土壤中有效态砷钒铬的两种提取方法比较

从提取液对测定结果的影响、消解方法对测定结果的影响和提取效率3个方面,对碳酸氢铵-二乙烯三胺五乙酸(AB-DTPA)法和氯化钙-二乙烯三胺五乙酸(CaCl_2-DTPA)法提取、电感耦合等离子体发射光谱(ICP-OES)法测定土壤中有效态As、V和Cr的优缺点进行了对比,结果表明:AB-DTPA法比CaCl_2-DTPA法提取效率更高。用ICP-OES法测定AB-DTPA法提取有效态As、V和Cr,检出限为0.007～0.019 mg/kg,加标回收率为95.0%～119.0%,相对标准偏差为2.42%～6.30%。该方法快速高效、灵敏度高、准确度和精密度好,实现了多元素同时提取,方法适用性广泛。     

花溪区思雅河水质分析与评价

在花溪区思雅河大学城段布设10个采样点,监测pH值、温度(T)、悬浮物(SS)、化学需氧量(COD)、氨氮(NH_3-N)、总磷(TP)和细菌总数(TPC)等指标,并采用单因子指数法、综合指数法和模糊综合法3种方法对水质进行评价。结果表明:河流主要污染指标为COD,且增势最明显,TPC和NH_3-N测定值的RSD均超过1,比其他指标变异程度更大;COD和TPC春冬季测定值高于夏秋季,NH_3-N测定值秋季最低,TP季节变化不明显,而冬季测定值较其他季节更稳定;思雅河大学城段水质较差,上游水质等级为Ⅳ类,中下游为劣Ⅴ类,主要污染源自农业和高校生活用水;3种方法中,模糊综合法更适用于小流域河流水质的定性定量评价,评价结果更加科学合理。     

重量法与光散射法监测北京市PM_(2.5)的结果比对分析

选择大气污染较重的北京西三环典型交通带作为研究区域,采用重量法和光散射法监测PM_(2.5)。参照美国EPA关于PM_(2.5)连续监测仪器手工采样比对测试的性能指标和认证方法,结合我国现行的相关技术规范,采用平行性检验及线性回归分析两种方法测定结果间的有效性和可比性。结果表明:两种方法测定PM_(2.5)的结果具有较好的相关性,然而受颗粒物物理性质、化学组成及温湿度等的影响,测定结果间存在一定偏差,采用光散射法监测PM_(2.5)仍需用重量法做修正。     

铅蓄电池企业废气中铅及其化合物便携式XRF检测方法

在企业污染源现场实现污染物排放浓度水平的快速判定和超标风险筛查,对生态环境管理部门提高执法效率、企业提高环境管理水平意义重大。铅是一种对人体危害极大的有毒重金属,目前缺少含铅废气中铅及其化合物的便携式直读检测设备和检测方法。探索性地将X射线荧光光谱(XRF)法应用于铅蓄电池企业含铅废气中铅及其化合物的便携式快速、直读检测。研究结果表明,基于XRF的面密度法适用于铅蓄电池企业含铅废气处理设施后铅及其化合物的快速、直读检测,相对国标方法具有快速、直读、对样品无损、便于复测等特点,可用于铅及其化合物排放浓度水平的快速判定和超标风险筛查。     

黄河甘宁蒙段表层沉积物中总磷3种提取方法的比较

通过微波消解法、标准测试方法(SMT)和碱熔法分别测定了水系沉积物成分分析标准物质GBW07307a(GSD-7a)中的总磷(TP)含量,并分别采用3种方法对采集于黄河流域甘宁蒙段表层沉积物样品进行TP含量和样品加标回收率的测定。结果表明:测定标准物质的相对误差绝对值:微波消解法碱熔法SMT法;变异系数:微波消解法碱熔法SMT法。同时,微波消解法提取的表层沉积物TP含量的范围为634.3~909.2μg/g;SMT法TP含量的范围为627.1~889.5μg/g;碱熔法TP含量的范围为559.1~784.8μg/g。微波消解法的测定结果相对偏高,SMT法的测定结果相对偏低。样品加标回收率平均值:微波消解法SMT法碱熔法;变异系数:微波消解法碱熔法SMT法。综合测定标准物质中TP含量以及样品加标回收率实验结果的准确度和精密度,对于黄河甘宁蒙段表层沉积物,使用SMT法提取TP较优于微波消解法和碱熔法。     

便携式XRF土壤重金属检测仪在环境应急监测中的应用探讨

系统评估了便携式XRF重金属检测仪的精密度、准确度及测定影响因素,开展了该方法测定土壤中Cu、Zn、As、Pb、Cr与国标分析方法的系统比对。结果表明:上述5种元素的方法检出限为5.7 mg/kg~16.0 mg/kg,土壤标准样品测定6次结果的RSD为1.0%~4.7%,Zn、Pb和As测定结果的相对误差10%;与国标法相比,便携式XRF重金属检测仪测定Cu、Zn、As、Pb的准确度较好,测定Cr的准确度波动较大。将该方法用于应急污染事故监测,可迅速锁定污染物及污染区域,实现野外分析的预判。     

关于水中悬浮物测定的几点建议

《水和废水监测分析方法 (第 3版 )》测定悬浮物有滤膜法、滤纸法和石棉坩埚法。GB 1 1 90 1 - 89水质悬浮物的测定重量法中明确规定 ,测定悬浮物应使用孔径 0 45 μm、直径 60mm微孔滤膜。在实际工作中 ,由于滤纸法成本低 ,设备简单 ,故仍有不少单位使用 ,这不符合ISO 1 70 2 5中的相关规定。为使更多的单位尽快使用规范的方法 ,现将滤膜法与滤纸法作以下比较 :( 1 )滤膜易恒重。由于滤膜吸水性比滤纸差 ,因此在称量的过程中 ,滤膜的质量相对更为稳定 ,易恒重 ,可缩短测定时间 ,提高工作效率。( 2 )滤膜测定误差小。对于干净的空滤膜 2…     

用DPP法测定饮用水中痕量As（Ⅲ）和总无机砷

砷是一种剧毒的痕量元素,其毒性取决于砷的化学形态.笔者用DDP法测定饮用水中痕量AS(Ⅲ)和总无机砷,克服了原子吸收光谱法或发射光谱法对微量H_3As的测定困难,测定速度又比溶出伏安法快,且精密度高,虽然其方法的灵敏度低于溶出伏安法,但检测限是允许的.1 操作条件:仪器参数、支持电解质、去除干扰物、As(V)还原为 As(Ⅲ).     

淋洗处理土壤的重金属冲刷量测定

利用人工淋洗的方法模拟自然径流对土壤的冲刷,测定城市不同区域的各类土壤中重金属的冲刷量。通过电感耦合等离子体发射光谱(ICP-OES)法对铜、锌、铅、铬、镍5种重金属元素进行连续测定,回收率为96%～103%,线性相关系数r均大于0.999,相对标准偏差(RSD)小于5%。该方法灵敏度、精密度、和准确度均能满足相关检测标准的质量控制要求,具有多元素同时分析、样品前处理简单、干扰少、测定快速、准确等优点。该方法可以提高工作效率,对于大批量或突发性土壤重金属污染的监测具有实际应用价值。     

M3法测定土壤有效态Cd、Cr、Pb和Ni

通过M3法对耕地土壤重金属的联合测定,为土壤重金属污染监测应用提供快速联合测定的方法。用M3法测定北方耕地土壤的有效Cd、Cr、Pb和Ni,通过对M3法与其他方法进行有效重金属测定值差异性及其相关性比较,与全量的浸出率分析等探讨M3法对耕地土壤有效重金属测定的特征。结果表明,M3法在《土壤环境质量标准》(GB 15618—1995)的土壤重金属含量范围内可以测定土壤有效态重金属Cd、Cr、Pb和Ni,且呈线性极显著相关。M3法与其他方法有效Cd、Cr、Pb和Ni有较好的相关性,与DTPA法呈极显著相关;与NaNO₃法除有效Pb外,呈极显著和显著相关;与HCl法除褐土和潮土的有效Pb外,也呈极显著和显著相关。M3法的有效态Cd、Cr、Pb和Ni的测定值均为最大。M3法对4种耕地土壤有效Cd、Cr、Pb和Ni的浸出率,因土壤类型不同,有效重金属含量所占比率不同,但利用M3法测定的有效态Cd、Cr、Pb和Ni的浸出率最大。     

锅炉烟尘测试中锅炉负荷率的计算方法探讨

GB5468 -91规定 ,锅炉烟尘测试时 ,必须对锅炉的运行负荷进行测试 ,而实际监测过程中 ,许多锅炉房不具备测试的计量条件 ,为了解决这一问题 ,文章提出利用烟气量和空气过剩系数计算锅炉负荷率。在实际监测工作中 ,该方法方便、易于操作 ,所得结果和标准规定方法所得结果有很好的一致性     

城市空气质量周报效用分析

介绍了世界上一些发达国家的空气污染预报的做法和采取的措施,阐述了我国开展空气质量预报的方针和方法,指出了周报是预报的基础工作。叙述了我国空气质量周报的污染参数的选取、污染指数的分级及其浓度限值和污染指数计算及确定,分析并总结了开展城市空气质量周报所发挥的效用是提高公众的环保意识,加大了治理污染的力度,转变了环境监测的职能,促进了环境监测事业的发展     

水中总硬度测量不确定度的评定

采用EDTA滴定法测定水质总硬度的测量不确定度评定。充分考虑测量重复性、标准溶液的配制、滴定等过程对测量的影响,计算水中总硬度的测量相对合成标准不确定度为1·81×10-3。     

贵州黔东南州三板溪水库春季拟多甲藻水华特征

2011年3月13日对贵州省黔东南州三板溪水库进行春季浮游植物调查的结果表明,三板溪水库Ⅱ号采样点(下革东)发生以佩纳形拟多甲藻为优势种的拟多甲藻水华,细胞密度高达1.15×10⁷cell/L;板溪水库总氮的最低值为2.09 mg/L,总磷的最低值为0.95 mg/L,三板溪水库的总氮、总磷含量较丰富,不存在总氮或总磷是限制性因子;通过SPSS16.0统计软件分别进行Pearson 积距相关系数分析表明,氮磷比是三板溪水库发生拟多甲藻水华的主要影响原因。     

Environmental Assessment of the Impact of Ozone to the Neuston of the Sea-Surface Microlayer of the Gulf of Mexico

Substantial amounts of NOx (146 000 t/y) and total hydrocarbons (294 000 t/y) are released to the marine atmosphere by the large number of oil and gas operations over Federal waters of the Gulf of Mexico (GOM). Under appropriate meteorological conditions these emissions react to form ozone (0–54 g/m3 over-water) which can affect the marine environment. Using a dry deposition model, this work examines the amount of ozone derived from oil and gas offshore operations and deposited in the sea surface of the Gulf of Mexico, and assesses its impact on the neuston of the sea-surface microlayer. Surface integrated estimates of ozone deposited from oil and gas operations over the sea surface ranges from 400 kg to 1800 kg which results in sea surface concentrations of 15 g/m3. This estimate and the actual toxic ozone levels suggest no acute, toxic impacts to the neuston. However, indirect effects may occur through changes to the pelagic foodwebs and organic carbon pathways. Another potential pathway for ozone impacting the environment is through the production of bromate. Based on the concentrations and time scales (11–139 days) only sublethal effects appear to occur, but uncertainties associated with this assessment need to be further studied. From an ecological perspective, the environmental impacts and risks of NOx and VOC discharges from offshore platforms need to be assessed for neuston and other components of the marine ecosystem.     

实验室质量管理体系内部审核的实施

在实施GB/T15481-2000 idt ISO/IEC17025:1999标准《检测和校准实验室能力的通用要求》的过程中,通过实验室质量管理体系内部审核的实践与系统分析,识别出内部审核实施阶段的关键环节,提出召开首次会议、收集审核证据、确定审核发现和召开末次会议的技术方法,对提高内部审核的质量和有效性、获得可靠的审核结论具有重要意义。     

Fractionation of heavy metals and assessment of contamination of the sediments of Lake Titicaca

Chemical weathering is one of the major geochemical processes that control the mobilization of heavy metals. The present study provides the first report on heavy metal fractionation in sediments (8–156 m) of Lake Titicaca (3,820 m a.s.l.), which is shared by the Republic of Peru and the Plurinational State of Bolivia. Both contents of total Cu, Fe, Ni, Co, Mn, Cd, Pb, and Zn and also the fractionation of these heavy metals associated with four different fractions have been determined following the BCR scheme. The principal component analysis suggests that Co, Ni, and Cd can be attributed to natural sources related to the mineralized geological formations. Moreover, the sources of Cu, Fe, and Mn are effluents and wastes generated from mining activities, while Pb and Zn also suggest that their common source is associated to mining activities. According to the Risk Assessment Code, there is a moderate to high risk related to Zn, Pb, Cd, Mn, Co, and Ni mobilization and/or remobilization from the bottom sediment to the water column. Furthermore, the Geoaccumulation Index and the Enrichment Factor reveal that Zn, Pb, and Cd are enriched in the sediments. The results suggest that the effluents from various traditional mining waste sites in both countries are the main source of heavy metal contamination in the sediments of Lake Titicaca.     

二乙氨基二硫代甲酸银试剂质量对测砷的影响

用简单合成了二乙氨基二硫代甲酸银试剂，并比较了自制和市售的二乙氨基二硫人 银对测砷的影响。结果表明，采用自制的二乙氨基二硫代甲酸银能大大降低试剂空白，提高方法的灵敏度和降低检出限，试剂质量明显优于市售产品。     

氨氮测量不确定度的评定

采用纳氏试剂光度法测定水质氨氮的测量不确定度评定,应该考虑工作曲线、测量重复性、标准溶液、仪器读数分辨率等对测量的影响.     

Evaluation of method of preparation of passive diffusion tubes for measurement of ambient nitrogen dioxide

This study was carried out in response to suggestions that the measurement of NO(2) by Palmes-type passive diffusion tubes (PDT) is affected by the method of preparation of the triethanolamine (TEA) absorbent coating on the grids. The following combinations of factors were investigated: TEA solvent (acetone or water), volume composition of TEA in solvent (50% or 20%), and grid coating method (dipping in solution prior to assembly or pipetting solution on after assembly). Duplicate PDTs prepared by each of the 8 methods were exposed in parallel, in urban air, for a total of 80 separate 1 week exposures. NO(2) concentrations derived from PDTs prepared by pipetting methods were significantly less precise than concentrations from dipping methods, with mean RSDs for duplicate measurements of 13.8% and 8.5%, respectively (n= 316 each category). Pipetting methods using solutions of 50% TEA composition were particularly imprecise (mean RSD 17.2%). Data from PDTs prepared by pipetting methods were systematically more poorly correlated with each other and with data from co-located chemiluminescence analysers, than corresponding data from PDTs prepared by dipping methods, indicating that more consistent accuracy was also obtained by the latter PDTs. The statistical evidence suggested that PDTs prepared by pipetting 50% TEA in water generally gave lower NO(2) concentrations. Although this is in agreement with a previous study, it is also possible that such an observation here may be a statistical artefact given the demonstrably poorer precision of this method. The general tendency of PDTs to show positive bias in NO(2) measurement in urban air in 1 week exposures was again evident in this study (mean biases at roadside and urban centre locations of +35% (n= 475) and +18% (n= 112), respectively) consistent with augmentation of within-tube NO(2) flux by chemical reaction between co-diffusing NO and O(3). Overall, it is recommended that the pipetting method of PDT grid preparation is avoided, or at least investigated further, because of the apparent degradation in precision and accuracy of NO(2) measurement. Potential reasons for the effect are discussed.