A method for adjusting valence state distribution of metal cluster ions in electrospray ion source

An electrospray ion source and metal cluster technology, which is applied in the direction of material analysis, analysis materials, instruments, etc. by electromagnetic means, can solve the problem of not being able to obtain molecular ion peaks, etc.

Inactive Publication Date: 2020-04-10
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Therefore, in the current situation, in many cases, molecular ion peaks cannot be obtained, only quasi-molecular ion peaks can be obtained [5]

Method used

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  • A method for adjusting valence state distribution of metal cluster ions in electrospray ion source
  • A method for adjusting valence state distribution of metal cluster ions in electrospray ion source
  • A method for adjusting valence state distribution of metal cluster ions in electrospray ion source

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Embodiment 1

[0025] The present invention adopts organic solvent acetonitrile to dissolve sample Zn 8 PD 6 L 24 (BF 4 ) 28 crystals, made at a concentration of 4 x 10 - 10 mol / mL solution. The sample solution was collected three times under the conditions of dry nitrogen temperature of 80°C, flow rate of 4 L / min, nebulizer pressure of 20 psig, capillary voltage of 4000 V, and fragmentation voltage of 200 V. Before each experiment, the instrument was calibrated to correct the deviation of the mass axis. Set the flow rate of the injector to 240 μL / h to push the injection needle, and the acquisition time is 1min (Stop Time under the TOF acquisition parameter setting page), to obtain figure 1 . Table 1 is Zn 8 PD 6 L 24 (BF 4) 28 Specific structural analysis of each fragment peak in the mass spectrum.

[0026] Table 1

[0027]

Embodiment 2

[0029] The obtained mass spectrum was imported into Agilent's mass spectrum analysis software Mass Hunter and combined with Waters' isotope analysis software Isotope Pattern to resolve fragment peaks in the mass spectrum. Isotope Pattern can not only accurately calculate the mass-to-charge ratio of the assumed fragment peaks, but also simulate isotopic peaks, while Mass Hunter can not only clearly display the isotopic distribution of each fragment peak, but also the structure and spectrum of the assumed fragment peaks. The actual peaks in the figure are fitted to verify the accuracy of the guess. Table 1 is Zn 8 Pd 6 L 24 (BF 4 ) 28 Specific structural analysis of each fragment peak in the mass spectrum.

Embodiment 3

[0031] Zn 8 Pd 6 L 24 (BF 4 ) 28 The salt NaBF was added to the acetonitrile solution 4 , where C 盐 :C 配合物 = 0:1, 10:1, 100:1. Same as 2, collect 4 new sample solutions 3 times, each for 1 min. It is necessary to import the obtained 3 spectra into the Origin data processing software again, and get figure 2 . like figure 2 , Zn 8 Pd 6 L 24 (BF 4 ) 28 Continue adding NaBF to methanol solution 4 After that, the peak position of the mass spectrum changed gradually. when C NaCl :C Zn8Pd6L24(BF4)28 = 100:1, there are many impurity peaks in the small mass-to-charge ratio range, it is inferred that (NaBF 4 ) n Na + ; large mass-to-charge ratio [Zn 8 Pd 6 L 24 (BF 4 ) 23 ] 5+ NaBF is also added to the 4 , becomes [Zn8Pd 6 L 24 (BF 4 ) 23 (NaBF 4 ) n ] 5 +. Specifically as image 3 . In order to display the experimental results more clearly, use Origin to read out the relative signal intensity values ​​of the main quasi-molecular ion peaks, draw a...

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Abstract

The invention discloses a valence distribution adjustment method of electrospray ion source metal-cluster ions and relates to ESI (electronic spray ion)-TOFMS (time-off-flight mass spectrometer) spectrograms. The valence distribution adjustment method includes the following steps of 1), dissolving metal complex by adopting organic solvent, collecting sample solutions under conditions of set dry nitrogen temperature, flow velocity, atomizer pressure, capillary voltage and fragmentor through an ESI-TOFMS to acquire the spectrograms of the metal complex; 2), leading the spectrograms of the metal complex, acquired in the step 1) to spectrogram analysis software and specifically analyzing the structure of each fragment peak; 3), under the positive ion mode and under the condition that molecular ion peaks, doping electrolyte with different proportions to the metal complex, dissolving the samples with the organic solvent once more and collecting the sample spectrograms with the ESI-TOFMS; 4), using the spectrogram analysis software to specifically analyzing changes of the fragment peaks once more to acquire the result of valence distribution adjustment.

Description

technical field [0001] The invention relates to an ESI-TOF MS spectrum of a metal complex, in particular to a method for adjusting the valence distribution of metal cluster ions in an electrospray ion source. Background technique [0002] Organic compounds are composed of covalent bonds, inorganic compounds are composed of covalent bonds, ionic bonds and metal bonds (and only need to determine their constituent atoms or ions during analysis), while metal complexes are combined by relatively weak coordination bonds Together, they are prone to dissociation during ionization and cannot obtain the desired molecular ion peak (or not prominent enough). We say that the electrospray ion source (ESI) is a "soft ionization source", but in order to actually realize the mass spectrometry analysis of metal complexes, the following three conditions must be met at the same time: first, the ion source is more than the conventional electrospray ion source (ESI)— Soft, that is, our ESI ioniz...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/64
CPCG01N27/64
Inventor 林水潮王亚云杨静苏海峰吴小虎韩英姿施再发郑兰荪
Owner XIAMEN UNIV
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