With the help of FESEM, high resolution electron backscatter diffraction can investigate the grains/subgrains as small as a few tens of nanometers with a good angular resolution (~0.5°). Fast development of EBS...With the help of FESEM, high resolution electron backscatter diffraction can investigate the grains/subgrains as small as a few tens of nanometers with a good angular resolution (~0.5°). Fast development of EBSD speed (up to 1100 patterns per second) contributes that the number of published articles related to EBSD has been increasing sharply year by year. This paper reviews the sample preparation, parameters optimization and analysis of EBSD technique, emphasizing on the investigation of ultrafine grained and nanostructured materials processed by severe plastic deformation (SPD). Detailed and practical parameters of the electropolishing, silica polishing and ion milling have been summarized. It is shown that ion milling is a real universal and promising polishing method for EBSD preparation of almost all materials. There exists a maximum value of indexed points as a function of step size. The optimum step size depends on the magnification and the board resolution/electronic step size. Grains/subgrains and texture, and grain boundary structure are readily obtained by EBSD. Strain and stored energy may be analyzed by EBSD.展开更多
Gold has been present throughout the history of mankind and used to make jewelry and coins, and recently, acquired several industrial uses. The price of gold in international market had a significant increasing, surpa...Gold has been present throughout the history of mankind and used to make jewelry and coins, and recently, acquired several industrial uses. The price of gold in international market had a significant increasing, surpassing 100% in the last five years. Thereby, deposits with low levels of gold content, gold with complex associations or in a very fine particle size became exploitable again, allowing new projects and expansion of existing ones. However, for maximum process efficiency is indispensable a deep knowledge of the characteristics of these minerals and their behavior in face of beneficiation processes. Consequently, an accurate routine for mineralogical and technological characterization is essential.展开更多
Abstract Heavy metals in water can be deposited on graphite flakes, which can be used as an enrichment method for laser-induced breakdown spectroscopy (LIBS) and is studied in this paper. The graphite samples were p...Abstract Heavy metals in water can be deposited on graphite flakes, which can be used as an enrichment method for laser-induced breakdown spectroscopy (LIBS) and is studied in this paper. The graphite samples were prepared with an automatic device, which was composed of a loading and unloading module, a quantitatively adding solution module, a rapid heating and drying module and a precise rotating module. The experimental results showed that the sample preparation methods had no significant effect on sample distribution and the LIBS signal accumulated in 20 pulses was stable and repeatable. With an increasing amount of the sample solution on the graphite flake, the peak intensity at Cu I 324.75 nm accorded with the exponential function with a correlation coefficient of 0.9963 and the background intensity remained unchanged. The limit of detection (LOD) was calculated through linear fitting of the peak intensity versus the concentration. The LOD decreased rapidly with an increasing amount of sample solution until the amount exceeded 20 mL and the correlation coefficient of exponential function fitting was 0.991. The LOD of Pb, Ni, Cd, Cr and Zn after evaporating different amounts of sample solution on the graphite flakes was measured and the variation tendency of their LOD with sample solution amounts was similar to the tendency for Cu. The experimental data and conclusions could provide a reference for automatic sample preparation and heavy metal in situ detection.展开更多
A protocol for enrichment and adsorption of karyocyte from whole blood by using magnetic nanometer beads as solid phase absorbents was presented. The PCR amplification could be accomplished by using the nanobeads wit...A protocol for enrichment and adsorption of karyocyte from whole blood by using magnetic nanometer beads as solid phase absorbents was presented. The PCR amplification could be accomplished by using the nanobeads with karyocyte as template directly and the PCR products were applied on an oligonucleotide array to do gene typing. The HLA A PCR amplification system and a small HLA A oligonucleotide microarray were applied as the platform and an experiment protocol of separating karyocyte from whole blood using the magnetic nanometer beads (Fe 2O 3) were set up. The experimental conditions were also discussed. It showed that pH level of PBS eluent, Taq enzyme quantity and fragment length of products could influent the amplification results, and the magnetic nano beads could succeed in sample preparation in microarray to provide a promising way in automatic detection and lab on a chip.展开更多
The procedures of sample preparation for isotopic determination of boron in clay sediments is very cumbersome, by far, there haven't been relevant reports on that. In order to establish an effective method for sam...The procedures of sample preparation for isotopic determination of boron in clay sediments is very cumbersome, by far, there haven't been relevant reports on that. In order to establish an effective method for sample preparation, a series of experiments were carried out. In this paper, boron in clay sediments was extracted with HCl solution and purified by two-step ion exchange method. Extracted HCl solution should be adjusted to alkalescency before passing through the Amberlite IRA 743 resin column due to the fact that Amberlite IRA 743 resin absorbs boron only from alkalescent solution. However, a mass of hydroxides of Al and Fe will be precipitated when the extracted HCl solution becomes alkalescent. Hydroxides of Al and Fe have a strong adsorption capacity for boron, which can cause boron isotope fractionation. To treat precipitated hydroxides of Al and Fe, four procedures, namely direct ion exchange (DRIE), decationizing ion exchange (DCIE), once sedimentation ion exchange (OSIE) and repeated sedimentation ion exchange (RSIE) were used and assessed. The influences of the four procedures on separation and extraction and isotopic composition of boron in experimental solutions and clay sediments were also discussed. According to the results, the DRIE, DCIE and OSIE are improper. The result of sample determination indicates that when extracting boron via RSIE, with the increase of precipitation times, there's an obvious decrease in boron content in the precipitated hydroxides while a sharp increase in recovery of boron and it is favorable for weakening the influence of boron isotope fractionation. But the process of RSIE is time consuming and it may introduce boron. It needs further research to establish a more effective sample preparation method for isotopic deter- mination of boron in clay sediments.展开更多
1 Scope This standard specifies the definition and test methods of flowability of dense and insulating refractory castables, and moulding equipment, moulding methods, curing and drying conditions of castables samples.
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
Acetylcholine is an essential neurotransmitter found throughout the nervous system. Its action on postsynaptic receptors is regulated through hydrolysis by various carboxylesterases, especially cholinesterases (ChEs)....Acetylcholine is an essential neurotransmitter found throughout the nervous system. Its action on postsynaptic receptors is regulated through hydrolysis by various carboxylesterases, especially cholinesterases (ChEs). The acute toxicity of organophosphate (OP) compounds is directly linked to their action as inhibitors of ChE. One widely used assay for evaluating ChE activity is a spectrophotometric method developed by Ellman et al. When the enzyme source is from tissues or, in particular, blood, hemoglobin displays a spectrophotometric peak at the same wave-length used to analyze cholinergic activity. This creates a substantial background that interferes with the Ellman’s assay and must be overcome in order to accurately monitor cholinesterase activity. Herein, we directly compare blood processing methods: classical method (1.67 ± 0.30 U/mL) and HemogloBindTM treatment (1.51 ± 0.17 U/mL), and clearly demonstrate that pretreatment of blood samples with HemoglobindTM is both a sufficient and rapid sample preparation method for the assessment of ChE activity using the Ellman’s method.展开更多
Capillary electrophoresis (CE) coupled with mass spectrometry (MS) with a sheath liquid interface is nowadays recognized as a powerful separation technique for drugs and metabolites analysis in human urine and can...Capillary electrophoresis (CE) coupled with mass spectrometry (MS) with a sheath liquid interface is nowadays recognized as a powerful separation technique for drugs and metabolites analysis in human urine and can be applied in numerous fields such as clinical toxicology, drug substitution monitoring, forensic sciences and antidoping. With an acidic background electrolyte containing 15 mM ammonium formate at pH 2.5 and a sheath liquid consisting in a mixture of isopropanol/water (50:50, v/v) with 0.5% formic acid, CE-ESI-MS in positive mode demonstrated excellent performance for simultaneous analysis of basic drugs of abuse and metabolites in urine (e.g. cocaine, amphetamine, morphine and phase II metabolites). To achieve the desired level of sensitivity, two injection modes and three sample pre-treatments were evaluated. The detection of basic drugs and phase Ⅱ metabolites in diluted urine was achieved at concentrations above 1μg/mL. In order to enhance sensitivity, a sample preparation was required. A liquid-liquid extraction (LLE) was compared with solid-phase extraction. LLE was performed at alkaline pH and samples were electrokinetically injected. A chemometric approach (Doehlert design) was carried out in order to determine optimized injection parameters. Limits of detection (LOD) down to 10 ng/mL were reached with field-amplified sample injection but phase II metabolites were not extracted. Therefore, instead of LLE a SPE was performed on C 18 sorbent, and elution fraction after washing step containing phase Ⅱ metabolites was loaded on mixed-mode anion exchanger cartridges. After electrokinetic injection, this two-step SPE allowed LOD ca. 10 ng/mL for drugs and phase Ⅱ metabolites.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 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
In this study, a miniaturized analytical technique based on high density solvent based dispersive liquid-liquid microextraction (HD-DLLME) was developed for extraction of trace residues of multiclass pesticides includ...In this study, a miniaturized analytical technique based on high density solvent based dispersive liquid-liquid microextraction (HD-DLLME) was developed for extraction of trace residues of multiclass pesticides including three striazine herbicides, two organophosphate insecticides and two organochlorine fungicides from environmental water and sugarcane juice samples. The analytical method was validated and found to offer good linearity: R2 ≥ 0.991;repeatability varied from 0.73% - 5.28%;reproducibility varied from 1.14% - 8.74% and limit of detection ranged from 0.005 to 0.02 μg/L. Moreover, accuracy of the optimized method was evaluated and the recovery was varied from 80.39% - 114.05%. Analytical applications of this method to environmental waters and sugarcane juice samples indicate the presence of trace residues of ametryn in the lake water and sugarcane juice samples. Atrazine and ametryn were also detected in irrigation water.展开更多
This paper focuses on work related to post irradiation examination of 300-series austenitic stainless steel taken from reactor vessel internals of PWR. High neutron irradiation dose in NNP's leads to a degradation of...This paper focuses on work related to post irradiation examination of 300-series austenitic stainless steel taken from reactor vessel internals of PWR. High neutron irradiation dose in NNP's leads to a degradation of microstructure of the material in a nano-metric scale. Hence, it is important to characterize the irradiated materials to understand the physical basis of the degradation mechanisms. Microstructural characterization of neutron-irradiated materials by TEM requires enhanced sample preparation methodologies, which commonly needs general improvements regarding particular experiment to be performed. In this study, the authors have developed methodology specialized in 1 mm TEM thin foil preparation from a deformed shank of a broken miniaturized tensile specimen. TEM foil size in current studies is smaller than standard because of the small shank diameter and high radioactivity of the studied material. The reduction of the TEM foil radioactivity to minimum is crucial to perform EDX chemical analysis and to increase the EDX detector lifetime. This paper describes whole process from bulk sample handling, including remote-controlled material cutting in shielded hot-cells and disc polishing in glow-boxes, up to the final procedure of electrolytic-polishing of electron transparent 1 mm TEM foils. Eventually, results of TEM microanalysis of radiation-induced defects were present.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
Flue gas containing volatile elements, fine fly ash particulates not retained by particle control devices, and limestone are the most important sources of trace and major elements (TMEs) in wet flue gas desulphurizati...Flue gas containing volatile elements, fine fly ash particulates not retained by particle control devices, and limestone are the most important sources of trace and major elements (TMEs) in wet flue gas desulphurization (WFGD) gypsum. In this study, samples of gypsum slurry were separated into fine and coarse fractions. Multi-elemental analysis of 45 elements in the different size fractions of gypsum, slurry waters and lignite were performed by k0-INAA (k0-instrumental neutron activation analyses). The study found that the volatile elements (Hg, Se and halogens) in the flue gas accumulate in the fine fractions of gypsum. Moreover, the concentrations of most TMEs are considerably higher in the fine fractions compared to the coarse fractions. The exceptions are Ca and Sr that primarily originate from the limestone. Variations of TMEs in the finer fractions are dependent on the presence of CaSO4·2H2O that is the main constituent of the coarse fraction. Consequently, the content of TMEs in the fine fraction is highly dependent on the efficiency of separating the fine fraction from the coarse fraction. Separation of the finer fraction, representing about 10% of the total gypsum, offers the possibility to remove effectively TMEs from WFGD slurry.展开更多
A three-dimensional graphene-based composite was prepared by a simple one-step in-site reduced-oxide method under atmospheric pressure. The obtained hydrogel was modified with 4-amino-benzenesulfonic acid and connecte...A three-dimensional graphene-based composite was prepared by a simple one-step in-site reduced-oxide method under atmospheric pressure. The obtained hydrogel was modified with 4-amino-benzenesulfonic acid and connected with ethylenediamine, and freeze-dried into an aerogel, which was characterized. Then the surface interaction with platinum (Pt, IV) was explored. The obtained aerogel showed good adsorption for Pt (IV) at acid conditions, giving a rising to the adsorption rate > 98% while pH ≥ 6. Using hexadecyl trimethyl ammonium bromide of 2% (m/V) as an eluent to desorb the Pt (IV) from the surface of the aerogel, a desorption rate of 81.1% was obtained in this process. Urea, buffer aquation and other surfactants were used in the desorption experiment to understand the adsorption mechanism between the aerogel and Pt (IV). In this work, hydrogen bond, van der Waals force and electronic interaction force mainly drove the adsorption process. For obtaining more purified Pt (IV), we used 0.5% CTAB to desorb Pd (II). A new three-dimensional graphene-based composite was prepared and the surface interaction between Pt (IV) and composite was experimented for understanding the adsorption mechanism and exploring its potential application in sample preparation in low concentration.展开更多
基金Project (192450/I30) supported by the Norwegian Research Council under the Strategic University Program
文摘With the help of FESEM, high resolution electron backscatter diffraction can investigate the grains/subgrains as small as a few tens of nanometers with a good angular resolution (~0.5°). Fast development of EBSD speed (up to 1100 patterns per second) contributes that the number of published articles related to EBSD has been increasing sharply year by year. This paper reviews the sample preparation, parameters optimization and analysis of EBSD technique, emphasizing on the investigation of ultrafine grained and nanostructured materials processed by severe plastic deformation (SPD). Detailed and practical parameters of the electropolishing, silica polishing and ion milling have been summarized. It is shown that ion milling is a real universal and promising polishing method for EBSD preparation of almost all materials. There exists a maximum value of indexed points as a function of step size. The optimum step size depends on the magnification and the board resolution/electronic step size. Grains/subgrains and texture, and grain boundary structure are readily obtained by EBSD. Strain and stored energy may be analyzed by EBSD.
文摘Gold has been present throughout the history of mankind and used to make jewelry and coins, and recently, acquired several industrial uses. The price of gold in international market had a significant increasing, surpassing 100% in the last five years. Thereby, deposits with low levels of gold content, gold with complex associations or in a very fine particle size became exploitable again, allowing new projects and expansion of existing ones. However, for maximum process efficiency is indispensable a deep knowledge of the characteristics of these minerals and their behavior in face of beneficiation processes. Consequently, an accurate routine for mineralogical and technological characterization is essential.
基金supported by National Natural Science Foundation of China(No.60908018)National High Technology Research and Development Program of China(No.2013AA065502)Anhui Province Outstanding Youth Science Fund of China(No.1108085J19)
文摘Abstract Heavy metals in water can be deposited on graphite flakes, which can be used as an enrichment method for laser-induced breakdown spectroscopy (LIBS) and is studied in this paper. The graphite samples were prepared with an automatic device, which was composed of a loading and unloading module, a quantitatively adding solution module, a rapid heating and drying module and a precise rotating module. The experimental results showed that the sample preparation methods had no significant effect on sample distribution and the LIBS signal accumulated in 20 pulses was stable and repeatable. With an increasing amount of the sample solution on the graphite flake, the peak intensity at Cu I 324.75 nm accorded with the exponential function with a correlation coefficient of 0.9963 and the background intensity remained unchanged. The limit of detection (LOD) was calculated through linear fitting of the peak intensity versus the concentration. The LOD decreased rapidly with an increasing amount of sample solution until the amount exceeded 20 mL and the correlation coefficient of exponential function fitting was 0.991. The LOD of Pb, Ni, Cd, Cr and Zn after evaporating different amounts of sample solution on the graphite flakes was measured and the variation tendency of their LOD with sample solution amounts was similar to the tendency for Cu. The experimental data and conclusions could provide a reference for automatic sample preparation and heavy metal in situ detection.
文摘A protocol for enrichment and adsorption of karyocyte from whole blood by using magnetic nanometer beads as solid phase absorbents was presented. The PCR amplification could be accomplished by using the nanobeads with karyocyte as template directly and the PCR products were applied on an oligonucleotide array to do gene typing. The HLA A PCR amplification system and a small HLA A oligonucleotide microarray were applied as the platform and an experiment protocol of separating karyocyte from whole blood using the magnetic nanometer beads (Fe 2O 3) were set up. The experimental conditions were also discussed. It showed that pH level of PBS eluent, Taq enzyme quantity and fragment length of products could influent the amplification results, and the magnetic nano beads could succeed in sample preparation in microarray to provide a promising way in automatic detection and lab on a chip.
基金financially supported by the National Natural Science Foundation of China (Nos. 40976074 and 41173019)project for doctors in the western supported by CAS
文摘The procedures of sample preparation for isotopic determination of boron in clay sediments is very cumbersome, by far, there haven't been relevant reports on that. In order to establish an effective method for sample preparation, a series of experiments were carried out. In this paper, boron in clay sediments was extracted with HCl solution and purified by two-step ion exchange method. Extracted HCl solution should be adjusted to alkalescency before passing through the Amberlite IRA 743 resin column due to the fact that Amberlite IRA 743 resin absorbs boron only from alkalescent solution. However, a mass of hydroxides of Al and Fe will be precipitated when the extracted HCl solution becomes alkalescent. Hydroxides of Al and Fe have a strong adsorption capacity for boron, which can cause boron isotope fractionation. To treat precipitated hydroxides of Al and Fe, four procedures, namely direct ion exchange (DRIE), decationizing ion exchange (DCIE), once sedimentation ion exchange (OSIE) and repeated sedimentation ion exchange (RSIE) were used and assessed. The influences of the four procedures on separation and extraction and isotopic composition of boron in experimental solutions and clay sediments were also discussed. According to the results, the DRIE, DCIE and OSIE are improper. The result of sample determination indicates that when extracting boron via RSIE, with the increase of precipitation times, there's an obvious decrease in boron content in the precipitated hydroxides while a sharp increase in recovery of boron and it is favorable for weakening the influence of boron isotope fractionation. But the process of RSIE is time consuming and it may introduce boron. It needs further research to establish a more effective sample preparation method for isotopic deter- mination of boron in clay sediments.
文摘1 Scope This standard specifies the definition and test methods of flowability of dense and insulating refractory castables, and moulding equipment, moulding methods, curing and drying conditions of castables samples.
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.
文摘Acetylcholine is an essential neurotransmitter found throughout the nervous system. Its action on postsynaptic receptors is regulated through hydrolysis by various carboxylesterases, especially cholinesterases (ChEs). The acute toxicity of organophosphate (OP) compounds is directly linked to their action as inhibitors of ChE. One widely used assay for evaluating ChE activity is a spectrophotometric method developed by Ellman et al. When the enzyme source is from tissues or, in particular, blood, hemoglobin displays a spectrophotometric peak at the same wave-length used to analyze cholinergic activity. This creates a substantial background that interferes with the Ellman’s assay and must be overcome in order to accurately monitor cholinesterase activity. Herein, we directly compare blood processing methods: classical method (1.67 ± 0.30 U/mL) and HemogloBindTM treatment (1.51 ± 0.17 U/mL), and clearly demonstrate that pretreatment of blood samples with HemoglobindTM is both a sufficient and rapid sample preparation method for the assessment of ChE activity using the Ellman’s method.
文摘Capillary electrophoresis (CE) coupled with mass spectrometry (MS) with a sheath liquid interface is nowadays recognized as a powerful separation technique for drugs and metabolites analysis in human urine and can be applied in numerous fields such as clinical toxicology, drug substitution monitoring, forensic sciences and antidoping. With an acidic background electrolyte containing 15 mM ammonium formate at pH 2.5 and a sheath liquid consisting in a mixture of isopropanol/water (50:50, v/v) with 0.5% formic acid, CE-ESI-MS in positive mode demonstrated excellent performance for simultaneous analysis of basic drugs of abuse and metabolites in urine (e.g. cocaine, amphetamine, morphine and phase II metabolites). To achieve the desired level of sensitivity, two injection modes and three sample pre-treatments were evaluated. The detection of basic drugs and phase Ⅱ metabolites in diluted urine was achieved at concentrations above 1μg/mL. In order to enhance sensitivity, a sample preparation was required. A liquid-liquid extraction (LLE) was compared with solid-phase extraction. LLE was performed at alkaline pH and samples were electrokinetically injected. A chemometric approach (Doehlert design) was carried out in order to determine optimized injection parameters. Limits of detection (LOD) down to 10 ng/mL were reached with field-amplified sample injection but phase II metabolites were not extracted. Therefore, instead of LLE a SPE was performed on C 18 sorbent, and elution fraction after washing step containing phase Ⅱ metabolites was loaded on mixed-mode anion exchanger cartridges. After electrokinetic injection, this two-step SPE allowed LOD ca. 10 ng/mL for drugs and phase Ⅱ metabolites.
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In this study, a miniaturized analytical technique based on high density solvent based dispersive liquid-liquid microextraction (HD-DLLME) was developed for extraction of trace residues of multiclass pesticides including three striazine herbicides, two organophosphate insecticides and two organochlorine fungicides from environmental water and sugarcane juice samples. The analytical method was validated and found to offer good linearity: R2 ≥ 0.991;repeatability varied from 0.73% - 5.28%;reproducibility varied from 1.14% - 8.74% and limit of detection ranged from 0.005 to 0.02 μg/L. Moreover, accuracy of the optimized method was evaluated and the recovery was varied from 80.39% - 114.05%. Analytical applications of this method to environmental waters and sugarcane juice samples indicate the presence of trace residues of ametryn in the lake water and sugarcane juice samples. Atrazine and ametryn were also detected in irrigation water.
文摘This paper focuses on work related to post irradiation examination of 300-series austenitic stainless steel taken from reactor vessel internals of PWR. High neutron irradiation dose in NNP's leads to a degradation of microstructure of the material in a nano-metric scale. Hence, it is important to characterize the irradiated materials to understand the physical basis of the degradation mechanisms. Microstructural characterization of neutron-irradiated materials by TEM requires enhanced sample preparation methodologies, which commonly needs general improvements regarding particular experiment to be performed. In this study, the authors have developed methodology specialized in 1 mm TEM thin foil preparation from a deformed shank of a broken miniaturized tensile specimen. TEM foil size in current studies is smaller than standard because of the small shank diameter and high radioactivity of the studied material. The reduction of the TEM foil radioactivity to minimum is crucial to perform EDX chemical analysis and to increase the EDX detector lifetime. This paper describes whole process from bulk sample handling, including remote-controlled material cutting in shielded hot-cells and disc polishing in glow-boxes, up to the final procedure of electrolytic-polishing of electron transparent 1 mm TEM foils. Eventually, results of TEM microanalysis of radiation-induced defects were present.
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funded by the Slovenian Research Agency program P1-0143 and project L1-5446 and the young researchers programsupported by the EMPIR MercOx project(16ENV01).
文摘Flue gas containing volatile elements, fine fly ash particulates not retained by particle control devices, and limestone are the most important sources of trace and major elements (TMEs) in wet flue gas desulphurization (WFGD) gypsum. In this study, samples of gypsum slurry were separated into fine and coarse fractions. Multi-elemental analysis of 45 elements in the different size fractions of gypsum, slurry waters and lignite were performed by k0-INAA (k0-instrumental neutron activation analyses). The study found that the volatile elements (Hg, Se and halogens) in the flue gas accumulate in the fine fractions of gypsum. Moreover, the concentrations of most TMEs are considerably higher in the fine fractions compared to the coarse fractions. The exceptions are Ca and Sr that primarily originate from the limestone. Variations of TMEs in the finer fractions are dependent on the presence of CaSO4·2H2O that is the main constituent of the coarse fraction. Consequently, the content of TMEs in the fine fraction is highly dependent on the efficiency of separating the fine fraction from the coarse fraction. Separation of the finer fraction, representing about 10% of the total gypsum, offers the possibility to remove effectively TMEs from WFGD slurry.
文摘A three-dimensional graphene-based composite was prepared by a simple one-step in-site reduced-oxide method under atmospheric pressure. The obtained hydrogel was modified with 4-amino-benzenesulfonic acid and connected with ethylenediamine, and freeze-dried into an aerogel, which was characterized. Then the surface interaction with platinum (Pt, IV) was explored. The obtained aerogel showed good adsorption for Pt (IV) at acid conditions, giving a rising to the adsorption rate > 98% while pH ≥ 6. Using hexadecyl trimethyl ammonium bromide of 2% (m/V) as an eluent to desorb the Pt (IV) from the surface of the aerogel, a desorption rate of 81.1% was obtained in this process. Urea, buffer aquation and other surfactants were used in the desorption experiment to understand the adsorption mechanism between the aerogel and Pt (IV). In this work, hydrogen bond, van der Waals force and electronic interaction force mainly drove the adsorption process. For obtaining more purified Pt (IV), we used 0.5% CTAB to desorb Pd (II). A new three-dimensional graphene-based composite was prepared and the surface interaction between Pt (IV) and composite was experimented for understanding the adsorption mechanism and exploring its potential application in sample preparation in low concentration.