水质丁基黄原酸测定难点探讨

丁基黄原酸是水质监测的重要项目之一。水中丁基黄原酸的测定,在样品采集保存、前处理及仪器分析各阶段都存在一定的技术难点。实际分析时很容易出现测定结果不理想,甚至定性定量错误等问题。结合实验对丁基黄原酸测定中容易出现的问题及注意事项进行探讨,正确区分丁基黄原酸及其盐,有效保存样品,采用低损失的前处理方法以及选择性好的分析仪器,有利于提高丁基黄原酸测定的准确性。众多丁基黄原酸测定方法中,液相色谱质谱法、离子色谱法以及液相色谱法在选择性和灵敏度方面更具优势,也可用于其他方法检出丁基黄原酸时对测定进行确认。     

废干电池铜帽中铜锌分离与回收

本文研究了一种回收废干电池铜帽中Cu、Zn的有效方法．此方法是利用锌粉还原酸溶解后溶液中的Cu^2＋形成海绵铜，其纯度达到85％，铜帽中Cu的回收率达96％．沉淀Cu后的溶液经进一步处理可制备出ZnO，纯度达97％以上．     

吹扫捕集-气相色谱-质谱法测定水中痕量丁基黄原酸

建立了吹扫捕集-气相色谱-质谱联用测定水中丁基黄原酸的方法.丁基黄原酸在酸性条件下分解成易挥发的二硫化碳,经吹扫捕集富集后用气相色谱分离质谱定量测定.与传统的分光光度法相比,更简便快捷,在0.25～10.0μg/L范围内线性良好,准确度高,添加回收率为98.3％～105％,精密度好,相对标准偏差为5.92％ ～ 10.7％,方法检出限为0.07μg/L.与顶空法相比,灵敏度更高.     

顶空-气相色谱-质谱法测定水中痕量丁基黄原酸

建立了顶空-气相色谱-质谱联用测定水中丁基黄原酸的方法。丁基黄原酸在酸性条件下分解成易挥发的二硫化碳,可用顶空-气相色谱分离、质谱定量测定。与传统的分光光度法相比,该法简便、快捷,在0.010～1.00 mg/L范围内线性良好,准确度高,加标回收率为95.1%～100.6%,精密度好,相对标准偏差为3.1%～6.5%,方法检出限为0.002 mg/L,适用于水中丁基黄原酸的监测。     

超高效液相色谱-质谱法直接进样测定水中草甘膦和丁基黄原酸

通过优化色谱条件、稀释样品、加入氨水等措施,建立了超高效液相色谱-质谱法直接进样分析地表水及自来水中草甘膦和丁基黄原酸的方法。草甘膦和丁基黄原酸在各自线性范围内线性关系良好,相关系数(R2) 0. 999。方法检出限分别为5. 20(前处理中对样品进行了20倍稀释)和0. 08μg/L,远低于国家标准限值要求。草甘膦和丁基黄原酸的加标回收率分别为73. 8%～92. 3%和85. 0%～113. 0%,样品间的标准偏差均10%,准确度和精密度均满足质控要求。该方法简化了样品前处理过程,成功降低了基质效应对草甘膦和丁基黄原酸测定的干扰。     

巯基棉富集分离铜试剂─吐温─80—OP水相光度法测定水中微量铜

研究了在非离子表面活性剂吐温－８０和乳化剂ＯＰ存在下，于ｐＨ８．５缓冲介质中，铜（Ⅱ）与铜试剂显色反应条件。结果表明：配合物的最大吸收波长为４５３ｎｍ，表观摩尔吸光系数为１．５４×１０４Ｌ·ｍｏｌ－１．ｃｍ－１，铜（Ⅱ）含量在０～７０μｇ／２５ｍｌ范围内符合比耳定律。该法与巯基棉富集分离相结合，应用于天然水及废水中微量铜的测定，结果满意。     

人发中微量铜的催化光度法测定

本文报道了一种新的测定铜(Ⅱ)的高选择性和高灵敏度的催化光度分析法.基于在氨水介质中,曙红Y与H_O_2的氧化还原反应受铜(Ⅱ)催化使曙红Y褪色,据此建立的测定铜(Ⅱ)的新方法的检出限为3×10~(-10)g/ml,该法用于人发、指甲样品中铜(Ⅱ)的测定,相对标准偏差为5％～6％,加标回收率为88％～114％.     

高效液膜分离富集测定微量铜

应用高效乳状液膜技术分离、富集水和土壤样品中微量铜（Ⅱ）．研究了流动载体（Ｐ２０４）、表面活性剂（ＳＰａｎ８０）、膜的增强剂（液体石蜡）、膜溶剂（煤油）和内相解吸剂（２．５ｍｏｌ／ＬＨ２ＳＯ４）等液膜体系，对分离富集微量铜（Ⅱ）的影响．确定了Ｓｐａｎ８０—Ｐ２０４─液体石蜡─煤油─Ｈ２ＳＯ４高效液膜体系的最佳组成和最适宜的实验条件．富集后的溶液用１－（２－吡啶偶氮）－２－萘酚（ＰＡＮ）分光光度法测定铜（Ⅱ）．用本法富集水和土壤中微铜（Ⅱ）．回收率在９９％以上。应用于测定水和土壤中的微量铜．相对标准偏差为１．２％～４．５％。     

4—（H—酸偶氮）—1—苯基—3—甲基吡唑酮光度法测定铜的研究及应用

合成了新试剂４－（Ｈ－酸偶氮）１－苯基－３－甲基吡唑酮（ＨＰＭＰ）,研究了其和铜的显色反应。在ｐＨ＝７的ＮＨ４Ａｃ缓冲介质中,ＣＴＭＡＢ存在下,ＨＰＭＰ与Ｃｕ（Ⅱ）生成２∶１紫色络合物,λｍａｘ＝５８０ｎｍ,ε＝５．６８×１０４Ｌ·ｍｏｌ－１·ｃｍ－１。铜含量在０～０．６ｍｇ／Ｌ内符合比耳定律。方法用于水样和生物样品中铜的测定,结果令人满意。     

超高效液相色谱-质谱法测定地表水中丁基黄原酸

建立了直接测定水中丁基黄原酸的超高效液相色谱-电喷雾串联四极杆质谱法,无需对水样进行富集,水样过滤后就可直接测定。该方法简单、快捷、灵敏度高,方法检出限可达0.2μg/L。     

Air formaldehyde and solvent concentrations during surface coating with acid-curing lacquers and paints in the woodworking and furniture industry

An investigation of contemporary exposure to formaldehyde and organic solvents has been carried out during surface coating with acid-curing lacquers and paints in the Norwegian woodworking and furniture industry over a period of 3 years. The investigation covered 27 factories of different sizes and with different types of production, and totally 557 parallel formaldehyde and solvent samples were collected. The formaldehyde concentration (geometric mean) was 0.15 ppm (range 0.01-1.48 ppm) with about 10% of the samples exceeding the Norwegian occupational exposure limit of 0.5 ppm. The solvent concentration as additive effect (geometric mean) was 0.13 (range 0.0004-5.08) and about 5% of the samples exceeded the Norwegian occupational exposure limit. The most frequently occurring solvents from acid-curing lacquers were n-butyl acetate, ethanol, ethyl acetate and 1-butanol, which were found in 88-98% of the samples. Toluene, n-butyl acetate and 1-butanol were the only solvents with maximum concentrations exceeding their respective occupational exposure limits. Curtain painting machine operators were exposed to the highest concentrations of both formaldehyde (geometric mean 0.51 ppm, range 0.08-1.48 ppm) and organic solvents (additive effect, geometric mean 1.18, range 0.02-5.08). Other painting application work tasks such as automatic and manual spray-painting, manual painting and dip painting, showed on average considerably lower concentrations of both formaldehyde (geometric means 0.07-0.16 ppm) and organic solvents (additive effect, geometric mean 0.02-0.18). Non-painting work tasks also displayed moderate concentrations of formaldehyde (geometric means 0.11-0.17 ppm) and organic solvents (additive effect, geometric mean 0.04-0.07).     

Occupational exposure to airborne solvents during nail sculpturing

This study describes occupational exposure to acrylates and other solvents during nail sculpturing, including comparative measurements of the exposure using four different sculpturing methods: The acrylic method, the UV-gel method, the acrylic powder method and the resin method. Thirty-two nail technicians working in 22 different salons participated in the study. In total, 92 measurements were performed, comprising 70 solvent measurements and 22 measurements of ethyl 2-cyanoacrylate. The solvents most frequently present in all samples were acetone, ethyl acetate, toluene and n-butyl acetate, measured in 96%, 94%, 91% and 81% of the samples, respectively. The study shows that the overall solvent exposure was low, with all measurements calculated as the additive effect (n = 70) below 20% of the OEL (arithmetic mean 0.06 and range 0.01-0.19). No statistically significant difference between sculpturing methods were observed (p = 0.05).     

甲萘酚显色光度法测定水中苯胺

对甲萘酚偶氮显色光度法测定水中苯胺的方法进行了验证性研究。结果表明,该方法具有简单、快速、稳定等优点。线性区间在0.05～5.5mg/L范围内,相关系数等于0.9997,苯胺浓度小于0.05mg/L或大于5.5mg/L时,测量误差比较大。还考察了NaCl、KCl、NaNO_3、KNO_3、Na_2SO_4、K_2SO_4、TiO_2、ZnO,苯酚,以及由吐温-80/苯/水/正丁醇组成的O/W微乳液对测量的影响。     

Statistical approaches for hydrogeochemical characterization of groundwater in West Delhi, India

Parametric statistical approaches, correlations and multiple linear regressions were used to develop models for the interpretation of hydrogeochemical parameters in the Western part of Delhi state, India. The hydrogeochemical parameters indicated that the groundwater quality is not safe for consumption. The water is moderately saline and the salinity level is increasing over time. There is also the problem of nitrate pollution. The correlation between electrical conductivity (EC) and other water quality parameters except potassium (K(+)), nitrate (NO(3)(-)) and bicarbonate (HCO(3)(-)) is significantly positive and Ca(++)+ Mg(++)/Na(+)+ K(+) is significantly negative. In predicting EC, the multiple R(2) values of 0.996 and 0.985 indicate that 99.6% and 98.5% variability in the observed EC could be ascribed to the combined effect of Na(+), HCO(3)(-), Cl(-), SO(4)(--), NO(3)(-) and Ca(++)+ Mg(++) for the year of 2005 and 2006 respectively. Out of 99.6% of the variability in EC in 2005, 51.2% was due to Cl(-) alone, and 8.5%, 12.5%, 6.1%, 14.7% and 6.7% were due to Na(+), HCO(3)(-), SO(4)(--), NO(3)(-) and Ca(++) + Mg(++). Similarly in 2006, out of 98.5% of the variability in EC, 48.5% was due to Cl(-) alone, and 10.4%, 12.7%, 5.3%, 17.2% and 4.4% were due to Na(+), HCO(3)(-), SO(4)(--), NO(3)(-) and Ca(++)+ Mg(++). The analysis shows that a good correlation exists between EC, Cl(-) and SO(4)(--) either individually or in combination with other ions and the multiple regression models can predict EC at 5% level of significance.     

顶空气相色谱法在测定水中三氯乙醛的应用

研究以DB-624交联石英毛细管柱分离,微电子捕获检测器-顶空气相色谱法测定水中三氯乙醛的应用,与以往的方法相比,准确可靠、省工省时省试剂,符合"绿色分析化学"的要求。最低检出限为0.2μg/L,标准偏差为0.028μg/L,相对标准偏差为6.0%,加标回收率为88.7%～109%。     

基于Berthollet反应示波极谱法测定水中微量氨

在亚硝基铁氰化钾存在下,氨在氢氧化钠介质中与苯酚、次氯酸钠反应,其产物靛酚在滴汞电极上产生－灵敏的吸附波,ＮＨ３－Ｎ在０．００３～０．２２ｍｇ／Ｌ内,导数峰电流与其呈良好的线性关系。用于环境水中ＮＨ３－Ｎ的测定,其相对标准偏差小于３％,回收率为９７％～１０５％,方法具有较好的选择性。     

Near-surface ozone levels and trends at rural stations in France over the 1995–2003 period

There is a considerable interest in quantifying near-surface ozone concentrations and associated trends, as they serve to define the impacts on ozone of the anthropogenic precursors reductions and to evaluate the effects of emission control strategies. A statistical test has been used to the ozone air concentrations measured in the French rural monitoring network stations, called MERA, in order to bring out spatio-temporal trends in air quality in France over the 1995-2003 period. The non-parametric Mann-Kendall test has been developed for detecting and estimating monotonic trends in the time series and applied in our study at annual values: mean, 98th percentile and median based on hourly averaged ozone concentrations and applied to daily maxima. In France, when averaged overall 9 stations between 1995 and 2003, a slight increasing trend of the O(3) levels (+0.6 +/- 1.3% year( - 1)) is observed, which is strongly influenced by the concentrations of the high altitude stations. In stations below 1000 m a mean rate of -0.48% year( - 1) from annual average concentrations, of -0.45% year( - 1) for medians and of +0.56% year( - 1) for P.98 over the 1995-2003 period were obtained. In stations above 1,000 m a mean rate of +1.75% year( - 1) from annual averages values, of +4.05% year( - 1) for medians and of +2.55% year( - 1) for P.98 were calculated over the 1997-2003 period. This situation is comparable to the one observed in other countries. In Europe and in France a reduction of precursor emissions is observed whereas a slight increasing trend of the O(3) levels is observed over the 1995-2003 period. One reason is the non-linearity of chemical ozone production with respect to precursor emissions. Possible explanations are an increase in near-surface ozone values caused by a reduced ozone titration by reduced NO( x ), the meteorological parameters change, an increase in bio-geogenic compound concentrations, the intercontinental transport from North America and Asia and the influence of stratospheric-tropospheric exchanges. These possible explanations must be interpreted carefully as on the short time scales considered.     

Speciation and sources of atmospheric aerosols in a highly industrialised emerging mega-city in central China

Monitoring air quality in large urban agglomerations is the key to the prevention of air pollution-related problems in emerging mega-cities. The city of Wuhan is a highly industrialised city with >9 million inhabitants in Central China. Simultaneous PM10 sampling was performed during 1 year at one urban and one industrial site. Mean PM10 daily levels (156 microg m(-3) at the urban site and 197 microg m(-3) at the industrial hotspot) exceed the US-EPA or EU annual limit values by 3-4 times. A detailed study of daily speciation showed that the mean chemical composition of PM10 presents minimal differences between peak and low PM episodes. This implies that PM10 aerosols in the study area result from local emissions, and air quality management and abatement strategies in Wuhan should thus focus on local anthropogenic sources. The levels of some elements of environmental concern are relatively high (409-615 ngPb m(-3), 66-70 ngAs m(-3), 116-227 ngMn m(-3), 10-12 ngCd m(-3)) due to industrial, but also urban emissions. Principal component analysis identified a mineral source (probably cement and steel manufacture) and smelting as the main contributors to PM10 levels at the industrial site (34%), followed by a coal fired power plant (20%) and the anthropogenic regional background (16%). At the urban site the major PM10 source is a mixed coal combustion source (31%), followed by the anthropogenic regional background (28%) and traffic (16%).     

南通市PM2.5中水溶性离子季节分布特征

对南通市2016年12月-2018年10月大气污染季节分布特征进行了分析。结果表明,南通市ρ(PM2.5)和ρ(水溶性离子)为冬、春季高,夏、秋季低。春夏秋冬四季ρ(水溶性离子)占ρ(PM2.5)百分比分别为68.2%,70.6%,64.5%和74.5%,其中二次离子SNA(NO3-、SO42-和NH4+)占ρ(PM2.5)的百分比分别为63.1%,67.0%,59.3%和66.8%;ρ(NO3-)/ρ(SO42-)表明,移动源已成为南通市春、秋、冬季的主要污染源,四季均存在不同程度的二次转化,且SO2的转化率均大于NO2,NO2冬季转化率最大、夏季最小,SO2夏季转化率最大、秋季最小。南通市NO2转化为硝酸盐的主要形式是气相均相反应,非均相反应和均相反应对SO2转化为硫酸盐的贡献差异不大。     

TOA—苯体系萃取分离—原子吸收法测定环境水样中铬（Ⅲ）和铬（Ⅵ）

研究了三正辛胺（ＴＯＡ）－茉体系对Ｃｒ（Ⅲ）和Ｃｒ（Ⅵ）的选择性萃取作用,在硫酸介质中可将水相中的Ｃｒ（Ⅵ）萃取到有机相里,而Ｃｒ（Ⅲ）仍留在留在水相中,用原子吸收法（ＡＡＳ）测定可求得Ｃｒ（Ⅲ）和Ｃｒ（Ⅵ）的含量,回收率分别为９４％￣１０５％和９４％￣１０４％。方法简单、快速、准确。