影响顶空-气相色谱法测定水中吡啶准确度的关键因素探讨

通过试验,讨论盐析效应、顶空的平衡温度和平衡时间、水样的p H值、色谱条件等对顶空-气相色谱法测定环境水体中吡啶准确度的影响。优化上述条件后,方法在0 mg/L~3.95 mg/L范围内线性良好,检出限可达0.016 mg/L,测定下限为0.064 mg/L。用该方法对地表水和生活污水做3个质量浓度水平的加标回收试验,测定6次结果的RSD为1.7%~5.7%,回收率为93.9%~113%。     

高效液相色谱法测定地下水中洛克沙胂

地下水水样经磷酸二氢钾提取后,用MAX固相萃取小柱对其净化、浓缩,再用高效液相色谱仪测定样品中的洛克沙胂。对色谱条件进行优化,使该方法在0.500 mg/L~10.0 mg/L范围内线性良好,方法检出限为0.047μg/L。空白加标样6次测定结果的RSD为5.3%,空白水样的3个质量浓度水平的加标回收率为79.8%~88.8%。将该方法用于测定6个地下水实际样品中洛克沙胂,其中1个被检出,测定值为0.42μg/L。     

气相色谱法测定废气中非甲烷总烃的标准气体选择

气相色谱法测定废气中非甲烷总烃,国内外相关标准选用的标准气体各不相同,通过试验考察各标准气体对测定的影响,并比对相关文献信息。结果表明:甲烷和丙烷(浓度以碳计)在填充柱气相色谱仪和毛细管柱气相色谱仪FID检测器上的响应无明显差异,而采用甲烷作为标准气体,分析时间短,工作效率高。     

桂林市细颗粒物部分典型排放源的粒径谱及成分分析

采用在线单颗粒气溶胶质谱技术源解析方法,对桂林市PM2.5典型排放源的粒径和化学成分进行质谱分析,采集燃煤/燃气源、工业工艺源、扬尘源、油烟源4类共计7个典型排放源。结果表明,桂林市4类排放源细颗粒物的粒径分布为0.25~1.25μm,80%以上的细颗粒分布在0.2~1.0μm的小粒径范围,峰值约0.68μm。细颗粒物离子成分含有Na~+、Mg~+、K~+、NH~+4、Fe~+、Pb~+、Cd~+、V~+、Mn~+、Li~+、Al~+、Ca~+、Cu~+、Zn~+、Cr~+、CN~-、PO_3~-、NO_2~-、NO_3~-、Cl~-、SO_4~(2-)、SiO_3~-等成分,桂林市细颗粒物为元素碳、有机碳元素碳、有机碳、富锰颗粒、富铁颗粒、富钾颗粒、矿物质、左旋葡聚糖以及其他金属等9类。     

固体吸附/热脱附-气相色谱法测定环境空气中苯系物的不确定度评定

建立固体吸附/热脱附-气相色谱法测定环境空气中苯系物的不确定度评定方法,分析测定过程中不确定度的来源,进行各不确定度分量的评估,并给出合成相对标准不确定度和扩展不确定度。     

塞曼原子吸收光谱法测定固定污染源废气中的汞

用PMS 30B型汞采样器采集固定污染源废气,再用塞曼原子吸收汞分析仪测定样品中的汞,高、低浓度汞标准样品测定结果均在标准范围内,相对误差分别为0和4.3%。汞吸收管对高、低浓度含汞废气的穿透效率表明,当废气汞质量浓度达到mg/m3级别时,穿透率仅为1.3%。用该方法测定稳定工况固定污染源废气中的汞,6次测定结果的RSD为5.9%,方法检出限为1.04 ng,当采样体积为20 L时,检出限为0.05μg/m3。实际监测表明,钢铁企业、燃煤电厂、垃圾焚烧厂废气中汞为0.07μg/m3~1 031μg/m3。     

超高效液相色谱/串联质谱法测定饮用水源水中多种藻毒素

饮用水源水样品经过直接进样或固相微萃取法净化后,用超高效液相色谱/串联质谱测定水中11种藻毒素。通过试验优化测定条件,使该方法在0.500μg/L~50.0μg/L范围内线性良好,检出限为0.01μg/L~0.05μg/L。对同一实际环境样品做3个质量浓度水平加标回收试验,6次测定结果的RSD为2.2%~9.3%,回收率为76.1%~108%。将该方法用于测定环巢湖湖面12个监测断面水样,结果 3组样品中MC-YR、MC-LR和MC-RR值为0.3μg/L~0.8μg/L。     

Thermal analysis of polyethylene glycol: evolved gas analysis with ion attachment mass spectrometry

The thermal decomposition of polyethylene glycol was investigated by using a technique combining evolved gas analysis (time-resolved pyrolysis) with ion-attachment mass spectrometry. This technique allows the detection of intact pyrolysis products and, therefore, offers the opportunity for direct real-time monitoring of thermal by-products. Unstable products can thus be detected; for instance, many highly reactive organic peroxides, such as CH₃OOH and HOCH₂OOH, were found in this study. Classification analysis revealed 10 major compositional formulas among the product species: C_nH_2n+2O, C_nH_2n+2O₂, C_nH_2n+2O₃, C_nH_2n+2O₄, C_nH_2n+2O₅, C_nH_2n+2O₆, C_nH_2n+2O₇, C_nH_2nO, C_nH_2nO₂, and HO(CH₂CH₂O)_nH ethylene glycol oligomers. The Li⁺ ion adduct mass spectra showed a characteristic profile in terms of both the appearance of unique components and the distribution of pyrolysis products. Among the products of the thermal decomposition of PEG, formaldehyde (HCHO) and organic peroxides were particularly interesting. Formaldehyde, one of the 10 most abundant products, is a known human carcinogen. The detection of peroxides suggests that they may form during the incineration of PEG, which may have important environmental implications. The existence of peroxide products may have implications for chemical evolution in incinerator systems.     

Multiresidue analysis and evaluation of the matrix effect on 20 pesticides in Brazilian maize (Zea mays L.) flour

Abstract

Maize consists of a cereal widely used in the preparation of different food products. Brazil is one of the world's largest maize producers. Several types of pesticides have been applied in maize crop, which can lead to the contamination of the derived products. The present work aims at the validation of multiresidue method to analyze the matrix effect and level of pesticides in maize flour. Twenty residues were investigated in samples commercialized in the state of Ceará, Brazil. The method was satisfactorily validated, according to parameters recommended by European Union. About 55% of the pesticides had an intense negative matrix effect. Multiresidue analyzes showed the presence of traces of fenitrotion in 20% of maize flour samples. Detected levels were below maximum residue limits recommended for maize. The results indicate that maize products need continuous monitoring to ensure food security.     

Simultaneous determination of organophosphorus and organonitrogen pesticides residues in Angelica sinensis

Gas chromatography with nitrogen phosphorus detector (GC-NPD) was applied to the simultaneous determination of 15 organophosphorus and 6 organonitrogen pesticides residues in Angelica sinensis. The pesticides were extracted by microwave-assisted extraction (MAE) and ultrasound-assisted extraction (UAE) techniques, respectively. The experimental variables were optimized through orthogonal array experimental design. Cleanup of extracts was performed with column chromatography using florisil and neutral aluminum as the sorbents. The determination of pesticides in the final extracts was carried out by GC-NPD. Under optimized conditions, the average recoveries obtained from MAE and UAE are in the range of 75.1–129% and 70.6–129%, respectively, and the relative standard deviations of MAE and UAE were 3.1–10.6% and 1.0–17.8%, respectively.