激光烧蚀固体进样法测定出口铝锭中硅、铁、镓、铜和镁

用激光烧蚀固体进样法测定出口铝锭中硅、铁、镓、铜和镁,与国标方法相比较,无需样品前处理,直接测定,提高了工作效率。经对实际样品进行测定,结果与国标方法相一致。测量结果的相对标准偏差小于8.5%。     

巯基棉富集-DMA-80测汞仪测定环境空气中的汞

使用DMA-80测汞仪对空气中汞进行测定,无需前处理,直接进样,将巯基棉样品进行分析.采用标准土样品ESS-3进行方法的准确度和精密度测定,同时进行了方法检出限和模拟实际样品的测定.结果表明该方法检出限0.006ng,低于实际测定方法检出限的要求（0.1ng）;准确度和精密度均能满足分析质量控制要求.     

以利多卡因为探针共振光散射法测定血清白蛋白的含量

实验发现在十二烷基苯磺酸钠(SDBS)存在下,利多卡因能增强血清白蛋白的共振光散射强度,据此,建立了以利多卡因为探针,利用共振光散射法测定牛血清白蛋白(BSA)和人血清白蛋白(HSA)含量的新方法。考察了反应时间、试剂的加入顺序、pH值、SDBS和利多卡因的浓度以及共存干扰物等因素对共振光强度的影响。在优化的条件下,测定BSA和HSA的线性范围分别为1.0~45.0和0.5~30.0 mg·L-1。该方法用于人血清样品中蛋白含量的分析,获得了较高的精密度和准确度,五次平行测定的相对标准偏差在4.9%~5.7%之间,加标回收率在90%~103%之间。该方法使用常规荧光仪和常用化学试剂即可测定,操作简便、具有较高的灵敏度(检出限为0.14 mg·L-1)。对新鲜的人血清样品可以直接进行分析,无需进行样品前处理。本方法为人血清样品中蛋白含量的测定提供了一个可供选择的新途径。     

石墨炉原子吸收法直接测定奶粉中铅镉含量

本文报道了运用悬浮技术－石墨炉原子吸收法直接测定奶粉中的铅镉含量，并就此进行了一些探讨，实验无需进行消化处理，充分利用石墨炉本身所具有的对样品进行部分预处理的功能，用１ｍｇ／ｍｌ磷酸二氢铵作悬浮剂和基体改进剂，将奶粉样品制成均匀悬浮样液，直接进行测定，灰化温度可提高到８００℃，基体干扰被消除，铅和镉无灰化损失，方法简便，快捷，准确，避免了因样品预处理而带来的干扰和损失，铅的回收率为１００．１％，Ｃ     

X射线荧光光谱法测定增产丙烯助剂中磷和铁的研究

使用X射线荧光光谱仪,采用人工合成标样,设计合成了一套标准样品,采用数学校正法中的经验系数法校正元素间的互相干扰,样品不经任何处理,粉末直接压片,经验系数法校正基体效应,建立了分析测定增产丙烯助剂中磷和铁含量的方法。讨论了样品制作方法,合适的测量条件,探讨了试样中元素间的相互影响。实验结果表明,该方法重现性好,准确度和精密度较高,测定磷和铁的相对标准偏差为：0.34%和0.59%;测定范围磷为0.01%～2.5%,铁为0.01%～2.5%。分析结果与化学法、等离子发射光谱法测定结果吻合。该方法快速、简便,样品处理简单,可以不分解;分析速度远快于其他分析方法,结果准确,单次测量一个样品只需要5 min,适用范围广,满足了科研和工业生产的需要。     

用于ICP-MS多元素分析的致病菌前处理方法

细菌样品所含脂肪、蛋白质以及有机物含量较少,但元素含量低,因此相对于步骤繁复的微波消解前处理,相对简单方便的冷消化法更适合此类样品。本文建立了一种简化的冷消化方法,用于细菌样品中无机元素分析的前处理。此方法采用浓硝酸直接在盛放样品的容器中消化细胞样品,然后直接定量进样。这个方法简化了细胞样品预处理的实验步骤,降低了被测物质损失和污染的可能性。通过与微波消解方法比对试验的结果发现,冷消化与微波消解两种方式处理的元素含量经过统计学分析无显著性差别(p0.05)。同时浓硝酸冷消化样品检测浓度在微波消解样品测定值的±15%以内。加标回收率试验的回收率为91%~109%,精密度为0.4%~7.7%,方法符合检测要求,各项方法学指标均达到理想效果。     

拉曼光纤技术快速无损鉴别甲硝唑片

采用光纤探头直接放在甲硝唑片上进行检测,采集谱图,对拉曼光谱峰进行指认,并改变测定条件(药品隔铝塑包装、刮除包膜)进行测定。建立了光纤传感技术结合拉曼光谱快速无损鉴别甲硝唑片的方法,所测药物图谱峰形良好、峰强明显、指纹性强、测定快速准确,可瞬间获得片剂的特征图谱。样品无需进行前处理,可无损鉴别。药片检测时,是否隔铝塑包装和刮除包膜不影响谱图识别。本法快速、准确、专属性强、灵敏度高,可用于对甲硝唑片进行有效的鉴别。     

直接进样ICP-OES法测定N-甲基吡咯烷酮(NMP)中的12种杂质元素

建立电感耦合等离子体发射光谱(ICP-OES)法测定N-甲基吡咯烷酮(NMP)中12种杂质元素(Mo, Cr, Zn, Pb, Ni, Mn, Fe, Cu, Ca, Al, Na, K)的分析方法。将NMP用硝酸酸化后直接进样分析,无需对样品进行消解,避免了样品前处理时引入误差的风险。通过优化等离子体工作参数,减轻了有机溶剂对等离子体的负载,确保了等离子体的稳定工作,优化后等离子体射频功率为1 350 W,载气流量为0.40 L·min-1。采用轴向观测方式获取样品原子化或离子化过程中的所有信号,降低了方法的检出限,提高了分析灵敏度。通过选择各元素合适分析谱线、采用附加氧气除积碳并结合背景校正技术消除了各类谱线及背景干扰,选用标准加入法校正了基体效应,抵消了高浓度有机基质对易电离元素产生的干扰。结果表明,标准工作曲线的线性相关系数在0.999 5～1.000 0之间,检出限在3.8～106.4 ng·g-1范围内,各元素的回收率在92.0%～108.0%之间,11次测定的相对标准偏差(RSD)≤4.8%。方法操作简单,无需复杂的样品预处理,分析速度快,测定结果准确可靠,精密度高,完全满足大批量实际产品的分析要求。方法可应用于NMP产品中杂质元素的监测。     

基于银溶胶表面增强拉曼光谱对菠菜毒死蜱农药的快速检测

利用表面增强拉曼光谱(SERS)技术,建立了一种用于菠菜中毒死蜱农药残留的非破坏、快速检测方法。以碱性环境下盐酸羟胺还原法制备的银溶胶作为表面增强剂滴涂于菠菜样品表面后,采用实验室自行搭建的拉曼系统直接采集样品的拉曼信息,该方法无需对样品进行前处理,可以实现菠菜中毒死蜱含量的实时在线定量分析。采集24片不同毒死蜱含量的菠菜样品拉曼光谱,每个样品采集20个点。拉曼信号采集后,用气相色谱法对24个菠菜样品中毒死蜱含量进行检测。为了消除光谱噪音以及荧光背景对分析建模的影响,分别采用Savitzky-Golay平滑和有效峰线性拟合法对原始拉曼光谱进行预处理。该表面增强拉曼方法具有较好的重复性,实验中对50个相同毒死蜱含量,但不同状态的菠菜进行光谱采集,其相对标准偏差为13.4%,说明该方法具有一定的普适性。光谱预处理后,选取615.5~626.4 cm-1波段为感兴趣区域,建立0.05~37.4 mg·kg-1浓度范围内毒死蜱含量的多元线性预测模型,结果表明感兴趣区域的拉曼信号和毒死蜱浓度呈良好的线性关系,其校正集和验证集相关系数R_C和R_P分别为0.961和0.954。该方法的最低检出含量为0.05 mg·kg-1,低于国家标准规定的农药残留最大限量。该方法简单快速,无需样品前处理,可以实现果蔬的农药残留快速、定量检测。     

一种用于冶金炉前快速分析的新仪器——激光诱导击穿光谱仪

冶金炼钢要求快速分析冶金炉前样品来及时掌握冶炼过程。文章介绍了自主研制的一种新型的光谱仪——激光诱导击穿光谱仪,该仪器采用ns级脉宽的Nd∶YAG激光器作为样品离子化光源,激光聚焦样品表面激发产生的等离子体光谱依次经帕邢-龙格光学系统进行分光、光电倍增管探测、门控积分器积分、模拟数字转换器转换后获得的最终结果输入计算机进行数据处理。和目前冶金炉前样品分析常用的光谱仪相比,该仪器无需样品预处理,分析速度快(1 min或更少),准确灵敏度高,非常适用于冶金炉前样品的快速分析。近年来随着光纤技术的迅速发展,使用该仪器进行钢液实时在线分析和动态控制冶金工艺必将成为现实。     

Efficient Entrapment of Dye in Hollow Silica Nanoparticles: Direct Evidence Using Fluorescence Spectroscopy

Using hollow silica nanoparticles we demonstrate a simple and highly efficient way of removing hydrophilic dye (Rhodamine B) from water by encapsulation within these hollow spheres. The hollow silica spheres were obtained by using a surfactant templated procedure. Using fluorescence spectroscopy, we also show the evidence of the dye being absorbed within the hollow core of the silica shell (which is crucial for many applications) and differentiate from the adsorption of dye on the surface of the silica shell. It was found that that up to 94 % of the hydrophilic dye could be entrapped using these hollow shells within 72 h of exposure. Fluorescence spectroscopy shows a red shift in the dye encapsulated in the hollow silica which is due to aggregation of the dye and enables us to follow quantitatively the uptake of the dye molecules by the silica shells with time. The evidence for the encapsulation of the dye in these hollow spheres was reinforced by carrying out a comparative study, using solid silica particles.

Direct laser written waveguide-Bragg gratings in bulk fused silica

Optical waveguides that incorporate Bragg gratings have been written in bulk fused silica by using the femtosecond laser direct-write method and without the need for lithography or ion-beam techniques. A single manufacturing process is used to create waveguide-Bragg grating reflectors for operation in the C band.     

Direct laser fabrication of blaze gratings in fused silica

Results of our investigations on direct laser fabrication of blaze gratings in fused silica using a special fluorine-laser mask projection technology allowing to produce plane and smooth reflecting areas and optimum blaze geometry will be presented. In particular, it will be shown that gratings with nearly optimum blaze geometry and relatively low surface roughness of the reflecting areas can be produced. The technique is a one-step method and has a high variability with regard to grating geometry and also substrate materials. We use masks made of tantalum foil, projected onto a fused silica substrate surface with a demagnification ratio of 26:1 and also novel scattering masks made of calcium fluoride. In these masks, up to 25 times smaller transmission apertures can be manufactured allowing thus grating constants in the range of a few μm. The average surface roughness of the reflecting areas along a blaze grating line was measured to be R _a=38 nm without any surface smoothing. The maximum variance of the blaze angle within one grating is about 0.5 degree.     

用紫外光直接在光纤内写入布拉格反射光栅的实验研究

用紫外光直接在光纤内写入布拉格反射光栅的实验研究杜卫冲谭华耀＊刘颂豪华南师范大学，激光生命科学研究所，广州５１０６３１＊香港理工大学，电机系自１９８９年Ｍｅｌｔａｚ［１］首次提出采用两束波长位于掺Ｇｅ－石英光纤吸收带内的相干紫外激光相干涉，从侧面照射...     

光学元件群延迟的直接测量

提出了一种测量群延迟的新方法,利用白光干涉仪产生的光谱干涉,通过时间频率联合分析直接得出群延迟,减小了传统相位差分方法产生的误差,并通过测量结果减去系统背景,进一步提高了光学元件色散测量的准确度. 该方法适合于具有复杂色散光学元件群延迟和色散的准确测量,也适合于慢光器件群速度延迟的测量. 关键词： 色散测量 白光干涉 时间频率分析 超快激光     

Direct joining of glass substrates by 1 kHz femtosecond laser pulses

When a femtosecond laser pulse is focused at the interface of two transparent substrates, localised melting and quenching of the two substrates occur around the focal volume, bridging them due to nonlinear absorption. The substrates can then be joined by resolidification of the materials. We investigate the optimum irradiation conditions needed to join borosilicate glass substrates and fused silica substrates using a 1 kHz 800 nm Ti:sapphire amplifier. We characterised the joint strength and the transmittance through joint volumes as a function of laser energy and translation velocity. We found that a joining strength as large as 14.9 MPa could be obtained in both fused silica and borosilicate glass. Annealing the joint samples led to an increase in the joint strength. PACS 42.65.Jx; 42.70.Ce; 81.20.Vj     

Applied electric field to fabricate colloidal crystals with the photonic band-gap in communication waveband

The macropore silica colloidal crystal templates were assembled orderly in a capillary glass tube by an applied electric field method to control silica deposition. In order to achieve the photonic band gap (PBG) of colloidal crystal in optical communication waveband, the diameter of silica microspheres is selected by Bragg diffraction formula. An experiment was designed to test the bandgap of the silica crystal templates. This paper discusses the formation process and the close-packed fashion of the silica colloidal crystal templates was discussed. The surface morphology of the templates was also analyzed. The results showed that the close-packed fashion of silica array templates was face-centered cubic (FCC) structure. The agreement is very good between the experimental data and the theoretical calculation.     

低压化学气相沉积技术制备锗反蛋白石三维光子晶体

采用溶剂蒸发对流自组装法将单分散SiO2微球组装形成三维有序胶体晶体模板,用低压化学气相沉积法填充高折射率材料锗,酸洗去除SiO2模板,获得了锗反蛋白石三维光子晶体.通过扫描电镜、X射线衍射仪和紫外-可见-近红外光谱仪对锗反蛋白石的形貌、成分、结构和光学性能进行了表征.结果表明：锗在SiO2微球空隙内具有较高的结晶质量,填充致密均匀.通过改变沉积工艺,可控制锗的填充率;制备的锗反蛋白三维光子晶体具有明显的光学反射峰,表现出光学带隙效应.测试的光学性能与理论计算基本吻合.     

Shear-thickening behavior of modified silica nanoparticles in polyethylene glycol

The surface of silica nanoparticles with an average diameter of 650 nm was modified by ball milling and chemical treatment with ethylene glycol (EG). The Fourier-transform infrared spectra and particle size analysis methods were used to characterize the modified silica nanoparticles. The morphologies of the silica nanoparticles before and after the different surface treatments were examined by transmission electron microscope, scanning electron microscope. The rheological behaviors of modified silica suspensions in polyethylene glycol were studied by using Anton-paar 301 stress-controlled rheometer. The results of rheological tests indicated that the surface treatments had a great effect on increasing the maximum weight fraction of silica nanoparticles in Shear-thickening fluids, especially treated by the chemical method with EG.     

提拉法SiO_2化学膜厚度与折射率的变化规律研究

采用提拉法在硅基底上制备了多孔溶胶凝胶SiO2膜,用椭偏法测量薄膜的厚度与折射率,考察了提拉速度和胶体浓度对膜层厚度与折射率的影响。对厚度与提拉速度的关系进行线性与幂函数拟合,并比较分析两种拟合的关系及其对工艺流程的作用。比较了不同浓度胶体所得到的同一厚度薄膜的折射率变化规律。结果表明:对于同一胶体浓度下薄膜厚度与提拉速度的正相关关系,线性拟合相比幂函数拟合可以更好地解释实验结果的规律性。同时,折射率在一定范围内也会随着提拉速度的增加而减小。镀同一厚度膜时,浓度大的胶体膜层折射率大。通过对提拉速度和胶体浓度的控制可以得到理想的薄膜厚度与折射率。