离子色谱法中高浓度盐基体对无机阴离子分析影响规律的研究

本文首次研究高浓度盐基体中，大量盐的存在对无机阴离子的保留时间，峰高峰面积等参数的影响规律，并对其影响机理进行了初步探讨，实验证明，在样品中离子总浓度不超过柱容量孤情况下，虽然由于某些离子的浓度过高，使待测离子的保留时间变短，峰形改变，但用峰面积和标准加入外推法计算，仍可得到较即的结果。     

Using fluorescence surrogates to track algogenic dissolved organic matter (AOM) during growth and coagulation/flocculation processes of green algae

Tracking the variation of the algogenic organic matter (AOM) released during the proliferation of green algae and subsequent treatment processes is crucial for constructing and optimizing control strategies. In this study, the potential of the spectroscopic tool was fully explored as a surrogate of AOM upon the cultivation of green algae and subsequent coagulation/flocculation (C/F) treatment processes using ZrCl₄ and Al₂(SO₄)₃. Fluorescence excitation emission matrix coupled with parallel factor analysis (EEM-PARAFAC) identified the presence of three independent fluorescent components in AOM, including protein-like (C1), fulvic-like (C2) and humic-like components (C3). Size exclusion chromatography (SEC) revealed that C1 in AOM was composed of large-sized proteins and aromatic amino acids. The individual components exhibited their unique characteristics with respect to the dynamic changes. C1 showed the highest correlation with AOM concentrations (R²?=?0.843) upon the C/F processes. C1 could also be suggested as an optical predictor for the formation of trihalomethanes upon the C/F processes. This study sheds a light for the potential application of the protein-like component (C1) as a practical surrogate to track the evolution of AOM in water treatment or wastewater reclamation systems involving Chlorella vulgaris green algae.     

环境大气中半/中等挥发性有机物(S/IVOCs)的测量技术进展

总结了环境大气中半/中等挥发性有机物（S/IVOCs）的主要测量技术及其进展,重点介绍了基于气相色谱技术和化学电离质谱技术的测量方法.S/IVOCs的测量主要由气相色谱技术开始发展,并随着质谱技术的发展而不断发展.基于气相色谱技术的测量方法,能够直接测量非极性化合物,但在面对组分多达千万种的复杂体系时,传统的一维色谱相对耗时,而且由于峰容量不够,峰重叠现象十分严重,难以实现全组分的准确分离.新近发展的多维分离系统如全二维气相色谱,通过正交的分离系统,能够实现复杂体系中物种组分的准确、快速分离.目前基于化学电离质谱技术的在线测量方法已经逐渐应用于S/IVOCs的测量,虽然在物种定性方面相对较弱,但其可提供高时间分辨率的测量结果,帮助分析S/IVOCs在大气中的快速变化.在未来的研究中,高时间分辨率和全组分准确测量是S/IVOCs研究的关键.     

溴化衍生-气相色谱法测定地表水中丙烯酰胺

采用溴化衍生-气相色谱技术,建立了地表水中丙烯酰胺的分析方法。分别使用工作曲线和标准曲线对丙烯酰胺进行定量分析。实验结果表明:利用溴化衍生生成,β-二溴丙酰胺的工作曲线线性范围更宽,灵敏度更高。用乙酸乙酯萃取衍生物,萃取浓缩后进行气相色谱分析,方法检出限为0.03μg/L,工作曲线在0.20~10μg/L范围内具有良好的线性相关性。地表水样品的加标回收率为87.6%~97.8%,其相对标准偏差为2.03%~5.31%。     

高效液相色谱法测定环境空气酰胺类化合物

高效液相色谱法测定环境空气中酰胺类化合物,采用多孔玻板吸收管采集环境空气中的酰胺类化合物,吸收液经0.22μm膜过滤后,经C18色谱柱分离,采用紫外检测器检测。丙烯酰胺、二甲基甲酰胺、二甲基乙酰胺的检出限分别为0.04μg/m3、0.000 2 mg/m3、0.000 2mg/m3（10 ml吸收液,采集15 L环境空气样品计）。高、中、低三种浓度三种酰胺类化合物的回收率区间为70.8%~90.2%,相对标准偏差范围小于9.6%。该方法操作简单,结果准确、可靠,适用于环境空气中酰胺类化合物的快速、准确监测。     

Determination of carazolol in pharmaceutical formulations by gas‐liquid‐chromatography (GLC)

A gas‐liquid‐chromatographic procedure for the quantitative determination of authentic carazolol and carazolol in tablets (Conducton^(R)?) has been described. Carazolol in tablets was extracted with absolute alcohol before injecting onto the gas Chromatograph. The concentration range adopted varied between 0.2 mg to 1.0 mg/ml of carazolol in alcohol solution. The results obtained were 97.6%±3.2 and 98.4%±2.6 for the stated and added amounts respectively.     

Safety line method for the prediction of deep coal-seam gas pressure and its application in coal mines

Gas pressure is an important index for evaluating the outburst risk and determining the gas content in coal seams. It is recommended to predict coal-seam gas pressure of the workface at deep levels before extending mining activities to deeper levels. According to the prediction results, measurements are taken for gas outburst prevention and control and for workload estimation. At present, regression methods are always used to process the numerous gas pressure data for prediction. Because there are many factors that influence the gas pressure which could lead to a deviation from actual values, the measured data do not possess basic conditions for regression methods; this can cause unexpected dangers if the methods are adopted.Based on a statistical analysis of actual measured results of coal-seam gas pressure in a same geological section in certain coal mine, two symbol measured points are selected to make a line for prediction, i.e. safety line, and the other measured points should be below the line except the abnormal points due to the confined water. It has been successfully applied in numerous coal mines in China. Particularly, this method is analyzed in this paper for the case of the No. 8₂ coal seam in the Taoyuan coal mine in Huaibei coalfield, China. By comparatively analyzing the relationship between gas pressure and depth from surface using regression methods, it is found that the safety line method could lead to a better prediction for deep coal-seam gas pressure, and therefore promote early warning ability and mining safety.     

Rapid and sensitive headspace gas chromatographic method for cyanide determination in whole blood

We reported a simple and rapid headspace (HS) gas chromatographic (GC) assay for the determination of cyanide in human whole blood obtained from both cadaveric and intoxicated subjects. The poison was extracted from whole blood samples by HS technique after 10 min incubation at 80°C with a HCl (1N) acidic solution supplemented with 30 g L^?1 of sodium chloride and 10 mg L^?1 of isopropanol as internal standard. A SGE WAX capillary column (30 m × 0.32 mm ID × 0.5 µm df) was used. The Flame Ionization Detector (FID) was set at 250°C. The detection and the quantification limits were 0.02 and 0.2 mg L^?1, respectively. In the within-day study, the coefficients of variation for three different whole blood cyanide concentrations varied between 3.2 and 6.5%, whereas those in the day-to-day study varied between 4.8 and 6.3%. The assay was performed in less than 20 min per sample, which appears to be suitable for emergency toxicological tasks involved in diagnosis of cyanide poisoning.     

Unignited High-Pressure Methane Jet Impinging a Pipe Rack: Practical Tools for Risk Assessment

Although the diffusion of its storage and transport under liquefied conditions, nowadays it is common to have methane in gaseous form in several industrial applications. This leads to safety implications to be considered: hazards are linked to both the high-pressure at which the gas is kept and to its flammability. Scenarios where flammable jets impact an obstacle are of paramount importance because of their possible occurrence. Following a numerical approach, literature shows up that their assessment can be reliably performed by means of only Computational Fluid Dynamics tools. However, despite the improvements of computing power, Computational Fluid Dynamics costs still limit its use in daily risk analysts’ activities. Therefore, considering an accidental jet-obstacle scenario of industrial interest, the present work investigates how a pipe rack can influence the development of a high-pressure methane jet. Based on a Computational Fluid Dynamics analysis, main achievements of this work are a simple criterion able to identify the situations where the pipe rack does not influence the high-pressure methane jet behavior, therefore allowing to identify the scenarios where simpler models can be used (i.e., analytical correlations known for the free jet situation), and, if present, a simple analytical relationship that roughly predicts the influence of the pipe rack without the need of performing complex Computational Fluid Dynamics simulations.     

Screening of antibiotic residues in fresh milk of Kathmandu Valley,Nepal

The prevalence of two groups of antibiotics; namely penicillin and sulfonamides was studied in fresh milk available in Kathmandu Valley of Nepal. The milk samples (n = 140) were collected from three different sources; individual farmers, cottage dairies and organized dairies of Kathmandu valley. Qualitative and semi-quantitative analysis with rapid screening kits revealed that 23% samples were positive for antibiotic residues in the fresh milk for penicillin and sulfonamide groups (1–256 µg/kg). High performance liquid chromatography (HPLC) analyses detected 81% samples positive for amoxicillin (68–802 µg/kg), 41% for sulfadimethoxine (31–69 µg/kg), 27% for penicillin G (13–353 µg/kg), and 12% for ampicillin (0.5–92 µg/kg). Due to the precision and accuracy of liquid chromatography method, it detected more positive samples and consequently presented higher prevalence than the rapid screening kits. The antibiotic residues were found above the maximum residue limits that presented serious threat to consumer health and raised a serious concern regarding the implementation and monitoring of international regulations in developing countries.