Mass transfer enhancement and hydrodynamic performance with wire mesh coupling solid particles in bubble column reactor

It is of vital significance to investigate mass transfer enhancements for chemical engineering processes.This work focuses on investigating the coupling influence of embedding wire mesh and adding solid particles on bubble motion and gas-liquid mass transfer process in a bubble column.Particle image velocimetry(PIV)technology was employed to analyze the flow field and bubble motion behavior,and dynamic oxygen absorption technology was used to measure the gas-liquid volumetric mass transfer coefficient(kLa).The effect of embedding wire mesh,adding solid particles,and wire mesh coupling solid particles on the flow characteristic and kLa were analyzed and compared.The results show that the gas-liquid interface area increases by 33%-72%when using the wire mesh coupling solid particles strategy compared to the gas-liquid two-phase flow,which is superior to the other two strengthening methods.Compared with the system without reinforcement,kLa in the bubble column increased by 0.5-1.8 times with wire mesh coupling solid particles method,which is higher than the sum of kLa increases with inserting wire mesh and adding particles,and the coupling reinforcement mechanism for affecting gas-liquid mass transfer process was discussed to provide a new idea for enhancing gas-liquid mass transfer.

Characterization of volatiles Tribolium castaneum(H.)in flour using solid phase microextraction–gas chromatography mass spectrometry(SPME–GCMS)

The objective of this study was to identify volatile organic compounds(VOCs)from flour,Tribolium castaneum(Herbst)and flour infested by T.castaneum separately,to confirm the difference of healthy flour and flour infested by T.castaneum and to explore the new technique to diagnose stored flour’s quality by its VOCs change.Headspace-solid phase microextraction(HS-SPME)coupled with gas chromatography(GC)and gas chromatography–mass spectrometry(GC–MS)were used to detect the VOCs of three different samples.Totally,71 different compounds were identified in flour,T.castaneum and T.castaneum infested flour.Therefore,27 VOCs were identified from flour alone,32 VOCs from T.castaneum and 39 VOCs from T.castaneum infested flour.The compound 2-ethyl-2,5-cyclohexadiene-1,4-dione is only found in T.castaneum infested flour.This suggests that 2-ethyl-2,5-cyclohexadiene-1,4-dione can be a useful VOC for detecting T.castaneum in flour.

Simultaneous Determination of Bisphenols and Alkylphenols in Water by Solid Phase Extraction and Ultra Performance Liquid Chromatography-tandem Mass Spectrometry

To establish an analytical method for determination of four bisphenols （BPA, BPB, BPF, and BPS） and two alkylphenols （4-n-OP, 4-n-NP） in water by ultra performance liquid chromatography- tandem mass spectrometry （UPLC/MS/MS）. The water samples were extracted and condensed with solid-phase extraction （SPE） using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%.

Rapid analysis of fifteen sulfonamide residues in pork and fish samples by automated on-line solid phase extraction coupled to liquid chromatography–tandem mass spectrometry

The aim of this work was to develop an automated on-line solid phase extraction(SPE)with liquid chromatography-tandem mass spectrometry method for the detection of fifteen sulfonamides in pork and fish samples.Samples were extracted with 0.2%formic acid acetonitrile solution,purified by on-line SPE device with HLB column,then separated by XBridge C18 column,using 0.1%formic acid solution and acetonitrile as the mobile phase.Mass spectrometric data was acquired under multiple reaction monitoring(MRM)mode using positive ionization electrospray.Internal standard method was used in the quantification,good linear relationship was got in range of 0.1–100 ng/mL and correlation coefficient was higher than 0.9990.The limits of detection were in the range of 0.125–2.00g/kg and the limits of quantitation were in the range of 0.250–5.00g/kg.Recoveries of the method were in range of 78.3%–99.3%,relative standard deviation were lower than 10%.The method was simple,sensitivity,and could be used for routine supervision and analysis of fifteen sulfonamides in pork and fish.

Liquid-solid mass transfer in a rotating packed bed reactor with structured foam packing

A rotating packed bed(RPB) reactor has substantially potential for the process intensification of heterogeneous catalytic reactions. However, the scarce knowledge of the liquid–solid mass transfer in the RPB reactor is a barrier for its design and scale-up. In this work, the liquid–solid mass transfer in a RPB reactor installed with structured foam packing was experimentally studied using copper dissolution by potassium dichromate. Effects of rotational speed, liquid and gas volumetric flow rate on the liquid–solid mass transfer coefficient(kLS) have been investigated. The correlation for predicting kLSwas proposed, and the deviation between the experimental and predicted values was within±12%. The liquid–solid volumetric mass transfer coefficient(kLSaLS) ranged from 0.04–0.14 1^-1, which was approximately 5 times larger than that in the packed bed reactor. This work lays the foundation for modeling of the RPB reactor packed with structured foam packing for heterogeneous catalytic reaction.

Uncertainty Evaluation of Determination of Microcystin MC-LR in Environmental Samples by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

To assess uncertainty of determination of MC-LR in environmental samples by solid phase extraction- ultra performance liquid chromatography- tandem mass spectrometry,the sources of the uncertainty were evaluated firstly,and the expanded uncertainty was calculated finally.The results show that when MC-LR concentration in the water samples was 0.50 μg/L,the expanded uncertainty was 0.00628 μg/L(k=2).

Fluid-solid coupling numerical simulation of charge process in variable-mass thermodynamic system

A joint solution model of variable-mass flow in two-phase region and fluid-solid coupling heat transfer,concerned about the charge process of variable-mass thermodynamic system,is built up and calculated by the finite element method(FEM).The results are basically consistent with relative experimental data.The calculated average heat transfer coefficient reaches 1.7×105 W/(m2·K).When the equal percentage valve is used,the system needs the minimum requirements of valve control,but brings the highest construction cost.With the decrease of initial steam pressure,the heat transfer intensity also weakens but the steam flow increases.With the initial water filling coefficient increasing or the temperature of steam supply decreasing,the amount of accumulative steam flow increases with the growth of steam pressure.When the pressure of steam supply drops,the steam flow gradient increases during the maximum opening period of control valve,and causes the maximum steam flow to increase.

Experimental Study on Gas-Solid Mass Transfer in Circulating Fluidized Beds

This study is devoted to gas-solid mass transfer behavior in heterogeneous two-phase flow. Experiments were carried out in a cold circulating fluidized bed of 3.0m in height and 72mm in diameter with naphthalene particles. Axial and radial distributions of sublimated naphthalene concentration in air were measured with an online concentration monitoring system HP GC-MS. Mass transfer coefficients were obtained under various operating condition, showing that heterogeneous flow structure strongly influences the axial and radial profiles of mass transfer coefficients. In the bottom dense region, mass transfer rate is high due to intensive dynamic behavior and higher relative slip velocity between gas and clusters. In the middle transition region and the upper diluter region, as a result of low mass transfer driving force and the influence of flow structure, mass transfer rate distribution becomes non-uniform. In conclusion, among the operating parameters influencing mass transfer coefficients, the superficial gas velocity is the most important factor and the solid circulation rate should be also taken into account.

Improved preparation and identification of aristolochic acid-DNA adducts by solid-phase extraction with liquid chromatography-tandem mass spectrometry

Aristolochic acid （AA） is a known nephrotoxin and potential carcinogen, which can form covalent DNA adducts after metabolic activation in vivo and in vitro. A simple method for preparation and characterization of aristolochic acid-DNA adducts was developed. Four AA-adducts were synthesized by a direct reaction of AAI/AAII with 2′-deoxynucleosides. The reaction mixture was first cleaned-up and pre-concentrated using solid phase extraction （SPE）, and further purified by a reversed-phase high performance liquid chromatography （HPLC）. By the application of developed SPE procedure, matrices and byproducts in reaction mixture could be greatly reduced and adducts of high purity （more than 94% as indicated by HPLC） were obtained. The purified AA-DNA adducts were identified and characterized with liquid-electrospray ionization-quadrupole-time of flight-mass spectrometry （LC-ESI-Q-TOF-MS/MS） and LC-Diode array detector-fluorescence （LC-DAD-FL） analysis. This work provides a robust tool for possible large-scale preparation of AA-DNA adduct standards, which can promote the further studies on carcinogenic and mutagenic mechanism of aristolochic acids.

Multiresidue Method for Determination of 67 Pesticides in Water Samples Using Solid-Phase Extraction with Centrifugation and Gas Chromatography-Mass Spectrometry

A new multi-residue method based on solid-phase extraction (SPE) with centrifugation was developed for determination and quantitation of 67 pesticides in water samples. Two SPE cartridges were tested: Chromabond C18 and Oasis HLB. Parameters that influence the extraction efficiency such as the eluent volume, the sample loading volume, the addition of organic solvent to water sample, sorbent drying and elute concentration were optimized. The innovation of this work was the examination of the use of a centrifugation technique in both the drying and elution steps. When combined with centrifugation, the volume of the elution solvent was reduced to 2 mL and the time for sorbent drying decreased also to 10 min under vacuum. Under the optimized conditions, this method showed good recoveries higher than 65% - 68% for the 67 analyzed pesticides using the C18 and HLB cartridges with relative standard deviations lower than 9.7% - 12.3%. Limits of quantification were between 2 and 20 ng.L–1. The simplicity of the described method, use of less of organic solvent, short procedure time, and good recoveries demonstrate the advantages of this environmentally friendly approach for routine analysis of numerous samples.

Numerical evaluation of virtual mass force coefficient of single solid particles in acceleration

Virtual mass force is an indispensable component in the momentum balance involved with dispersed particles in a multiphase system.In this work the accelerating motion of a single solid particle is mathematically formulated and solved using the vorticity-stream function formulation in an orthogonal curvilinear coordinate system.The total drag coefficient was evaluated from the numerical simulation in a range of the Reynolds number(Re)from 10 to 200 and the dimensionless acceleration(A)between2.0 to 2.0.The simulation demonstrates that the total drag is heavily correlated with A,and large deceleration even drops the drag force to a negative value.It is found that the value of virtual mass force coefficient(CV)of a spherical particle is a variable in a wide range and difficult to be correlated with A and Re.However,the total drag coefficient(CDV)is successfully correlated as a function of Re and A,and it increases as A is increased.The proposed correlation of total drag coefficient may be used for simulation of solid–liquid flow with better accuracy.

Evaluation of Sensitivity and Positive Predictive Values of Cytopathologic Diagnosis of Solid Masses in Dogs

In this retrospective study, a total of 275 solid masses were examined for cytopathologic diagnosis. Twenty four percent (67/275) of these cytologic samples were followed by surgical biopsy and histopathologic diagnosis, allowing for comparisons. On average, the cutaneous and subcutaneous solid masses were recognized when the dogs were aged between 6 and 9 years old. The origins of the solid masses included connective tissue tumors 37.1% (23/62), epithelial tissue tumors 33.9% (21/62), round cell tumors 19.4% (12/62), masses of inflammatory lesions 4.8% (3/62) and lesions due to other causes 4.8% (3/62). The sensitivity and positive predictive value (PPV) of cytopathology in the diagnosis of solid masses were 93% (62/67) and 97% (62/64), respectively. Generally, neo-plasms were over diagnosed by cytopathology as was indicated by the positive predictive value. Both the sensitivity and the PPV of cytopathology comparative to histopathology in the diagnosis of inflammatory processes were 100% (3/3). The inflammatory lesions were eventually confirmed as necrotizing myositis, necro-suppurative cystitis and endocrine inflammatory dermatopathy based on histopathology. Less than 8% (5/67) of samples were incorrectly diagnosed by cytology. The study showed high accuracy between cytological and histopathological examination of solid masses in dogs, and thus a reliable diagnostic tool in patient care.

Design of fan beam optical sensor and its application in mass flow rate measurement of pneumatically conveyed solids

The fan-beam optical sensor is made up of many semiconductor lasers and detectors fixed around the wall alternately at a cross section of pneumatically conveying pipe. When the sensor works, a scanning light source emits a 50° lamellar fan-beam through the gas-solid two phase flow, and the projection data resulting extinction effect of solid particles are detected at the same time. With the projection data, the flow rate mass can be calculated, and then the flow image can be reconstructed. In this paper, the design of the sensor including spatial arrangement of the structural parts, basic principle and measurement sensitivity distribution are introduced. The mathematical measurement model of solid mass flow rate is presented together with the testing results.

Combustion Characteristics of Solid Sustained-Release Energetic Materials

A solid sustained-release energetic material sample,an eruption device and a complete test system were prepared further to analyse the combustion characteristics of solid sustainedrelease energetic materials.The high-temperature heat flux generated by the combustion of the samples from the eruption device was used to penetrate the Q235 target plate.In addition,the meaning and calculation formula of energy density characterising the all-around performance of heat flux were proposed.The numerical simulation of the combustion effect of samples was carried out.According to the data comparison,the numerical simulation results agreed with the experimental results,and the maximum deviation between the two was less than 8.9%.In addition,the structure of the combustion wave and high-temperature jet was proposed and analysed.Based on theoretical analysis,experimental research and numerical simulation,the theoretical burning rate formula of the sample was established.The maximum error between the theoretically calculated mass burning rate and the experimental results was less than 9.8%.Therefore,using the gas-phase steady-state combustion model to study the combustion characteristics of solid sustained-release energetic materials was reasonable.The theoretical burning rate formula also had high accuracy.Therefore,the model could provide scientific and academic guidance for the theoretical research,system design and practical application of solid sustained-release energetic materials in related fields.

不同产地沃柑挥发性成分的差异分析

该研究旨在分析4个主产地(四川、重庆、云南和广西)的沃柑果皮中挥发性成分的差异性,并为沃柑的产地溯源和深加工提供数据支撑。利用顶空固相微萃取-气相色谱-质谱联用技术测定了沃柑果皮挥发性成分,共鉴定出50种挥发性成分,其中萜烯类18种、醇类11种、醛类10种、酯类8种、酮类1种、其他类2种。柠檬烯是主要的挥发性物质,月桂烯、α-蒎烯、芳樟醇、正辛醇、正辛醛、香茅醇、己醛、反式-2-己烯醛、桧烯、香芹酮和α-松油醇等次之。基于挥发性成分半定量结果,建立四川和重庆,云南和广西沃柑的正交偏最小二乘法判别分析模型,进而筛选出潜在生物标志物。结果表明,柠檬烯、芳樟醇和香茅醇可作为区分重庆和四川的潜在生物标志物,醋酸辛酯和α-松油醇可作为区分广西和云南的潜在生物标志物。

固相萃取-液相色谱-串联质谱法测定海参中62种兽药残留

目的建立固相萃取结合高效液相色谱-串联质谱同时测定海参中62种药物的检测方法。方法样品加水分散后经1.0%甲酸乙腈溶液提取,PEP固相萃取柱净化后,采用WatersX-Bridge-C18色谱柱分离、0.2%甲酸水溶液-甲醇为流动相进行梯度洗脱,使用选择离子监测模式检测。结果62种兽药在0.50~100.00ng/m L范围内呈现出良好的线性关系,线性相关系数r^(2)在0.9953~1.0000范围内。方法检出限为0.25~2.50μg/kg;在3个不同浓度添加水平下,62种兽药的平均回收率在70.3%~119.0%,批内和批间的相对标准偏差(n=5)为0.13%~14.90%,均小于15.00%。将该方法应用于30批次海参样品的检测,其中4批次样品的喹诺酮检测结果阳性,检出量为5.30~28.00μg/kg,与国家标准方法的检测结果相比,该方法对于本次喹诺酮药物筛查的准确率为100%。结论该方法灵敏度高,准确度和精密度良好,满足我国兽药残留检测要求,可适用于海参中62种兽药多残留的定性定量分析检测。

液相色谱-串联质谱法测定土壤、沉积物和水中3种新型除草剂残留

除草剂在杂草和有害植物防控上发挥着重要的作用,但其有效利用率低,大量除草剂进入环境中,对生态环境和人类健康构成了潜在威胁,因此建立环境样品中除草剂的残留分析方法尤为重要。该文采用电喷雾正离子源模式,建立了液相色谱-串联质谱法(LC-MS/MS)测定土壤、沉积物和水中异噁唑草酮、吡唑草胺和苯嘧磺草胺残留量的方法。土壤和沉积物样品经乙腈振荡提取、盐析后经C18固相萃取小柱净化,水样过滤后经C_(18)固相萃取小柱净化;再用LC-MS/MS测定样品中异噁唑草酮、吡唑草胺和苯嘧磺草胺的残留量。实验优化了仪器检测和前处理条件,考察了方法的线性关系、基质效应、检出限和定量限,并选取4种土壤、2种沉积物和水样进行了方法验证。在0.0005~0.02 mg/L范围内,异噁唑草酮、吡唑草胺、苯嘧磺草胺的线性关系均良好,r≥0.9961。3种除草剂在土壤、沉积物和水中的基质效应为-10.1%~16.5%。异噁唑草酮、吡唑草胺和苯嘧磺草胺的检出限分别为0.05、0.02、0.01μg/kg,定量限分别为0.2、0.05、0.05μg/kg。异噁唑草酮、吡唑草胺和苯嘧磺草胺在土壤、沉积物和水样中3个水平(0.005、0.1、2.0 mg/kg)下的加标回收率分别为77.2%~101.9%、77.9%~105.1%、80.8%~107.1%;相对标准偏差(RSD)分别为1.4%~12.8%、1.2%~7.7%、1.5%~11.5%。结果表明:本方法操作简单,方法稳定,定量准确,实用性强,可用于土壤、沉积物和水中异噁唑草酮、吡唑草胺和苯嘧磺草胺残留量的检测。

基于HS-SPME-GC-MS的不同成熟度‘青皮’无花果挥发性成分分析

为探讨不同成熟度威海‘青皮’无花果挥发性成分差异,本研究采用固相微萃取(SPME)和气相色谱-质谱联用技术(GC-MS)对鲜食无花果挥发性成分进行分析,并采用内标法对风味物质进行定量分析。结果显示,在威海‘青皮’无花果中共检测出73种挥发性成分,主要为酯类、醛类、醇类、烯类、烷烃类等,其中六成熟无花果检出33种、八成熟检出29种、十成熟检出36种。不同成熟度无花果的挥发性组分、特征风味物质种类和含量差异明显。

顶空箭形固相微萃取–气相色谱质谱法分析烃源岩和稠油中的金刚烷类化合物

采用顶空箭型固相微萃取–气相色谱质谱联用技术(HS-SPME Arrow-GC/MS)直接检测分析烃源岩粉末样品和稠油中的单金刚烷类和双金刚烷类化合物,考察并优化了影响萃取效率的萃取纤维头类型、萃取温度、萃取时间和解析时间等关键因素。对于小于80目的烃源岩样品,推荐最优HS-SPME Arrow实验条件为:使用250μm PDMS箭形固相微萃取头, 120℃下萃取20 min, 260℃下解析8 min。对于稠油,当使用250μm PDMS萃取纤维头、萃取温度为120~150℃、萃取时间为15~20 min、解析时间为3~8 min时,稠油中的单金刚烷类和双金刚烷类化合物都能取得较理想的质谱响应。该方法实现了对烃源岩粉末和稠油中金刚烷类化合物的直接分析,灵敏度高,检出限低(0.004~0.977 ng/g),重现性好,测量峰面积和比值参数的相对标准偏差分别小于20%和5%,避免了复杂的前处理过程,是一种快捷可靠的分析方法。