淡水环境沉积物中微塑料的密度分离方法研究

微塑料污染已广泛覆盖了全球海洋和淡水环境的表层水体、深层水体以及沉积物,沉积物中的泥沙和其他杂质颗粒会严重影响对沉积物中微塑料的实验分析.因此,将微塑料从沉积物中分离出来至关重要,而目前我国微塑料分离方法暂无统一的系统程序和检测标准.该研究在岷江成都段选取4个采样点采集沉积物样品,通过对比研究基于密度分离法的3种分离方...     

海洋沉积物基质多环芳烃标准参考物质的原料样品制备研究

海洋沉积物基质多环芳烃(PAHs)标准参考物质是海洋环境沉积物监测分析中质量控制和质量保证的重要保障。由于缺少对相关原料样筛选研究,目前我国尚未有自主制备的海洋沉积物基质PAHs标准参考物质。通过海洋沉积物原始数据调研、定点筛查、实验室间验证等手段,对江苏近岸海域海洋沉积物原料样进行筛选研究。结果表明,连云港赣榆某入海口点位的海洋沉积物样品∑PAHs的质量分数为413μg/kg,该样品各粒径中的PAHs质量分数分布均匀,精密度能够满足我国海洋沉积物环境监测质量控制需求,可以为进一步制备海洋沉积物PAHs标准参考物质提供技术支持。     

微波消解-石墨炉原子吸收分光光度法测定海洋沉积物中镉和铬

以硝酸作为消解液,采用微波消解仪对海洋沉积物进行消解,用石墨炉原子吸收分光光度法测定消解液中的Cd和Cr。该方法在0μg/L~10.0μg/L范围内线性良好,Cd和Cr的方法检出限分别为0.04 mg/kg和2.0 mg/kg,实际样品的加标回收率在96.0%~100%之间,RSD为0.3%~5.2%。用该方法与国标法同时测定北部湾海域海洋沉积物实际样品,结果无明显差异,而该方法处理样品更为省时省力。     

水系沉积物重金属分析前处理方法

建立了水系沉积物中6种重金属分析的前处理方法,研究了样品粒径、消解前处理对测定结果的影响,对方法适用性作出评价,并对实际样品进行测定。结果表明:通过Hg元素含量的测定,粒径为0.147 mm的沉积物粒径可满足分析要求;采用微波-硝酸-盐酸-氢氟酸消解、ICP-MS法,对5种不同类型沉积物标准样品的6种重金属的测定结果显示,该方法精密度好、准确度高。利用建立的方法测定广西某河流湖库沉积物样品,6种元素测定结果 RSD为1.57%~11.1%,加标回收率大于74.4%。     

能量色散X射线荧光光谱法测定土壤和沉积物中稀土元素

建立了偏振能量色散X射线荧光光谱法测定土壤和沉积物中稀土元素的方法,该方法较传统的方法具有前处理简单、测量自动化程度高、灵敏度高和检出限低(检出限范围为0.05~2.80 mg/kg)等优点。对土壤和沉积物标准物质的测定结果表明:测定结果与认定值能较好吻合,相对标准偏差范围为0.2%~9.4%,能满足测试的需求。分别用该方法和电感耦合等离子体质谱法对实际样品进行测定,2种方法的测定结果有较好的一致性,表明该方法测定结果准确可靠,可用于实际样品的测定。     

超高效液相色谱-串联质谱法分析土壤及沉积物中氨基甲酸酯农药

利用超高效液相色谱-串联质谱,建立土壤和沉积物中痕量氨基甲酸酯农药的分析方法。该方法用体积比1:1的二氯甲烷/甲醇对土壤和沉积物样品进行加速溶剂萃取,GCB/PSA固相萃取小柱对萃取液进行净化,内标法定量,用超高效液相色谱-串联质谱法分析土壤和沉积物中20种氨基甲酸酯农药。20种氨基甲酸酯农药在0.02~1.0 μg/mL范围内线性良好(r≥0.99),检测限为0.20~0.60 ng/g。沉积物加标样品(20ng/g)和土壤加标样品(20ng/g)的回收率分别为33.2%~101.9%、38.8%~120.5%,相对标准偏差为6.1%~28.0%、2.3%~16.0%。沉积物加标样品(2.0 ng/g)回收率为43.0%~100.0%,相对标准偏差为2.1%~11.3%。     

重点流域水系沉积物中多环芳烃标准样品制备

环境标准样品是监测过程中重要的质量控制手段,中国受天然基体标准样品制备技术的制约,尚未拥有自己的沉积物中多环芳烃标准样品。为制备符合中国重点流域沉积物类型及多环芳烃浓度水平的沉积物标准样品,对中国6个重点流域的沉积物进行了采样,获得了制备多环芳烃标准样品的原料。分析常温及冷冻2种干燥方式对多环芳烃的影响,为制备大批量多环芳烃标准样品提供数据支持。对11个点位样品采用气相色谱质谱法测定16种优控多环芳烃化合物浓度,结果表明,样品均匀性良好,样品中多环芳烃检出率在99%以上,江河沉积物样品中多环芳烃浓度区间为664~2.91×103μg/kg,湖泊样品最高值达到1.25×105μg/kg,其主要污染源是化学燃料的燃烧。为中国制备水系沉积物中多环芳烃标准样品积累了技术基础。     

偏振能量色散X-射线荧光光谱法测定土壤中Ni、Cu、Zn、Pb四种重金属元素

以土壤和水系沉积物标准物质为校准样品,采用粉末样品压片制样,建立了偏振能量色散X-射线荧光光谱仪测定土壤中Ni、Cu、Zn、Pb四种重金属元素的方法。该方法分别采用Ge,Zn,Zr等3个不同二次靶对被分析元素进行选择性激发和测定,利用经验系数和康普顿散射线作内标校正基体效应,优化了元素校准曲线方程,实验结果表明,土壤和水系沉积物标准物质准确度实验结果符合定值要求,方法精密度RSD在1.12%~6.09%之间(n=10),Ni、Cu、Zn、Pb四种重金属元素的检出限分别达到2.54、0.93、0.96、0.98 mg/kg。土壤样品测定值与原子吸收法测定结果一致,该方法准确度、精密度、检出限均能满足土壤检测的需要。     

优化QuEChERS结合HPLC测定沉积物中14种多环芳烃

以美国国家标准技术研究院(NIST)2种沉积物标样SRM 1944和SRM 1941b为研究对象,建立并优化了QuEChERS结合HPLC测定沉积物中14种多环芳烃的前处理方法,并与传统索氏提取进行比较。优化后的QuEChERS方法:样品经乙腈浸泡后,超声15 min,漩涡振荡3 min,以NaCl和无水MgSO_4盐析,提取液经PSA净化后经HPLC-FLD测定。该条件下14种PAHs的方法检出限为0.5~5.0μg/kg,SRM 1944和SRM 1941b中PAHs回收率分别为73.4%~104.9%和71.9%~96.4%,相对标准偏差分别为0.47%~3.45%和0.87%~3.05%。索氏提取SRM 1944与1941b回收率分别为78.9%~109.3%和80.9%~108.2%,相对标准偏差分别为1.46%~10.3%和1.27%~10.8%。优化后的QuEChERS回收率与索氏提取较为接近,但具有更高的精密度。将该方法用于实际海洋沉积物提取,PAHs测定值与索氏提取较为接近。优化后的QuEChERS方法满足批量沉积物样品中PAHs的快速测定要求。     

X射线荧光光谱分析空气滤膜颗粒物中多种元素

采用X射线荧光光谱分析空气滤膜采集悬浮颗粒物中的多种元素,样品不需要前处理,不使用试剂,测量1个样品中40余种元素约耗时1 h。重复测量10次NIST SRM 2783空气滤膜标准样品,多数元素的测量值与标准值基本一致,测量值的标准偏差较小;测量20个空气滤膜实际样品,并与ICP-MS法作比对,大多数元素两种方法测量结果的相对偏差较小,测量值基本一致。     

Analysis of volatile organic compounds (VOCs) in sediments using in situ SPME sampling

A new method of determining the composition of sediment/soil gases and their volatile organic compound (VOC) content is described. VOCs were collected in situ from intertidal sediments in the Menai Strait and surrounding areas. The sampling was performed using a portable sampler comprising a funnel coupled to a SPME fibre. Gases were extracted from the sediments using a small vacuum pump pulling 100 mL min(-1) at atmospheric pressure. Sixty one different compounds were detected in the samples, and their fluxes and concentrations were determined. The compounds were classified into groups: halogenated, sulfur containing compounds, aldehydes, BTEXs (benzene, toluene, ethyl benzene and xylene) and aliphatic hydrocarbons. Results of principal component analysis (PCA) showed that the chemical composition of extracted gas was influenced primarily by sediment type. Muddy anoxic sediments were dominated by halogenated and sulfur containing compounds and sandy sediments had more aldehydes and BTEXs.     

Optimizing the weight loss-on-ignition methodology to quantify organic and carbonate carbon of sediments from diverse sources

The sequential weight loss-on-ignition (WLOI) method for determination of organic and carbonate or inorganic carbon (C) content was evaluated on sediments from diverse sources with a great range of C contents. The sediments were collected from canal, wetland, river, estuary, lake, and marine sites. The organic and inorganic C contents of these samples ranged from 1 to 430 g kg^???1 and from 4 to 97 g kg^???1, respectively. Combinations of the combustion time and temperature and optimal weight ranges of representative samples were tested, and comparisons of the WLOI method with other methods, including dry combustion and wet combustion, were made. These methods were (1) use of the carbon?Cnitrogen?Csulfur (CNS) autoanalyzer with normal and reduced temperatures for total and organic C, (2) thermogravimetry for both organic and inorganic C, (3) use of the CNS autoanalyzer after removal of inorganic (carbonate) C by fumigating samples with concentrated HCl for organic C, (4) Walkley?CBlack wet combustion method for organic C, and (5) pressure-calcimeter associated with subtraction method (total C minus inorganic C) for organic C determinations. The results of analyzing samples of sediments of diverse origins showed that the optimal combination of temperature and time of WLOI depended mostly on the sources of the analyzed sediment. The WLOI analysis of sediment samples for organic C from wetlands, canal, estuary, or river sites needed a relatively low temperature but that of sediment samples from lake and marine sites required a relatively high temperature. Overall, to obtain reliable analysis results of samples from widely varied sediment sources except marine sediments, 500°C for 12 h was optimal for organic C content determination, and 800°C for yet another 12 h was optimal for inorganic C content determination. The temperature could even be reduced to 475°C if only wetland and stream sediments were included, but for marine sediments, 550°C for 12 h was necessary. Precise C content determinations for most sediment sources could be obtained by WLOI when sample quantities ranged from 2.0 to 4.0 g. The WLOI method, when conducted properly, resulted in precise measurements of C contents in ??standard samples?? used for calibration, and these values were closely comparable to results obtained with other dry combustion methods (R ²????0.96). We conclude that WLOI, which has advantages of simplicity, cost-effectiveness, and no waste disposal over other methods, can provide precise measurements of organic and inorganic C contents in sediments from a wide range of sources, but the selection of heating temperature and exposure time should be carefully considered based on sediment sources.     

江苏如东贝类养殖区重金属的含量分布特征及潜在生态风险评价

根据2010年3月(冬季)、5月(春季)、8月(夏季)、11月(秋季)对江苏省如东县贝类养殖区4次现场监测资料,着重对养殖区海水和表层沉积物中重金属的分布特征进行了分析,并对养殖区进行了生态环境质量评价及潜在生态风险评价。结果表明:海水中重金属污染程度顺序为Pb>Zn>Hg>Cu>As>Cd;表层沉积物中重金属的污染程度顺序依次为Zn>Pb>As>Cu>Hg>Cd;表层沉积物中重金属的潜在生态危害程度顺序依次为Hg>Cd>As>Pb>Cu>Zn。4次调查结果的多种重金属的潜在生态风险指数(RI)均低于140,表明这些重金属对海洋生态系统的潜在生态风险属于低潜在生态风险水平,养殖环境良好。     

Variation of Metals in Bed Sediments of Qaraaoun Reservoir, Lebanon

The Qaraaoun Reservoir (impoundment of the River Litani) is the only artificial surface water body in the country, Lebanon. Earlier study on the water quality of the Qaraaoun Reservoir identified three water quality zoning with a central distinct zone suitable for multipurpose water usage. The objective of this study was to extend the earlier work by considering the total metal content of reservoir bed sediments and hence to evaluate factors that control metal deposition or capture. Water samples were collected from 15 sampling sites and sediment samples were simultaneously collected from 9 sites. Water parameters analyzed were pH, Eh, DO and temperature. Sediment samples were dried and sieved and sediment < 75 μ m was retained for analysis. Sediments were subjected to a stepwise heating process with aqua regia to extract the metals, and their content in sediments determined by ICP-MS. The sediment data revealed higher metal contents where the river entered the reservoir which matched higher concentrations of water parameters at the influx site. Regression analysis of total metals in sediments with distance from the river Litani influx point to the dam revealed a log trend for Fe, Cr and Ni, whereas, the concentrations of Cu, Zn, Cd, Pb were better described by a polynomial regression. Three sediment zones were identified: entrance, oxidation (central) and reducing (near dam) zones. Sediment contents of Zn, Cu and Pb correlated with organic content, whereas sediment Cr and Ni were associated with iron. It was concluded that sediments act as a sink for metals and the deposition of metals is primarily related to sediment organic content and the level of dissolved oxygen in water.     

Determination of heavy metals in lower Sakarya river sediments using a BCR-sequential extraction procedure

A BCR-sequential extraction procedure for the determination of extractable heavy metals was applied to sediments of various rivers and lakes. There are many rivers basins in Turkey. Sakarya River Basin is one of the most important basins, which consists of three parts: Upper, Middle and Lower Sakarya River Basins. In this study, the Lower Sakarya River was selected as the study area for sediments. The samples were collected monthly from 10 pre-determined stations through the river for 10 months time and analysed for the distribution of Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb and Zn elements. The determination of extractable heavy metals in sediments was carried out by using Flame Atomic Absorption Spectrometer. The validation of the results was performed by the analysis of a BCR 701 standard reference material.     

Distribution characteristics of polycyclic aromatic hydrocarbons in sediments and biota from the Zha Long Wetland, China

In this paper, the concentrations of polycyclic aromatic hydrocarbons (PAHs) were measured in biota (reed, grass, mussel, fish, and red-crowned crane) and sediments collected from seven locations in the Zha Long Wetland. PAHs were recovered from the sediments and biota by ultrasonic extraction and then analyzed by means of gas chromatography-mass spectrometry. The total PAH concentrations were 244–713 ng/g dw in sediments, 82.8–415 ng/g dw in plants and 207–4,780 ng/g dw in animals. The total sediment PAH concentrations were categorized as lower to moderate contamination compared with other regions of China and the world. In the plant samples, the accumulation abilities of reed roots and stems for PAHs were higher than those of grass roots. In addition, the concentration of individual PAHs in mussel muscles was the highest in all of the animal samples, followed by fish, feeding crane fetuses, and wild crane fetuses. Compositional analysis suggests that the PAHs in the sediments from the Zha Long Wetland were derived from incomplete biomass combustion. Risk assessment shows that the levels of PAHs in sediments are mostly lower than the effects range mean value (effects range mean), whereas only naphthalene in all sample sites was higher than the effects range low value. It is worthwhile to note that benzo(b)fluoranthene, benzo(k)fluoranthene, indeno(1,2,3-cd)pyrene and benzo(ghi)perylene were detected in crane fetal, which have potential carcinogenicity for organisms from the Zha Long Wetland.     

ICP—AES光谱法同时测定固体废弃物中的多种元素

采用常规酸消化方法分解锑渣和铋渣固体废弃物试样．处理后的消解液直接用ＩＣＰ—ＡＥＳ法同时测定了Ｃｕ、Ｐｈ、Ｍｎ、Ｃｒ、Ｎｉ、和Ｚｎ等多种重金属元素。方法的精密度和准确度较好，适合于常规固体环境样品的分析。     

Mercury concentration in fish from Piracicaba River (Minas Gerais, Brazil)

Mercury emissions from some upstream gold mining areas and recent findings of high natural Hg levels in sediments motivated studies on the Hg cycle in the Minas Gerais state. The study presents the total mercury amount found in Geophagus brasiliensis' muscular tissue (wet weight) and sediments from Piracicaba River. Mercury was analyzed using acid digestion followed by determination of total mercury by cold vapour atomic absorption spectrophotometry. This study was also complemented with the analysis of the limnological parameters (water temperature, conductivity, total dissolved solids, suspended particles, pH, dissolved oxygen, maximum depth, photic index and total carbon). The mercury concentration in sediments samples was higher than the mercury concentration in muscular tissue of fish. The lowest Hg level measured in fish was 0.0147 microg g( - 1), while the highest was 0.101 microg g( - 1). In the sediment samples, the lowest and highest levels were 0.02 microg g( - 1) and 0.16 microg g( - 1), respectively. The Hg concentrations in fish and sediment were both under the maximum limit permitted by the World Health Organization.