NBS氧化流动注射化学发光法在土壤腐殖酸含量测定中的应用

在碱性条件下,NBS直接氧化腐殖酸产生强烈的化学发光信号,结合流动注射技术,建立了测定土壤腐殖酸含量的流动注射化学发光分析法并详细研究了影响化学发光信号强度的各种因素。方法的测定线性范围为1.0×10-7-1.0×10-3g/ml,检出限(3σ)为3×10-8g/ml。对5.0×10-5g/ml的腐殖酸进行11次平行测定,相对标准偏差为1.8%。将该法用于实际土壤样品分析,结果令人满意。     

搅拌子吸附-热脱附-气相色谱-质谱法分析北京大气中33种多氯联苯

用包覆聚二甲基硅氧烷(PDMS)吸附层的搅拌子作被动大气采样器,建立了搅拌子吸附-热脱附-气相色谱-质谱法(SBSE-TD-GC-MS)分析大气中多氯联苯(PCBs)的方法。优化后的热脱附温度为280℃,热脱附时间为6 min,聚焦冷阱的温度为-40℃,33种PCB单体的热脱附残留比例低于7%。验证了方法的线性、精密度和重复性。标准曲线5个点线性关系良好,33种PCB单体的相关系数r>0.998。方法精密度验证的相对标准偏差(RSD)为0.79%~20.2%(n=8),日内重复性实验的RSD为0.43%~29.8%(n=10),日间重复性实验的RSD为3.20%~29.6%(n=20),方法检出限(LOD)为0.01~2.51 pg,回收率为98%±18%。将建立的方法用于北京大气中PCBs的分析。检出8种PCB单体,质量为2.94~129 pg。在32 d的采样周期内PCB-52、PCB-123、PCB-155一直处于线性吸附阶段,而PCB-1和PCB-3经过了线性吸附阶段、曲线吸附阶段和平衡阶段。研究结果表明,SBSE-TD-GC-MS可以用于大气中PCBs的样品采集和快速分析。     

全自动消解-石墨炉原子吸收法测定土壤中镉的探讨

探讨全自动消解-石墨炉原子吸收法测定土壤中镉的方法。选用硝酸-氢氟酸-高氯酸作为消解体系,采用全自动消解仪对土壤样品进行消解,通过研究干燥、灰化和原子化温度对吸光度的影响,优化出最佳的石墨炉升温程序,依据国标方法 (GB/T17141-1997)石墨炉原子吸收分光光度法测定土壤样品中的镉元素含量。该方法检测土壤国家标准物质GSS-8、 GSS-22、GSS-24等,所得结果与标准值相吻合。方法简便、快速、重现性好、灵敏度高,适用于批量土壤样品中Cd的测定。     

原子荧光法测定土壤中砷前处理方法影响因素的研究

针对方法(GB/T 22105.2—2008)中土壤样品前处理过程中影响砷测定结果的因素进行了各类批次实验,得出各种因素对结果的影响程度及其消解的最佳条件。土壤样品的最佳称量范围为0.2～0.6g,消解液加入量的最佳范围为10～15ml,最佳消解时间为2h,硫脲溶液和抗坏血酸溶液的加入量必须满足20～30ml的条件,样品中加入还原剂后,静置时间不得低于20min,通常为30min。     

ASD-ICP-AES联用快速测定土壤中部分重金属

采用样品全自动消解系统(Automated Sample Digestion)对土壤样品进行前处理,采用ICP-AES对土样中的重金属元素一次性测定.通过优化实验,获得土壤中各种重金属的最佳消解条件.结果表明,经优化的消解程序A1能够快速、稳定消解土壤样品,并获得理想测试结果.经检验,ASD-ICP-AES联用的土样测...     

化学耗氧量标准样品及其使用

经实验,CW1007 COD标准样品(中国环境监测总站研制)可用于实验室间质量考核或实验室内质量控制。本文适对CW1007 COD标准样品的使用进行了酸性高锰钾法和重铬酸钾法两种方法实验比较,其结果表明,CW1007 COD标准样品适用于铬法,不适用于锰法。     

丙酮法和热乙醇法测定浮游植物叶绿素a的方法比对

将丙酮法和热乙醇法用于测定浮游植物叶绿素a,分析水样中是否加入碳酸镁、水样体积、萃取时间、萃取剂、破碎方法、离心时间、水样存放时间和滤膜样品存放时间等8个因素对测定的影响,并确定最佳试验条件。结果表明:2种方法的测定值之间有较好的线性关系,相比丙酮法,热乙醇法更具优势。     

异辛烷中2,2'',4,4'',5,5''-六溴联苯标准样品的研制

介绍了异辛烷中2,2',4,4',5,5'-六溴联苯(PBB-153)标准样品的研制方法。分别采用气相色谱法、差示扫描量热法对PBB-153原料进行纯度分析,测定了原料中水分、杂质的含量,利用质量平衡法计算得到纯品纯度为99.0%,相对扩展不确定度为1.2%(k=2)。异辛烷中PBB-153标准样品采用称量-容量法制备,配制浓度为50.00μg/m L,利用气相色谱法对其进行均匀性检验和稳定性监测,结果显示均匀性良好,稳定性可达18个月以上。对不确定度进行评估,结果显示相对扩展不确定度为4%(k=2)。该标准样品与国外同类样品具有量值一致性,能有效支撑中国六溴联苯的履约监测与环境管理等工作。     

土壤中重金属可提取态(氯化钙法)分析质量控制样品的研制

为真实反映土壤中重金属的生态风险和环境效应,全国农用地土壤污染状况详查土壤检测要求测定土壤中重金属可提取态(氯化钙法)指标。针对农用地土壤污染状况详查分析质量控制工作要求,研制了土壤中重金属可提取态(氯化钙法)分析质量控制样品。土壤样品为采自江西省旱地农田的红壤,经除杂、干燥、球磨、筛分(0.250 mm)、混匀等加工处理后装瓶。采用重金属总量和重金属可提取态(氯化钙法)两大类指标评价土壤样品的均匀性,均匀性分析结果同时采用单因素方差分析法(F检验法)和相对标准偏差法(RSD法)评价。结果表明:土壤样品均匀性良好,样品最小取样量为4.0g。8家实验室对土壤中As、Cd、Cr、Cu、Hg、Ni、Pb和Zn等8种元素开展联合定值。标准值为联合定值结果的总平均值(X-),标准值上、下限值分别为(X-+3S)和(X--3S),S为联合测定平均值的标准偏差,低于《全国土壤污染状况详查土壤样品分析测试方法技术规定》中分析方法检出限的元素不做量值评定。As、Cd、Cu、Ni和Zn等5种元素评定了标准值,含量范围为0.190 ～ 13.6 mg/kg。Cr、Pb和Hg等3种元素分析结果低于分析方法检出限,未能定值。研制的土壤分析质量控制样品已应用于土壤详查工作,在保证土壤详查检测结果准确可比等方面发挥了重要作用。     

容量法测定土壤阳离子交换量的方法探讨

探讨了乙酸铵交换-容量法测定土壤阳离子交换量过程中影响测定结果的关键分析条件。试验结果表明,最佳分析条件是:土壤样品粒径为20目,土壤样品与乙酸铵溶液的固液比为2 g∶50 m L,振荡频率为240 r/min、振荡时间为4 min,铵离子洗脱剂乙醇使用量为150 m L(均分3次),水蒸气蒸馏的馏出液体积为120 m L,用盐酸标准溶液容量法测定土壤阳离子交换量。结果表明,方法检出限为1.0 cmol/kg,测定下限为4.0 cmol/kg,代表性样品(p H值=5.69~8.13)测定结果的相对标准偏差为2.4%~4.6%(n=6),土壤标准样品测定结果与标准值相符,说明方法具有良好的适用性,能够满足国家土壤环境质量监测及农用地详查分析工作质量要求。     

Toxic effect caused on microflora of soil by pesticide picloram application

The toxic effect of the herbicide picloram on the microbial population of a typical Brazilian red Latosol soil was studied in a series of microcalorimetric experiments. The activity of the soil was stimulated by the addition of 6.0 mg of glucose and 6.0 mg of ammonium sulfate, under 34.8% controlled moisture, to a 1.50 mg soil sample, at 298.15 +/- 0.02 K. The net thermal effect due to the addition of the picloram to the soil was determined by interpreting the power-time curves, which were recorded on the microcalorimeter. The total thermal effect evolved by the microorganisms was affected by the increasing doses of herbicide, and varied from 0 to 10.00 micrograms g-1. An increase in picloram exposure caused a decrease of the original thermal effect, reaching a null value above 20.89 micrograms of herbicide per gram of soil. The decreases of the thermal effect evolved by microorganisms and the increase of the lag phase period are associated with the death of the microbial population. The effects caused by picloram application in this typical Brazilian soil resulted in a strong effect on the soil microbial communities.     

Factors dominating stratification cycle and seasonal water quality variation in a Korean estuarine reservoir

A comprehensive monitoring program was conducted during 2005-2007 to investigate seasonal variations of hydrologic stability and water quality in the Yeongsan Reservoir (YSR), located at the downstream end of the Yeongsan River, Korea. A principal component analysis (PCA) was performed to identify factors dominating the seasonal water quality variation from a large suite of measured data--11 physico-chemical parameters from 48 sampling sites. The results showed that three principal components explained approximately 62% of spatio-seasonal water quality variation, which are related to stratifications, pollutant loadings and resultant eutrophication, and the advective mixing process during the episodic rainfall-runoff events. A comparison was then made between YSR and an upstream freshwater reservoir (Damyang Reservoir, DYR) in the same river basin during an autumn season. It was found that the saline stratification and pollutant input from the upstream contributed to greater concentrations of nutrients and organic matter in YSR compared to DYR. In YSR, saline stratification in combination with thermal stratification was a dominant cause of the longer period (for two consecutive seasons) of hypoxic conditions at the reservoir bottom. The results presented here will help better understand the season- and geography-dependent characteristics of reservoir water quality in Asian Monsoon climate regions such as Korea.     

Advanced techniques for characterization of organic matter from anaerobically digested grapemarc distillery effluents and amended soils

The effects of grapemarc distillery effluents on the quality of soil organic matter is extremely important to ensure the environmentally-safe and agronomically efficient use of these materials as organic amendment. In this work, the effects of the application of untreated (UG) and anaerobically digested grapemarc distillery effluents, either added with (AGM) or without mycorrhiza (AG), on soil humic acid (HA) were investigated in field plot experiments in comparison to HAs from a control soil and an inorganic fertilized soil. The humic acid-like fractions (HALs) isolated from UG, AG and soils were characterized for compositional, structural and functional properties by the use of elemental and functional group analysis, and ultraviolet/visible, Fourier transform infrared and fluorescence spectroscopies. Results obtained indicated that anaerobic digestion of effluents produced an extended mineralization with loss of organic C and stabilization of residual organic matter by increasing the content of HALs in the effluent. With respect to control soil HA, HALs isolated from UG and AG were characterized by smaller acidic functional group contents, a prevalent aliphatic character and smaller aromatic polycondensation and humification degrees. The chemical and spectroscopic characteristics of native soil HA were not substantially modified by application of UG, AG and AGM to soil, which suggests the occurred incorporation of the effluent HAL into native soil HA. In conclusion, these results showed the possibility of a beneficial and safe recycling of grapemarc distillery effluents as soil amendment.     

In situ laser-induced fluorescence (LIF) analysis of petroleum product-contaminated soil samples

General considerations of the calibrations of in situ measurements are presented and the concept of using an "average oil" with average analysability for calibration purposes is introduced. The in situ analysis of 30 petroleum product-contaminated soil samples with laser-induced fluorescence (LIF) spectroscopy was performed. Compared to an uncontaminated laboratory reference (LR) soil, 23 soil samples exhibited significantly higher LIF signals, so that these soil samples were classified as contaminated. The repeatability and reproducibility of the in situ LIF analysis were investigated. For the calibration of the LIF data, two LR oils (a fuel oil and a crude oil) were employed. The degree of soil contamination with petroleum products ranged from the limit of detection (LOD) for LIF analysis (ca. 100 ppm), or below, to more than 10,000 ppm. The petroleum product concentrations determined with in situ LIF analysis reveal a reasonable correlation with the results of standard IR analysis after extraction of the contaminated soils.     

Assessing soil quality indicator under different land use and soil erosion using multivariate statistical techniques

Soil degradation associated with soil erosion and land use is a critical problem in Iran and there is little or insufficient scientific information in assessing soil quality indicator. In this study, factor analysis (FA) and discriminant analysis (DA) were used to identify the most sensitive indicators of soil quality for evaluating land use and soil erosion within the Hiv catchment in Iran and subsequently compare soil quality assessment using expert opinion based on soil surface factors (SSF) form of Bureau of Land Management (BLM) method. Therefore, 19 soil physical, chemical, and biochemical properties were measured from 56 different sampling sites covering three land use/soil erosion categories (rangeland/surface erosion, orchard/surface erosion, and rangeland/stream bank erosion). FA identified four factors that explained for 82 % of the variation in soil properties. Three factors showed significant differences among the three land use/soil erosion categories. The results indicated that based upon backward-mode DA, dehydrogenase, silt, and manganese allowed more than 80 % of the samples to be correctly assigned to their land use and erosional status. Canonical scores of discriminant functions were significantly correlated to the six soil surface indices derived of BLM method. Stepwise linear regression revealed that soil surface indices: soil movement, surface litter, pedestalling, and sum of SSF were also positively related to the dehydrogenase and silt. This suggests that dehydrogenase and silt are most sensitive to land use and soil erosion.     

Investigation of 15-year-old municipal solid waste deposit profiles by means of FTIR spectroscopy and thermal analysis

Five profiles of a 15-year-old bank containing over three weeks composted municipal solid waste were characterized by means of different parameters habitually applied in waste management (loss on ignition, total organic carbon, total nitrogen, NH(4)-N, pH), and in addition by humic acid determination, FTIR spectroscopy and thermal analysis. Stabilization processes are revealed by humic acid contents. Over the 15 year period organic matter had developed in various ways. Highest humic acid contents were found at 0.5 m below the surface. Below 1.0-1.5 m anaerobic conditions dominated causing a strong decline of humic acid concentrations. Despite similar contents of organic matter at 0.5 m and at 3.0 m organic matter quality differed. These differences were verified by infrared spectroscopic investigations and thermal analyses (differential scanning calorimetry DSC). The spectral pattern of 15-year-old profile samples (municipal solid waste including the biogenic fraction) was compared to current municipal solid waste and abandoned landfill materials. Current municipal solid waste samples comprised different degradation stages from fresh materials to stabilized waste, suitable for landfilling according to Austrian standards. Municipal solid waste originating from abandoned landfills closed in the seventies represented stable material. Principal component analysis was performed to detect similarities and differences. It is evident that the profile samples constitute a particular group in between municipal solid waste and abandoned landfill material. Some differences can be attributed to the divergent composition of municipal solid waste in the eighties when the organic fraction was not separated. Otherwise, landfill materials from the seventies with the same composition regarding the organic fraction were deposited together with construction waste. Heat flow curves (DSC profiles) of municipal solid waste, representing different decomposition stages, illustrate the development of enthalpies and reveal the status of the profile samples. It is evident that mechanical-biological pretreatment leads to a faster stabilization of waste organic matter.     

Application of MODIS satellite data in monitoring water quality parameters of Chaohu Lake in China

This study aims to apply Moderate Resolution Imaging Spectroradiometer (MODIS Data) to monitor water quality parameters including chlorophyll-a, secchi disk depth, total phosphorus and total nitrogen at Chaohu Lake. In this paper, multivariate regression analysis, Back Propagation neural networks (BPs), Radial Basis Function neural networks (RBFs) and Genetic Algorithms-Back Propagation (GA-BP) were applied to investigate the relationships between water quality parameters and the MODIS bands combinations. The study results indicated that a simple, efficient and acceptable model could be established through multivariate regression analysis, but the model precision was relatively low. In comparison, BPs, RBFs and GA-BP were significantly advantageous in terms of sufficient utilization of spectra information and model reliance. The relative errors of BPs, RBFs and GA-BP were below 35%. Based on method comparison, it can be concluded that GA-BP is more suitable for simulation and prediction of water quality parameters by applying genetic algorithm to optimize the weight value of BP network. This study demonstrates that MODIS data can be applied for monitoring some of the water quality parameters of large inland lakes.     

加速溶剂萃取-凝胶净化色谱-气相色谱质谱法测定农用地土壤中有机氯农药方法研究

通过对加速溶剂萃取、平行蒸发及净化方法等环节的优化实验,建立了加速溶剂萃取-凝胶净化色谱-气相色谱质谱法测定农用地土壤中23种有机氯农药的检测方法。结果表明,方法检出限为0.0034~0.0052 mg/kg;对化合物质量分数为0.25 mg/kg的土壤加标样品进行平行实验,回收率为82.0%~93.7%;测定结果的相对标准偏差（RSD）≤8.7%。对土壤有证标准质控样品进行分析,测定结果均在验收范围之内。该方法准确可靠,灵敏度较高,样品净化效果较好,能够满足农用地土壤中有机氯农药残留痕量分析的要求。     

钱塘江南源流域异常水质预测及影响因素分析

基于数据驱动的水质预测模型存在局限性,对突发水质异常事件的预测效果不佳。该研究选取钱塘江南源流域马戍口监测断面为研究对象,综合采用相关性分析方法对水质异常事件的主要影响因素进行分析,明确流域内、外因及土壤条件对水质异常指标的影响程度,探究造成模型局限性的深层原因。结果表明:异常水质的影响因素及其耦合机制复杂多变,异常浊度受降雨量、径流量的直接影响更大,异常高锰酸盐指数与温度、降雨量相关关系更明显,而总磷、总氮的异常变化与相对湿度、降雨量、径流量具有相关关系。研究结果对于提高气候变化背景下的水质预报能力具有重要的参考价值,可为自然流域水污染防治提供科学参考。     

Interpretation and Discrimination of Marshy Wetlands by Soil Factors in the Kuan-Tu Natural Park, Taiwan

This work investigated soil samples collected from Kuan–Tu wetlands, Taiwan. Factor analysis was performed to explain the impact of various soil factors on this marshy wetlands located in suburban Taipei. The results indicated that the latent factors were heavy metals, salinity, and soil organic matter. Canonical discriminant analysis was used to improve an existing vegetation classi–fication scheme by identifying the physical-chemical properties of sediment in Kaun–Tu wetlands, Taiwan. Predictive discriminant analysis was used to examine the ability of the models to predict class membership for unknown soil sample. Multivariate analysis of the spatial patterns of soil quality and vegetation types showed that different properties of soil grew different types of vegetation and absorbed contaminants differently. We can feasibly conserve a suitable habitat for wetland biology by processing these unstable predictor variables. The methodology and results provide useful information concerning the Kuan–Tu wetlands and may be applicable to other wetlands with similar properties that are experiencing similar environmental issues.