AAS与ICP－AES间接测定天然水中硫酸盐

本文以与过量形成ＢａＳＯ＿４沉淀反应为基础，较详细地讨论了反应条件、从而拟定了用ＡＡＳ和ＩＣＰ－ＡＥＳ间接测定天然水中的方法、确定了方法的精密度，ＡＡＳ法的ＲＳＤ％为１．５，ＩＣＰ－ＡＥＳ法为３．２．两种方法对比分析的结果接近，误差为１．０％（相对）。用于天然水中的测定，获得满意的结果。     

在线衍生化吹扫捕集-气相色谱/质谱分析水中的五氯酚

建立了通过乙酸酐衍生化-吹扫捕集-气相色谱／质谱分析水中五氯酚的新方法，探讨了吹扫时间、样品池温度、离子强度以及衍生化试剂的加入量等条件对捕集效果的影响。结果表明：采用吹扫时间25min、样品池温度60℃、离子强度20％氯化钠以及衍生化试剂的量200μl等条件对水中的五氯酚有较好的捕集效果，用于水中五氯酚的测定，结果满意。     

军用浸渍活性炭中银含量测定方法——火焰原子吸收分光光度法

本研究建立了一种用空气-乙炔火焰原子吸收分光光度法测定浸渍活性炭中银含量的分析方法，对酸介质浓度、共存元素的干扰进行了探讨，在0—1．0ml沪范围内，银含量与吸光度呈线性关系，相关系数为0．9999。对09型浸渍活性炭标准物质进行测定，测定结果的相对标准偏差为0．191％（n=10），加标回收率为97．5％-101．4％。     

Increase in Hair Lead, but not Blood Lead Content of Occupationally-Exposed Workers

This study attempted to investigate whether increased hair lead concentrations due to environmental exposure are accompanied by parallel increases in blood lead concentrations. A sample set consisting of both occupationally-exposed individuals and persons from the general population was investigated. The lead content of scalp and pubic hair from the general population (n=189), traffic police personnel (n=27) and battery workers (n=22) were analysed. The hair samples were taken from the nape of the neck by cutting 23 cm closest to the scalp and cleaned using a washing procedure developed in our laboratory. The effectiveness of the washing procedure was partly determined by examining the scanning electron micrographs of the hair samples. Venous samples of blood were taken from each volunteer's arm.The traffic police and battery plant operators sampled had significantly higher average scalp hair and pubic hair lead levels than the non occupationally-exposed general population. No significant differences were found between the blood lead values of these workers and the general population. Compared to the general population both occupationally-exposed groups had significantly more symptoms of lead toxicity.Lead particles were still observed on the hair shafts after the washing procedure. The amount of such lead contamination was difficult to quantify, the problem being further exacerbated by the difference in hair texture of the persons sampled. This exogenous contamination therefore detracts from the usefulness of hair as an indicator of lead exposure.     

Analysis of trace dicyandiamide in stream water using solid phase extraction and liquid chromatography UV spectrometry

An improved method for trace level quantification of dicyandiamide in stream water has been developed. This method includes sample pretreatment using solid phase extraction. The extraction procedure (including loading, washing, and eluting) used a flow rate of 1.0 mL/min, and dicyandiamide was eluted with 20 mL of a methanol/acetonitrile mixture (V/V = 2:3), followed by pre-concentration using nitrogen evaporation and analysis with high performance liquid chromatography–ultraviolet spectroscopy (HPLC–UV). Sample extraction was carried out using a Waters Sep-Pak AC-2 Cartridge (with activated carbon). Separation was achieved on a ZIC^®-Hydrophilic Interaction Liquid Chromatography (ZIC-HILIC) (50 mm × 2.1 mm, 3.5 μm) chromatography column and quantification was accomplished based on UV absorbance. A reliable linear relationship was obtained for the calibration curve using standard solutions (R² > 0.999). Recoveries for dicyandiamide ranged from 84.6% to 96.8%, and the relative standard deviations (RSDs, n = 3) were below 6.1% with a detection limit of 5.0 ng/mL for stream water samples.     

气相分子吸收光谱法测定氨氮校准曲线斜率、截距参考值研究

主要阐述了气相分子吸收光谱法测定氨氮的校准曲线斜率、截距参考值的分析.文章收集了临安市环境监测站实验室自2012年以来气相分子吸收光谱法氨氮校准曲线制作的一系列原始数据,并通过数理统计方法对校准曲线、残余标准偏差、斜率扩展不确定度、截距扩展不确定度开展了详细讨论,得出气相分子吸收光谱法氨氮校准曲线截距a值、斜率b值实验室参考值.此结果对实验室分析人员判定氨氮项目校准曲线制作是否合格具有一定的参考价值.     

高效液相色谱-电感耦合等离子体质谱联用测定生物样品中的有机汞

建立了酸提取-高效液相色谱-电感耦合等离子体质谱联用技术(HPLC-ICP-MS)测定生物样品中甲基汞、乙基汞、苯基汞等3种有机汞的分析方法。鱼肉和贝类样品经盐酸消解,苯萃取,硫代硫酸钠溶液反萃取后,采用醋酸铵/L-半胱氨酸缓冲盐及甲醇体系组成的流动相按一定比例进行梯度洗脱,经前处理的生物样品在液相色谱中经C18柱分离后,进入电感耦合等离子体质谱检测其甲基汞、乙基汞和苯基汞的浓度。3种有机汞化合物均在0.50~50.0μg/L范围内呈现良好的线性关系,线性相关系数(r)均大于0.9998。方法检出限为0.010~0.038mg/kg;3种有机汞样品加标的RSD均小于12.2%;两个水平的加标回收率在50.8~129%。     

捕集阱顶空-气相色谱/质谱法检测地表水中25种挥发性有机物

建立了捕集阱顶空-气相色谱/质谱法检测地表水中25种挥发性有机物的分析方法。采用正交实验设计对捕集阱顶空条件进行了优化,该方法相关系数0.995,加标回收率为90%~110%,方法检出限为0.08~0.39μg/L,相对标准偏差(n=7)为0.7%~4.8%,仪器检出限低于0.04μg/L。方法准确度和灵敏度较好,可以满足对地表水中25种挥发性有机物的检测要求。