高锰酸盐指数测定方法改进

标准方法用沸水浴加热30min,不但效率低,观察水浴是否沸腾不直观,而且水浴沸腾温度受地势、气象条件影响,加热温度达不到要求,结果偏低.本文改用电热板直接加热12min可克服上述缺陷,结果与标准方法相对标准偏差-3.93%～3.24%符合规范要求,经检验无显著差异.注意事项:地区和设备不同,加热时间须经试验确定,以保证结果准确性.     

提高GCMS离子源温度准确定量低浓度DEHP和PAHs

为解决GCMS难以准确定量环境样品中低浓度多环芳烃、酞酸酯类等高沸点、难挥发性有机物的难题,对比了GC进样口温度与MS温度对测定低浓度邻苯二甲酸二(2-乙基己)酯(DEHP)、PAHs的影响。结果证明,MS离子源温度是准确定量DEHP、PAHs的关键因素,通过提高MS离子源温度能大幅度提高PAHs的灵敏度,且MS温度对沸点越高的PAHs灵敏度影响越大。在高MS离子源温度(330℃)条件下,建立了16种PAHs的SIM校准曲线,定量浓度低至5 ng/m L,表现出极高的灵敏度。为今后开发各类环境中低浓度难挥发性有机物的GCMS定量方法提供借鉴意义。     

顶空气相色谱法测定水中硝基氯苯类化合物

建立顶空气相色谱法分析水中16种硝基氯苯类化合物的方法。在研究过程中讨论了盐、顶空平衡温度和平衡时间等因素对测定结果的影响。结果表明,无机盐的加入可以提高硝基氯苯类化合物的响应值,顶空平衡温度80℃和平衡时间50 min为最优的实验分析条件。在此条件下,目标物各组分回归方程的线性相关性较好。方法的检出限为0.05~0.09μg/L,加标回收率为70.6%~119%,相对标准偏差不超过7.9%。该方法简单、快捷、无污染、省时省力,具有较好的推广性。     

用甲醛法测定SO2的影响因素及质量保证措施

探讨了甲醛法测定ＳＯ_２浓度时ＰＲＡ浓度和实验温度对ＳＯ_２曲线斜率的影响。根据实验结果，提出测定ＳＯ_２方法１的实验室质量保证措施，得出不同显色温度的显色时间；ＲＳＤ小于４％，系统误差小、精密度好、准确度高。     

影响紫外法测定总氮的因素研究

用紫外分光光度法测定水中总氮时由于受到试剂质量、消化温度、消化时间、环境等因素的影响,往往使空白吸光值偏高,标准曲线线性和结果重现性差,直接影响测定结果.本文通过对上述因素的研究,提出保证测定质量的条件,找到消除干扰的方法.     

田湾核电温排水遥感监测与数模一致性分析

利用温度反演和数值模拟的方法,对田湾核电站航天遥感测量和数值模拟结果作对比分析。结果显示:遥感监测和数值模拟结果在田湾核电站附近海域的海面温度场羽迹展布方向、不同季节大小潮型、潮态规律上都是相似的,只是在规模和数量上存在着一定差异,两者可以相互验证。     

影响BOD测定结果的因素分析

1反应速率常数 K值的影响 :K值可通过实验 ,由对数——差分法或图解法得到。 K=0 .2 5时 ,BOD5代表总 BOD的 94%。分析时 ,应注意 K的不同其结果在意义上的差异。 2硝化过程的影响 :硝化过程需要加以抑制 ,其方法可采取“巴氏灭菌法”或“去接种法”。 3温度的影响 :温度对生化反应速率有明显影响 ,温度越低 ,温度系数 θ越大。 4p H的影响 :降解有机物的微生物只能在p H6.5～ 8.3内存活。 5营养物影响 :氮、磷含量明显影响分析结果 ,应采用水体水为稀释水。6有毒物影响 :应注意水中微量铜元素影响。影响BOD测定结果的因素分析@赵欣$…     

生化需氧量测定中若干因素探讨

介绍了生化需氧量的方法建立过程,指出测定生化需氧量时,除了温度对测定有影响外,pH值、无机盐类、微生物种类和数量、稀释度、硝化作用、缓冲剂,以及充分的营养和毒性物质的存在与否都会对测定结果有影响.     

电导率计算方法的再改进

电导率测试合格率处于75％的低水平上,究其原因,很大程度是计算公式中的温度校正常数a不适应所有温度所致。文献［1］和文献［2］从不同角度对计算方法作了改进。在精度上有了很大程度的提高,但较繁琐,本文提出了对温度校正常数a直接作修正的方法。1温度校正常数a的测定方法参考温度系数的测定和温度校正方法［3］,考虑到离子浓度等因素对电导率温度校正常数a的影响,选择4个有代表性的KCI标准样品及两个实际样品,逐一测定各温度下的电导率,计算出各温度的常数a（6个样品25℃时电导率分别为1#：111900μs／cm、2＃：12900μs／cm、…     

TTL-HS型吹气仪影响因素的权重分析

对TTL-HS型酸化吹气仪影响因素进行五因素三水平的正交试验研究,并采用SPSS统计分析软件对试验结果进行主效应检验。结果表明,处理前后吹气时间在2、3、5min内对试验结果影响不显著;反应温度、吹气时间、吹气流量对试验结果影响极显著,且对试验结果的影响权重为反应温度吹气时间吹气流量。     

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.     

Mercury emission and dispersion models from soils contaminated by cinnabar mining and metallurgy

The laboratory flux measurement system (LFMS) and dispersion models were used to investigate the kinetics of mercury emission flux (MEF) from contaminated soils. Representative soil samples with respect to total Hg concentration (26-9770 μg g(-1)) surrounding a decommissioned mercury-mining area (Las Cuevas Mine), and a former mercury smelter (Cerco Metalúrgico de Almadenejos), in the Almadén mercury mining district (South Central Spain), were collected. Altogether, 14 samples were analyzed to determine the variation in mercury emission flux (MEF) versus distance from the sources, regulating two major environmental parameters comprising soil temperature and solar radiation. In addition, the fraction of the water-soluble mercury in these samples was determined in order to assess how MEF from soil is related to the mercury in the aqueous soil phase. Measured MEFs ranged from less than 140 to over 10,000 ng m(-2) h(-1), with the highest emissions from contaminated soils adjacent to point sources. A significant decrease of MEF was then observed with increasing distance from these sites. Strong positive effects of both temperature and solar radiation on MEF was observed. Moreover, MEF was found to occur more easily in soils with higher proportions of soluble mercury compared to soils where cinnabar prevails. Based on the calculated Hg emission rates and with the support of geographical information system (GIS) tools and ISC AERMOD software, dispersion models for atmospheric mercury were implemented. In this way, the gaseous mercury plume generated by the soil-originated emissions at different seasons was modeled. Modeling efforts revealed that much higher emissions and larger mercury plumes are generated in dry and warm periods (summer), while the plume is smaller and associated with lower concentrations of atmospheric mercury during colder periods with higher wind activity (fall). Based on the calculated emissions and the model implementation, yearly emissions from the "Cerco Metalúrgico de Almadenejos" decommissioned metallurgical precinct were estimated at 16.4 kg Hg y(-1), with significant differences between seasons.     

Mercury fractionation in contaminated soils from the Idrija mercury mine region

Mercury (Hg) fractionation was investigated in contaminated soil in the Idrija Hg-mine region, Slovenia. The main aim of this study was to test and apply sequential extraction and quantification of different Hg phases in order to estimate the mobility and potential bioavailability of Hg in contaminated soils. Separation of Hg phases was performed by means of a selective sequential extraction procedure complemented by volatilization of elemental mercury (Hg0). The influence of temperature, moisture and storage on Hg0 volatilization was also investigated. The total Hg concentrations varied between 8.4 and 415 mg kg(-1) and were up to 40-fold higher than the maximum permissible set by Slovenian legislation. Fractionation measurements indicated cinnabar as the predominant Hg fraction, followed by Hg0. Accumulation of cinnabar predominantly occurred in coarse grained flood plain sediments, where on average it constituted more than 80% of total Hg. In contrast non-cinnabar fractions were found to be enriched in areas where fine grained material was deposited, reaching up to 60% of total Hg. The strong positive correlation (R2 = 0.71-0.99) among non-cinnabar fractions suggested that these fractions predominantly control the mobility and potential bioavailability of Hg. Sample pretreatment before fractionation influenced the partition of Hg between different fractions, and therefore fractionation in fresh, nontreated samples is suggested. In addition, the specificity of the extraction steps needs further attention, as it was shown that some extraction steps, such as the organo-chelating Hg fraction, do not provide meaningful results. This further suggests that protocols for mercury fractionation need further harmonization in order to improve the comparability of the results and their use in risk assessment. Volatile mercury fluxes averaged between 0.04 and 6.5 ng g(-1) h(-1). Good agreement (R2 = 0.81-0.95) was found between the non-cinnabar fractions and evaporation of Hg0. Both the temperature and sample moisture had significant effects on mercury volatilization. The results in this study were obtained at 70 degrees C, which may be somewhat high, in particular for bacterial activity which may also play an important role in Hg volatilization. Therefore it is strongly suggested that further optimisation of the protocol to assess Hg volatilization from soil is required.     

A Method of Mercury Removal from Topsoil Using Low-Thermal Application

Mercury contamination in the environment is problematic due to the unusual physical properties and well-recognized toxicity of this common metal. The bioavailability of mercury depends strongly on its chemical speciation. Anthropogenic mercury and its compounds appear in soil as hot spots located close to industrial facilities that used or produced mercury. The nature of the chemical production process, transportation and disposal practices often determined the chemical composition and distribution of mercury in the surrounding soils. Current ex situ soil remediation methods are expensive, produce undesirable side effects to the environment and usually involve transportation of contaminated soil.In this project, sponsored by the U.S. Department of Energy, a low-cost, simple approach to removing mercury from soil was evaluated. The process uses low-temperature thermal desorption of volatile metallic mercury and its compounds, and subsequent vapor capture.The project consisted of laboratory and plot-scale experiments. The laboratory efforts evaluated theoretical calculations of mercury removal as a function of time and temperature. The plot-scale experiment was a practical application of the laboratory results. For both experiments, mercury-polluted soil was obtained from a chemical production facility located in southern Poland. In laboratory experiments, at temperature 373 K total mercury concentration decreased in soil by nearly 32%. In plot-scale experiments, at temperature 440 K, about 60–70% of total mercury was removed from the soil.At the end of the experiment, a test of soil biological activity was performed to check if the high temperature applied to the soil did not impair the soil growth properties. There was no negative effect of temperature found.     

Mercury Vapor Determination in Hospitals

The measurements of metallic mercury vapor were carried out in seven local hospitals, where mercury-containing products are widely used, as well as in one residence to check effectiveness of decontamination after mercury spillage. Hopcalite as a solid sorbent was used in active and passive sampling methods, and mercury was analyzed by CV-AAS technique. Good agreement was found between results of mercury measurements using active samplers (pumped hopcalite adsorption tubes) and passive (diffusion) monitors applied in indoor atmosphere. The results indicated the presence of metallic mercury vaporization sources in the assessed hospital rooms but in the majority of cases mercury levels did not exceed 1 g/m³ i.e. Polish permissible concentration for residence. However, in some of the hospital rooms, elevated concentrations of mercury vapor were found and airborne levels of up to 13.9 g/m³ were recorded. Higher concentrations of mercury vapor were observed in autumn season when compared to summer.     

基于吸附原理的双路独立汞采样方法

参照美国EPA 30B方法,基于吸附原理,研制了用于燃煤燃烧源排放烟气中总气态汞的双路独立采样系统,结合热解析分析技术,现场测试结果符合30B方法的质控指标要求。建议加大国产吸附管的研制力度,开发适用于中国工况的汞采样器。     

环境空气中汞的直接测定方法研究与应用

研究了环境空气中汞浓度的直接测定方法。利用金汞齐富集－便携式测汞仪对环境空气中的汞进行直接测定,具有简便、快捷、不使用化学试剂的优点。经测试,该方法在0～180 ng／m^3范围内具有良好的线性关系,最低检出浓度为5 ng／m^3。     

燃煤电厂排放总气态汞连续自动监测技术的选择

介绍了汞连续排放监测系统和汞吸附管采样系统的主要特点,比较了不同仪器的测定原理、样品处理技术、检出限和测定汞的形态,报道了美国环境保护署认证中心关于两个系统的认证结果.建议将汞连续排放监测系统与汞吸附管监测系统两种技术联合用于我国燃煤电厂排放总气态汞的自动监测.     

Formation of a Mercury Plated Carbon Paste Electrode by Electroreduction of a Mercury(II) Diethyldithiocarbamate Modified Carbon Paste

A novel approach to formation of a mercury film electrode (MFE) at the surface of a carbon paste electrode is proposed in this paper. This MFE is easy to fabricate, has good reproducibility and avoids the use of a plating mercury solution. In this new type of MFE, mercuric diethyldithiocarbamate (Hg(DDTC)2) was mixed with graphite powder and paraffin oil to form a chemically modified carbon paste electrode. When a -0.95V potential was applied to the electrode, the Hg(II) (in Hg(DDTC)2) was reduced to metallic Hg, thus forming a mercury film at the surface of the carbon paste electrode. The characteristics of this MFE were studied. This modified electrode was used in anodic stripping voltammetry. Conditions for the simultaneous determination of trace amount of Pb(II) and Cd(II) were also investigated.     

北京市大气气态汞变化特征

采用Tekran 2537X大气汞分析仪在线测量北京市城区大气中气态元素汞(GEM,简称大气汞) 浓度,研究大气汞浓度随不同气象条件的变化特征。通过分析2016年10月—2017年9月大气汞监测数据发现,该监测点全年大气汞浓度为0.48～16.25 ng/m³,均值为(3.41±1.79)ng/m³。春季、夏季、秋季和冬季大气汞浓度均值依次为2.93 、2.95、4.27、3.37 ng/m³,其中,秋季大气汞浓度明显高于其他季节 。秋季大气汞浓度显著偏高可能由不利的大气扩散条件导致。大气汞夜间浓度显著高于白天浓度。同时,将大气汞与SO₂、CO及PM_2.5进行相关性分析,发现大气汞浓度变化趋势与SO₂、CO和PM_2.5呈显著正相关。结合风向和风速进行污染来源分析,得到该点位大气汞在西南和东北方向上受人为排放源影响较大。污染源类型分析表明,冬季大气汞与CO同源性强,主要来自本地供暖用煤。