CN114199810A - Method for analyzing hydrogen chloride in nitrogen by using standard curve method - Google Patents
Method for analyzing hydrogen chloride in nitrogen by using standard curve method Download PDFInfo
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- CN114199810A CN114199810A CN202111521756.7A CN202111521756A CN114199810A CN 114199810 A CN114199810 A CN 114199810A CN 202111521756 A CN202111521756 A CN 202111521756A CN 114199810 A CN114199810 A CN 114199810A
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910000041 hydrogen chloride Inorganic materials 0.000 title claims abstract description 37
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 11
- 238000002835 absorbance Methods 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims description 10
- 238000005259 measurement Methods 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- 238000011088 calibration curve Methods 0.000 claims description 2
- 238000012417 linear regression Methods 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000012886 linear function Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
- G01N2021/3509—Correlation method, e.g. one beam alternating in correlator/sample field
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a method for analyzing hydrogen chloride in nitrogen by using a standard curve method, which is characterized by comprising the following steps of: and fitting the data of a plurality of gradient hydrogen chloride samples by using a correlation equation and taking the concentration of the hydrogen chloride samples as a Y axis and the absorbance corresponding to the concentration of the hydrogen chloride samples as an X axis to obtain a standard curve, wherein when the concentration of the hydrogen chloride samples is in a concentration range of 10-60ppm, 3-4 sample standard points are taken in the range, and when the concentration of the hydrogen chloride samples exceeds a concentration limit of 60ppm, sample standard points are taken at the concentration interval of 40-50 ppm. The method measures the concentration of the hydrogen chloride in the nitrogen more accurately and quickly by a linear regression method.
Description
Technical Field
The invention relates to the field of hydrogen chloride analysis, in particular to a method for analyzing hydrogen chloride in nitrogen by using a standard curve method.
Background
Hydrogen chloride is a very active corrosive gas, is easily adsorbed on the metal surface, and is easily influenced by moisture in the environment. When analyzing hydrogen chloride, the standard of each concentration is not linear, and the sample is difficult to be quantified, so that a relatively accurate method is needed for analyzing and quantifying.
Disclosure of Invention
In order to overcome the above-mentioned drawbacks of the prior art, it is an object of the present invention to provide a method for analyzing hydrogen chloride in nitrogen using a standard curve method. The accuracy of the analysis result is improved by overcoming the defect of difficult sample value determination.
A method for analyzing hydrogen chloride in nitrogen using a standard curve method, comprising:
fitting the data of the plurality of gradient hydrogen chloride samples by using a correlation equation and taking the concentration of the hydrogen chloride samples as an axis Y and the absorbance corresponding to the concentration of the hydrogen chloride samples as an axis X to obtain a standard curve;
wherein,
when the concentration of the hydrogen chloride sample is in a concentration range of 10-60ppm, taking 3-4 sample standard points in the range, and when the concentration of the hydrogen chloride sample exceeds a concentration limit of 60ppm, taking the sample standard points at intervals of 40-50 ppm.
In a preferred embodiment of the present invention, the detection lower limit concentration may be 7ppm, or may be adjusted according to actual needs.
In a preferred embodiment of the invention, a single sample standard point is measured 4-5 times repeatedly.
In a preferred embodiment of the invention, the number of times of rinsing the gas cell before the measurement is not less than three, and the sampling is performed by adopting a dynamic sample injection method.
In a preferred embodiment of the invention, the concentration of the sample to be tested does not exceed 50% of the maximum sample standard point concentration.
The invention has the beneficial effects that:
the method measures the concentration of the hydrogen chloride in the nitrogen more accurately and quickly by a linear regression method.
Drawings
FIG. 1 is a linear regression equation diagram of an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings and examples. It should be understood, however, that the description herein of specific embodiments is only intended to illustrate the invention and not to limit the scope of the invention. Moreover, in the following structures, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "top/bottom", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description. And are not intended to indicate or imply that the device or element so referred to must have a particular orientation, be constructed and operated in a particular orientation and, therefore, should not be taken to be limiting of the invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
The analytical principle of the invention is as follows:
when the concentration of a substance is analyzed by fourier infrared analysis, the substance is generally expressed as a ═ abc, where a is absorbance, a is the absorption coefficient, b is the optical path length, and c is the sample concentration. It can be seen from this equation that a is a constant for one of the substances a and b, a is a linear function of c, but in the actual analysis the absorbance and the true concentration have deviated from this function model because of the adsorbability of hydrogen chloride itself.
Therefore, a standard curve is drawn through a series of standard points, the concentration of the sample is taken as the Y axis, the absorbance corresponding to the concentration is taken as the X axis, and the data of a plurality of gradient hydrogen chloride samples are fitted to obtain the standard curve. The function of the curve is calculated by computer software, the concentration is calculated by the function when the sample is analyzed, and the curve needs to be updated frequently to improve the accuracy.
The instrument used by the invention is a Fourier infrared analyzer, and is provided with various types of gas cells, and metal elements in the gas cells are subjected to corrosion resistance treatment. Gas was injected using dynamic injection method from 201811602174. X.
1. Determination of detection lower limit: the lower limit of detection reflects the lower limit at which the instrument can analyze the concentration under certain conditions, which cannot be determined by actual measurement only by deduction or is given by the instrument supplier. The formula given by the gas cell supplier for example in my company apparatus, the absorbance at 2945.2cm-1 of the wave speed of the standard hydrogen chloride in nitrogen gas with a concentration of 100ppm at 10 meters optical path is 0.1400A, and the lower detection limit concentration under this condition is 0.01 x 100/0.1400 x 7 ppm.
However, the concentrations are not generally included in the plotted data, although this point data needs to be taken into account when the measured concentration is near the lower concentration limit.
2, how to select the standard point of the sample is very important, because the hydrogen chloride is a gas sample, and compared with a solid or liquid sample, the difficulty of selecting the standard point is very large, and the inventor of the invention finds that a good standard curve can be obtained based on the following standard point selection based on multiple experiments:
when the concentration of the hydrogen chloride sample is in the concentration range of 10-60ppm, 3-4 sample standard points are taken in the range, because the slope change of the curve in the range of 10-60ppm is large when the hydrogen chloride standard curve is drawn, and 3-4 points need to be taken;
when the concentration of the hydrogen chloride sample exceeds the concentration limit of 60ppm, the concentration at the interval of 40-50ppm is taken as a sample standard point, because the slope of the curve is smaller as the concentration increases, and a point can be taken at the interval of 40-50 ppm. As shown in fig. 1 (in the figure, the equation is that Y is 3E-05X2+0.0262X+6.9294,R2＝0.9998)。
3. Measurement of sample standard points: and measuring the absorbance of the sample standard point from low to high according to the standard concentration gradient, repeating the measurement of each point for 4-5 times, rinsing the gas pool for more than 3 times before each measurement, and injecting the sample by using a dynamic sample injection method. The plotted curve was fitted with a 2-fold equation.
4. Use of standard curve: the concentration of the sample can be obtained by directly substituting the absorbance of the sample into a fitting formula, and the absorbance of the sample is required to fall within the curve range. When the sample concentration approaches the lower detection limit, the lower detection limit can be regarded as the point where the Y-axis intercept is temporarily added to the curve, and the sample is calculated after the curve is obtained again.
This curve does not apply when the sample concentration is 50% greater than the maximum standard point concentration. Because of the reactive nature of hydrogen chloride, the calibration curve needs to be updated at least once per week.
The sampling method can reduce the sampling times required by point making, so that the data of a single point is faster and more stable, and the traditional curve drawing needs the single point sampling more than 5 times and needs intensive point fetching to be stable. There is a large consumption of standard and sample gases.
Claims (4)
1. A method for analyzing hydrogen chloride in nitrogen by using a standard curve method, which is characterized by comprising the following steps:
fitting the data of the plurality of gradient hydrogen chloride samples by using a correlation equation and taking the concentration of the hydrogen chloride samples as an axis Y and the absorbance corresponding to the concentration of the hydrogen chloride samples as an axis X to obtain a standard curve;
wherein,
when the concentration of the hydrogen chloride sample is in a concentration range of 10-60ppm, taking 3-4 sample standard points in the range, and when the concentration of the hydrogen chloride sample exceeds a concentration limit of 60ppm, taking the sample standard points at intervals of 40-50 ppm.
2. The method for analyzing hydrogen chloride in nitrogen using the calibration curve method as set forth in claim 1, wherein the single sample calibration point is repeatedly measured 4 to 5 times.
3. The method for analyzing hydrogen chloride in nitrogen by using the standard curve method as claimed in claim 1, wherein the number of times of rinsing the gas cell before the measurement is not less than three times, and the sampling is performed by using a dynamic sample injection method.
4. The method of claim 1, wherein the concentration of the sample to be measured does not exceed 50% of the maximum sample standard point concentration.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111521756.7A CN114199810A (en) | 2021-12-13 | 2021-12-13 | Method for analyzing hydrogen chloride in nitrogen by using standard curve method |
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| CN202111521756.7A CN114199810A (en) | 2021-12-13 | 2021-12-13 | Method for analyzing hydrogen chloride in nitrogen by using standard curve method |
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| CN114199810A true CN114199810A (en) | 2022-03-18 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114441477A (en) * | 2022-04-11 | 2022-05-06 | 华电智控（北京）技术有限公司 | Method and device for detecting concentration of gas based on wide absorption spectrum line |
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| US20020139934A1 (en) * | 2001-03-30 | 2002-10-03 | Shih-Yi Chang | Multi-component gas analyzer having cassette-type light path system |
| TW200615531A (en) * | 2004-08-25 | 2006-05-16 | Environmental Syst Prod | System and method for calibrating remote emissions sensing instruments |
| CN104730021A (en) * | 2013-12-24 | 2015-06-24 | 北京万联达信科仪器有限公司 | Method for calibrating non-dispersive infrared gas sensor |
| WO2019172584A1 (en) * | 2018-03-05 | 2019-09-12 | 건국대학교 산학협력단 | Gas analyzer using hitran data and multi-filter, and gas analyzing method |
| CN111837025A (en) * | 2018-03-12 | 2020-10-27 | 关东电化工业株式会社 | Gas analysis method and apparatus |
-
2021
- 2021-12-13 CN CN202111521756.7A patent/CN114199810A/en not_active Withdrawn
Patent Citations (5)
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| US20020139934A1 (en) * | 2001-03-30 | 2002-10-03 | Shih-Yi Chang | Multi-component gas analyzer having cassette-type light path system |
| TW200615531A (en) * | 2004-08-25 | 2006-05-16 | Environmental Syst Prod | System and method for calibrating remote emissions sensing instruments |
| CN104730021A (en) * | 2013-12-24 | 2015-06-24 | 北京万联达信科仪器有限公司 | Method for calibrating non-dispersive infrared gas sensor |
| WO2019172584A1 (en) * | 2018-03-05 | 2019-09-12 | 건국대학교 산학협력단 | Gas analyzer using hitran data and multi-filter, and gas analyzing method |
| CN111837025A (en) * | 2018-03-12 | 2020-10-27 | 关东电化工业株式会社 | Gas analysis method and apparatus |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114441477A (en) * | 2022-04-11 | 2022-05-06 | 华电智控（北京）技术有限公司 | Method and device for detecting concentration of gas based on wide absorption spectrum line |
| CN114441477B (en) * | 2022-04-11 | 2022-07-01 | 华电智控（北京）技术有限公司 | Gas concentration detection method and device based on wide absorption spectrum line |
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Application publication date: 20220318 |