fact never been illustrated in detail. Heterogeneous materials can be well characterized by the two first factors, while all essential sampling process characteristics can be summarized by combinations of the latter three. We here present simulations based on an experimental design that varies all five factors. Within the framework of the Theory of Sampling, the empirical Total Sampling Error is a function of the fundamental sampling error and the grouping and segregation error interacting with a specific sampling process. We here illustrate absolute and relative sampling variance levels resulting from a wide array of simulated repeated samplings and express the effects by pertinent lot mean estimates and associated Root Mean Squared Errors/sampling variances, covering specific combinations of materials’ heterogeneity and typical sampling procedures as used in current science, technology and industry. Factors, levels and interactions are varied within limits selected to match realistic materials and sampling situations that mimic, e.g., sampling for genetically modified organisms; sampling of geological drill cores; sampling during off-loading 3-dimensional lots (shiploads, railroad cars, truckloads etc.) and scenarios representing a range of industrial manufacturing and production processes. A new simulation facility “SIMSAMP” is presented with selected results designed to show also the wider applicability potential. This contribution furthers a general exposé of all essential effects in the regimen covered by “correct sampling errors”, valid for all types of materials in which non-bias sampling can be achieved.     

固体分层取样方案的最优化设计

本文首次从理论上探讨了取得量对分层取样误差的影响,提出了总取样量一定时各层的最佳取样量和最小取样方差的计算公式,从而为分层取样的最佳取样方案设计提供了理论依据。     

Field sampling demonstration of portable thermal desorption collection and analysis instrumentation

The HAPSITE® (Hazardous Air Pollutants on Site) is a portable gas chromatography-mass spectrometry (GC–MS) unit designed to aid air sampling technicians by identifying and quantifying volatile organic compounds from occupational and environmental sampling. The main goal of the present study was to extend prior laboratory-based work with the portable HAPSITE® ER (extended range model) thermal desorption (TD) capability to real-world field samples from both indoor and outdoor environments using different types of active and passive sampling mechanisms. Understanding the performance of the HAPSITE® ER in a realistic field setting will allow air quality sampling technicians to make improved decisions related to sampling and analysis methods in the field. An important finding was that certain charcoal-based TD sorbents were contraindicated for the HAPSITE® ER because of a substantial hydrocarbon bleed which degraded system performance. A novel time series TD sampler (Logistically Enabled Sampling System-Portable [LESS-P]) was validated using Tenax TA TD tubes against standard active sampling across multiple field sampling sites, and the qualitative analytical trends and compound identities were similar between LESS-P replicates analysed via benchtop GC–MS and HAPSITE® ER. Once validated, the LESS-P was used to determine the reference concentrations for passive sampling calculations. The results confirmed the passive sampling methodology within the benchtop system, but highlighted some systemic sensitivity limitations that must be addressed in order for the HAPSITE® to be accurately applied to passive sampling. We propose that the LESS-P time-series sampler may help to alleviate the requirement for sampling technicians to be on-site during active sampling, allowing for automated sampling throughout the duration of a sampling event.     

探讨二元颗粒混合物取样误差的新的数学模型

采用新的数学模型研究二元颗粒混合物的取样误差,首次提出了取样的逻辑质量单元的理论,探讨了逻辑质量单元的物理意义,建立了按质量取样的标准偏差的计算公式.应用颗粒药品二元混合物的取样实验,证实了该公式的正确性.     

在线采样技术在中国的发展

在线采样技术能实时采样,满足在线监测的采样要求。按照采样进样介质的不同分为气体、液体、固体三类。对气体中有毒气体、大气颗粒物、VOCs,液体中水样、原油,固体中煤的机械化采样技术进行了概述,旨在帮助了解在线采样技术在国内矿业、环境行业的发展和应用。随着5G时代的到来,在线采样技术一定会发挥越来越重要的作用。     

Solid-phase microextraction under controlled agitation conditions for rapid on-site sampling of organic pollutants in water

An electric drill coupled with a solid-phase microextraction (SPME) polydimethylsiloxane (PDMS) fiber or a PDMS thin film was used for rapid sampling of polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. Laboratory experiments demonstrated that the sampling rates of SPME fiber and thin film can be predicted theoretically. Compared with the SPME fiber, the PDMS thin film active sampler exhibited a higher sampling rate and much better sensitivity due to its higher surface-to-volume ratio and its larger extraction phase volume. The amount of the analytes extracted by the thin film was around 100 times higher than those obtained by fiber, for both 5 min rapid sampling and equilibrium extraction. A new thin film active sampler was then developed for rapid on-site water sampling. The sampling kit included a portable electric drill, a copper mesh pocket, a piece of thin film, and a liner. Laboratory experiments indicated that the sampling remained in the linear uptake phase with this sampler to 8 min for the PAHs. Field test illustrated that this novel sampler was excellent for rapid on-site water sampling due to its short sampling period, high sampling efficiency and durability The thin film sampling kit facilitates on-site sampling, sample preparation, storage and transport. This new sampler is more user-friendly and easier to commercialize than previous samplers.     

Sampling and sampling strategies for environmental analysis

Sampling errors are generally believed to dominate the errors of analytical measurement during the entire environmental data acquisition process. Unfortunately, environmental sampling errors are hardly quantified and documented even though analytical errors are frequently yet improperly reported to the third decimal point in environmental analysis. There is a significant discrepancy in directly applying traditional sampling theories (such as those developed for the binary particle systems) to trace levels of contaminants in complex environmental matrices with various spatial and temporal heterogeneities. The purpose of this critical review is to address several key issues in the development of an optimal sampling strategy with a primary goal of sample representativeness while minimizing the total number of samples and sampling frequencies, hence the cost for sampling and analysis. Several biased and statistically based sampling approaches commonly employed in environmental sampling (e.g. judgmental sampling and haphazard sampling vs. statistically based approaches such as simple random, systematic random, and stratified random sampling) are examined with respect to their pros and cons for the acquisition of scientifically reliable and legally defensible data. The effects of sample size, sample frequency and the use of compositing are addressed to illustrate the strategies for a cost reduction as well as an improved representativeness of sampling from spatially and temporally varied environmental systems. The discussions are accompanied with some recent advances and examples in the formulation of sampling strategies for the chemical or biological analysis of air, surface water, drinking water, groundwater, soil, and hazardous waste sites.     

二元颗粒混合物按质量取样的误差研究

二元颗粒混合物的随机取样方式有两种：一是按颗粒数目取样,二是按质量取样本文对二元颗粒混合物按质量取样的误差进行了深入研究,详细分析了混合物的各种参对被测组分含量取样误差的影响,应用Ｍｏｎｔｅ Ｃａｒｌｏ技术对取样进行了模拟。以颗粒药品的二元混合物为例对按颗粒数目取样和按质量取样的误差进行了比较。此项研究对于分析取样理论和应用具有重要的价值。     

Quantitative Sampling of Trace Organic Vapours by Gas Syringe and Porous Polymer Adsorbent Methods. A Comparative Study Using Naphthalene as a Reference Substance

Abstract

Two methods of sampling high molecular weight vapours, gas syringe sampling and porous polymer adsorbent sampling were studied. The methods were compared using a saturated naphthalene reference vapour of known concentration. The results showed that the porous polymer adsorbent method was more accurate than the gas syringe method. The accuracies of both methods were dependent on details in their respective techniques. For porous polymer adsorbents it was shown that the technique should be such that passive sampling did not occur. Sample volume, sampling rate, the number of fills before injecting and cleaning the syringe before sampling all influenced the accuracy of the gas syringe sampling method.