Determination of triazine herbicide residues in water samples by on-line sweeping concentration in micellar electrokinetic chromatography

A new method for the determination of atrazine, simazine and prometryn in water samples by on-line sweeping concentration technique in micellar electrokinetic chromatography （MEKC） was developed. Various parameters affecting sample enrichment and separation efficiency were systematically studied. Compared with the conventional MEKC method, up to 60-200-fold improvement in concentration sensitivity was achieved in terms of peak height by using this sweeping injection technique. The compound strychnine was used as the internal standard for the improvement of the experimental reproducibility. The limits of detection （S/ N = 3：1） for atrazine, simazine and prometryn were 9, 10 and 0.5 ng mL-1, respectively. This method has been successfully applied to the analysis of atrazine, simazine and prometryn in lake, steam and ground water.

On-line Sweeping Sample Concentration in Micellar Electrokinetic Chromatography with Enhanced Sensitivity for the Deter-mination of Carbamazepine in Human Serum

A sensitive and simple micellar electrokinetic chromatography （MEKC） method was developed for the determination of antiepileptic drug, carbamazepine （CBZ）, using sweeping on-line concentration method with photodiode array detection. Under the optimal conditions, the calibration curve was linear over a range of 0.5-40μg·mL^-1 for CBZ with a correlation coefficient of 0.998. The detection limit （S/N = 3：1） of CBZ was 0.10 μg·mL^-1. The sweeping-MEKC method has been successfully applied to the analysis of CBZ in human serum.

DETERMINATION OF ANTIMONY IN WATER SAMPLES BY FLOW-INJECTION HYDRIDE GENERATION ATOMIC ABSORPTION SPECTROMETRY WITH ON-LINE ION-EXCHANGE COLUMN PRECONCENTRATION

On-line ion-exchange separation and preconcentration were combined with flow-injection hydride generation atomic absorption spectrometry (HGAAS) to determine ultra-trace amounts of antimony in water samples. Antimony(Ⅲ) was preconcentrated on a micro-column packed with CPG-8Q chelating ion-exchanger using time-based sample loading and eluted by 4 mol l^(-1) HCl directly into the hydride generation AAS system. A detection limit (3σ) of 0.0015μg l^(-1) Sb(Ⅲ) was obtained on the basis of a 20 fold enrichment and with a sampling frequency of 60h^(-1). The precision was 1.0% r.s.d.(n=11) at the 0.5μg l^(-1) Sb(Ⅲ) level. Recoveries for the analysis of antimony in tap water, snow water and sea water samples were in the range 97-102%.

ON-LINE ELECTROLYTIC DISSOLUTION OF SOLID METAL SAMPLE AND DETERMINATION OF COPPER IN ALLOY BY AAS

On-line dissolution of solid metal sample can be carried out by electrolysis under the control of flow injection analyzer(FIA),and the dissolved sample can be transferred to atomic spectrometer for the direct analysis.The hyphenated technique of FIA on-line electrolytic dissolution of alloy and atomic absorption spectrometer(AAS)detection is developed.The research is focused on the effects of electrolyte composition and electrolysis parameters on the sample dissolving,as well as the quantitative analysis of Cu in Al alloy samples.

Application of Capillary Electrophoretic On-Line Sequential Concentration Based on Micelle to Solvent Stacking

To take advantage of micelle to solvent stacking (MSS) to achieve more sensitivity enhancement with enough selectivity, the application of capillary electrophoretic online sequential concentration based on the MSS was reviewed. MSS has been coupled to sweeping FASS, FASI and normal EKI. Furthermore, multiple stacking by coupling MSS with more than one stacking method has also been reported. It is more sensitive and selective than solely used of one or two stacking methods and is very suitable for complex and trace sample analysis.

Geochemical Orientation Study of Stream Sediment Samples in the Southern Part of Nuggihalli Schist Belt: Ore Mineral Phases and Their Implications on the Bedrock Potential for Ores

Stream sediment sampling is a significant tool in geochemical exploration. The stream sediment composition reflects the bedrock geology, overburden cover, and metalliferous mineralization. This research article focuses on assessing selected trace element concentrations in stream sediments and interpreting their inter-element relationships using multivariate statistical methods. Tagadur Ranganathaswamy Gudda and its surroundings in the Nuggihalli schist belt of southern India have been investigated in the present work. The geology of the study area is complex, with a diverse range of litho units and evidence of strong structural deformation. The area is known for its mineralization potential for chromite, vanadiferous titanomagnetite, and sulfides. The topography of the region is characterized by an undulating terrain with a radial drainage pattern. Most part of the schist belt is soil covered except the Tagadur Ranganathaswamy Gudda area. For this study, a discrete stream sediment sampling method was adopted to collect the samples. Stream sediment samples were collected using a discrete sampling method and analyzed for trace elements using an ICP-AES spectrophotometer: Fe, Cr, Ti, V, Cu, Ni, Zn, Pb, Mn, Cd, and As have been analyzed. The analytical data were statistically treated using the SPSS software, including descriptive statistics, normalization of data using natural log transformation, and factor analysis with varimax rotation. The transformed data showed a log-normal distribution, indicating the presence of geochemical anomalies. The results of the study provide valuable insights into the geochemical processes and mineralization potential of the study area. The statistical analysis helps in understanding the inter-element relationships and identifying element groups and their implications on bedrock potential mineralization. Additionally, spatial analysis using inverse distance weighting interpolation provides information about the distribution of geochemical parameters across the study area. Overall, this research contributes to the understanding of stream sediment geochemistry and its application in mineral exploration. The findings have implications for future exploration efforts and can aid in the identification of potential ore deposits in the Nuggihalli schist belt and similar geological settings.

Reagent optimization for on-line simultaneous polarographic determination of trace amounts of Cu^(2+), Cd^(2+) and Co^(2+) in the presence of anextremely large excess of Zn^(2+)

Reagents are optimized for the simultaneous determination of trace amounts of Cu^(2+), Cd^(2+) and Co^(2+) in zinc sulfate solution, which contains an extremely large excess of Zn^(2+). First, the reagents and their doses for the experiment are selected according to the characteristics of the zinc sulfate solution. Then, the reagent doses are optimized by analyzing the influence of reagent dose on the polarographic parameters(i.e. half-wave potential E_(1/2) and limiting diffusion current I_p). Finally, the optimization results are verified by simultaneously determining trace amounts of Cu^(2+), Cd^(2+) and Co^(2+) in the presence of an extremely large excess of Zn^(2+). The determination results indicate that the optimized reagents exhibit wide linearity, low detection limits, high accuracy and good precision for the simultaneous determination of trace amounts of Cu^(2+), Cd^(2+) and Co^(2+) in the presence of an extremely large excess of Zn^(2+).

Radon Concentration in Soil and Radon Exhalation Rate at Al-Dora Refinery and Surrounding Area in Baghdad

Radongas concentrations in soil samples were determined from depths (surface, 15, and 30) cm for nine locations in Al-Dora refinery and surrounding area using “sealed can technique” and CR-39 solid state nuclear track detectors. The radon concentration in surface samples ranged from 810.08 to 1380.08 Bq/m3 with an average 1137.71 Bq/m3. The radon concentration in soil at the depth 15 cm was ranged from 490.5 to 1197.52 Bq/m3 with an average 732.78 Bq/m3 and at the depth 30 cm was ranged from 362.07 to 889.53 Bq/m3 with an average 529.41 Bq/m3. The surface exhalation rate in surface soil samples ranged was 0.44, to 0.99 Bq·m-2·h-1 with average 0.61 Bq·m-2·h-1. The surface exhalation rate in soil samples at the depth 15 cm was ranged from 0.22 to 0.64 Bq·m-2·h-1 with average 0.39 Bq·m-2·h-1. The surface exhalation rate in soil samples at the depth 15 cm was ranged from 0.22 to 0.64 Bq·m-2·h-1 with average 0.39 Bq·m-2·h-1. The surface exhalation rate and the mass exhalation rate in soil samples at the depth 30 cm ranged from 0.19, to 0.48 Bq·m-2·h-1 with average 0.28 Bq·m-2·h-1. The mass exhalation rate in surface soil samples ranged from 0.09 to 0.21 Bq·kg-1·h-1 with average 0.12 Bq·kg-1·h-1. The mass exhalation rate in soil samples from depth 15 cm was ranged from 0.046 to 0.14 Bq·kg-1·h-1 with average 0.08 Bq·kg-1·h-1. The mass exhalation rate in soil samples at the depth 30 cm was ranged from 0.042 to 0.1 Bq·kg-1·h-1 with average 0.06 Bq·kg-1·h-1.

Measurements of Sulfur Isotope Composition on Ultrasmall(80 Nanomole) Sulfide and Sulfate Samples by a Modified EA-IRMS

The traditional method for sulfur isotope measurement using EA-IRMS commonly requires sulfur content greater than 2 μmol. Such a large sample size limits its application to low-S materials, the size mainly being due to ineffective utilization of sample gas, almost 99.7% of which is discarded with carrier gas through the split port of the continuous-flow interface. A modified EA-IRMS system with a gas chromatographic(GC) column and a custom-built cryogenic concentration device is used in this study. We measured six reference materials to test the performance of this method. The results were consistent with those obtained through traditional EA-IRMS. Precisions ranging from ±0.24‰ to ±0.76‰(1σ)can be obtained with samples equivalent to ~80 nmol sulfur, which were similar to results obtained from an alternative method using an absorption column. Our improved method is a powerful tool for sulfur isotope measurement in ultrasmall sulfide and sulfate samples, which can be further applied to carbon, nitrogen and oxygen isotope analyses of samples at about 100 nmol level.

Concentrated and gastight sampling technique of deepsea microplankton

A new sampling method of deepsea microplankton with function of in-situ concentrated sampling and gastight sampling was proposed. In-situ concentrated sampling technique was realized as follows: a microplankton membrane was used as filtration membrane, and a deepsea pump was used to pump seawater; the microplankton was captured and the density of microplankton was increased when seawater flow through the filtration membrane. Gastight sampling technique was realized as follows: a precharged accumulator was used as pressure compensator. During the process of lifting the sampler, the accumulator compensated the pressure drop continuously. The laboratory experimental results show that with in-situ concentrated sampling technique, in-situ concentrated sampling can be realized and the maximum concentration ratio reaches up to 500. With pressure compensation technique based on accumulator, gastight sampling can be realized. When sampling at 6 km and the precharge pressure of accumulator is 18 MPa, pressure drop of the sample is less than 2% compared with its original pressure. Deepsea experiment (at 1.9 km) results show that the sampler can realize in-situ concentrated sampling and gastight sampling.

Measurement of Volcanic SO₂Concentration in Miyakejima Using Differential Optical Absorption Spectroscopy (DOAS)

Since the volcanic eruption in 2000, continuous monitoring of sulfur dioxide (SO2) gas has been conducted with in-situ samplers located along the seashore road in Miyakejima, a volcano island around 180 kmsouth of Tokyo. The purpose of these sampling measurements has been to issue warning on the hazardous air pollution to the local residents. Therefore, the resulting data do not provide direct information on pollution levels inside the restricted areas where high concentration of SO2 still takes place frequently. From the ecological point of view, it is desirable to have pollution data covering wider regions of the island. In this paper we report on our differential optical absorption spectroscopy (DOAS) measurements carried out inside the highly-polluted, restricted areas in Miyakejima in December 2009 and September 2010. The system is based on continuous light emitted from a xenon light sources, while detector setups consisting of a telescope and a compact spectrometer detect the light after passing a nearly horizontal optical path of460 m-1300 m. By virtue of the portability of the DOAS observation systems, we achieved the measurement of the concentrations inside the restricted districts in the eastern and southwestern parts of the island. The DOAS results in both of these districts revealed the occurrence of pollution of volcanic gas even when no pollution was observed at nearby sampling stations. In addition, simultaneous measurements with two nearly orthogonal DOAS paths were conducted for examining the spatial distribution of the volcanic gas over the spatial range of several hundred meters. The result of this two paths measurement has indicated the importance of orography, in addition to the wind speed and wind direction, in determining the spatial concentration of SO2 emitted from the volcano crater.

Radiological Effects of Soil and Rock Samples of Different Libyan Regions

The activity concentration of natural radioactivity for soil samples collected from western and mid Libyan regions were measured using HPGe detector. The average activity concentration of 226Ra, 232Th and 40K for ten regions was found to be 51.86 ± 7.14, 75.56 ± 10.95 and 128.98 ± 6.88 Bq/kg respectively. The results obtained for the corresponding nuclides 226Ra and 232Th are above the worldwide average values (35 and 30 Bq/kg) while 40K was smaller than worldwide average (400 Bq/kg). The average outdoor absorbed dose and the annual effective dose rates due to 226Ra, 232Th and 40K were observed to be 21.51 ± 2.93 nGy/h and 0.297 ±.03 mSv/y respectively, which are lower than world average values (60 nGy/h and 0.8 mSv/y). The radium equivalent activity and external hazard indices were found less than the world wide average values.

Multi-Scale Variation Prediction of PM2.5 Concentration Based on a Monte Carlo Method

Haze concentration prediction,especially PM2.5,has always been a significant focus of air quality research,which is necessary to start a deep study.Aimed at predicting the monthly average concentration of PM2.5 in Beijing,a novel method based on Monte Carlo model is conducted.In order to fully exploit the value of PM2.5 data,we take logarithmic processing of the original PM2.5 data and propose two different scales of the daily concentration and the daily chain development speed of PM2.5 respectively.The results show that these data are both approximately normal distribution.On the basis of the results,a Monte Carlo method can be applied to establish a probability model of normal distribution based on two different variables and random sampling numbers can also be generated by computer.Through a large number of simulation experiments,the average monthly concentration of PM2.5 in Beijing and the general trend of PM2.5 can be obtained.By comparing the errors between the real data and the predicted data,the Monte Carlo method is reliable in predicting the PM2.5 monthly mean concentration in the area.This study also provides a feasible method that may be applied in other studies to predict other pollutants with large scale time series data.

Diffusion Process of High Concentration Spikes in a Quasi-Homogeneous Turbulent Flow

When a mass spreads in a turbulent flow, areas with obviously high concentration of the mass compared with surrounding areas are formed by organized structures of turbulence. In this study, we extract the high concentration areas and investigate their diffusion process. For this purpose, a combination of Planar Laser Induced Fluorescence (PLIF) and Particle Image Velocimetry (PIV) techniques was employed to obtain simultaneously the two fields of the concentration of injected dye and of the velocity in a water turbulent channel flow. With focusing on a quasi-homogeneous turbulence in the channel central region, a series of PLIF and PIV images were acquired at several different downstream positions. We applied a conditional sampling technique to the PLIF images to extract the high concentration areas, or spikes, and calculated the conditional-averaged statistics of the extracted areas such as length scale, mean concentration, and turbulent diffusion coefficient. We found that the averaged length scale was constant with downstream distance from the diffusion source and was smaller than integral scale of the turbulent eddies. The spanwise distribution of the mean concentration was basically Gaussian, and the spanwise width of the spikes increased linearly with downstream distance from the diffusion source. Moreover, the turbulent diffusion coefficient was found to increase in proportion to the spanwise distance from the source. These results reveal aspects different from those of regular mass diffusion and let us conclude that the diffusion process of the spikes differs from that of regular mass diffusion.

药师参与下的标本评估对万古霉素血药浓度解读的改善性研究

目的评价由药师参与下的血液标本质量评估对万古霉素血药浓度解读的影响。方法回顾性收集2022年1月—12月在武汉市第一医院使用万古霉素抗感染治疗并监测血药浓度的患者资料。以不合格标本分布类型及占比、科室分布、再评估不合格标本复查前后结果差值、血药浓度分布等作为观察指标。结果共纳入92例患者,177个血液标本,涉及20个科室,最终进入谷浓度监测环节的有162个。59个(36.42%)标本合格且浓度达窗(10~20 mg/L),浓度不足10 mg/L占22.84%(37/162个),高于20 mg/L占30.86%(50/162个)。合格标本共115个(64.97%)。不合格标本共62个(占35.03%),初评估不合格15个(8.47%),再评估不合格47个(26.55%)。对再评估不合格的标本在规范宣教后进行复测,其中有44个前后浓度结果具有显著差异(P<0.05),其中“给药后采血”的情况,复测前后差值最大(-16.5 mg/L)。结论以标本为中心的管理模式下,在分析前和分析后分别对标本做合理评估,使得万古霉素TDM数据的可靠性大大提升,临床应用价值得到充分发挥。

熔片制样-X射线荧光光谱法测定铜精矿中7种组分

铜精矿中硫化物重金属含量较高,样品需要充分氧化后才可熔片,否则熔融过程严重腐蚀铂-金坩埚。一般方法采用硝酸盐作为氧化剂,单一的硝酸盐难以完全氧化铜精矿样品,并且氧化反应剧烈容易发生样品喷溅。采用四硼酸锂-偏硼酸锂混合熔剂(m∶m=67∶33),样品和熔剂质量比为1∶35,通过考察氧化剂过氧化钡-硝酸钠-碳酸钠的氧化效果,以及脱模剂的用量和加入方式、预氧化和熔融条件等,样品在高温炉中预氧化后转移至熔样机熔融,可制成合格的玻璃样片。选用合适的铜精矿国家一级标准物质,以标准物质相互混合或向标准物质中添入纯氧化铜的方式扩大校准曲线含量范围,以熔片法制样,建立了波长色散X射线荧光光谱法测定铜精矿中的铜、硫、全铁、氧化钙、氧化镁、二氧化硅、三氧化二铝等7种组分含量的方法。各组分检出限在0.054%~0.22%,校准曲线相关系数(r)均在0.9998以上,选用的3个铜精矿矿石国家一级标准物质按建立的方法进行处理后,测定结果均在认定值的误差范围内,各组分测试结果的相对标准偏差(RSD,n=12)在0.28%~4.1%;选取3个铜精矿实际样品做方法比对实验,测定值与标准分析方法的测定值无明显差异。

熔融制样X射线荧光光谱法快速测定铌精矿中10种元素

采用高温熔融制样方式将铌精矿制备成均匀稳定的玻璃片,利用X射线荧光光谱法测定铌精矿中铌、硅、钙、镁、钛、磷、锶、锰、钡、钍10种元素的含量。将样品与四硼酸锂-偏硼酸锂混合溶剂(质量比67∶33)按照1∶14的质量比混合,加入30 g/L溴化锂溶液0.2 mL,在全自动熔样机上于1050℃熔融8 min,摇摆6 min,静置冷却脱模后得到测定玻璃样片。采用人工配制标准样品的方法建立标准工作曲线,以经验系数法校正谱线重叠效应,用理论α系数法校正基体效应,两个不同含量水平铌精矿样品测定结果的相对标准偏差为0.23%~3.91%(n=9),该方法与化学法测定值基本一致。该方法可实现实际铌精矿样品中10种主次量元素的快速批量日常检测。

一种基于粒子计数器采样机理的洁净室粒子浓度仿真计算方法及验证

洁净度(用粒子浓度表征)是洁净室重要受控参数之一。基于采样机理,提出了一种可精准预测洁净室内粒子浓度的瞬态CFD仿真计算方法。该方法在拉格朗日离散相模型基础上,加入粒子计数器等效模型,模拟空气和粒子通过采样口的动态行为。搭建实验平台进行验证,结果显示仿真与实测数据吻合良好。成果不仅为洁净室粒子浓度仿真提供新方法,同时也为HVAC系统的优化设计提供支持。

虚拟现实技术应用于臭气浓度采样考核系统软件初探

臭气浓度是表征恶臭污染程度的感官性指标,臭气浓度监测是当前国内外通用的主流监测方法。监测采样人员考核培训是保证臭气浓度监测质量的重要基础。目前臭气浓度现场采样考核主要以操作演示、现场提问的方式为主,存在专家考核手势不一、考核内容覆盖面较窄、考核效率较低、无法开展大规模集中考核等问题。为进一步实现臭气浓度监测采样人员考核的规范化、系统化,引入虚拟现实技术(VR),开发了浸入式臭气浓度采样考核系统软件,通过模拟考核测试和软件效果评估,证明VR在臭气浓度采样考核中应用的必要性和重要性。

附有集中质量的飞艇囊体材料动力特性

针对平流层飞艇刚柔一体大型复杂结构系统设计与分析,开展了附有集中质量的飞艇囊体材料动力特性仿真分析研究,将刚度大、质量相对集中的结构零部件简化为集中质量,飞艇囊体简化为双向拉伸的十字形囊体材料试样,分析预张力大小、集中质量的质量和尺寸对囊体材料试样的动力特性影响.结果表明,试样的固有频率随着预张力增大而增大,随着集中质量的质量增大而减小,随着集中质量与试样连接的边长增加而增大;试样的基频与集中质量的高度无关,但第2,3阶频率随着集中质量的高度增加而减小.研究结论为飞艇结构的总体设计与分析以及进一步开展附有集中质量的飞艇囊体材料动力试验提供了理论依据.