Automated indirect fluoride determination by ICP-OES using discontinuous-flow analysis

An automated method for the indirect determination of fluoride by inductively coupled plasma atomic emission spectrometry using discontinuous-flow analysis has been developed. A modified flow injection analysis system was used for sample preparation. The method is based on the determination of excess cerium(III) ion after precipitation of CeF₃. Separation of the precipitate is performed online on a syringe membrane filter that is cleaned each analysis cycle by 1 M nitric acid, ensuring a long life-time for the filter. As a result of the short reaction time, a detection limit of 9.5 mg L^?1 was obtained. The precision (RSD) of the proposed method is 1.02% at fluoride concentration of 28 mg L^?1. The applicability of the technique for groundwater monitoring of fluoride-contaminated area is demonstrated.     

微波消解-ICP-OES联合测AZ61镁合金中Zn、Mn、Al的不确定度分析

目的研究AZ61镁合金中合金元素成分分析过程中的不确定度因素,以提高分析结果的准确性。方法采用微波消解仪消解样品,以电感耦合等离子体发射光谱仪(ICP-OES)测定AZ61镁合金中锌、锰、铝元素的含量。分析测试过程中产生不确定度的因素,并且进行评定和计算。结果采用微波消解-ICP-OES法测定镁合金中锌、锰、铝元素的含量时,测量不确定度主要由样品溶液稀释、移液枪、标准曲线以及测试的重复性引起,AZ61镁合金主要的合金成分为锌(1.1270%±0.0433%)、锰(0.1797%±0.0064%);铝(6.4468%±0.2029%)。结论对分析过程中产生的不确定度因素进行分析及评定,可以确保分析结果的可靠性以及准确性,从而更好地控制镁合金的性能,提高镁合金的装备环境适应性。     

Determination of heavy metals (Cd, Cr, Cu, Fe, Ni, Pb, Zn) by ICP-OES and their speciation in Algerian Mediterranean Sea sediments after a five-stage sequential extraction procedure

Surface sediment samples (n = 18) were collected from the Algerian Mediterranean coasts and analyzed for seven metals using inductively coupled plasma-optical emission spectrometry in order to asses the distribution and bioavailability of metals and to study the anthropogenic factors affecting their concentrations. Sediment samples were size-fractionated into three sizes: 1,080–500 (coarse), 500–250 (medium), and <250 mm (fine). Bulk sediments were subjected to both sequential extraction and total digestion to evaluate the reliability of the sequential extraction procedure (SEP), while the fractions have been only sequentially extracted for metals speciation. The metals were sequentially extracted into five phases namely exchangeable (P1), carbonates (P2), Fe–Mn oxides (P3), organic (P4) and residual (P5). Metal recoveries in sequential extractions were ±20% of the independently measured total metal concentrations; the high recovery rates indicate the good reliability of the SEP used in this study. Correlation coefficients indicated that the grain size has an effect on the distribution of metals in the investigated samples. The order of metal levels in the fractions was medium > fine > coarse for all the metals. The average total extractable metal concentrations for Cd, Cr, Cu, Fe, Ni, Pb, and Zn were 1.1, 8.8, 4.7, 1,291.3, 13.9, 5.7 and 20.4 μg/g, respectively. The northeastern shelf had the lowest metal levels while the highest were in northwestern part mainly due to the significant tourism activities in the northwestern part. Comparison of our results to Earth’s crust values and to previous studies points out that our samples were relatively unpolluted with respect to the heavy metals investigated; most of the metals are not from anthropogenic sources. Enrichment factors as the criteria for examining the impact of the anthropogenic sources of heavy metals were calculated, and it was observed that the investigated samples were not contaminated with Cr, Cu, and Fe, moderately contaminated with Ni, Pb, and Cd, and contaminated with Cd in some sites. The P5 phase had the highest percents of Cr, Cu, Fe, Ni, and Zn. Cadmium and lead were predominant in the P4 phase, while Cu, Fe and Zn were distributed in the order P5 > P3 > P4 > P2 > P1. The following order of bioavailability was found with the heavy metals Pb > Cr > Cd > Ni > Zn > Cu > Fe.     

测定降尘中的多种重金属的方法研究

降尘采用全自动石墨消解仪消解,用电感等离子体发射光谱仪(ICP-OES)测定降尘中的Cu、Ni、Zn、Pb、Ba、As、Mn、AL、Fe、Cr、Sr、Cd、Ti等13种重金属元素含量.选择合适的波长,标准曲线的相关系数均大于0.999,各元素的分析信号值与浓度呈良好的线性关系,分析标准土壤样品都在不确定度范围内.并计算其空白加标和样品加标回收率,建立了测定降尘中重金属的最优消解方法.结果表明,空白加标和样品加标回收率均处于合理范围,分别为90.1%~104%和85.9%~96.7%.     

Trace metal concentrations in hairs of three bat species from an urbanized area in Germany

Metal-contaminated soils and sediments are widespread in urbanized areas due to atmospheric deposition close to emission sources. These metals are bio-available for organisms, e.g., insects, and accumulate in food chains of insectivorous mammals. Especially bats, which live in urban regions and ingest large amounts of food relative to their body mass, are at risk of being poisoned due to the accumulation of trace metals. To determine species-specific trace metal contents in bats from urban environments, hair samples were analyzed by ICP-OES. Observed trace metal concentrations were related to species-specific foraging habitat, prey spectrum and degree of synanthropy. The species studied were Pipistrellus pipistrellus, Myotis daubentonii and Nyctalus noctula. P. pipistrellus showed the highest concentrations of lead and zinc and slightly higher concentrations of cadmium than the other two species, which was related to its high degree of synanthropy with foraging habitat mostly located in cities. In contrast, N. noctula displayed the highest contents of manganese and copper. The reason might be found in its prey spectrum, as N. noctula feeds mainly on beetles that are caught in cultured areas. Trace metal concentrations determined in hair samples of M. daubentonii ranged between the values of P. pipistrellus and N. noctula, probably reflecting an intermediate level of synanthropy. Positive correlations were observed between the concentrations of cadmium and lead and those of manganese and copper. Hair samples from bats are suitable monitoring tools to study trace metal exposure and can be used to determine differences in trace metal levels between species.     

江西地域煤炭中重金属元素分布研究

通过微波消解、电感耦合等离子发射光谱法(ICP-OES)分析了江西区域各煤矿煤中Cd、Cr、Cu、Mn、Ni、Pb和Zn等7种金属元素的含量,该7种金属元素在0～5ppm的浓度区间具有良好的线性关系,其相关系数r≥0.9997;回收率为92.55%～114.27%,实验数据真实可靠,结果表明:江西地域煤炭中重金属含量分布较广,各地域煤炭中各金属元素的分布与当地环境有关。     

电感耦合等离子体发射光谱法测定土壤和沉积物中硫的适用性研究

为探讨不同消解方式下电感耦合等离子体发射光谱法测定土壤及沉积物中硫的适用性,研究了不同标准物质消解液建立的工作曲线、谱线干扰对分析结果的影响。结合土壤和沉积物来源特点、主成分和待测物含量、干扰物情况,筛选20个典型标准物质分别采用王水水浴法和四酸电热板法进行消解,研究了电感耦合等离子体发射光谱法中3条分析谱线(180.669、181.972、182.562 nm)测定样品中硫的情况。结果表明,0.500 0 g样品经10.0 mL王水(体积比1∶1)沸水浴消解4 h,采用电感耦合等离子体发射光谱仪分析谱线硫181.972 nm建立的18个标准物质工作曲线相关系数高达0.999 9,标准溶液实测浓度相对误差为-6.9%～16%,2个标准物质测定结果的精密度和认定值回收率分别为3.3%～4.3%和90%～96.7%,满足生态环境和自然资源行业的质量控制要求,该方法测定结果与波长色散X射线荧光标准分析方法具有可比性。建立工作曲线的标准物质应考虑待测物和干扰物含量,宜选用标准浓度认定值测试的相对误差而非工作曲线的相关系数作为评价工作曲线优劣的主要技术指标,谱线干扰的理论推导情况和实验结果在趋势...     

荧光探针PTAID固态试纸法测定土壤中Pd2+和Cu2+的比较研究

将新型荧光探针PTAID以固态形式用于检测土壤中的钯离子（Pd²⁺）和铜离子（Cu²⁺）,检出限分别为 0.63 和1.19 μmol/L,说明探针PTAID对Pd²⁺ 和Cu²⁺有很高的灵敏度。通过条件优化实验,说明探针PTAID在pH值为4.0～12.0,反应时间为0～15 min内可以快速检测Pd²⁺和Cu²⁺。对土壤样品中的Pd²⁺和Cu²⁺进行检测,该方法与电感耦合等离子体发射光谱法相比,准确度和精密度均较高,具有响应时间短、灵敏度高、选择性好等优点,在土壤重金属检测方面具有广阔的应用前景。     

ICP—OES法在测定降水中金属离子的研究

本文主要研究了应用电感耦合等离子体发射光谱法（ICP—OES法）同时测定降水中钾、钠、钙、镁金属离子的应用。通过多次测试待测标准物质,确定各待测元素的最佳分析谱线和仪器的工作参数。根据ICP-OES法测定模拟降水混合标准样品、降水样品及其加标样品的结果,与AAS法（原子吸收分光光度法）进行实验室间比对测定,得出ICP—OES法测定降水中钾、钠、钙、镁各离子的检出限、线性范围、标准偏差、准确度等均比AAS法得到的结果要好。ICP-OES法与国家标准方法——原子吸收分光光度法（GB13580．12—92,GB13580．13—92）相比,具有操作简单、多种元素同时测定、方便快捷、检出限低、线性范围宽、干扰少等优点;有良好的准确度和精密度,相对标准偏差在0．3％～1．5％之间,加标回收率在97％～105％之间;该方法明显优于国家标准方法。