提高火焰原子吸收灵敏度的途径

评述了提高火焰原子吸收灵敏度的各种途径 ,诸如包括MIBK -萃取 ,离子交换和沉淀在内的富集分离法 ,在线流动注射法 ,原子捕集法以及间接测定法等技术。     

强酸型离子交换纤维富集-火焰原子吸收测定水中痕量铜、铅、镉、镍

通过强酸型离子交换纤维柱,在同一水样中同时富集和洗脱了铜、铅、镉、镍,采用火焰原子吸收光谱法测定,并对富集条件及洗脱条件、干扰因素进行了探讨。该方法简便易行,回收率在96.1%~105.5%之间,测定的相对标准偏差小于5.0%。     

螯合树脂在线富集——火焰原子吸收光度法测定水中微量Cu,Pb,Zn,Cd

对螯合树脂在线富集，火焰原子吸收光度法进行了条件试验。试验证实方法对Ｃｕ、Ｐｂ、Ｚｎ、Ｃｄ４个元素检出浓度可达μｇ／Ｌ级，校准曲线性、样品重现性及准确度可满足测定要求。     

巯基棉富集分离水中痕量铅,镉,铜——火焰原子吸收测定法的研究

水中痕量铅、镉、铜的测定一般需采用石墨炉原子吸收法,此法对仪器要求高,耗费大,精密度、准确度相对较差.本文对巯基棉富集后用火焰原子吸收测定上述元素的方法进行了研究,并与蒸发浓缩和石墨炉原子吸收法作了对比.结果证明巯基棉富集——火焰原子吸收法测定水中微量铅、镉、铜能获得满意的结果.     

在线富集进样—火焰原子吸收法测定水中低含量Cu,Pb,Cd

用在线富集进样火焰原子吸收法测定水中低含量Ｃｕ,Ｐｂ,Ｃｄ,富集倍数分别烟１２２、１３６和９４倍,相对标准为１６％、１５％和４．６％,检测限为１．６μｇ／Ｌ和０．１８μｇ／Ｌ。探讨了分析精密度差的原因;改进了富集进样方法。     

HNO3—KI—MIBK萃取／原子吸收光谱法测定固体废物浸提液中的微量银

采用选择性较好的HNO3-KI-MIBK萃取体系对铋渣和尾矿渣浸出液中的痕量银进行预分离富集后，用火焰原子吸收法（AAS）进行测定，此法不仅变异系数小（约为3.1%)，而且检出限比直接火焰AAS法降低两个数量级，达0.5ng/ml。另外，还就样品细度对银测定结果的影响原因做了初步探讨。     

离子交换预富集—火焰原子吸收法测定降水中铜、锌、镉、铁、锰等重金属

利用离子交换树脂对降水中的铜、锌、镉、铁、锰等金属元素进行富集,之后经3 mol/L的盐酸进行洗脱,最后用火焰原子吸收分光光度法进行测定。该方法成本较低,操作简便,方法灵敏度高,方法检出限接近ppb级,对于降水中痕量金属元素的测定,结果令人满意。     

WF-8型在线富集进样器应用于水中痕量CuPbCd测定的研究

用 WF 8型在线富集进样器与火焰原子吸收光度计联用 ,应用于水中痕量 Cu、Pb、Cd的测定 ,其富集倍数分别是 1 2 2、1 3 6和 94倍 ,测定的精密度分别是 3 7%、2 8%和 3 9% ,检出限分别是 0 4 7、1 3和 0 2 2μg L,在地表水样中的加标回收率分别为 94 2 %～ 1 0 0 %、98 8%～ 1 0 7%和 1 0 8%～ 1 2 0 % ,并对 WF 8型进样器与火焰原子吸收光度计的成功联用 ,提出了一种新操作程序。     

HNO_3─KI─MIBK萃取／原子吸收光谱法测定固体废物浸提液中的微量银

采用选择性较好的ＨＮＯ３—ＫＩ—ＭＩＢＫ萃取体系对铋渣和尾矿渣浸出液中的痕量银进行预分离富集后，用火焰原子吸收法（ＡＡＳ）进行测定。此法不仅变异系数小（约为３．１％），而且检出限比直接火焰ＡＡＳ法降低两个数量级，达０．５ｎｇ／ｍｌ．另外，还就作品细度对银测定结果的影响原因做了初步探讨。     

在线离子交换-ICP-OES测定水中微量六价铬

建立了流动注射离子交换预富集与电感耦合等离子体原子发射光谱法(FIA-IE-ICP-OES)测定制革废水中微量六价铬的分析方法,确定了最佳的分析条件,其准确度和精密度较国标方法明显提高,检出限为0.003 mg/L。     

废水COD在线监测系统现场比对试验及管理的几点建议

通过分析总结辽宁省废水COD在线监测系统试点工作中在线监测系统的安装、验收、现场实际样品的比对分析,以及试运行过程中存在的问题,就今后废水在线监测系统的运行与管理提出相应的建议.     

The use of rapidly synergistic cloud point extraction for the separation and preconcentration of trace amounts of Ni (II) ions from food and water samples coupling with flame atomic absorption spectrometry determination

A novel improved preconcentration method known as rapidly synergistic cloud point extraction (RS-CPE) was established for nickel preconcentration and determination prior to its determination by flame atomic absorption spectrometry. In this work, the traditional CPE pattern was changed and greatly simplified in order to be applicable in metal extraction and detection. This method was accomplished in room temperature in 1 min. Non-ionic surfactant Triton X-114 was used as extractant. Octanol worked as cloud point revulsant and synergic reagent. The various parameters affecting the extraction and preconcentration of nickel such as sample pH, 2,2′-Furildioxime concentration, amounts of octanol, amounts of Triton X-114, type of diluting solvent, extraction time, and ionic strength were investigated and optimized. Under optimal conditions, the calibration curve showed an excellent linearity in the concentration range of 2–200 μg L^?1, and the limit of detection was 0.6 μg L^?1 for nickel. The developed method was successfully applied for the determination of nickel in food and water samples. The results showed that, the proposed method can be used as a cheap, rapid, and efficient method for the extraction and preconcentration of nickel from real samples.     

On-Line Adaptive and Nonlinear Process Monitoring of a Pilot-Scale Sequencing Batch Reactor

This article describes the application of on-line nonlinear monitoring of a sequencing batch reactor (SBR). Three-way batch data of SBR are unfolded batch-wisely, and then a adaptive and nonlinear multivariate monitoring method is used to capture the nonlinear characteristics of normal batches. The approach is successfully applied to an 80 L SBR for biological wastewater treatment, where the SBR poses an interesting challenge in view of process monitoring since it is characterized by nonstationary, batchwise, multistage, and nonlinear dynamics. In on-line batch monitoring, the developed adaptive and nonlinear process monitoring method can effectively capture the nonlinear relationship among process variables of a biological process in a SBR. The results of this pilot-scale SBR monitoring system using simple on-line measurements clearly demonstrated that the adaptive and nonlinear monitoring technique showed lower false alarm rate and physically meaningful, that is, robust monitoring results.     

污染源在线监控系统平台应用过程质量控制

根据质量管理的要求,结合污染源在线监控的特殊性,探讨了如何根据国家环境监测的质量管理体系,通过在线监控系统平台实现在线监测的质量管理目标,并提出了在线监控系统的质量控制指标体系及解决方案.     

化学需氧量和总有机碳在水质在线监测中的比较

化学需氧量(COD)和总有机碳(TOC)是定量表示水体受有机物污染的2个重要代表性指标。传统的COD在线监测方法在监测有机污染物方面存在一定的挑战,系统比较了COD和TOC在线监测方法在特殊水质中的应用。结果显示:TOC对难氧化有机物的氧化效率高达98%,高氯离子和无机还原性离子对TOC测量误差影响分别约为10%和7%。TOC可更直接、更准确地反映出水体受有机物污染的情况,最后对TOC指标在水质在线监测中的推广应用提出建议。     

PM2.5中OC/EC测定的离线分析法与在线分析法比较

采用离线分析法和在线分析法同步监测了武汉市PM_(2.5)中有机碳(OC)、元素碳(EC)和总碳(TC)的浓度,分析了2种方法的差别。结果表明,离线分析法与在线分析法对TC的测定结果具有很好的可比性,2种方法对TC的测定结果显著相关(r=0.970 9)。离线分析法得到的OC浓度普遍高于在线分析法,前者为后者的1.12倍,造成OC结果差异的主要原因可能是采样系统的差异。2种方法对EC测定的相关性较低(r=0.763 0),且2种方法对EC测定的精密度(相对偏差为13.14%)也不如其对TC和OC测定的精密度(相对偏差分别为3.42%和5.95%),造成EC结果差异的原因较复杂。离线分析法测得的OC/EC值明显高于在线分析法,鉴于OC/EC值在颗粒物源解析研究中具有重要意义,需要规范OC/EC分析方法。     

Speciation of arsenic in plants by HPLC-HG-AFS: extraction optimisation on CRM materials and application to cultivated samples

A recently developed method for the determination of arsenic species (arsenite, arsenate, monomethylarsonate, MMAA, and dimethylarsinate, DMAA) has been applied to the study of arsenic speciation in plants. This method uses ion-exchange liquid chromatography coupled on-line to atomic fluorescence spectrometry through continuous hydride generation. Various extraction procedures have been studied in detail using three plant certified reference materials. None of the procedures tested revealed fully satisfying results with all kinds of plant samples; microwave assisted extraction with 0.3 mol dm-3 orthophosphoric acid was found to be the most convenient for dealing with terrestrial plants. Species stability appears good. This method was applied to real world cultivated plant parts. Arsenate appears to predominate in soils, roots and leaves; unidentified species (probably arsenosugars) play an important role (60%) in rice fruits. Carrot was found to be the most contaminated edible plant part, containing 1 mg kg-1 essentially as arsenate species. MMAA was detected in all soils and some plant parts especially shallots at low levels, whereas DMAA was found only in one soil sample and in hot pepper leaves. Arsenite is a minor component of all soils; it is also present in some plant parts at low levels. However, no evident relationships were found between As speciation in the various plant parts and much more detailed studies will be necessary to elucidate As behaviour in plants.     

Direct coupling of supercritical fluid extraction-supercritical fluid chromatography for the determination of selected polycyclic aromatic hydrocarbons in aqueous environmental samples

A rapid and simple method is described for the quantitative determination of polycyclic aromatic hydrocarbons in aqueous environmental samples. A microscale on-line supercritical fluid extraction-supercritical fluid chromatography system using carbon dioxide is employed. The extract is analysed using capillary supercritical fluid chromatography with UV detection. Detection was carried out at 254 nm. An extraction efficiency of as high as 91% was obtained for the PAHs.     

UV Spectroscopic Monitoring of Vaporized Monoaromatic Hydrocarbons from Petroleum-Contaminated Soils

Fast and simple systems using ultraviolet (UV) absorbance were examined for on-line monitoring of monoaromatic hydrocarbons from petroleum-contaminated soils in this research. Since soil particles hinder the UV light transmittance, the absorbance measurement of vaporized monoaromatic hydrocarbons in soil gas extracted from petroleum-contaminated soils was proposed. In the fixed system that exhibited higher sensitivity than the portable one, the absorbance intensity of benzene, toluene, ethylbenzene, and xylene increased in proportion to the concentration of the contaminants. The portable system, however, was suitable for screening purpose, while it exhibited faster response. There was no interference from water, which helps the applicability of the proposed systems to the actual fields.     

人工神经网络用于铅的化学形态模拟计算

用前馈线性网络法求解水体系中Ｐｂ（２＋）与ＯＨ－之间的反应常数，不同训练算法对求解结果的精度、收敛速度及权值均有影响．结果表明，批处理算法的精度最好，权值不出现负值，但运算时间最长；在线算法的精度虽不如批处理算法，而比数据变换－在线算法好，权值有时会出现负值．运算时间较长；数据变换－在线算法的优点是运算时间短，但相对误差较大，权值出现负值的机会多。采用反馈网络模拟计算铅的各种化学形态的浓度．用物料核算的方法对反馈网络模型进行检验表明，此种模型用于平衡计算是可行的，详细分析了理论模拟和实验曲线的差异的原因，温度的影响最小，在４＜ｐＨ＜９时，ＣＯ有重要的影响．在国代检验时，ｎ值取整所引入的误差的影响亦不可忽视。从本文的结果可以看到，采用前馈网络和反馈网络相结合的方法考察水体中的化学形态是可行的．从而为解决这一类问题提供了一种可能的途径．