Disclosure of Invention
In view of this, the present invention provides an oxygen interference compensation method for an FID detector, which can effectively solve the problem of poor oxygen interference compensation effect of a single-range point calibration method in the prior art.
The following presents a simplified summary of the invention in order to provide a basic understanding of some aspects of the invention. It should be understood that this summary is not an exhaustive overview of the invention. It is not intended to determine the key or critical elements of the present invention, nor is it intended to limit the scope of the present invention. Its sole purpose is to present some concepts in a simplified form as a prelude to the more detailed description that is discussed later.
The invention provides an oxygen interference compensation method for an FID detector, which comprises the following steps:
carrying out single-range point calibration on the FID detector;
introducing gas to be detected into an FID detector to obtain first concentration data of the gas to be detected;
introducing the sample gas into an FID detector, and obtaining an oxygen interference compensation model based on the nominal value of the sample gas and the obtained concentration data of the sample gas;
inputting the first concentration data of the gas to be detected into an oxygen interference compensation model to obtain second concentration data of the gas to be detected;
and judging whether the ratio of the second concentration data of the gas to be detected to the laboratory standard data is in a preset range, if the ratio exceeds the preset range, updating the oxygen interference compensation model, and if the ratio does not exceed the preset range, keeping the oxygen interference compensation model.
In some embodiments, the oxygen interference compensation model is a second order polynomial:
y(x)=ax2+bx+c,
wherein x is the first concentration data of the gas to be detected, y (x) is the second concentration data of the gas to be detected, and a, b and c are second-order polynomial coefficients.
Further, let in the FID detector with sample gas, based on the gaseous nominal value of sample and the concentration data of the sample gas who obtains, obtain oxygen interference compensation model, specifically include:
respectively introducing at least three sample gases with different concentrations into an FID detector to obtain concentration data of the sample gases;
substituting the concentration data of the sample gas as x and the corresponding nominal value of the sample gas as y into a second-order polynomial y (x) ax2+ bx + c, the values of coefficients a, b, c are obtained.
Further, the oxygen content of the sample gas is not zero.
In some embodiments, the updating the oxygen interference compensation model specifically includes replacing the coefficient c in the oxygen interference compensation model with c':
c′=c+(d-d′)
wherein d is standard data of the laboratory, and d' is second concentration data of the gas to be measured.
In some embodiments, the laboratory standard data is a nominal value of a standard gas used in a single-range point calibration.
The invention provides an oxygen interference compensation method for an FID (flame ionization detector) on the basis of the existing single-range point calibration, and effectively solves the problem that the oxygen interference compensation effect of the single-range point calibration method in the prior art is poor.
Detailed Description
The technical solutions in the embodiments of the present application will be described below with reference to the drawings in the embodiments of the present application.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures. Meanwhile, relational terms such as "first," "second," and the like may be used solely in the description herein to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
Exemplary embodiments of the present invention will be described below with reference to the accompanying drawings. In the interest of clarity and conciseness, not all features of an actual embodiment are described in the specification. It will of course be appreciated that in the development of any such actual embodiment, numerous implementation-specific decisions may be made to achieve the developers' specific goals, such as compliance with system-related and business-related constraints, which will vary from one implementation to another.
Here, it should be further noted that, in order to avoid obscuring the present invention by unnecessary details, only the device structure closely related to the scheme according to the present invention is shown in the drawings, and other details not closely related to the present invention are omitted.
It is to be understood that the invention is not limited to the described embodiments, since the description proceeds with reference to the drawings. In this context, embodiments may be combined with each other, features may be replaced or borrowed between different embodiments, one or more features may be omitted in one embodiment, where feasible.
Fig. 1 shows a flowchart of an oxygen interference compensation method 100 for an FID detector according to an embodiment of the present invention, which specifically includes:
step 110: a single range point calibration is performed on the FID detector.
In embodiments of the invention, a single-range point calibration of the FID detector is performed, one common way being to remove hydrocarbons firstIntroducing air (obtained after hydrocarbon is removed by a zero gas generator) serving as zero gas into an FID detector, and recording the signal value of the FID detector as zero Z (unit: pA); then, a standard gas with a nominal value of N (unit: ppm) using air as a diluent gas is introduced into the FID detector, and the signal value of the FID detector is recorded as a (unit: pA), so that the calibration magnification of the single-span point calibration is k N/(a-Z). Further, a certain concentration of hydrocarbon-containing gas is passed through the FID detector, and the signal value of the FID detector is obtained as AnIn this case, the formula k (A) can be calibrated according to the single-range point calibrationn-Z) calculating a concentration value of said hydrocarbon-containing gas.
Step 120: and introducing the gas to be detected into the FID detector to obtain first concentration data of the gas to be detected.
In the embodiment of the present invention, the oxygen content of the gas to be measured is not zero, for example, the gas to be measured may be methane gas with air as a diluent gas or other hydrocarbon gas with air as a diluent gas.
In the embodiment of the invention, after the gas to be detected is introduced into the FID detector, the signal value obtained by the FID detector is A1(unit: pA), and obtaining first concentration data k (A) of the gas to be measured by using a single-range point calibration formula1-Z) (unit ppm).
Step 130: and introducing the sample gas into the FID detector, and obtaining an oxygen interference compensation model based on the nominal value of the sample gas and the obtained concentration data of the sample gas.
In the embodiment of the present invention, the oxygen content of the sample gas is not zero, and the sample gas in the embodiment of the present invention may be methane gas or other hydrocarbon gas with a known nominal value and air as a diluent gas.
In an embodiment of the present invention, the oxygen interference compensation model may be a second-order polynomial preset by software: y (x) ax2+ bx + c, where x is the first concentration data of the gas to be measured, y (x) is the second concentration data of the gas to be measured, and a, b, and c are second-order polynomial coefficients.
In the embodiment of the invention, in order to further obtain the values of the coefficients a, b and c of the second-order polynomial, at least three coefficients can be usedRespectively introducing sample gas with different concentrations into an FID detector, wherein the nominal value of the sample gas is a known preset value, and after the sample gas is introduced into the FID detector, the concentration data of the sample gas can be acquired according to the signal value of the FID detector1、y2、y3Respectively introducing the sample gas into FID detectors to obtain FID detector signal values B of the sample gas1、B2、B3The concentration data of the sample gas obtained by using the single-range point calibration formula of the FID detector are respectively as follows: x is the number of1=k*(B1-Z) (in ppm), x2=k*(B2-Z) (in ppm), x3=k*(B3-Z) (unit ppm).
Further, the concentration data of the sample gas of at least three different concentrations is taken as x, and the corresponding nominal value of the sample gas is taken as y, and is substituted into the second-order polynomial y (x) ax2+ bx + c, the values of coefficients a, b, c can be obtained.
For example, in the embodiment of the present invention, four different sample gases may be selectively and respectively introduced into the FID detector, and the obtained concentration data of the sample gas and the corresponding nominal value of the sample gas are shown in table 1.
TABLE 1 concentration data of sample gas and nominal value of sample gas
Further, in the embodiment of the present invention, the first three sets of data in table 1 may be selected, and the second order polynomial y (x) ax may be substituted with the concentration data of the sample gas as x and the corresponding nominal value of the sample gas as y2+ bx + c, yielding:
131=10167.092224a+100.832b+c
264=40118.087025a+200.295b+c
394=90179.489401a+300.299b+c
further, the second-order polynomial is calculated as y: (x)=-0.0002x2+1.3934x-7.6047, in the embodiment of the present invention, the range of the first concentration data x of the gas to be detected may be set to 0 < x ≦ 1000, and then a second-order polynomial curve may be obtained as shown in fig. 2.
Step 140: and inputting the first concentration data of the gas to be detected into an oxygen interference compensation model to obtain second concentration data of the gas to be detected.
In the embodiment of the invention, the first concentration data of the gas to be detected is input into an oxygen interference compensation model: y (x) ax2+ bx + c, where x is the first concentration data of the gas to be measured, and y (x) is the second concentration data of the gas to be measured, so as to obtain the second concentration data of the gas to be measured.
For example, the oxygen interference compensation model provided in step 130 in the embodiment of the present invention specifically includes: y (x) ═ 0.0002x2And under the condition of +1.3934x-7.6047, substituting the first concentration data of the gas to be measured as x into the oxygen interference compensation model to obtain second concentration data of the gas to be measured.
Table 2 shows comparison of oxygen interference compensation effects of first concentration data obtained by calibrating only a single-range point of the same gas to be measured and second concentration data further obtained by using the oxygen interference compensation model provided in the embodiment of the present invention.
TABLE 2 Single Range Point calibration and comparison of Compensation Effect of oxygen disturbance Compensation model
In practical use, after a period of time, the second concentration data obtained by the oxygen interference compensation model may be shifted, so that it is necessary to identify the shift and perform a shift correction on the oxygen interference compensation model when the shift exceeds a preset range.
Step 150: and judging whether the ratio of the second concentration data of the gas to be detected to the laboratory standard data is in a preset range, if the ratio exceeds the preset range, updating the oxygen interference compensation model, and if the ratio does not exceed the preset range, keeping the oxygen interference compensation model.
In the embodiment of the invention, whether the ratio of the second concentration data of the gas to be detected to the laboratory standard data is within a preset range is judged through the preset function of software. In the embodiment of the present invention, the laboratory standard data is a nominal value of a standard gas used in a single-range point calibration of the FID detector, that is, it is determined whether a ratio of the second concentration data of the gas to be detected to the nominal value of the standard gas used in the single-range point calibration is within a preset range, for example, in the embodiment of the present invention, the preset range may be 0.9 to 1.1, the oxygen interference compensation model is updated when the ratio of the second concentration data to the nominal value of the standard gas used in the single-range point calibration is out of the preset range, and the oxygen interference compensation model is maintained when the ratio of the second concentration data to the nominal value of the standard gas used in the single-range point calibration is not out of the preset range. It should be noted that the preset ranges given above in the embodiments of the present invention are only examples, and those skilled in the art can select suitable value ranges according to actual needs.
In the embodiment of the present invention, the updating the oxygen interference compensation model may specifically be implemented by replacing a coefficient c in the oxygen interference compensation model with c':
c′=c+(d-d′)
wherein d is standard data of the laboratory, and d' is second concentration data of the gas to be measured.
In the embodiment of the invention, the laboratory standard data is standard gas adopted in single-range point calibrationThe nominal value of the volume, and therefore the difference between the nominal value of the standard gas used in calculating the single-span point calibration and the second concentration data of the gas to be measured, is updated in the embodiment of the present invention, for example, in the case where the nominal value of the standard gas is 100ppm and the second concentration data of the gas to be measured is 97.32ppm, c ═ c +2.68 can be obtained, that is, the oxygen interference compensation model is updated as: y (x) ax2+bx+c+2.68。
In the embodiment of the invention, the updating oxygen interference compensation model can be implemented by sending a reminding message to a user after software recognizes that the ratio of the second concentration data to the nominal value of the standard gas adopted in the single-range point calibration exceeds a preset range, and selecting to trigger or not to trigger the updating of the oxygen interference compensation model according to actual conditions after the user obtains the reminding message; or after the software recognizes that the ratio of the second concentration data to the nominal value of the standard gas adopted in the single-range point calibration exceeds a preset range, the software automatically updates the oxygen interference compensation model.
In the embodiment of the invention, the second concentration data is subjected to offset identification, and the oxygen interference compensation model is updated when the offset exceeds the preset range, so that the influence of the offset on the oxygen interference compensation can be effectively reduced, and the accuracy of the oxygen interference compensation is ensured.
The above-mentioned embodiments are only specific embodiments of the present invention, which are used for illustrating the technical solutions of the present invention and not for limiting the same, and the protection scope of the present invention is not limited thereto, although the present invention is described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: any person skilled in the art can modify or easily conceive the technical solutions described in the foregoing embodiments or equivalent substitutes for some technical features within the technical scope of the present disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included therein.