基于邻域贡献权值细化的圆心亚像素定位算法

针对传统的圆心算法过程复杂、定位精度受初始边缘提取效果影响较大等问题,提出了一种基于邻域贡献权值细化的圆心亚像素定位算法。首先引入邻域贡献权值系数,改进传统非极大值抑制法,细化边缘;然后在边缘点的梯度方向对灰度值进行高斯拟合,确定亚像素边缘位置;最后针对边缘突变点提出了基于随机抽样一致的最小二乘法来拟合圆心。实验结果表明,该算法具有较好的精度和稳定性,圆心的提取精度可以达到0.1个像素。     

X-射线荧光光谱法测定溶样后熔融制样金属硅中铁、铝、钙、钛、磷、铜

本文提出了溶解、蒸干然后用熔剂熔融残渣的样品制备方法,解决了金属硅不易直接熔融制样的难题,可以同时测定金属硅中多种杂质元素,消除了基体效应的影响,克服了标准样品对测定的限制,测定范围广,准确度高,通过安排正交试验确定了样品制备条件。     

Improved Performance of On-line Atom Trapping in Flame Furnace Atomic Absorption Spectrometry by Chemical Vapor Generation: Determination of Cadmium in High-Salinity Water Samples

ABSTRACT

On-line atom trapping inside a nickel flame furnace using chemical vapor generation for sample introduction was proposed for the determination of trace cadmium by flame atomic absorption spectrometry (AAS). Cadmium volatile species was generated upon reaction with potassium borohydride and then flushed into a flame furnace for on-line trapping by a flow of nitrogen carrier gas. The middle part of the flame furnace, where the carrier gas impacts, is cooled by the gas flow, and this provides a fine strategy for on-line atom trapping for the purpose of preconcentration. A stainless steel plate is put on the top of the flame burner in the middle to form a flame-free zone, which also greatly lowers the temperature of the flame furnace and facilitates the atom-trapping process. Due to the introduction of chemical vapor generation, matrix effect was greatly alleviated compared with direct pneumatic nebulization for on-line atom trapping in flame furnace AAS. With trapping time of 35 s, the current approach achieved an excellent limit of detection of 20 ng L^?1. The proposed method was successfully applied for the quantification of cadmium in high-salinity samples.     

Sample Preparation for the Determination of Metals in Food Samples Using Spectroanalytical Methods—A Review

Abstract

The present article gives an overview of recent publications and modern techniques of sample preparation for food analysis employing atomic and inorganic mass spectrometric techniques, such as flame atomic absorption spectrometry, chemical vapor generation atomic absorption and atomic fluorescence spectrometry, graphite furnace atomic absorption spectrometry, inductively coupled plasma optical emission spectrometry, and inductively coupled plasma mass spectrometry. Among the most frequently applied sample preparation techniques for food analysis are dry ashing, usually with the addition of an ashing aid, and acid digestion, preferably with the assistance of microwave energy. Slurry preparation, particularly with the assistance of ultrasound, is increasingly used to reduce acid consumption and sample preparation time. Direct analysis of solid samples is gaining importance in the field of food analysis as it offers the highest sensitivity, avoids the use of acids and other aggressive reagents, makes possible the analysis of micro‐samples, and can be applied for fast screening analysis, e.g., of fresh meat.     

Isotope Studies of Hydrogen and Oxygen in Ground Ice - Experiences with the Equilibration Technique

Abstract

Equilibration technique suitable for a large amount ofsamples is described for hydrogen and oxygen isotope analyses of ground ice, especially ice wedges, including the sampling strategy and the analytical procedure as well as the calibration of the Finnigan MAT Delta-S mass spectrometer in June, 1999. Since for future analyses of ice wedges, a higher sampling resolution with limited sample volume is required, the limit of the equliibration technique for small water samples size of between 0.05 and 5 ml was checked. For water samples smaller than 1ml, corresponding to a molar ratio [H₂O]/[H₂] of smaller than 0.994, a balance correction has to be applied. The experimental errors due to partial evaporation during evacuation, the balance calcultion of the isotope equilibration process, the linearity as well as memory effects of the mass spectrometer for smaples with large differences in δ¹⁸O and δD are tackled in this paper. In the polar regions of Northern Siberia without Late Pleistocene and Holocene glaciation, ground ice is used as an archive for paleoclimate studies. First results of stable isotope measurements on ice wedges clearly show a shift towards heavier isotopes and thus warmer winter temperatures as well as a change in the source of the precipitation between Late Pleistocene and Holocene. These results indicate the high potential of ground ice for paleoclimate studies.     

Entropy and equilibrium property of QCD-instanton induced final state in deep-inelastic scattering

The scaling and additivity properties of Rényi entropy in rapidity space of the instanton final state (IFS) and current jet identified by the r-sorting method from the QCDINS Monte Carlo event sample are to saturation with decreasing phase space scale. Furthermore, it is found that the additivity of H2 holds well for the IFS in narrow rapidity windows at different positions. These results indicate that the IFS produced in the instanton-induced process of deep inelastic scattering has reached local equilibrium.     

超分子溶剂在样品前处理与检测技术中的应用研究进展

随着绿色分析化学概念的提出,新型绿色溶剂的开发和利用成为当前的研究热点.将绿色溶剂替代传统有机溶剂用于样品前处理过程,可以减少对实验人员及环境的危害.超分子溶剂由于两亲物质含量高,萃取分离条件温和,近年来被广泛应用于萃取富集宽极性范围内的目标分析物,兼具萃取和净化的效果.该文介绍了超分子溶剂的形成过程和基本性质,综述了...     

组合蒸馏技术用于气相色谱分析的样品前处理

研究了一种组合蒸馏方法的样品前处理技术,并将其研制成样品预处理装置,运用载体、携带体和组合蒸馏技术实现待测样品中微量成分的提取、分离和富集。将分子蒸馏收集端的冷端接收器设计为可更换结构,避免了样品的交叉污染问题。在乙酸乙酯中添加4种有机磷农残标样作为评价样品,所研制的装置能自动将农残组分富集到2 mL邻苯二甲酸二甲酯中。利用气相色谱分析的结果,对该样品前处理装置的分离富集参数进行了优化。实验结果表明,该方法能完全除去蛋白、脂肪、色素等对气相色谱分析有干扰的组分;能将待测微量组分的浓度富集150倍以上;回收率为90%～117%,相对标准偏差为1.3%~10%;最小检出浓度为1 ng/mL;可以处理高于100 g的样品量;可以得到几十毫克至上百毫克的目标组分;有机试剂的回收利用率大于95%;操作简单方便。用模拟样品做了实际应用实验。该技术适合沸程为120～600 ℃组分的富集。所研制的装置适用于大量样品中痕量组分的半制备级富集。     

Resistivity－temperature characteristics of sol gel YBa2Cu3Oy samples synthesized in flowing oxygen atmosphere

The relationship of resistivity versus synthesizing temperature of sol gel YBa_2Cu_3O_y samples was studied when prepared under flowing oxygen conditions. A set of high-temperature ρ－T curves was obtained for the whole process. After the sample finished the test measuring, its resistivity was ρ_{300}=9.83×10^{-3 }Ω·cm at room temperature. The ρ－T curve also showed that the orthorhombic－tetragonal phase transformation of sol-gel YBa_2Cu_3O_y sample occurred at 581℃ for the sample in the rising temperature process, but at 613℃ in the cooling process, lower than that of the samples made by using the conventional powder metallurgy methods.     

Quantification of imatinib and related compounds using capillary electrophoresis-tandem mass spectrometry with field-amplified sample stacking

A quantification method for imatinib (IM), its major metabolite N-desmethyl imatinib (NDI), and a degradation by-product was developed using CE–MS combined with an online concentration technique. The use of multiple reaction monitoring (MRM)–MS/MS further improved the sensitivity of this technology. Liquid–liquid extraction (LLE) using tertiary butyl methyl ether yielded high recovery and reproducibility for the pretreatment of serum samples. The recovery rate exceeded 83% for all three analytes, and was 90% for IM. To improve quantification results, a conductivity-induced online analyte concentration technique, field-amplified sample stacking (FASS), was used. The S/N ratios were improved at least 10-fold when compared with conventional capillary zone electrophoresis. The detection limits were 0.2 ng/mL for IM, 0.4 ng/mL for NDI, and 4 ng/mL for the degradation by-product. These results are superior to those previously obtained by other reported methods. The new method was validated in terms of its selectivity, intra- and interday repeatability and accuracy, and sample storage stability, following the guidelines issued by the European Medicines Agency. Considering the convenient pretreatment procedure (LLE), superior sensitivity, and fast analysis speed (<15 min), this method can be useful in the determination of imatinib levels in blood.