Metal furnace heated by flame as a hydride atomizer for atomic absorption spectrometry: Sb determination in environmental and pharmaceutical samples

The present work describes a metallic hydride atomizer for atomic absorption spectrometry, by evaluating the performance of the Inconel 600^® tube. For this purpose, stibine was used as the model volatile compound and antimony determination in river and lake sediments and in pharmaceutical samples was carried out to assess the metal furnace performance. Some parameters are evaluated such as those referring to the generation and transport of the hydride (such as KBH₄ and acid concentrations, carrier gas flow rate, injected volume, etc.), as well as those referring to the metal furnace (such as tube hole area, flame composition, long-term stability, etc.). The method presents linear Sb concentration from 2 to 80 μg L⁻¹ range (r > 0.998; n = 3) and the analytical frequency of ca. 140 h⁻¹. The limit of detection (LOD) is 0.23 μg L⁻¹ and the precision, expressed as R.S.D., is less than 5% (40 μg L⁻¹; n = 10). The accuracy is evaluated through the reference materials, and the results are similar at 95% confidence level according to the t-test.     

固相萃取-气相色谱-高分辨质谱法测定巢湖水中半挥发性有机化合物

描述了巢湖水中半挥发性有机化合物的提取、测定过程和初步结果。湖水中半挥发性有机化合物的提取采用XAD-2和XAD-4混合树脂富集，用气相色谱-高分辨质谱法测定了所萃取的有机化合物，并给出相应的分子式和结构式。春季湖水中检测到14种有机化合物。     

Study of parameters associated with the determination of cadmium in lake sediments by slurry sampling electrothermal atomic absorption spectrometry

Cadmium concentration in lake sediments is determined by suspending the solid samples in a solution containing 5% (v/v) concentrated nitric acid and 0.1% (v/v) Triton X-100. Three modifiers were tested for the direct determination. The furnace temperature programmes and appropriate amount for each modifier were optimised to get the highest signal and the best separation between the atomic and background signals. The drying stage is performed by programming a 400 °C temperature, a ramp time of 25 s and hold time of 10 s on the power supply of the atomiser. No ashing step is used and platform atomisation is carried out at 2200 °C. W–Rh permanent modifier combined with conventional modifier by delivering 10 μl of 0.50% (w/v) NH₄H₂PO₄ solution was the best chemical modifier for cadmium determination. This modifier also acts as a liquid medium for the slurry, thus simplifying the procedure. Calibration is performed using aqueous standards in the 1–5 μg l⁻¹ range. The optimised method gave a limit of detection of 0.56 ng ml⁻¹, characteristic mass of 10.1±0.8 pg for aqueous standard, 9.6±0.7 pg for slurry samples containing different Cd concentrations and good precision (7.6–5.2%). The method was validated by analysing four certified reference lake sediment materials: LKSD-1, LKSD-2, LKSD-3 and LKSD-4; satisfactory recoveries were obtained (90.0–96.3%) and no statistical differences were observed between the experimental and the certified cadmium concentration. The developed methodology was used to determine cadmium in three ‘real’ sediment samples from lakes in the area of Wielkopolski National Park, Poland.     

Multiresidue determination of UV filters in water samples by solid‐phase extraction and liquid chromatography with tandem mass spectrometry analysis

UV filters, contained in sunscreens and other cosmetic products, as well as in some plastics and industrial products, are nowadays considered contaminants of emerging concern because their widespread and increasing use has lead to their presence in the environment. Furthermore, some UV filters are suspected to have endocrine disruption activity. In the present work, we developed an analytical method based on liquid chromatography with tandem mass spectrometry for the determination of UV filters in tap and lake waters. Sixteen UV filters were extracted from water samples by solid‐phase extraction employing graphitized carbon black as adsorbent material. Handling 200 mL of water sample, satisfactory recoveries were obtained for almost all the analytes. The limits of detection and quantification of the method were comparable to those reported in other works, and ranged between 0.7–3.5 and 1.9–11.8 ng/L, respectively; however in our case the number of investigated compounds was larger. The major encountered problem in method development was to identify the background contamination sources and reduce their contribution. UV filters were not detected in tap water samples, whereas the analyses conducted on samples collected from three different lakes showed that the swimming areas are most subject to UV filter contamination.     

片段化森林中檵木幼苗种内叶经济性状变异及其驱动因子

在异质性生境中,种内功能性状变异有助于植物对环境的适应,进而影响种群更新、群落构建和生态系统过程。探讨了种内叶经济性状的变异及受生境异质性的塑造情况。以千岛湖片段化生境中的常见种檵木（Loropetalum chinense）的幼苗为研究对象,测定了200株檵木幼苗个体水平的7个叶经济性状（比叶面积SLA、叶全碳量C、叶全氮量N等）及其对应的生境因子（郁闭度、土壤全碳量、土壤全氮量等）,采用相关性检验、主成分分析和线性混合效应模型等方法探讨片段化森林中檵木幼苗的种内叶经济性状变异及生境异质性对该变异的驱动作用。结果显示：（1） 在7个叶经济性状所构成的21对相关性分析中,有12对显著相关。经主成分分析降维后,主成分1（PC1）占性状总变异的43.02%,主要与比叶面积、叶绿素浓度、叶全氮量呈正相关,与叶干物质质量分数和叶碳氮比呈负相关,体现了檵木的种内叶经济谱,可反映叶片的最大光合效率。（2）片段化对生境条件和叶经济性状均有影响。岛屿森林群落的郁闭度显著低于大陆。相对于大陆,岛屿中的檵木幼苗趋向于更小的PC1值（缓慢投资-收益策略）;大岛边缘较大岛内部偏向于更小的PC1值。（3）生境因子中,郁闭度对PC1具有显著正效应。研究表明,片段化生境中的檵木在幼苗阶段存在叶经济谱,生境片段化可通过影响生境条件进而改变檵木幼苗的叶经济性状。随着生境片段化程度的加剧,檵木幼苗的叶经济性状逐渐向缓慢投资-收益策略靠拢。     

内陆水体叶绿素a含量定量检测的研究

以武汉东湖为实验基地,通过对其水体的多次检测,获得了从2006年6月到9月4个月的东湖水体透射光谱,并与蒸馏水透射光谱进行比较,对东湖水富营养化程度进行了定性分析.采用一种新的测量方法得到叶绿素a浓度与677 nm和703 nm处相对强度的差值和比值有很好的线性相关性,建立了东湖水体叶绿素a含量的准确定量检测模型,为实现对东湖水实时、快速、准确监测提供了基础,为高精度遥感水质分析提供了参考.     

双电极法现场快速检测地下水和湖水中碳酸氢根和碳酸根

地下水和湖水中碳酸氢根( HCO-3)和碳酸根( CO2-3)含量是地球化学碳行为和碳循环的重要表征,但两种离子的浓度易受环境影响而改变,因此,地下水和湖水中HCO-3和CO2-3真实含量的测定一直是个难题。实验利用CO2的水解平衡,通过pH电极和二氧化碳电极联用,建立了HCO-3和CO2-3现场快速测定的新方法,解决了地下水和湖水中HCO-3和CO2-3真实含量的测定难题。研究结果表明,在pH=4.8±0.1的底液中, HCO-3和CO2-3的线性范围分别为0.027~570 mg/L和1.25×10-8~39.7 mg/L。共存的金属离子、强酸阴离子(K+、Na+、Mg2+、Cl-、SO2-4,100 mg/L)、弱酸阴离子和弱酸(HSO-3、NO-2、HOAc,50 mg/L)对测定干扰小于5%。实际水样加标实验回收率在95.2%~99.2%之间,相对标准偏差为2.6%~3.7%。与酸碱滴定法进行对比,本方法的准确性良好。但方法受温度影响,因此标准溶液与样品应在同一温度下测量。总体而言,双电极法灵敏、快速、经济且电极携带方便、操作简单、对环境要求不高,十分适合现场和室内一般自然水体的快速检测。本方法已成功应用于青海省地下水和青海湖湖水中HCO-3和CO2-3的现场测定。实验表明,海东地区地下水样品pH在6.4~7.4之间,HCO-3含量为234~4096 mg/L,CO2-3含量为0.16~1.89 mg/L;青海湖湖水样品pH≈8.7,HCO-3含量范围在1.36~1.86 g/L,CO2-3含量在32.3~43.9 mg/L,与文献结果吻合。     

Sediment records of Sb and Pb stable isotopic ratios in Lake Qinghai

A sediment core in Lake Qinghai in northwest China was collected in 2006. ¹³⁷Cs and ²¹⁰Pb activities were analyzed to investigate the chronology of the sediment core. Sb and Pb concentrations, and Pb stable isotopic ratios were analyzed to study the historical atmospheric deposition records and sources of Sb over the past 15 centuries. The Sb concentration was 4.21 ± 1.52 μg/g in the sediments, its vertical distribution of Sb shows three large peaks in the recent two centuries, 1799, 1896 and 1944, coincided with Sb contamination from large wars, respectively. The peak in 1920 responded the large earthquake that happened in northern China, which was not far away from Lake Qinghai. The Sb/Pb ratio, ²⁰⁶Pb/²⁰⁷Pb and ²⁰⁸Pb/²⁰⁶Pb results suggest that Sb and Pb were probably from the ores in South China and coals in North China before 1965, but obviously from uses of leaded gasoline after 1965.     

微波消解-ICP-AES测定鄱阳湖流域沉积物中微量元素

为了研究鄱阳湖沉积物中微量元素近几年来随季节、年度及沿程的变化情况,对2003年和2005年不同季节采集的鄱阳湖流域各采样点底泥进行了ICP-AES测定.结果表明,鄱阳湖沉积物中各元素的含量随着季节和年度变化而发生一定改变,枯水期普遍大于丰水期;南矶山2005年Cu和Pb含量较2003年有所降低;蔡家湾则与南矶山相反;姚公渡2005年Cu含量也较2003年低,Pb含量则高于2003年;与鄱阳湖流域底泥背景值相比,所测几个样点的Cu,Pb,Cr和Zn含量均在一定程度上超标;除大坞河外,其余各样点As含量均在背景值范围内;从饶河到鄱阳湖入湖口处,各元素含量呈逐渐降低趋势.文章提出的研究方法操作简便,效率高,劳动强度低.     

湖北网湖^137Cs、^210Pb计年与沉积速率研究

采用放射性核素^137Cs和^210Pb计年法测定百年来湖北网湖沉积物的年代，据此计算出网湖的沉积速率．结果表明：2种计年方法测得的沉积速率基本一致，以1954年和1963年为时标，^137Cs测得的沉积速率分别为0．594cm·a^-1和0．557cm·a^-1。^210Pb计年法CIC模式计算得到网湖平均沉积速率为0．56cm·a^-1．CRS模式得到百年来网湖沉积速率变化较大，20世纪50年代以前，平均沉积速率为0．2cm·a^-1左右；50年代至80年代中期，平均沉积速率上了一个台阶，约为0．4cm·a^-1；80年代中期以后平均沉积速率攀升至约0．6cm·a^-1，网湖沉积速率变化与湖区自然环境的改变和人类活动的影响密切相关．