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%。     

氧化铝对矿物油中动植油脂脱除实验研究

1植物油脂对矿物油测定影响 :豆油含量小于原油 4倍时影响小 ,相对误差 <5% ,大于 1 0倍时误差 >1 5%。2动物油对矿物油测定的影响 :猪油含量小于矿物油 2倍时 ,原油测定误差 <5% ,大于 1 0倍时相对误差 >2 0 %。 3动植油小于1 0 0 mg时 ,加 1 .0 g氧化铝 ,吸附效率均在 90 %以上 ;动植油含量为 2 0 mg或 50 mg时 ,只需氧化铝0 .5g或 1 .0 g即可满足分离要求 ,相对误差均在5%以内 ,本法操作简单并适合各种油的测定。氧化铝对矿物油中动植油脂脱除实验研究@李纪云$石油大学炼制系!山东东营257062 @李德军$北关油田钻井三公司!河南南考 …     

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。     

土壤和河流沉积物中六六六和滴滴涕残留的测定

采用密闭微波提取、超声波提取、索氏提取对土壤和河流沉积物进行前处理,提取液经弗罗里硅土柱净化或浓硫酸净化.通过回收率实验和精密度实验对三种提取方法和两种净化方法进行比较,建立了微波提取土壤和河流沉积物中六六六和滴滴涕,浓硫酸净化,气相色谱一质谱测定的分析方法,方法回收率在84%～110%之间,精密度(RSD)在2.8%～9.9%之间.采用该方法对阜阳市废弃农药厂周围的土壤和河流沉积物中六六六和滴滴涕进行了监测.     

镇江市金山湖沉积物磷元素分布特征研究

以镇江市金山湖为研究区域，于2019年1月（冬季）和2019年7月（夏季）采集了10个点位的表层沉积物样品，参照欧洲标准测试测量组织建立的沉积物磷形态分析方法（SMT）测定沉积物总磷（TP）、无机磷（IP）、有机磷（OP）、铁/铝-磷（Fe/Al-P）和钙-磷（Ca-P）质量分数，研究金山湖表层沉积物磷元素及其赋存形态的季节分布特征。结果表明，金山湖表层沉积物中TP质量分数在冬、夏季分别为727.39~1 073.70 mg/kg和700.90~1 002.17 mg/kg，处于中等污染水平；金山湖表层沉积物磷以IP为主，IP在TP中的占比在冬、夏季分别为68.58%~88.86%，73.09%~87.21%；除了Fe/Al-P以外，OP作为生物有效磷源，其冬、夏季质量分数分别为69.37~190.93 mg/kg和108.45~210.42 mg/kg；其平均值分别为129.01，160.15 mg/kg。金山湖冬、夏季沉积物各形态磷质量分数所占比例均表现为Ca-P>Fe/Al-P>OP，表明该研究区域沉积物以Ca-P占优势。金山湖表层沉积物pH值呈现弱碱性，通过Ca-P直接释放到上覆水中的磷较少，故金山湖沉积物磷元素的潜在风险较小。各形态磷的相关性分析结果发现，冬季沉积物TP与Fe/Al-P、IP呈极显著正相关（P<0.01）。夏季沉积物TP与IP、Fe/Al-P之间呈极显著正相关（P<0.01），与Ca-P呈显著正相关（P<0.05）。此外，金山湖沉积物OP、Fe/Al-P以及Ca-P的来源不一致。pH值对沉积物IP会产生一定影响，而其余磷形态则受pH值的影响程度较小。     

异丙醇增感电感耦合等离子体质谱法直接测定土壤和沉积物中硒

提出了沸水浴混合酸法消解,以异丙醇为增感剂,电感耦合等离子体质谱直接测定土壤和沉积物中硒的方法。实验表明2mol/L硝酸-4mol/L盐酸混酸能有效溶出土壤和沉积物中各种形态的硒。相对于1%硝酸基体,4%(V/V)异丙醇基体中硒的ICP-MS响应值提高了12.1倍;而且4%(V/V)异丙醇基体可有效抑制硒的质谱干扰。ICP发射功率和雾化气流速是影响异丙醇在ICP-MS测定过程增敏效应的主要因素。以78硒为测定同位素,方法检出限为0.005mg/kg,实际样品测定精密度均小于5%。用于测定土壤和沉积物国家标准样品并对其消解液进行加标回收实验,结果令人满意。     

微波消解-ICP/MS法测定水系沉积物中多种元素

采用微波消解-电感耦合等离子体质谱法测定水系沉积物中12种元素,通过优化试验相关条件消除质谱干扰和非质谱干扰对测定的影响,使方法在0μg/L~200μg/L范围内线性良好,当取样质量为0.25 g,定容体积为50 m L时,各元素的方法检出限为0.002 mg/kg~0.05 mg/kg。用该方法测定沉积物标准物质,6次测定结果均在标准值范围内,RSD为1.3%~6.1%,实际样品的加标回收率为83.0%~97.0%。     

贵州煤矿区表层水-沉积物重金属分布特征及来源分析——以新寨河为例

为探索贵州煤矿区表层水-沉积物中重金属的分布特征及来源,科学制定环境保护与污染治理措施,以新寨河为研究对象,在11个样点共采集66个表层水体和沉积物样品,通过对Cd、Pb、Cr、Zn、Cu、As、Hg、Fe、Mn等9种重金属元素进行分析,揭示其在新寨河的空间分布特征。同时,利用多指数法开展了有毒重金属元素污染状况评价,通过相关性分析和主成分分析解析了重金属的来源。结果表明,新寨河流域表层水体中,Fe、Mn点位超标率达100%。表层水中重金属元素的平均含量排序为Fe＞Mn＞Zn＞Cu＞Cr＞As＞Cd＞Pb＞Hg,而沉积物中重金属元素的平均含量排序则是Fe＞Mn＞Zn＞Cr＞Cu＞As＞Pb＞Cd＞Hg,表明新寨河表层水体和沉积物中重金属元素的空间分布存在一定差异。各重金属元素的内梅罗综合污染指数介于0.59~1.13之间,表明新寨河表层水体中重金属的污染程度达到轻微污染水平。单种重金属元素的潜在生态危害系数计算结果显示,90.91%和9.09%的沉积物样点分别被归类为轻微风险和中等风险。所有样点沉积物的潜在生态危害指数介于14.57~120.55之间(均值为72.08),表明新寨河沉积物的潜在生态风险较低。Cu、As在多个样点存在污染现象,需予以重点监控管理。新寨河流域重金属的来源可分为三大类:Cd、Pb、Cr、Zn、Cu为第一类,对应地表径流源;As、Fe、Mn为第二类,对应煤矿开采源;Hg为第三类,对应复合源。     

高锰酸盐指数在 BOD 5 分析中的应用

在水质BOD5测定中 ,稀释倍数的选择是保证获得准确数据的重要步骤 ,《水和废水监测分析方法 (第 4版 )》介绍了地表水可从测得的高锰酸盐指数与一定系数的乘积求得稀释倍数。例如高锰酸盐指数为 5mg/L～ 1 0mg/L ,则系数为 0 2、0 3。但这一系数对污水处理厂经过处理的出水来说 ,并不适用。根据工作实践 ,高锰酸盐指数在 5mg/L～1 0mg/L之间时 ,系数应选择 0 4～ 0 8之间 ,方可获得最佳稀释倍数。实验结果见表 1。表 1　污水处理厂出水的分析结果处理系统 A组出水1994-0 3 -2 3 1994-0 4-13 1994-0 5 -2 5B组出水2 0 0 0 -0 7-19C组…     

氢化物发生—电加热石英管原子吸收法测定环境水样中痕量铅的研究

研究了将氢化物发生技术用于电加热石英管原子吸收法测定环境水样中痕量铅 ,讨论了最佳测定条件和干扰元素的消除。方法的线性范围为 0～ 2 5 ng/m l,检出限为 0 .48ng/ml,相对标准偏差小于 2 .5 % ,回收率在 95 %～ 116%之间。     

低浓度SO_2检测管的研制

通过对常见的几种检测管法的比较，筛选出灵敏度较高的亚硝基铁氰化钠法；同时筛选出载体为６０—８０目的素陶瓷，指示剂浓度为２０％。玻璃管内径为２．０—２．３ｍｍ，采气速度为０．３（Ｌ／ｍｉｎ），采样体积为１２Ｌ，以此条件进行实验．结果表明，检测管变色长度对应ＳＯ２浓度的相关性很好；变异系数均小于１１０％，检测的重现性较好。检测管的测定值与理论值的平均相对误差为５．０９％（＜±１５％），最大相对误差为７．１３％（＜±２５％），准确度较高．测定结果可靠；与化学法比较，两者无显著性差异；浓度小于０．１５ｍｇ／ｍ３的Ｈ２Ｓ及浓度小于０．０１ｍｇ／ｍ３的ＮＯ２对ＳＯ２检测管无干扰．     

Submicrometer elemental carbon as a selective measure of diesel particulate matter in coal mines

A monitoring method for diesel particulate matter was published as Method 5040 by the National Institute for Occupational Safety and Health (NIOSH). Organic and elemental carbon are determined by the method, but elemental carbon (EC) is a better exposure measure. The US Mine Safety and Health Administration (MSHA) proposed use of NIOSH 5040 for compliance determinations in metal and nonmetal mines. MSHA also published a rulemaking for coal mines, but no exposure standard was provided. A standard based on particulate carbon is not considered practical because of coal dust interference. Interference may not be a problem if an appropriate size-selective sampler and EC exposure standard are employed. Submicrometer dust concentrations found in previous surveys of nondieselized, underground coal mines were relatively low. If a large fraction of the submicrometer dust is organic and mineral matter, submicrometer EC concentrations would be much lower than submicrometer mass concentrations. Laboratory and field results reported herein indicate the amount of EC contributed by submicrometer coal dust is minor. In a laboratory test, a submicrometer EC concentration of 31 microg m(-3) was found when sampling a respirable coal dust concentration over three times the US compliance limit (2 mg m(-3)). Laboratory results are consistent with surveys of nondieselized coal mines, where EC results ranged from below the method limit of detection to 18 microg m(-3) when size-selective samplers were used to collect dust fractions having particle diameters below 1.5 microm-submicrometer EC concentrations were approximate 7 microg m(-3). In dieselized mines, submicrometer EC concentrations are much higher.     

毛细管柱气相色谱法测定环境空气中1,2-二氯乙烷

采用毛细管柱气相色谱法测定环境空气中的1,2-二氯乙烷,用活性碳吸附,二硫化碳解析,FID检测器分析.方法在0 mg/L～311mg/L范围内线性良好,当采样体积为20 L时,最低检出质量浓度为0.006 mg/m3,标准溶液平行测定的RSD≤2.2%,加标回收率为98.4%～101%.     

活性炭吸附-毛细管柱气相色谱法测定大气中吡啶

以活性炭吸附大气中的吡啶,用二硫化碳解析、毛细管柱分离、FID检测器分析,采用保留时间定性、峰面积外标曲线法定量。方法在0～367mg/L范围内线性关系良好,当采样体积为20L时,最低检出质量浓度为0.007mg/m3,标准溶液平行测定的RSD≤2.0%,加标回收率为97.9%～104%。     

高通量固定污染源废气颗粒物中总汞的测定

用玻璃纤维滤筒采集固定污染源废气颗粒物,借助硝酸和氢氟酸的作用,使滤筒和废气颗粒物在160℃下消解,再用原子荧光法测定消解液中总汞。用50%热硝酸溶液处理玻璃纤维滤筒,消除滤筒本底值不一对测定结果的干扰,并优化消解过程,使该方法在0.050μg/L~1.00μg/L范围内线性良好。当采样体积为10 L时,方法检出限为4.5×10~(-5)mg/m~3,空白加标样6次测定结果的RSD为7.2%,加标回收率为87.0%~113%。将该方法用于测定某固定污染源废气颗粒物中总汞,测定值在标准排放限值内。     

热分解-冷原子吸收法测定土壤中汞

采用热分解处理土壤样品,用冷原子吸收法测定样品中的汞,通过优化固体测汞仪的分析条件、确定校准曲线的线性范围和样品的称样量,使该方法在0.025 mg/kg~1.50 mg/kg范围内线性良好。当取样量为0.2 g时,方法检出限为0.000 9 mg/kg,有证标准物质的测定结果在保证值范围内,高、低浓度标准物质6次测定结果的RSD分别为4.6%和4.8%。用热分解法与国标法同时处理样品并测定,其测定结果无显著差别。     

Ion chemistry and individual particle analysis of atmospheric aerosols over Mt. Bogda of eastern Tianshan Mountains, Central Asia

Aerosol samples were collected during the scientific expedition to Mt. Bogda in July-August, 2009. The major inorganic ions (Na(?+?), NH??, K(?+?), Mg(2?+?), Ca(2?+?), Cl(?-?), SO2??, and NO??) of the aerosols were determined by ion chromatography. SO2??, NO??, and Ca(2?+?) were the dominate ions, with the mean concentrations of 0.86, 0.56, and 0.28 μg m?3, respectively. These mean ion concentrations were generally comparable with the background conditions in remote site of Xinjiang, while much lower than those in ürümqi. Morphology and elemental compositions of 1,500 particles were determined by field emission scanning electron microscopy equipped with an energy dispersive X-ray spectrometer. Based on the morphology and elemental compositions, particles were classed into four major groups: soot (15.1%), fly ash (4.7%), mineral particles (78.9%), and little other matters (0.8% Fe-rich particles and 0.5% unrecognized particles). Presence of soot and fly ash particles indicated the influence of anthropogenic pollutions, while abundance mineral particles suggested that natural processes were the primary source of aerosols over this region, coinciding with the ionic analysis. Backward air mass trajectory analysis suggested that ürümqi may contribute some anthropogenic pollution to this region, while the arid and semi-arid regions of Central Asia were the primary source.     

Assessment of vehicular pollution in Kolkata, India, using CALINE 4 model

Michigan water quality standards for public bathing beaches require local health departments to collect and analyze a minimum of three water samples for Escherichia coli during each sampling event. The geometric mean number of E. coli colonies is then compared to the 300 colonies per 100 ml standard to determine compliance. This article compares the results of the currently mandated procedure to a composite sampling method, whereby the three samples are mixed in equal volumes and analyzed once. This effectively replaces the geometric mean of the individual sample results with an arithmetic mean. Although arithmetic means are more affected by outliers, this sensitivity to high concentrations is more health conservative than the geometric mean. During the 2007 sampling season, nine bathing beaches were monitored once each week. Three individual point samples and a composite sample were analyzed for each sampling event. No statistically significant differences in bacteria concentrations were found between composite sample analysis and the arithmetic mean of individual point sample analyses. No violations were detected in the 2007 sampling season, so using historical data, a retrospective analysis was performed on samples gathered at nine bathing beaches in Kalamazoo County, Michigan during the years 2001–2007. The arithmetic mean of the three samples taken at each site served as a surrogate composite sample. The benefits of compositing the three samples were investigated assuming a 2/3 reduction in analytical costs. In the traditional sampling method, three individual samples were obtained and analyzed once in every 3-week period during the summer season, whereas compositing was simulated by taking the arithmetic mean of each week’s results. The results of this retrospective cost analysis indicates that ten to 14 violations would have been missed using the less frequent traditional sampling and analysis methodology. Composite sampling is a cost-saving alternative to traditional sampling techniques that can be more protective of public health, particularly when the savings are applied to increased numbers of samples in time or space.     

离子色谱法测定空气中氟化氢氯化氢和硫酸

以多孔玻板吸收管采样,采用离子色谱法同时测定作业场所空气中的氟化氢、氯化氢和硫酸,采样效率>92%。氟化氢在0 mg/L～2.00 mg/L、氯化氢在0 mg/L～2.50 mg/L、硫酸在0 mg/L～4.00 mg/L范围内线性良好,检出限分别为0.003 mg/m3、0.02 mg/m3、0.023 mg/m3(按采样体积60 L计),标准溶液平行测定的RSD≤8.0%,两个质量浓度水平加标的平均回收率为92.6%～106%。     

气相色谱法测定固定污染源废气中氯甲基甲醚和二氯甲基醚的研究

氯甲基甲醚(CMME)和二氯甲基醚(BCME)属于确认人类致癌物，因此，建立精准、绿色的CMME和BCME检测分析方法十分必要。基于2,4,6-三氯苯酚+乙醇钠+乙醇衍生化体系，利用气相色谱法(电子捕获检测器)测定了固定污染源废气中的CMME和BCME,并且系统地优化了采样条件、衍生化条件，确定了衍生化产物的结构及衍生比率。结果表明：工作曲线相关系数均大于0.990;当采样量为10 L时，检出限均为0.003 mg/m³;当实际样品加标量分别为0.010、0.100、1.00 mg/m³时，测定结果的相对标准偏差分别为15%～16%、8.9%～13%、10%～11%,加标回收率分别为89.2%～90.8%、75.3%～78.6%、76.5%～77.2%。