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.
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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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