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1.
介绍了国家重大科学仪器设备开发专项"基于质谱技术的全组分痕量重金属分析仪器开发和应用示范"项目在电感耦合等离子体质谱仪(ICP-MS)研发、低温等离子体样品引入ICP-MS联用系统、ICP-MS监测汞的采样与预处理等方面的研究进展,并对ICP-MS应用发展及产业化前景进行了展望。  相似文献   

2.
通过研究土壤消解体系、混合基体改进剂的使用、石墨管类型的选择和标准加入定量过程对测定结果的影响,建立了适用于土壤中重金属铊的微波消解-平台石墨炉原子吸收方法。结果表明,使用HNO_3-HF-H_2O_2消解体系对土壤进行微波消解,石墨炉原子吸收测定过程采用Pd(NO_3)_2/Mg(NO_3)_2混合基体改进剂和平台石墨管,土壤中铊的检出限可达0.05 mg/kg,线性相关系数为0.996,加标回收率在95.0%~105.0%。使用该方法测得的结果与ICP-MS法比较,无统计学差异。改进后的方法具有简单快捷、灵敏度高、重现性好、线性范围广、结果准确等优势,易于推广使用。  相似文献   

3.
较系统地研究了基体改进剂硝酸铵、磷酸二氢铵、硝酸钯等在测定海水中铜、铅、镉、铬的运用,建立了海水中重金属直接测定的方法并讨论了基体改进剂消除干扰的作用机理.方法用于测定北仑港近岸海域海水中的痕量元素,结果令人满意.  相似文献   

4.
多道石墨炉原子光谱法同时测定水中的Cu,Pb,Zn,Cd   总被引:2,自引:2,他引:0  
使用多道石墨炉原子吸仪,采用石墨管涂层处理技术,在对几种基体改进剂的改进作用进行实验比较的基础上,选择1%ZrOCl2为基体改进剂,对水中的Cu,Pb、Zn、Cd4种元素进行了同时测定,并应用此方法对北京化工二厂和京密引水渠的水样进行了加标回收试验,取得了较为满意的结果。  相似文献   

5.
环境中Cd、Pb是危害人体健康的有害元素,人们广泛开展了对铅、镉的分析方法的研究,火焰原子吸收法测定土壤中的Cd、Pb因基体复杂,含量较低,要采用分离富集的技术,来消除干扰,提高方法的灵敏度,但手续繁琐。采用石墨炉原子吸收直接测定,灵敏度高,但也存在基体干扰严重的问题。同时,Cd、Pb在灰化期间易挥发损失,许多文献介绍采用基体改进剂提高灰化温度,以消除基体干扰。本实验对文献所介绍的基体改进剂进行了实验,表明以H_3PO_4为改进剂测定土壤中Cd、Pb抑制干扰的效果明显,并有效地提高了灰化温度。我们采用高压罐消解土壤样品,把H_3PO_4直接注入石墨管以测定Cd、Pb。其方法简便,检  相似文献   

6.
土壤中含Cd量一般在ppb级,需用石墨炉原子吸收法测定。然而由于Cd是易挥发元素,加之 土壤基体成份复杂,灰化温度和原子化温度较难确定。Kaisec等曾用平台技术及磷酸盐基体改进剂测定了环境水和血,肝脏组织及尿中的Cd,对于基体复杂的土壤样品及高氯酸的干扰,据报导利用有机溶剂萃取可消除基体组分和高氯酸对Cd的干扰。我们使用自制的石墨平台,以H_3PO_4作基体改进剂研究了基体及高氯酸对Cd的影响及消除,确定了Cd的灰化温度,原子化温度和测定方法。并用此方法测定了五种标准土样。  相似文献   

7.
石墨炉法测定铅的基体改进剂的选择   总被引:9,自引:0,他引:9  
毛志瑛 《干旱环境监测》2001,15(3):139-141,186
通过一系列实验,选择了石墨炉法测定铅的最佳基体改进剂,并确定了使用该基体改进剂的最佳灰化温度和原子化温度。  相似文献   

8.
尝试了使用5%钼酸铵-5%磷酸二氢铵溶液组成石墨管连续涂覆结合基体改进剂的方法,应用于地表水Pb的测量中。实验表明,本法具有提高石墨管在使用过程中的稳定性,消除基体效应的作用。  相似文献   

9.
石墨炉升温程序的灰化技术   总被引:5,自引:0,他引:5  
本文以测定铅为例,研究了石墨炉升温程序的灰化技术,包括基体干扰的消除,基体改进剂和L’vov平台的应用。  相似文献   

10.
电感耦合等离子体-质谱(ICP-MS)法测定水中镉在环境监测系统得到了广泛应用,本文主要从实验室内部控制和实验室外部控制两个角度来对电感耦合等离子体-质谱(ICP-MS)法测定镉的环境监测质量控制进行分析。  相似文献   

11.
姜娜 《中国环境监测》2014,30(2):118-124
电感耦合等离子体质谱技术(ICP-MS)是目前发展最快的痕量元素分析测试技术之一。由于该技术提供了极低的检出限、极宽的动态线性范围,干扰少、分析精密度高,可进行多元素同时快速分析,可与多种分离技术及样品前处理方法和进样方法相结合等优点,得到了迅速的发展。介绍了ICP-MS的基本原理及仪器构造、与其他分析测试技术的比较及发展趋势,并着重介绍了其在环境监测和环境科学研究领域的应用。  相似文献   

12.
用等离子发射光谱和等离子发射光谱-质谱作比较,等离子发射光谱-质谱用于饮用水As、Sb、Se的测量时需考虑校正系数,通过不确定度分析,确定了ICP-MS测定方法不确定度大小,得出结论:不要氢化物发生器,不加EDTA作为掩蔽剂,也可以直接用于实际.  相似文献   

13.
分别用原子荧光法(AFS)和电感耦合等离子体质谱法(ICP-MS)测定水中锑。AFS法和ICP-MS法均线性良好,相关系数分别为0.999 8和0.999 9,检出限分别为0.17和0.03μg/L,相对标准偏差均1.15%,加标回收率分别为96.6%~111.9%和95.4%~111.5%,2种方法均能很好地用于水中锑的测定。其中,ICP-MS法适合较清洁地表水和地下水样品中锑的分析,AFS法则对地表水、地下水和废水样品均适用。  相似文献   

14.
Mosses are used as biomonitors on a regular basis to study trends in the atmospheric deposition of trace elements in Norway. In this paper the analytical scheme used so far, based on a combination of instrumental neutron activation analysis and atomic absorption spectrometry (INAA/AAS) is compared with inductively coupled plasma emission spectrometry (ICP-ES) and inductively coupled plasma mass spectrometry (ICP-MS). ICP-ES provided satisfactory data for nearly 20 elements, but detection limits were inadequate for some elements of importance. For ICP-MS quantitative data were obtained for 33 elements including the heavy metals of key interest in air pollution studies. In most cases where comparison was possible the ICP-MS data compared favourably with data obtained by the reference scheme or by ICP-ES. On the basis of this study ICP-MS is considered to be an equivalent alternative to INAA/AAS in multielement studies using mosses as biomonitors. In addition ICP-MS offers some promise for the study of elements such as Be, Ga, Mo, Te, Tl, and Bi, for which very little information exists regarding their behaviour as air pollutants.  相似文献   

15.
近年来,环境样品中237Np的准确测量受到越来越多的关注。随着质谱技术的发展,电感耦合等离子体质谱(ICP-MS)成为研究和测量环境样品中237Np的重要手段。文章从样品制备、定量方法、干扰降低、进样系统改进、与色谱联用等方面,对ICP-MS分析环境样品中237Np的研究进展作了评述。  相似文献   

16.
通过测定深圳某河流水样中的主要成分,确定ICP—MS碰撞模式测定se的主要基体干扰,并对碰撞气流量进行条件优化和水样基体干扰消除试验,确定当氦气流量为3.0L/min时,测定77Se的干扰能基本被消除。该方法测定实际水样的结果与原子荧光法的测定值无显著差异。  相似文献   

17.
A continuous-flow system comprising a novel, custom-built extraction module and hyphenated with inductively coupled plasma-mass spectrometric (ICP-MS) detection is proposed for assessing metal mobilities and geochemical associations in soil compartments as based on using the three step BCR (now the Measurements and Testing Programme of the European Commission) sequential extraction scheme. Employing a peristaltic pump as liquid driver, alternate directional flows of the extractants are used to overcome compression of the solid particles within the extraction unit to ensure a steady partitioning flow rate and thus to maintain constant operationally defined extraction conditions. The proposed flow set-up is proven to allow for trouble-free handling of soil samples up to 1 g and flow rates < or =10 mL min(-1). The miniaturized extraction system was coupled to ICP-MS through a flow injection interface in order to discretely introduce appropriate extract volumes to the detector at a given time and with a given dilution factor. The proposed hyphenated method demonstrates excellent performance for on-line monitoring of major and trace elements (Ca, Mn, Fe, Ni, Pb, Zn and Cd) released when applying the various extracting reagents as addressed in the BCR scheme, that is, 0.11 M CH(3)COOH, 0.1 NH(2)OH.HCl and 30% H(2)O(2), even when a well recognized matrix-sensitive detector, such as ICP-MS, is used. As a result of the enhanced temporal resolution of the ongoing extraction, insights into the breaking down of phases and into the kinetics of the metal release are obtained. With the simultaneous multielement detection capability of ICP-MS, the dynamic fractionation system presents itself as an efficient front-end for evaluation of actual elemental association by interelement comparison of metals leached concurrently during the extraction time. Thus, the intimate elemental association between Cd and Zn in contaminated soils could be assessed.  相似文献   

18.
Inductively coupled plasma mass spectrometry (ICP-MS) is becoming more widely used for trace elemental analysis in the occupational hygiene field, and consequently new ICP-MS international standard procedures have been promulgated by ASTM International and ISO. However, there is a dearth of interlaboratory performance data for this analytical methodology. In an effort to fill this data void, an interlaboratory evaluation of ICP-MS for determining trace elements in workplace air samples was conducted, towards fulfillment of method validation requirements for international voluntary consensus standard test methods. The study was performed in accordance with applicable statistical procedures for investigating interlaboratory precision. The evaluation was carried out using certified 37-mm diameter mixed-cellulose ester (MCE) filters that were fortified with 21 elements of concern in occupational hygiene. Elements were spiked at levels ranging from 0.025 to 10 μg filter(-1), with three different filter loadings denoted "Low", "Medium" and "High". Participating laboratories were recruited from a pool of over fifty invitees; ultimately twenty laboratories from Europe, North America and Asia submitted results. Triplicates of each certified filter with elemental contents at three different levels, plus media blanks spiked with reagent, were conveyed to each volunteer laboratory. Each participant was also provided a copy of the test method which each participant was asked to follow; spiking levels were unknown to the participants. The laboratories were requested to prepare the filters by one of three sample preparation procedures, i.e., hotplate digestion, microwave digestion or hot block extraction, which were described in the test method. Participants were then asked to analyze aliquots of the prepared samples by ICP-MS, and to report their data in units of μg filter(-1). Most interlaboratory precision estimates were acceptable for medium- and high-level spikes (RSD <25%), but generally yielded greater uncertainties than were anticipated at the outset of the study.  相似文献   

19.
Former battery factories have created environmental and health problems for years and the exposure to lead in surface soils has been underestimated. Nonetheless, the identification of lead contamination and its spatial distribution is crucial. The determination of heavy metals in soils can be performed using inductively coupled plasma mass spectrometry (ICP-MS). However, alternative techniques such as X-ray fluorescence (XRF) have been used lately in environmental studies since measurements can be taken in the field in a prompt manner, despite its lower accuracy. In this study, a former battery factory site in Monterrey, Mexico, has been studied in order to detect lead contamination. Soil samples were assessed for contamination by using an analytical hybrid method that comprises both analytical techniques, namely, ICP-MS and XRF. Samples were taken in 215 locations and, after a simple homogenization process, they were analyzed by using a portable XRF device. Within those 215 sampling points, 25 samples were analyzed concurrently by using ICP-MS according to international sampling guidelines. Results obtained were adjusted in order to define an analytical hybrid method, which encompasses the advantages of each technique. An improved characterization was achieved by using the proposed analytical hybrid method since maps of lead distribution and calculated areas of concern showed better predictability. The combination of spectroscopic techniques is of great applicability for environmental agencies and decision makers.  相似文献   

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