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1.
内装活性氧化铝(碱式)和阴离子交换树脂的微型柱流动注射在线富集分离水体中的铬(Ⅲ)和铬(Ⅵ),火焰原子吸收法直接检测。微型住可同时富集两种价态的离子,分别用1mol/L的NH4NO3和HNO3洗脱Cr(Ⅵ)和Cr(Ⅲ)于喷雾器中。进样时间25s,铬(Ⅵ)和铬(Ⅲ)的富集倍数分别为11倍和20倍,实际水样的加标回收率在90%~106%之间;分析速率为50个样/h;铬(Ⅵ)、铬(Ⅲ)的检出限(3δ)分别为1.5μg/L和0.7μg/L;相对标准偏差(50μg/L)分别为1.9%和2.6%。  相似文献   

2.
壳聚糖-CdS复合膜制备及其对吡啶的传感特性   总被引:10,自引:0,他引:10  
利用壳聚糖(CS)易于成膜的特点,模拟生物矿化,在有机物调制下通过异相成核生长制备了CS/CdS纳米颗粒复合膜.研究了成膜条件对膜的水热稳定性和发光性能的影响,以及CS/CdS纳米颗粒复合膜对水体中吡啶的响应特性.扫描电镜分析表明CS/CdS纳米颗粒复合膜均匀性好, CdS以物理掺杂方式均匀分布于CS薄膜中, CdS颗粒尺寸在70 nm左右.但薄膜荧光光谱位置和形状表明实际发光的CdS簇集体直径小于20 nm.由此推测电镜观察到的CdS颗粒可能是由许多CdS小颗粒聚集而成,小颗粒之间因有机物的存在而相互隔离. CS/CdS纳米颗粒复合膜的荧光发射对水体中吡啶的存在十分敏感,微量吡啶的存在会引起薄膜荧光发射急剧增强.除铜和碘离子外,水体系中其他常见离子对薄膜荧光发射没有显著影响,预期CS/CdS纳米颗粒复合薄膜有可能发展成为一种重要的水体系吡啶测定专用传感薄膜材料.  相似文献   

3.
龙岩煤不同宏观煤岩组分的颗粒及其燃烧性质实验研究   总被引:5,自引:2,他引:5  
用浮选法分选出3个密度档、代表不同宏观岩相的龙岩煤颗粒,进行工业分析、元素分析和煤岩分析;并进一步通过扫描电镜结合压汞实验分析颗粒的结构,通过热天平实验研究不同宏观煤岩组分的燃烧性质。结果表明,(1)龙岩煤颗粒的煤岩主要由镜质组组成。其中,亮煤富含镜质组,密度相对较低,挥发分极少、固定碳高达80%以上;暗煤富含矿物质成分,密度极高但含碳量却很少,热值很低,接近于原煤中的矸石。灰煤中惰性组的量是三种岩相中最多的,其工业分析性质与原煤接近;(2)龙岩煤颗粒结构致密,密度在1.6g/cm3以上。颗粒中绝大多数孔隙的孔径在1μm以下。其中亮煤颗粒表面光洁致密,内部孔隙以亚微孔(0.01μm<d<0.10μm)居多,大孔径较少,比表面积较大;暗煤颗粒的表面孔隙较发达,内部结构相对较蓬松,颗粒中细孔、微孔、亚微孔都存在;而灰煤颗粒中的孔隙最不发达,以超微孔(d<0.01μm)为主;(3)不同宏观煤岩组分龙岩煤的着火温度相近,约580℃;但燃尽温度相差较大:亮煤最高,大于800℃;暗煤最低,两者相差约100℃;(4) 龙岩煤不同宏观煤岩颗粒的反应性按亮煤、煤(混煤)、灰煤、暗煤依次递减,亮煤的反应性最好,暗煤的反应性最差。  相似文献   

4.
利用改性皮革胶原纤维作为水体中重金属离子的富集材料,研究了该材料对水体中Cd^2+、Cr^3+、Pb^2+、Ni^2+、Co^2+等重金属离子的分离富集能力。实验表明,在pH4~7的酸性和中性的条件下,该材料对重金属离子的富集量最大。其中,Cr^3+在pH4~5时富集率达到100%;Co^2+、Ni^2+在pH6~7时富集率达到100%左右;Cd^2+和Pb^2+在pH8~9时富集率达到100%左右;在混和溶液中和存在络合配位体时,可以通过控制待测液的酸度对水体中的重金属离子进行选择性吸附。通过样品的分析,可以利用改性皮革胶原纤维作为测定水体中的重金属离子的吸附剂,对水体中的重金属离子进行分析测定。  相似文献   

5.
中药配方颗粒红外指纹图谱研究   总被引:16,自引:0,他引:16  
黄昊  李静  秦竹  周群  孙素琴 《分析化学》2003,31(7):828-832
采用傅里叶变换红外光谱(FTIR)技术分析鉴别了350种中药配方颗粒红外指纹图谱的结构特征。结果表明,借助于各种药用植物和动物配方颗粒的FTIR指纹图谱的差别可进行快速分类鉴别;根据配方颗粒与中药原药材谱图之间的相关性,以及中药材经过炮制、加热、水提处理后,配方颗粒与原药材之间在谱图上所代表的化学成分上的异同可以进行中药配方颗粒的质量控制;凭借不同炮制方法与未经炮制处理的配方颗粒间FTIR谱图的差别,可以进一步分析炮制后配方颗粒化学成分的变化,不同炮制方法对配方颗粒化学成分的影响;对于不同厂家的配方颗粒及同一厂家不同生产批号的配方颗粒也进行了较系统的分析研究。方法快速,简便,专属性强,不需对样品进行分离提取。  相似文献   

6.
杨松  邹楠  高云  许乐园  张文文  潘灿平  慕卫 《色谱》2020,38(7):826-832
建立了固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)同时检测环境水体中不同极性范围的18种农药残留的分析方法。样品经大体积固相萃取装置,以2 mL/min的速率通过Cleanrt®-PEP固相萃取柱进行净化和富集,浓缩50倍后结合UPLC-MS/MS检测,外标法定量。研究表明,目标化合物在0.5~50 μg/L范围内线性关系良好,线性相关系数(R2)≥0.995;在10、100和1000 ng/L 3个添加水下,18种农药在3种不同环境水体中的平均回收率为71.3%~105.9%,相对标准偏差(RSD,n=5)为1.3%~9.9%;定量限(LOQ)均为10 ng/L。该方法应用于泰安市区周围水环境的检测,各采集位点均未检出农药残留。该方法具有净化效果好、通用性强、灵敏度高、准确度高和操作简单等优点,适用于环境水体中18种农药的残留检测。  相似文献   

7.
综合考虑化学反应速率、内扩散和反应热的影响,建立单个催化剂颗粒表面烧焦过程的数学模型,模拟研究了粒径1000μm的球形催化剂的表面烧焦过程。研究表明,650℃再生,化学反应速率为控制步骤,催化剂的再生过程符合整体反应模型;800℃再生,内扩散影响严重,碳含量、氧分压沿径向变化剧烈。再生温度升高,催化剂颗粒的瞬时温升增大;催化剂初始碳含量越高、CO2/CO摩尔比越大,催化剂颗粒的瞬时温升越大,但再生过程所需时间增加;催化剂颗粒的径向温度分布均一。在排除外扩散影响的条件下,反应气速对再生过程影响很小。  相似文献   

8.
单分散二氧化硅球形颗粒的制备与形成机理   总被引:52,自引:1,他引:52  
赵丽  余家国  程蓓  赵修建 《化学学报》2003,61(4):562-566
在醇水混合溶剂中以氨作催化剂,正硅酸乙酯为硅源,通过溶胶—凝胶工艺制 备单分散二氧化硅球形颗粒,通过透视电镜进行研究各种反应条件如溶剂类型、氨 和水的浓度、水解温度等对二氧化硅的颗粒大小和形貌的影响.结果显示:以甲醇 和乙醇为溶剂可以形成单分散的二氧化硅球形颗粒,以丙醇和丁醇为溶剂,二氧化 硅球形颗粒容易聚集;在其它条件不变的情况下,球形颗粒的粒径随水和硅源的浓 度增加而增大;而且水解温度的升高,生成的颗粒粒径也逐渐增大,仔细研究和讨 论了二氧化硅颗粒在不同反应条件下的形成机理.  相似文献   

9.
内装活性氧化铝(碱式)和阴离子交换树脂的微型柱流动注射在线富集分离水体中的铬(Ⅱ)和铬(Ⅳ),火焰原子吸收法直接检测,微型柱可同时富集两种价态的离子,分别用1mol/L的NH4NO3和HNO3洗脱Cr(Ⅳ)和Cr(Ⅲ)于喷雾器中,进样时间25s,铬(Ⅳ)和铬(Ⅲ)的富集倍数分别为11倍和20倍,实际水样的加标回收率在90%~106%之间,分析速率为50个样/h,铬(Ⅳ),铬(Ⅲ)的检出限(3δ)分  相似文献   

10.
大孔球形纤维素吸附剂的制备及性能研究   总被引:1,自引:0,他引:1  
本课题以天然棉纤维为原料,通过碱化、老化、碳化以及溶解,制得纤维素粘胶,按一定比例加入Ca-CO3,然后,采用反相悬浮再生法,制备纤维素球,在HCl-NaCl-CaCl2。混合溶液中除去CaCO3后,得大孔球形纤维素经SEM对整体结构和表面结构进行了表征。这种大孔球经环氧化后,制备了一种开链氮杂冠醚化大孔球形纤维素吸附剂(PSC-OCAC),测定了PSC-OCAC对几种常见金属离子的吸附性能,并应用到江河水体中几种金属的分离、富集,建立起PSC-OCAC-分离富集-火焰原子吸收分光光度法,测定水体中痕量重金属总量的方法,测定了南充境内两河、嘉陵江水体中的几种常见重金属含量。  相似文献   

11.
Sedimentation and drying dissipative patterns formed in the course of drying green tea (Ocha) have been studied in tea cup (Ochawan), glass dish, polystyrene dish, and watch glass. The broad-ring patterns are formed within several tens of minutes in suspension state by the convectional flow of water and colloidal particles of green tea (7 μm in mean size and 5 μm in its dispersion from the mean size). Formation of the broad-ring patterns is retarded when a tea cup is covered with a watch glass, which demonstrates the important role of the convectional flow of tea particles and water induced by the evaporation of water at the air-suspension interface under the gravity. The sedimentary particles are suspended above the substrate plate and always move by the convectional flow of water. The broad-ring patterns become sharp just before the solidification occurs. The broad rings are formed even in an inclined glass dish, though the rings are transformed slightly, which demonstrates the strong convectional flow of the particles. The drying broad rings and the microscopic fine structures are formed in the solidification processes on the bases of the convectional and sedimentation patterns in suspension state.  相似文献   

12.
磁流体净化含油污水研究   总被引:10,自引:0,他引:10  
研究了磁粉性能与表面活性剂对除油效果的影响,并探讨了除油机理。结果表明,应用磁流体净化含油污水,可使水中含油量从几百ppm降到几十ppm。  相似文献   

13.
A mixture of natural and anthropogenic particles is ubiquitous in the troposphere and exerts an important influence on air quality. This work reports the study of mixing and heterogeneous chemistry of particles of natural-like mineral dust (CaCO(3)) and anthropogenic-like microparticle (PbSO(4)) in turbulent air flow under varying relative humidity. Sparse monolayers of laboratory-generated particles were collected on substrates using impaction. The grain size distribution and chemistry of micrometer-sized particles were determined as CaCO(3)-PbSO(4) internal and external mixtures by Raman imaging, scanning electron microscopy, and time-of-flight static secondary ionization mass spectrometry. The condensation of a thin water layer on mixed aggregates initiates the formation of complex internal mixtures of Pb(3)(CO(3))(2)(OH)(2), PbCO(3), CaSO(4)·2H(2)O, CaCO(3), and PbSO(4) fine particles. These heterogeneous chemistry processes which may occur in ambient air can increase dramatically the amounts of hazardous breathable particles.  相似文献   

14.
润湿剂促进燃煤细颗粒声波团聚脱除的实验研究   总被引:3,自引:0,他引:3  
在声波团聚室中研究了润湿剂液滴与细颗粒碰撞团聚脱除特性,提出了一种利用润湿剂促进细颗粒在声波场中捕集的新方法。结果表明,不同润湿剂溶液对细颗粒在声波场中的团聚脱除效果存在较大差异,采用JFC和FS-310润湿剂溶液时,细颗粒分级脱除效率与采用水时的分级脱除效率相近。而SDS和Silanol w22溶液,则可有效提高细颗粒在各粒径段的分级脱除效率。细颗粒在声波场中的脱除效率与润湿剂润湿性能具有很好的相关性,随润湿剂对细颗粒相对接触角增大而降低,在声压级为150 dB时,相对接触角由83°降低到0°,细颗粒脱除效率提高了18%,在无声场作用下,脱除效率仅提高了5%。细颗粒脱除效率随声压级的增大而提高,在低声压级条件下,添加润湿剂可有效提高细颗粒脱除效率,声压级在130 dB时,添加SDS溶液液滴后细颗粒脱除效率比声场单独作用时的脱除效率提高了25%。表明添加润湿剂可有效提高细颗粒在声波场中的团聚脱除效率,实现在低声压级条件下,获得高的细颗粒脱除效率。  相似文献   

15.
To obtain large-sized, monodispersed spherical particles of silica by sol precipitation, a seed particle growth method was attempted. The formation of secondary particles during seed particle growth causing a multimodal distribution of particle size was suppressed via fine adjustment of the reaction conditions, such as TEOS, ammonia, and water concentrations, as well as operational conditions such as feeding time and agitation speed. Among the reaction conditions, an increase of TEOS concentration promoted secondary particle formation, resulting in bimodal particle distribution. However, secondary particle formation was depressed with increasing ammonia and water concentrations. In addition, long feeding time (low feed flow rate) and rigorous agitation significantly reduced secondary particle formation because they contributed to the slow generation of supersaturation and rapid seed particle growth, respectively.  相似文献   

16.
Modeling of a counterflow plasma reactor   总被引:2,自引:0,他引:2  
Modeling of a counterflow plasma reactor is presented, using liquid injection for the synthesis of fine particles. An experimental reactor has been developed in this laboratory, and feasibility has been demonstrated for synthesizing advanced ceramic powders. The flow field calculations show two major recirculating regions which are of importance for increasing the particles' residence time inside of the reactor. In addition, the temperature within these recirculation zones remains relatively uniform. For simulation, water droplet trajectories have been calculated for droplets produced by an injection probe. It is shown that the droplets in a size range below 50 m in diameter will follow the streamlines and evaporate completely within a short traveling distance. This finding suggests that this reactor configuration provides a favorable environment for the synthesis of fine particles using liquid precursors.  相似文献   

17.
The formation of equilibrium spectrum of particles in a disperse system with the coagulation–fragmentation of aggregates at a steady-state shear flow was analyzed in terms of two-fraction model. It was suggested that an initial dispersed phase contains only small particles coagulating by the Brownian mechanism; the growth of larger aggregates proceeds by the gradient mechanism and is accompanied by the detachment of fragments. Parameters of equilibrium spectrum characterizing average masses and the number of particles in fine and coarse fractions were determined as functions of a flow shear rate, aggregate fractal dimension, parameters of particle interaction in aggregates, and the properties of the initial dispersed phase.  相似文献   

18.
Bacterial cold water disease, caused by Flavobacterium psychrophilum, is a serious problem in the aquaculture industry worldwide. Several methods to prevent and treat cold water disease have been studied. Although detection at the early stage of F. psychrophilum infection is very important for the prevention and treatment of cold water disease, an effective detection method has not yet been developed. The use of flow cytometry (FCM) for the rapid determination of bacterial cell numbers with high sensitivity is beginning to attract attention. Immunomagnetic separation (IMS) has also been used to detect F. psychrophilum. The purpose of the present study was to develop a method to quickly determine the number of bacterial cells by combining the FCM and IMS methods. Because samples can be more effectively concentrated using smaller magnetic beads and stronger magnetism, we used carbonyl iron powder as the magnetic beads for the IMS. The detection level of F. psychrophilum using FCM combined with IMS was 5 orders lower than that using FCM without IMS. The values determined using FCM combined with IMS strongly correlated with those obtained using the colony-counting method, in the range of approximately 10–108 colony-forming units per milliliter. One FCM assay could be completed within 60 s and the total assay time, including sample preparation, was less than 2 h. The combined method of FCM with IMS developed in this study can be used reliably for the rapid detection of F. psychrophilum.  相似文献   

19.
The content of the fine and ultrafine particles in the raw material results in difficulty of the separation, the loss of the valuable components and ecological contamination. Secondary using of the fine particles is impossible without their granulation. This problem has been solved by the agglomeration-in-liquid method.An agglomeration-in-liquid method is a process to produce agglomerates in a liquid phase from solid particles suspended in the liquid. The surface of solid particles and the binding liquid must be of identical polarity, but the continuous phase must be of the opposite polarity. The water solutions of the surfactant are the binding liquids or the organic liquids.  相似文献   

20.
Nanosized pure TiO2 particles with high crystallinity and large surface area were prepared by hydrolysis of tetrabutyl titanate in water/Triton X-100/isooctane reverse micelle solutions as reaction media followed by hydrothermal treatment to improve crystallinity. The prepared TiO2 nanoparticles were characterized by XRD, BET, TGA, FT-IR and TEM. The size of ultrafine particles was controlled by changing the water content of the reverse micelle solution. The TiO2 particles showed monodispersity, large surface area and high degrees of crystallinity and thermostability. The photocatalytic activity of the TiO2 particles was evaluated by decomposition of toluene in the gas phase. The activity of the TiO2 nanoparticles was higher than that of commercially available anatase fine particles, such as ST-01, which is one of the most active photocatalysts for degradation of organic compounds in the gas phase.  相似文献   

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