The CeO_2-ZrO_2 solid solutions were prepared by a reverse microemulsion method. The effect of preparation parameters on the surface area and crystalline form of the solid solutions were studied by the BET surface are...The CeO_2-ZrO_2 solid solutions were prepared by a reverse microemulsion method. The effect of preparation parameters on the surface area and crystalline form of the solid solutions were studied by the BET surface area and XRD analysis. The studies indicate that the separation of the microemulsion phase during the preparation procedure can decrease the specific surface area of sample, adding hydrogen peroxide in the matrix solution can increase the specific surface area and stability of sample. The surface area of sample calcined at 550 ℃ for 5 h is 149 m^2·g^(-1), and that calcined at 900 ℃ for 6 h is 88 m^2·g^(-1). The sample with tetragonal symmetry Ce_(0.5)Zr_(0.5)O_2 phase has a higher stability.展开更多
Vacuum loading has been examined as a way of preparing uniformly consolidated soft clay samples. The facility and loading procedure are described in this paper. An analytical solution to the three dimensional consolid...Vacuum loading has been examined as a way of preparing uniformly consolidated soft clay samples. The facility and loading procedure are described in this paper. An analytical solution to the three dimensional consolidation equation is derived for estimating the degree of consolidation of the soil sample with vacuum loading. The given example shows that the predicted degree of consolidation of a soft clay bulk with vacuum loading is close to that measured in the consolidation process.展开更多
Although previous investigations of the trace elements in snow and ice from the Qinghai-Tibetan Plateau obtained interesting information about pollution from human activities on the plateau, most were based on traditi...Although previous investigations of the trace elements in snow and ice from the Qinghai-Tibetan Plateau obtained interesting information about pollution from human activities on the plateau, most were based on traditional acidification methods.To emphasize the influence of the different sample-preparation methods on the records of trace elements and rare earth elements, snow samples were collected from glaciers on the Qinghai-Tibetan Plateau in China and prepared using two methods: traditional acidification and total digestion. Concentrations of 18 trace elements(Al, Ti, Fe, Rb, Sr, Ba, V, Cr, Mn, Li,Cu, Co, Mo, Cs, Sb, Pb, Tl, and U), along with 14 rare earth elements(REEs: La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er,Tm, Yb, and Lu), Y, and Th in the snow samples, were measured using inductively coupled plasma-sector field mass spectrometry(ICP-SFMS). The results showed that the mass fraction of the trace elements(defined as ratio of concentration in the acid-leachable fraction to that in the digested sample) such as Mo, Ti, Al, Rb, and V, varied from 0.06 to 0.5. The mass fraction of other trace elements varied from about 0.6 to more than 0.9; those of the REEs, Y, and Th varied from 0.34 to0.75. Lower mass fractions will lead to an overestimated contribution of other sources, especially human activities, and the underestimated fluxes of these trace elements(especially REEs, Y, and Th, as well as dust) if the REEs are used as the proxy for the crust dust. The two sample-preparation methods exhibited different REE normalized distribution patterns,REE ratios, and provenance-tracing results. The REE normalized distribution patterns and proxies in the digested samples are more reliable and integrated than those found in traditional acidification method for dust-provenance tracing.展开更多
The sample preparation of samples conlaining bovine serum albumin（BSA）,e.g..as used in transdermal Franz diffusion cell（FDC） solutions,was evaluated using an analytical qualily-by-design（QbD）approach.Traditional...The sample preparation of samples conlaining bovine serum albumin（BSA）,e.g..as used in transdermal Franz diffusion cell（FDC） solutions,was evaluated using an analytical qualily-by-design（QbD）approach.Traditional precipitation of BSA by adding an equal volume of organic solvent,often successfully used with conventional HPLC-PDA,was found insufficiently robust when novel fused-core HPLC and/or UPLC-MS methods were used.In this study,three factors（acetonitrile（%）.formic acid（%） and boiling time（min）） were included in the experimental design to determine an optimal and more suitable sample treatment of BSAcontaining FDC solutions.Using a QbD and Derringer desirability（D） approach,combining BSA loss,dilution factor and variability,we constructed an optimal working space with the edge of failure defined as D〈0.9.The design space is modelled and is confirmed to have an ACN range of 83 ± 3% and FA content of 1 ±0.25%.展开更多
Sample preparation by fusion for XRF analysis is all about knowing the exact weights of the sample and the flux (sample-to-flux ratio). The whole analytical chain, including the weighing step in sample preparation pri...Sample preparation by fusion for XRF analysis is all about knowing the exact weights of the sample and the flux (sample-to-flux ratio). The whole analytical chain, including the weighing step in sample preparation prior to fusion, is of crucial importance to get precise and accurate x-ray fluorescence (XRF) results. Consequently, the weighing method will affect the quality of the analytical results given by the spectrometer. In this study, the effects of different weighing methods on the precision (RSD) of the obtained XRF results are compared to determine the best weighing method for sample preparation by fusion in terms of comparable precisions in the XRF results.展开更多
The quantitative determination of heavy metals in aquatic products is of great importance for food security issues.Laser-induced breakdown spectroscopy(LIBS)has been used in a variety of foodstuff analysis,but is stil...The quantitative determination of heavy metals in aquatic products is of great importance for food security issues.Laser-induced breakdown spectroscopy(LIBS)has been used in a variety of foodstuff analysis,but is still limited by its low sensitivity when targeting trace heavy metals.In this work,we compare three sample enrichment methods,namely drying,carbonization,and ashing,for increasing detection sensitivity by LIBS analysis for Pb and Cr in oyster samples.The results demonstrate that carbonization can remove a significant amount of the contributions of organic elements C,H,N and O;meanwhile,the signals of the metallic elements such as Cu,Pb,Sr,Ca,Cr and Mg are enhanced by3–6 times after carbonization,and further enhanced by 5–9 times after ashing.Such enhancement is not only due to the more concentrated metallic elements in the sample compared to the dried ones,but also the unifying of the matter in carbonized and ashed samples from which higher plasma temperature and electron density are observed.This condition favors the detection of trace elements.According to the calibration curves with univariate and multivariate analysis,the ashing method is considered to be the best choice.The limits of detection of the ashing method are 0.52 mg kg-1 for Pb and0.08 mg kg-1 for Cr,which can detect the presence of heavy metals in the oysters exceeding the maximum limits of Pb and Cr required by the Chinese national standard.This method provides a promising application for the heavy metal contamination monitoring in the aquatic product industry.展开更多
Over the past decade,the swift advancement of metabolomics can be credited to significant progress in technologies such as mass spectrometry,nuclear magnetic resonance,and multivariate statistics.Currently,metabolomic...Over the past decade,the swift advancement of metabolomics can be credited to significant progress in technologies such as mass spectrometry,nuclear magnetic resonance,and multivariate statistics.Currently,metabolomics garners widespread application across diverse fields including drug research and development,early disease detection,toxicology,food and nutrition science,biology,prescription,and chinmedomics,among others.Metabolomics serves as an effective characterization technique,offering insights into physiological process alterations in vivo.These changes may result from various exogenous factors like environmental conditions,stress,medications,as well as endogenous elements including genetic and protein-based influences.The potential scientific outcomes gleaned from these insights have catalyzed the formulation of innovative methods,poised to further broaden the scope of this domain.Today,metabolomics has evolved into a valuable and widely accepted instrument in the life sciences.However,comprehensive reviews focusing on the sample preparation and analytical methodologies employed in metabolomics within the life sciences are surprisingly scant.This review aims to fill that gap,providing an overview of current trends and recent advancements in metabolomics.Particular emphasis is placed on sample preparation,sophisticated analytical techniques,and their applications in life science research.展开更多
文摘The CeO_2-ZrO_2 solid solutions were prepared by a reverse microemulsion method. The effect of preparation parameters on the surface area and crystalline form of the solid solutions were studied by the BET surface area and XRD analysis. The studies indicate that the separation of the microemulsion phase during the preparation procedure can decrease the specific surface area of sample, adding hydrogen peroxide in the matrix solution can increase the specific surface area and stability of sample. The surface area of sample calcined at 550 ℃ for 5 h is 149 m^2·g^(-1), and that calcined at 900 ℃ for 6 h is 88 m^2·g^(-1). The sample with tetragonal symmetry Ce_(0.5)Zr_(0.5)O_2 phase has a higher stability.
文摘Vacuum loading has been examined as a way of preparing uniformly consolidated soft clay samples. The facility and loading procedure are described in this paper. An analytical solution to the three dimensional consolidation equation is derived for estimating the degree of consolidation of the soil sample with vacuum loading. The given example shows that the predicted degree of consolidation of a soft clay bulk with vacuum loading is close to that measured in the consolidation process.
基金supported by grants provided by the National Natural Science Foundation of China(Grant Nos.41276194,40771046,and 40601021)
文摘Although previous investigations of the trace elements in snow and ice from the Qinghai-Tibetan Plateau obtained interesting information about pollution from human activities on the plateau, most were based on traditional acidification methods.To emphasize the influence of the different sample-preparation methods on the records of trace elements and rare earth elements, snow samples were collected from glaciers on the Qinghai-Tibetan Plateau in China and prepared using two methods: traditional acidification and total digestion. Concentrations of 18 trace elements(Al, Ti, Fe, Rb, Sr, Ba, V, Cr, Mn, Li,Cu, Co, Mo, Cs, Sb, Pb, Tl, and U), along with 14 rare earth elements(REEs: La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er,Tm, Yb, and Lu), Y, and Th in the snow samples, were measured using inductively coupled plasma-sector field mass spectrometry(ICP-SFMS). The results showed that the mass fraction of the trace elements(defined as ratio of concentration in the acid-leachable fraction to that in the digested sample) such as Mo, Ti, Al, Rb, and V, varied from 0.06 to 0.5. The mass fraction of other trace elements varied from about 0.6 to more than 0.9; those of the REEs, Y, and Th varied from 0.34 to0.75. Lower mass fractions will lead to an overestimated contribution of other sources, especially human activities, and the underestimated fluxes of these trace elements(especially REEs, Y, and Th, as well as dust) if the REEs are used as the proxy for the crust dust. The two sample-preparation methods exhibited different REE normalized distribution patterns,REE ratios, and provenance-tracing results. The REE normalized distribution patterns and proxies in the digested samples are more reliable and integrated than those found in traditional acidification method for dust-provenance tracing.
基金the Special Research Fund of Ghent University(BOF 01D23812 to Lien Taevernier and BOF O1J22510 to Evelien Wynendaele and Professor Bart De Spiegeleer)the Institute for the Promotion of Innovation through Science and Technology in Flanders(IWT 101529 to Matthias D'Hondt)for their financial funding
文摘The sample preparation of samples conlaining bovine serum albumin（BSA）,e.g..as used in transdermal Franz diffusion cell（FDC） solutions,was evaluated using an analytical qualily-by-design（QbD）approach.Traditional precipitation of BSA by adding an equal volume of organic solvent,often successfully used with conventional HPLC-PDA,was found insufficiently robust when novel fused-core HPLC and/or UPLC-MS methods were used.In this study,three factors（acetonitrile（%）.formic acid（%） and boiling time（min）） were included in the experimental design to determine an optimal and more suitable sample treatment of BSAcontaining FDC solutions.Using a QbD and Derringer desirability（D） approach,combining BSA loss,dilution factor and variability,we constructed an optimal working space with the edge of failure defined as D〈0.9.The design space is modelled and is confirmed to have an ACN range of 83 ± 3% and FA content of 1 ±0.25%.
文摘Sample preparation by fusion for XRF analysis is all about knowing the exact weights of the sample and the flux (sample-to-flux ratio). The whole analytical chain, including the weighing step in sample preparation prior to fusion, is of crucial importance to get precise and accurate x-ray fluorescence (XRF) results. Consequently, the weighing method will affect the quality of the analytical results given by the spectrometer. In this study, the effects of different weighing methods on the precision (RSD) of the obtained XRF results are compared to determine the best weighing method for sample preparation by fusion in terms of comparable precisions in the XRF results.
基金supported by the National Key Research and Development Program of China(No.2019YFD0901701)National Natural Science Foundation of China(Nos.12174359and 61975190)Provincial Key Research and Development Program of Shandong,China(No.2019GHZ010)。
文摘The quantitative determination of heavy metals in aquatic products is of great importance for food security issues.Laser-induced breakdown spectroscopy(LIBS)has been used in a variety of foodstuff analysis,but is still limited by its low sensitivity when targeting trace heavy metals.In this work,we compare three sample enrichment methods,namely drying,carbonization,and ashing,for increasing detection sensitivity by LIBS analysis for Pb and Cr in oyster samples.The results demonstrate that carbonization can remove a significant amount of the contributions of organic elements C,H,N and O;meanwhile,the signals of the metallic elements such as Cu,Pb,Sr,Ca,Cr and Mg are enhanced by3–6 times after carbonization,and further enhanced by 5–9 times after ashing.Such enhancement is not only due to the more concentrated metallic elements in the sample compared to the dried ones,but also the unifying of the matter in carbonized and ashed samples from which higher plasma temperature and electron density are observed.This condition favors the detection of trace elements.According to the calibration curves with univariate and multivariate analysis,the ashing method is considered to be the best choice.The limits of detection of the ashing method are 0.52 mg kg-1 for Pb and0.08 mg kg-1 for Cr,which can detect the presence of heavy metals in the oysters exceeding the maximum limits of Pb and Cr required by the Chinese national standard.This method provides a promising application for the heavy metal contamination monitoring in the aquatic product industry.
基金supported by the Science Foundation of Heilongjiang Administration of Traditional Chinese Medicine(No.2018-21).
文摘Over the past decade,the swift advancement of metabolomics can be credited to significant progress in technologies such as mass spectrometry,nuclear magnetic resonance,and multivariate statistics.Currently,metabolomics garners widespread application across diverse fields including drug research and development,early disease detection,toxicology,food and nutrition science,biology,prescription,and chinmedomics,among others.Metabolomics serves as an effective characterization technique,offering insights into physiological process alterations in vivo.These changes may result from various exogenous factors like environmental conditions,stress,medications,as well as endogenous elements including genetic and protein-based influences.The potential scientific outcomes gleaned from these insights have catalyzed the formulation of innovative methods,poised to further broaden the scope of this domain.Today,metabolomics has evolved into a valuable and widely accepted instrument in the life sciences.However,comprehensive reviews focusing on the sample preparation and analytical methodologies employed in metabolomics within the life sciences are surprisingly scant.This review aims to fill that gap,providing an overview of current trends and recent advancements in metabolomics.Particular emphasis is placed on sample preparation,sophisticated analytical techniques,and their applications in life science research.
