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Ion-pair dissociation is an important molecular process and frequently happens when the target molecule is pumped to its electronically superexcited states. In contrast to the experimental studies of photoexcitation ion-pair dissociation, there are some experimental challenges in the electron-impact ion-pair dissociation study, in particular, on determination of the energetic threshold. Here we report an experimental development for the ion-pair dissociation study by using the monochromized electron impacts. As an example, the threshold of BrCN→Br?+CN+ is determined as 13.78 eV according to the appearance energy of CN+ signals, meanwhile, the time-sliced ion velocity image of CN+ is recorded at 16.09 eV and indicates an anisotropic distribution of the CN+ momentum. 相似文献
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研究级激光微探针飞行时间质谱仪及其应用 总被引:8,自引:2,他引:8
本文介绍了自行研制的激光微探针飞行时间质谱仪,阐述了该仪器的基本原理、结构特点、研究功能及其所达到的参量。该仪器是一台具有高分辩率、高灵敏度、研究功能强并兼具常规分析所需的简便、快捷的现代大型分析仪器。文章还介绍了该仪器的应用实例,如可作几万道尔顿以上的大分子物质分析,大分子蛋白质混合物的分析,有机化合物特别是难挥发和热不稳定有机物的分析,少至几十埃薄膜,如C60等薄膜材料成分分析,负离子分析,以 相似文献
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采用离子对高效液相色谱法,结合峰面积归一化法测定并计算脂肪烷基二甲基苄基季铵盐的平均相对分子质量(M)。用C18键合硅胶色谱柱(4.6mm×250mm,5μm)作固定相,以含10mmol.L-1戊基磺酸的乙腈-水(95+5)溶液为流动相,对试液进行离子对色谱分离。于波长262nm处用二极管阵列检测器进行测定。方法用于样品1227的平均相对分子质量的测定,测得M为344.5,经F和t检验,测定值与气相色谱法测定结果一致。 相似文献
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本文研究了离子对反相液相色谱分析氨基酚异构体的可能性、影响因素和色谱条件,发现以含4×10-8mol/L四丁基碘化铵、0.184mol/L醋酸钠的甲醇水溶液(23:77)作为流动相,ODS为固定相时可以实现氨基酚异构体的良好分离. 相似文献
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本文研究了离子对反相液相色谱分析氨基酚异构体的可能性、影响因素和色谱条件,发现以含4×10-8mol/L四丁基碘化铵、0.184mol/L醋酸钠的甲醇水溶液(23:77)作为流动相,ODS为固定相时可以实现氨基酚异构体的良好分离。 相似文献
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常用的气体分析质谱仪使用四极杆质谱作为分析器,分辨率一般低于300,无法解决同质量数离子带来的干扰问题.本实验自行研制了一种小型高分辨气体分析质谱仪,它采用电子轰击离子源反射式飞行时间质量分析器.仪器腔体总长45 cm,在m/z 28的位置,质量分辨率达到3000(Full width at half maximum,FWHM),实现了CO和N2的半峰谷分离;在m/z 69的位置,仪器分辨率达到5000(FWHM).在直接大气压进样条件下,可以检测到空气中136Xe(含量7.8 μ g/m3)和80Kr(含量2.8 μg/m3).使用ADC采集时,仪器的动态范围为1 06.该仪器将作为高端气体质谱仪,应用于过程监测在线分析、环境有机挥发物研究、热分析质谱及催化反应监测等领域. 相似文献
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铜硫团簇离子的形成与光解 总被引:1,自引:0,他引:1
本文首次报导用激光溅射方法产生了铜硫团簇离子Cll。S:,并对其进行了紫外激光解离,得出了团簇离子的组成及光解规律.与以前关于过渡金属与非金属的二元团簇研究结果[‘-‘]有所不同,铜是具有满壳层d电子结构的过渡金属元素,这使得无论是所产生的团簇的组份,还是其光解规律,都表现出了明显的特点.本文在分析铜硫团簇离子的形成和光解规律的基础上,初步讨论了团簇的结构特征以及过渡金属满壳层d电子结构对团簇的形成与结构的影响.实验是在本实验室自制的串级飞行时间质谱仪上进行的,有关仪器的详情参见文献问.所用样品为:… 相似文献
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《Analytical letters》2012,45(9):1448-1456
A simple and accurate ion-pair reversed-phase high-performance liquid chromatographic (RP-HPLC) method has been developed and validated for determination of acebutolol (ACE) in tablet dosage forms. Both ACE and ambroxol (internal standard) were well separated using a reversed phase column and a mobile phase consisting of a mixture of methanol-0.05 M acetic acid (containing 8 mM sodium 1-heptanesulfanate) (65:35 v/v) with pH adjusted to 3.2 with triethylamine. The mobile phase was pumped at 0.80 mL min?1 flow rate and ACE was detected by diode-array detection at 240 nm. The retention times for ACE and internal standard (IS) were 4.574 and 8.236 min, respectively. A linear response (r = 0.9998) was observed in the range of 0.27–2.93 μg mL?1 in mobile phase. The limit of detection and limit of quantification were found as 0.07 and 0.23 μg mL?1 in the mobile phase. Validation parameters such as precision, accuracy, selectivity, reproducibility, and system suitability tests were also determined. The excipients did not interfere with the assay of ACE in tablet dosage forms. It is suggested that the proposed method can be used for routine quality control and dosage-form assay of ACE. 相似文献
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以表阿霉素及其6种相关物质为研究对象,系统评价了其在反相离子对色谱模式下的色谱行为.分别考察了流动相中有机相种类、有机相比例、水相中离子对试剂浓度、pH值对表阿霉素及其相关物质的影响.结果表明,使用乙腈作为有机相洗脱能力及分离效果优于甲醇,保留时间随乙腈比例增大而减小;随着离子对试剂十二烷基硫酸钠浓度增加,杂质阿霉素酮及柔红霉酮几乎无影响,其他5种物质保留时间增加.同时,表阿霉素及其杂质的保留行为受流动相pH值影响较大,当pH不高于4时可获得较好的分离效果.通过对表阿霉素及其相关物质反相离子对模式下的保留行为进行了系统的评价和定量描述,研究结果将有助于该类化合物液相色谱分离方法的发展. 相似文献
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Yu-chao Zhao Zeng-guang Zhang Jin-yun Yuan Hong-guang Xu Wei-jun Zheng 《化学物理学报(中文版)》2009,(6):655-662
We introduce a modification of reflectron time-of-flight mass spectrometer for laser photodissociation of mass-selected ions. In our apparatus, the ions of interests were selected by a mass gate near the first space focus point and decelerated right after the mass gate, were then crossed by a laser beam for dissociation. The daughter ions and surviving parent ions were re-accelerated and analyzed by the reflectron time-of-flight mass spectrometer. Compared to the designs reported by other research groups, our selection-deceleration-dissociation-reacceleration approach has better daughter-parent-ions-separation, easier laser timing, and better overlapping between the ion beam and laser beam. We also conducted detailed cal- culations on the parent ion and daughter ion flight times, and provided a simplified formula for the calibration of daughter ion mass. 相似文献
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溴代烷烃在紫外波段的光解离过程 总被引:1,自引:3,他引:1
在飞行时间质谱仪中,采用波长为234 nm和267 nm的激光,研究溴代烷烃CHBr3、CH2Br2、C2H5Br及C2H4Br2的光离解过程.在UV激光的作用下,溴代烷烃分子主要发生的是吸收1个光子解离出Br原子,然后继续吸收光子发生Br原子的(2+1)共振增强多光子电离的过程.其中由溴代烷烃分子解离得到的Br原子可能存在着两种布居:基态Br(2P03/2)及激发态Br*(2P01/2).研究解离得到的Br原子的分支比 N(Br*)/N(Br),并给出测量结果:溴代烷烃分子解离得到的Br原子在267 nm激光作用下的分支比明显大于在234 nm激光作用下的结果.对此多光子过程的机理,也进行了分析讨论. 相似文献
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《Analytical letters》2012,45(13):1687-1696
Abstract This paper reports a simple, accurate, reproducible, stability-indicating procedure which may be used to quantitatively determine methenamine base, methenamine mandelate or methenamine hippurate in tablet dosage forms. The procedure initially involves the separation of methenamine from the dosage form and from formaldehyde, the decomposition product, by a cartridge ion-pair extraction process. The methenamine may then be assayed by a number of methods. In this paper the methenamine was hydrolyzed to formaldehyde and the formaldehyde determined by the Nash procedure. The method compares favorably with the USP XXI procedure for methenamine tablets. Advantages of the procedure include the ability to use a single method for the base and salt forms of the drug and the potential application to stability and quality control studies of methenamine dosage forms. 相似文献
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快速测量挥发性有机物的膜进样-飞行时间质谱仪的设计和应用 总被引:4,自引:0,他引:4
研制了一种膜进样-微型飞行时间质谱仪, 该仪器使用双层50 μm硅橡胶膜作为大气压下直接进样的接口. 实验结果表明, 随着样品流速的提高, 膜富集效率信号强度呈线性提高. 双膜中间具有真空差分系统, 富集得到的样品被迅速抽走, 进样系统中样品无记忆效应. 样品在膜中的响应时间为100 s, 而打开差分系统后仅需10 s信号即下降为平稳状态. 与毛细管直接进样相比, 双层膜的富集作用显著, 在相同的实验条件下使用膜进样技术测定10×10-6 (体积分数)苯、甲苯和对二甲苯的信号强度分别提高了280, 370和600倍. 膜进样系统与真空紫外光软电离方式联用, 对于苯的检出限已经达到了25×10-9 (体积分数), 线性范围为3个数量级. 由于采用了软电离方法, 无碎片离子产生, 所以能够根据分子量进行快速定性分析. 将该仪器应用于香烟主烟气中可挥发性有机物的在线分析, 得到50多种可挥发性的有机物. 实验结果表明, 膜进样-飞行时间质谱将在在线分析(特别是环境监测)方面具有广泛的应用空间. 相似文献