用低功率微波热雾化器与十字交叉气动雾化器作为ICP-AES进样装置的比较

在 ICP- AES中 ,最常用来引入液体样品的方法是雾化法 .因此 ,雾化器雾化效率的高低直接影响到 ICP- AES的分析性能 [1,2 ] .目前 ,在 ICP- AES中最常用的雾化器是气动雾化器 (PN) .它的优点是简单、稳定性好 ;缺点是产生的雾滴的直径范围很宽 (一般为 1～ 50 μm) ,进样效率低 ,一般仅为 1 %～3% [3] .热雾化器是近年发展起来的一种雾化效率较高的雾化法 ,已被越来越多地用于 ICP- AES[4～ 7] .热雾化法的雾化原理与同轴气动雾化法类似 ,不同之处在于 :对于热雾化法来说 ,(1 )雾化所需的气体来自于液体样品本身而不是外加的惰性…     

用于MIP-AES的气动雾化法的研究

水溶液样品经气动雾化后引入低功率微波诱导等离子体, 由于采用了新的去溶系统和分离器, 大大改进了微波诱导等离子体原子发射光谱法的光谱分析性能。详细考察了各实验参数对测定一些元素的影响。这些元素的检出限和测定精密度令人满意。     

低功率微波热雾化器与同轴气动雾化器作为电感耦合等离子体发射光谱法进样装置的比较

对用低功率微波热雾化器(MWTN)和同轴气动雾化器(PN)作为电感耦合等离子体发射光谱仪(ICP-AES)进样装置时，仪器的操作条件(样品提升速率(Q1)、载气流速(Fc))进行了选择和比较。在选定的条件下，比较了两种雾化器的分析性能。发现HCI的浓度对两种雾化器的影响不同，对于MWTN，Cr、Cd、Co、Mn和Ls，谱线的发射强度随HCl浓度的增加而略有增加；而对于PN，谱线的发射强度随HCl浓度的增加而略有降低；MWTN对于上述5种元素的检出限均优于PN，而精密度则不如后者。     

用微波诱导等离子体发射光谱法测定铁及其它一些元素

水溶液样品用超声雾化法雾化经加热后用常规冷凝器和浓H_2SO_4吸收法去溶,然后引入微波等离子体。详细考察了载气流量、微波功率和HCl浓度等实验条件的影响和KCl对谱线的增强作用。测定了一些地质样品中的铁,得到了满意的结果。     

一种可用于微波等离子体炬原子发射光谱法的热雾化系统

建立了一种新的热雾化系统，用蠕动泵代替高压泵，去掉了加热管部分，使整个热雾化系统更加紧凑，经济，并将其用于微波等离子体炬（ＭＰＴ）－原子发射光谱法（ＡＥＳ），考察了实验参数的影响，与气动雾化相比，对Ｍｇ，Ｐｂ的检出限改善了５～１０倍，同时发现本装置具有元素选择性增强的现象。     

微波浸取测定土壤中总溶解固体

微波溶样技术是近年来分析化学领域中应用很广泛的一种样品预处理的新技术 ,它具有对样品的分析快速、安全、无污染、无损失、省试剂等特点[1,2 ] 。由于水溶性无机盐是吸附在土壤颗粒表面 ,而土壤颗粒是一种蜂窝状结构 ,渗透在蜂窝内的盐分较难溶解 ,所以传统的测定土壤中总溶解固体的方法是采用振荡法[3 ,4 ] ,此法在测定大量样品时费时、操作繁琐。本文研究了用微波溶样方法浸取土壤中的总溶解固体。试验表明 ,本法简单、快速 ,且浸取完全 ,测定结果准确可靠。1　试验部分1.1　仪器与试剂ＷＲ 1Ｃ型微波样品处理系统双层密封微波消化罐Ｃ…     

一种新型微波辅助萃取法用于中药刺五加中总黄酮萃取的研究

微波萃取法是目前世界上公认的绿色样品预处理技术之一 .它在环境、生化、食品、工业以及天然产物和中药等领域均有广泛的应用 [1～ 4 ] .目前 ,最常用的微波萃取系统有两种 [5] ,一种是使用多模式微波炉 ,在密闭容器中加热样品及有机溶剂 ,将目的组分从样品基体中萃取出来 .由于在密闭容器中 ,被萃取样品和溶剂处于高压下 ,温度很高 ,使待萃取物的溶解度增大 ,可获得更高的萃取率 .同时 ,用于这种微波萃取的系统一般可同时容纳 9～ 1 2个萃取罐 ,使试样的批量处理能力大大提高 .该法最主要的缺点是萃取后的液体一般需经离心分离或微孔玻璃…     

一种原子光谱分析用新激发光源——千瓦级微波等离子体炬(kW-MPT)

<正>微波等离子体炬(MPT)[1]在小功率下工作时,形成的ArM PT原子光谱分析技术(ArM PT-AES)只要在进样系统中加入一套溶液雾化和去溶装置,把样品气溶胶中大量存在的溶剂水除去后,对多种元素的检测能力即已接近在千瓦以上功率下工作的电感耦合等离子体发射光谱(ICP-AES)[2~5],而以氦作为工作气体的He MPT-AES还可检测包括ICP-AES难以检测的卤素在内的非金属元素[2].如果将其     

微波法高度分散CuCl_2-β沸石上CO吸附的IR光谱研究

近年来 ,人们发现含铜沸石对 NO和 CO等有害气体的直接分解具有较高的活性和较好的稳定性 [1～ 3] .催化剂的活性与其铜含量密切相关 ,而由传统离子交换法制得的沸石催化剂中铜含量较低 ,且受沸石骨架中铝含量的限制 [4 ] .直接固态离子交换法是将金属离子引入沸石中的有效途径 [5～ 7] .本文采用微波法制备了 Cu Cl2 高度分散的 β沸石 ,用 XRD和 2 9Si MAS NMR对催化剂进行了表征 ,并以CO吸附 IR光谱法考察了 Cu Cl2 在β沸石中的扩散机理 .1　实验部分1 .1　样品的制备　将自制 β沸石原粉 [8,9]于 82 3K焙烧 4h以除去有机模板…     

影响微波辅助萃取虎杖中白藜芦醇产率的一些重要操作参数

研究了溶剂类型以及萃取时间和温度、微波功率、虎杖颗粒大小和水分等主要操作参数对微波辅助萃取虎杖(po1ygonum cuspidatum)中白黎芦醇(Res)产率的影响。实验表明：由于甲醇和丙酮具有较高的介电常数和损耗因子，是微波辅助萃取Res的最佳选择。微波辅助萃取温度和时间以及虎杖颗粒大小的影响较显著，其次为虎杖样品水分。微波功率在所实验范围内(300-1200W)基本无影响。最佳的萃取条件为：温度80℃；时间15ｍin；微波功率800－900Ｗ；虎杖颗粒大小为0．45—0．30mm；水分含量约为20％。     

Determination of metal concentrations in lichen samples by inductively coupled plasma atomic emission spectroscopy technique after applying different digestion procedures

Three digestion procedures have been tested on lichen samples for application in the determination of major, minor and trace elements (Al, Ca, Cd, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, V and Zn) in lichen samples collected in Aegean Region of Turkey by inductively coupled plasma atomic emission spectrometer (ICP-AES). The acid mixture of concentrated HNO₃, H₂O₂ and HF were used. The instrument was optimized using lichen matrix considering RF power, nebulizer pressure, auxiliary flow rate and pump rate. The accuracy of the overall analyses was first estimated by analysis of two certified reference materials. Good agreement between measured and reference values were found for almost all elements. As the second way of determining the accuracy, results obtained from independent analytical techniques (ICP-AES and instrumental neutron activation analysis (INAA)) were compared for all elements by analyzing real samples. Correlation coefficients of two techniques for the elements ranged between 0.70 (Mg) and 0.96 (Fe). Among the three digestion systems, namely microwave, open vessel and acid bomb, microwave digestion system gave the best recovery results. The method detection limit (MDL) was computed using reagent blanks of microwave digestion system since it provides cleaner sample preparation. Detection limit is adequate for all elements to determine the elements in lichen samples. The precision was assessed from the replicate analyses of reagent blanks of microwave digestion system and was found to be less than 1.5% relative standard deviation (R.S.D.).     

Thermospray nebulizer as sample introduction technique for microwave plasma torch atomic emission spectrometry

A thermospray nebulizer was used as a sample introduction device for microwave plasma torch (MPT) atomic emission spectrometry (AES). Experimental parameters, including the power supplied to the MPT, the flow rates of support and carrier gases, the observation height, the sample uptake rate, the thermospray working temperature, the temperature of the aerosol spray chamber and cooling water were optimized. Under optimum conditions, the relative standard deviation (RSD) of 10 measurements for 21 elements is in the range 0.3–2.0%. The detection limits were improved in comparison with the ultrasonic nebulizer as sample introduction technique for MPT–AES. The inclusion of 20% methanol into the MPT showed there is no effect on the stability of MPT discharge. The technique can thus be held to have the potential for interface to reverse-phase HPLC systems.     

热喷雾作为电感耦合等离子体原子发射光谱的进样技术

设计并建立了热喷雾器及其去溶装置。用热喷雾作为电感耦合等离子体原子发射光谱的进样技术，并对其性能作了系统研究。与气动雾化器比较，对２３个元素检出限的改善为５￣２０倍。     

A low-energy-consumption electroactive valveless hydrogel micropump for long-term biomedical applications

Stimuli-responsive hydrogels have attracted considerable interest in the field of microfluidics due to their ability to transform electrical energy directly into mechanical work through swelling, bending, and other deformations. In particular, electroactive hydrogels hold great promise for biomedical micropumping applications such as implantable drug delivery systems. In such applications, energy consumption rate and durability are key properties. Here, we developed a valveless micropump system that utilizes a hydrogel as the main actuator, and tested its performance over 6 months of continuous operation. The proposed micropump system, powered by a single 1.5 V commercial battery, expended very little energy (less than 750 μWs per stroke) while pumping 0.9 wt% saline solution under a low voltage (less than 1 V), and remained fully functional after 6 months. CFD simulations were conducted to improve the microchannel geometry so as to minimize the backflow caused by the valveless mechanism of the system. Based on the simulation results, an asymmetric geometry and a stop post were introduced to enhance the pumping performance. To demonstrate the feasibility of the proposed system as a drug delivery pump, an anti-cancer drug (adriamycin) was perfused to human breast cancer cells (MCF-7) using the pump. The present study showed that the proposed system can operate continuously for long periods with low energy consumption, powered by a single 1.5 V battery, making it a promising candidate for an implantable drug delivery system.     

AC electroosmotic pump with bubble-free palladium electrodes and rectifying polymer membrane valves

We present the design, test and theoretical analysis of a novel micropump. The purpose is to make a pump with large flow rate (approximately 10 microL min-1) and high pressure capacity (approximately 1 bar) powered by a low voltage DeltaV<30 V. The pump is operated in AC mode with an electroosmotic actuator in connection with a full wave rectifying valve system. Individual valves are based on a flexible membrane with a slit. Bubble-free palladium electrodes are implemented in order to increase the range of applications and reduce maintenance.     

A micro-spherical heart pump powered by cultured cardiomyocytes

Miniaturization of chemical or biochemical systems creates extremely efficient devices exploiting the advantages of microspaces. Although they are often targeted for implanted tissue engineered organs or drug-delivery devices because of their highly integrated systems, microfluidic devices are usually powered by external energy sources and therefore difficult to be used in vivo. A microfluidic device powered without the need for external energy sources or stimuli is needed. Previously, we demonstrated the concept of a cardiomyocyte pump using only chemical energy input to cells as a driver (Yo Tanaka, Keisuke Morishima, Tatsuya Shimizu, Akihiko Kikuchi, Masayuki Yamato, Teruo Okano and Takehiko Kitamori, Lab Chip, 6(3), pp. 362-368). However, the structure of this prototype pump described there included complicated mechanical components and fabricated compartments. Here, we have created a micro-spherical heart-like pump powered by spontaneously contracting cardiomyocyte sheets driven without a need for external energy sources or coupled stimuli. This device was fabricated by wrapping a beating cardiomyocyte sheet exhibiting large contractile forces around a fabricated hollow elastomeric sphere (5 mm diameter, 250 microm polymer thickness) fixed with inlet and outlet ports. Fluid oscillations in a capillary connected to the hollow sphere induced by the synchronously pulsating cardiomyocyte sheet were confirmed, and the device continually worked for at least 5 days in this system. This bio/artificial hybrid fluidic pump device is innovative not only because it is driven by cells using only chemical energy input, but also because the design is an optimum structure (sphere). We anticipate that this device might be applied for various purposes including a bio-actuator for medical implant devices that relies on biochemical energy, not electrical interfacing.     

Characterization of aerosols generated by thermospray nebulization for atomic spectroscopy

The performance of an inductively coupled plasma (ICP) for atomic emission spectroscopy (AES) is strongly dependent upon the sample introduction system. The Thermospray Vaporizer has recently been shown to yield enhanced sensitivity compared to conventional pneumatic nebulizers when used as a sample introduction source for the ICP. This report is a study of the properties of the aerosols produced by the thermospray. Aerosol particle diameter distributions have been related to droplet size distribution and nebulization efficiencies as a function of the relevant variables of the nebulization system. The results help explain high emission intensities and lower detection limits achieved using the thermospray. The higher efficiencies with thermospray, compared to conventional pneumatic nebulization, also makes the thermospray a prime candidate for sample introduction into molecular gas ICPs.     

微波消解-FAAS法测定元胡中的镁

采用微波消解法溶解样品,火焰原子吸收分光光度法（FAAS）测定了元胡中的镁,探讨了微波消解预处理的条件,优化了FAAS测定参数。结果表明,该法具有良好的准确度和精密度,加标回收率在93．25％-96．25％范围内,相对标准偏差（RSD）1．16％,线性范围在0．5～3．5μg·mL^-1之间,为研究金属元素在元胡中的功能提供了有用的数据。