目的 建立一种Qu ECh ERS EMR-Lipid净化结合同位素稀释-超高效液相色谱-串联质谱技术(UPLC-MS/MS)同时测定蜂房及其制剂中10种真菌毒素的检测方法。方法 样品经80%乙腈水溶液提取,Qu ECh ERS EMRLipid净化,采用UPLC-MS/MS,在多反应监测...目的 建立一种Qu ECh ERS EMR-Lipid净化结合同位素稀释-超高效液相色谱-串联质谱技术(UPLC-MS/MS)同时测定蜂房及其制剂中10种真菌毒素的检测方法。方法 样品经80%乙腈水溶液提取,Qu ECh ERS EMRLipid净化,采用UPLC-MS/MS,在多反应监测(MRM)模式下进行测定,内标法定量。结果 10种真菌毒素含量在各自质量浓度范围内具有较好的线性关系(r>0.999),目标化合物在低、中、高3个质量浓度下的平均回收率为83.8%~107.1%(RSD<6.5%),定量限(LOQ)为0.18~129μg/kg。结论 该法前处理步骤简便,净化效果良好,提高了样品检测效率,内标法定量精准可靠,适用于蜂房及其制剂中10种真菌毒素的同时检测。展开更多
NF_(3)is commonly used as an etching and cleaning gas in semiconductor industry,however it is a strongly greenhouse gas.Therefore,the destruction of disposal NF_(3)is an urgent task to migrate the greenhouse effect.Am...NF_(3)is commonly used as an etching and cleaning gas in semiconductor industry,however it is a strongly greenhouse gas.Therefore,the destruction of disposal NF_(3)is an urgent task to migrate the greenhouse effect.Among the technologies for NF_(3)abatement,the destructive sorption of NF_(3)over metal oxides sorbents is an effective way.Thus,the search for a highly reactive and utilized sorbent for NF_(3)destruction is in great demand.In this work,AlOOH supported on carbon-sphere(AlOOH/CS)as precursors were synthesized hydrothermally and heat-treated to prepare the Al_(2)O_(3)sorbents.The influence of AlOOH/CS hydrothermal temperatures on the reactivity of derived Al_(2)O_(3)sorbents for NF_(3)destruction was investigated,and it is shown that the Al2O3 from AlOOH/CS hydro-thermalized at 120℃is superior to others.Subsequently,the optimized Al_(2)O_(3)was covered by Mn(OH)x to prepare Mn/Al_(2)O_(3)sorbents via changing hydrothermal temperatures and Mn loadings.The results show that the Mn/Al_(2)O_(3)sorbents are more utilized than bare Al_(2)O_(3)in NF_(3)destructive sorption due to the promotional effect of Mn_(2)O_(3)as surface layer on the fluorination of Al_(2)O_(3)as substrate,especially the optimal 5%Mn/Al2O3(160℃)exhibits a utilization percentage as high as 90.4%,and remarkably exceeds all the sorbents reported so far.These findings are beneficial to develop more efficient sorbents for the destruction of NF_(3).展开更多
Steelmaking industry faces urgent demands for both steel slag utilization and CO_(2)abatement.Ca and Mg of steel slag can be extracted by acid solution and used to prepare sorbents for CO_(2)capture.In this work,the c...Steelmaking industry faces urgent demands for both steel slag utilization and CO_(2)abatement.Ca and Mg of steel slag can be extracted by acid solution and used to prepare sorbents for CO_(2)capture.In this work,the calcium-based sorbents were prepared from stainless steel slag leachate by co-precipitation,and the initial CO_(2)chemisorption capacity of the calcium-based sorbent prepared from steel slag with the Ca and Mg molar ratio of 3.64:1 was 0.40 g/g.Moreover,the effect of Ca/Mg molar ratio on the morphology,structure,and CO_(2)chemisorption capacity of the calcium-based sorbents were investigated.The results show that the optimal Ca/Mg molar ratio of sorbent for CO_(2)capture was4.2:1,and the skeleton support effect of MgO in calcium-based sorbents was determined.Meanwhile,the chemisorption kinetics of the sorbents was studied using the Avrami-Erofeev model.There were two processes of CO_(2)chemisorption,and the activation energy of the first stage(reaction control)was found to be lower than that of the second stage(diffusion control).展开更多
Using environment-friendly and low-cost biowaste adsorbents as toxic metal ion removal substrates from aqueous solutions has a great economic advantage. This work evaluated pumpkin and potato peel biowastes for the ad...Using environment-friendly and low-cost biowaste adsorbents as toxic metal ion removal substrates from aqueous solutions has a great economic advantage. This work evaluated pumpkin and potato peel biowastes for the adsorption of cadmium ions. The biowastes were treated with acid or base. Batch experiments were carried out by introducing a known concentration of metal ion solution into the biowaste sorbent at various pH levels. The pH and metal ion concentration was monitored with pH and cadmium ion-selective electrode continuously for two hours, and the final concentration for the metal ion after 24 hours was measured with the cadmium electrode and then confirmed with ICP-OES. L-type isotherms were obtained that fit to Freundlich model. Adsorption isotherms showed chemical adsorption and the kinetics following the second order model. Equilibrium adsorption capacity is higher than 29 mg/g at pH 5.6 when the initial concentration is 220 ppm. Dynamic cadmium adsorption capacity is 17 mg/g from aqueous solution when the feed solution is 220 ppm with pumpkin peel biowaste sorbent. The biowaste materials can be regenerated with acid washing.展开更多
提出了滤过型固相萃取柱净化-超高效液相色谱-串联质谱法同时测定鸡蛋中全氟丁酸、全氟戊酸、全氟己酸、全氟庚酸、全氟辛酸、全氟壬酸、全氟癸酸、全氟十一酸、全氟十二酸、全氟十三酸、全氟十四酸、全氟丁烷磺酸、全氟己烷磺酸、全氟...提出了滤过型固相萃取柱净化-超高效液相色谱-串联质谱法同时测定鸡蛋中全氟丁酸、全氟戊酸、全氟己酸、全氟庚酸、全氟辛酸、全氟壬酸、全氟癸酸、全氟十一酸、全氟十二酸、全氟十三酸、全氟十四酸、全氟丁烷磺酸、全氟己烷磺酸、全氟庚烷磺酸、全氟辛烷磺酸等15种全氟化合物含量的方法。鸡蛋样品(2 g)中加入0.1 mL 20.0μg·L^(-1)同位素内标混合溶液,经10 mL 80%(体积分数)乙腈溶液振荡和超声提取后,离心;分取5 mL滤液,直接过滤过型Captive EMR-Lipid柱净化,收集流出液,氮吹至近干,加入500μL甲醇复溶,经涡旋、离心处理后测定。采用Agilent Eclipse Plus C_(18)RRHD色谱柱(100 mm×2.1 mm,1.8μm)分离,以不同体积比的2 mmol·L^(-1)乙酸铵溶液和甲醇的混合溶液梯度洗脱,在电喷雾离子源负离子扫描模式下,以多反应监测模式检测,同位素内标法定量。结果表明:15种全氟化合物标准曲线的线性范围均为0.125~20.0μg·L^(-1),测定下限(10S/N)为0.05~0.16μg·kg^(-1);在0.500,4.00,16.0μg·kg^(-1)加标浓度水平下,15种目标物的回收率为78.0%~111%,测定值的相对标准偏差(n=6)为0.87%~14%。展开更多
A kind of industrial solid waste, i.e., carbide slag, was used as CaO precursor to synthesize CO2 sorbent. The highly reactive synthetic sorbent was prepared from carbide slag, aluminum nitrate hydrate and glycerol wa...A kind of industrial solid waste, i.e., carbide slag, was used as CaO precursor to synthesize CO2 sorbent. The highly reactive synthetic sorbent was prepared from carbide slag, aluminum nitrate hydrate and glycerol water solution by the combustion synthesis method. The results show that the synthetic sorbent exhibits a much higher CO2 capture capacity compared with carbide slag. The CO2 capture capacity and the carbonation conversion of the synthetic sorbent are 0. 38 g/g and 0. 70 after 50 cycles, which are 1.8 and 2. 1 times those of carbide slag. The average carbonation conversion and the CO2 capture efficiency of the synthetic sorbent are higher than those of carbide slag with the same sorbent flow ratios. The required sorbent flow ratios are lower for synthetic sorbent to achieve the same CO2 capture efficiency compared with carbide slag. With the same sorbent flow ratio and CO2 capture efficiency, the energy requirement in calciner for the synthetic sorbent is less than that for carbide slag.展开更多
低浓度煤层气的提质利用对缓解国内天然气不足的现状具有重要意义,然而煤层气中存在的氮气杂质限制了该类资源的进一步应用,进行低浓度煤层气中CH_(4)/N_(2)混合物的分离至关重要。制备了两种具有弱极性超微孔的金属有机框架材料Sc-CPM-...低浓度煤层气的提质利用对缓解国内天然气不足的现状具有重要意义,然而煤层气中存在的氮气杂质限制了该类资源的进一步应用,进行低浓度煤层气中CH_(4)/N_(2)混合物的分离至关重要。制备了两种具有弱极性超微孔的金属有机框架材料Sc-CPM-66A和In-CPM-66A,研究材料从CH_(4)/N_(2)混合物中富集CH_(4)的性能,利用PXRD、77 K N_(2)吸附、TGA和FTIR光谱对材料的结构进行了表征。IAST选择性计算表明,In-CPM-66A和Sc-CPM-66A的CH_(4)/N_(2)选择性达到6.0。受益于材料表面存在的大量的甲基基团,两种材料对CH_(4)的吸附热低于被报道的大部分材料,材料与甲烷分子之间弱的相互作用有利于吸附剂的脱附再生。穿透实验进一步表明,CPM-66A可以实现动态条件下CH_(4)/N_(2)混合物的分离,循环穿透实验显示该类材料具有良好的可重复性。展开更多
基金The financial support from the Natural Science Foundation of Shandong Province (ZR2020KB003)
文摘NF_(3)is commonly used as an etching and cleaning gas in semiconductor industry,however it is a strongly greenhouse gas.Therefore,the destruction of disposal NF_(3)is an urgent task to migrate the greenhouse effect.Among the technologies for NF_(3)abatement,the destructive sorption of NF_(3)over metal oxides sorbents is an effective way.Thus,the search for a highly reactive and utilized sorbent for NF_(3)destruction is in great demand.In this work,AlOOH supported on carbon-sphere(AlOOH/CS)as precursors were synthesized hydrothermally and heat-treated to prepare the Al_(2)O_(3)sorbents.The influence of AlOOH/CS hydrothermal temperatures on the reactivity of derived Al_(2)O_(3)sorbents for NF_(3)destruction was investigated,and it is shown that the Al2O3 from AlOOH/CS hydro-thermalized at 120℃is superior to others.Subsequently,the optimized Al_(2)O_(3)was covered by Mn(OH)x to prepare Mn/Al_(2)O_(3)sorbents via changing hydrothermal temperatures and Mn loadings.The results show that the Mn/Al_(2)O_(3)sorbents are more utilized than bare Al_(2)O_(3)in NF_(3)destructive sorption due to the promotional effect of Mn_(2)O_(3)as surface layer on the fluorination of Al_(2)O_(3)as substrate,especially the optimal 5%Mn/Al2O3(160℃)exhibits a utilization percentage as high as 90.4%,and remarkably exceeds all the sorbents reported so far.These findings are beneficial to develop more efficient sorbents for the destruction of NF_(3).
基金financially supported by the National Natural Science Foundation of China(No.52074078)the National Key R&D Program of China(No.2021YFC2901200)+4 种基金the Applied Fundamental Research Program of Liaoning Province(No.2023JH2/101600002)the Liaoning Provincial Natural Science Foundation of China(No.2022-YQ-09)the Shenyang Young Middle-Aged Scientific and Technological Innovation Talent Support Program,China(No.RC220491)the Liaoning Province Steel Industry-University-Research Innovation Alliance Cooperation Project of Bensteel Group,China(No.KJBLM202202)the Fundamental Research Funds for the Central Universities,China(Nos.N2201023,N2325009)。
文摘Steelmaking industry faces urgent demands for both steel slag utilization and CO_(2)abatement.Ca and Mg of steel slag can be extracted by acid solution and used to prepare sorbents for CO_(2)capture.In this work,the calcium-based sorbents were prepared from stainless steel slag leachate by co-precipitation,and the initial CO_(2)chemisorption capacity of the calcium-based sorbent prepared from steel slag with the Ca and Mg molar ratio of 3.64:1 was 0.40 g/g.Moreover,the effect of Ca/Mg molar ratio on the morphology,structure,and CO_(2)chemisorption capacity of the calcium-based sorbents were investigated.The results show that the optimal Ca/Mg molar ratio of sorbent for CO_(2)capture was4.2:1,and the skeleton support effect of MgO in calcium-based sorbents was determined.Meanwhile,the chemisorption kinetics of the sorbents was studied using the Avrami-Erofeev model.There were two processes of CO_(2)chemisorption,and the activation energy of the first stage(reaction control)was found to be lower than that of the second stage(diffusion control).
文摘Using environment-friendly and low-cost biowaste adsorbents as toxic metal ion removal substrates from aqueous solutions has a great economic advantage. This work evaluated pumpkin and potato peel biowastes for the adsorption of cadmium ions. The biowastes were treated with acid or base. Batch experiments were carried out by introducing a known concentration of metal ion solution into the biowaste sorbent at various pH levels. The pH and metal ion concentration was monitored with pH and cadmium ion-selective electrode continuously for two hours, and the final concentration for the metal ion after 24 hours was measured with the cadmium electrode and then confirmed with ICP-OES. L-type isotherms were obtained that fit to Freundlich model. Adsorption isotherms showed chemical adsorption and the kinetics following the second order model. Equilibrium adsorption capacity is higher than 29 mg/g at pH 5.6 when the initial concentration is 220 ppm. Dynamic cadmium adsorption capacity is 17 mg/g from aqueous solution when the feed solution is 220 ppm with pumpkin peel biowaste sorbent. The biowaste materials can be regenerated with acid washing.
文摘提出了滤过型固相萃取柱净化-超高效液相色谱-串联质谱法同时测定鸡蛋中全氟丁酸、全氟戊酸、全氟己酸、全氟庚酸、全氟辛酸、全氟壬酸、全氟癸酸、全氟十一酸、全氟十二酸、全氟十三酸、全氟十四酸、全氟丁烷磺酸、全氟己烷磺酸、全氟庚烷磺酸、全氟辛烷磺酸等15种全氟化合物含量的方法。鸡蛋样品(2 g)中加入0.1 mL 20.0μg·L^(-1)同位素内标混合溶液,经10 mL 80%(体积分数)乙腈溶液振荡和超声提取后,离心;分取5 mL滤液,直接过滤过型Captive EMR-Lipid柱净化,收集流出液,氮吹至近干,加入500μL甲醇复溶,经涡旋、离心处理后测定。采用Agilent Eclipse Plus C_(18)RRHD色谱柱(100 mm×2.1 mm,1.8μm)分离,以不同体积比的2 mmol·L^(-1)乙酸铵溶液和甲醇的混合溶液梯度洗脱,在电喷雾离子源负离子扫描模式下,以多反应监测模式检测,同位素内标法定量。结果表明:15种全氟化合物标准曲线的线性范围均为0.125~20.0μg·L^(-1),测定下限(10S/N)为0.05~0.16μg·kg^(-1);在0.500,4.00,16.0μg·kg^(-1)加标浓度水平下,15种目标物的回收率为78.0%~111%,测定值的相对标准偏差(n=6)为0.87%~14%。
基金The National Natural Science Foundation of China(No.51376003)
文摘A kind of industrial solid waste, i.e., carbide slag, was used as CaO precursor to synthesize CO2 sorbent. The highly reactive synthetic sorbent was prepared from carbide slag, aluminum nitrate hydrate and glycerol water solution by the combustion synthesis method. The results show that the synthetic sorbent exhibits a much higher CO2 capture capacity compared with carbide slag. The CO2 capture capacity and the carbonation conversion of the synthetic sorbent are 0. 38 g/g and 0. 70 after 50 cycles, which are 1.8 and 2. 1 times those of carbide slag. The average carbonation conversion and the CO2 capture efficiency of the synthetic sorbent are higher than those of carbide slag with the same sorbent flow ratios. The required sorbent flow ratios are lower for synthetic sorbent to achieve the same CO2 capture efficiency compared with carbide slag. With the same sorbent flow ratio and CO2 capture efficiency, the energy requirement in calciner for the synthetic sorbent is less than that for carbide slag.
文摘低浓度煤层气的提质利用对缓解国内天然气不足的现状具有重要意义,然而煤层气中存在的氮气杂质限制了该类资源的进一步应用,进行低浓度煤层气中CH_(4)/N_(2)混合物的分离至关重要。制备了两种具有弱极性超微孔的金属有机框架材料Sc-CPM-66A和In-CPM-66A,研究材料从CH_(4)/N_(2)混合物中富集CH_(4)的性能,利用PXRD、77 K N_(2)吸附、TGA和FTIR光谱对材料的结构进行了表征。IAST选择性计算表明,In-CPM-66A和Sc-CPM-66A的CH_(4)/N_(2)选择性达到6.0。受益于材料表面存在的大量的甲基基团,两种材料对CH_(4)的吸附热低于被报道的大部分材料,材料与甲烷分子之间弱的相互作用有利于吸附剂的脱附再生。穿透实验进一步表明,CPM-66A可以实现动态条件下CH_(4)/N_(2)混合物的分离,循环穿透实验显示该类材料具有良好的可重复性。
