石墨炉原子吸收法测定水中铊的方法改进

采用石墨炉原子吸收法测定水中铊,对样品前处理的多个细节进行改进,使前处理过程耗时缩短,回收率提高。试验表明,方法在0μg/L ～50．0μg/L范围内线性良好,相关系数r为0．9995;检出限为2．0μg/L,取样量为500 mL,富集50倍时,方法检出限为0．04μg/L;实际水样测定结果的 RSD 为4．9％～8．4％;实际样品的加标回收率为94．0％～102％。     

水中乙醛和丙烯醛分析方法的对比

对测定水中乙醛和丙烯醛的3种方法——2,4-二硝基苯肼衍生化法、顶空气相色谱法和吹扫捕集一气相色谱质谱法进行概述和总结,并对各方法的试验条件、方法原理、测定影响因素以及效能验证等分析、比对,突出表现各自的优势和特点。用3种方法同时测定实际水样,结果无显著差异,精密度、准确度满足监测要求。     

气相色谱-质谱法测定饮用水中消毒副产物卤代腈

采用顶空加盐气相色谱-质谱法检测饮用水中的消毒副产物氯乙腈、二氯乙腈和三氯乙腈,并对样品前处理方法及GC/MS仪器条件进行优化,使得3种卤代腈在5．00μg/L ～80．0μg/L 范围内线性良好,方法检出限分别为2．52μg/L、1．02μg/L和1．57μg/L。空白水样的加标回收率为75．9％～94．1％, RSD为3．6％～6．2％。     

顶空固相微萃取-气相色谱法测定水中氯苯类化合物

采用顶空固相微萃取（HS －SPME）技术萃取水中6种氯苯类化合物,全面分析对目标物萃取效率的影响因素,并确定萃取试验的最佳条件。用顶空固相微萃取联合气相色谱法（HS －SPME －GC）测定水中6种氯苯类化合物,方法在0.500 ng／L～2.00×10^5 ng／L范围内线性良好,检出限为0.05 ng／L ～2000 ng／L,空白样品加标回收率为69.8％～121％, RSD为4.8％～18.3％。用该方法测定实际水样,平行双样的相对偏差低于20％。     

气相色谱-高分辨双聚焦磁质谱测定水中超痕量多氯萘

采用固相萃取法处理水样,气相色谱-高分辨双聚焦磁质谱法测定水中超痕量多氯萘,同位素内标法定量,并对样品前处理条件和仪器条件进行优化。试验表明：方法在0．500 ng/L～500 ng/L范围内线性良好;当取样体积为1 L时,方法检出限为0．005 ng/L～0．01 ng/L;对实际水样进行2个质量浓度水平的加标回收试验,平行测定6次的 RSD为2．7％～8．7％,回收率为70．2％～110％。方法适用性试验表明,水样中复杂的基质对测定无影响。     

直接测汞法和原子荧光法测定土壤中总汞的比对研究

采用DMA-80直接测汞技术,与国标方法原子荧光法对土壤中总汞的测定进行了方法比对研究。试验结果表明,直接测汞法的检出限优于原子荧光法,精密度和准确性能够满足土壤实际样品的测定,对30个实际样品分析结果的比对表明,方法间无显著差异,该方法快速、准确、无污染。     

全二维气相色谱-飞行时间质谱法分离复杂体系中7种指示剂 多氯联苯

采用全二维气相色谱-飞行时间质谱法(GC×GC TOF-MS)分析了混标样品Aroclor 1260、Aroclor 1254、Aroclor 1242中的多氯联苯(PCBs)单体,考察了在复杂体系下对7种PCBs指示剂的分离能力。结果表明,与优化柱系统的分离效果相比,136种单体的混标样品中共分离出121种单体,7种指示剂经一维和二维的保留时间及质谱定性,在121种单体的2D斑点图中清晰可辨。全二维对于复杂体系的PCBs和指示剂的分离表明其强大的分离能力和对于检测复杂体系中指示剂的分辨能力,对该类物质的定性和定量检测具有重要意义。     

星形大分子液晶在气相色谱分析中的应用研究

将首次合成的偶氮苯硅氧烷类星形液晶大分子化合物用于毛细管柱气相色谱固定液 ,在其相转变温度附近具有良好的选择性 ,成功地分离了二甲酚异构体。     

Indoor and outdoor PM mass and number concentrations at schools in the Athens area

Simultaneous indoor and outdoor PM₁₀ and PM_2.5 concentration measurements were conducted in seven primary schools in the Athens area. Both gravimetric samplers and continuous monitors were used. Filters were subsequently analyzed for anion species. Moreover ultrafine particles number concentration was monitored continuously indoors and outdoors. Mean 8-hr PM₁₀ concentration was measured equal to 229 ± 182 μg/m³ indoors and 166 ± 133 μg/m³ outdoors. The respective PM_2.5 concentrations were 82 ± 56 μg/m³ indoors and 56 ± 26 μg/m³ outdoors. Ultrafine particles 8-h mean number concentration was measured equal to 24,000 ± 17,900 particles/cm³ indoors and 32,000 ± 14,200 particles/cm³ outdoors. PM₁₀ outdoor concentrations exhibited a greater spatial variability than the corresponding PM_2.5 ones. I/O ratios were close or above 1.00 for PM₁₀ and PM_2.5 and smaller than 1.00 for ultrafine particles. Very high I/O ratios were observed when intense activities took place. The initial results of the chemical analysis showed that accounts for the 6.6 ± 3.5% of the PM₁₀ and for the 3.1 ± 1.4%.The corresponding results for PM_2.5 are 12.0 ± 7.7% for and 3.1 ± 1.9% for . PM_2.5 indoor concentrations were highly correlated with outdoor ones and the regression line had the largest slope and a very low intercept, indicative of no indoor sources of fine particulate . The results of the statistical analysis of indoor and outdoor concentration data support the use of as a proper surrogate for indoor PM of outdoor origin.     

串联四极杆质谱(GC-QqQ-MS/MS)测定土壤中的有机氯农药和多氯联苯

建立了用加速溶剂萃取仪(ASE)萃取、凝胶渗透色谱(GPC)净化、气相色谱/串联四极杆质谱多反应监测、同时测定土壤中17种有机氯农药和19种多氯联苯的方法.加标浓度在3.3μg/kg时的平均回收率在79.6%～93.2%之间,相对标准偏差在2.9%～13.0%之间,定量限在0.01～0.51μg/kg之间.在检测土壤样品中的有机氯农药和多氯联苯残留方面,Gc-QqQ-MS/MS相对于气相色谱/电子捕获检测器(GC-ECD)和GC-MS的选择离子检测(SIM)模式具有非常明显的优势,尤其是在低浓度水平的定性和定量方面.