A study of the precision and accuracy of peak quantification in comprehensive two-dimensional liquid chromatography in time

Simulated chromatographic data were used to determine the precision and accuracy in the estimation of peak volumes (i.e., peak sizes) in comprehensive two-dimensional liquid chromatography in time (LC × LC). Peak volumes were determined both by summing the areas in the second dimension chromatograms and by fitting the second dimension areas to a Gaussian peak. The Gaussian method is better at predicting the peak volume than the moments method provided there are at least three second dimension injections above the limit of detection (LOD). However, when only two of the second dimension signals are substantially above baseline, the accuracy and precision of the Gaussian fit method become quite poor because the results from the fitting algorithm become indeterminate. Based on simulations in which the modulation ratio (M_R = 4¹σ/t_s) and sampling phase (?) were varied, we conclude for well-resolved peaks that the optimum precision in peak volumes in 2D separations will be obtained when the M_R is between two and five, such that there are typically four to ten second dimension peaks recorded over the eight σ width of the first dimension peak. This sampling rate is similar to that suggested by the Murphy–Schure–Foley criterion. This provides an RSD of approximately 2% for the signal-to-noise ratio used in the present simulations. The precision of the peak volume of experimental data was also assessed, and RSD values were in the range of 4–5%. We conclude that the poorer precision found in the LC × LC experimental data as compared to LC may be due to experimental imprecision in sampling the effluent from the first dimension column.     

Evaluation of 1.0 mm i.d. column performances on ultra high pressure liquid chromatography instrumentation

The present study focuses on the evaluation of 1.0 mm i.d. (internal diameter) columns on a commercial Ultra-High Pressure system. These systems have been developed specifically to operate columns with small volumes, typically 2.1 mm i.d., by reducing extra-column volume dispersion. The use of columns with smaller i.d. results in a reduced solvent consumption and required sample volume. The evaluation of the columns was carried out with samples containing neutral and pharmaceutical compounds. In isocratic mode, the extra-column volume produced additional band broadening leading to poor performances compared to equivalent 2.1 mm i.d. columns. By increasing the length of the column, the influence of the extra-column bandspreading could be reduced and 75,000 plates were obtained when four columns were coupled. In gradient mode, the effect of the extra-column contribution on efficiency was limited and about 80% of the performance of the 2.1 mm i.d. columns was obtained. Optimum conditions in gradient mode were further investigated by changing flow rate, gradient time and column length. A different approach of the calculation of peak capacity was also considered for the comparison of the influence of these different parameters.     

基于二极管阵列检测器的色谱峰纯度的快速直观鉴定

基于二极管阵列检测器（DAD）得到的色谱-光谱图,通过去噪、归一化、计算欧氏距离,聚类分析等方法,建立了一种快速直观的评价色谱峰纯度的有效方法：可直观的判断色谱峰的纯度,并判断存在干扰峰的位置,为色谱工作者评价色谱峰,进行下一步工作提供了依据。     

Collisional broadening and shifting of the 211-202 transition of H2O, H2O, H2O by atmosphere gases

Broadening and shifting of the 2₁₁-2₀₂ transition of H₂¹⁶O, H₂¹⁷O, H₂¹⁸O by pressure of water, nitrogen and oxygen were precisely measured at room temperature using spectrometer with radio-acoustic detection of absorption. Shift parameters for all studied lines as well as broadening parameters of H₂¹⁷O, H₂¹⁸O lines were measured for the first time. Comparison of obtained results with previously known experimental and theoretical data is presented.     

Measurements of self-broadening and self-pressure-induced shift parameters of the methane spectral lines in the 5556-6166 cm range

The absorption spectra of methane at different path lengths and different pressures for three temperatures 180, 240 and 296 K have been recorded in the 5556-6166 cm⁻¹ region using the Bruker IFS 120 HR and 125 HR high-resolution Fourier transform spectrometers. The multispectrum fitting procedure has been applied to these spectra to recover the spectral line parameters. The main goal of this procedure was the determination of self-broadening and self-pressure-induced shift coefficients and the exponents of their temperature dependences. These parameters have been derived for 406 assigned lines with good values of the signal to noise ratio. The rotational dependence of these parameters is discussed.     

纳米Fe3 O4 颗粒的正电子湮没谱学研究

测量了磁性纳米Fe₃O₄颗粒的X射线衍射谱(XRD)、正电子湮没寿命谱(PALS)和符合多普勒展宽谱(CDBS),研究了不同压力和退火温度对磁性纳米Fe₃O₄颗粒物相、电子结构、缺陷及电子动量分布等的影响. XRD,PALS,CDBS测量结果表明:纳米Fe₃O₄颗粒的缺陷浓度随压力的增加而增大,但物相和缺陷类型并未发生变化;磁性纳米Fe₃O_{4< 关键词： 正电子 3}O₄')" href="#">Fe₃O₄ 寿命谱 多普勒展宽谱     

高密度平面靶等离子体中激光驱动冲击波加速离子的能谱展宽

本文对超短超强激光脉冲辐照高密度等离子体产生的静电冲击波加速离子的能谱展宽机理进行了数值研究.着重讨论了三种冲击波加速离子的能谱展宽机理:能量沉积到离子中使得冲击波前沿不断减速,被加速离子与背景粒子的碰撞,以及高能离子到达靶背面时受到鞘层场进一步加速.还研究了驱动激光脉冲宽度对冲击波加速离子能谱宽度的影响. 关键词： 激光等离子体 冲击波加速 能谱展宽     

掺Er光纤飞秒激光器载波包络位相偏移的探测

本文介绍了基于掺Er光纤飞秒激光器光学频率梳中光学部分的研制. 实验上采用重复频率为230 MHz的掺Er光纤飞秒激光器,通过放大、光谱展宽以及单臂f—2f系统,在优化及分析相关参数影响的基础上,获得了~30 dB信噪比f₀的输出,为光纤光学频率梳的建立奠定了基础. 关键词： 掺Er光纤激光器 光学频率计量 光纤光学频率梳 光谱展宽     

Nondestructive evaluation for remanent life of modified 9Cr-1Mo steel by reversible magnetic permeability

We present a magnetic and nondestructive method to evaluate the remanent life of modified 9Cr-1Mo steel by measuring the reversible magnetic permeability. Specimens with ten different kinds of aging periods were prepared using an isothermal heat treatment at 690 °C. The Larson-Miller parameter (LMP) was calculated and the peak interval of reversible magnetic permeability (PIRMP) was measured using the surface type probe. PIRMP was inversely proportional to LMP. We can evaluate the remanent life of modified 9Cr-1Mo steel using the relationship between PIRMP and LMP. Also, we present the possibility that the tensile strength and yield strength measured by destructive methods could be estimated by PIRMP measured nondestructively.