土壤、沉积物系列标准物质中38种元素的ICP-MS定值

探讨了电感耦合等离子体质谱测定土壤元素的基体效应及元素间的基体干扰，采用模拟土壤元素天然组成比值的校正溶液，利用^115In-^103Rh双内标校正系统有效地抑制了分析信号的动态漂移，建立了测定土壤中元素的ICP－MS方法；对GBW07410－07416土壤、沉积物系列标准物质进行定值，测定结果与XRF分析结果比较，同时用于GBW07404、GBW07405、GBW07408、GBW07309管理样分析，结果令人满意。     

ICP–MS将首入水质检测标准

<正>不久前,环保部公布了国家环境保护标准《水质65种元素的测定电感耦合等离子体质谱法》(征求意见稿),这是ICP–MS法(电感耦合等离子体质谱法)首次进入我国水质检测标准,而且和EPA 200.8,EPA 6020A,EPA 200.1,ISO17294–2等国际标准相比,这一新标准可用于更多水中元素的测定。以ICP–MS法对水中铁(Fe)、钛(Ti)、铌(Nb)3种元素的测定,尚未在其它国外标准方法中被采用。另外,由于目前国内需要消解处理的地表水和废水(处理设施出口)中无机元素总量的测定尚没有统一的前处理方法,新标准采     

高效液相色谱/电感耦合等离子体质谱联用技术用于元素形态分析的研究进展

介绍了高效液相色谱与电感耦合等离子体质谱（HPLC－ICP－MS）联用技术在环境、材料和生命科学样品的元素形态分析中的研究进展，着重介绍该联用方法的接口技术及几种与ICP－MS联用的主要色谱类型，阐述了几种样品预处理方法，并对样品引入系统、复杂基体分离和元素形态定量和结构分析等联用技术在元素形态分析中所面临的问题进行讨论。     

鲜魔芋及其种植土壤中矿物元素的ICP-AES法测定

采用电感耦合等离子体原子发射光谱法（ICP－AES）测量了不同产区鲜魔芋球茎及其种植土壤中10种矿物元素的含量，并初步讨论其相关性；采用湿法消化处理样品并考察了不同元素测定的精密度、回收率；测定的相对标准偏差（RSD）均小于2％，回收率为95％－104％，结果可信度高。     

固相萃取-衍生化-气相色谱质谱法测定水中9种烷基酚类化合物

针对地表水、地下水及饮用水中9种烷基酚类化合物的含量检测，建立了一种适合于气相色谱-质谱分析的衍生化方法。分别对样品预处理的衍生化温度、反应时间、水体样品pH、洗脱溶剂类型及用量进行优化。优化结果表明，烷基酚类化合物的质量浓度在20.0～1 000μg/L范围内与色谱峰面积具有良好的线性关系，线性相关系数均不低于0.999 1，方法检出限为4.49～9.46 ng/L。地表水、地下水及饮用水样品加标回收率为77.6%～98.8%，测定结果的相对标准偏差不大于11.4%(n=7)。该方法适用于地表水、地下水及饮用水中烷基酚类化合物的检测。     

预富集电感耦合等离子体质谱法测定地下水中超痕量稀土元素及钪、钇

以P507萃淋树脂为固定相，HCl/EDTA为流动相，建立了地下水中超痕量稀土元素及钪、钇的ICP－MS测定的新方法。详细探讨了稀土元素（REEs）、Sc、Y与基体元素的分离、EDTA小体积洗脱的实验条件及ICP－MS工作参数。在pH2.6时上柱，大部分Ca、Mg，其体可不经淋洗而直接与REEs分离；以100mmol的EDTA洗脱，5mL淋洗体积REEs、Y、Sc回收率为96％－98.5%。详细考察了La、Ce、Pr的氧化物离子及氢氧化物离子的干扰及校正方法。分析方法的检测限为0.7-10.1ng/L，加标回收率为95％－99％。用于实际地下水及人工模拟水样的分析，结果令人满意。     

脱线柱预富集 ICP-MS法测定南极水样中的痕量元素

采用脱螯合阳离子树脂（D401）将待分析元素预富集并与基体元素分离，采用电感耦合等离子体质谱法（ICP－MS）测定了极拉斯曼丘陵地区环境水样中的难于或不能直接检测的超痕量元素Mn,Co,Ni,Cu,Cd,Ba和Pb；建立了一种准确，简便、快速的在线加内标准方法，被分析元素的测定灵敏度均提高了30倍左右；对于100mL，水样检测限为1．425ng/L-24.84ng/L。     

ICP-AES法同时测定石英砂中的痕量元素

采用微波溶样，并通过条件试验，建立了微波溶样ICP－AES法同时测定石英砂中13种痕量元素的分析方法并已应用于实际样品的分析，方法的相对标准偏差≤10％，加标回收率为90％－107％。     

锆存在时铀中杂质元素的化学分离-ICP-AES法

采用磷酸三丁酯（TBP）－氢化煤油萃取油、过氧化氢掩蔽钛、磷酸氢二铵沉淀锆的方法，用ICP－AES法同时测定了锆存在在时铀中的铁、锰、铜、硅、铝、镍和钛7种杂质元素的含量。当测定范围在100μg/g-1000μg/g时，相对标准偏差＜9．0％，回收率为96％－109％。     

HPLC-ICP-MS在紫菜中砷形态分析的应用

通过HPLC－ICP－MS联用技术初步探讨了紫菜中砷的形态；选用了纯水萃取，再用甲醇稀释，用阴离子交换色谱柱经HPLC分离，再用ICP－MS测定，实验发现了2个未知形态色谱峰；该技术将液相色谱的分离技术与ICP－MS高灵敏度的检测方式相结合，具有分离效果好，灵敏度高，耗样量少，速度快，线性范围宽等优点。     

电感耦合等离子体发射光谱(ICP-OES)法同时测定矿泉水界限指标中的4种元素

国家标准方法中,对矿泉水界限指标中的四种矿物质元素锌、锂、锶、偏硅酸(以H2SiO3计),需每种元素分别测定且步骤繁琐,采用电感耦合等离子体发射光谱(ICP-OES)法对矿泉水中这4种元素的含量进行同时测定,四种元素的检出限在0.01~0.10 mg/L,对市售矿泉水进行了检测,加标回收率在83%~100%,相对标准偏差为0.31%~2.0%,方法简便省时,精密度和准确度较高,可以作为一种鉴别矿泉水品质的方法。     

ICP-OES同时测定矿泉水界限指标中的4种元素

矿泉水界限指标中的四种矿物质元素锌、锂、锶、偏硅酸(以H₂SiO₃计),国标方法需每种元素分别测定且步骤繁琐,本实验采用ICP-OES对矿泉水中这4种元素的含量进行同时测定,四种元素的检出限在0.01~0.10 mg/L,对市售矿泉水进行了检测,加标回收率在83 %~100 %,相对标准偏差为0.31 %~1.96 %,方法简便省时,精密度和准确度较高,可以作为一种鉴别矿泉水品质的方法。     

心血管病患者饮用天然矿泉水的探讨

天然矿泉水是来自地下深处的泉水，水质清纯无污染，含有人体必需的微量元素。分析测定了来自不同地区的矿泉水样，对矿泉水中硅元素（硅酸含量）与钾、钠元素含量进行相关性研究，并从医学角度为心血管病患者饮用天然矿泉水提供依据。     

Performance of total reflection and grazing emission X-ray fluorescence spectrometry for the determination of trace metals in drinking water in relation to other analytical techniques

An intercomparison survey has been carried out in order to evaluate the performance of two related X-ray fluorescence techniques as compared to the achievements of several other analytical techniques applied for trace elements determination in drinking water. A relatively new technique, total reflection X-ray fluorescence (TXRF) and a novel related technique, grazing emission X-ray fluorescence (GEXRF) have been used for the analysis of a mineral water sample. The concentrations of the following elements have been determined: Na, Mg, K, Ca, Ni, Cu, Zn and Sr. The mineral water sample has also been analyzed by a number of other analytical techniques, routinely utilized in drinking water quality control. The analyses were performed in eleven laboratories which reported 286 individual determinations producing 75 laboratory means. From the obtained results, it can be concluded that the TXRF technique is suitable for a direct determination of heavy elements in drinking water (above potassium, Z = 19). This technique can compete with other analytical techniques routinely used in water quality monitoring. First results obtained with GEXRF spectrometry show that this technique can be successfully applied for the determination of low-Z elements in drinking water. However, results for sodium and magnesium were systematically too low, indicating that modifications of the quantification procedure may be required to improve the accuracy of determination for these light elements.     

火焰原子吸收光谱法测定温泉矿泉水中微量元素

用火焰原子吸收光谱仪对乌鲁木齐市水磨沟区温泉矿泉水中的铜、钾、锌、钙、镁等微量元素进行了分析测定,并探讨了酸度、干扰离子对测定的影响.同时用吸光光度法测定了矿泉水中铁,用容量分析法测定了矿泉水中硫化氢,取得较好的结果.     

福州市售蔬菜和水果中13种矿质元素含量的测定与分析

为了解福州市冬季市售蔬菜和水果中矿物质元素含量,给福州市居民合理选择食物提供指南,用湿法消化法对样品进行预处理,经ICP—AES和ICP—MS法测定样品矿物质元素含量,采用相关分析等统计方法对结果进行了综合评价。结果表明,所测蔬菜中莲藕、小白菜、西兰花、马铃薯、四季豆、芥菜和大蒜各种矿物质含量较高,水果中青橄榄、荸荠、芦柑、草莓各种矿物质含量较高,市民可根据个人对营养的需求,合理选择,科学搭配;相关分析表明,大部分元素之间都有显著的正相关性,仅P与所测元素之间表现出一定的负相关性。可见所测蔬菜和水果中含有丰富的矿物质元素,这些矿物元素之间的交互关系主要以协同作用为主。     

黄龙山天然矿泉水临床应用观察

观察了黄龙山天然矿泉水系统治疗多种常见慢性病,如：消化功能紊乱,小儿厌食症,高血压病,神经衰弱、皮肤病等的效果,总有效率达92．58%,其原因是该矿泉水富含人体必需微量元素。     

Performance of total reflection and grazing emission X-ray fluorescence spectrometry for the determination of trace metals in drinking water in relation to other analytical techniques

An intercomparison survey has been carried out in order to evaluate the performance of two related X-ray fluorescence techniques as compared to the achievements of several other analytical techniques applied for trace elements determination in drinking water. A relatively new technique, total reflection X-ray fluorescence (TXRF) and a novel related technique, grazing emission X-ray fluorescence (GEXRF) have been used for the analysis of a mineral water sample. The concentrations of the following elements have been determined: Na, Mg, K, Ca, Ni, Cu, Zn and Sr. The mineral water sample has also been analyzed by a number of other analytical techniques, routinely utilized in drinking water quality control. The analyses were performed in eleven laboratories which reported 286 individual determinations producing 75 laboratory means. From the obtained results, it can be concluded that the TXRF technique is suitable for a direct determination of heavy elements in drinking water (above potassium, Z = 19). This technique can compete with other analytical techniques routinely used in water quality monitoring. First results obtained with GEXRF spectrometry show that this technique can be successfully applied for the determination of low-Z elements in drinking water. However, results for sodium and magnesium were systematically too low, indicating that modifications of the quantification procedure may be required to improve the accuracy of determination for these light elements. Received: 5 January 1998 / Revised: 17 February 1998 / Accepted: 18 February 1998     

Study of interlayer water on the active sites of mineral sorbent: Thermal analysis

The programmed heating of montmorillonite samples is accompanied by their dehydration and dehydroxilation, this being registered by means of Derivatograph. The form of the endothermal effects within the 80–250°C interval can be of simple or double character depending on the nature of exchange cations. Though this phenomenon has been known for a long time, no satisfactory explanation has been provided so far. The herewith paper contains the results of bound water researches at various forms (Na, Ca, Al, Fe) of montmorillonite by means of thermal analysis as well as other physico-chemical methods. It has been found that the form of dehydration endoeffects depends on the state of the active centers of the mineral. In certain conditions, by means of thermal analysis one can determine corresponding quantities of bound water that are in agreement with various kinds of active centers of the mineral sorbent.This revised version was published online in November 2005 with corrections to the Cover Date.