用ICS-90型离子色谱仪测定水中钙离子的不确定度分析

对离子色谱法测定水中钙离子的不确定度进行评定,并分析了其影响因素主要有来自重复测量引入的A类不确定度和来自工作曲线的不确定度以及来自标准溶液的不确定度。     

离子色谱法测定降水中部分阴离子含量的测量不确定度评定

通过对离子色谱法测定降水中F^-、Cl^-、NO3^-、SO4^2- 测量不确定度的分析，找出导致不确定度的因素。对测量不确定度进行计算和评定，结果表明，影响其测量不确定度的主要因素是标准曲线精密度。     

离子色谱法测定水中氟离子含量的不确定度评定

文章对离子色谱法测定水中氟离子(F-)可能产生的不确定度来源进行全面分析,通过对氟离子测定结果的不确定度的量化评定,得出由线性最小二乘法拟合曲线所产生的不确定度对总不确定度贡献最大,占总不确定度的33.3%。     

离子色谱法测定水中亚硫酸根的优化

为了提高离子色谱法测定水中亚硫酸根的准确性,通过条件实验,对亚硫酸根稳定性、淋洗液有机改进剂等进行优化。选择Metrosep A Supp 5150色谱柱,以3.2 mmol/L的碳酸钠+1.0 mmol/L的碳酸氢钠+5.0%的丙酮溶液为淋洗液,经离子色谱检测,亚硫酸盐的质量浓度在0~10.0 mg/L范围内与色谱峰面积线性关系良好,检出限为0.034 mg/L。实际样品测定结果的相对标准偏差为2.4%~4.7%,加标回收率为96.8%~103%。该方法可延长亚硫酸盐标准溶液的保存时间,有效分离亚硫酸根和硫酸根,灵敏度高、正确度与精密度良好,适用于水中亚硫酸根的测定。     

石墨炉原子吸收光谱法测定全血中铅的不确定度评定

根据《测量不确定度评定与评定表示指南》(JJF 1059-1999)建立了石墨炉原子吸收光谱法测定全血中铅不确定度的数学模型,分析了测试过程中不确定度的来源,并对各不确定度分量进行量化。本次测量的合成相对不确定度值为0.047 3,其中最大的分量是样品消化前处理重复测定引入的,其不确定度分量值为0.04。本次全血中铅测定结果为(130.7±12.4)μg/L,k=2,即测定结果置信水平为95%。     

碱片-离子色谱法测定硫酸盐化速率影响因素

采用碱片-离子色谱法测定空气的硫酸盐化速率,方法在硫酸盐质量浓度为1.00~20.0 mg/L范围内线性良好(r≥0.999 0);碱片剪碎或不剪碎对空白碱片中硫酸根离子质量浓度的测定无明显影响,且高低两种加标浓度的回收率均在80.0%~120%之间;对于碱片实际样品,碱片剪碎更有利于硫酸根离子的快速溶出;随浸泡时间的延长,碱片中溶出的硫酸根离子质量浓度呈上升趋势,7 h硫酸根离子基本溶出完全,从保证结果质量和节省时间的角度考虑,确定最佳浸泡时间为3.5 h,建议碱片全部采取剪碎处理。     

离子色谱法测定大气降水中的氟离子、乙酸、甲酸、氯离子、硝酸根和硫酸根离子

用氢氧化钾淋洗离子色谱法同时测定降水样品中的氟离子、乙酸、甲酸、氯离子、硝酸根、硫酸根离子等无机和有机阴离子。该方法简便、快速、精密度好、6种阴离子在12min内全部分析完毕。8次测试的相对标准偏差小于2.8%,检出限在0.39~7.6μg/L之间,加标回收率在94.7%~105.3%之间,能满足降水样品中阴离子的检测,是降水样品中阴离子检测的理想方法。     

滤膜氟离子选择电极法测定大气中氟化物的改进

通过对国标方法中标准溶液系列的配制、样品滤膜处理方法进行研究,改进滤膜采样氟离子选择电极法测定大气中氟化物的实验方法,并利用改进方法对大气样品和氟化物标准样品进行对比实验。结果表明,标准样品的标准偏差为0.010~0.019 mg/L,相对标准偏差为3.0%~3.2%;大气样品的标准偏差为0.058~0.12μg/m3,相对标准偏差为4.2%~4.5%,加标回收率在95%~105%之间,满足国家标准的要求。     

热分解法测定水质中总氮的不确定度分析

采用实验测定和误差分析的方法,对TOC分析仪测定水质中总氮含量的不确定度进行了分析,测量过程中不确定度的来源有样品重复性测量、标准曲线拟合、标准溶液配制、测量仪器本身等,量化估算了不确定度的各分量。结果表明,标准曲线拟合是影响水质中总氮测定不确定度的主要因素,其次为标准溶液配制所产生的不确定度,样品重复性测量和测量仪器本身所产生的不确定度也不容忽视。同时提出了在测定过程中减小不确定度的有效途径。     

离子色谱仪分析测定制药废水中的氟离子

文中主要介绍离子色谱仪在环境监测中的应用，特别是样品的前处理技术。并例举了应用离子色谱仪分析测定制药废水中的氟离子的全过程来说明只要对样品进行有效的预处理。很多复杂样品均能应用离子电谱仪进行分析测定。     

离子色谱技术在环境监测中的应用

详细介绍了离子色谱仪的构造，功能，以及离子色谱技术的发展状况，离子色谱作为一种新的分析方法以其独特的优点可广泛应用于水，气，土壤，生物等环境监测领域。     

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。     

离子色谱分析中的几个问题探讨

在掌握离子色谱技术最新发展动态的基础上,对离子色谱的新进展、前处理新技术、常用的改善分离度方法、若干注意事项、常遇到的问题等进行了分析探讨,以期用离子色谱技术更多更好地解决实际问题.     

A conductive polypyrrole based ammonium ion selective electrode

In view of the development of miniaturized sensor arrays, a solid-contact ammonium ion selective electrode has been investigated. A conductive polypyrrole film was electrochemicallydeposited on a glassy carbon surface and used as an internal solid contact layer between the sensing membrane and solid electrode surface. A systematic evaluation of the importantparameters affecting the electromotive force (emf) response ispresented. The performances of this solid-contact sensor were verified using a batch-mode measurement setup and a wall-jet flow cell system. The designed sensor exhibited excellent selectivity for the primary ion and a linear response over the pNH₄ ⁺ range 1–5 with a slope of 56.3 mV decade^-1. The sensor has a fast response and is relativelyrobustness, and was also used to determine ammonium concentrations in natural waters, with promising results.     

Detection of sulfur-free odorants in natural gas using ion mobility spectrometry

Beside the primary motivation of the public gas suppliers for odorizing natural gas with a sulfur-free odorant, which relates to the image of the environment-friendly fuel, natural gas, competing with low-sulfur heating fuel and diesel, a question of crucial importance of how to detect such sulfur-free odorants comes up. Concerning the replacement of sulfur-containing by sulfur-free odorization, the availability of a fast and sensitive detection method that can, further, be used on-site plays a key role. The minimum concentration of the new sulfur-free odorant Gasodor S-Free (S-Free) in natural gas should be added at a level of at least 8.8 mg m(-3) to assure a significant warning smell. Therefore, a dynamic range between 0 and approx. 25 mg m(-3) must be realised in the rather complex matrix of natural gas. By means of a handheld ion mobility spectrometer, the odorant content in natural gas is determined within less than 80 s total analysis time directly at the gas pipe. The concentration of S-Free is monitored between 4 and 23 mg m(-3) respecting the quality of the natural gas (high- and low-caloric gas). Results of the validation using a gas chromatograph as a reference standard will be discussed in detail.     

离子色谱法测定空气中的甲酸和氯化氢含量

阐述了离子色谱法测定空气和环境样品中甲酸、氯化氢含量的方法与步骤。测定结果显示,甲酸和氯化氢的检测限分别为0.01mg/L、0.02mg/L,方法的回收率为98%～101%、98%～102%,相对标准误差为1.9%、1.6%,线性范围为0.00～10mg/L、0.00～16mg/L,是一种简单、快速、可靠测定降水、空气、废气、地表水、地下水中甲酸和氯化氢的好方法。     

北京市大气颗粒物的浓度水平和离子物种的化学形态

用离子色谱法测定了 1 998年 1 1月至 1 999年 2月期间的 2 4个总悬浮颗粒物 (TSP)样品中 NH+ 4、NO- 3、SO2 - 4和Na+ 质量浓度。研究结果表明 ,北京市冬季大气颗粒物中离子物种的化学形态可以分为三种情况 :污染严重时 ,离子物种以 H2 SO4 、NH4 HSO4 、Na NO3为主要存在形态 ,气溶胶酸性强 ;污染轻时 ,离子物种以 (NH4 ) 2 SO4 、Na NO3为主要存在形态 ,气溶胶呈弱酸性 ;中等污染时 ,离子物种以 (NH4 ) 2 SO4 、NH4 HSO4 、Na NO3几种化学形态存在 ,气溶胶呈中等酸性     

Determination of trace transition metals in environmental matrices by chelation ion chromatography

Trace transition metals (Fe^3?+?, Mn, Cu, Cd, Co, Zn, Ni) in environmental samples were analyzed by chelation ion chromatography using a mixed bed ion-exchange column with pyridine-2,6-dicarboxylic acid (PDCA) and oxalic acid as eluent and large volume direct injection (1,000 ??l). The two eluents, PDCA and oxalic acid, were tested, and repeatability and detection limits were compared. The total analysis time was ~15 min. The separation with PDCA was more successful than that obtained with acid oxalic. It was observed that utilizing PDCA resulted in lower detection limits, higher repeatability, and a quantitative detection of Cd and Mn, which coelute as a single peak when using the oxalic acid. At last, the PDCA calibration graphs resulted linear (r ²?>?0.999) in the range 0.4?C1,000 ??g/L. The procedure was applied to the analysis of metals in soils and in water samples. The results obtained from the analysis of natural waters have demonstrated that the method is simple and efficient, therefore, can be used for the determination of metals in natural waters using a continuous and automatic monitoring system.     

31P-NMR evaluation of organophosphorus pesticides degradation through metal ion promoted hydrolysis

The degradation of some organophosphorus pesticides (OPPs) in the presence of metal ions was studied by ³¹P-NMR spectroscopy. Both ³¹P-NMR and gas chromatography/mass spectroscopy results were used in order to determine the nature of metabolites formed after degradation. The degraded organophosphorus pesticide were investigated for chlorpyrifos and phoxim in the presence of several metal ions including Hg²⁺, Cu²⁺, Cd²⁺, Ni²⁺, Pb²⁺, and Ag⁺. ³¹P-NMR results indicated Ag⁺ and Hg²⁺ ion promoted degradation of OPPs and other metal ions formed complex with OPPs and cannot degrade OPPs. We found that the degradation of chlorpyrifos and phoxim with Ag⁺ or Hg²⁺ led to the formation of O,O-diethyl-O-methyl phosphorothionate, (C₂H₅O)₂(CH₃O)PS, at metal ion/pesticide mole ratios ≤1.0 and completely decomposed at a higher mole ratio of 10. Finally, the method was successfully applied to the degradation study of a number of technical and formulated pesticides in the presence of Ag⁺ ion at a metal ion/pesticide mole ratio of 10.     

Ion-soot interaction: a possible mechanism of ion removal in aircraft plume

The phenomenon of the ion-soot interaction in the aircraft plume at the ground conditions is investigated. The ion-soot attachment coefficients, taking into account the polarization of the soot particles in the ion electric field, are calculated. It is shown that the ion-soot attachment may play the important role in the evolution of the ion concentrations in the plume. Comparison of the model results with the ground-based measurements for the ion depletion along the plume demonstrates that the concentration of the positive and negative ions at the nozzle exit for these observations is close to 1.2 x 10(8) cm(-3).