Primary Speciation Analysis on 6 Kinds of Microelements in Glycyrrhiza uralensis Fisch.

[Objective]The aim was to analyze the primary speciation of 6 microelements in Glycyrrhiza uralensis Fisch. and provide theoretical basis for explaining pharmacodynamic principle of liquorice and discussing quality control of liquorice planting. [Method]The 6 elements Cu,Zn,Ca,Fe,Mg and Mn in roots of G.uralensis were extracted based on traditional decoction method and were separated into water-soluble state and suspension state by micro porous filtering film. The elements in water-soluble state were detected by flame atomic adsorption spectrophotometry （FAAS）. [Result]The results showed that extractive rates of the elements were in the range of 1.71%-60.06%,and immerse-residue ratio in 0.018 3-1.682 0; the results also indicated that the immerse-residue ratio of Zn was biggest （1.68）,Zn played an important medical role and might be considered as the best characteristic element in G.uralensis; the recoveries of the elements were ranged from 95.72% to 103.15% and relative standard deviations （RSD） were less than 2.38%. [Conclusion]Because of its high accuracy,FAAS method is feasible for analyzing primary speciation of microelements in G.uralensis.

Determination of Inorganic Antimony Species Conversions during Its Speciation Analysis in Soil Using Isotope Dilution Techniques

A new method was developed in this work to account for inorganic Sb species interconversion during soil sample preparation and subsequent separation steps. The Sb(III) and Sb(V) concentrations at each investigated step in the analytical procedure were determined using species specific spikes (121Sb(III) with 81.18% and 123Sb(V) with 74.04% enrichment). The spiking of these enriched isotopes species solutions was done separately before soil sample extraction and before HPLC separation. Simply by subtracting the final concentration of each species done by on-line isotope dilution (ID) from its concentration at different stages of the analytical procedure done by species specific ID, the influence of each step on species transformation can be estimated. After optimization, the extraction procedure for inorganic Sb species 6% Sb(III) (1.3 RSD, n = 3) and 43.2% Sb(V) (2.9% RSD, n = 3) as percent of total Sb were detected in the examined soil sample using online ID. Using the above described methodology we found that there was no reduction of Sb(V) to Sb(III) during sample preparation or species separation. While about 9.3% of extractable Sb (4.6% of total) was converted from Sb(III) to Sb(V) during the extraction step, no conversion during HPLC separation step was observed. By compensating for Sb(III) transformation during the sample preparation step;the extractable Sb(III) and Sb(V) as percent of total Sb yielded 10.6% and 38.7%, respectively.

Application of ultrasonic to speciation analysis of heavy metals in soil

In order to reduce the operation time and improve the extraction efficiency, ultrasonic energy by means of ultrasonic bath was used to the modified Tessier sequential extraction for speciation analysis of heavy metals in soil. Extractable contents of Cu, Fe, Mn, Ni, Pb and Zn were measured by atomic absorption spectroscopy(AAS). The merit of the ultrasonic extraction(UE) applied to the modified Tessier method is not only that the operation time for the first 4 fractions was reduced from ca.18 h to 8 h, comparing with conventional extraction(CE), but also the extraction efficiency was higher. The results for both of UE and CE were consistent. The extractable Cu, Ni and Zn in the sample No.1 were mainly associated with the third fraction(Fe-Mn oxides fraction), and fourth fraction(organic matter fraction) in the sample No.2. The extractable Fe and Mn were all mainly associated with the third fraction, and Pb the fourth fraction in both of the samples. The effects of concentration of hydroxylamine chloride on the capability for the extraction of studied metals were also studied.

Study of heavy metal speciation in branch sediments of Poyang Lake

This study concentrates on the environmental pollution level of sediments in the six branches of Poyang Lake, the biggest fresh water lake in China. This is the first systematic report on the speciation analysis of heavy metals （Cu, Co, Cd, Pb, and Ni） in the six branches of the lake. A reported analytical procedure involving a five-step sequential extraction is used for the partition of particulating heavy metals. The sediment samples are analyzed using flame atomic absorption spectroscopy （FAAS）. Experimental results obtained from five replicate samples of fluvial bottom surface sediments at the sampling points demonstrated that the relative standard deviation of the sequential extraction procedure was generally better than 10% （Cd except）. The average extracted contents of the five elements, analyzed after all five steps, are found to be （mg/kg） for Cu： 26.89, Co： 16.25, Cd： 1.08, Pb： 37.98, and Ni： 20.46. The content of the exchangeable species was generally lower. Except Cu, the percentage of the species bond to organic matter was lower than 20%. The fractions containing the most metal for Cu, Co, and Ni were the residues （52.26%, 45.28%, and 74.82%, respectively）.

Analytical Relevance of Trace Metal Speciation in Environmental and Biophysicochemical Systems

This article presents a review of the analytical relevance of trace metal speciation analysis, which must be considered in environmental and biophysicochemical systems for reliable and efficient assessment and monitoring of trace metals. Examples are given of methodological approaches used for speciation analysis. An overview of speciation analysis in sediments, aquatic ecosystems and agrosystems is also presented.

Trace-Level Analysis of Hexavalent Chromium in Lake Sediment Samples Using Ion Chromatography Tandem Mass Spectrometry

The analysis of hexavalent chromium, Cr(VI), in soil and sediment samples has been predominantly carried out in materials containing elevated levels. Reliable analysis of trace-level of Cr(VI) in sediment samples remains challenging. Cr(VI) analyses with multipoint calibration and speciated isotope dilution (SID) adapted from U.S. EPA method 6800 were used to measure lower-level Cr(VI) on an ion chromatograph coupled with a tandem mass spectrometer (IC-MS/MS). Lake sediment samples were collected from various locations in Northern Ontario and Cr(VI) was extracted using both alkaline digestion and ethylene diaminetetraacetic acid (EDTA) extraction. Certified reference materials were extracted and analyzed by IC-MS/MS and UV-VIS detection. The SID-MS approach allowed for the quantification of Cr(VI) in samples with concentration levels below 0.5 μg.g-1 wet weight.

Physico-Chemical Characterization and Speciation of Sulphur of Nigerian Coal Samples

Studies of physico-chemical characterization, and chemical speciation of sulphur of seven Nigerian coal samples have been undertaken. The seven coal samples originated from South-east, North-central and North-east of Nigeria where there are proven economic deposits of this mineral. Moisture content, bulk density, percentage ash and loss of mass on ignition of all the coal samples were determined. The ultimate analysis of the raw coal, the corresponding coal ash as well as sulphur content of all samples were carried out with the aid of X-ray fluorescence technique (XRF). The major elements were Fe, Ca and S while the minor metals were K, Sc, Zn, Ni, Ti and Zr. Other metals including Ga, Cu, Mn, Cr and V were found in traces. The Nickel/Vanadium ratio which is a means of providing information on the source rock depositional environment ranged between 8.8 - 32.9. Three different source rock depositional environments were deduced for the coals from their nickel/vanadium ratios, while the calculated values of V/(V+Ni) suggested that they were all formed under oxic condition. The three chemical species of sulphur, sulphate, pyritic and organic sulphur in the seven coal samples were determined using the ASTM method.

Novel Approach to the Rapid Differentiation of Common Prunus Allergen Species by PCR Product Melt Analysis

Food allergies represent a clear threat to the general health and wellbeing of those affected which place increasing pressure on food producers and regulatory authorities. Current analytical techniques typically find difficulties distinguishing between closely related Prunus species which include almond (Prunus dulcis), an EU listed allergenic species. This study describes a proof of principle real-time PCR approach utilising DNA melt analyses that targets the internal transcribed spacer (ITS) sequence to differentiate between a panel of Prunus test species. The method was successfully applied to the characterisation of a commercial paprika sample suspected of having being adulterated with almond, referred to the UK Government Chemist in 2015 in its advisory capacity. Subject to further validation work, the method appears to specifically amplify Prunus species and is capable of discrimination based on the resultant melt profiles. The developed method provides analysts with a simple and broad molecular tool to identify common Prunus species for food authenticity and allergen testing purposes. Initial development work demonstrates a promising approach with the potential to improve discrimination between Prunus species not easily resolved by routine analytical methods.

Heavy Metals Concentration and Speciation in Arid Zone Rivers （Amudarya and Syrdarya） of Central Asia

The arid zone rivers Amudarya and Syrdarya are located in Central Asia and are subjected to the influx of different kinds of natural and anthropogenic pollutants. The concentrations and speciation of heavy metals, namely, Hg, Cr, Cd, Co, U, Zn, Sc, Fe, Br, Au, and Sm. in the Amudarya and Syrdarya rivers water in the territory of Uzbekistan were investigated by applying the neutron-activation analysis and through experimental modeling using appropriate radionuclides. The heavy metals speciation in the rivers water was separated in cationic, anionic, and a combination of colloidal and neutral forms. The experimental results showed that heavy metals in the Amudarya and Syrdarya rivers water migrate as a complex set of suspended solids, cationic, anionic, and a combination of colloidal neutral forms. The ratio of neutral and colloidal forms averages approximately 40% for the majority of the investigated heavy metals, and the share of neutral and colloidal forms of heavy metals in the Syrdarya river water is slightly less than in the Amudarya river water （10-20%）, which might be due to discharge of water from agricultural and industry sectors into the river.

Elemental analysis of rain-and fresh water by neutron activation analysis

Analysis of rain-and fresh water for trace constituents is it manda- tory part of environmental monitoring. This text gives a survey of neutron activation analysis (NAA) within the framework of current environmental water research pro- grammes, based on the practice developed in co-operation with the Dutch Energy Research Centre at Petten (ECN). While the procedures reported in literature cover about thirty five elements, our routine procedures of instrumental neutron activation analysis (INAA) is limited to ten to fifteen elements. The use of some dedicated ra- diochemical separations (RNAA) adds another six, some of which are speciatcd as well. Current contributions of NAA to water analysis center on determination and speciation of anionic trace elements, notably Br, I, As, and Se, on the assay of some ultra traces like Ag, Au and Hg and on validation.

某铬渣堆污染地下水六价铬污染特征与迁移转化规律研究

我国铬渣堆历史存量较大,渣堆渗滤液中的六价铬[Cr(Ⅵ)]毒性大、迁移性强。为探究污染源特征、场地水文地质条件和水文地球化学过程综合作用下Cr(Ⅵ)在地下水中的迁移转化规律,文章以某铬污染场地为例,通过水样采集与分析,利用克里格插值、因子分析、水化学计算、Piper三线图和离子比等方法查明地下水中Cr(Ⅵ)的空间分布与水化学特征,识别水体中Cr(Ⅵ)的主要赋存形式,并探讨影响Cr(Ⅵ)在地下水中迁移转化的主控因素。结果表明:(1)场地40 m以浅的2个含水层均受到了Cr(Ⅵ)污染,污染范围和程度差异显著。(2)Cr(Ⅵ)在地下水中主要以和Cr_(2)O_(2)-7 HCO_(3)^(-) SO_(4)^(2-)2种形式存在,浓度极低,高浓度Cr(Ⅵ)水点的阴离子以和为主,阳离子以Na^(+)和Ca^(2+)为主。(3)降水淋滤SO_(4)^(2-) HCO_(3)^(-)和渗漏导致含有大量Na+、和Cr(Ⅵ)的渗滤液进入地下水,使地下水pH值升高;高浓度的和弱氧化环境下铁氧化物的溶解可以促进Cr(Ⅵ)在地下水中的迁移;锰氧化物和有机质通过氧化还原反应改变地下水中Cr(Ⅵ)浓度;浅层地下水的蒸发浓缩作用加剧Cr(Ⅵ)在地下水中的富集。研究成果可为铬渣类污染场地的风险管控与后期修复提供有力支撑。

土壤和沉积物重金属形态分析研究进展

人类社会的发展进程导致土壤和沉积物中的重金属含量远远超过背景值,具有严重的潜在威胁隐患。然而,由于重金属的流动性、毒性以及生物累积性会对环境造成深远影响,重金属形态分析已然成为环境研究的重要一环。目前最具代表性的形态提取方法为Tessier法和BCR三步法,为标准物质研制、重金属污染评估、生态修复以及生物有效性风险等问题提供了有效解决方案,但也有着各自的局限性。总结目前常用的元素形态提取分析方法,系统对比论证,讨论重金属形态分析方法未来可能出现的问题和发展方向,以期为土壤及沉积物重金属污染研究提供思路与支撑。

复合稳定剂对污泥中重金属的稳定化效能研究

重金属赋存是制约污泥资源化利用的重要因素。选取碳酸钙(CaCO3)、羟基磷灰石(HAP)和海泡石(Sepiolite)3种稳定剂,以污泥干重的2%、5%、10%投加到供试污泥中,21 d后,采用四分法取样分析浸出毒性及重金属形态,结果表明:3种稳定剂对Cd的稳定作用较弱;另外,HAP的投入量与As的稳定效果成反比。将3种稳定剂按比例复配后,以同样方法研究各组配比对污泥重金属稳定效果,结果表明:HAP∶sepiolite∶CaCO3(质量比)为1∶1∶1时效果最好;此时,污泥中Cd的稳定率达到了80%以上,As、Cr、Pb及Cu的浸出稳定率接近100%,只有Zn和Ni的稳定率与单一稳定剂时相比无明显变化;Cd、Cr、Pb及Cu的稳定态较之前单一稳定剂作用无明显变化甚至减少,但复合稳定剂可提高残渣态的比例;As、Zn和Ni的形态则未有明显变化;复合稳定剂间的协同作用,促使Cd、Cr、Pb及Cu的形态向更稳定态转化。

金属组学方法识别水中络合态重金属形态及其吸附净化技术研究进展

Cu^(2+)、Pb^(2+)和Ni^(2+)等重金属离子可与水中乙二胺四乙酸、柠檬酸、酒石酸等有机分子形成络合态重金属。相比于游离态离子,络合态重金属具有更高的水溶性和环境毒性,在广泛的pH值范围内稳定存在且形态复杂,难以通过化学沉淀等常规方法高效去除。对近年来基于金属组学方法的水中络合态重金属复杂形态分析方法进行总结,对吸附净化技术在络合态重金属废水处理中的研究进展进行综述,并对上述领域需要解决的问题进行了探讨和展望。

土壤中重金属形态及有机物组分的电化学-质谱分析

本研究建立了一种电化学-质谱(EC-MS)法高通量分析土壤样品中的金属组分和有机物。首先,根据理化性质,将土壤样品中的金属组分和有机物组分分为水溶态、脂溶态、难溶态和可氧化态等4种形态;然后,分别采用萃取、反应、电解等方式对4种形态组分进行在线顺次提取;将提取后的组分在线传输至电喷雾电离源进行离子化,随后进行正、负离子模式检测。实际样品分析结果表明,该方法成功检测出土壤样品中多种水溶态金属盐和有机物(如Mg、Cr、Ni、Zn、Co、Cu、Al、Pb等多种水溶性金属盐,尿素及多种有机胺)、20多种脂溶态有机羧酸、以及难溶态金属盐(Mg、Ni、Cr、Pb、Co)和可氧化态(Cu、Pb)。该方法可为环境评估和环境治理提供技术支持。

水环境中元素形态分析技术研究进展

综述了水环境中元素形态分析技术研究进展。水环境中元素形态分析技术主要包括电感耦合等离子体质谱法、原子荧光法、气相色谱法、比色法、毛细管电泳法、原子吸收光谱法等技术及其联用技术。电感耦合等离子体质谱与液相色谱联用技术选择性好、分析速度快、分离效果好;原子荧光与液相色谱联用技术灵敏度高、检出限低、操作简单;气相色谱与电感耦合等离子体质谱联用技术可以实现非常低的检测限和良好的回收率。探索新技术的相互融合,提高元素形态分析技术的灵敏度,获得更低的检测下限,降低分析成本,是未来研究的重点。

陕西紫阳地区茶园土壤氟形态测定及影响茶叶氟含量主要因素

氟在人体生长发育和骨骼代谢中起着重要作用,近年来通过饮茶摄入氟与人体健康的关系受到较大关注。本文以大巴山区紫阳县茶园土壤为研究对象,采集64组茶园土壤和对应茶叶样品,测定土壤理化性质、土壤氟形态、茶叶氟含量,通过多元回归分析建立了影响大巴山区茶叶氟含量的Freundlich模型,并检验了模型的预测精度。结果显示:①研究区茶园表层土壤氟含量范围为487.37~1120.78mg/kg,平均值为730.63mg/kg;研究区茶叶氟含量为31.23~112.49mg/kg,平均值为57.58mg/kg,所有样品均未超过农业标准(NY659-2003)限值;②研究区茶园土壤氟的形态分布为:残渣态>水溶态>有机态>铁锰结合态>可交换态,水溶态氟含量范围为5.27~23.15mg/kg,平均值为9.72mg/kg,远高于中国地氟病发生区水溶态氟的平均含量2.5mg/kg,说明研究区存在一定生态风险。土壤水溶态氟与茶叶氟含量有显著相关性(n=64,r=0.82,p<0.01),其余形态与茶叶氟含量无显著相关性;③以水溶态氟、CEC、交换性铝、有机质、pH五个因子为变量,构建了影响茶叶氟含量的多元回归方程,采用Freundlich模型预测茶叶氟含量,该模型可以解释86.0%的变异,通过验证模型的预测精度达到88.0%,总体来说预测效果较好。本研究结合土壤理化性质、土壤氟形态数据构建了预测茶叶氟的模型,并达到可靠程度,可以为紫阳地区及相似地区茶叶氟生态风险评价、指导绿色农业发展提供理论依据。

Chemical degradation of platinum oncolytics in urine and speciation of the inorganic contaminants cisplatin and carboplatin relevant in waste water

Understanding the prevalent form of platinum(Pt)based antineoplastic agents,used in chemotherapy,is of importance to develop a remediation strategy that restricts aquatic exposure.The speciation of Pt-based compounds was measured in actual patients’urine using hydrophobic interaction liquid chromatography(HILIC)equipped with an ICP-MS detector.Carboplatin showed poor metabolization and intact excretion 11 h after administration,whereas cisplatin underwent a rapid aquation in the first 7 h.To compare,the in vitro degradation rate of cisplatin,carboplatin and oxaliplatin was determined in synthetic human urine,mimicking true environmental conditions.The fraction of intact molecules was measured at regular intervals following incubation at 37°C,resulting in degradation rate constants.The chemical stability was highest for carboplatin(k=0.0143±0.0012 min−1),versus faster degradation of oxaliplatin and cisplatin by exponential decay with k1 of 0.0026±0.0001 min−1 and k_(2)=5.59±0.46×10^(−6) min−1,respectively.These kinetic parameters can serve as input to further expand modelling databases and improve the predictive power of speciation software to estimate eco-toxicity risks.Considering the strong residual cytotoxicity of the platinum antineoplastic molecules following renal clearance and human excretion,the contaminants are of high environmental concern and offer potential for metal recovery using advanced treatment steps.In such water treatment processes,especially carboplatin,above all cancerostatic platinum compounds,should be addressed since it is more persistent in the aquatic environment.

高炉矿渣与磷酸盐复配材料对Cu、Pb、Zn污染土壤的钝化效果研究

选取湖北某矿区重金属污染土壤,通过钝化实验和金属赋存形态分析实验探究了经高炉矿渣(BFS)及其与磷酸二氢钾(MKP)的复配材料修复前后重金属Cu、Pb、Zn的浸出毒性及赋存形态的变化情况。结果表明,BFS-MKP复配材料对土壤的钝化效果优于BFS单独处理,BFS-MKP复配材料对土壤中Cu、Pb的钝化效果要优于Zn,针对Cu、Pb的钝化效率最高分别达到86.1%与88.2%。此外,BFS-MKP复配材料可以促进土壤中活性较高形态的Cu、Pb向较稳定的形态转化。添加复配材料并养护28 d后,土壤中可交换态Cu、Pb含量占比可分别从16.6%、22.7%最低降至0.6%、4.3%,而残渣态Cu、Pb含量占比可分别从64.3%、41.7%最高升至89.3%、81.9%。