微波消解原子吸收光谱法测定土壤中铅镉铬铜

采用微波消解进行样品前处理,原子吸收光谱法测定土壤中铅、镉、铬、铜,对样品前处理、基体改进剂等一些影响因素进行了探讨。利用该方法对土壤样品进行了测定,回收率为91%～114%,相对标准偏差为2.8%～7.4%,并利用国家标准物质验证了方法的准确度。该方法快速、准确,能够满足土壤中铅、镉、铬、铜的分析要求。     

微波消解-ICAP法测定土壤中总铬含量的研究

采用微波消解仪对土壤样品进行前处理,用ICAP测定土壤中总铬含量。通过硝酸-氢氟酸以及硝酸-盐酸-过氧化氢体系消解液对土壤样品消解,优化试验选择出微波最佳消解条件和ICAP的工作参数。结果表明,发现用硝酸-氢氟酸体系消解液,在谱线283.56 nm、267.72 nm处用ICAP能够准确而稳定地测得土壤中总铬含量。     

普通消解与微波消解分析植物样品中Al等元素的方法比较

采集红壤地区植物样品65个,普通消解和微波消解后用ICP测定A l等6种元素含量。对两种消解结果进行线性回归分析发现,Al、Ca、Fe、Mg、Mn、P的回归系数分别为1.0014、1.0056、1.0725、1.0831、1.0039、0.9915;相关系数分别为0.9988、0.9834、0.9891、0.9970、0.9941、0.9945。两种消解方法对A l的消解具有很强的可比性。微波消解法具有能耗少、试剂利用率高、运行条件一致、样品损失少等优点。     

微波消解-原子吸收法测定土壤中的铜铬锌铅镉

采用专门的speedwaveMWS-3微波消解仪对土壤进行前处理,用AAS对其中的重金属元素进行连续测定,通过不同的酸类型和采取不一样的时间-温度曲线的对比研究,通过优化试验得出该方法的最佳前处理条件。结果表明,加入HNO3-HF和前两步采用T=150℃、ta=3min、t=5min,T=180℃、ta=3min、t=10min的时间-温度曲线能够使测定结果准确而稳定。使用该方法测量土壤标样,标准偏差、变异系数均达到质控要求。     

微波消解法快速测定土壤中有机质的含量

报道了用微波消解取代油浴消解或灼烧法来测定土壤中有机质的含量,详细讨论了微波消解法的有关测定条件.该法和传统的重铬酸钾油浴法相比,具有快速、经济、重复性好等优点,值得在相关行业中推广应用.     

微波消解-电感耦合等离子体发射光谱法测定土壤有效硼

探究用微波消解进行前处理与电感耦合等离子体发射光谱仪(ICP-OES)检测相结合的方法,通过实验对消解时间、消解温度、升温时间及测定过程中铁共存干扰元素、土壤的pH进行了研究。在ICP-OES光谱仪的最优工作条件下,谱线249.773 nm的硼灵敏度高、峰形好,测定结果表明,当样重为10.00 g,浸提液体积为20 mL时,方法检出限为0.005 mg/kg,测定下限为0.020 mg/kg,精密度和准确度满足检测要求,此法适用于批量土壤有效硼的测定。     

火焰原子吸收分光光度法测定污染土壤中5种重金属

采用微波消解法预处理待测土壤,火焰原子吸收分光光度法测定污染土壤消解液中的锌、铜、铅、镉、铬5种重金属.方法简便、灵敏、准确,土壤中锌的相对标准偏差为1.2%;铜的相对标准偏差为1.9%;铅的相对标准偏差为1.2%;镉的相对标准偏差为5.2%;铬的相对标准偏差为1.8%.方法的加标回收率锌为76.8%～104%;铜为86.9%～95.3%;铅为83.0%～94.4%;镉为83.2%～91.9%;铬为90.9%～96.1%,适用于污染土壤中重金属含量的测定.     

微波消解—ICP-MS法测定有机肥料中8种元素

采用电感耦合等离子体质谱法(ICP-MS)测定,来比较不同混合酸体系对有机肥料中As、Pb、Cd、Cr、Hg、Ni、Cu、Zn 8种元素的提取效果,建立了微波消解—ICP-MS测定有机肥料多元素含量的方法。研究结果表明,8种元素在0.10～1600 μg/L质量范围内线性关系良好,线性相关系数为0.99970～0.99995,检出限范围为0.003～0.400 μg/L。三水平加标回收率范围为81.8%～108.0%,相对标准偏差为0.9%～4.9%(n=6)。国家标准物质灌木枝叶GBW07603(GSV-2)除汞元素缺少相应的认定值以外,其余7种元素的测定值均在标准物质证书认定值的范围内,且相对标准偏差为0.5%～5.0%(n=6)。该方法灵敏度、准确度高,可实现有机肥料中多元素的通量检测。     

土壤中重金属的生物有效性研究进展

综述了年十年来国内及国际上研究土壤中重金属的生物有效性的态势，尤其是影响土壤中重金属生物有效性的诸多因素，以期进一步推动国内的土壤中重金属生物有效的研究工作和重金属污染土壤的生物治理工作。     

土壤样品的王水回流消解重金属测定方法的研究

通过对土壤标样多次重复王水回流消解实验的研究,分别给出了原子吸收和ICP-MS2种仪器分析测定土壤中6种重金属元素的消解方法。分析结果显示,2种消解方法都可以将标准样品中的Cd、Cu、Zn、Ni、Pb、Cr元素定量回收,方法误差在10%以内,Pb、Cr的方法误差则在16%～35%,所有实验结果的RSD<10%,符合痕量分析的要求。     

乳化剂OP增敏——火焰原子吸收光谱法连续测定土壤中有效铜、锌

研究了用非离子表面活性剂乳化剂OP为增敏剂,火焰原子吸收光谱法测定土壤有效铜、锌的方法。试验结果表明,加入乳化剂OP可使铜吸光度增加70%,锌吸光度增加25%,提高了分析的灵敏度。方法操作简便、快速,相对标准偏差小于8.12%,加标回收率为95.2%~102.5%。     

Determination of Available Cadmium and Lead in Soil by Flame Atomic Absorption Spectrometry after Cloud Point Extraction

A cloud point extraction (CPE) procedure has been developed for the determination of available cadmium (Cd) and lead (Pb) in soil by flame atomic absorption spectrometry. The proposed method was based on the CPE of a complex from ammonium pyrrolidine dithiocarbamate (APDC) and metal Cd and Pb using emulsifier octyl polyethylene glycol phenol ether (OP) as surfactant. Conditions that would affect the complex formation and separation were researched in detail, including extraction conditions as well as pH, amount of the chelating agent, concentration of the surfactant, equilibration temperature and time, and salt effect. Under the optimized conditions, both of the calibration graphs were linear in range of 0–1.0 μg mL^?1 with detection limits of 0.29 ng mL^?1 for Cd and 2.10 ng mL^?1 for Pb. The relative standard deviation (RSD) for 11 replicate measurements at 0.10 μg mL^?1 of Cd and Pb were 2.18% and 4.04%, respectively. The enhancement factors were 48.8 and 61.6 for Cd and Pb, respectively. The recoveries of Cd and Pb at the spiking level of 0.10 μg g^?1 in soil samples were from 91.7% to 115% and from 91.0% to 115%, respectively. The proposed method has been applied to the determination of available Cd and Pb in soil.     

原子吸收测定土壤镍的测量不确定度评定研究

本文评定了火焰原子吸收测定土壤中镍含量的测量不确定度。以标准土壤样品(GSW 17401)为测试对象,通过应用火焰原子吸收法测定土壤镍含量,对其测量不确定度的来源、计算和结果表示等问题进行探讨。样品消解前处理产生的不确定度最大,标准曲线拟合测定溶液产生的不确定度其次。在测定中前处理和标准曲线拟合测定溶液应给予足够重视,以减小测量不确定度。     

原子吸收次灵敏线法直接测定土壤中Fe、Mn

用原子吸收次灵敏线法塞曼效应扣除背景测定土壤中Fe、Mn,实验结果表明:此方法有较好的准确度,精密度,操作简单,适合一般土壤中Fe、Mn的测定。     

Determination of Water-Soluble and Acid-Soluble Zinc in Soils by Flame Atomic Absorption Spectrometry after Cloud Point Extraction

A cloud point extraction (CPE) procedure has been developed for the determination of water-soluble and acid-soluble zinc (Zn) in soils by flame atomic absorption spectrometry. Deionized water and 0.1 mol L^–1 hydrochloric acid (HCl) were selected as extracting agents. In the proposed approach, 2-(5-bromo-2-pyridylazo)-5-diethylam-inophenol (5-Br-PADAP) was used as a chelating agent, and polyethylene glycol octyl phenyl ether (OP) was selected as the surfactant. Some factors including the pH of analytical solution, concentrations of the chelating agent and surfactant, equilibration temperature and time, and salt effect, which would affect the extraction efficiency and subsequent determination of Zn, were studied and optimized. Under the optimized conditions, the calibration graph was linear in the range of 5.0?×?10^–3 to 0.5 μg mL^–1, and preconcentration of 20 mL sample solution gave an enhancement factor of 25. The detection limit was 4.93?×?10^–3 μg mL^–1. Recoveries in the range of 95.0–110% were obtained. Some metal ions including iron (Fe²⁺), cobalt (Co²⁺), and manganese (Mn²⁺) would interfere with the determination of Zn. The interference from these ions can be eliminated using thiourea (0.5% w/v) and triethanolamine (0.5% w/v) as masking agents. The proposed method was applied to the determination of water-soluble and acid-soluble Zn in soils, which were collected from the suburbs of Zhengzhou, and satisfactory results were obtained. To have more understanding of the soils, we determined the total content of Zn in soils. The results showed that the water-soluble and acid-soluble Zn contents in different soils are not correlated with the total content. For example, the total content of Zn for the soil from a farm in north loop was very low, but the percentage of water-soluble Zn was very high.     

塞曼石墨炉原子吸收测定蔬菜、水果及制品中铬和钴

本文介绍了用塞曼石墨炉原子吸收测定蔬菜、水果及其制品中Ｃｒ和Ｃｏ的方法。样品经高温灰化，以磷酸二氢铵作基体改良剂，用平台热解涂层石墨管进行样品测定。经１１组白菜参考样测定验证，铬和钴的相对偏差分别为８．４％和９．０％；两组不同浓度的铬和钴的加标回收率分别９３－１０１％和９４－１０５％。铬和钴的检出限分别为０．４１μｇ／１和０．３９μｇ／ｌ。本法也适用于其它生物样品中Ｃｒ和Ｃｏ的测定。     

石墨炉原子吸收光谱法测定土壤铝的条件优化

酸性土壤中的活性Al是影响作物生长发育的主要因子之一,土壤Al的测定一直是人们关注的问题。石墨炉原子吸收光谱法测土壤Al所需的样品量少、灵敏度高、离子干扰小,目前在国内外应用较为广泛。由于其测试条件多是应用单因素轮换法来确定,存在实验量大且未考虑交互作用的影响等缺点。采用双因素重复实验及正交实验可显著降低确定最佳测试条件的工作量,且实验条件代表性强,对于准确快捷测定土壤Al具有重要意义。通过双因素（波长和灯电流）重复试验对石墨炉原子吸收光谱仪测定土壤Al的波长和灯电流进行了优化选择,确定最佳波长为309.3nm,最佳灯电流为14mA;应用L2（556）正交试验法对控温程序及基体改进剂、基体酸度条件进行了优化,得出最佳的灰化温度为1400℃、灰化时间为10s,原子化温度为2300℃、原子化时间为5s,最佳基体改进剂为0.1%NH4H2PO4、最佳基体酸度为0.2%硝酸。优化后的方法检出限为1.14μg.L-1,加标回收率达到93.6%~104.1%,相对偏差均小于8%。     

岷江成都段底泥中重金属的原子吸收多元素同时测定及趋势分析

在单元素原子吸收法的基础上，使用瓦里安SpectrAA220FS原子吸收光谱仪，建立了底泥中部分金属元素的原子吸收多元素同时测定方法。应用本法测定了岷江成都段底泥中的部分金属元素铜、镍、锌、铅、镉的含量，分析了污染物质的分布规律与变化趋势，为水环境研究、保护和管理提供更快捷方便的测试方法。     

Statistical Comparison of Wet and Dry-Ashing Digestion Methods for the Determination of Copper and Iron Species in Orange Peel,Flesh and Tree Leaves by Flame Atomic Absorption Spectroscopy

In this study, two methods of wet digestion and dry-ashing digestion are performed and compared statistically for the determination of iron (Fe) and copper (Cu) species in the orange peel, flesh and leaves by means of flame atomic absorption spectroscopy (AAS). In wet digestion, the effects of two reagents and their mixtures were studied. In dry digestion, various factors affecting the digestion were studied and optimal condition established. Based on the average concentration (mg L^?1), standard deviation (n = 5) and relative standard deviation (RSD)%, the best conditions of dry digestion and wet digestion to extract Fe and Cu were chosen. Finally, some 12 measurements were performed based on the optimum conditions of dry and wet digestions and the best method was selected with regard to the obtained results. In orange tree leaves because t_exp (0.016) is smaller than t_theorical (2.18), it shows that there is no difference between the two methods for analysis of Fe. However, the determination of Cu in orange tree leaves was practical with wet digestion in that t_{exp (57.14)}? t_{theorical (2.18)} shows there is a difference between the two methods and wet digestion is more suitable than dry-ashing due to obtaining less RSD%. In flesh orange, it is seen that for both t_exp ? t_theorical, showing there is a difference between the two methods and wet digestion is more suitable than dry-ashing one. Furthermore, in both Fe and Cu species, the t_exp ? t_theorical, indicating that the two digestion methods are different and wet digestion was selected as a suitable method because of obtaining smaller values of RSD%. Finally, after comparison of the results, the wet digestion vessel for Fe and Cu extraction in the samples was suggested. The developed digestion methods were validated with certified reference materials.