无富集进样原子荧光光谱法测定地表水中的痕量汞

通过增大样品进样量的方式,样品进样量是标准进样量的10-100倍,降低了汞的检出限,从而达到了无富集直接进样测定地表水中痕量汞.其检出限为0.008μg/L;浓度为0.05μg/L和0.10μg/L左右的有证标准物质测定均值分别为0.0483μg/L和0.1016μg/L,加标回收率为92.3％和95.2％.灵敏度高,精密度好,能达到准确定量Ⅰ类和Ⅱ类地表水汞(0.05μg/L以下)的要求.对汉江湖北段水样进行测定,在较洁净的地表水分析中,氧化还原处理后与酸化水样测定结果差异不大,处理后水样结果略微增大.建议对较洁净的地表水样品将氧化还原预处理步骤省略掉,直接进样.     

Test for dispersion constancy in stochastic differential equation models

In this paper, we propose a constancy test for volatility in It processes based on discretely sampled data. The test statistic constitutes an integration of the Ljung–Box test statistic and the kurtosis statistic in the Jarque–Bera test. It is shown that under regularity conditions, the proposed test asymptotically follows a chi‐square distribution under the null hypothesis of constant volatility. To evaluate the test, empirical sizes and powers were examined through a simulation study. Analysis of real data including ultra‐high frequency transaction data and interest rates was also conducted for illustration. Copyright © 2011 John Wiley & Sons, Ltd.     

Solution of a General Linear Complementarity Problem Using Smooth Optimization and Its Application to Bilinear Programming and LCP

This paper addresses a General Linear Complementarity Problem (GLCP) that has found applications in global optimization. It is shown that a solution of the GLCP can be computed by finding a stationary point of a differentiable function over a set defined by simple bounds on the variables. The application of this result to the solution of bilinear programs and LCPs is discussed. Some computational evidence of its usefulness is included in the last part of the paper. Accepted 28 June 1999. Online publication 4 December 2000.     

Failure of normality in the box product of uncountably many real lines

We prove in ZFC that the box product of many copies of is neither normal nor collectionwise Hausdorff. As an addendum to the proof, we show that if the cardinality of the continuum is , then these properties also fail in the closed subspace consisting of all functions which assume the value on all but countably many indices.

     

Ground state sigmatropic and electrocyclic rearrangements in some monoterpenes: The pyrolysis of α-pinene

Alloocimene 7, obtained via ocimene 6 by heating α-pinene 2, was further pyrolysed to a complex mixture of products derived primarily from antarafacial 1,7- and suprafacial 1,5-hydrogen migrations, and 6-eleetron disrotatory electrocyclizations.     

Vibrational,NQR and thermogravimetric study of complexes between triphenyl group VB compounds and mercuric halides

The synthesis, identification, vibrational (IR—FIR), NQR and thermal (TGA) study of a series of donor-acceptor complexes (Ph₃E^VB)_n(HgX₂)_m (E^VB = As, Sb, Bi;Ph = phenyl; X = Cl, Br, I; n/m = 2/2, 2/1) is reported. Elemental analysis proved that the aimed stoichiometry is only obtained for the (Ph₃Sb)_n(HgI₂)_m and (Ph₃As)_n(HgX₂)_m complexes, (Ph₃As)₂(HgI₂)₂ excepted. In all other cases a much lower Ph₃E^VB content is found. Assignments for the skeletal vibrational frequencies are based upon a “tetrahedral” C_2v and a “bridge-like” C_2h symmetry for (Ph₃E^VB)₂HgX₂ and (Ph₃E^VB)₂(HgX₂)₂ complexes, respectively. Changes in the electron distribution of the Hg—X bond dominate the halogen NQR frequency. TG curves are characterized by a single step mass loss and the absence of any residue suggests volatilization rather than decomposition.     

Influence of structure and polarity of polysiloxanes on retention of N-TFA butyl esters of amino acids

In this work, we have investigated the influence of the polarities and structures of 13 polysiloxanes on the retention of some N-TFA N-butyl esters of amino acids. Gehrke [1] was the first to examine the possible relationship between polarity and retention data of amino acid derivatives for 9 stationary liquid phases. He concluded that the molecular structure of the stationary liquid phase is an important factor determining retention.     

A study of adsorption characteristics of traces of chromium(III) and (VI) on selected surfaces

The adsorption losses of chromium(III) or (VI) on the walls of Pyrex, flint glass and polyethylene beakers have been investigated. Chromium(III) or (VI) solutions were stored in beakers at different hydrogen ion concentrations, and losses due to adsorption were measured at various contact times by counting the γ-ray activity from chromium-51 radiotracer. At pH 6.95, chromium(III) solutions showed the greatest instability, particularly in polyethylene beakers, where losses up to 25% were observed at the end of the 15-day contact period. Chromium(VI) showed a completely different pattern; losses less than 1% were observed at the end of 15 days on all the three types of containers.     

Characterization of noise in inductively-coupled plasma emission spectrometry

The nebulizing process in inductively-coupled plasma emission spectrometry is a major source of the instrumental variability; an attempt has been made to isolate this source so that its influence on the final result could be evaluated. Direct measurements of the time-dependent variations of the sample supply to the plasma were achieved by using a device based on the light-scattering property of nebulized test solutions. The noise from the nebulizer and of the emission signal was characterized by autocovariance functions and power spectral densities. The types of noise observed showed f^{-$\text{1}\text{2}$} and f^{-$\text{1}\text{4}$} character, depending on the concentration of the test elements employed. Cross-covariance revealed a strong correlation between the noise sources considered. The applicability and limitations of possible correction and electronic filtering procedures are indicated.