过氯乙烯滤膜采样—酸消解—钼蓝光度法测定磷酸才

建立了过氯乙烯滤膜采样－酸消解－钼蓝分光乐度法测定磷化车间磷酸雾的监测方法。实验室模拟采样的捕集效率为９５．７％～９９．１％，单个实验室对含５μｇ和１５μｇ样品进行多次测定，其相对标准差小５％，样品加标回收率为９８．２％～１００．５％，方法检测限为０．００７ｍｇ／ｍ＾３，对标样测定，结果均在给定值范围内，用该法与等离子发射光谱法（ＩＣＰ）对５个样品进行比对测定，结果均令人满意。     

测定废水中BOD_5技术问题探讨

测定废水中ＢＯＤ_５技术问题探讨王俊贤（广西柳州地区环境监测站，柳州５４５００２）１．快速测定ＣＯＤ的方法：加大重铬酸钾量（１５．０ｍｌ），用１：１浓硫酸－浓磷酸混合液作反应介质，使水样中有机物快速氧化，一个水样用３分钟回流时间，无需任何附加条件，与?..     

钼锑抗光度法测定鱼饲料中的总磷

研究了钼锑抗光度法测定鱼饲料中的总磷，采用鱼饲料样品经550～600℃高温前处理．选择了最佳显色还原剂的用量及显色还原温度和时间，方法的变异系数为1．8％～5．7％，回收率达98．0％～100．5％，最低检出浓度为0．5mg／kg.该方法操作简便，颜色稳定，灵敏度高．     

氮气吹出分离法测定氨化物

本工作对多级串联吹出分离法测定氰化物的可行性作了探讨。试验确定在磷酸－ＥＤＴＡ体系中用氮气吹出分离氰化氢的条件。一次可以同时处理四个样品，富集浓缩效率可达２０倍。标准水样试验结果的平均回收率为９５％，相对标准偏差为１．６—５．３％。环境水样测定结果本方法和标准方法基本相符．     

复合絮凝剂对工业废水氨氮测定的预处理

针对带色浊度高的工业废水中氨氮测定的预处理，提出了使用硫酸铝和聚丙烯酰胺复合絮凝沉淀法，试验结果表明，方法不仅具有操作简单，试剂用量少，絮凝效果好，去色，去浊度高，且对ｐＨ５－ｐＨ１０是各种带色浊度高的废水都能起到良好的效果，还能提高测定的精密度，其变异系数为１．５％－３．６％，回收率在９５％－１０４％之间，确保数据的准确和可靠。     

加热砷锑钼蓝杂多酸光度法测定水中痕量砷

本文采用单纯形最优化法探讨了加热显色砷锑钼蓝杂多酸的最佳条件，砷锑钼蓝杂多酸的最大吸收波长位于６９０ｎｍ，砷在０～５μｇ／２５ｍｌ范围内符合比耳定祁。方法灵敏、准确与简便，应用于水样痕量测的测定，结果满意．     

聚四氟乙烯高压密封罐消解样品测定五氧化二钒

利用聚四氟乙烯高压密封罐消解矿石样品测定五氧化二钒，具有操作手续相对简便、轻松、快捷等优点，与传统的硫酸－磷酸混合酸消解或采用碱熔融前处理法比较，相对误差小于１．６％，样品的添加标准回收率为９２．９％～１０３．５％。     

L-半胱氨酸对氢化物发生原子吸收法测定砷增强信号作用的研究

将生化试剂Ｌ－半胱氨酸用于砷氢化物发生体系，在ｐＨ１．７～２．０，Ｌ－半胱氨酸用量大于１．５ｍ ｇ／ｍ ｌ时，Ｌ－半胱氨酸的存在使砷信号增强最大，该条件下使砷检出限低了２．６ 倍，水样加标加收率为９６％ ～９８．８％ ，应用于自来水和地表水中痕量砷的测定，获得了满意的结果。     

恒电流库仑滴定法测定铬渣中的铬（Ⅵ）

铬渣样品以（１＋１０）磷酸溶液加热消解１．５ｈ，可得到完全澄清的消解液。采用恒电流库仓滴定法测定消解液中的Ｃｒ（Ⅵ），测得值（１．６４％）与标样参考值（１．７％）接近，准确度高，相对标准偏差为０．９８％。适于铬渣中Ｃｒ（Ⅵ）的日常监测。     

用钼兰法定量微量磷

1.前言 有磷酸离子存在的溶液呈酸性,如果在溶液中加入钼酸铵,就生成钼磷酸,若将其还原为兰色物质,就生成钼兰。这是一个古老的反应,因可用来定量微量磷酸离子,故对其反应机制和反应条件已进行过众多研究。例如,下式所示为钼磷酸生成反应: XH_3PO_4+YM_o(Ⅵ)=MoP+ZH~+ 钼磷酸的生成速度与H_3PO_4浓度的X倍,     

A new catalytic oxidation method for sensitive quantification of bromate in flours and bottled water using AgNPs

In this paper, a simple and sensitive spectrophotometric method for the determination of nanomolar level of bromate, based on the catalytic effect of silver nanoparticles on the oxidation of acid red 14 by potassium bromate, is described. The reaction rate was monitored spectrophotometrically by measuring the decrease in absorbance of acid red 14 at 516 nm. The detection limit of the method was 8 ng/mL, and the linear range was between 15 and 130 ng/mL. The effects of acidity, concentration of reactants and reaction time, and external ions were also discussed. The optimum reaction conditions were fixed, and some kinetic parameters determined. The relative standard deviation for the determination of bromate at the concentration of 50 ng/mL was calculated to be 0.996 % (n?=?10). The method has been successfully applied to the determination of bromate in flours and bottled waters.     

电感耦合等离子体原子发射光谱法测定废气中的铅方法研究

以石英纤维滤筒采样，采用硝酸一氢氟酸消解体系，建立了电感槌合等离子体原子发射光谱法测定废气中铅分析方法。研究了仪器工作条件、方法的干扰和消除因素，探讨了空白实验对分析结果的影响；在选定的最优条件下。铅标准曲线的线性相关系数为0．9999；检出限为0．010mg／L；平均相对标准偏差为2．8％；加标回收率为97．8％～104％。与国家标准方法相比，本方法准确可靠，检测限更低，灵敏度更高，线性范围更宽，可用于废气中铅的含量测定。     

土壤重金属元素检测国际实验室比对研究

IERM和CNAS合作组织开展了亚太实验室合作组织(APLAC)能力验证计划"APLAC T066土壤重金属元素检测",其目的是评价参加实验室定量分析土壤重金属元素总量的能力。研究所用的能力验证样品为IERM研制的土壤标准样品。结果表明,参加实验室检测土壤砷、铜、汞、镍、铅和锌的结果满意率分别为85.7%、95.8%、77.1%、83.3%、93.5%和91.7%。样品消解过程加入氢氟酸时,铅和锌的检测结果与标准值更加接近,说明检测土壤重金属元素总量时氢氟酸的加入非常关键。文章还对比对实验室结果评价的统计方法进行了探讨。     

二氯甲烷萃取与气相色谱—质谱结合新方法测定饮用水源地水中的苦味酸

为建立饮用水源地中苦味酸分析测定的新方法,将10 ml水样中的苦味酸氯化后,以二氯甲烷萃取,用气相色谱—质谱法(GC—MSD)测定水中苦味酸的含量,采用保留时间定性,外标法定量。结果表明,最佳萃取时间为4 min,最佳萃取剂用量为1.5 ml,该法能快速而有效的提取并测定水中苦味酸,检出限低(0.4μg/L)、精密度(RSD=1.8%)和准确度高(加标回收率93.16%)、标准曲线线性(r=0.999)较好,能满足饮用水源地水中苦味酸的测定要求。     

A gas-phase biosensor for environmental monitoring of formic acid: laboratory and field validation

In order to encourage more exposure measurements to be performed, a formic acid gas-phase biosensor has been developed for this purpose. In the present paper, an enzyme based biosensor has been validated with respect to analyte selectivity and on-site use. To ensure that the sampler developed measures the compound of interest the biosensor was exposed to three near structural homologues to formic acid, i.e. acetic acid, methanol and formaldehyde. These vapours were generated with and without formic acid and the only compound that was found to have an effect on the performance of the biosensor, albeit a small one, was acetic acid. The field test was performed in a factory using formic acid-containing glue for glulam products. In parallel to the measurements with the biosensor a well defined reference method was used for sampling and analysing formic acid. It was found that the biosensor worked satisfactorily in this environment when used in a stationary position. It was also shown that the biosensor could determine formic acid vapour concentrations down to 0.03 mg m(-3).     

气相色谱-质谱法测定废酸油渣中的16种多环芳烃

建立了废酸油渣中16种多环芳烃超声萃取、Florisil萃取柱净化、气相色谱-质谱测定的方法。笔者对提取方式、提取剂类型和体积、提取时间和次数、净化方式等进行研究,采用无水硫酸钠分散,二氯甲烷作为提取剂超声40 min,提取液经纯水清洗、离心后取适量有机相经过3 g Florisil萃取柱净化,采用气相色谱-质谱选择离子模式(SIM),加入内标进行定量分析。结果表明:二氯甲烷提取效率比正己烷好,丙酮可能引起酸性样品中多环芳烃的降解,丙酮超声萃取时加入无水硫酸钠能在一定程度上防止目标物降解,但萃取效率不可控制,宜采用二氯甲烷作为萃取剂。分散提取能有效减少提取时间,超声清洗仪超声40 min提取效率为86.2%～104%。3g Florisil萃取柱净化比1 g Florisil萃取柱净化和GPC净化效果略好。方法检出限为0.4～1.3 mg/kg,6次空白加标的相对标准偏差为2.3%～15.3%,6个实际样品测定结果的相对标准偏差为1.2%～27.3%,基体加标回收率为51.3%～126%,连续校准稳定。该方法适用于废酸油渣样品中16种多环芳烃的检测,比直接溶解有效,比加速溶剂萃取、索氏提取、微波萃取和超声探头萃取简单、快捷,能有效减少设备污染和腐蚀,净化方法有效,测定结果准确可靠,是实现大批量样品检测的可行方法。     

长江入海口北岸单站降水组分10年变化状况探讨

分析2001—2010年南通市区城中子站降水监测点位数据,得出降水中起致酸作用的阴离子硫酸根、硝酸根、氟离子和氯离子中除硝酸根呈现显著性上升趋势,其余上升趋势不明显;氯离子、钠离子与降水量存在高度线性负相关,硫酸根、硝酸根与降水量分别为低度非线性负相关和正相关,其他项目与降水量为显著性非线性负相关;将pH分5级,pH<4.7为重酸雨频率,pH4.7～5.0为较重酸雨频率,pH5.0～5.3为中度酸雨频率,pH5.3～5.6为轻度酸雨频率,pH≥0.56为非酸雨频率,其结果表明:南通市区2009、2010年酸雨频率降低,分别为44.1%和38.2%,主要是重酸雨频率减少,非酸雨频率增加;2003、2007年酸雨频率升高,分别为67.4%和69.8%,主要是重酸雨频率增加,非酸雨频率减小;降水量大小与电导率浓度高低没有对应性;阴阳离子浓度总量逐年、逐月同步变化;阴离子中硫酸根、硝酸根浓度逐年、逐月变化量与幅度较大;阳离子中钙离子、铵离子浓度逐年、逐月变化量与幅度较大;阴阳离子浓度逐年、逐月占比呈准对称形。     

2009—2017年南充市城区酸雨特征分析

为了更为有效地治理酸雨污染,根据南充市环境监测中心站提供的2009—2017年降水监测数据,对南充市城区酸雨污染情况进行了分析及源解析。结果表明:2009—2017年,南充市降水pH从4.60波动上升至5.6以上,酸雨频率波动下降,酸雨污染情况有所改善;[SO4^2-]/[NO3^-]从4.92下降至0.86,酸雨污染类型从硫酸型转变为硝酸-硫酸型。同时,对比分析2014—2016年大气污染物排放源可知,NOx排放源中,工业污染源占比由14%降至11%,生活污染源由2%上升至5%;SO2排放源中,工业污染源占比由62%降至43%,生活污染源由38%上升至57%,表明南充市SO2污染已从以工业污染源为主转变为工业污染源与生活污染源并重。     

Heavy metal concentrations in water and sediments in Tasik Chini, a freshwater lake, Malaysia

The purpose of this paper are to determine the concentration of heavy metals namely cadmium (Cd), copper (Cu) and lead (Pb) in water and sediment; and to investigate the effect of sediment pH and sediment organic matter on concentration of cadmium, copper and lead in sediment at oxidation fraction. For this purpose the concentration of heavy metals were measured in water and sediments at 15 sites from Tasik Chini, Peninsular Malaysia. The sequential extraction procedure used in this study was based on defined fractions: exchangeable, acid reduction, oxidation, and residual. The concentration of heavy metals in residual fraction was higher than the other fractions. Among the non-residual fractions, the concentration of heavy metals in organic matter fraction was much higher than other fractions collected from all sampling sites. The pH of the sediment in all sites was acidic. The mean pH ranges from 4.8 to 5.5 with the higher value observed at site 15. Results of organic matter analysis showed that the percentage of organic matter present in sediment samples varies throughout the lake and all sites of sediments were relatively rich in organic matter ranging from 13.0% to 34.2%. The highest mean percentage of organic matter was measured at sampling site 15, with value of 31.78%.     

On-line solid phase extraction with polyurethane foam: trace level spectrophotometric determination of iron in natural waters and biological materials

This paper reports the development of a simple and accurate on-line procedure for preconcentration and determination of dissolved iron in waters and biological materials using unloaded polyether-type polyurethane foam as solid extractor. In the developed flow injection system, the analyte was preconcentrated from acidic aqueous medium as iron-thiocyanate complex with post-elution with ascorbic acid solution and spectrophotometric measurement with 1,10-phenanthroline as colorimetric reagent. In order to improve the performance of the system several chemical and flow variables were investigated as well as the effect caused by the presence of possible interferents. The method was validated by the analysis of two certified reference materials. Application of the methodology was carried out by the determination of dissolved iron content in eight natural water samples with different characteristics. The results were compared with those obtained by electrothermal atomic absorption spectrometry (ETAAS) and no statistical difference was observed. The detection limit was 0.75 microgram l-1 and the RSD was 1.2% for 2 min preconcentration time. At this condition, a productivity of 20 samples h-1 was achieved. Increasing the preconcentration time up to 3 min, a detection limit of 0.45 microgram l-1, an RSD of 1.5% and an analytical throughput of 15 h-1 were verified.