测定黄磷中砷方法的样品前处理的改进

标准方法(GB 7816-1998)测定黄磷中砷时,采用敞开式消解法预处理样品。实践表明该方法耗时,易引入污染,造成测定误差,而且稍有不慎易使黄磷自燃。作为改进,提出了回流冷凝消解法,即2~3 g试样于硝酸(3+2)溶液60 mL中,在160℃电热板上加热回流消解。消解完成后的试液按Ag-DDTC方法进行砷的测定。结果表明:回流冷凝消解法不仅避免了试样的自燃,而且大大缩短了试样消解时间,所测得砷结果的准确度达到原标准方法的水平。     

不同色浆质量分数的水性聚氨酯涂料对聚氯乙烯表皮低温爆破性能的影响

本文制备了一系列不同色浆质量分数的水性聚氨酯涂料,并将其喷涂在汽车仪表板聚氯乙烯(PVC)表皮的背面形成复合材料。 用旋转流变仪表征了涂料的粘度以评价其喷涂性能;用差示扫描量热仪表征了材料的玻璃化转变温度(T_g);利用万能材料试验机表征了材料在-30 ℃条件下的拉伸性能及抗撕裂性能;用动态热机械分析仪表征了材料的损耗比随温度的变化。 结果表明:不同色浆质量分数的涂料都能喷涂,含有涂层材料PVC表皮在-30 ℃低温爆破性能与涂层材料的T_g、低温拉伸性能、抗撕裂性能的关系并不大,而与涂层材料的阻尼性能直接相关。 材料的阻尼性能越好,其低温爆破性能越好。     

结晶度对尖晶石LiMn2O4动力学性质的影响

应用溶胶-凝胶法制备两种结晶度尖晶石锂锰氧化物.X射线衍射(XRD)、电感耦合等离子体原子发射光谱(ICP)、扫描电镜(SEM)、恒电流充放电、循环伏安(CV)和交流阻抗谱(EIS)等方法测试表明:以较高温度焙烧制得的L iMn2O4样品结晶度较高,但结晶度较低的样品却具有较高的放电容量和较好的循环稳定性,这主要是结晶度较低的样品具有较快的电荷交换速率和锂离子扩散速率.     

Pesticide analysis by micellar electrokinetic capillary chromatography

On-capillary sample concentration using sample stacking for the improvement of detection limits for various pesticides separated by micellar electrokinetic capillary chromatography was examined. The dependence of the stacking on different parameters was investigated. An approximately 30-fold preconcentration was achieved by applying sample stacking. Employing a two-step enrichment process (solid-phase extraction combined with sample stacking), detection limits were improved and the sample volume for SPE was reduced. In addition, the total time for the analysis was considerably reduced. Detection limits were between 0.01 and 0.1 ng/ml under these enrichment conditions.     

An automatic sampling device for capillary zone electrophoresis

An automatic sampling device has been developed for capillary zone electrophoresis. The sample is introduced to the column electrokinetically by rapidly exchanging buffer for sample in a narrow channel drilled in a plexiglass block. The autosampler is capable, under computer control, of performing multiple sample injections from a large volume sample source (such as a reaction vessel) as the sample concentration changes, and thus presents the possibility of analyzing time-varying processes by CZE. Peak area reproducibility in electropherograms obtained after use of the sampler is less than 1% and efficiency is more than 2.2 × 10⁵ theoretical plates.     

Electrospray ionization mass spectrometry from discrete nanoliter‐sized sample volumes

We describe a method for nanoelectrospray ionization mass spectrometry (nESI‐MS) of very small sample volumes. Nanoliter‐sized sample droplets were taken up by suction into a nanoelectrospray needle from a silicon microchip prior to ESI. To avoid a rapid evaporation of the small sample volumes, all manipulation steps were performed under a cover of fluorocarbon liquid. Sample volumes down to 1.5 nL were successfully analyzed, and an absolute limit of detection of 105 attomole of insulin (chain B, oxidized) was obtained. The open access to the sample droplets on the silicon chip provides the possibility to add reagents to the sample droplets and perform chemical reactions under an extended period of time. This was demonstrated in an example where we performed a tryptic digestion of cytochrome C in a nanoliter‐sized sample volume for 2.5 h, followed by monitoring the outcome of the reaction with nESI‐MS. The technology was also utilized for tandem mass spectrometry (MS/MS) sequencing analysis of a 2 nL solution of angiotensin I. Copyright © 2010 John Wiley & Sons, Ltd.     

超高效液相色谱-串联质谱法测定食品中的三氯蔗糖

建立了食品中三氯蔗糖的超高效液相色谱-电喷雾串联质谱(UPLC- MS/MS)测定方法.样品中的三氯蔗糖用水提取,简单除杂后根据样品基质选用HLB柱净化或用沉淀剂去除样品中的脂肪和蛋白质,用甲醇-水定容.经反相色谱柱分离后,采用多反应监测(MRM)负离子模式检测,定性离子对为m/z 395.07/358.90和397....     

A spinning thermometer to monitor microwave heating and glass transitions in dynamic nuclear polarization

As previously demonstrated by Thurber and Tycko, the peak position of ⁷⁹Br in potassium bromide (KBr) allows one to determine the temperature of a spinning sample. We propose to adapt the original design by using a compact KBr tablet placed at the bottom of the magic angle spinning rotor, separated from the sample under investigation by a thin disk made of polytetrafluoroethylene (or ‘Teflon’®). This design allows spinning the sample up to at least 16 kHz. The KBr tablet can remain in the rotor when changing the sample under investigation. Calibration in the range of 98 < T < 320 K has been carried out in a static rotor by inserting a platinum thermometer. The accuracy is better than ± 0.9 K, even in the presence of microwave irradiation. Irradiation with 5 W microwaves at 263 GHz leads to a small temperature increase of 3.6 ± 1.4 K in either static or spinning samples. The dynamic nuclear polarization enhancement decreases with increasing temperature, in particular when a frozen glassy sample undergoes a glass transition. Copyright © 2011 John Wiley & Sons, Ltd.     

Advanced sedex ( nsitive etector of othermic processes)

The instrument described is suitable for the investigation of the thermal behaviour of substances and reaction mixtures under production conformable conditions; this is made possible by the sophisticated design of the sample chamber: easy stirring of the samples, measuring under any gas atmosphere and while bubbling gas through the sample, choice of the sample container and visual observation during the measurement. The control device allows the choice of one of three operational modes: constant temperature, linear increase in temperature, and adiabatic control; this permits the application of the SEDEX apparatus for a variety of methods including dynamic scanning, isoperibolic measurements, and (quasi) adiabatic studies.     

机械振动对聚丙烯结晶作用的影响

对热塑性高分子作熔体加工时,在此过程中同时再叠加机械振动,设计制造的加工机器一方面具有卓越的技术经济指标,另一方面制品的物理性能也得到了提高[1,2].此类研究的重点多集中在动态成型过程中聚合物的流变行为或者成型后制品的力学性能方面[3,4],对聚合物本身在此外加交变力     

Sample stacking of fast-moving anions in capillary zone electrophoresis with pH-suppressed electroosmotic flow

On-line sample concentration of fast moving inorganic anions by large volume sample stacking (LVSS) and field enhanced sample injection (FESI) with a water plug under acidic conditions is presented. Detection sensitivity enhancements were around 100 and 1000-fold for LVSS and FESI, respectively. However, reproducibility and linearity of response in the LVSS approach is superior compared to the FESI approach.     

Advanced sedex (sensitive detector of exothermic processes)

The instrument described is suitable for the investigation of the thermal behaviour of substances and reaction mixtures under production conformable conditions; this is made possible by the sophisticated design of the sample chamber: easy stirring of the samples, measuring under any gas atmosphere and while bubbling gas through the sample, choice of the sample container and visual observation during the measurement. The control device allows the choice of one of three operational modes: constant temperature, linear increase in temperature, and adiabatic control; this permits the application of the SEDEX apparatus for a variety of methods including dynamic scanning, isoperibolic measurements, and (quasi) adiabatic studies.     

LiFePO4的制备、结构与电性能研究

应用高速球磨-高温固相反应法于不同煅烧温度(400~700℃)下合成L iFePO4锂离子电池正极材料,X-射线衍射、扫描电镜和恒电流充放电等测试表明,煅烧温度对合成的L iFePO4晶体结构、表观形貌以及电化学性能均有很大影响;经600℃煅烧得到的L iFePO4样品具有良好的充放电性能,以0.1C倍率充放电,首次放电比容量为128.8 mAh/g,第15次放电比容量为129.1 mAh/g,充放电效率在99.7%以上;其高温充放电性能亦佳.     

核级碳化硼试样分解方法的研究

在对核级碳化硼试样的多种分解方法进行简要介绍和分析之后,提出了以碳酸钙作熔剂在高温下分解试样,以盐酸浸取的方法,此方法应用于核级碳化硼中总硼、铁、铝等的测定获得了满意的结果。     

Volume-load capacity in fast-gradient liquid chromatography effect of sample solvent composition and injection volume on chromatographic performance

We studied the effects of sample solvent composition and injection volumes on the chromatographic performance of ODS-bonded silica columns under fast-gradient running conditions. Chromatographic performance is compromised as a function of both sample injection volume and sample solvent strength, with earlier-eluting analytes being much more affected than later-eluting ones. In general, when injecting samples dissolved in a strong solvent, performance was improved by diluting the strong injection solvent and injecting a proportionally larger volume. Volume loading capacity can be increased by using a longer column, or by using a column of equivalent length, but with a larger inner diameter. Data also suggest that sample solvent strength, not viscosity, is responsible for the noted effects.     

Factors Affecting the Stability of Cellulose Peroxides

Factors affecting the stability of three kinds of cellulose peroxides prepared by reactions of aldehyde cellulose, carboxy-methyl cellulose, and unmodified cellulose with hydrogen peroxide, Peroxides A, B, and C, respectively, were investigated. The relative stability of the peroxides was in the order Peroxide A > B > C, which was greatly improved by applying ethylenediaminetetraacetic acid as the chelating reagent for the metals in a very small amount in the sample. The sample kept under nitrogen retained stable activity of the peroxide longer than that under air atmosphere. Water in the sample seemed to participate in the decomposition of the peroxide to some extent. The functions of metals, water, and atmosphere on the decomposition of peroxide are discussed.     

Investigation of corrosion processes on cleavage edges of potash-lime-silica glasses by atomic force microscopy

Corrosion phenomena on surfaces of potash-lime-silica glass with medieval composition have been imaged in-situ using AFM in combination with a home built sample holder and a commercial liquid cell. Measurements under ambient atmosphere lead to pit corrosion. Sample preparation and measurement performed under liquids such as isobutanol inhibit the corrosion process. Addition of water (10 vol%) induces the formation of a leached layer, where the network modifiers such as K and Ca are exchanged by hydrogen-bearing species. During the measurements interactions of the tip with the sample surface have been observed.     

高压微波消解-电感耦合等离子体原子发射光谱同时测定进口奶粉中Fe、Zn、Ca、Mg、Cu含量

通过优化试验确定仪器的最佳工作参数,硝酸-过氧化氢微波消解样品,采用电感耦合等离子体原子发射光谱同时测定进口奶粉中的Fe、Zn、Ca、Mg、Cu多种金属元素含量．试验过程方便快捷,多种元素同时测定节约测定时间．方法的准确度、精密度均符合日常检验的需要．     

An experimental method for studying nonisothermal crystallization of polymers at very high cooling rates

A new technique based on light depolarizing microscopy was developed for studying non-isothermal crystallization of polymers at average cooling rates up to about 5000°C/min. The polymer is cooled down by a gaseous cooling medium supplied at a constant temperature. The temperature of polymer is measured by a thermocouple imbedded directly in the sample. A heat transfer analysis was used to establish appropriate sample geometry to assure that, under the applied cooling condition, the temperature distribution along the sample thickness can be neglected. A light-scattering effect, which occurs when crystallization is carried out under high cooling rates, was observed. This required the development of a method to correct the depolarized light intensity for the effect of light scattering. An appropriate correction method was developed based on both a theoretical and an experimental analysis of the light intensity measurement. This provided a means to measure the overall crystallization kinetics. Examples of such measurements for iPP, HDPE, and LDPE are presented. In addition to the overall crystallization kinetics, the developed technique includes a video camera and VCR system used for measurements of spherulite growth rates during crystallization under high cooling rates. Constant spherulite growth rates were observed for isotactic polypropylene crystallized under very non-isothermal conditions. © 1996 John Wiley & Sons, Inc.     

新型氧离子导体La2Mo1.9Al0.1O9-α陶瓷的合成及电性能

通过高温固相法合成了La2Mo1.9Al0.1O9-α陶瓷样品. XRD测试结果表明, 该样品为一立方相结构, Al3＋离子在 Mo6＋位置的固溶摩尔浓度为5%时能完全抑制La2Mo2O9的相变. 采用交流阻抗谱、氧浓差电池、氧泵等电化学方法系统地研究了该陶瓷样品在600～1000 ℃下的离子导电特性. 结果表明, 氧浓差电池电动势的实测值与理论值吻合得很好, 离子迁移数为1, 表明该陶瓷样品在该温度下氧气气氛中为一纯离子导体; 氧浓差电池放电及氧的电化学透过(氧泵)实验结果进一步证实了该样品在氧气气氛中为一纯氧离子导体; 1000 ℃时其氧离子电导率达到了0.12 S&#8226;cm－1, 明显高于相同条件下母体及La2Mo1.9Ga0.1O9-α的氧离子电导率.