超高效液相色谱-串联质谱法测定污水中14种有机磷酸酯阻燃剂

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)联用法同时测定污水中14种有机磷酸酯阻燃剂(OPEs)的分析方法.样品采集后,经GF/C膜过滤,HLB固相萃取小柱净化后进样分析.以BEH C18色谱柱为分离柱,乙腈和水混合液为流动相(0.2 mL min-1)梯度洗脱,15 min内可完成14种OPEs的分离.在电喷雾正离子模式下,采用多反应监测模式(MRM)进行质谱测定.在加标浓度为1.0μg·L-1时,14种OPEs在污水处理厂进水和出水中的回收率分别为52.1%—119%、43.6%—114%,相对标准偏差(RSD)分别为1.2%—16.2%、0.4%—9.2%,方法的检出限(LOD)在0.3—6.0 ng·L-1间.方法精密度好,准确度高,可满足同时对污水样品中的14种OPEs进行定性及定量分析的要求.     

室内环境中的邻苯二甲酸酯类化合物的研究进展

综述了室内环境中的邻苯二甲酸酯类化合物的存在状况,及其对人的危害。介绍了主要的几种环境中邻苯二甲酸酯类化合物的前处理方法及其分析测定技术。     

Experimental investigation on engine performances,combustion characteristics and emission of exhaust gases of VCR engine fuelled with cottonseed oil methyl ester blended with diesel

This research work investigates the engine performances, combustion characteristics, and emission of exhaust gases of variable compression ratio engine fuelled with cottonseed oil methyl ester (COME) and diesel at different blends. The analysis showed that heat release rate and cylinder pressure is higher for diesel than COME blends. Higher BTE is obtained at the maximum load condition. The higher BTE and lower SFC are obtained for blend B15 as 42.17% and 0.2 kg/kW-hr at brake mean effective pressure (BMEP) of 4.64 bar. Also it is found that the peak cylinder gas pressure and combustion duration increases when the BMEP increases. At the BMEP of 3.51 bar, higher HRR is observed as 18.12 J/deg. Increase in HRR is obtained as 6.07% for B30 at BMEP of 4.64 bar when compared to diesel. Ignition delay decreased by 13.16% for B100, by the increment of blend proportions when compared to diesel, at BMEP of 4.64 bar. Lower smoke, HC and CO emissions are observed when increasing the blend proportions, whereas the nitric oxide emissions increases due to the better combustion resulted in higher temperatures. At BMEP of 4.64 bar, the CO emissions are reduced to 25.24% for neat biodiesel when compared with the diesel.     

Transesterification of hazelnut oil by ultrasonic irradiation

Ultrasonic irradiation is considered an effective way to increase mass transfer between immiscible liquid–liquid phases in a heterogeneous system leading to faster transesterification and higher yield and saving excess methanol and catalyst. In this study, the transesteri?cation of hazelnut oil with methanol and ethanol was performed in the presence of potassium hydroxide or sodium methoxide as a catalyst using two types of ultrasonic irradiation with a probe (20 kHz, 200 W) and a bath (35 kHz, 400 W); a conventional production method was also used. The reaction time, alcohol:oil molar ratio, catalyst type (KOH or NaOCH₃), and catalyst amount (wt.% of oil) were studied as experimental parameters. The highest methyl ester conversion was obtained as 98.12% by using ultrasonic probe at a 5:1 methanol:oil molar ratio with KOH 1 wt.% of oil as catalyst in 20-min reaction time at autogenous temperature. The application of ultrasonic irradiation by using a probe decreased the level of energy consumption, showing that this method may be a promising alternative compared with the conventional production method.     

Nano Fe2O3 embedded in montmorillonite with citric acid enhanced photocatalytic activity of nanoparticles towards diethyl phthalate

Nano-Fe₂O₃ embedded in montmorillonite particles (Fe-Mt) were prepared to degrade diethyl phthalate (DEP) with citric acid (CA) under xenon light irradiation. Compared to pristine montmorillonite (Na-Mt), the embedding process increased 14.5-fold of iron content and 1.8-fold of specific surface area. The synthesized Fe-Mt have more oxygen vacancies than Fe₂O₃ nanoparticles (nFe₂O₃), which could induce more reactive oxygen species (ROSs) generation in the presence of CA under xenon lamp irradiation. Fe-Mt with CA enhanced photo-assisted degradation of DEP 2.5 times as compared to nFe₂O₃ with CA. Quenching experiments, electron paramagnetic resonance (EPR) spectroscopy and identification of products confirmed that surface-bound ?OH was the main radical to degrade DEP. Common anions (i.e., NO₃^?, CO₃^2?, Cl^?) and humic acid could compete ?OH with DEP and cause slower degradation of DEP. The removal efficiency of DEP was more than 56% with Fe-Mt after three recycles, and the dissolved Fe concentration from Fe-Mt was below 75 μmol/L, indicating Fe-Mt had a good stability as a catalyst. Fe-Mt together with CA appeared to be a promising strategy to remove organic pollutants in surface water, or topsoil under solar irradiation.     

新型侧链聚硅氧烷液晶高分子用作毛细柱气相色谱固定液的研究

以合成的新型胆甾酯类侧链聚硅氧烷液晶高分子作固定液 ,涂渍在弹性石英毛细管柱上 ,具有较高的柱效和选择性 ,热稳定性好 ,适于分离多种异构体混合物。     

固相萃取—高效液相色谱法测定水中阿特拉津和2种邻苯二甲酸酯

采用固相萃取法对水样进行提取富集,液相色谱法测定水中2种邻苯二甲酸酯类和阿特拉津有机污染物,并对方法进行了探索、优化和验证。在固相萃取过程中,研究了水体p H、洗脱液组份对邻苯二甲酸酯和阿特拉津萃取回收率的影响,解决了邻苯二甲酸酯和阿特拉津回收率不高的问题。在空白水加标实验中,邻苯二甲酸酯的回收率为89.3%~92.2%,阿特拉津回收率为88.9%,获得了较高的回收率及测定精度。除此之外,还对地表水进行了加标回收实验,结果符合要求。     

已二酸生产副产物——混合二元酸的综合利用

采用一水合硫酸氢钠作为催化剂，催化己二酸生产副产物——混合二元酸与甲醇反应合成混合二元酸二甲酯。优化工艺条件为：混合二元酸加入量0．1mol，无水甲醇加入量0．5mol，一水合硫酸氢钠加入量4．0g，环己烷加入量20mL，反应时间1．5h。合成混合二元酸二甲酯的酯化反应收率大于97％。经气相色谱检测，产物中酯的质量分数为98．91％。一水合硫酸氢钠可重复使用3次。     

浅谈串联四极杆质谱（GC—QqQ-MS／MS）在土壤样品有机污染物分析中的应用

建立了ASE-GPC—GC-QqQ—MS／MS测定土壤中17种有机氯农药和19种多氯联苯以及MAE-SPE—GC-QqQ—MS／MS测定土壤中16种多环芳烃和18种邻苯二甲酸酯的方法。多环芳烃和邻苯二甲酸酯定量限在0．02～2．81μg／kg之间，有机氯农药和多氯联苯定量限在0．01～0．51μg/kg之间。样品加标浓度在5μg/kg时多环芳烃和邻苯二甲酸酯的平均回收率在66．6％～122．1％之间，相对标准偏差均小于20％；有机氯农药和多氯联苯平均回收率在79．6％～93．2％之间，相对标准偏差均小于15％。     

有机磷酸酯阻燃剂降解方法的研究进展

有机磷阻燃剂(OPFRs)已取代溴代阻燃剂广泛应用于各行业,并很容易通过挥发、磨损等方式进入各环境介质中.目前,已在水体、土壤等环境介质中检测到了OPFRs的存在.本文总结了目前已有的OPFRs在环境中的降解方式,据其原理主要可分为化学法和生物法,化学法主要包含Fenton/类Fenton氧化法、紫外-双氧水法(UV/H2O2)、光催化法、过硫酸盐活化法和水解光解等,能够产生大量具有强氧化性的自由基(·OH、SO4·-等)破坏烃链使其降解.但该方法容易受到实际水体中的复杂成分影响,导致效果降低.生物法则是利用不同的细菌将OPFRs作为碳源或磷源在生长过程中将其消耗或和微生物体内的特异性酶发生酶促反应从而降解.通过总结归纳目前OPFRs的降解方法,了解现有方法存在的优点和缺点,为高效去除OPFRs提供理论基础.