南海高钙沉积物中18种常微量元素的ICP-AES测定方法研究

在利用ICP-AES分析南海高钙沉积物中的常微量元素时,钙、镁常常干扰其它元素测试。通过采用优化仪器工作参数、扣除背景值、谱线干扰校正和基体匹配的步骤,消除了元素干扰和钙、镁基体效应,提高了方法的灵敏度和准确度。通过对南海沉积物样品的大量实验和国家一级标准样验证,建立了适宜高钙海洋沉积物元素含量的ICP-AES测试方法。该方法检出限为1.55~271μg/L,相对标准偏差RSD<4.54%(n=6)。     

大洋锰结核调查船上金属品位速测方法的研究——Ⅱ.镍、钴的示波极谱测定法

通过对一些底液作比较和选择,建立了一个新的用示波极谱分析测定镍和钴的方法。此法已用于锰结核调查。基体元素锰、铁对测定无干扰,现场取得的结果是满意的。与ICP-AES及AAS法测得的结果比较,本法准确、简易、快速。     

东太平洋多金属结核中稀土元素的测试及其地球化学特征

本文研究了大洋多金属结核中稀土元素的测试方法.多金属结核这种特殊地质样品,含铁、锰一般在20%～40%左右,而铁、锰属富线光谱元素,对稀土元素谱线均有干扰.本文根据样品特性,仅取250mg多金属结核样品,碱熔后,通过小型阳离子树脂交换柱,采用不同类型酸和不同酸度,洗脱交换柱上的杂质和稀土元素,使稀土元素与杂质元素分离.采用此方法测试国家一级多金属结核标准物质GBW07249中的稀土元素,取得了满意结果.同时利用本法测试了东太平洋多金属结核中稀土元素,并对其地球化学特征进行了初步研究.     

石墨炉原子吸收法测定海水中的铜

一、前言 原子吸收分光光度法已发展成为重要的痕量元素分析手段之一。高温石墨炉原子吸收法具有原子化效率高,取样量少,绝对灵敏度高,操作简便等优点,已被广泛应用于环境监测、临床化学、生物样品、超纯金属及海水中痕量元素的测定。由于石墨炉原子吸收的干扰比火焰原子吸收严重,特别是海水样品基体成分复杂,干扰尤为明显。因此,在测定前必     

红树植物红海榄叶化学组成研究

对红树植物红海榄叶的基本化学成分水分,灰分,灰分中酸不溶物,灰分中S(SO42-),粗蛋白,粗脂肪等及氨基酸和微量元素的组成和含量进行了系统的分析测定。其基本化学组成各成分含量分别为:水分(69.18%),灰分(3.04%),灰分中酸不溶物(0.094%),灰分中S(SO42-)(0.052%),粗脂肪(7.75%),粗蛋白(7.14%);测得了红海榄叶中17种氨基酸,其总含量为10.7mg/g,其中人体必须氨基酸有7种,占所含氨基酸总量约26%;采用全谱直读等离子体原子发射光谱仪对红海榄叶进行了31种微量元素的分析测定,测得了其中18种元素的含量,红海榄叶中含有丰富的人体必须的矿物质元素。     

石墨炉原子吸收法直接测定海洋沉积物和悬浮物中的镉、铅、铜

海洋沉积物和悬浮物样品基体组成十分复杂,而待测元素在样品中的含量也相差甚远,这给分析工作带来了一定的困难.石墨炉原子吸收法虽然具有灵敏度高,取样量少等优点,但存在着严重基体干扰[1-2].因此很多作者不得不采用费时的分离手段或标准加入法进行测定.本文应用自制简易石墨平台和基体改进技术以及峰面积测量相结合,直接测定了海洋沉积物和悬浮物中的镉、铅、铜.方法有效地消除了普遍石墨炉原子吸收测定法分析镉、铅时所遇到的基体干扰,使标准加入法曲线与标准工作曲线的斜率比接近1.0.方法简便快速,稳定可靠。     

导数-伏安法同时直接一次连测海水中Zn、Cd、Pb、Cu及Bi

本文提出采用悬汞电极示差脉冲阳极溶出伏安法和导数技术直接同时一次连测海水中Zn、Cd、Pb、Cu及Bi,研究了在本实验条件下Cu是否干扰Zn的测定,本方法的精密度和准确度均好,测定步骤简便快速,只需调海水的pH为2.5,电解富集10分钟就能测定近岸海水中这五种元素的存在含量,五种元素的单份海水测定约需25分钟。     

氢化法—原子吸收测定海洋沉积物和悬浮物中痕量砷

本文介绍了硼氢化钾还原氢化法—原子吸收快速测定海洋沉积物和悬浮物中痕量砷的方法。经试验比较,选择硝酸—硫酸消化样品,砷(Ⅴ)经0.7％硫脲和0.35％抗坏血酸预先还原为砷(Ⅲ),样品中共存元素对测定无干扰。本法简便、快速、灵敏。     

海洋沉积物中Cu、Zn、Pb、Ba的能量色散X射线荧光光谱测定

能量色散X射线荧光光谱仪是一种较为先进的化学分析仪器。我们应用此仪器,采用谱线背景作内标的方法对海洋沉积物中的Cu、Zn、Pb、Ba元素进行了测定,结果比较令人满意。本方法的准确度要优于重量法、比色法,与原子吸收法相比,本法不需要经过萃取分离处理样品,方法简便、快速。因此,本方法适用于大批量样品和多元素的快速测量。     

海洋沉积物中硒的分析方法研究

建立了海洋沉积物中硒的测定方法。样品用混合酸分解，加入Fe^3 消除干扰，用氢化物原子荧光法测海洋沉积物中的硒，选择了仪器的最佳工艺条件，探讨了共存元素的干扰情况及其消除方法，方法简便，快速，有较好的精确度与准确度，对多种地质标准物质中的硒进行了测定，结果与推荐值十分接近，对海底沉积物标准物质（GBW07314）进行了11次测定，相对标准偏差为6．13％。     

ICP-AES光谱法测定南沙海域沉积物中的少量和微量元素

本文用ICP-AES法对南沙海域沉积物中的Cu,Sr,Ba,Co,Ni,V,Sc,Mo,Mn,Ti,Ga,Cr的测定作了探讨。测量了检测限和背景当量浓度,拟订了较有效的分析方法。     

Interactions among metals in the spectrochemical determination of trace amounts of cadmium in marine mussels

The determination of trace amounts of inorganic elements by electrothermal atomic absorption spectrophotometry (ETA-AAS) or inductively coupled plasma atomic emission spectrometry (ICP-AES) suffers from some kinds of interference due to the inorganic fraction of the matrix of many environmental samples. The ratio between a major matrix element and the analyzed trace element plays an important role in the spectrochemical behaviour of the latter. The resulting enhancing or depressing effect also gives rise to severe faults when the well known standard addition method (SAM) is used. The present work shows the interactions due to the presence of elements such as calcium, sodium, potassium, magnesium and iron during the spectrochemical determinations of trace amounts of cadmium in marine mussels. A possible liquid anion exchange extraction is suggested for the analysis of cadmium by ETA-AAS.     

高压密闭消解-电感耦合等离子体光谱和质谱联合测定海洋地质样品中52种元素

An improved analytical method to determine the content of 52 major, minor and trace elements in marine geological samples, using a HF-HCl-HNO_3 acid system with a high-pressure closed digestion method(HPCD), is studied by an inductively coupled plasma optical emission spectrometry(ICP-OES) and an inductively coupled plasma mass spectrometry(ICP-MS). The operating parameters of the instruments are optimized, and the optimal analytical parameters are determined. The influences of optical spectrum and mass spectrum interferences, digestion methods and acid systems on the analytical results are investigated. The optimal spectral lines and isotopes are chosen, and internal standard element of rhodium is selected to compensate for matrix effects and analytical signals drifting. Compared with the methods of an electric heating plate digestion and a microwave digestion, a high-pressure closed digestion method is optimized with less acid, complete digestion,less damage for digestion process. The marine geological samples are dissolved completely by a HF-HCl-HNO_3 system, the relative error(RE) for the analytical results are all less than 6.0%. The method detection limits are 2–40μg/g by the ICP-OES, and 6–80 ng/g by ICP-MS. The methods are used to determine the marine sediment reference materials(GBW07309, GBW07311, GBW07313), rock reference materials(GBW07103, GBW07104,GBW07105), and cobalt-rich crust reference materials(GBW07337, GBW07338, GBW07339), the obtained analytical results are in agreement with the certified values, and both of the relative standard deviation(RSD) and the relative error(RE) are less than 6.0%. The analytical method meets the requirements for determining 52 elements contents of bulk marine geological samples.     

电感耦合等离子体发射光谱法(ICP-OES)测定海洋浮游生物中总磷的方法优化

磷作为海洋浮游生物生长必需营养元素之一,其准确测定对海洋生态系统元素循环过程的研究具有重要意义。目前,文献中对于海洋浮游生物中总磷的测定方法报道不多。由于海洋浮游生物生存的高盐海洋环境,高盐基体的存在导致常规检测方法不能准确测定磷的含量。为剔除高盐基体效应及干扰,本文运用微波密闭消解预处理样品,采用电感耦合等离子体发射光谱法(ICP-OES)联合标准加入法建立工作曲线,同时结合样品的特异性,对ICP-OES分析谱线、射频功率、雾化气流速、观测高度、蠕动泵泵速和观测方式等仪器参数进行优化,构建确定了准确测定海洋浮游生物中总磷的优化条件和技术流程。实验结果显示, ICP-OES最佳工作条件为分析谱线P213.617 nm,射频功率1 300 W,雾化气流量0.8 L/min,观测高度14mm,进样泵速1.5 m L/min,观测方式轴向。标准加入法标准曲线相关系数大于0.999,相对标准偏差为1.36%~1.67%,加标回收率为92.6%~94.3%,方法检出限为0.010 mg/L,检测结果具有较高的准确度和精密度,可为海洋浮游生物及其它高基体生物样品中磷含量的准确测定提供技术支持。     

The solubility of coal fly ash and marine aerosols in seawater

The elemental solubilities of three coal fly ash samples and two coastal marine-aerosol samples in seawater are different. The coal fly ash samples were collected from the electrostatic precipitators on coal-fired power plants. The air particulates were collected by a high-volume air sampler located near the Washington coast. Samples were neutron-activated then contacted with seawater for several hours. The elements that were partially solubilized from both fly ash and aerosols included As, Sb, Se, Br and Cr. Zinc and Co were more soluble in aerosols then fly ash.     

基于PXRF的西南印度洋脊硫化物表层沉积物地球化学找矿研究

海底热液喷发形成的热液羽状流中富含成矿物质,并沉淀在距离热液喷口不等的范围内。对西南印度洋中脊热液喷口附近、距离喷口中等距离、远离喷口的六个表层沉积物样品开展了不同粒度沉积物的便携式XRF（PXRF）分析。结果表明,PXRF可以有效获得的洋中脊钙质沉积物中成矿元素的富集特征。>40目的沉积物样品具有较高的Cu、Zn、Fe、Mn等元素含量,40目以下沉积物中则相对稳定,可能与粗粒沉积物中玄武岩碎屑/玻璃含量较高有关,与镜下鉴定结果一致。以热液喷口为中心,表层沉积物中表现出Cu、Zn、As、Fe、Mn的元素分带,靠近喷口的沉积物中具有较高的成矿元素的含量,并具有较高的Cu/Fe、Zn/Fe比值或者Cu/Mn与Zn/Mn比值。上述结论表明,洋中脊沉积物中成矿元素的含量主要受与喷口的距离的影响,而与粒度的关系不大,洋中脊沉积物地球化学找矿应采用40目以下粒径沉积物作为分析样品。通过PXRF获得的Cu、Zn、As、Fe、Mn等元素含量及其比值特征可以作为海底多金属硫化物沉积物地球化学找矿的指标,该方法满足快速有效识别洋中脊沉积物中地球化学异常的要求。     

Optimization of the direct simultaneous atomic absorption determinations of several elements in marine or riverine particulate matter

A highly sensitive procedure is proposed for direct simultaneous atomic absorption determinations of three elements (Ag, Cd, and Pb or Cd, Pb, and Tl) in marine and riverine particulate matter. To decrease the influence of nonselective interference and matrix effects and to improve the detection limits of the elements, the course of the analysis included a preliminary stage of fractional evaporation of the sample (a graphite rod with a diaphragm as the evaporator) and condensation of the elements (a graphite rod as the collector). The condensate atomization proceeded in a rod-cell electrothermal graphite atomizer with independent heating of the zones of evaporation and atomization.     

海南岛南岸三亚湾海水Sr/Ca、Mg/Ca变化及对珊瑚微量元素温度计的响应

本文对海南岛南岸三亚湾2008~2009年海水的周间隔取样,用全谱直读等离子体原子发射光谱(ICP-AES)分析方法对其Sr/Ca、Mg/Ca比值进行了测定。结果显示其比值（Sr/Ca=8.558~9.227mmol/mol,Mg/Ca=4.924~5.403 mol/mol）与全球各大洋和主要珊瑚礁区有明显地高异常偏差,而且在春末夏初和秋末冬初两个过渡期,三亚湾海水Sr/Ca比值波动幅度比Mg/Ca相对较大,且体现了一定的差异性。在此基础上,结合海水的Sr/Ca、Mg/Ca比值在时间和地域空间上的变化对珊瑚温度计标定的影响,及对不同站点建立的珊瑚Sr/Ca温度计进行了重新校正,并与分配系数法对比分析,我们认为利用珊瑚的Sr/Ca、Mg/Ca比值重建古SST记录时必须综合考虑包括海水微量元素比值变化在内的各种影响因素对温度计标定的干扰。     

Comparative studies on analytical methods for the assessment of petroleum contamination in the marine environment II. Gas chromatographic analyses

Although determinations of hydrocarbons in the marine environment are usually based on the same analytical steps, i.e. organic solvent extraction, column chromatographic purification, and hydrocarbon detection and identification; variations in equipment and solvent systems used in the extraction step, and also in the columns for purification and analysis, seriously impaired the development of a consistent data base concerning oil pollution on a global scale.Many authors and conferences emphasized the need, in this field, for a comparative study on the efficiency of various published analytical techniques.Fifteen techniques with 24 applications were chosen and applied to a fixed weight of uniform samples of sediments, mussels, fish, shrimps and green algae. The final hydrocarbon extracts were analyzed individually on a 2 m stainless-steel packed column (SE 30).The results obtained from this work showed considerable variations in the efficiency of different techniques from identical samples. The hydrocarbon yields varied from 94 to 1.4 ppm in sediments, from 40 to 9 ppm in mussels; from 216 to 1.3 ppm in fish; from 8.3 to 3.1 ppm in shrimps; and from 343 to 273 ppm in algae, all relative to wet weight of the samples. The gas chromatograms of the hydrocarbons obtained were found to be quite different with regard to peak intensities and distributions. This means that hydrocarbons obtained by the application of different techniques varied in their compositions and relative concentrations of their constituents. These results confirm what was already obtained and discussed previously using spectrofluorometric analyses.It can be concluded that it is necessary to establish a standard technique for the preparation of marine samples, for extraction and purification of the hydrocarbon extracts which should be applied by all laboratories specializing in this field.