全自动消解-石墨炉原子吸收法测定土壤中镉的探讨

探讨全自动消解-石墨炉原子吸收法测定土壤中镉的方法。选用硝酸-氢氟酸-高氯酸作为消解体系,采用全自动消解仪对土壤样品进行消解,通过研究干燥、灰化和原子化温度对吸光度的影响,优化出最佳的石墨炉升温程序,依据国标方法 (GB/T17141-1997)石墨炉原子吸收分光光度法测定土壤样品中的镉元素含量。该方法检测土壤国家标准物质GSS-8、 GSS-22、GSS-24等,所得结果与标准值相吻合。方法简便、快速、重现性好、灵敏度高,适用于批量土壤样品中Cd的测定。     

密闭微波消解电感耦合等离子体发射光谱(ICP-AES)法同时测定大气颗粒物PM10中的18种无机元素

建立了测定大气颗粒物PM10中18种无机元素的密闭微波消解电感耦合等离子体发射光谱法。考察了微波消解体系和消解条件,选取了适宜的仪器工作条件和最佳的分析谱线,合理地进行了背景扣除,并对共存元素的干扰情况进行了研究。样品采用硝酸-盐酸-过氧化氢-氢氟酸体系进行消解并经饱和硼酸溶液络合后上机测定,测定值与参考样品标准值相符,主量元素的方法精密度(RSD%)小于3%,次量、微量元素的方法精密度小于10%。各元素的检出限在0.0001~0.0141mg/L之间,回收率在90%~110%之间,应用建立的方法对北京市的颗粒物膜样品进行了分析。     

《干旱环境监测》2006年第20卷总目次

监测方法研究4,5-二甲基-2-噻唑偶氮重氮氨基偶氮苯固相萃取光度法测定环境样品中锌的研究………………………………………………………………微波萃取—高效液相色谱(HPLC)法测定土壤中16种多环芳烃的研………………究杨杰(1 5)石墨炉原子吸收光谱法测定水中微量…………………钡梁延鹏刘辉利朱义年卢洁(2 65)微波消解ICP—AES法测定土壤及底泥等中常量及微量元素陈素兰胡冠九陈波王霞(2 69)……………………………………………………………………………………………………分光光度法测定环境水样中铂的研究谢琦莹王宇韦群艳杨项军黄章…     

微波消解-ICP-MS测定土壤和底泥中的12种金属元素

以20.0μg/L铟作内标,采用硝酸-氢氟酸-过氧化氢体系微波消解,ICP-MS(电感耦合等离子体质谱法)同时测定土壤和底泥中的12种金属元素,各元素方法检出限为0.003～0.2μg/g,相对标准偏差小于6.1%,土壤标准样品的测定值与标准值吻合。方法简便快捷,灵敏度高,重现性好,是分析大批量土壤和底泥样品中多元素的可靠、高效方法。     

微波消解-ICP法测定土壤中重金属元素的不确定度评定

对微波消解-电感耦合等离子发射光谱法测定土壤样品中Cu、Pb、Zn、Cr、Ni的不确定度进行评估,在测定过程中,对样品称量、消解、定容体积、标准溶液的配制、曲线拟合、仪器测量重复性等影响不确定度的分量进行分析,按《测量不确定度评定与表示》(JJF 1059—1999)的规定进行合成,最终给出扩展不确定度,为电感耦合等离子发射光谱法测量土壤中重金属元素的实验室质量控制和不确定度评定提供参考依据。     

微波消解-火焰原子吸收光谱法测定土壤中的锶

建立了微波消解-火焰原子吸收光谱法测定土壤中锶的方法.用微波消解土壤、电热板加热赶酸的方法对土壤样品进行前处理,优化了微波消解条件.检出限为3.0 mg/kg,加标回收率为84.7％ ～ 107％,相对标准偏差均小于5％.方法快速、简便、准确度高、线性范围宽.     

微波消解和ASD消解ICP-MS测定土壤中重金属元素的比较

采用微波消解和ASD消解2种消解方式对不同土壤样品进行消解,ICP-MS测定其中重金属含量。微波和ASD2种消解方式均能够较好地提取土壤中的Cr、Co、Ni、Mn和V元素,实验结果的相对误差和相对标准偏差均≤10%,符合实验分析的要求。微波消解精密度优于ASD,可作为优先选择的前处理方法。     

微波消解-石墨炉原子吸收法测定土壤中铊

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。     

土壤重金属含量测定不同消解方法比较研究

消解是影响土壤重金属测定结果准确性的关键步骤.比较电热板消解、微波消解和全自动石墨消解3种消解方法的操作流程,同时对不同类型土壤样品中Cu、Zn、Pb、Cd、Cr、Ni 6种元素含量进行对比测定,结果表明,电热板消解设备简单,但步骤繁锁,操作不当易造成组分损失；微波消解速度快,测定结果精密性和准确性较好,但仍需人工赶酸程序且罐位少,不适合大批量样品分析；全自动石墨消解不仅测定结果精密性和准确性较好,而且自动化程度高,可实现无人值守,大大节省人力,尤其适合大批量样品的分析.     

自动石墨消解-石墨炉原子吸收法测定土壤中铅和镉

本文建立了一种自动石墨消解仪消解土壤样品,石墨炉原子吸收法测定土壤中的铅、镉的方法。铅、镉元素在标准曲线范围内线性良好,相关系数均大于0.999,检测限分别为0.02、0.007 mg/kg,加标回收率在90.8%~104.0%,方法重复性RSD(n=7)低于3%。实验结果表明,该方法操作简单、准确度高、精密度好、检测限低,可用于大批量土壤中铅、镉的测定。     

Ko method of quantification in neutron activation analysis as applied to environmental samples

The _Ko factor method in neutron activation analysis adopts all the principles of comparator method and can be used for the rapid determination of elemental comcentrations during routine monitoring of environmental samples. The method necessiates the use of same in-pile conditions, such as irradiation time, irradiation position and the type of neutron spectrum, for which the factors have been generated. The _{K_o} factors were estimated for various elements of environmental importance for three irradiation positions of Apsara Reactor at Bhabha Atomic Research Centre. Standard reference materials of soil and coal were used for all the elements except for Hg for which HgCl₂ was used. The concentration of the elements determined using these factors in a flyash standard reference material revealed good agreement within 10% of the certified values. The efficacy of the method compared well with that of specific element comparator method as revealed by the elemental concentrations obtained by both the techniques.     

波长色散-X射线荧光光谱法测定PM2.5中23种元素

研究以单元素标准膜为基础，结合NIST SRM 2783颗粒物滤膜标准样品，建立了波长色散-X射线荧光光谱法测定PM_2.5中23种无机元素的测定方法，优化了测试条件，测量一个样品耗时约15 min，计算了各元素的方法检出限。对NIST SRM 2783滤膜标准品在一周内重复测定10次来计算方法的准确度与精密度，测定结果显示大多数元素的测量值在给出的参考值范围内，且测量标准偏差一般在10%以内。对比了石英与聚四氟乙烯材质（Teflon）滤膜的空白值，石英滤膜中Si、Fe、Na、Mg、Al、K、Ca等元素的背景值较高，Teflon滤膜的背景值较低，推荐选用Teflon滤膜作为PM_2.5组分分析采样滤膜。分别用波长色散-X射线荧光光谱法及酸消解-ICP-MS法测定了样品膜中的元素组分，得到的测定结果基本一致。     

Spatial variation of salts in a Gyanpur canal command area

This study was aimed to establish background and reference values of total heavy metals in soils from a representative area of Albania (Tirana). Thirty-eight soil samples collected from genetic horizons of major soil types of Tirana were analyzed for important physicochemical properties by standard methods and for total contents of Cd, Cr, Ni, Pb, Zn, and Cu by atomic absorption spectrometer, after extraction with aqua regia. The results showed that the total contents of Cd, Cr, Ni, Pb, Zn, and Cu in surface horizons varied widely with respective mean values of 0.3 (??0.6), 174.2 (??63.7), 305.9 (??133.0), 19.7 (??12.4), 95.5 (??26.3), and 42.7 (??6.8) mg/kg. The highest metal contents were found in two soils developed in limestone. The depth distribution of metals showed a tendency for accumulation of Cd and Pb in the surface horizons of three soils, suggesting that these metals partially come from anthropogenic inputs. Correlation analysis indicated that the metal contents of soils were controlled by soil properties, including pH, CaCO₃, clay, organic matter, cation exchange capacity, and Fe oxides. The background values (given as the 90th percentile) were much higher than those reported in the literature, showing that the levels of respective metals were naturally higher. The total metal contents of some soils were above background levels, suggesting metal pollution. The reference values for all the analyzed metals were quite consistent with those of the Dutch system. The proposed background and reference values can be used to evaluate the soil pollution with these elements.     

气相色谱-串联质谱法测定土壤中十氯酮

研究了提取溶剂效率、净化方式等因素对十氯酮测定的影响,对比了加速溶剂提取、微波萃取及超声波等提取方式,考察了不同电子轰击能量、碰撞能量下特征离子对的响应。建立了加速溶剂萃取,H2SO4净化分离,气相色谱法-三重四极杆质谱法测定土壤中十氯酮的分析方法。取5.0 g土壤干样,内标法定量,线性相关系数为0.999 7,加标回收率为91.7%~121%,相对标准偏差为3.4%(n=6),检出限为0.1 ng/kg。     

两种消解法测定沉积物总磷的对比

通过过硫酸钾消解法与HClO₄-H₂SO₄消解法对土壤和水系沉积物的标准物质,以及三峡水库沉积物未知样品中的总磷含量进行测定,并对检测结果进行对比,分析过硫酸钾消解法测定沉积物总磷的可行性。结果表明,在标准样品中,HClO₄-H₂SO₄消解法的检测结果是标准值的83%~100%,并且所有结果均在其不确定度范围之内;过硫酸钾消解法的检测结果仅达到标准值的19%~42%,超出其不确定度范围,不能作为有效数据。在未知样品中,过硫酸钾消解法检测结果也远低于HClO₄-H₂SO₄消解法检测结果,只达到后者的32%~52%。由此可见,过硫酸钾消解法测定沉积物或土壤中总磷,仍需要进一步的研究,以达到符合实际的检测结果。     

Assessment of trace elements in animal tissues from Turkey

In this study, trace element contents of animal tissues were determined by atomic absorption spectrometry after microwave digestion method. The accuracy of the method was confirmed by analysis of standard reference material (NIST SRM 1577b Bovine Liver). Trace element contents in animal tissue samples were found in the range of 98.3-18.2 μg/g (Fe), 2.89-0.26 μg/g (Mn), 23.9-4.54 μg/g (Zn), 0.08-0.01 μg/g (Pb), 32.9-1.66 μg/g (Cu), and 0.32-0.01 μg/g (Cd). The results were compared with literature values. The results obtained for toxic and trace elements in analyzed animal tissue samples were acceptable to human consumption at nutritional and toxic levels.     

液液萃取-气相色谱法测定水质可萃取性石油烃C10~C40

建立了以环己烷为萃取剂、气相色谱法(氢火焰离子化检测器,FID)测定水质样品中可萃取性石油烃(C_(10)～C_(40))的分析方法。以正构烷烃混合标准溶液为定性和定量校准标准,以色谱峰面积总和与混合标准溶液总浓度建立校准曲线进行外标法定量。方法检出限为0.01 mg/L,经验证方法精密度和准确度良好。同时,分别以气相色谱法和红外光度法测定了地表水、污水处理厂出水、海水和化工废水等实际样品,对比实验结果表明,在可萃取性石油烃C_(10)～C_(40)的碳数范围内,气相色谱法的测试结果与红外光度法无明显差异,有较好的可比性。     

Fractions and background concentrations of potentially toxic elements in Hungarian surface soils

This work established background concentrations for the pseudo total (HNO₃ + H₂O₂-soluble), mobilisable (NH₄-acetate + EDTA-soluble) and mobile (1?M NH₄NO₃-soluble) element fractions of Hungarian surface soils that can be used as reference values for the soil quality standards. The 193 soils investigated were taken from the Hungarian Soil Information and Monitoring System. The background values for Al, As, B, Cd, Co, Cr, Cu, Mn, Ni, Pb, Sr and Zn were given as a range covering 95% of the variance of the representative samples. The differences between observed element concentrations and the calculated background values indicated anthropogenic or pedogenic impact in each fraction. The comparison of the calculated background values with the Hungarian quality standards and the contamination limit values of other countries showed that the limit values of a certain region or country are not suitable for other areas. Generally, Mn and Al had the highest, while Cd had the lowest concentration in each fraction. Cr and Al were the least and Sr was the most mobile element. The principal component analysis indicated different geochemical and physico-chemical behaviour of the elements in the fractions; the pseudo total fraction was influenced more by the geological behaviour, while mobilisable and mobile fraction explained a much higher proportion of the total variance of soil physico-chemical properties than soil geochemical properties. The Cd–Ni and Co–Mn element pairs were always in the same principal component in each fractions indicating similar geogenic origin and showing that their solubility changes are similar in function of soil properties.     

Determination of total and partially extractable solid-bound element concentrations using collision/reaction cell inductively coupled plasma-mass spectrometry and their significance in environmental studies

Determination of solid-bound element concentrations is an important initial step in environmental studies especially for assessment of contamination level, and of origin, relative mobility, and fate of contaminants. This study revealed that a relatively new collision/reaction cell inductively coupled plasma-mass spectrometry is a potent tool for determining total and partially extractable solid-bound element (V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, and Pb) concentrations in a complex matrix solution containing HF and/or HCl. Six different extraction methods commonly used for environmental monitoring studies were tested for their bias and variability using estuarine and marine standard reference materials. Microwave-assisted methods based on concentrated [HNO₃] or [HNO₃?+?HF (4:1)] and [HNO₃?+?HF?+?HCl (10:3:2)] were applied for determining pseudo-total and total element concentrations, respectively. Dilute-acids (1 M HNO₃, 1 M HCl, and 0.5 M HCl) were utilized in single-step partial extraction protocols. Except the 0.5 M HCl cold-extraction method which was performed at room temperature, other partial extraction protocols used microwave-digestion. This study demonstrated that the use of microwave-assisted methods in studies aimed at determining the non-residual, non-specific extractable fractions of elements in solid environmental samples may result in overestimation, and thus needs to be re-examined. We believe that the cold extraction method will play a significant role in future environmental monitoring studies. Nevertheless, results of the cold extraction method not accompanied with total element concentrations have limited value, as the amount of extraction may vary significantly with the nature (origin) of the elements, and with the types of the samples. Therefore, we suggest combining microwave-assisted total digestion and 0.5 M HCl cold-extraction methods as a relatively cost- and time-effective, environmentally sound screening procedure for routine environmental monitoring programs involving a large number of samples from diverse geological and anthropogenic settings.