A simple,rapid and sensitive method based on modified multiwalled carbon nanotube for preconcentration and determination of lead ions in aqueous media in natural pHs

In this study, multiwalled carbon nanotube (MWCNT) was modified by the pyridine group using a silane agent and characterized by infrared spectroscopy (IR), thermal analysis (TG/DTA), and elemental analysis (CHN) and scanning electron microscopy (SEM). The application of this sorbent was investigated in determination of lead ions in aqueous samples, using flame atomic absorption spectrometry (FAAS). Through this study, different parameters such as pH and sample flow rate on adsorption process and eluent concentration, volume and flow rate were optimized. The limit of detection (LOD), the relative standard deviation and the recovery of the method were 2 ng mL^?1, 1.3% and 99.7%, respectively. Two standard reference materials (NIST 1571 and NIST 1572) were used to verify accuracy of this method. Finally, the sorbent was successfully applied for extraction and determination of low levels of Pb(II) ions in aqueous samples.     

Choquet-type Integral Representation of Invariant Functions for some Product Semigroups

We show that functions which are invariant for suitable product semigroups (one of which is a quasi-Poisson semigroup on a general state space) decompose into a singular eigen-function and a mixture of products of minimal eigen-functions.     

燃煤烟气中As、Se、Pb的形态分布及S、Cl元素对其形态分布的影响

基于化学热力学平衡分析方法，计算分析了燃煤烟气中重金属As、Se、Pb的形态分布规律，研究了S、Cl等元素对As、Se、Pb的形态分布规律的影响。结果表明，氧化性气氛下，As以As₂O₅、As₄O₆、AsO等氧化物的形式存在；Se主要以SeO₂形式存在；Pb在1000 K以下主要是固态PbSO₄，1200 K以上为气态PbO。还原性气氛下，As在较低温度时为固态As₂S₂，900-1400 K以As₂、AsS、AsN气体共存，2000 K以上全部转化为气态AsO。Se在1100 K以下主要以气态H₂Se存在，1100 K开始生成SeS和Se₂气体，1800 K时主要是气态Se和少量气态SeO；Pb在中低温时主要是PbS，1800 K以上气态Pb为主要存在形态。S在还原性气氛下增大了AsS（g）、PbS（g）、SeS（g）的比例，氧化性气氛下对As、Se、Pb形态分布基本无影响；Cl无论在氧化还是还原气氛下对As、Se影响均较小，但对Pb的形态分布影响较大。     

火焰原子吸收光谱法测定磁化杯中铅、镉和铁

本文研究了火焰原子吸收光谱法测定磁化杯陶瓷内胆中Ｐｈ、Ｃｄ和Ｆｅ含量的方法。样品经粉碎，用硝酸－高氯酸混合液进行消解后测定。本法灵敏度高，干扰少，简单，快速，具有良好的精密度和准确度，其相对标准偏差分别为Ｐｂ３．９９％，Ｃｄ１０．７％，Ｆｅ０．９％。回收率Ｐｂ１００．６１％，Ｃｄ１０１．１８％，Ｆｅ１０２．４％。     

Modification of a three-way catalyst washcoat by aging: A study along the longitudinal axis

This work reports the research carried out by studying aliquots extracted at different axial coordinates from Three Way Catalyst (TWC) monoliths aged under real traffic conditions. Our study focused on the catalytic properties and on several chemical and physical effects caused in the Front and Rear monolith washcoat surfaces by vehicle aging after 60,000 km. Regarding the catalytic properties, all the used aliquots showed poorer activity than their corresponding fresh counterparts. The strongest deactivation was detected for NO and hydrocarbon conversion. CO conversion was less affected and the Rear monolith was as deactivated as the Front one. The characterisation techniques (TXRF, N₂ adsorption-desorption isotherms, XRD and H₂-TPR) detected - (i) the deposition of P, Zn and Pb; (ii) the formation of CePO₄ on account of the Ce from the washcoat; (iii) thermal sintering; (iv) inhibition of the reducibility of Ce oxides - as the main effects brought about by vehicle aging conditions. The deactivation observed at the beginning of the Front monolith was the result of a combination of the former effects. When moving downstream to higher axial coordinates, Pb accumulation and the loss of specific area appeared to be the only probable sources of deactivation.     

WS2 超细粉体的固相法合成

WS2 超细粉体的固相法合成;WS2;固相反应;过硫系数;高能球磨;粒度     

Accuracy and long-term reproducibility of lead isotopic measurements by multiple-collector inductively coupled plasma mass spectrometry using an external method for correction of mass discrimination

The precision of isotopic measurements of Pb by thermal ionization mass spectrometry (TIMS) is limited by the fact that this element does not possess an invariant isotope ratio that can be used for the correction of mass fractionation by internal normalization. Multiple-collector inductively coupled plasma mass spectrometry (MC-ICPMS) can overcome this limitation, because with plasma ionization, elements with overlapping mass ranges are thought to display identical mass discrimination. With respect to Pb, this can be exploited by the addition of Tl to the sample solutions; the mass discrimination factor obtained for Tl can then be used for the correction of the measured Pb isotope ratios. In this article we present the results of a detailed study that investigates the accuracy and precision of such an external correction technique for mass discrimination based upon the results of multiple analyses of a mixed standard solution of NIST SRM-981 Pb and SRM-997 Tl. Our data indicate that normalization of the Pb isotope ratios to the certified isotopic composition of SRM-997 Tl produces Pb isotopic results that are significantly lower than recently published reference values by TIMS. This systematic offset can be eliminated by renormalization of the Pb data to a different Tl isotopic composition to obtain an empirically determined mass discrimination factor for Pb that generates accurate results. It is furthermore shown that a linear law is least suited for the correction of mass discrimination, whereas a power or exponential law function provide significantly more accurate and precise results. In detail, it appears that a power law may provide the most appropriate correction procedure, because the corrected Pb isotope ratios display less residual correlations with mass discrimination compared to the exponentially corrected data. Using an exponential or power law correction our results, obtained over a period of over seven months, display a precision (2σ) of better than 60 parts per million (ppm) for ²⁰⁸Pb/²⁰⁶Pb and ²⁰⁷Pb/²⁰⁶Pb and of better than 350 ppm for ²⁰⁶Pb/²⁰⁴Pb, ²⁰⁷Pb/²⁰⁴Pb/²⁰⁴Pb, and ²⁰⁸Pb/²⁰⁴Pb. This represents a significant improvement compared to conventional TIMS techniques and demonstrates the potential of MC-ICPMS for routine, high-precision measurements of Pb isotopic compositions.     

真珠钙驱铅实验研究

研究了真珠钙驱铅效果，给亚急性中毒的大鼠服用后，可增加铅从尿中排量，降低骨中蓄积量，对防治铅中毒有一定作用。     

ICP-AES法测定锌阳极中的铝、镉、铁、铜、铅

通过分析高频功率、雾化压力、辅助气流量和泵速等试验条件，建立了ICP-AES法测定锌阳极中铝、镉、铁、铜、铅的方法。用该方法测定锌阳极中的铝、镉、铁、铜、铅，其RSD分别为0.17%、0.63%、2.7%、5.2%、2.5%，回收率分别为99.3%-101.2%，99.3%-100.3%、97.1%-102.2%、97.8%-102.9%。对锌阳极试样进行测定，该方法的测定结果与GB4951-85方法的测定结果基本一致。     

Determination of trace elements in biological materials using tetramethylammonium hydroxide for sample preparation

A method to prepare milk powder, bovine liver and bovine muscle samples for analysis by electrothermal atomic absorption spectrometry (ETAAS) is proposed. Samples are mixed with a small amount of tetramethylammonium hydroxide (TMAH) and a stable and homogeneous slurry is produced in ca. 2 h with heating at 60–70 °C. After such sample preparation and dilution with water, trace elements are determined in certified reference materials. Pyrolysis and atomisation temperatures are optimised for each element, and several modifiers are investigated. External calibration is used for every analyte. Limits of detection (LODs), precision and accuracy are reported for Cd, Pb, Ni, Cr, Cu and Ag and compared with those obtained after conventional acid digestion. The main advantages of the proposed method are the simplicity of sample preparation and the longer lifetime of the graphite tube.