CN112162056A - Method for detecting ultralow nitrogen content in petroleum product - Google Patents
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Abstract
The invention discloses a method for detecting ultralow nitrogen content in petroleum products, which comprises the following steps: 1) solvent pretreatment: adding a certain amount of silica gel into an organic solvent of petroleum, adsorbing nitrogen-containing organic matters in the organic solvent, filtering the silica gel, and removing the nitrogen-containing organic matters in the organic solvent; 2) diluting a petroleum sample: setting a corresponding dilution ratio according to the concentration of the petroleum, and diluting the petroleum sample by using the organic solvent treated in the step 1; 3) homogenizing the sample; 4) using the organic solvent treated in the step 1 as a solvent for configuring a working curve, and using analytically pure nitrogen-containing organic matters as standard substances for preparing a standard curve; 5) and (3) analyzing and determining the nitrogen content in the petroleum sample by adopting an oxidative combustion and chemiluminescence detector. The detection method provided by the invention has the advantages of lower detection limit, higher detection precision, higher detection efficiency and better linear range and correlation coefficient of the working curve of the heavy petroleum sample.
Description
Technical Field
The invention relates to the technical field of petroleum detection, in particular to a method for detecting ultralow nitrogen content in petroleum products.
Background
At present, the nitrogen content of petroleum products is generally detected by an oxidative combustion and chemiluminescence detection method in national standards. The sample is burnt at high temperature and reacts with ozone to generate excited nitrogen dioxide (NO)2And photons emitted when the excited nitrogen dioxide returns to the ground state are received by the chemiluminescence detector to generate signals, and then the total nitrogen content of the sample is obtained. When measuring the nitrogen content by using the existing instrument, argon is generally used as a carrier, and oxygen is used as an oxidant. Although high-purity argon (99.999%) and high-purity oxygen (99.999%) exist in the nitrogen which cannot be removed in the preparation process, and although the test system is a closed system, the atmosphere also has high content of nitrogen, and the trace nitrogen cannot be substantially removed in the test process, namely the detection limit of the instrument analysis is positioned. In addition, the organic solvent used for dissolving the oil sample also contains a small amount of nitrogen-containing organic matters which can reach about 1ppm, and the nitrogen-containing organic matters can generate decisive errors for the detection of the sample with ultralow nitrogen content. Therefore, how to eliminate the interference of nitrogen-containing organic matters as much as possible becomes a key for improving the accuracy of the detection of the ultra-low nitrogen in the petroleum products.
In addition, the existing detection instrument generally has the problem of poor linear range of a working curve and a correlation coefficient for the determination of the nitrogen content in a heavy oil sample, and if the heavy oil sample becomes a sample with low nitrogen content after being diluted and then is subjected to nitrogen detection, the heavy oil sample is interfered by nitrogen-containing organic matters in a solvent, so that the detection accuracy is poor, and therefore, the detection method of the heavy oil sample needs to be improved.
In the prior art, the detection limit LOD of the detection scheme of the nitrogen content in the petroleum product is about 1ppm, and if the nitrogen content of a sample is lower than 1ppm, serious detection errors can be generated.
Disclosure of Invention
The invention aims to provide a method for detecting the ultralow nitrogen content in a petroleum product, which can solve the problems that the detection limit is higher due to nitrogen-containing organic matters in an organic solvent during detection of the nitrogen content in the petroleum product in the prior art, the error is large during detection of ultralow nitrogen, the linear range and the correlation coefficient of a working curve are poorer during detection of a heavy petroleum sample, and the like.
In order to achieve the purpose, the invention is realized by the following technical scheme: the method for detecting the ultralow nitrogen content in the petroleum product is characterized by comprising the following steps: which comprises the following steps:
1) solvent pretreatment: adding a certain amount of silica gel into an organic solvent of petroleum, uniformly dispersing the silica gel in the organic solvent by stirring, adsorbing nitrogen-containing organic matters in the organic solvent by the silica gel, filtering the organic solvent, filtering out the silica gel, repeatedly adding the silica gel for a plurality of times, and removing the nitrogen-containing organic matters in the organic solvent;
2) diluting a petroleum sample: setting a corresponding dilution ratio according to the concentration of the petroleum, and diluting the petroleum sample by using the organic solvent treated in the step 1;
3) sample homogenization treatment: carrying out ultrasonic treatment on the diluted sample to fully dissolve the petroleum sample and homogenize the solution;
4) using the organic solvent treated in the step 1 as a solvent for configuring a working curve, and using analytically pure nitrogen-containing organic matters as standard substances for preparing a standard curve;
5) and (3) analyzing and determining the nitrogen content in the petroleum sample after the homogenization treatment in the step (3) by using an analytical instrument through an oxidative combustion and chemiluminescence detector.
In a further scheme, the organic solvent is benzene, toluene, m-xylene, o-xylene or p-xylene.
The further scheme is that the silica gel is 10-500 meshes. Silica gel of 10-500 meshes is selected, so that the filtering effect of nitrogen-containing organic matters in the organic solvent can be enhanced.
In a further scheme, the standard substance is N-methylcarbazole, carbazole, acridine, 8-hydroxyquinoline or pyridine.
In a further scheme, in the step 2, the light oil sample is diluted by the solvent treated in the step 1, and the dilution ratio is 1: 1-1: 100. after the light oil sample is diluted by the organic solvent processed by filtering the nitrogen-containing organic matter, error interference is not generated, and the linear range and the correlation coefficient of the detected working curve are better.
In a further scheme, in the step 2, the heavy oil sample is diluted by the solvent treated in the step 1, and the dilution ratio is 1: 100-1: 100000. heavy oil sample, after filtering the organic solvent dilution that nitrogenous organic matter was handled, detect the nitrogen content through oxidation burning and chemiluminescence detector, neither can produce error interference, can make the linear range and the correlation coefficient of the working curve who detects again better.
The further scheme is that the light oil sample and the heavy oil sample are diluted and then detected under the same working curve. The detection is carried out through the same working curve, so that the detection efficiency and the detection accuracy are higher.
In step 5, the process of analyzing and measuring the nitrogen content in the petroleum sample homogenized in step 3 by an oxidative combustion and chemiluminescence detector is as follows: 5.1) injecting the petroleum sample into a gasification chamber, and gasifying the petroleum sample under the action of high temperature in the gasification chamber; 5.2) taking argon as carrier gas, inputting the gasified petroleum sample into a combustion chamber, inputting oxygen into the combustion chamber, and reacting nitrogen-containing organic matters in the petroleum sample with the oxygen to generate nitric oxide; 5.3) reacting the combusted gas with ozone to generate excited nitrogen dioxide; and 5.4) emitting photons from the excited nitrogen dioxide to return to the ground state, and receiving the photons by a chemiluminescence detector to obtain the nitrogen content in the petroleum sample.
Further, the gas burned in step 5.2 is passed through a membrane dryer to remove moisture. Moisture is removed through the membrane type drying tube, and the interference of the moisture on detection can be avoided.
In a further embodiment, a particulate filter is used to remove particulate matter from the gaseous sample by the combusted gases of step 5.2. The removal of the particles by the particle filter can avoid the interference of the particles with the equipment.
The invention has the beneficial effects that: 1) according to the method for detecting the ultralow nitrogen content in the petroleum product, the organic solvent for diluting the petroleum sample is treated, the silica gel is used for adsorbing nitrogen-containing organic matters in the organic solvent, and then the silica gel is filtered out, so that the nitrogen-containing organic matters in the organic solvent are removed, errors generated when the organic solvent dilutes the petroleum sample are eliminated, and the detection limit is greatly reduced, in a blank experiment, the nitrogen content can be reduced to be below 0.02ppm, which means that the detection method has better detection capability and lower detection limit compared with the prior art for the sample with the nitrogen content of 2 ppm-0.1 ppm; 2) because the detection method removes the nitrogenous organic matters in the organic solvent, the detection precision is higher; 3) for the petroleum sample with high nitrogen content, the treated organic solvent is diluted to a proper concentration and then detected, so that the detection accuracy is not influenced, the light petroleum sample and the heavy petroleum sample can be detected and analyzed under the same working curve, the linear range and the correlation coefficient of the working curve are better, and the detection efficiency can be greatly improved.
Drawings
FIG. 1 is a flow chart of the detection according to the present invention.
FIG. 2 is a schematic diagram of the structure of the oxidative combustion and chemiluminescence detector.
Fig. 3 is a graph of the operation of the present invention.
Fig. 4 is a prior art operating curve.
In the figure, the direction of the arrow is the direction of conveyance of the air flow.
Detailed Description
The technical solutions of the present invention are described clearly and completely by the following embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A method for detecting the content of ultra-low nitrogen in petroleum products, as shown in fig. 1 and 2, comprising the following steps:
1) solvent pretreatment: adding a certain amount of silica gel into chromatographic grade toluene, uniformly dispersing the silica gel in an organic solvent by stirring, adsorbing nitrogen-containing organic matters in the organic solvent by the silica gel, filtering the organic solvent, filtering out the silica gel, repeatedly adding the silica gel for a plurality of times, and removing the nitrogen-containing organic matters in the organic solvent, wherein the silica gel is 10-mesh silica gel powder;
2) diluting a petroleum sample: and (3) diluting the light oil sample by using the chromatographic grade toluene treated in the step (1), wherein the dilution ratio is 1: 100, respectively;
3) sample homogenization treatment: carrying out ultrasonic treatment on the diluted sample to fully dissolve the petroleum sample and homogenize the solution;
4) using the chromatographic grade toluene treated in the step 1 as a solvent for configuring a working curve, and using analytically pure (> 99.0%) N-methyl carbazole as a standard substance for preparing a standard curve;
5) adopting an oxidative combustion and chemiluminescence detector to analyze and measure the nitrogen content in the petroleum sample after the homogenization treatment in the step 3, and specifically comprising the following steps:
5.1) injecting the petroleum sample into a gasification chamber, and gasifying the petroleum sample under the action of high temperature in the gasification chamber, wherein the temperature of the gasification chamber is 500 ℃;
5.2) taking argon as carrier gas, setting the flow rate of the argon at 100mL/min, inputting a gasified petroleum sample into a combustion chamber, setting the temperature of the combustion chamber at 1000 ℃, inputting oxygen into the combustion chamber, setting the flow rate of the oxygen at 300mL/min, setting the flow rate of compensated oxygen at 100mL/min, reacting nitrogenous organic matters in the petroleum sample with the oxygen to generate nitric oxide, removing water vapor generated after the sample is combusted by using a membrane type drying tube, and removing particles in a gaseous sample by using a particle filter;
5.3) taking air as carrier gas, wherein the air carrier gas flow rate is 300mL/min, reacting the combusted gas with ozone, providing ozone through an ozone generator, enabling the oxygen of the ozone generator to enter the ozone generator at the flow rate of 50mL/min, enabling the flow rate of the generated ozone to be 50mL/min, and enabling nitric oxide to react with the ozone to generate excited nitrogen dioxide (NO 2);
5.4) the excited nitrogen dioxide emits photons to return to the ground state, the chemiluminescence detector receives the photons to obtain the nitrogen content in the petroleum sample, the temperature of the chemiluminescence detector is set to be 50 ℃, and the cooling temperature is-3 ℃.
The organic solvent used in the above scheme is chromatographic grade toluene, but in specific implementation, other organic solvents such as toluene, m-xylene, o-xylene or p-xylene can be selected.
In the scheme, analytically pure N-methyl carbazole is selected as the standard substance, but other nitrogen-containing organic substances which can be completely combusted in an air environment at 500 ℃ can be used as the standard substance, and the commonly used standard substances also include carbazole, acridine, 8-hydroxyquinoline or pyridine.
In the scheme, argon is selected as the carrier gas, and other inert gases can be used for substitution during specific implementation.
The temperature of the gasification chamber in the scheme can be set to be 400-600 ℃; the flow rate of the carrier gas argon is 50-150 mL/min; the temperature of the combustion chamber is 900-1200 ℃; the flow rate of the input oxygen in the combustion chamber is 200-400 mL/min, and the flow rate of the compensation oxygen is 50-150 mL/min; the air carrying flow rate is 200-400 mL/min; the flow rate of the oxygen entering the ozone generator is 10-100 mL/min, and the flow rate of the generated ozone is 10-100 mL/min; the temperature of the chemiluminescence detector is set to be 30-60 ℃, and the cooling temperature is 0-minus 10 ℃.
Example 2
On the basis of example 1, unlike example 1, the silica gel powder was a 100-mesh silica gel powder, and the dilution ratio of the light oil sample was 1: 1.
example 3
On the basis of example 1, the silica gel powder is 300-mesh silica gel powder, and the dilution ratio of the light oil sample is 1: 90.
example 4
On the basis of the embodiment 1, different from the embodiment 1, the silica gel powder is 500-mesh silica gel powder, the oil sample is a heavy oil sample, and the dilution ratio is 1: 100.
example 5
In example 4, unlike example 4, the silica gel powder was 400 mesh silica gel powder, and the dilution ratio of the heavy oil sample was 1: 2000.
example 6
In example 4, unlike example 4, the silica gel powder was a 100-mesh silica gel powder, and the dilution ratio of the heavy oil sample was 1: 20000.
example 7
In example 4, unlike example 4, the silica gel powder was a 100-mesh silica gel powder, and the dilution ratio of the heavy oil sample was 1: 100000.
the detection method of the invention is compared with the prior art by two comparative experiments as follows:
comparative analysis example 1
According to the method of the steps 1 to 3 in the previous embodiment, the petroleum sample is diluted by the organic solvent treated by the silica gel, and the petroleum samples with different concentration points are prepared, wherein the specific concentrations are 0.1ppm, 0.2ppm, 0.5ppm, 1ppm and 2ppm, and the concentration of the chromatographic grade toluene cleaned by the silica gel is 0 ppm. The nitrogen content of the petroleum samples at the different concentration points is detected by the schemes of steps 4 and 5 of example 1. The response (peak area) of photons emitted from excited nitrogen dioxide (NO 2) generated by different concentrations of the solution to the signal of the chemiluminescence detector was plotted to obtain a working curve.
The relevant detection data of the working curve of the invention are as follows:
in the above table, RSD is the relative standard deviation, R2The correlation coefficient of nitrogen content and LOD are detection limits.
The working curve is shown in figure 3.
Using chromatographic grade toluene without silica gel treatment to dilute the same petroleum sample to prepare a petroleum sample with the same concentration, using the concentration of the chromatographic grade toluene without silica gel treatment as 0ppm, adopting the scheme of steps 3-5 in example 1 to detect the nitrogen content, and drawing the response (peak area) of photons emitted by excited nitrogen dioxide (NO 2) generated by solutions with different concentrations to the signal of a chemiluminescence detector to obtain a working curve.
The relevant test data for the prior art working curve is as follows:
the working curve is shown in figure 4.
As can be seen from the above comparison, the scheme of the invention has the nitrogen content correlation coefficient R2Compared with the prior art, the detection method has the advantages that the detection precision and the correlation coefficient are higher, the linear range is larger, the detection limit is lower, and the detection precision and the detection efficiency of ultralow nitrogen content in petroleum products can be obviously improved.
Comparative analysis example 2
The following table shows the results of the relative recovery rate and the repeatability detection of the nitrogen content in the petroleum product by the detection method of the invention:
as can be seen from the table above, the method of the invention has lower relative standard deviation RSD of the detection result, and the relative recovery rate shows that the accuracy of the detection test is very high and the relative recovery rate is close to 100%.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A method for detecting the content of ultralow nitrogen in petroleum products is characterized by comprising the following steps:
1) solvent pretreatment: adding a certain amount of silica gel into an organic solvent of petroleum, uniformly dispersing the silica gel in the organic solvent by stirring, adsorbing nitrogen-containing organic matters in the organic solvent by the silica gel, filtering the organic solvent, filtering out the silica gel, repeatedly adding the silica gel for a plurality of times, and removing the nitrogen-containing organic matters in the organic solvent;
2) diluting a petroleum sample: setting a corresponding dilution ratio according to the concentration of the petroleum, and diluting the petroleum sample by using the organic solvent treated in the step 1;
3) sample homogenization treatment: carrying out ultrasonic treatment on the diluted sample to fully dissolve the petroleum sample and homogenize the solution;
4) using the organic solvent treated in the step 1 as a solvent for configuring a working curve, and using analytically pure nitrogen-containing organic matters as standard substances for preparing a standard curve;
5) and (3) analyzing and determining the nitrogen content in the petroleum sample after the homogenization treatment in the step (3) by using an analytical instrument through an oxidative combustion and chemiluminescence detector.
2. The method for detecting the content of ultra-low nitrogen in petroleum products according to claim 1, characterized in that: the organic solvent is benzene, toluene, m-xylene, o-xylene or p-xylene.
3. The method for detecting the content of ultra-low nitrogen in petroleum products according to claim 1, characterized in that: the silica gel is 10-500 meshes.
4. The method for detecting the content of ultra-low nitrogen in petroleum products according to claim 1, characterized in that: the standard substance is N-methylcarbazole, carbazole, acridine, 8-hydroxyquinoline or pyridine.
5. The method for detecting the content of ultra-low nitrogen in petroleum products according to claim 1, characterized in that: in step 2, the light oil sample is diluted by the solvent treated in step 1, and the dilution ratio is 1: 1-1: 100.
6. the method for detecting the content of ultra-low nitrogen in petroleum products according to claim 1, characterized in that: in step 2, the heavy oil sample is diluted by the solvent treated in step 1, and the dilution ratio is 1: 100-1: 100000.
7. the method for detecting the content of ultra-low nitrogen in petroleum products according to claim 1, characterized in that: and (3) diluting the light oil sample and the heavy oil sample, and detecting under the same working curve.
8. The method for detecting the content of ultra-low nitrogen in petroleum products according to claim 1, characterized in that: in step 5, the process of analyzing and determining the nitrogen content in the petroleum sample after the homogenization treatment in step 3 by using an oxidative combustion and chemiluminescence detector is as follows: 5.1) injecting the petroleum sample into a gasification chamber, and gasifying the petroleum sample under the action of high temperature in the gasification chamber; 5.2) taking argon as carrier gas, inputting the gasified petroleum sample into a combustion chamber, inputting oxygen into the combustion chamber, and reacting nitrogen-containing organic matters in the petroleum sample with the oxygen to generate nitric oxide; 5.3) reacting the combusted gas with ozone to generate excited nitrogen dioxide; and 5.4) emitting photons from the excited nitrogen dioxide to return to the ground state, and receiving the photons by a chemiluminescence detector to obtain the nitrogen content in the petroleum sample.
9. The method for detecting the content of ultra-low nitrogen in petroleum products according to claim 7, characterized in that: the gas after combustion in step 5.2 is passed through a membrane dryer to remove moisture.
10. The method for detecting the content of ultra-low nitrogen in petroleum products according to claim 1, characterized in that: particulate matter in the gaseous sample is removed by the combusted gas of step 5.2 using a particulate filter.
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