HPLC法测定水和废水中的醛酮类化合物

将水样用1mol／L柠檬酸缓冲液调节至酸性(pH=3)，其中醛酮类化合物与2，4-二硝基苯肼(DNPH)发生衍生化反应，生成稳定的化合物——腙，经C18固相萃取小柱富集、乙腈淋洗后，用带有二极管阵列检测器的高效液相色谱仪(HPLC)经32 min完成15种醛酮类化合物定性、定量分析。当测定样品为100mL时，检测限均为μg／L级，其中丙酮最高为16μg／L，丁醛最低为1.1μg／L，一般在2μg／L～6μg／L之间。     

连续流动-固相微萃取方法富集水中多环芳烃的探讨

建立了连续流动-固相微萃取富集、气相色谱测定水中多环芳烃的方法，探讨了流量和溶液体积对萃取效果的影响。方法在0μg／L-40μg／L范围内线性良好，8种多环芳烃的检出限为0．05μg／L-0．5μg／L，样品测定的相对标准偏差〈7％，加标回收率为87．0％～112％。     

固相萃取-毛细管气相色谱法测定地表水中硝基苯类化合物

建立了固相萃取-毛细管气相色谱测定地表水中硝基苯类化合物的方法，优化了试验条件。方法线性良好，10种硝基苯类化合物的检出限为0．05μg／L～0．15μg／L，实际样品测定的RSD为1．7％～5．0％，平均加标回收率为80．8％～117％。     

固相萃取- GC/MS法测定水中邻苯二甲酸酯类

采用固相萃取-GC／MS法测定水中6种邻苯二甲酸酯类有机污染物，比较了不同固相萃取柱对萃取效果的影响，优化了水样pH值、水样流量、穿透体积、洗脱溶剂、洗脱剂体积、洗脱流量等萃取条件。方法在0．050μg/L-800μg/L范围内线性良好，检出限为0．008μg/L～0．03μg／L，标准溶液测定的RSD≤10．5％，实际水样加标回收率为80．0％-100％。     

毛细管低温吸附气相色谱法同时测定空气中痕量甲硫醇和硫化氢

建立了毛细管低温吸附气相色谱同时测定空气中痕量甲硫醇和硫化氢的方法，介绍了冷冻吸附装置的制备方法和样品冷凝吸附流程。甲硫醇和硫化氢分别在0.467ng～5.16ng和0.327ng～3.60ng范围内线性良好，当进样体积为1L时，检出限为0．205μg/m^3和0．213μg／m^3，空白加标平均回收率为88．6％和90．2％，RSD为6.0％和6．5％。     

ASE萃取-SPE净化-气相色谱法测定土壤中有机氯农药

建立了加速溶剂萃取-固相萃取净化-气相色谱测定土壤中α-六六六、β-六六六、γ-六六六、δ-六六六、P，P′-DDE、P，P′-DDD、O，P′-DDT、P，P′-DDT等8种有机氯农药的方法。在0μg／L～500μg／L范围内方法线性良好，8种有机氯农药的检出限在0．06μg／kg～0．21μg／kg之间，基质加标试验的相对标准偏差为2．2％～5．8％，回收率为81．5％～113％。     

加速溶剂萃取-高效液相色谱法测定环境空气中的苯并(a)芘

采用加速溶剂萃取一高效液相色谱法荧光检测器测定环境空气中的苯并（a）芘，以乙腈／水为流动相，检测器激发波长为290nm，发射波长为430nm。方法线性良好，检出限为0．08μg／L，当采样体积为1080m。时，最低检测质量浓度为3×10^-7μg／m^3（标准状态下），实际样品加标回收率为87．2％～109％。与超声波萃取法相比，两种方法回收率相近，而加速溶剂萃取法乙腈用量更少。     

HPLC和GC-MS法测定环境空气中醛酮类化合物比对分析

对2，4-二硝基苯肼吸附衍生-高效液相色谱（DNPH-HPLC）法和罐采样/气相色谱-质谱（GC-MS）法的测定条件进行优化，将两种方法测定环境空气中13种醛酮类化合物（OVOCs）的结果做比对分析。结果表明，HPLC法和GC-MS法均可实现一次进样13种OVOCs全分析，方法检出限分别为0.26μg/m3～1.39μg/m3和0.49μg/m3～1.10μg/m3，加标回收率分别为95.9%～111%和52.0%～138%。两种方法测定实际样品，检出组分的测定结果无显著性差异；HPLC法适合测定环境空气中低碳类（C1～C3）低浓度OVOCs，GC-MS法适合测定多碳类（C4～C8）低浓度OVOCs。     

固相萃取- GC/MS法测定水中有机氯农药

建立了固相萃取-气相色谱／质谱联用测定水中痕量六六六、滴滴涕和环氧七氯的方法。采用C18固相萃取柱富集水样，二氯甲烷／丙酮混合溶剂洗脱，加入菲-d10作为内标，利用气相色谱／质谱联用仪选择离子监测模式检测，内标法定量，定性、定量准确，线性响应良好，干扰小，按采样1 L计算，方法检出限为4．26ng／L～19、2ng／L，RSD在0、4％-6、3％之间，平均加标回收率在77．7％～118％之间，实际样品测定结果表明方法能满足环境水体中痕量有机氯农药的监测要求。     

石墨炉原子吸收法测定降水中重金属

建立了石墨炉原子吸收测定大气降水中Pb、Mn、Fe、Zn、Cu、Cr、Cd的方法，优化了试验条件。方法线性良好，7种元素的检出限为0．54μg／L-2．2μg／L，RSD为3．0％-7．3％，加标回收率为101％-105％，实际降水样品的测定结果令人满意。     

长沙市大气中醛酮类化合物浓度变化特征

参照美国环保署EPA-TO11标准方法,于2014年7—10月监测了长沙市大气中醛酮类化合物的质量浓度。主要监测到的醛酮类化合物为甲醛、乙醛、丙酮、丙醛、甲基丙烯醛,夏季质量浓度最高的是甲醛(13.86 mg/m³),其次是乙醛(7.28 mg/m³)、丙酮(7.14 mg/m³),秋季质量浓度最高的是甲醛(10.31 mg/m³),其次是丙酮(8.37 mg/m³)、乙醛(5.78 mg/m³)。夏季醛酮类化合物的总量高于秋季,甲醛、乙醛、丙酮的质量浓度最大值基本出现在13:00—15:00。C1/C2(甲醛/乙醛)、C2/C3(乙醛/丙醛)的平均值分别为2.02、10.19。分析了醛酮类化合物之间的相关性以及它们可能的来源。丙醛和甲醛、乙醛的相关性较好,三者有共同的人为来源。夏季大气中除丙酮外,其他醛酮类化合物的相关性均较好。夏季甲基丙烯醛和甲醛、乙醛、丙酮有相同的自然来源。综合分析可知,长沙大气中醛酮类化合物质量浓度受自然因素和人为因素的双重影响。     

Validation of diffusive mini-samplers for aldehyde and VOC and its feasibility for measuring the exposure levels of elementary school children

Exposure to various chemicals can cause adverse effects to health, such as asthma and allergies, especially in children. Data on personal exposure levels in children are scarce, thus small lightweight diffusive mini-samplers for aldehydes and volatile organic compounds (VOCs) were designed to measure the exposure level of children to these chemicals. The aim of the study was to validate and examine the applicability of these mini-samplers for measuring daily chemical exposure. The diffusive mini-samplers are 20 mm in length, 11 mm in diameter, and 1.67 g in weight. The devices are cylindrically shaped with polytetrafluoroethylene membrane filters placed at each end. To measure aldehydes and acetone, 20 mg of 2,4-dinitrophenylhydrazine was used as an absorbent. To measure VOCs, a carbon molecular sieve was used. The sampling rate for each chemical was determined by parallel sampling with active samplers in a closed exposure bag. The blank levels of the chemicals and the storage stability of the device were tested. The mini-samplers were compared to commercially available diffusive samplers. To examine the applicability of the samplers, 65 elementary school children carried them for 24 h. The sampling rates for formaldehyde, acetaldehyde, and acetone were 20.9, 22.9, and 19.7 mL min(-1), respectively. The limits of quantification (LOQ) for the 24-hour sampling by high-performance liquid chromatography/ultraviolet (HPLC/UV) analysis were 8.3, 7.6, and 8.8 μg m(-3) for formaldehyde, acetaldehyde, and acetone, respectively. The sampling rates for the 11 VOCs were determined and ranged from 3.3 mL min(-1) for styrene and 2-ethyl-1-hexanol to 11.7 mL min(-1) for benzene. The LOQ for the 24-hour sampling by gas chromatography-mass spectrometry (GC-MS) analysis ranged from 5.9-105.2 μg m(-3), 1.1-24.7 parts per billion. The storage stability after 5 days ranged from 94.8 to 118.2%. Formaldehyde, acetone, benzene, and toluene were detected above the LOQ in more than 90% of the children, and the median concentrations were 21.7, 20.9, 10.1, and 21.5 μg m(-3), respectively. This study shows that the diffusive samplers developed were suitable for children to carry and were capable of measuring the children's daily chemical exposure.     

乌鲁木齐市采暖期SO_2污染空间分布特征分析

对乌鲁木齐市采暖期进行SO2网格布点监测。结果表明:采暖期SO2浓度值分布在49~364μg/m3之间,72.4%的网格监测值超过国家二级日标准,污染严重。SO2浓度基本呈现4个梯度:第一梯度为市区西北部,SO2浓度小于120μg/m3;第二梯度为市区东北部,浓度为120~160μg/m3;第三梯度为第四梯度外围,SO2浓度为160~200μg/m3;第四梯度为市区中部及市区南部,SO2浓度大于200μg/m3。SO2污染随海拔高度的递增而增加,城市北部污染较轻,城市中心地带为重污染区域。     

动态顶空气相色谱法测定水中极性水溶性有机物

采用动态顶空气相色谱FID法测定水中乙醛、丙酮、甲醇、丙烯醛、丙烯腈、乙腈、吡啶等7种极性水溶性有机物，通过优化动态顶空条件，使该方法在0．157mg／L～7．92mg!L之间线性良好。方法检出限在0．008mg／L～0．048mg／L之间，空白水样的加标回收率为103％～111％，RSD为5．4％～8．7％。用该方法测定某制药企业排口污水和地表水，只有污水中甲醇、乙腈、吡啶有响应值。     

基于SOA和O3生成潜势的上海市VOCs优控物种研究

为评估上海市挥发性有机物(VOCs)对二次有机气溶胶(SOA)和臭氧生成潜势的贡献,采用SUMMA罐采样实验室GC-FID/MS分析方法开展了环境空气104种臭氧前体物和TO-15组分分析,采用DNPH吸附管采样实验室HPLC高效液相色谱法开展了环境空气13种醛酮类组分分析。结果表明:2018年8-11月上海市代表点位VOCs摩尔分数均值范围为20. 61~50. 38 nmol/mol,臭氧生成潜势(OFP)均值范围为60. 55~184. 12μg/m^3,二次有机气溶胶生成潜势(AFP)为21. 63~61. 72μg/m^3。醛酮类和芳香烃类是OFP的主要贡献因子,贡献占比分别为31. 5%~55. 2%和21. 6%~37. 8%。芳香烃类对AFP贡献超过90%。从主要组分构成来看,城区人口密集区点位乙烷、丙烷浓度最高,其他点位甲醛浓度最高;甲醛对OFP贡献最大;间/对二甲苯在浦东书院点位AFP贡献最大,其他点位为甲苯。OFP和AFP双控物种各点位均有4~5个主要物种,以芳香烃类为主。     

Concentrations of formaldehyde and other carbonyls in environments affected by incense burning

Burning incense to pay homage to deities is common in Chinese homes and temples. Air samples were collected and analyzed for carbonyls from a home and a temple in Hong Kong where incense burning occurs on a daily basis. Carbonyls in the air were trapped on a solid sorbent coated with O-(2,3,4,5,6-pentafluorobenzyl)-hydroxylamine, followed by thermal desorption and subsequent GC/MS analysis. The carbonyls identified include formaldehyde, acetaldehyde, acrolein, 2-furfural, benzaldehyde, glyoxal, and methylglyoxal. The levels of the above carbonyls correlate with the intensity of the incense-burning activities. The total mixing ratios of the carbonyls in the temple exceed those in the ambient air outside the temple by 11-23 times. Formaldehyde is the most abundant species, contributing to approximately 55% of the total carbonyl mixing ratios in both the temple and the home environments during incense burning. The mixing ratio of formaldehyde ranges from 108 to 346 ppbv in the temple and averages 103 ppbv in the home during incense burning. These values exceed the World Health Organization (WHO) air quality guideline of 100 microg m(-3) (88 ppbv) for formaldehyde. The highest formaldehyde level in the temple exceeds the WHO guideline by 3 times at peak incense burning hours. The mixing ratio of acrolein in the temple ranges from 20 to 99 ppbv, approaching or exceeding the WHO air quality guideline of 50 microg m(-3) (22 ppbv) for acrolein. Our measurements indicate that incense burning significantly elevates the concentrations of a number of carbonyls, most notably formaldehyde and acrolein, in the surrounding environments. This study provides preliminary insights on indoor air quality problems created by incense burning.     

吹扫捕集-气相色谱法同时测定水中的乙醛、丙烯醛和甲醛

研究了吹扫捕集-气相色谱法同时测定水中乙醛、丙烯醛和甲醛的方法并优化了实验条件.实验结果表明,该方法操作简便,灵敏高效,目标化合物的检出限分别为0.037、0.012、0.0006mg/L,相对标准偏差在3.9％ ～15.8％之间,实际水样的加标回收率在73.0％ ～118％之间,能很好满足《地表水环境质量标准》中相关项目的要求.     

Levels, sources, and health risks of carbonyls in residential indoor air in Hangzhou, China

Concentrations of formaldehyde, acetaldehyde, acetone, propionaldehyde, i-pentanal, and butyraldehyde in residential indoor air in Hangzhou were determined. The mean concentration of the total carbonyl compounds in summer was 222.6 μg/m³, higher than that in winter (68.5 μg/m³). The concentration of a specific carbonyl in indoor air was higher than the outdoor air measurement, indicating the release of carbonyls from the indoor sources. Formaldehyde and acetone were the most abundant carbonyls detected in summer and winter, respectively. Multiple regression analysis indicated that carbonyl concentrations in residential indoor air depended on the age of decoration and furniture, as well as their concentrations in outdoor air. In addition, a primary estimation showed that the health risks of carbonyls in summer were higher than those in winter.     

气相色谱/质谱联用法测定环境空气中恶臭类硫化物

采用冷阱预浓缩-气相色谱/质谱联用法测定环境空气中硫化氢、甲硫醇、甲硫醚、二硫化碳、二甲二硫、噻吩等6种硫化物,讨论了采样容器材质的影响。方法线性良好,6种硫化物的检出限为1.0μg/m3～5.0μg/m3,混合标准气平行测定的RSD≤8.1%,加标回收率为93.5%～97.3%。