Trace analysis of airborne toluene diisocyanate as a pentafluorobenzyl derivative by gas chromatography with electron capture detection

Trace analysis of airborne toluene diisocyanate (TDI) vapor was accomplished by measuring the derivative using gas chromatography with electron‐capture detector after collecting gas samples with a microimpinger containing 2 ml toluene, 1 μl pentafluorobenzyl alcohol, and 1 μl triethylamine. The sampling efficiency was determined to be 99.4% for short‐term exposure level of TDI and the 2,4‐ and 2,6‐isomers of TDI were well separated. The derivative was identified to be a new compound with a molecular weight of 570 by mass spectrometry in fast atomic bombardment mode and nuclear magnetic resonance spectrometry. This method is convenient and can be applied in the field where airborne TDI is in vapor form.     

加速溶剂萃取-气质联用同步测定土壤中17组分多溴二苯醚

建立了加速溶剂萃取-气相色谱-质谱法(ASE-GC/MS)同步定量分析土壤中17组分多溴二苯醚(PBDEs)的方法.选用正己烷和二氯甲烷混合液(体积比为1∶1)为萃取剂,样品经加速溶剂萃取后由氧化铝复合硅胶柱净化,气相色谱-负化学源-质谱法测定.结果表明:在32 min内,包括高溴代二苯醚在内的17组分PBDEs同族体在同一较短毛细管色谱柱上得到了较好的分离.该方法中BDE209的回收率为80.80%,其余BDE的回收率为86.39%～103.19%;BDE209的方法检出限为198.33 pg/g,其他16组分PBDEs同族体的方法检出限为0.85～114.33 pg/g.该方法检测土壤中多组分PBDEs的灵敏度高、重现性和回收率良好,可用于土壤样品PBDEs的分析.      

微波Sol-Gel制备TiO2的研究及其对活性艳红X-3B的降解

采用微波Sol-Gel法在石英表面制备了负载型TiO2光催化剂,通过紫外吸收光谱和X衍射分析表征了TiO2溶胶的变化过程及锐钛型TiO2的生成。以活性艳红X-3B为模拟污染物进行光催化降解,探讨了微波功率、反应温度和反应时间对微波Sol-Gel法制备TiO2光催化活性的影响。由因素试验确定了最佳工艺条件:微波功率400W,反应温度90℃,反应时间2min。在此条件下制备的TiO2催化剂对活性艳红X-3B溶液进行光催化降解,反应30 min的脱色率达93%,TOC去除率为55%。采用中空纤维膜三相液相微萃取-毛细管电泳(HF-LLLME-CE)联用技术对降解生成的小分子有机物进行了测定。     

食醋中总酸、总酯含量的连续测定

提出了利用连续分析技术定量地测定食醋中总酸、总酯的含量。操作简捷、快速、准确、所获的结果与常规法基本一致,此法对食醋的质量控制具有一定的现实意义。     

五管发酵测定粪大肠菌群的研究

通过实验摸索出粪大肠菌群的一种五管发酵法。该方法检测下限为9个/L,适用于地表水和废水中粪大肠菌群的测定。     

顺序进样流动注射光度法测定水中氨氮

将顺序进样与流动注射分光光度法相结合,研发了氨氮自动在线检测仪,用于测定水中氨氮质量浓度.实验结果表明:当进样量为0.39 mL、显色剂体积为0.33 mL、停留时间为5 min、载流液流量为2.0 mL/min时,氨氮质量浓度p与吸光度A在氨氮质量浓度为0～ 15.00 mg/L的范围内呈良好的线性关系,标准工作曲线方程为A=0.01929+ 0.2362,相关系数为0.9993(n=11);检出限为0.020 mg/L;相对标准偏差为0.50％～2.38％;实际水样的加标回收率为94.5％～106.0％.     

Identification of important factors for water vapor flux and CO2 exchange in a cropland

Water vapor flux and carbon dioxide (CO₂) exchange in croplands are crucial to water and carbon cycle research as well as to global warming evaluation. In this study, a standard three-layer feed-forward back propagation neural network technique associated with the Bayesian technique of automatic relevance determination (ARD) was employed to investigate water vapor and CO₂ exchange between the canopy of summer maize and atmosphere in responses to variations of environmental and physiological factors. These factors, namely the photosynthetically active radiation (PAR), air temperature (T), vapor pressure deficient (VPD), leaf-area index (LAI), soil water content in root zone (W), and friction velocity (U*), were used as inputs in neural network analysis. Results showed that PAR, VPD, T and LAI were the primary factors regulating both water vapor and CO₂ fluxes with VPD and W more critical to water vapor flux and PAR and T more crucial to CO₂ exchange. Furthermore, two time variables “day of the year (DOY)” and “time of the day (TOD)” could also improve the simulation results of neural network analysis. The important factors identified by the neural network technique used in this study were in the order of PAR > T > VPD > LAI > U* > TOD for water vapor flux and in the order of VPD > W > LAI > T > PAR > DOY for CO₂ exchange. This study suggests that neural network technique associated with ARD could be a useful tool for identifying important factors regulating water vapor and CO₂ fluxes in terrestrial ecosystem.     

松花江、黑龙江水中可溶性铁与有机质含量的相关性

以黑龙江和松花江为研究对象,分析了河水中可溶性铁含量的分布特征及其与有机质含量、pH值的关系.结果表明,黑龙江、松花江水体中可溶性铁质量浓度分别为0.10～0.62和0.11～0.73 mg·L-1,Fe2+质量浓度分别为0.01～0.16和0.04～0.35 mg·L-1.松花江水体中可溶性铁、Fe2+浓度平均值均略高于黑龙江.同一年份内水体可溶性铁含量峰值以平水期居多.黑龙江水体CODCr与Fe2+含量呈显著负相关,松花江水体CODCr与可溶性铁含量呈显著正相关.松花江水体中BOD5、pH值与Fe2+含量呈显著负相关.人为来源的难生物降解有机质的大量输入提高了河水中铁离子的络合容量,使水中可溶性铁和有机络合铁含量增加.     

差压式直读BOD测定仪的验证实验

本文对“Ⅱ型差压式直读BOD测定仪进行了精密度、准确度、适用性和等效性的一系列验证实验,结果表明,“差压式直读BOD测定仪”是一种较为理想的BOD测定仪器,从而为该仪器法定为国家标准分析方法提供了科学依据。