CN112903879A - Method and apparatus for flame ionization detection of oxygen-containing samples - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 39
- 230000027734 detection of oxygen Effects 0.000 title claims description 3
- 239000001301 oxygen Substances 0.000 claims abstract description 111
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 111
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 110
- 239000007789 gas Substances 0.000 claims abstract description 105
- 238000012937 correction Methods 0.000 claims abstract description 78
- 238000005259 measurement Methods 0.000 claims abstract description 42
- 238000001514 detection method Methods 0.000 claims abstract description 22
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 50
- 229930195733 hydrocarbon Natural products 0.000 claims description 19
- 150000002430 hydrocarbons Chemical class 0.000 claims description 19
- 238000012360 testing method Methods 0.000 claims description 11
- 238000004817 gas chromatography Methods 0.000 claims 1
- 239000004215 Carbon black (E152) Substances 0.000 description 11
- 230000008859 change Effects 0.000 description 6
- 150000001335 aliphatic alkanes Chemical class 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000000945 filler Substances 0.000 description 3
- 239000012855 volatile organic compound Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000012887 quadratic function Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000013100 final test Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
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Abstract
The invention provides a method and a device for flame ionization detection of a sample containing oxygen, which can eliminate or reduce interference caused by the oxygen contained in the sample gas without the need of adjusting a pipeline system. Specifically, the method comprises the following steps: a calibration step of providing a correction relationship established based on a measured value obtained using a plurality of standard gases containing different oxygen concentrations and a reasonable value, wherein the reasonable value is the measured value obtained using the standard gas containing no oxygen; a measuring step, measuring the sample to obtain a measured value of the sample; and a correction step of correcting the measured value obtained in the measurement step according to the oxygen concentration in the sample and the correction relation provided in the calibration step.
Description
Technical Field
The invention relates to the field of flame ionization detection, in particular to a method and a device for flame ionization detection of a sample containing oxygen.
Background
The non-methane total hydrocarbon content of the sample can be conveniently measured using a differential method using a Gas Chromatography-Flame Ionization Detector (GC-FID, Gas Chromatography-Flame Ionization Detector).
Referring to fig. 1, the conventional gas chromatography-flame ionization detector combination includes a total Hydrocarbon column, in which a filler is not generally disposed, and a Methane column, in which a filler capable of separating Non-Methane total hydrocarbons (NMHC) from Methane is filled.
In the measurement, the sample is first introduced into both the total hydrocarbon column and the methane column. During the flowing process of the total hydrocarbon column, the sample firstly enters a FID (Flame Ionization Detector) to peak because no filler blocks; meanwhile, in the methane column, non-methane total hydrocarbons are gradually separated from methane. Then, continuing to pass the carrier gas in the forward direction, the methane in the methane column will move first to the FID peak because of its lower molecular weight and weaker polarity. When the methane in the methane column is detected to be completely peaked, the flow path valve is used for changing the direction of the carrier gas, and the non-methane total hydrocarbons in the methane column are blown out reversely.
By analyzing the peak-out result of the sample after passing through the Total Hydrocarbon column and the peak-out result of the methane after being separated, the Total Hydrocarbon Content (THC) and the methane content of the sample can be respectively obtained, and the difference between the Total Hydrocarbon Content (THC) and the methane content is the non-methane Total Hydrocarbon content.
However, in the above measurement method, since the sample is directly peaked after passing through the total hydrocarbon column, oxygen in the sample may affect the flame while passing through the FID, resulting in deviation of the measurement result.
In order to solve the above problem, patent CN109991345A provides a method for eliminating the influence of oxygen, which eliminates or reduces the interference caused by oxygen contained in the sample gas by additionally introducing a compensation gas containing oxygen. The method requires adjustment of the pipeline system of the device, and is inconvenient to implement.
Disclosure of Invention
In view of the above problems, the present invention provides a method for performing flame ionization detection on a sample containing oxygen, which can eliminate or reduce interference caused by oxygen contained in the sample gas without adjusting a pipeline system.
The inventor finds that the influence of oxygen with different concentrations on the measurement result can be effectively corrected by establishing an empirical functional relation in a targeted manner through intensive research on a GC-FID combination instrument in the prior art.
Based on the above recognition, the present invention provides a method for performing flame ionization detection on a sample containing oxygen, for determining the concentration of one or more gases to be detected in the sample, comprising the steps of: a calibration step of providing a correction relationship established based on a measured value obtained by using a plurality of standard gases containing different oxygen concentrations and a reasonable value, wherein the reasonable value is the measured value of the standard gas containing no oxygen; a measuring step, measuring the sample to obtain a measured value of the sample; and a correction step of correcting the measured value of the sample obtained in the measurement step according to the oxygen concentration in the sample and the correction relation provided in the calibration step.
The standard gas without oxygen is used as a reasonable value, and the measured value of the standard gas with different oxygen concentrations is compared with the reasonable value, so that an empirical relation reflecting the interference of oxygen on the measurement result can be effectively formed. Subsequently, in the case where the oxygen concentration in the sample is known, the measured value can be corrected more accurately by means of the empirical relationship between the oxygen concentration and the value obtained in the calibration step.
In a preferred embodiment of the present invention, the type of the gas to be measured in the standard gas used in the calibration step is the same as the type of the gas to be measured in the sample. The empirical relationship is calibrated according to the target standard gas with the same type as the sample, so that the established empirical function can better accord with the self characteristics of the gas, and the matching degree between the determined correction relationship and the actual condition is improved.
In a preferred technical scheme of the invention, the concentration of the gas component to be detected in the standard gas used in the calibration step is the same as the concentration of the gas component to be detected in the sample.
In a preferred embodiment of the present invention, the correction relationship is a correction function that varies non-linearly with the oxygen concentration.
More preferably, the correction function is
Wherein A' is a correction value, A is a measured value of the sample, a1、a2、…、anConstants determined for the calibration step from the measured values and the rational values, CO2Is the oxygen concentration and n is an integer.
The inventors of the present invention have found through intensive studies on oxygen interference that the oxygen interference can be effectively corrected by a correction function of nonlinear change. Particularly, the polynomial function is used for correction, not only can the fitted curve accurately reflect the influence trend of oxygen on the final test result, but also the polynomial function needs fewer constants determined through calibration steps, the correction relation can be obtained by using fewer times of calibration tests, and the correction is more convenient.
Further, the correction function is
The number of constants to be determined can be further simplified into a and b by further simplifying the correction function, so that the correction function can well balance the convenience of the calibration step and the accuracy of fitting.
In the preferred technical scheme of the invention, the values of a and b are determined by using the standard gas without oxygen and two or more bottles of standard gas with different oxygen concentrations. In the calibration step, a reasonable value A' can be determined from the measured value A of the oxygen-free standard gas; and then, measuring the standard gas with two or more bottles of different oxygen concentrations, and establishing a linear equation of two variables by using the measurement result to determine the values of a and b. By the method, the constants in the correction function can be determined quickly and effectively.
In a preferred embodiment of the present invention, the flame ionization detection method for an oxygen-containing sample further comprises the following steps: the oxygen concentration in the sample is measured in real time or periodically using an oxygen measurement device.
The concentration of oxygen in the sample is obtained through measurement, so that the content of oxygen in the sample can be more dynamically mastered, and the time-varying correction of the measurement result is facilitated.
In the preferred technical scheme of the invention, the flame ionization detection method for the oxygen-containing sample is implemented by using an instrument combining a gas chromatograph and a hydrogen flame ionization detector.
In a preferred embodiment of the present invention, the gas to be measured for target analysis is non-methane total hydrocarbons in the sample.
The present invention also provides an apparatus for performing flame ionization detection on a sample containing oxygen, for determining the concentration of one or more gases to be detected in the sample, comprising:
the calibration unit is used for providing a correction relation established according to the measured values and reasonable values of a plurality of standard gases containing different oxygen concentrations, wherein the reasonable values are the measured values of the standard gases containing no oxygen;
the measuring unit is used for measuring the sample to obtain a measured value;
and the correction unit is used for correcting the measured value obtained by the measurement unit according to the oxygen concentration in the sample and the correction relation provided by the calibration unit.
Drawings
FIG. 1 is a schematic diagram of a prior art GC-FID process for non-methane total hydrocarbon measurement using a difference method;
FIG. 2 is a schematic flow chart of a method for performing flame ionization detection on a sample containing oxygen in an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Implementation mode one
In the prior art, when a difference method measurement is carried out by using a GC-FID (gas chromatography-flame ionization detector) combined instrument, the presence of oxygen interferes with the measurement result of non-methane total hydrocarbons, so that the measurement result is deviated. In order to correct the measurement result, in the present embodiment, a method of numerical correction is used to eliminate the oxygen interference, and the method of numerical correction includes a plurality of steps as shown in fig. 1, which is further discussed below in conjunction with the correction principle.
Since different concentrations of oxygen affect the measurement to different extents, a correction relationship based on the oxygen concentration needs to be provided. To determine the correction relationship, the present embodiment first employs: s01 calibration step, which provides a correction relation established by using a plurality of standard gases containing different oxygen concentrations to obtain the measured value and the reasonable value, to respectively determine the influence of oxygen with different concentrations.
Wherein the reasonable value A0In order to obtain a measured value using a standard gas containing no oxygen, the concentration of the gas to be measured in the target measurement sample gas is equal to the concentration of the gas to be measured in the standard gas (i.e., the standard gas used to determine the correction relationship), that is, in the present embodiment, the sample gas and the standard gas have the same component ratio of alkane gas, and the concentrations of oxygen in different sample gases are different in order to reduce the number of tests.
In the present embodiment, first, the criterion of the correction relationship is determined by determining the rational value. In particular, the rational value can be determined directly using measurements on a standard gas free of oxygen. Because the standard gas does not contain oxygen, the measured value of the standard gas without oxygen in the test is a reasonable value which is not interfered by oxygen and can be used as a correction reference.
In addition, because the concentration of the gas to be measured is set to be the same in each bottle of standard gas, the influence of the variable of the concentration of the standard gas can be effectively eliminated, so that the influence caused by the change of the oxygen concentration can be directly reflected on the change of the measured value, and the correction relation can be established by constructing the change function of the oxygen concentration to the measured value of the standard gas without oxygen.
In this embodiment, the test target is for non-methane total hydrocarbons contained in the sample, so the gas to be burned in the FID mainly includes alkane gases such as methane in addition to hydrogen introduced into the FID itself, and therefore, a standard gas containing alkane gases can be selected to determine the correction relationship. In some embodiments, the change in the type of sample gas to be tested may be corresponded by changing the type of gas to be tested in the standard gas, or, in other embodiments, the change in the concentration of gas to be tested in the sample gas may also be corresponded by changing the concentration of gas to be tested in the standard gas.
In this embodiment, a correction relationship is established based at least in part on the oxygen concentration data and the measurement data. The oxygen concentration data can be manually input by taking data displayed by a label of the configured standard gas as a standard; an oxygen content sensor can be arranged on an input pipeline of the standard gas to measure the concentration of the standard gas and substitute the measured value of the collected oxygen for calculation; in addition, the measurement process may be real-time, intermittent, such as timed, or triggered as needed.
When the rational value is determined, there are still some constants in the correction relation that are not determined, which requires the determination of the constants in the correction function by testing the standard gas, combining the concentration data and the test result. Different types of correction relations (or correction functions) have different numbers of constants to be determined. Because the number of constants to be determined varies, the number of trials that need to be performed to determine these constants also varies.
The inventors found through extensive studies on the influence of oxygen content that the influence of different oxygen concentrations on the measurement results is non-linear, and a polynomial fitting manner can be effectively used to fit a curve, such as a VOC (volatile organic compounds) area value-oxygen concentration curve.
In some embodiments, the correction coefficients in the polynomial fit may be expressed in the inverse form of the polynomial, e.g. using
In order to combine the above two, i.e. to determine all the constants to be determined with a small number of tests and to ensure that the correction function can better fit the effects of different oxygen concentrations on the measured values, in the present embodiment, the fitting is performed in the form of a quadratic function.
Specifically, the correction function is
Wherein a and b are constants to be determined, and the calibration step of S01 is performed according to the measured value A and the reasonable value A0Is determined, CO2Is the oxygen concentration.
In this embodiment, specific determination methods of the constants a and b include:
measuring zero index gas without oxygen, the measured value is reasonable value A0；
Measuring the first and second standard gases containing different concentrations of oxygen to obtain the measured values A of at least two tests1、A2(ii) a Wherein the oxygen concentration of the first standard gas is C1Corresponding measured value is A1(ii) a The oxygen concentration of the second standard gas is C2Corresponding measured value is A2。
Measuring the results of the first standard gas and the second standard gas and the reasonable value A0Respectively substituted into the correction function (2), an equation set can be established:
because A is0、A1、A2、C1、C2It is known that the values of a and b and hence the correction function can be determined from the system of linear equations with two elements (a and b).
After the determination of the correction function is completed, performing:
and S02, measuring the sample to obtain a measured value A of the sample.
S03 correction step, based on the oxygen concentration C in the sampleO2And S01 calibrating the correction relationship provided in the step of S02 to correct the measured value A of the sample obtained in the step of S02.
Measuring the measured value A of the sample and the concentration C of oxygen in the sampleO2The correction result A' can be obtained by substituting the determined correction function (2) of each constant, and the interference of oxygen to the measurement result can be effectively eliminated or reduced.
The embodiment also provides a GC-FID device which has a mode for carrying out flame ionization detection on a sample containing oxygen, and when the GC-FID device operates in the mode, the GC-FID device carries out correction operation by using the method provided by the embodiment, so that the measurement accuracy of the GC-FID is improved, and the deviation of the measurement result caused by the oxygen is corrected. Specifically, the GC-FID device is used for determining the content of non-methane total hydrocarbons in a sample, and comprises the following components:
the calibration unit is used for providing a correction relation established according to the measured values and reasonable values of a plurality of standard gases containing different oxygen concentrations, wherein the reasonable values are the measured values of the standard gases containing no oxygen;
the measuring unit is used for measuring the sample to obtain a measured value;
and the correction unit is used for correcting the measured value obtained in the measurement step according to the oxygen concentration in the sample and the correction relation provided in the calibration step.
Although the measurement result is corrected in the reciprocal form of the quadratic function in the present embodiment, the result may be corrected in any other nonlinear function form in other embodiments of the present invention, for example, an elementary function such as a logarithmic function, an exponential function, a power function, a trigonometric function, an inverse trigonometric function, or a polynomial function, or a function obtained by performing a finite rational operation or a finite function composition on the above functions. Accordingly, the number of constants to be determined differs depending on the correction function, for example, if the correction function is established based on the reciprocal form of the cubic equation, the number of constants to be determined is three, and the number of standard gases to be measured is usually four bottles or more; if the correction function is established based on the reciprocal form of the polynomial (n-th order equation), the number of constants to be determined is n, and the number of standard gases to be measured is usually n +1 bottles or more.
In the present embodiment, the method of correcting the flame ionization detection is described by taking the gas chromatography-flame ionization detector combination as an example, but the apparatus or system to which the method can be applied is not limited to this. In other embodiments, the method provided in the embodiments can be used to correct the situation where oxygen interferes with the detection result of flame ionization, such as a combination of the flame ionization detection device and other devices, or a device that uses the flame ionization detection device alone for measurement.
Second embodiment
The present embodiment provides a method for flame ionization detection of a sample containing oxygen, which is different from the method provided in the first embodiment in that a reasonable value a is not directly obtained by measurement in the calibration step in the present embodiment0To determine a correction function, which manner of determination should also be considered as an equivalent alternative to the embodiments of the present invention.
In the present embodiment, the correction function is calculated using the principle that the rational values corresponding to the standard gases having the same composition and concentration are equal. In the present embodiment, the calculation of the correction function depends on the measurement for three or more bottles of standard gas, each of which contains oxygen but has a different concentration.
In the calibration step of S01, the oxygen concentration for three bottles is respectively C1、C2、C3The non-methane total hydrocarbon is measured by the standard gas with the same component and concentration (such as alkane gas with the same component and concentration), and the measurement results (such as VOC area value or NMHC concentration value) of the three bottles of standard gas are respectively A1、A2、A3。
According to the measurement results, although the sample gas concentrations of the three bottles of standard gas are different, the target sample gas components and concentrations are the same, so although the measurement results of the three bottles of standard gas are different, the corrected reasonable values should be the same. Based on the above principle, the oxygen concentrations and the measurement results of different sample gases can be respectively substituted into the correction functions, and the equivalence relations of the correction functions are established and combined according to the condition of reasonable value equality, that is to say
By operating this equation set (5), constants a and b can be solved, and a correction function can be established.
The correction method provided above can calculate the correction function to reflect the deviation of the measurement result caused by the oxygen concentration without making or using the oxygen-free standard gas.
In some embodiments, the constants a, b may be compiled by manually entering the constants at the user interface of the GC-FID, calculated by manually entering the measurements and/or oxygen concentrations at the user interface of the GC-FID, and calculated by automatically obtaining the measurements and/or oxygen concentrations using a communication link with the detector and a communication link with the oxygen sensor. After the constants a and b are determined, the determined constants a and b or the correction function are written into the measurement program of the GC-FID and stored, so that the corrected measurement result, i.e. the correction value a', is fed back to the user in the subsequent test process.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (11)
1. A method of performing flame ionization measurements on a sample containing oxygen for determining the concentration of one or more gases to be measured in the sample, comprising the steps of:
a calibration step of providing a correction relationship established between a measured value obtained by using a plurality of standard gases containing different oxygen concentrations and a reasonable value, wherein the reasonable value is the measured value obtained by using the standard gas containing no oxygen;
a measuring step of measuring the sample to obtain a measured value of the sample;
and a correction step of correcting the measured value of the sample obtained in the measurement step according to the oxygen concentration in the sample and the correction relation provided in the calibration step.
2. The method for flame ionization detection of an oxygen containing sample as claimed in claim 1, wherein the type of gas to be detected in the standard gas used in the calibration step is the same as the type of gas to be detected in the sample.
3. The method for flame ionization detection of a sample containing oxygen of claim 2, wherein the concentration of the gas component to be detected in the standard gas used in the calibration step is the same as the concentration of the gas component to be detected in the sample.
4. The method of claim 1, wherein the correction relationship is a correction function that varies non-linearly with oxygen concentration.
5. The method of claim 4, wherein the correction function is a function of flame ionization detection of the sample containing oxygen
Wherein A' is a correction value, A is a measured value of the sample, a1、a2、…、anConstants, C, determined for the calibration step based on measured values and rational values obtained using a plurality of calibration gases containing different oxygen concentrationsO2Is the oxygen concentration and n is an integer.
6. The method of claim 5, wherein the correction function is a function of flame ionization detection of the sample containing oxygen
Wherein a and b are constants determined according to measured values and reasonable values obtained by using a plurality of standard gases with different oxygen concentrations in the calibration step, CO2Is the oxygen concentration.
7. The method for flame ionization detection of oxygen-containing samples according to claim 6, wherein in the calibration step, the values of a and b are determined using an oxygen-free standard gas and two or more bottles of standard gases having different oxygen concentrations.
8. The method for flame ionization detection of a sample containing oxygen of claim 1, further comprising the steps of:
measuring the oxygen concentration in the sample in real time or periodically with an oxygen measurement device.
9. The method for flame ionization detection of a sample containing oxygen of claim 1, wherein the method is performed using an instrument that combines gas chromatography with a flame ionization detector.
10. The method for flame ionization detection of a sample containing oxygen of claim 1, wherein the gas to be detected is non-methane total hydrocarbons in the sample.
11. An apparatus for performing flame ionization testing on an oxygen-containing sample to determine the concentration of one or more gases under test in the sample, comprising:
a calibration unit for providing a correction relationship established based on measured values obtained using a plurality of standard gases containing different oxygen concentrations and a reasonable value, wherein the reasonable value is the measured value obtained using the standard gas containing no oxygen;
the measuring unit is used for measuring the sample to obtain a measured value;
and the correction unit is used for correcting the measured value of the sample obtained by the measurement unit according to the oxygen concentration in the sample and the correction relation provided by the calibration unit.
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| CN114397395A (en) * | 2021-12-31 | 2022-04-26 | 杭州春来科技有限公司 | Oxygen interference correction method and system based on FID detector for non-methane total hydrocarbon determination |
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| Publication number | Publication date |
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| JP7380480B2 (en) | 2023-11-15 |
| CN112903879B (en) | 2024-06-07 |
| JP2021089268A (en) | 2021-06-10 |
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