目的建立在线监测注射用头孢唑林钠干燥过程中的水分含量测定方法。方法水分定量模型建模样品采以不同批次、不同干燥时间段五水头孢唑林钠原料为研究对象,结合干燥、引湿实验扩充样品水分范围,用积分球测定近红外漫反射光谱,并采用聚...目的建立在线监测注射用头孢唑林钠干燥过程中的水分含量测定方法。方法水分定量模型建模样品采以不同批次、不同干燥时间段五水头孢唑林钠原料为研究对象,结合干燥、引湿实验扩充样品水分范围,用积分球测定近红外漫反射光谱,并采用聚类分析挑选出建模光谱,光谱预处理方法为一阶导数+MSC法,谱段为7502~6499.2、5500.2~3 999.8 cm^(-1),回归方法偏最小二乘法。结果水分定量模型建模样品共计85个,水分含量质量分数为12.15%~16.41%,相关系数(coefficient of determination,R^2)为96.30,交叉验证均方差(root mean square error of cross validation,RMSECV)为0.181。外部验证样品52个,水分含量质量分数为13.28%~16.17%,外部验证均方差(root mean square error of predication,RMSEP)为0.149。模型专属性强,准确度、线性和精密度符合要求。结论建立的运用近红外监测注射用头孢唑林钠干燥过程的水分含量方法是可行的,为实现近红外在线干燥提供了实验基础。展开更多
目的建立微型近红外光谱仪测定硫酸羟氯喹颗粒水分含量的定量分析模型。方法真空干燥和加湿实验改变硫酸羟氯喹颗粒的含水量范围,采用标准正则变换(standard normal variate transformation,SNV)、二阶导数(second derivative,2nd Deriv...目的建立微型近红外光谱仪测定硫酸羟氯喹颗粒水分含量的定量分析模型。方法真空干燥和加湿实验改变硫酸羟氯喹颗粒的含水量范围,采用标准正则变换(standard normal variate transformation,SNV)、二阶导数(second derivative,2nd Derivative)和Karl Norris平滑的光谱预处理方法,选择617~1 068 nm波段,运用偏最小二乘回归(partial least squares,PLS)建立近红外定量分析模型。结果所建模型的校正误差均方根(root mean square error of calibration,RMSEC)为0.178,相关系数Rc为0.991 6,预测误差均方根(root mean square error of prediction,RMSEP)为0.197,相关系数Rp为0.989 6,验证集标准偏差与预测标准偏差的比值(ratio of standard deviation of the validation set to error of prediction,RPD)为6.95,方法学验证中准确度和重复性符合要求。结论微型近红外光谱仪应用于测定硫酸羟氯喹颗粒的含水量是可行的,为微型近红外光谱仪应用于药物的在线干燥过程提供了实验基础。展开更多
We present epi-diffraction phase microscopy(epi-DPM)as a non-destructive optical method for monitoring semiconductor fabrication processes in real time and with nanometer level sensitivity.The method uses a compact M...We present epi-diffraction phase microscopy(epi-DPM)as a non-destructive optical method for monitoring semiconductor fabrication processes in real time and with nanometer level sensitivity.The method uses a compact Mach–Zehnder interferometer to recover quantitative amplitude and phase maps of the field reflected by the sample.The low temporal noise of 0.6 nm per pixel at 8.93 frames per second enabled us to collect a three-dimensional movie showing the dynamics of wet etching and thereby accurately quantify non-uniformities in the etch rate both across the sample and over time.By displaying a gray-scale digital image on the sample with a computer projector,we performed photochemical etching to define arrays of microlenses while simultaneously monitoring their etch profiles with epi-DPM.展开更多
The carbon isotopic composition of CO_(2)inclusions trapped in minerals reflects the origin and evolution of CO_(2)-bearing fluids and melts,and records the multiple-stages carbon geodynamic cycle,as CO_(2)took part i...The carbon isotopic composition of CO_(2)inclusions trapped in minerals reflects the origin and evolution of CO_(2)-bearing fluids and melts,and records the multiple-stages carbon geodynamic cycle,as CO_(2)took part in various geological processes widely.However,the practical method for determination isotope composition of individual CO_(2)inclusion is still lacking.Developing a microanalytical technique with spatial resolution in micrometers to precisely determinate theδ^(13)C value of individual CO_(2)inclusion,will make it possible to analyze a tiny portion of a zoning mineral crystal,distinguish the differences in micro-scale,and possible to find many useful information that could not be obtained with the bulk extraction and analysis techniques.In this study,we systematically collected Raman spectra of CO_(2)standards with different d13C values(34.9‰to 3.58‰)at 32.0℃and from 7.0 MPa to 120.0 MPa,and developed a new procedure to precisely determinate theδ^(13)C value of individual CO_(2)inclusion.We investigated the relationship among the Raman peak intensity ratio,d13C value,and CO_(2)density,and established a calibration model with high accuracy(0.5‰1.5‰),sufficient for geological application to distinguish different source of CO_(2)with varyingδ^(13)CO_(2).As a demonstration,we measured theδ^(13)C values and the density of CO_(2)inclusions in the growth zones of alkali basalt-hosted corundum megacrysts from Changle,Shandong Province.We found the significant differences of density and d13C between the CO_(2)inclusions in the core of corundum and those inclusions in the outer growth zones,the d13C value decreases from core to rim with decreasing density:δ^(13)C values are from7.5‰to9.2‰for the inclusions in the core,indicating the corundum core was crystallized from mantle-derived magmas;from13.5‰to18.5‰for CO_(2)inclusions in zone 1 and from16.5‰to–22.0‰for inclusions in zone 2,indicating the outer zones of corundum grew in a lowδ^(13)C value environment,resulted from an infilli展开更多
文摘目的建立在线监测注射用头孢唑林钠干燥过程中的水分含量测定方法。方法水分定量模型建模样品采以不同批次、不同干燥时间段五水头孢唑林钠原料为研究对象,结合干燥、引湿实验扩充样品水分范围,用积分球测定近红外漫反射光谱,并采用聚类分析挑选出建模光谱,光谱预处理方法为一阶导数+MSC法,谱段为7502~6499.2、5500.2~3 999.8 cm^(-1),回归方法偏最小二乘法。结果水分定量模型建模样品共计85个,水分含量质量分数为12.15%~16.41%,相关系数(coefficient of determination,R^2)为96.30,交叉验证均方差(root mean square error of cross validation,RMSECV)为0.181。外部验证样品52个,水分含量质量分数为13.28%~16.17%,外部验证均方差(root mean square error of predication,RMSEP)为0.149。模型专属性强,准确度、线性和精密度符合要求。结论建立的运用近红外监测注射用头孢唑林钠干燥过程的水分含量方法是可行的,为实现近红外在线干燥提供了实验基础。
文摘目的建立微型近红外光谱仪测定硫酸羟氯喹颗粒水分含量的定量分析模型。方法真空干燥和加湿实验改变硫酸羟氯喹颗粒的含水量范围,采用标准正则变换(standard normal variate transformation,SNV)、二阶导数(second derivative,2nd Derivative)和Karl Norris平滑的光谱预处理方法,选择617~1 068 nm波段,运用偏最小二乘回归(partial least squares,PLS)建立近红外定量分析模型。结果所建模型的校正误差均方根(root mean square error of calibration,RMSEC)为0.178,相关系数Rc为0.991 6,预测误差均方根(root mean square error of prediction,RMSEP)为0.197,相关系数Rp为0.989 6,验证集标准偏差与预测标准偏差的比值(ratio of standard deviation of the validation set to error of prediction,RPD)为6.95,方法学验证中准确度和重复性符合要求。结论微型近红外光谱仪应用于测定硫酸羟氯喹颗粒的含水量是可行的,为微型近红外光谱仪应用于药物的在线干燥过程提供了实验基础。
基金The authors thank Hoa Pham for assistance with the power spectral density calculations and Brian Cunningham,Xiuling Li,Logan Liu and Daniel Wasserman for helpful discussions. This work is supported by NSF CBET-1040462 MRI award.
文摘We present epi-diffraction phase microscopy(epi-DPM)as a non-destructive optical method for monitoring semiconductor fabrication processes in real time and with nanometer level sensitivity.The method uses a compact Mach–Zehnder interferometer to recover quantitative amplitude and phase maps of the field reflected by the sample.The low temporal noise of 0.6 nm per pixel at 8.93 frames per second enabled us to collect a three-dimensional movie showing the dynamics of wet etching and thereby accurately quantify non-uniformities in the etch rate both across the sample and over time.By displaying a gray-scale digital image on the sample with a computer projector,we performed photochemical etching to define arrays of microlenses while simultaneously monitoring their etch profiles with epi-DPM.
基金supported by National Nature Science Foundation of China(92058208)the National Key Research and Development Program of China(2018YFC0310006-04).
文摘The carbon isotopic composition of CO_(2)inclusions trapped in minerals reflects the origin and evolution of CO_(2)-bearing fluids and melts,and records the multiple-stages carbon geodynamic cycle,as CO_(2)took part in various geological processes widely.However,the practical method for determination isotope composition of individual CO_(2)inclusion is still lacking.Developing a microanalytical technique with spatial resolution in micrometers to precisely determinate theδ^(13)C value of individual CO_(2)inclusion,will make it possible to analyze a tiny portion of a zoning mineral crystal,distinguish the differences in micro-scale,and possible to find many useful information that could not be obtained with the bulk extraction and analysis techniques.In this study,we systematically collected Raman spectra of CO_(2)standards with different d13C values(34.9‰to 3.58‰)at 32.0℃and from 7.0 MPa to 120.0 MPa,and developed a new procedure to precisely determinate theδ^(13)C value of individual CO_(2)inclusion.We investigated the relationship among the Raman peak intensity ratio,d13C value,and CO_(2)density,and established a calibration model with high accuracy(0.5‰1.5‰),sufficient for geological application to distinguish different source of CO_(2)with varyingδ^(13)CO_(2).As a demonstration,we measured theδ^(13)C values and the density of CO_(2)inclusions in the growth zones of alkali basalt-hosted corundum megacrysts from Changle,Shandong Province.We found the significant differences of density and d13C between the CO_(2)inclusions in the core of corundum and those inclusions in the outer growth zones,the d13C value decreases from core to rim with decreasing density:δ^(13)C values are from7.5‰to9.2‰for the inclusions in the core,indicating the corundum core was crystallized from mantle-derived magmas;from13.5‰to18.5‰for CO_(2)inclusions in zone 1 and from16.5‰to–22.0‰for inclusions in zone 2,indicating the outer zones of corundum grew in a lowδ^(13)C value environment,resulted from an infilli
