Detection method for measuring content of cement oxide by atomic emission spectrometry

Abstract

The invention belongs to the field of cement oxide detection, and particularly relates to a detection method for determining the content of cement oxide by atomic emission spectrometry, and the detection method comprises the following specific steps: S1, sample treatment: pretreating a cement sample to increase the surface area of the cement sample so as to improve the analysis sensitivity; s2, excitation source selection: selecting proper excitation sources according to different analysis methods, sample characteristics, detection sensitivity and resolution requirements, wherein the selectable excitation sources comprise a flame light source, an electric spark light source and an inductively coupled plasma light source; the method for detecting the content of the oxide in the cement by adopting the atomic emission spectrometry can effectively solve the problems that the content of the oxide does not meet the standard requirement, the strength of the cement is possibly insufficient, the structural safety of a building is influenced, the content of the oxide in the cement also influences the setting time of the cement, and if the content of the oxide is not appropriate, the cement cannot be cured. And the problem that the setting time of the cement is too long or too short is solved.

Description

Technical Field

[0001] The invention belongs to the field of cement oxide detection, in particular to a method for determining cement oxide content by atomic emission spectroscopy. Background Art

[0002] The oxide content in cement mainly includes calcium oxide, silicon dioxide, aluminum oxide and iron oxide, among which calcium oxide is a necessary component for producing CSH gel (silicate gel) and CAH gel (aluminate gel) during cement hardening. When its content is appropriate, it can increase the strength and compressive strength of cement. Silicon dioxide is one of the most important gel-forming components of cement, and reacts with calcium oxide to form CSH gel. When its content is appropriate, it can improve the strength and durability of cement. Alumina plays an important role in controlling and regulating the setting reaction of cement. When its content is appropriate, it can improve the durability and resistance to sulfate erosion of cement.

[0003] The basic principle of atomic emission spectrometry is that when atoms are excited to a high energy level, they will release photons of a specific wavelength when returning to the ground state, forming a characteristic spectrum. By detecting and analyzing these characteristic spectra, the content of various elements in the sample can be determined. This method has high sensitivity and selectivity and can achieve high-sensitivity analysis of elements.

[0004] The oxides in cement are the main components of cement clinker. Their content directly affects the hydration reaction and strength development of cement. If the content of these oxides does not meet the standard requirements, it may lead to insufficient strength of cement, thus affecting the structural safety of the building. At the same time, the oxide content in cement will also affect the setting time of cement. If the oxide content is not appropriate, it may cause the setting time of cement to be too long or too short, which is very unfavorable for the control of the construction process.

[0005] To this end, the present invention provides a detection method for determining cement oxide content by atomic emission spectroscopy. Summary of the invention

[0006] In order to make up for the deficiencies of the prior art, at least one technical problem raised in the background technology is solved.

[0007] The technical solution adopted by the present invention to solve the technical problem is: a detection method for determining the oxide content of cement by atomic emission spectrometry according to the present invention, the specific steps of the detection method are as follows:

[0008] S1. Sample processing: pre-treat cement samples to increase their surface area and thus improve the sensitivity of analysis;

[0009] S2. Excitation source selection: Select a suitable excitation source according to the analysis method, sample characteristics, detection sensitivity and resolution requirements. The available excitation sources include flame light source, electric spark light source and inductively coupled plasma light source;

[0010] S3, spectrometer settings: set the spectrometer parameters according to the characteristics of the sample and the purpose of analysis;

[0011] S4, sample introduction: introducing the treated cement sample into the spectrometer;

[0012] S5. Data collection: After the sample is excited, the atoms will emit light of a specific wavelength. These light signals are detected and recorded by the spectrometer. During the data collection process, attention should be paid to the signal strength and stability to ensure the accuracy of the data.

[0013] S6. Data analysis: The collected data needs to be processed and analyzed to determine the content of various oxides in the cement samples;

[0014] S7. Result report: Generate a report based on the analysis results, including the content of various oxides in the sample, the accuracy and reliability of the analysis method.

[0015] Preferably, the sample processing steps in S1 are as follows:

[0016] S21. Sample collection: Collect representative cement samples;

[0017] S22. Sample preparation: The collected cement samples usually need to be crushed and ground to reduce the particle size and increase the surface area of ​​the sample, thereby improving the sensitivity of the analysis. During the grinding process, care should be taken to avoid sample contamination and use clean grinding equipment and containers;

[0018] S23, sample dissolution: dissolve the ground cement sample in a suitable solvent, and use the solvent to dissolve the oxides in the sample. During the dissolution process, attention should be paid to the dissolution temperature, reaction time and acidity adjustment;

[0019] S24, sample dilution: dilute the dissolved sample solution to adjust the sample concentration to make it suitable for the analysis range of the atomic emission spectrometer. During the dilution process, accurate measuring tools and diluents are required to ensure the accuracy of the dilution multiple;

[0020] S25. Sample filtration: Before atomic emission spectrometry analysis, the sample solution needs to be filtered by filter paper, membrane filtration or centrifugal separation to remove insoluble impurities and particles;

[0021] S26. Sample preservation: The processed sample solution needs to be stored in an appropriate container and marked and recorded before analysis. The storage conditions of the sample should be determined according to the nature of the sample and the requirements of the analysis method. It usually needs to be stored at low temperature, away from light and in a dry condition.

[0022] Preferably, the solvent in S23 may be hydrochloric acid, nitric acid or hydrofluoric acid.

[0023] Preferably, the specific steps of sample dilution in S23 are:

[0024] S31. Preparation: Prepare processed samples and pure water;

[0025] S32, dilution: prepare an appropriate amount of pure water and add it to the diluter, then take a sample of 1 / 10 of the pure water and inject it into the diluter. Be careful not to pour the liquid above the mark line on the top of the diluter, otherwise it will cause concentration calculation errors;

[0026] S33, dilution operation: after the sample and pure water are injected into the diluter, the discharge valve of the diluter is opened to mix the diluent and the sample until the concentration reaches the required dilution degree;

[0027] S34. Storage operation: After the dilution is completed, clean the sample and diluent, close the corresponding drain valve and lubrication valve, and store the diluter in a clean and dry place.

[0028] Preferably, the spectrometer setting in S3 requires setting the wavelength range, resolution, integration time, scanning step, and detector; wherein the wavelength range is 400nm to 700nm; and the minimum resolution is 0.1nm.

[0029] Preferably, the sample introduction method in S4 is to dissolve the sample in a suitable solvent, then use a nebulizer to convert the solution into an aerosol, and then introduce the aerosol into the plasma.

[0030] Preferably, the data collection process in S5 includes the following specific steps:

[0031] S41, initialization: firstly, setting the parameters of the spectrometer;

[0032] S42, signal acquisition: start the spectrometer and start collecting spectrum data;

[0033] S43, data transmission: transferring the collected data from the spectrometer to the computer;

[0034] S44. Data storage: storing the received data in the hard disk of the computer for subsequent analysis.

[0035] Preferably, the data analysis in S6 generally involves establishment of a calibration curve, background correction and quantification of signal intensity.

[0036] The beneficial effects of the present invention are as follows:

[0037] The method for determining the oxide content of cement by atomic emission spectrometry described in the present invention can effectively solve the problem that the oxide content does not meet the standard requirements, which may lead to insufficient strength of cement and affect the structural safety of the building. At the same time, the oxide content in cement will also affect the setting time of cement. If the oxide content is not appropriate, it may cause the setting time of cement to be too long or too short. BRIEF DESCRIPTION OF THE DRAWINGS

[0038] The present invention will be further described below in conjunction with the accompanying drawings.

[0039] Figure 1 is a method flow chart of the detection method of the present invention;

[0040] Figure 2 is a flowchart of the specific steps of sample processing in the present invention;

[0041] Figure 3 is a flow chart of the specific steps of sample dilution in the present invention;

[0042] Figure 4 It is a flow chart of the specific steps of data collection in the present invention. DETAILED DESCRIPTION

[0043] In order to make the technical means, creative features, objectives and effects achieved by the present invention easy to understand, the present invention is further explained below in conjunction with specific implementation methods.

[0044] like Figure 1 to Figure 2 As shown, a detection method for determining cement oxide content by atomic emission spectrometry according to an embodiment of the present invention, the specific steps of the detection method are as follows:

[0045] S1. Sample processing: pre-treat cement samples to increase their surface area and thus improve the sensitivity of analysis;

[0046] S2. Excitation source selection: Select a suitable excitation source according to the analysis method, sample characteristics, detection sensitivity and resolution requirements. The available excitation sources include flame light source, electric spark light source and inductively coupled plasma light source;

[0047] S3, spectrometer settings: set the spectrometer parameters according to the characteristics of the sample and the purpose of analysis;

[0048] S4, sample introduction: introducing the treated cement sample into the spectrometer;

[0049] S5. Data collection: After the sample is excited, the atoms will emit light of a specific wavelength. These light signals are detected and recorded by the spectrometer. During the data collection process, attention should be paid to the signal strength and stability to ensure the accuracy of the data.

[0050] S6. Data analysis: The collected data needs to be processed and analyzed to determine the content of various oxides in the cement samples;

[0051] S7. Result report: Generate a report based on the analysis results, including the content of various oxides in the sample, the accuracy and reliability of the analysis method.

[0052] The specific steps of sample processing in S1 are as follows:

[0053] S21. Sample collection: Collect representative cement samples;

[0054] S22. Sample preparation: The collected cement samples usually need to be crushed and ground to reduce the particle size and increase the surface area of ​​the sample, thereby improving the sensitivity of the analysis. During the grinding process, care should be taken to avoid sample contamination and use clean grinding equipment and containers;

[0055] S23, sample dissolution: dissolve the ground cement sample in a suitable solvent, and use the solvent to dissolve the oxides in the sample. During the dissolution process, attention should be paid to the dissolution temperature, reaction time and acidity adjustment;

[0056] S24, sample dilution: dilute the dissolved sample solution to adjust the sample concentration to make it suitable for the analysis range of the atomic emission spectrometer. During the dilution process, accurate measuring tools and diluents are required to ensure the accuracy of the dilution multiple;

[0057] S25. Sample filtration: Before atomic emission spectrometry analysis, the sample solution needs to be filtered by filter paper, membrane filtration or centrifugal separation to remove insoluble impurities and particles;

[0058] S26. Sample preservation: The processed sample solution needs to be stored in an appropriate container and marked and recorded before analysis. The storage conditions of the sample should be determined according to the nature of the sample and the requirements of the analysis method. It usually needs to be stored at low temperature, away from light and in a dry condition.

[0059] The solvent in S23 can be hydrochloric acid, nitric acid or hydrofluoric acid.

[0060] The specific steps of sample dilution in S23 are as follows:

[0061] S31. Preparation: Prepare processed samples and pure water;

[0062] S32, dilution: prepare an appropriate amount of pure water and add it to the diluter, then take a sample of 1 / 10 of the pure water and inject it into the diluter. Be careful not to pour the liquid above the mark line on the top of the diluter, otherwise it will cause concentration calculation errors;

[0063] S33, dilution operation: after the sample and pure water are injected into the diluter, the discharge valve of the diluter is opened to mix the diluent and the sample until the concentration reaches the required dilution degree;

[0064] S34. Storage operation: After the dilution is completed, clean the sample and diluent, close the corresponding drain valve and lubrication valve, and store the diluter in a clean and dry place.

[0065] The spectrometer settings in S3 require the setting of wavelength range, resolution, integration time, scanning step, and detector; the wavelength range is 400nm to 700nm; the minimum resolution is 0.1nm.

[0066] The sample introduction method in S4 is to dissolve the sample in a suitable solvent, then use a nebulizer to convert the solution into an aerosol, and then introduce the aerosol into the plasma.

[0067] The specific steps of the data collection process in S5 are as follows:

[0068] S41, initialization: firstly, setting the parameters of the spectrometer;

[0069] S42, signal acquisition: start the spectrometer and start collecting spectrum data;

[0070] S43, data transmission: transferring the collected data from the spectrometer to the computer;

[0071] S44. Data storage: storing the received data in the hard disk of the computer for subsequent analysis.

[0072] The data analysis in S6 usually involves the establishment of calibration curves, background correction and quantification of signal intensity.

[0073] The above shows and describes the basic principles, main features and advantages of the present invention. It should be understood by those skilled in the art that the present invention is not limited to the above embodiments. The above embodiments and descriptions are only for explaining the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, which fall within the scope of the present invention. The scope of protection of the present invention is defined by the attached claims and their equivalents.

Claims

1. A method for determining the oxide content of cement by atomic emission spectrometry, characterized in that: The specific steps of this detection method are as follows: S1. Sample processing: pre-treat cement samples to increase their surface area and thus improve the sensitivity of analysis; S2. Excitation source selection: Select a suitable excitation source according to the analysis method, sample characteristics, detection sensitivity and resolution requirements. The available excitation sources include flame light source, electric spark light source and inductively coupled plasma light source; S3, spectrometer settings: set the spectrometer parameters according to the characteristics of the sample and the purpose of analysis; S4, sample introduction: introducing the treated cement sample into the spectrometer; S5. Data collection: After the sample is excited, the atoms will emit light of a specific wavelength. These light signals are detected and recorded by the spectrometer. During the data collection process, attention should be paid to the signal strength and stability to ensure the accuracy of the data. S6. Data analysis: The collected data needs to be processed and analyzed to determine the content of various oxides in the cement samples; S7. Result report: Generate a report based on the analysis results, including the content of various oxides in the sample, the accuracy and reliability of the analysis method.

2. The method for determining the oxide content of cement by atomic emission spectrometry according to claim 1, characterized in that: The specific steps of sample processing in S1 are as follows: S21. Sample collection: Collect representative cement samples; S22. Sample preparation: The collected cement samples usually need to be crushed and ground to reduce the particle size and increase the surface area of ​​the sample, thereby improving the sensitivity of the analysis. During the grinding process, care should be taken to avoid sample contamination and use clean grinding equipment and containers; S23, sample dissolution: dissolve the ground cement sample in a suitable solvent, and use the solvent to dissolve the oxides in the sample. During the dissolution process, attention should be paid to the dissolution temperature, reaction time and acidity adjustment; S24, sample dilution: dilute the dissolved sample solution to adjust the sample concentration to make it suitable for the analysis range of the atomic emission spectrometer. During the dilution process, accurate measuring tools and diluents are required to ensure the accuracy of the dilution multiple; S25. Sample filtration: Before atomic emission spectrometry analysis, the sample solution needs to be filtered by filter paper, membrane filtration or centrifugal separation to remove insoluble impurities and particles; S26. Sample preservation: The processed sample solution needs to be stored in an appropriate container and marked and recorded before analysis. The storage conditions of the sample should be determined according to the nature of the sample and the requirements of the analysis method. It usually needs to be stored at low temperature, away from light and in a dry condition.

3. The method for determining the oxide content of cement by atomic emission spectrometry according to claim 2, characterized in that: The solvent in S23 may be hydrochloric acid, nitric acid or hydrofluoric acid.

4. The method for determining the oxide content of cement by atomic emission spectrometry according to claim 3, characterized in that: The specific steps of sample dilution in S24 are as follows: S31. Preparation: Prepare processed samples and pure water; S32, dilution: prepare an appropriate amount of pure water and add it to the diluter, then take a sample of 1 / 10 of the pure water and inject it into the diluter. Be careful not to pour the liquid above the mark line on the top of the diluter, otherwise it will cause concentration calculation errors; S33, dilution operation: after the sample and pure water are injected into the diluter, the discharge valve of the diluter is opened to mix the diluent and the sample until the concentration reaches the required dilution degree; S34. Storage operation: After the dilution is completed, clean the sample and diluent, close the corresponding drain valve and lubrication valve, and store the diluter in a clean and dry place.

5. The method for determining the oxide content of cement by atomic emission spectrometry according to claim 4, characterized in that: The spectrometer setting in S3 needs to set the wavelength range, resolution, integration time, scanning step length, and detector; The wavelength range is 400nm to 700nm; the minimum resolution is 0.1nm.

6. The method for determining the oxide content of cement by atomic emission spectrometry according to claim 5, characterized in that: The sample introduction method in S4 is to dissolve the sample in a suitable solvent, then use a nebulizer to convert the solution into an aerosol, and then introduce the aerosol into the plasma.

7. The method for determining the oxide content of cement by atomic emission spectrometry according to claim 6, characterized in that: The specific steps of the data collection process in S5 are: S41, initialization: firstly, setting the parameters of the spectrometer; S42, signal acquisition: start the spectrometer and start collecting spectrum data; S43, data transmission: transferring the collected data from the spectrometer to the computer; S44. Data storage: storing the received data in the hard disk of the computer for subsequent analysis.

8. The method for determining the oxide content of cement by atomic emission spectrometry according to claim 7, characterized in that: The data analysis in S6 generally involves the establishment of a calibration curve, background correction, and quantification of signal intensity.

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