CN108169215B - Method for setting upper limit of integration time of emission spectrometer - Google Patents
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Abstract
A method for setting an upper integration time limit of an emission spectrometer comprises the following steps: acquiring blank spectrograms of a primary excitation light source under N different gradient integration time conditions; calculating average blank spectrograms under N different gradient integration time conditions; average blank spectral intensity I at different wavelengthsbLinear regression fitting is carried out on the obtained product and the integral time T to obtain a blank background spectrum time proportionality coefficient kdWith a background constant bd(ii) a Setting a range upper limit FS of the CCD detector; setting a confidence coefficient t of a detection limit; setting a light source blank spectrum fluctuation level characteristic value (RSD)]bThe method comprises the steps of setting α the upper limit of the measuring range of an element to be detected and the multiple of the estimated detection limit of the element, and calculating the upper limit of the integration time according to a formula.
Description
Technical Field
The invention relates to the technical field of emission spectrum analysis, in particular to a method for setting an upper limit of integration time of an emission spectrometer.
Background
Emission spectroscopy is an analytical chemistry method that performs accurate quantitation based on the linear relationship between the concentration of the element to be measured and its emitted characteristic spectral line intensity. Generally, elements in a sample are excited by plasma and emit characteristic spectral lines, the characteristic spectral lines are collected into a light splitting detection system through a front light path, dispersion is generated on space, photoelectric conversion is performed by a detector, and finally a full spectrum is obtained.
The CCD is a common photoelectric converter, and is often used as a detector of a spectroscopic detection system, such as a micro fiber spectrometer, an echelle grating spectrometer, etc.
When the element is quantified by using the emission spectrometry, an element concentration-intensity standard curve needs to be established firstly, so that a standard sample with gradient concentration is introduced during the test. In order to ensure the accuracy of the test result, it is necessary to ensure that the obtained element spectrum has a good signal-to-noise ratio and a good signal-to-back ratio, so that instrument parameters need to be optimized, and the integration time of the CCD is one of the terms. Generally, when other conditions are fixed, the number of photons entering the CCD per unit time is constant for a standard sample of elements with a fixed concentration, so that if the integration time of the CCD is small, the element net signal after photoelectric conversion of the CCD is relatively small and easily submerged in the dark noise of the CCD, that is, the signal-to-noise ratio/signal-to-back ratio of the element signal is low. When the time is too long, the CCD is likely to be saturated or the linear range of the CCD response is easily exceeded, both of which may damage the accuracy of the test result.
In order to obtain a better characteristic spectral line of an element to be tested, the integration time of the CCD is generally optimized in the test process, and a set upper limit value of the integration time is obtained.
There are two schemes for setting the integration time of CCD, one of which is trial and error method, that is, for some element, firstly, the element standard sample with the upper limit concentration of its measuring range is introduced, the integration time value is continuously adjusted, and the final suitable integration time is determined by the intensity value of its characteristic spectral line.
The other scheme is a preset method, namely, the integration time upper limits of different characteristic spectral lines of different elements under different concentration conditions are given or preset integration time is given through the arrangement and summarization of the test results in the early stage, and the integration time upper limits or the preset integration time is written into software in the form of a database and called when in use.
However, the disadvantages of the two schemes are: 1. optimization and trial and error are needed under the conditions of different elements, different characteristic spectral lines and different concentrations, so that the test time and the test cost are increased; 2. the scheme has poor transplanting effect and needs a large amount of repeated tests.
Disclosure of Invention
The application provides a method for setting the upper limit of the integration time of an emission spectrometer, wherein a detector of the emission spectrometer is a CCD detector, and a calculation method for setting the upper limit of the integration time of the CCD detector comprises the following steps:
acquiring blank spectrograms of a primary excitation light source under N different gradient integration time conditions, wherein N is more than or equal to 2;
calculating average blank spectrograms under N different gradient integration time conditions;
average blank spectral intensity I at different wavelengthsbLinear regression fitting is carried out on the obtained product and the integral time T to obtain a blank background spectrum time proportionality coefficient kdWith a background constant bd；
Setting a range upper limit FS of the CCD detector;
setting a confidence coefficient t of a detection limit;
setting a light source blank spectrum fluctuation level characteristic value (RSD)]b；
Setting α the upper limit of the measuring range of the element to be detected and the multiple of the estimated detection limit of the element;
according to the formula
An upper integration time limit is calculated.
In one embodiment, the calculating of the average blank spectrogram under N different gradient integration time conditions specifically includes:
performing M times of tests on the blank spectrogram under each gradient integration time condition, wherein a saturation value does not appear in the full spectrogram under the highest integration time condition, and M is more than or equal to 1;
the average blank spectrum for M tests was calculated.
In one embodiment, the upper range limit FS of the CCD detector is set to a full range value, or the range FS is set according to the linear influence range of the CCD detector.
In one embodiment, the time scale factor k of the blank background spectrumdIs k isd＝kn+kpWherein k isnTime scale factor, k, of dark noise of a CCD detectorpTime ratio of plasma backgroundAnd (4) the coefficient.
According to the calculation method for setting the upper limit of the integration time in the embodiment, because computer-aided calculation can be realized through a formula, the operation of workers is liberated, and after the experimental conditions are determined, only a blank spectrogram of an excitation light source under different gradient integration time conditions needs to be tested once, so that the integration condition optimization is avoided under the conditions of different elements, different characteristic spectral lines and different concentrations; the method is defined based on objective laws of physics and detection limit standards, and is accurate and reliable; the method has good portability and expandability, can be compatible with a detection limit definition method, and is suitable for different CCD types and the upper limit of the measuring range thereof, the stability levels of different excitation light source systems, different upper limits of measuring ranges of elements to be detected, different elements to be detected, characteristic wavelengths and the like.
Drawings
FIG. 1 is a flowchart of CCD integration time upper limit setting calculation;
FIG. 2 is a graph of the average blank spectra under different gradient integration time conditions;
FIG. 3 is a blank background spectrum time scale coefficient spectrogram obtained by linear fitting at different wavelengths;
FIG. 4 is a blank background spectral constant spectrum obtained by linear fitting at different wavelengths;
FIG. 5 is a graph of linearly fitted correlation coefficients at different wavelengths;
fig. 6 is an integrated time upper limit spectrum obtained at different wavelengths.
Detailed Description
The present invention will be described in further detail with reference to the following detailed description and accompanying drawings.
The present embodiment provides a method for setting an upper limit of integration time of an emission spectrometer, and preferably provides a method for calculating an upper limit of integration time of a CCD detector when the detector of the emission spectrometer is the CCD detector, and a flowchart thereof is shown in fig. 1, and specifically includes the following steps.
S1: and acquiring blank spectrograms of the primary excitation light source under N different gradient integration time conditions, wherein N is more than or equal to 2.
S2: and calculating the average blank spectrogram under N different gradient integration time conditions.
In the step, the blank spectrogram under each gradient integration time condition is tested for M times, namely, the blank spectrogram under each gradient integration time condition is tested for M times repeatedly, and the spectrogram under the highest integration time condition in N gradient integration times does not have a saturation value, wherein the highest integration time refers to the maximum value in the N gradient integration times, if the saturation value exists, the saturation value is removed so that the saturation value does not enter calculation, or the maximum integration time is reduced to avoid the saturation of intensity, and M is more than or equal to 1; and then, calculating the average blank spectrogram of M tests, and calculating the average blank spectrogram under N different gradient integration time conditions by analogy.
S3: average blank spectral intensity I at different wavelengthsbLinear regression fitting is carried out on the obtained product and the integral time T to obtain a blank background spectrum time proportionality coefficient kdAnd a background constant dd。
In this step, the linear regression fitting method is: i isb＝kdT+bdObtaining a time proportional coefficient k of a blank background spectrum after linear regression fittingdWith a background constant bd。
S4: and setting the upper limit FS of the measuring range of the CCD detector.
The upper limit FS of the CCD detector range may be set to its full-scale value, or the FS may be set according to the linear influence range of the CCD detector.
S5: a confidence coefficient t of the detection limit is set.
S6: setting a light source blank spectrum fluctuation level characteristic value (RSD)]b。
S7, setting the upper limit of the measuring range of the element to be detected and the multiple α of the estimated detection limit of the element.
S8: and calculating the upper limit of the integration time according to a formula.
The formula in this step is:
the derivation of this equation is as follows:
emitted by the element/sample to be measured after being excited by the plasmaConverting the characteristic spectrum into an electric signal by a light splitting detection system, if a CCD detector is selected as a detector of the light splitting detection system, the intensity of a pixel corresponding to the characteristic spectrum is I, and the light intensity is specifically the dark noise I of the CCD detectornPlasma background spectrum IpSignal characteristic spectrum net signal intensity IsTo sum, i.e.
I＝In+Ip+Is(1)；
As known from the working principle of the CCD detector, the spectral intensity of CCD response and the setting of integration time show a linear relation, namely, the CCD dark noise InPlasma background spectrum IpComprises the following steps:
In＝knT+bd(2)
Ip＝kpT (3)
where T is the integration time of the CCD, knAnd bdRespectively is the time proportionality coefficient and the dark noise constant of the CCD dark noise; k is a radical ofpTime scaling factor for the plasma background.
Net signal intensity for elemental signature spectra IsBesides being linear with respect to the integration time, it is also proportional to the concentration of the element to be measured, according to the basic principle of emission spectroscopy, and therefore:
Is＝ksCT (4)
wherein k issThe time scale coefficient of the signal is shown, and the concentration of the element to be detected is C;
let kd＝kn+kpAnd is defined asbThe blank background spectrum intensity obtained by the CCD when the element to be detected is not introduced is Ib＝In+Ip＝kdT+bd，kdSubstituting formulas 2-3 into formula 1 for corresponding blank background spectrum time proportionality coefficients to obtain:
I＝ksCT+kdT+bd(5)
the detection limit is generally defined as that a series of standard solutions are injected when an instrument is in a normal working state, a working curve is made, blank solutions are continuously measured for n times, and the concentration corresponding to t times of the standard deviation of the blank values for n times is taken as the detection limit, so that t is a confidence coefficient in the detection limit calculation method and is related to the test times n;
let the standard deviation of blank values n times be [ SD ]]bObtaining the slope k of the standard curve according to the formula 5sT, then defined according to the detection limit D L, obtaining a general expression:
the concentration C of the element to be detected is set to be a times of the detection limit D L of the element, namely
C＝α·DL (7)
From equations 6 and 7:
ksCT＝αt[SD]b(8)
substituting equation 8 into equation 5 and letting the relative standard deviation of the blank values for n times be
Finally, the following is obtained:
in the above equation, let the CCD intensity I be equal to the upper limit FS of the range allowed by the CCD, the upper limit of the CCD integration time setting is obtained as follows:
for convenience of understanding, an ocean optical HR4000 series spectrometer is taken as an example, a computer is used to calculate an upper limit of an integration time at a certain characteristic wavelength of an element through the above formula (10), and an excitation source uses argon microwave plasma (i.e., ArMPT);
first, operation S1-S3 is executed to obtain b by performing linear regression fitting according to the average blank spectrum intensity and the integration timed＝650，kd＝30；
AD conversion of ocean optical HR4000 spectrometerThe number of bits is 14, so the full-scale value FS of the CCD is 214-1＝16383；
According to JJG768-2005 emission spectrometer test protocol, taking a confidence coefficient t as 3;
for stable ArMPT, the plasma stability is higher, and a light source background spectrum fluctuation level characteristic value [ RSD ] is taken]b＝0.3％；
Taking the upper limit of the measuring range of the element to be measured as 100 times of the estimated detection limit of the element, namely α being 100;
substituting the above parameters into equation 10 to obtain TmaxThe upper limit of the CCD integration time is obtained 267 ms.
The CCD linear response range may be considered as the CCD upper limit FS allowed in step 4, and if FS is 95% of its full range, FS is 95% × (1)14-1) 15563.85, when Tmax＝253.65ms。
It should be noted that the method of this embodiment does not limit the element to be measured and the characteristic wavelength, and the method is effective for capturing all wavelengths in the spectral range by the photodetection system, that is, the parameters in the above steps S4-S7 may take different values at different wavelengths, that is, different characteristic spectral lines of different elements are processed separately, and the following description is made with reference to specific examples.
Blank spectrograms of a primary excitation light source under the conditions of 11 different gradient integration times are obtained, the test frequency under each gradient integration time is 11, and the full spectrogram under the highest integration time is ensured not to have a saturation value.
Calculating the average blank spectrogram under different gradient integration time conditions to obtain 11 calculated average blank spectrograms, as shown in fig. 2, the spectrograms under different gradient integration time conditions of T-4, 6, 8, 12, 16, 24, 32, 48, 64, 96 and 128ms are selected, N-11, and the maximum integration time is 128 ms; it should be noted that: the gradient integration time is not necessarily equally spaced, and may be a time that increases gradually.
Average blank spectral intensity I at different wavelengthsbLinear regression fitting with the integral time T to obtain the blank background spectrum timeCoefficient of proportionality kdWith a background constant bdIn order to further verify the rationality of the linear regression, the number of points fitted at different wavelengths in this example is 11, as shown in fig. 3 and 4, respectively, and fig. 5 shows the correlation coefficient R of the linear fit at different wavelengths2Spectrogram, R2∈(0.992，1]。
An allowable upper limit FS of the CCD range is set, and in this example, FS is 2 for all wavelengths14-1＝16383。
And setting a confidence coefficient t in the detection limit calculation method, and obtaining the confidence coefficient t as 3 according to JJG768-2005 emission spectrometer verification protocol.
Setting a light source blank spectrum fluctuation level characteristic value (RSD)]bFor stable ArMPT, the plasma stability is high, and a light source background spectrum fluctuation level characteristic value [ RSD ] is taken]b＝0.3％。
Setting α the upper limit of the measuring range of the element to be measured and the multiple of the estimated detection limit of the element, and taking the upper limit of the measuring range of the element to be measured as 100 times of the estimated detection limit of the element, namely α is 100.
Calculating an upper limit T of the integration time according to equation (10)maxAnd obtaining an integrated time upper limit spectrogram at different wavelengths, as shown in fig. 6.
The present invention has been described in terms of specific examples, which are provided to aid understanding of the invention and are not intended to be limiting. For a person skilled in the art to which the invention pertains, several simple deductions, modifications or substitutions may be made according to the idea of the invention.
Claims (2)
1. A method for setting an upper limit of integration time of an emission spectrometer, wherein a detector of the emission spectrometer is a CCD detector, and the method for calculating the upper limit of integration time setting of the CCD detector comprises the following steps:
acquiring blank spectrograms of a primary excitation light source under N different gradient integration time conditions, wherein N is more than or equal to 2;
calculating average blank spectrograms under N different gradient integration time conditions;
for averaging space at different wavelengthsWhite spectral intensity IbLinear regression fitting is carried out on the obtained product and the integral time T to obtain a blank background spectrum time proportionality coefficient kdWith a background constant bd；
Setting a measuring range upper limit FS of the CC D detector;
setting a confidence coefficient t of a detection limit;
setting a light source blank spectrum fluctuation level characteristic value (RSD)]b；
Setting α the upper limit of the measuring range of the element to be detected and the multiple of the estimated detection limit of the element;
according to the formula
The upper limit of the integration time is calculated,
wherein, [ SD]bIs the standard deviation of blank values n times, T is the integration time of CCD, kd＝kn+kp，knTime scale factor, k, of CCD dark noisepThe upper range limit FS of the CCD detector is set to be a full range value for the time scale factor of the plasma background, or the FS is set according to the linear influence range of the CCD detector.
2. The setting method according to claim 1, wherein the calculating of the average blank spectrogram under N different gradient integration time conditions specifically comprises:
performing M times of tests on the blank spectrogram under each gradient integration time condition, wherein a saturation value does not appear in the spectrogram under the highest integration time condition in the N gradient integration times, and M is more than or equal to 1;
the average blank spectrum for M tests was calculated.
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