液液萃取-气相色谱/串联质谱法测定水中五氯酚及其钠盐

采用液液萃取处理水样,用气相色谱-串联质谱法测定样品中五氯酚及其钠盐,通过优化测定条件,使方法在1.00μg/L~500μg/L范围内线性良好。检出限和定量限分别为1.00μg/L和5.00μg/L,空白水样五氯酚钠3个质量浓度水平的加标回收率为89.8%~98.4%,5次平行试验测定结果的RSD为5.5%~10.7%。     

Validation of liquid nitrogen vaporisation rate by small scale experiments and analysis of the conductive heat flux from the concrete

The vaporisation of a liquid nitrogen pool spilled on concrete ground was investigated in small scale field experiments. The pool vaporisation rate and the heat transfer from the concrete ground were measured using a balance and a set of embedded heat flux sensors and thermocouples. The ability to predict the concrete's thermal properties based on these measurements was investigated. This work showed that a simple, one-dimensional theoretical model, assuming heat conduction through a semi-infinite ground with ideal contact between the cryogenic liquid and the ground, commonly used to describe the heat transfer from a ground to the LNG, can be used to match the observed vaporisation rate. Though estimated parameters, thermal conductivity and thermal diffusivity, do not necessary represent real values. Although the observed vaporization rate follows a linear trend, and thus can be well represented by the model, the overall model prediction seems to be overestimated. The temperature profile inside the concrete is slightly over-predicted at the beginning and under-predicted at later stage of the spill. This might be an effect of the dependence of the concrete's thermal properties on the temperature or may indicate an incorrect modelling and a varying temperature of the ground surface.     

An LC-MS/MS method for creatine and creatinine analysis in paraquat-intoxicated patients

Abstract

A sudden increase in serum creatinine after paraquat intoxication has been reported in several clinical studies. However, this dramatic change of creatinine may be possibly due to an interconversion of creatine-creatinine in relation to paraquat toxicity. In order to investigate the creatine-creatinine relationship, a liquid chromatography tandem mass spectrometry in combination with electrospray ionization was developed and validated for simultaneous determination of creatine and creatinine in the serum. The chromatographic separation was achieved on a Gemini® C₆-Phenyl column with a gradient elution consisting of 0.1% formic acid in ultrapure water and methanol as the mobile phase. The method yielded suitable levels of specificity and selectivity, and calibration curves of creatine and creatinine in serum were linear over the concentration range of 0.5–200?µg mL^?1. The limit of quantification of both compounds was 0.5?µg mL^?1, and the method was accurate within the recovery range of 96.23–102.75%, indicating the robustness of the method. The method was successfully applied to toxicological samples from paraquat-intoxicated patients, and the concentrations of creatine and creatinine were quantified. High creatine concentrations in serum samples were observed which may lead to high serum creatinine despite normal kidney function as creatine is converted to creatinine in proportion to its concentration.     

Effect of particle size on CO adsorption and thermodynamic analysis

The liquid nitrogen adsorption method was used to characterize the pore structure of non-cohesive coal in the 061,404 working face of the Lingxin coal mine. The amount of specific surface area of micropores in the sample continuously rose as particle sizes reduced. The volumetric method was used to measure the CO isothermal adsorption curves of three samples (sample I, 0.425–0.25 mm, sample II, 0.18–0.25 mm, and sample III, 0.15–0.18 mm). The experimental results were fitted by the Langmuir model. According to the experimental results, it was conducive to CO adsorption with the conditions of high pressure and low-temperature. The decrease in grain diameter increased the number and volume of micropores in the sample, which improved the adsorption capacity of the sample. In addition, according to the adsorption data, the CO adsorption thermodynamics of three samples were analyzed, including surface potential (Ω), Gibbs free energy change (ΔG) and entropy change (ΔS). The results demonstrated that CO adsorption by coal was a spontaneous process. Sample III has the most substantial adsorption capacity, whereas the sample I has the weakest adsorption capacity.     

地表水和地下水中的砷、硒同时测定

通过利用双道原子荧光法,同时对地表水和地下水样品中砷、硒进行测定,具有操作更加简单、监测分析速度快、节省试剂等优点。     

低碳高氮污水处理应用技术研究

针对碳氮比小于7的污水,其碳源不能满足硝化与反硝化的要求这一问题,通过改变SBR工艺的运行方式、调解工艺参数等技术手段,使其能够达标处理此类工业废水,并通过某淀粉厂的工程实例进行了验证:采用改良的SBR工艺可以对低碳高氮污水进行有效的处理。     

鱼体中多氯联苯的气相色谱/质谱分析研究

建立了鱼体中共平面多氯联苯(co-PCBs)和指示性多氯联苯(indicator PCBs)残留量的快速溶剂萃取气相色谱质谱分析方法.结果表明,18种多氯联苯在20 μg/L～500 μg/L范围内线性良好(r＞0.998),方法的检出限为0.2 ng/kg～0.5 ng/kg.当添加浓度为100 ng/kg时,多氯联苯的回收率为70.2％～113.5％.该方法前处理简便快速,准确性高,满足鱼体痕量多氯联苯残留的分析要求.     

A review of measurement methods for peracetic acid (PAA)

• Physical and chemical properties and application of peracetic acid solution. • Determination method of high concentration peracetic acid. • Determination method of residual peracetic acid (low concentration). Peroxyacetic acid has been widely used in food, medical, and synthetic chemical fields for the past several decades. Recently, peroxyacetic acid has gradually become an effective alternative disinfectant in wastewater disinfection and has strong redox capacity for removing micro-pollutants from drinking water. However, commercial peroxyacetic acid solutions are primarily multi-component mixtures of peroxyacetic acid, acetic acid, hydrogen peroxide, and water. During the process of water treatment, peroxyacetic acid and hydrogen peroxide (H₂O₂) often coexist, which limits further investigation on the properties of peroxyacetic acid. Therefore, analytical methods need to achieve a certain level of selectivity, particularly when peroxyacetic acid and hydrogen peroxide coexist. This review summarizes the measurement and detection methods of peroxyacetic acid, comparing the principle, adaptability, and relative merits of these methods.     

液氮泡沫发生器内流动特性研究

低温液氮与泡沫混合液直接接触产生氮气泡沫是一种新型的掺混形式,利用液氮高汽化比的特点,搭建液氮泡沫可视化实验装置,进行氮气-水两相流及液氮泡沫流动特性的研究。结果表明,液氮相变产生大量氮气,其与泡沫液混合产生泡沫,温度有所回升,最终趋于泡沫混合液温度;管路沿程压降较小;液氮射流破碎及流动过程可分为6个区域:低温液氮区、向上循环翻滚区、滞留区、泡沫与泡沫混合液混合区、致密泡沫区、泡沫混合液区。流体向下游流动过程中持续发泡;为防止管路结冰,需合理控制泡沫混合液与液氮流量。     

Experimental research of LNG accidental underwater release and combustion behavior

Evaluating potential hazards caused by accidental LNG release from underwater pipelines or vessels is a significant consideration in marine transportation safety. The aim of this study was to capture the dynamic behavior of LNG jet released under water and to analyze its vapor dispersion characteristics and combustion characteristics on the water surface during different release scenarios. Controlled experiments were conducted where LNG was jet released from a cryogenic storage tank. The dynamic process of LNG being jet released from orifices of different sizes and shapes, as well as the rising plume structure, were captured by a high-speed camera. The leakage flow rate and pipeline pressure were recorded by a flow meter and pressure gauge, respectively. The concentration distribution that emanated from the water surface was measured utilizing methane sensors in different positions with various wind speeds. The flame combustion characteristics of LNG vapor clouds, which immediately ignited upon the enclosed water tank, were also recorded. Additionally, the mass burning rate of the flame on the water surface was evaluated, and a new correlation between the ratio of flame length and width was established. The results indicated a large dimensionless heat release rate (Q*) and a continuous release flow rate in a limited burning area. This study could provide greater understanding of the mechanisms of LNG release and combustion behavior under water.