Discrimination of line overlap interference and analysis line selection in ICP spectrometer analysis

ICP spectrometer has become one of the most conventional analytical instruments. There are more and more people using ICP emission spectrometer for elemental analysis, and its application field is also wider and wider. Therefore, people engaged in ICP emission spectrum analysis continue to follow. increase. The spectrum of the ICP spectrometer is very much. Many friends don't know which line to use in the analysis. Let's briefly talk about it here.

In the analysis technology, we will notice its interference problem, because the interference effect is one of the most complicated problems in analytical chemistry, or more than 90% of the theoretical problems in analytical chemistry are more or less solved with interference problems. Associated with.

The same is true for ICP spectrometer analysis, especially for spectral interference caused by line overlap. Because the spectrum of the emission spectrum is very large, for a simple structure element, the number of lines is at least two digits, and for those elements with complex structures, the number of lines is 5 digits. the above.

This is not difficult to understand, because gaseous free atoms can be excited after gaining energy, and each atom has many excited states. If the energy obtained by a gaseous free atom exceeds its ionization energy, it will also ionize. If the energy continues to be obtained after ionization, it will also be excited to transition to the excited state of the ion, so the atom of each element includes its ion. There will be many, many levels of energy.
Most of the current ICP spectrometers use the two-dimensional spectroscopic method of the echelle grating, so the obtained spectrum is no longer like the one-dimensional line spectrum of the past, it is two-dimensional or three-dimensional (the third dimension is the emission intensity). So whenever someone asks me how many lines there are in the emission spectrum, I will show them the spectrum of the two-dimensional emission spectrum of multiple elements. I will ask them that such a spectrum looks like a cloudless night. The stars in the sky, they are big and small, bright and dark. If someone asks you to count the stars, you still want to know how many of them?

Because there are so many spectral lines in the atomic emission spectrum, when the dispersive power and resolution of the spectroscopic system of the ICP emission spectrometer are insufficient, some spectral lines with small wavelength differences will partially or completely overlap. Spectral interference. To date, there is no spectroscopy instrument that can separate all atomic lines. This is why we have to deal with spectral interference when performing atomic emission spectroscopy. It is also a good thing that the spectral line is a bad thing, because it provides us with more choices while easily forming interference, and provides us with a very rich atomic structure information, which is why the qualitative analysis of the emission spectrum is accurate and reliable. important reason.

Fortunately, in the past emission spectroscopy instruments, there is a multi-channel instrument that uses a photomultiplier tube to detect the line intensity of the emission spectrum. Because it can perform multi-element simultaneous measurement, usually only one fixed wavelength is provided for each element. The spectral line, inevitably to solve the spectral interference caused by spectral line overlap, so in the past there have been many people specializing in this research, so many good and effective correction methods have been established, among which Now one of the more widely used direct reading instrument software is the interference coefficient method, and the other is the spectral line analysis method.

Knowing how the line overlap interference is corrected, the next question is how to judge and identify the interference. Today's full-spectrum direct-reading instruments use solid-state imaging detectors to record and measure the intensity of the line's emission. They generally have the function of presenting line profiles. We can directly observe the line of analysis through this function, even though They are all peak-shaped, but they may appear in various shapes depending on the elements or the lines. They may be symmetrical and asymmetrical, wide and thick, slim, and handsome. We can use this feature to see the wing overlap very intuitively.

For fully overlapping or nearly completely overlapping lines, the situation may be more complicated, because in general, the instrument software will provide more than one analysis line for each element, which can be selected for analysis and determination. For several spectral lines, if all the spectral lines can produce consistent results, it means that the analysis results are accurate and reliable, and there is no influence of the spectral line interference lines. Otherwise, if the results are obviously high, it is likely that there is complete overlap or near completeness. Overlapping interference lines. If we separate the matrix and subtract the blank, the spectral line that was previously significantly higher is no longer high, then it is generally possible to further determine that it has completely overlapping or nearly completely overlapping spectral line interference.
After talking about the judgment and identification of spectral line overlap interference, it is best to say that the analysis line is selected. This problem should be much easier than the previous one, and the following principles can usually be followed:

1. Try to select a spectrum with no interference or interference. The size of the interference can be judged by the self-emission intensity of the analysis line and the interference line and the relative content in the sample.
2. Select a spectral line with high sensitivity, that is, its own body strength;
3. The spectrum with small self-absorption effect, especially when the content of the analysis element is relatively high. If the content of the measured element is high, then a secondary sensitive line can be selected. If the measured element is a large number or a major element in the sample, even a non-sensitive line can be considered;
4. Select a small spectral line of the background;
5. Select a spectrum with good symmetry and peak shape.

For the selection of the analysis line is appropriate, the final depends on the quality of the analysis. If the analysis result is accurate, there is no doubt that the analysis line is selected. Otherwise, it will be analyzed according to the specific situation, because it also involves the sample. The pre-treatment and water and reagent blanks also involve matrix matching of standard and analytical samples, as well as questions about whether the content of the measured elements in the sample solution is within the detection range of ICP emission spectroscopy.

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