CN114994235A - Application of oxygen bomb combustion method in determination of palladium-carbon-chlorine content and determination method - Google Patents
Application of oxygen bomb combustion method in determination of palladium-carbon-chlorine content and determination method Download PDFInfo
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Abstract
The invention belongs to the technical field of analysis and detection, and discloses an application of an oxygen bomb combustion method in determination of palladium-carbon-chlorine content and a determination method. Mixing a palladium-carbon test material and a combustion improver, placing the mixture into a sample cup, adding an absorption liquid into an oxygen bomb, and sealing the oxygen bomb; oxygenating the oxygen bomb, and igniting for combustion; after the sintering is finished, the oxygen bomb is subjected to ultrasonic treatment and then is connected with a gas absorption device containing absorption liquid, and gas in the oxygen bomb is discharged; after the gas is discharged, opening the oxygen bomb, mixing absorption liquid in the oxygen bomb and absorption liquid in the gas absorption device, and diluting with water to obtain liquid to be detected; after the solution to be measured was filtered, the chlorine content was measured by using an ion chromatograph. The invention uses the absorption liquid to replace sulfuric acid to obtain a sample solution which can be directly used for subsequent IC detection, and compared with a sulfuric acid distillation method, the method does not use acid and improves the sensitivity of the method. The method is simple, convenient and quick, has good accuracy and repeatability, and is suitable for analyzing and determining the chlorine content in the palladium-carbon catalyst sample.
Description
Technical Field
The invention relates to the technical field of analysis and detection, in particular to application of an oxygen bomb combustion method in determination of palladium-carbon-chlorine content and a determination method.
Background
Palladium carbon is a catalyst, is prepared by loading metal palladium powder on active carbon, and mainly plays a role in catalytic hydrogenation of unsaturated hydrocarbon or CO. Widely used in the hydrogenation reduction refining process of petrochemical industry, pharmaceutical industry, electronic industry, perfume industry, dye industry and other fine chemical industry. With the rapid development of science and technology and economy in recent years, the demand of palladium-carbon catalysts in various application fields is increasing.
The palladium carbon catalyst is prepared by processing palladium chloride serving as a raw material, so that chlorine element residue is inevitably generated in the palladium carbon. Chlorine has an important influence on the catalytic performance of palladium-carbon and also has a corrosive effect on a reaction device. At present, the market circulation of palladium carbon is huge, and the chlorine content is used as an important index of the quality of palladium carbon products and plays a crucial role in the quality of the products. At present, relevant analysis methods exist for determining metal impurity elements in palladium-carbon, but the research on the determination method of chlorine elements in palladium-carbon is less.
Common pretreatment methods for chlorine determination include the use of sulfuric acid for distillation escape, requiring the use of large amounts of sulfuric acid; when the mercury titration method and the silver nitrate titration method are used for measuring the chlorine element, the indicator is used for changing color to be used as a titration end point, and the error of manual judgment is large.
Therefore, how to accurately and efficiently measure the chlorine content in the palladium-carbon plays an important role in the wide application of the palladium-carbon catalyst.
Disclosure of Invention
The invention aims to provide an application of an oxygen bomb combustion method in determination of palladium-carbon chlorine content and a determination method, which solve the defect of the determination method of the chlorine content in the palladium-carbon and can accurately determine the chlorine content of the palladium-carbon.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides an application of an oxygen bomb combustion method in determination of palladium-carbon chlorine content.
The invention also provides a method for measuring the content of palladium-carbon chloride by an oxygen bomb combustion method, which comprises the following steps of:
(1) mixing a palladium-carbon test material and a combustion improver, placing the mixture into a sample cup, adding an absorption liquid into an oxygen bomb, and sealing the oxygen bomb;
(2) oxygenating the oxygen bomb, and igniting for combustion;
(3) after the sintering is finished, the oxygen bomb is subjected to ultrasonic treatment and then is connected with a gas absorption device containing absorption liquid, and gas in the oxygen bomb is discharged;
(4) after the gas is discharged, opening the oxygen bomb, mixing absorption liquid in the oxygen bomb and absorption liquid in the gas absorption device, and diluting with water to obtain liquid to be detected;
(5) after the solution to be measured was filtered, the chlorine content was measured by using an ion chromatograph.
Preferably, in the method for measuring the palladium-carbon chlorine content by the oxygen bomb combustion method, the combustion improver in the step (1) is methanol, ethanol, ethylene glycol or glycerol; the mass ratio of the combustion improver to the palladium-carbon sample is 0.5-1.5: 0.1.
preferably, in the method for measuring the palladium-carbon chlorine content by the bomb combustion method, the volume-to-mass ratio of the absorption liquid to the palladium-carbon sample in the step (1) is 10 to 40 mL: 0.1 g.
Preferably, in the method for measuring the palladium-carbon chlorine content by the bomb combustion method, the absorption liquid in the step (1) and the absorption liquid in the step (3) are independently a solution containing sodium carbonate and sodium bicarbonate; the concentration of the sodium carbonate is independently 3-3.5 mmol/L; the concentration of sodium bicarbonate is independently 0.5-1.5 mmol/L.
Preferably, in the method for measuring the palladium-carbon-chlorine content by the oxygen bomb combustion method, the ultrasonic time in the step (3) is 30-40 min.
Preferably, in the method for measuring the palladium-carbon chlorine content by the bomb combustion method, the filtering in the step (5) is filtering by using a polyvinylidene fluoride microporous filter membrane.
Preferably, in the method for measuring the palladium-carbon chlorine content by the bomb combustion method, the method for measuring the chlorine content by using an ion chromatograph in the step (5) comprises the following steps:
a. preparing a series of standard solutions: diluting the chlorine standard solution to obtain a series of chlorine standard solutions;
b. drawing a standard working curve: carrying out quantitative analysis on the series of chlorine standard solutions by using an ion chromatograph to obtain a standard working curve;
c. sample detection: and c, under the same quantitative analysis condition as the step b, measuring the peak areas of the chlorine element in the solution to be detected and the blank solution, and calculating according to a standard working curve to obtain the chlorine content.
Preferably, in the method for measuring the chlorine content of the palladium-carbon by the oxygen bomb combustion method, the concentrations of the series of chlorine standard solutions in the step a are 0.5mg/L, 1mg/L, 2mg/L, 5mg/L and 10 mg/L.
Preferably, in the method for determining the palladium-carbon chlorine content by the bomb combustion method, in the step b, the method for obtaining the standard operating curve comprises the following steps: quantitatively analyzing the peak area of the chlorine element in the series of standard solutions of the chlorine, and establishing a standard working curve of the relationship between the peak area of the chlorine element and the concentration by using a calibration curve method.
Through the technical scheme, compared with the prior art, the invention has the following beneficial effects:
(1) the invention adopts the oxygen bomb combustion method to realize the rapid combustion of the sample, the oxygen bomb combustion method can realize the complete escape of the chlorine element in the sample within 2min at the high temperature (more than 1000 ℃) reached during the combustion, compared with the sulfuric acid distillation method, the time is greatly shortened, and the working efficiency is greatly improved.
(2) The invention uses the absorption liquid to replace sulfuric acid to obtain a sample solution which can be directly used for subsequent IC detection, and compared with a sulfuric acid distillation method, the method does not use acid and improves the sensitivity of the method.
(3) The oxygen bomb is connected with the gas absorption device, so that the escaped chlorine can be completely absorbed.
(4) According to the method, the chlorine content in the sample is detected by adopting IC, and when the chlorine element is detected by using a traditional mercury titration method and a traditional silver nitrate titration method, the indicator is used for changing color to be used as a titration end point, so that the error of manual judgment is large.
(5) The method is simple, convenient and quick, has good accuracy and repeatability, and is suitable for analyzing and determining the chlorine content in the palladium-carbon catalyst sample.
Detailed Description
The invention provides an application of an oxygen bomb combustion method in determination of palladium-carbon chlorine content.
The invention also provides a method for measuring the content of palladium-carbon chloride by an oxygen bomb combustion method, which comprises the following steps of:
(1) mixing a palladium-carbon test material and a combustion improver, placing the mixture into a sample cup, adding an absorption liquid into an oxygen bomb, and sealing the oxygen bomb;
(2) oxygenating the oxygen bomb, and igniting for combustion;
(3) after the sintering is finished, the oxygen bomb is subjected to ultrasonic treatment and then is connected with a gas absorption device containing absorption liquid, and gas in the oxygen bomb is discharged;
(4) after the gas is discharged, opening the oxygen bomb, mixing absorption liquid in the oxygen bomb and absorption liquid in the gas absorption device, and diluting with water to obtain liquid to be detected;
(5) after the solution to be measured was filtered, the chlorine content was measured by using an ion chromatograph.
In the present invention, the palladium-carbon sample in step (1) is selected from palladium-carbon produced by Xiantong catalytic new materials GmbH, Zhejiang.
In the invention, the specific method of the step (1) is as follows: putting a palladium-carbon test material into a sample cup, and adding a combustion improver; opening the oxygen bomb, taking a 9cm long ignition wire, loading the ignition wire, and enabling the ignition wire to contact the sample, wherein the ignition wire is not required to contact the crucible or the inner wall of the oxygen bomb; and adding an absorption liquid into the oxygen bomb, and screwing the oxygen bomb.
In the present invention, the combustion improver in the step (1) is preferably methanol, ethanol, ethylene glycol or glycerol, more preferably methanol, ethanol or glycerol, and more preferably ethanol; the mass ratio of the combustion improver to the palladium-carbon sample is preferably 0.5-1.5: 0.1, more preferably 0.7 to 1.3: 0.1, more preferably 0.9: 0.1.
in the present invention, the volume-to-mass ratio of the absorbing solution to the palladium-carbon sample in the step (1) is preferably 10 to 40 mL: 0.1g, more preferably 15 to 31 mL: 0.1g, more preferably 22 mL: 0.1 g.
In the present invention, the absorbing solution in the step (1) is preferably a solution containing sodium carbonate and sodium bicarbonate; the concentration of the sodium carbonate is preferably 3-3.5 mmol/L, more preferably 3.1-3.3 mmol/L, and even more preferably 3.2 mmol/L; the concentration of sodium bicarbonate is preferably 0.5 to 1.5mmol/L, more preferably 0.6 to 1.1mmol/L, and still more preferably 0.8 mmol/L.
In the invention, before oxygenating the oxygen bomb in the step (2), continuously oxygenating and discharging oxygen for 2-4 times to remove air in the oxygen bomb.
In the invention, the specific method of the step (2) is as follows: oxygenating the oxygen bomb, and stopping oxygenating when the pointer of the pressure gauge is 3-3.5 MPa; then putting the oxygen bomb into a cooling box of an ignition controller for ignition; and 5-7 s after the burning indicator light is turned off, turning off the power supply, and taking down the oxygen bomb.
In the invention, the time of the ultrasound in the step (3) is preferably 30-40 min, more preferably 32-38 min, and even more preferably 35 min.
In the present invention, the absorbing solution in the step (3) is preferably a solution containing sodium carbonate and sodium bicarbonate; the concentration of the sodium carbonate is preferably 3-3.5 mmol/L, more preferably 3.1-3.4 mmol/L, and even more preferably 3.3 mmol/L; the concentration of sodium bicarbonate is preferably 0.5 to 1.5mmol/L, more preferably 0.8 to 1.4mmol/L, and still more preferably 1.2 mmol/L.
In the invention, the solution to be detected in the step (4) further comprises a sample cup, an ignition screw rod, an inner surface of an oxygen bomb cover and a cleaning solution on the inner wall of the oxygen bomb.
In the invention, the water is used for diluting to 100-200 mL in the step (4).
In the present invention, the filtration in the step (5) is preferably performed by using a polyvinylidene fluoride microporous membrane, and a more preferred polyvinylidene fluoride microporous membrane has a pore size of 0.22 μm.
In the present invention, the method for determining the chlorine content by using an ion chromatograph in the step (5) is:
a. preparing a series of standard solutions: diluting the chlorine standard solution to obtain a series of chlorine standard solutions;
b. drawing a standard working curve: carrying out quantitative analysis on the series of chlorine standard solutions by using an ion chromatograph to obtain a standard working curve;
c. sample detection: and c, under the same quantitative analysis condition as the step b, measuring the peak areas of the chlorine element in the solution to be detected and the blank solution, and calculating according to a standard working curve to obtain the chlorine content.
In the invention, the concentration of the series of standard solutions of chlorine in the step a is 0.5mg/L, 1mg/L, 2mg/L, 5mg/L and 10 mg/L.
In the present invention, in the step b, the method for obtaining the standard working curve comprises: quantitatively analyzing the peak area of chlorine element in the series of standard solutions of chlorine, and establishing a standard working curve of the relation between the peak area of chlorine element and concentration by using a calibration curve method, wherein the correlation coefficient of the standard working curve is not less than 0.9998.
In the present invention, in the step b, the operating parameters of the ion chromatograph are:
and (3) chromatographic column: selecting anion separation column (4.0mm × 150mm) and guard column (4.0mm × 10 mm);
leacheate: a mixed solution of 3.2mmol/L sodium carbonate and 1.0mmol/L sodium bicarbonate;
a suppressor: a chemical suppressor;
flow rate of eluent: 0.7 mL/min;
sample introduction volume: 20 μ L.
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious 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 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
The embodiment provides a method for determining palladium-carbon chlorine content by an oxygen bomb combustion method, which comprises the following steps:
(1) weighing 0.1g of palladium-carbon sample A, adding the palladium-carbon sample A into an oxygen bomb sample cup with the volume of 200mL, and adding 1g of ethanol as a combustion improver; opening the oxygen bomb, taking a 9cm long ignition wire, and loading the ignition wire to enable the ignition wire to contact the sample, wherein the ignition wire is not required to contact the inner wall of the oxygen bomb; adding 25mL of a mixed solution of 3.2mmol/L sodium carbonate and 1.0mmol/L sodium bicarbonate into an oxygen bomb as an absorption liquid, and screwing the oxygen bomb;
(2) continuously charging and discharging oxygen for 3 times to remove air in the oxygen bomb, then filling oxygen, and stopping oxygen charging when the pointer of the pressure gauge is 3 MPa; putting the oxygen bomb into a cooling box of an ignition controller for ignition, turning off a power supply 5s after a combustion indicator lamp is turned off, and taking off the oxygen bomb; placing the whole oxygen bomb into ultrasonic water bath, vibrating and absorbing for 30min, so that chlorine elements released by the palladium-carbon sample A are fully dissolved in absorption liquid; then connecting the oxygen bomb with a gas absorption device (a mixed solution containing 25mL of 3.2mmol/L sodium carbonate and 1.0mmol/L sodium bicarbonate is used as an absorption liquid), opening an exhaust valve, opening an upper cover of the oxygen bomb after all gas is discharged, mixing the absorption liquid in the oxygen bomb with the absorption liquid in the gas absorption device, transferring the mixture into a volumetric flask, transferring a cleaning solution on the inner surface of a sample cup, an ignition screw rod, the cover of the oxygen bomb and the inner wall of the oxygen bomb into the volumetric flask, and then fixing the volume to 100mL by using water to obtain a liquid to be detected;
(3) preparing a series of standard solutions: diluting the chlorine standard solution to obtain a series of chlorine standard solutions, wherein the specific concentrations are as follows: 0.5mg/L, 1mg/L, 2mg/L, 5mg/L, 10 mg/L;
drawing a standard working curve: carrying out quantitative analysis on the series of standard solutions of chlorine by using an ion chromatograph to obtain the peak area of chlorine element, and drawing a standard working curve by taking the concentration of the chlorine element as a horizontal coordinate and the peak area as a vertical coordinate;
sample detection: and (3) filtering the solution to be detected by using a polyvinylidene fluoride microporous filter membrane with the thickness of 0.22 mu m, measuring the peak areas of chlorine elements in the solution to be detected and the blank solution under the same analysis condition as the standard working curve drawn, and calculating according to the standard working curve to obtain the chlorine content.
The working parameters of the ion chromatograph are as follows:
and (3) chromatographic column: selecting anion separation column (4.0mm × 150mm) and guard column (4.0mm × 10 mm);
leacheate: a mixed solution of 3.2mmol/L sodium carbonate and 1.0mmol/L sodium bicarbonate;
a suppressor: a chemical suppressor;
flow rate of eluent: 0.7 mL/min;
sample introduction volume: 20 μ L.
Example 2
The present example provides a method for determining palladium-carbon chloride content by using an oxy-bomb combustion method, and specifically refers to example 1, except that the palladium-carbon sample in step (1) is palladium-carbon sample B.
Comparative example 1
In the comparative example, chlorine content was measured for the palladium on carbon sample A and the palladium on carbon sample B by a sulfuric acid distillation method.
Comparative example 2
In the comparative example, chlorine content was measured for the palladium on carbon sample a and the palladium on carbon sample B by mercury titration.
The results of the measurement of the time used in the measurement process, the amount of the reagent used, and the chlorine contents in the obtained palladium on carbon sample A and palladium on carbon sample B (% of the product of the measured chlorine concentration and the volume of the liquid to be measured and the mass of the samples) in examples 1 to 2 and comparative examples 1 to 2 are shown in Table 1.
Table 1 test result data
The stability of the test methods of examples 1-2 was tested, specifically: respectively taking 5 parts of palladium-carbon sample A and 5 parts of palladium-carbon sample B, wherein the mass of each part is 0.1 g; the results of 5 measurements according to the methods of example 1 and example 2, respectively, are shown in Table 2.
Table 2 test methods stability test results
As can be seen from tables 1-2, the detection method provided by the invention is more accurate in determination of the chlorine content in the palladium-carbon, is more stable, and can still ensure the detection accuracy after multiple detections. Compared with the sulfuric acid distillation method, the method greatly reduces the consumption of acid, shortens the treatment time and improves the sensitivity of the method. Compared with a mercury titration method, the pH does not need to be strictly regulated, and the problem that the indicator changes color and is used as a titration end point, so that the artificial judgment error is large is solved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The application of the oxygen bomb combustion method in the determination of the content of palladium-carbon chloride.
2. The method for measuring the content of palladium-carbon chloride by using the oxygen bomb combustion method is characterized by comprising the following steps of:
(1) mixing a palladium-carbon test material and a combustion improver, placing the mixture into a sample cup, adding an absorption liquid into an oxygen bomb, and sealing the oxygen bomb;
(2) oxygenating the oxygen bomb, and igniting for combustion;
(3) after the sintering is finished, the oxygen bomb is subjected to ultrasonic treatment and then is connected with a gas absorption device containing absorption liquid, and gas in the oxygen bomb is discharged;
(4) after the gas is discharged, opening the oxygen bomb, mixing absorption liquid in the oxygen bomb and absorption liquid in the gas absorption device, and diluting with water to obtain liquid to be detected;
(5) and (4) filtering the solution to be detected, and then determining the chlorine content by using an ion chromatograph.
3. The method for determining the palladium-carbon chloride content by the Bomb combustion method as claimed in claim 2, wherein the combustion improver in the step (1) is methanol, ethanol, ethylene glycol or glycerol; the mass ratio of the combustion improver to the palladium-carbon sample is 0.5-1.5: 0.1.
4. the method for measuring the palladium-carbon chloride content by the bomb combustion method according to claim 2 or 3, wherein the volume-to-mass ratio of the absorption liquid to the palladium-carbon sample in the step (1) is 10-40 mL: 0.1 g.
5. The method for determining the chlorine content of palladium-carbon by using the bomb combustion method according to claim 2, wherein the absorption liquid in the step (1) and the absorption liquid in the step (3) are independent solutions containing sodium carbonate and sodium bicarbonate; the concentration of the sodium carbonate is independently 3-3.5 mmol/L; the concentration of sodium bicarbonate is independently 0.5-1.5 mmol/L.
6. The method for measuring the content of palladium-carbon chloride by using the bomb combustion method according to claim 2 or 5, wherein the ultrasonic time in the step (3) is 30-40 min.
7. The method for determining the palladium-carbon chloride content by the Bomb combustion method as claimed in claim 6, wherein the filtering in the step (5) is filtering by using a polyvinylidene fluoride microporous membrane.
8. The method for determining the chlorine content of palladium-carbon by using the bomb combustion method as claimed in claim 2, wherein the method for determining the chlorine content by using an ion chromatograph in the step (5) is as follows:
a. preparing a series of standard solutions: diluting the chlorine standard solution to obtain a series of chlorine standard solutions;
b. drawing a standard working curve: carrying out quantitative analysis on the series of chlorine standard solutions by using an ion chromatograph to obtain a standard working curve;
c. sample detection: and c, under the same quantitative analysis condition as the step b, measuring the peak areas of the chlorine element in the solution to be detected and the blank solution, and calculating according to a standard working curve to obtain the chlorine content.
9. The method for determining the chlorine content of palladium-carbon by using the bomb combustion method as claimed in claim 8, wherein the concentration of the series of standard solutions of chlorine in the step a is 0.5mg/L, 1mg/L, 2mg/L, 5mg/L or 10 mg/L.
10. The method for determining the chlorine content of palladium-carbon by using the bomb combustion method according to claim 8 or 9, wherein in the step b, the method for obtaining the standard working curve comprises the following steps: quantitatively analyzing the peak area of the chlorine element in the series of standard solutions of the chlorine, and establishing a standard working curve of the relationship between the peak area of the chlorine element and the concentration by using a calibration curve method.
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| CN101799407A (en) * | 2010-03-26 | 2010-08-11 | 苏州市贝特利高分子材料有限公司 | Method for measuring content of halogen |
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| CN111380942A (en) * | 2018-12-29 | 2020-07-07 | 广东阿格蕾雅光电材料有限公司 | Method for determining bromine content in organic photoelectric material based on oxygen bomb combustion method |
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2022
- 2022-06-23 CN CN202210715313.XA patent/CN114994235A/en not_active Withdrawn
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101799407A (en) * | 2010-03-26 | 2010-08-11 | 苏州市贝特利高分子材料有限公司 | Method for measuring content of halogen |
| CN106018666A (en) * | 2016-06-24 | 2016-10-12 | 苏州新区环保服务中心有限公司 | Oxygen bomb combustion method for testing content of halogens and content of sulphur in industrial solid waste |
| CN109030703A (en) * | 2018-06-08 | 2018-12-18 | 江苏省产品质量监督检验研究院 | A kind of method of content of halogen in Oxygen Bomb Combustion-sulfate by ion chromatography cable nonmetallic materials |
| CN111380942A (en) * | 2018-12-29 | 2020-07-07 | 广东阿格蕾雅光电材料有限公司 | Method for determining bromine content in organic photoelectric material based on oxygen bomb combustion method |
| CN110398564A (en) * | 2019-06-24 | 2019-11-01 | 广东省特种设备检测研究院中山检测院 | The detection method of chlorinity in a kind of solid biomass fuel |
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