A systematic investigation on the mechanism of dynamic liquid dispersing process via theoretical and experimental approach is presented.The experiments include weak and strong constrained scenarios using the high-spee...A systematic investigation on the mechanism of dynamic liquid dispersing process via theoretical and experimental approach is presented.The experiments include weak and strong constrained scenarios using the high-speed camera technique and the flash X-ray radiography technique.Based on dynamic analysis,one-dimensional characteristics analysis and some numerical simulations on the propagating processes of blast waves before the container shell rupturing,further and detailed analyses of the experimental results are presented.The effects of the liquid viscosity on the dynamic dispersing flow are also analyzed,and the spall fracture mechanism is explored.Thus,the dominating forces determining the dispersing liquid flow are revealed,that is,the stretching and shearing action due to the interaction of two reflecting rarefaction waves in opposite propagating directions.The influence of container shell strength on the dispersing liquid flow is also investigated,and the characters of cavitation layered in liquid before shell rupturing are uncovered.Results revealed that different shell material results in different cavitating layers.Then the different cavitating layers drive the different dynamic liquid dispersing process coming into being.The metastable liquid states caused by pressure drop and cavitation generation are discussed.展开更多
In order to clarify the dispersion of SiC particles in straight-blade mechanical stirring of A1-SiCp liquid, the dispersion of SiC particles in A356-3.5% SiCp （volume fraction） liquid in a cylindrical crucible was s...In order to clarify the dispersion of SiC particles in straight-blade mechanical stirring of A1-SiCp liquid, the dispersion of SiC particles in A356-3.5% SiCp （volume fraction） liquid in a cylindrical crucible was studied. The relationship between rotating speed of stirrer and radial relative deviation of SiCp content in A356 liquid between the center and the periphery of crucible was established in the conditions of 35° for the gradient angle a of blade and 10 mm/s for the speed of moving up and down of stirrer. The results show that the radial relative deviation of SiCp content increases gradually with increasing the rotating speed of stirrer. When the rotating speed of stirrer is 200 r/min, the vertical dispersion of SiC particles in A356 liquid is even, but the radial relative deviation of SiCp content is 0.24. Consequently, the northomogeneous dispersion of SiC particles in A356 liquid is mainly resulted from the nonhomogeneous radial dispersion of SiC particles.展开更多
为简化前处理过程,降低方法的检出限,进行了题示研究。采集鱼塘底泥样品,混匀、缩分、冷冻干燥、除杂、研磨、过筛后混匀,分取5.00 g,加入10.0μg·L^(-1)^(13)C_(6)-氯硝柳胺水合物标准溶液0.2 m L和含2.0%(体积分数)氨水的乙腈溶...为简化前处理过程,降低方法的检出限,进行了题示研究。采集鱼塘底泥样品,混匀、缩分、冷冻干燥、除杂、研磨、过筛后混匀,分取5.00 g,加入10.0μg·L^(-1)^(13)C_(6)-氯硝柳胺水合物标准溶液0.2 m L和含2.0%(体积分数)氨水的乙腈溶液20 m L,涡旋1 min,超声10 min,离心8 min。上清液于45℃旋蒸至近干,加入2.00 m L 70%(体积分数)乙腈溶液涡旋溶解残留物,再加入200 mg C18涡旋振荡30 s,离心5 min。收集上清液,过0.22μm有机滤膜,滤液采用高效液相色谱-串联质谱法测定。在色谱分析中,以Waters Atiantis^(TM) d C_(18)色谱柱为固定相,水-乙腈体系为流动相进行梯度洗脱;在质谱分析中,以电喷雾离子源负离子(ESI-)模式电离,选择反应监测(SRM)模式检测,内标法定量。结果显示,氯硝柳胺的质量浓度在0.20~50.00μg·L^(-1)内和其定量离子峰面积与同位素内标定量离子峰面积的比值呈线性关系,检出限(3S/N)为0.2μg·kg^(-1)。按照标准加入法进行回收试验,回收率为92.1%~113%,测定值的相对标准偏差(n=6)为1.6%~5.9%。方法用于实际样品的分析,检出的氯硝柳胺的质量分数为0.580~2.18 mg·kg^(-1)。展开更多
建立了液相色谱-串联质谱(LC-MS/MS)手性拆分和测定水产品中奥沙西泮和替马西泮对映体残留量的分析方法。样品经乙腈提取2次,40℃条件下氮气浓缩至近干,残渣加入2 mL 50%乙腈-水溶液溶解,采用分散固相萃取净化,LC-MS/MS测定。使用Enanti...建立了液相色谱-串联质谱(LC-MS/MS)手性拆分和测定水产品中奥沙西泮和替马西泮对映体残留量的分析方法。样品经乙腈提取2次,40℃条件下氮气浓缩至近干,残渣加入2 mL 50%乙腈-水溶液溶解,采用分散固相萃取净化,LC-MS/MS测定。使用EnantioPAK■Y1-R(5μm,150 mm×4.6 mm)手性色谱柱,乙腈和0.1%甲酸-5 mmol/L乙酸铵溶液作为流动相,采用等度洗脱方式实现奥沙西泮和替马西泮手性对映体的拆分。目标对映体采用电喷雾正离子(ESI^(+))模式电离,多反应监测(MRM)模式下,内标法测定。目标对映体在0.5~50μg/L质量浓度范围内线性关系良好,相关系数(r^(2))均不低于0.9990。水产品中对映体的检出限和定量下限分别为0.2μg/kg和0.5μg/kg。在5种空白基质中添加低、中、高浓度水平的目标对映体,样品平均加标回收率为82.6%~107%,相对标准偏差(RSD,n=6)为1.6%~9.2%。该方法灵敏可靠、适用性强,可用于不同水产品中奥沙西泮和替马西泮对映体的分析。展开更多
采用液液萃取(liquid-liquid extraction,LLE)和顶空固相微萃取(headspace solid-phase microextraction,HS-SPME)结合全二维气相色谱-飞行时间质谱(comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometr...采用液液萃取(liquid-liquid extraction,LLE)和顶空固相微萃取(headspace solid-phase microextraction,HS-SPME)结合全二维气相色谱-飞行时间质谱(comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry,GC×GC-TOFMS)技术解析了天龙泉米香型白酒挥发性组分特征。采用该技术并结合多种检索比对方式在天龙泉米香型白酒中鉴定出挥发性化合物505种,其中339种为天龙泉米香型白酒的潜在香气活性组分,包括86种酯类、50种芳香族、42种醇类、40种醛类、32种含氧杂环化合物、30种酮类、25种萜烯类、19种有机酸类、11种含硫化合物和4种含氮杂环化合物,表明了米香型白酒中香气成分的多样性和复杂性。在挥发性香气化合物含量角度上,不同贮存期的米香型白酒样品呈现明显差异,在时间维度上具有一定规律。其中,变化较大的化合物是醇类化合物、酯类化合物和醛类化合物,可能是受到了企业生产工艺的调整和陈化过程中发生的化学反应共同影响。该研究更深入地认识了米香型白酒的挥发性风味物质,丰富了米香型白酒风味化学的研究体系。展开更多
为实现饮料中常用防腐剂和抗氧化剂的同时检测,进行了题示研究。取饮料样品5.000 g,加入1.0 m L 50%(体积分数)盐酸溶液和1.0 g氯化钠,超声溶解后快速注入含900μL三氯甲烷(萃取剂)和900μL乙醇(分散剂)的混合萃取剂,涡旋3 min,离心2 m...为实现饮料中常用防腐剂和抗氧化剂的同时检测,进行了题示研究。取饮料样品5.000 g,加入1.0 m L 50%(体积分数)盐酸溶液和1.0 g氯化钠,超声溶解后快速注入含900μL三氯甲烷(萃取剂)和900μL乙醇(分散剂)的混合萃取剂,涡旋3 min,离心2 min,收集底部三氯甲烷相。再加入900μL三氯甲烷重复萃取一次,合并两次三氯甲烷相,于40℃氮吹至干。加入1.0 m L乙酸乙酯复溶,过0.22μm尼龙滤膜,滤液采用气相色谱-质谱法分析。6种防腐剂(山梨酸、苯甲酸、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯)和3种抗氧化剂(丁基羟基茴香醚、2,6-二叔丁基对甲酚、特丁基对苯二酚)在HP5-MS UI毛细管色谱柱上以程序升温条件分离,电子轰击离子源电离,选择离子监测模式检测,外标法定量。结果显示:9种添加剂的质量浓度均在1.0~100 mg·L^(-1)内与对应的定量离子的峰面积呈线性关系,检出限(3S/N)为0.07~0.22 mg·kg^(-1);以空白碳酸饮料、茶饮料和果汁饮料样品为基质进行3个浓度水平的加标回收试验,回收率为85.5%~105%,测定值的相对标准偏差(n=6)为1.2%~7.1%。方法用于22份实际样品的分析,在6份样品中检出了苯甲酸,在5份样品中检出了山梨酸,检出量均未超过GB 2760—2024规定的最大限量,且与标准方法GB 5009.28—2016的基本一致。展开更多
基金the support of National Nature Science Foundation of China, the support numbers are No. 10572149 and No.10676120the National Key Research and Development program of China (subject no. 2017YFC0209901) for its support to the work of this paper
文摘A systematic investigation on the mechanism of dynamic liquid dispersing process via theoretical and experimental approach is presented.The experiments include weak and strong constrained scenarios using the high-speed camera technique and the flash X-ray radiography technique.Based on dynamic analysis,one-dimensional characteristics analysis and some numerical simulations on the propagating processes of blast waves before the container shell rupturing,further and detailed analyses of the experimental results are presented.The effects of the liquid viscosity on the dynamic dispersing flow are also analyzed,and the spall fracture mechanism is explored.Thus,the dominating forces determining the dispersing liquid flow are revealed,that is,the stretching and shearing action due to the interaction of two reflecting rarefaction waves in opposite propagating directions.The influence of container shell strength on the dispersing liquid flow is also investigated,and the characters of cavitation layered in liquid before shell rupturing are uncovered.Results revealed that different shell material results in different cavitating layers.Then the different cavitating layers drive the different dynamic liquid dispersing process coming into being.The metastable liquid states caused by pressure drop and cavitation generation are discussed.
基金Project(50974010) supported by the National Natural Science Foundation of ChinaProject(3093023) supported by the Natural Science Foundation of Beijing,ChinaProject(2009JBM091) supported by the Fundamental Research Funds for the Central Universities of China
文摘In order to clarify the dispersion of SiC particles in straight-blade mechanical stirring of A1-SiCp liquid, the dispersion of SiC particles in A356-3.5% SiCp （volume fraction） liquid in a cylindrical crucible was studied. The relationship between rotating speed of stirrer and radial relative deviation of SiCp content in A356 liquid between the center and the periphery of crucible was established in the conditions of 35° for the gradient angle a of blade and 10 mm/s for the speed of moving up and down of stirrer. The results show that the radial relative deviation of SiCp content increases gradually with increasing the rotating speed of stirrer. When the rotating speed of stirrer is 200 r/min, the vertical dispersion of SiC particles in A356 liquid is even, but the radial relative deviation of SiCp content is 0.24. Consequently, the northomogeneous dispersion of SiC particles in A356 liquid is mainly resulted from the nonhomogeneous radial dispersion of SiC particles.
文摘为简化前处理过程,降低方法的检出限,进行了题示研究。采集鱼塘底泥样品,混匀、缩分、冷冻干燥、除杂、研磨、过筛后混匀,分取5.00 g,加入10.0μg·L^(-1)^(13)C_(6)-氯硝柳胺水合物标准溶液0.2 m L和含2.0%(体积分数)氨水的乙腈溶液20 m L,涡旋1 min,超声10 min,离心8 min。上清液于45℃旋蒸至近干,加入2.00 m L 70%(体积分数)乙腈溶液涡旋溶解残留物,再加入200 mg C18涡旋振荡30 s,离心5 min。收集上清液,过0.22μm有机滤膜,滤液采用高效液相色谱-串联质谱法测定。在色谱分析中,以Waters Atiantis^(TM) d C_(18)色谱柱为固定相,水-乙腈体系为流动相进行梯度洗脱;在质谱分析中,以电喷雾离子源负离子(ESI-)模式电离,选择反应监测(SRM)模式检测,内标法定量。结果显示,氯硝柳胺的质量浓度在0.20~50.00μg·L^(-1)内和其定量离子峰面积与同位素内标定量离子峰面积的比值呈线性关系,检出限(3S/N)为0.2μg·kg^(-1)。按照标准加入法进行回收试验,回收率为92.1%~113%,测定值的相对标准偏差(n=6)为1.6%~5.9%。方法用于实际样品的分析,检出的氯硝柳胺的质量分数为0.580~2.18 mg·kg^(-1)。
文摘采用液液萃取(liquid-liquid extraction,LLE)和顶空固相微萃取(headspace solid-phase microextraction,HS-SPME)结合全二维气相色谱-飞行时间质谱(comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry,GC×GC-TOFMS)技术解析了天龙泉米香型白酒挥发性组分特征。采用该技术并结合多种检索比对方式在天龙泉米香型白酒中鉴定出挥发性化合物505种,其中339种为天龙泉米香型白酒的潜在香气活性组分,包括86种酯类、50种芳香族、42种醇类、40种醛类、32种含氧杂环化合物、30种酮类、25种萜烯类、19种有机酸类、11种含硫化合物和4种含氮杂环化合物,表明了米香型白酒中香气成分的多样性和复杂性。在挥发性香气化合物含量角度上,不同贮存期的米香型白酒样品呈现明显差异,在时间维度上具有一定规律。其中,变化较大的化合物是醇类化合物、酯类化合物和醛类化合物,可能是受到了企业生产工艺的调整和陈化过程中发生的化学反应共同影响。该研究更深入地认识了米香型白酒的挥发性风味物质,丰富了米香型白酒风味化学的研究体系。
文摘为实现饮料中常用防腐剂和抗氧化剂的同时检测,进行了题示研究。取饮料样品5.000 g,加入1.0 m L 50%(体积分数)盐酸溶液和1.0 g氯化钠,超声溶解后快速注入含900μL三氯甲烷(萃取剂)和900μL乙醇(分散剂)的混合萃取剂,涡旋3 min,离心2 min,收集底部三氯甲烷相。再加入900μL三氯甲烷重复萃取一次,合并两次三氯甲烷相,于40℃氮吹至干。加入1.0 m L乙酸乙酯复溶,过0.22μm尼龙滤膜,滤液采用气相色谱-质谱法分析。6种防腐剂(山梨酸、苯甲酸、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯)和3种抗氧化剂(丁基羟基茴香醚、2,6-二叔丁基对甲酚、特丁基对苯二酚)在HP5-MS UI毛细管色谱柱上以程序升温条件分离,电子轰击离子源电离,选择离子监测模式检测,外标法定量。结果显示:9种添加剂的质量浓度均在1.0~100 mg·L^(-1)内与对应的定量离子的峰面积呈线性关系,检出限(3S/N)为0.07~0.22 mg·kg^(-1);以空白碳酸饮料、茶饮料和果汁饮料样品为基质进行3个浓度水平的加标回收试验,回收率为85.5%~105%,测定值的相对标准偏差(n=6)为1.2%~7.1%。方法用于22份实际样品的分析,在6份样品中检出了苯甲酸,在5份样品中检出了山梨酸,检出量均未超过GB 2760—2024规定的最大限量,且与标准方法GB 5009.28—2016的基本一致。
