Coulometric determination of dissolved hydrogen with a multielectrolytic modified carbon felt electrode-based sensor

A multielectrolytic modified carbon electrode (MEMCE) was fabricated by the electrolytic-oxidation/reduction processes. First, the functional groups containing nitrogen atoms such as amino group were introduced by the electrode oxidation of carbon felt electrode in an ammonium carbamate aqueous solution, and next, this electrode was electroreduced in sulfuric acid. The redox waves between hydrogen ion and hydrogen molecule at highly positive potential range appeared in the cyclic voltammogram obtained by MEMCE. A coulometric cell using MEMCE with a catalytic activity of electrooxidation of hydrogen molecule was constructed and was used for the measurement of dissolved hydrogen. The typical current vs. time curve was obtained by the repetitive measurement of the dissolved hydrogen. These curves indicated that the measurement of dissolved hydrogen was finished completely in a very short time (ca. 10 sec). A linear relationship was obtained between the electrical charge needed for the electrooxidation process of hydrogen molecule and dissolved hydrogen concentration. This indicates that the developed coulometric method can be used for the determination of the dissolved hydrogen concentration.     

环境水中总挥发性有机硫化物的检测方法

建立了一种捕集、解析、氧化、紫外荧光检测技术,用于水中痕量总挥发性有机硫化物的检测.自行研制的低温捕集－热解析装置实现水中痕量挥发性有机硫化物的富集,富集的有机硫化物在高温和助燃气作用下,充分氧化为二氧化硫,采用紫外荧光法检测二氧化硫含量,从而间接获得水中总挥发性有机硫化物的浓度值.方法的捕集温度5℃,解析温度150℃,氧化温度1000℃,气提室温度65℃,气提时间20min,精密度5.5%,检测限为6ng/L,加标回收率为91.6%~95.1%.利用该装置对青岛市某池塘水样进行检测分析,检测结果中总挥发性有机硫化物的含量为1503~1911ng/L.     

大气中总挥发性有机硫化物检测方法的研究

建立了一种捕集、解析、氧化、紫外荧光检测技术,用于大气中痕量总挥发性有机硫化物的检测.自行研制的低温捕集-热解析装置综合了固体阻留法和低温冷凝法的优点,应用于大气中痕量挥发性有机硫化物的富集,富集的有机硫化物在高温和助燃气作用下,充分氧化为二氧化硫,采用紫外荧光法检测二氧化硫含量,从而间接获得大气中总挥发性有机硫化物的浓度值.方法的捕集温度5℃,解析温度150℃,氧化温度1 000℃,精密度5.46%,回收率为99.6%～109.2%.利用该装置测定了2011年2～4月青岛大气中痕量总挥发性有机硫化物的含量为42～195 ng·m-3.     

Modelling of the relationship betwen trace elements and three species of sulfur in coal

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Modelling of the relationship between trace elements and three species of sulfur in coal

Based on the determination of several trace elements in coal particulate of different specific gravity, three-variables regression equations relate the contents of trace elements Be, Cd, Co, Pb, Cu, Ni, As and three species of sulfur in coal were well established. For elements Cd, Co, Pb, Cu and Ni, the regression equations were successfully used for prediction of these trace elements in individual part of coal with different specific gravity. Factor analysis was also used to analyze the data sets. The results showed that a three factor model can interpret the data sets reasonably. Trace elements Cd, Co, Pb, Cu, Ni, inorganic sulfide and total sulfur in coal are high correlated with the first factor. Trace elements Be, sulfate and organic sulfide are high correlated with the second factor and trace elements Cr and As are high correlated with the third factor. The factors can be interpreted by the chemical properties of these elements.     

阻抑动力学光度法测定痕量邻二硝基苯

研究发现,在盐酸介质中,痕量邻二硝基苯能灵敏地阻抑溴酸钾氧化甲基红褪色的反应。研究了该阻抑褪色反应的最佳条件,建立了一种测定痕量邻二硝基苯的新方法。该方法线性范围为0.0～0.16μg,检测限为1.15×10-10gmL。用于环境水样中邻二硝基苯的测定,结果满意。     

流动注射在线离子交换富集-原子荧光光谱法测定环境水样中痕量汞

提出了一种流动注射在线离子交换富集一氢化物发生原子荧光光谱法测定水样中总汞的分析方法。设计了双柱并联富集，串联洗脱的在线离子交换流路及操作程序，优化了各项化学条件及流路参数。方法操作简便快速，灵敏度高，干扰少。富集倍数达25倍以上，采样频率为30次／h，回收率达90％－105％。应用于环境水样中痕量汞的测定，获得了满意的结果。     

水中毒死蜱的固相萃取气相色谱测定法

建立水中毒死蜱的固相萃取——气相色谱FPD测定法。本方法的线性范围为0.25～5.00mg/L,回收率为94.2%,RSD为2.5%,检出限为0.25μg/L。该方法灵敏、准确,能很好地排除干扰,可满足水中痕量毒死蜱的测定。     

阻抑动力学光度法测定痕量锡

基于痕量锡在稀硫酸介质中对溴酸钾氧化酸性品红反应的抑制作用 ,建立了测定痕量锡的动力学光度法 ,检出限为 1 .6× 1 0 - 11/ g·m L- 1,测定范围为 0～ 0 .2 / μg· 2 5 m L- 1。用于天然水中痕量锡的测量。     

测定地表水中微量亚硝酸盐的灵敏光度法

研制了一种测定微量亚硝酸盐的灵敏光度法。在pH1 0～ 2 0盐酸介质中 ,亚硝酸盐与对氨基苯乙酮 萘乙二胺形成可溶于水的红紫色染料 ,其最大吸收波长为 5 5 0nm ,摩尔吸光系数为 5 78× 10 4L mol·cm。 0～ 3 6 μg 2 5mL的亚硝酸盐遵守比尔定律 ,方法应用于测定地表水中微量亚硝酸盐 ,获得了满意的结果     

离子色谱法测定水中总硬度

水质硬度的测定方法很多,本研究选用离子色谱法和EDTA络合滴定法对地下水和地表水样品分别进行测定,结果表明离子色谱法相对于传统的EDTA络合滴定法有干扰小,对环境污染少的优点,但水质测定的国标方法中没有该方法,因此建议可用离子色谱法测定水质硬度。     

流动注射化学发光测定痕量亚硝酸根的研究

基于NO_2~-对I_2-EDTA光化学反应的抑制作用和I_2与鲁米诺的化学发光反应,建立了痕量亚硝酸根的流动注射化学发光分析方法.试验并选择了最佳条件,测定了天然水中亚硝酸根的含量,回收率在93—103.5％,方法线性范围为1.0×10~(-7)—4.0×10~(-6)mol.L~(-1),检测限为1.1×10~(-6)mol.L~(-1).对2.0×10~(-7)mol·L~(-1)NO_2~-进行测定,相对标准偏差为2.2％.     

水中痕量微囊藻毒素的检测

微囊藻毒素是由蓝藻产生的一类环状七肽物质,该毒素可引起动物中毒并对人类产生危害,迫切需要对饮用水源中的微囊藻毒素进行检测.实验建立了固相萃取(SPE)结合高效液相色谱(HPLC)分析水中痕量微囊藻毒素方法,该方法快速、灵敏,适用于快速分析环境水样中的2种常见微囊藻毒素MC-LR和MC-RR,绝对量检出限可达1.00 ng,线性定量范围为0.125～50 μg/L.      

Determination of arsenic in air particulates and diesel exhaust particulates by spectrophotometry

A method was developed for the determination of trace arsenic by spectrophotometry. The proposed method is rapid, simple,and inexpensive. This method can be used for sensitive determination of trace arsenic in environmental samples and especially in air particulates. The results obtained by this method as a proposed method were compared with those obtained by hydride generation atomic absorption spectrometry as a popular reported method for the determination of arsenic and an excellent agreement was found between them. The method was also used for determination of arsenic associated with airborne particulate matter and diesel exhaust particulates.The results showed that considerable amount of arsenic are associated with diesel engine particulates. The variation in concentration of arsenic was also investigated. The atmospheric concentration of arsenic was different in different sampling stations was dependent to the traffic density.     

固相萃取-气相色谱/质谱法测定水中四乙基铅的方法研究

建立了固相萃取-GC/MS法测定水中四乙基铅的方法。对固相萃取条件、气相色谱条件和质谱条件进行了优化,并对实际水样进行了测定。方法检出限为0.004μg/L,水样的加标回收率为71.5%～103.2%,精密度(RSD,n=6)为4.4%～11.6%。方法准确、灵敏可靠、干扰小、适应范围广,可以满足水中痕量四乙基铅的分析要求。     

富氧空气—乙炔火焰原子吸收法测定水样中锶

研究了富氧空气-乙炔火焰原子吸收光谱法测定锶的方法,优化了实验条件,选择了最佳的观察高度、氧气流量和乙炔流量,研究了有机试剂的增感作用,0.5%的磺基水杨酸可以提高测定的灵敏度约40%,并可很好的抑制共存离子的干扰,方法的检出限为4ng/mL,该法快速、简便、准确,适合一般水样中痕量锶的测定。     

Determination of paraquat in water samples using a sensitive fluorescent probe titration method

Paraquat (PQ), a nonselective herbicide, is non-fluorescent in aqueous solutions. Thus, its determination through direct fluorescent methods is not feasible. The supramolecular inclusion interaction of PQ with cucurbit[7]uril was studied by a fluorescent probe titration method. Significant quenching of the fluorescence intensity of the cucurbit[7]uril-coptisine fluorescent probe was observed with the addition of PQ. A new fluorescent probe titration method with high selectivity and sensitivity at the ng/mL level was developed to determine PQ in aqueous solutions with good precision and accuracy based on the significant quenching of the supramolecular complex fluorescence intensity. The proposed method was successfully used in the determination of PQ in lake water, tap water, well water, and ditch water in an agricultural area, with recoveries of 96.73% to 105.77%. The fluorescence quenching values (ΔF) showed a good linear relationship with PQ concentrations from 1.0×10^-8 to 1.2× 10^-5 mol/L with a detection limit of 3.35×10^-9 mol/L. In addition, the interaction models of the supramolecular complexes formed between the host and the guest were established using theoretical calculations. The interaction mechanism between the cucurbit[7]uril and PQ was confirmed by ¹H NMR spectroscopy.     

复合螯合剂/活性碳分离富集和ICP—AES同时测定水样中痕量元素

本文提出将复合螯合剂（NaDDTC／8—Oxin）饱和吸附于活性碳上作为吸附材料．分离富集和ICP—AES同时测定水中痕量金属元素的方法。用ICP—AES研究了该吸附材料对某些痕量元素的吸附和解吸性能；考察了共存元素的影响。方法应用于湖水中Fe、Cu、Mn、Y和Sc的测定，检出限为ng／ml级，RSD为1．9％～4．4％，加入回收率81％～101％间，试样分析结果满意。     

丙酮－H_2O_2－ClO~－化学发光新体系的研究及应用

本文针对碘量法测定痕量次氯酸根（ＣｌＯ－）时，滴定中存在费时费试剂、痕量测定准确度欠佳的问题，研究并建立了流动注射化学发光法测定痕量ＣｌＯ－的新方法，具有较高的灵敏度、较好的准确度、重现性，为ＣｌＯ－的测定提供了一条新途径．该法在水质检验和环境监测中有一定的适用性．     

湖泊水体悬浮物中痕量砷的测定方法

重金属在悬浮物和水相中的分配是水体重金属形态研究的重要组成部分,对于追踪水体中重金属元素的来源、迁移转化规律以及重金属生态与健康效应具有重要意义.水中砷元素以其极强的毒性严重危害人类的健康,已越来越引起政府和社会的广泛关注.然而,目前关于痕量悬浮物中砷测定的前处理过程及室内分析的方法与质量控制的叙述不够详尽,有必要对此做深入的研究.本文针对悬浮物较少的水域,选用7个滇池水样,采用不同滤膜、不同预处理方法、不同消解用酸及消解时间,测定并比较砷空白值,试图通过改变实验条件降低空白值,探索前处理的最佳条件及步骤.结果表明,对于悬浮物较少的湖泊水域,采用预称重的醋酸纤维膜过滤水样、载有颗粒物的滤膜冷冻干燥、HNO3-HCl O4加热共消解36 h,消解上清液用氢化物发生原子荧光光度计测定砷空白值低于悬浮物一个数量级以上,膜空白砷相对标准偏差为2.80%~11.38%,膜空白加标回收率为83%~103%;与滇池5个实际样品验证误差范围0.27%~6.92%.此方法可以可靠地获得悬浮物中的砷含量,在砷含量较低的水体悬浮物测定方面具有优势.