Method for measuring element content of sodium aluminate clinker by X-ray fluorescence spectrometry

Abstract

The invention discloses a method for measuring the element content of a sodium aluminate clinker through X-ray fluorescence spectrometry in the technical field of element measurement, and particularly relates to the X-ray fluorescence spectrometry for measuring the element content. The method is suitable for determining the components of Al2O3, SiO2, Fe2O3, CaO and Na2O of the sodium aluminate clinker prepared from the aluminum ash. The method comprises the following steps of: measuring the following components in percentage by weight: 10.75 to 83.07 percent of Al2O3, 1.73 to 21.36 percent of SiO2, 3.77 to 30.37 percent of Fe2O3, 0.078 to 39.09 percent of CaO, and 0.092 to 35.00 percent of Na2O.

Description

Technical Field

[0001] The invention relates to the technical field of element content determination, and in particular to a method for determining the element content of sodium aluminate clinker by using an X-ray fluorescence spectrometry method. Background Art

[0002] Aluminum ash is a waste generated in the production of aluminum industry, but it contains a variety of valuable elements and has a high recycling value. Sodium aluminate clinker is an important raw material obtained by processing aluminum ash, and its component analysis is crucial for product quality control and process optimization. However, since sodium aluminate clinker prepared from aluminum ash is a new material, there is currently neither a national standard nor an industry standard, and there is a lack of unified standards and effective analysis methods, which brings great difficulties to the quality control and application of sodium aluminate clinker.

[0003] The composition of sodium aluminate clinker is diverse and complex, mainly including alumina, silicon dioxide, ferric oxide, calcium oxide and sodium oxide, and the content of these components varies in different production batches. This complexity places high demands on the determination of the composition. The interaction between different elements may lead to problems such as spectral line overlap and signal interference during the determination process, which directly affects the accuracy of the determination. In addition, the physical properties of sodium aluminate clinker, such as particle size and density, may also affect the uniformity of sample preparation and measurement, thereby increasing the uncertainty of the determination. Although traditional methods for determining the composition of sodium aluminate clinker, such as chemical titration and gravimetric analysis, can provide relatively accurate results under certain specific conditions, they often show obvious limitations when facing complex multi-element systems. These methods usually require cumbersome sample pretreatment processes and are easily affected by the operator, resulting in poor repeatability of the results. In addition, the measurement cycle of traditional methods is long, which makes it difficult to adapt to the needs of modern industrial production for rapid and accurate analysis. With the continuous development of production technology, the requirements for component determination are also increasing, and traditional methods can no longer meet the current analysis needs of complex samples. Summary of the invention

[0004] The present invention aims to provide a method for determining the element content of sodium aluminate clinker by X-ray fluorescence spectrometry to solve the problems of limited measurement range, complicated sample pretreatment process and high finished product cost of traditional measurement methods.

[0005] In order to solve the above technical problems, the present invention provides the following technical solution: a method for determining the element content of sodium aluminate clinker by X-ray fluorescence spectrometry, comprising the following steps:

[0006] S1. Sample preparation: The sample is sieved through a stainless steel sieve, ground to a specified particle size using a vibration mill, and stored for analysis;

[0007] S2. Establishing a standard curve: Establishing a standard substance library, using the melting method to make a glass piece from the standard sample, and making an intensity-concentration analysis curve based on the corresponding standard sample;

[0008] S3, sample dissolution: weigh a certain amount of sample, put it in a beaker, add standard solution and water, stir and heat in a water bath, and perform dissolution reaction for a period of time;

[0009] S4, filtration and washing: after dissolution, vacuum filtration is performed, and the beaker and filter cake are washed with boiling water for several times;

[0010] S5. Sample drying and grinding: Dry the washed filter cake together with the filter paper, grind the dried sample into uniform fine powder using an agate mortar and store it for analysis;

[0011] S6, preparation of fused sheet: weigh a certain amount of sample and a mixed flux of lithium tetraborate and lithium metaborate, mix them evenly, add a release agent, put them into a fusion machine for melting treatment, take out the fused sheet, weigh and record it after cooling;

[0012] S7. X-ray fluorescence spectrometry analysis: Use an X-ray fluorescence spectrometer to analyze the molten sheet and determine the content of each element based on a pre-established standard curve;

[0013] S8. Data recording and processing: record the X-ray fluorescence spectrum data of each sample, compare it with the standard value, and calculate the difference between the measured value and the standard value.

[0014] Furthermore, the sample in step S1 is screened with a 200-mesh stainless steel screen, and the standard substance library in step S2 is established by combining the purchased bauxite national standard substance and the sodium aluminate clinker sent to an authoritative institution for value determination.

[0015] Furthermore, the standard solution in step S3 is prepared by dissolving and diluting 194.0 g of analytical pure NaOH and 85.5 g of analytical pure Na2CO3 to a constant volume of 10 L, weighing 50 g of sample, taking 625 ml of standard solution, 125 ml of water, the water bath temperature is 90°C, using a magnetic stirrer with a rotation speed of 350-400 rpm, and the dissolution reaction time is 30 min.

[0016] Furthermore, in the step S4, the beaker and the filter cake are washed with boiling water 8 times.

[0017] Furthermore, in the step S5, the drying temperature is 105° C. and the drying time is 1 hour.

[0018] Further, in the step S6, 1.2 g of sample is weighed and mixed with 6 g of lithium tetraborate and lithium metaborate mixed flux, 2-3 drops of 2:5 (ammonium bromide: water) ammonium bromide release agent are added, the temperature of the melting machine is 1050°C, pre-melting is 2 minutes, melting is 15 minutes, and standing is 1 minute.

[0019] Beneficial effects of the present invention: 1. Filling the gap: It provides a reliable method for determining the element content of a new material, sodium aluminate clinker, prepared from aluminum ash, filling the gap in this field and providing strong technical support for the comprehensive utilization of aluminum ash and the quality control of sodium aluminate clinker.

[0020] 2. High precision: X-ray fluorescence spectrometry can accurately determine the content of each element in sodium aluminate clinker prepared from aluminum ash to ensure the stability of product quality. This method has high sensitivity and accuracy, can detect changes in the content of trace elements, and provide accurate data basis for process optimization.

[0021] 3. Easy operation: The sample preparation process is relatively simple and does not require complicated pre-treatment steps, which reduces the workload of operators and improves work efficiency. Operators only need to follow the prescribed steps to complete sample preparation and analysis, greatly shortening the analysis time.

[0022] 4. Strong reliability: The accuracy and reliability of the analysis results are guaranteed by establishing a standard substance library. The establishment of a standard substance library makes the analysis results traceable and comparable, and can effectively avoid the influence of human errors and system errors.

[0023] 5. Low cost: Compared with some traditional determination methods, the cost of instruments and reagents required by the present invention is relatively low, which is conducive to reducing production costs. At the same time, the method has high analysis efficiency, can reduce the input of manpower and material resources, and further reduce costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 The present invention is a standard curve diagram of a method for determining the element content of sodium aluminate clinker by X-ray fluorescence spectrometry. DETAILED DESCRIPTION

[0025] The following is further described in detail through specific implementation methods:

[0026] Example:

[0027] 1. Instrument

[0028] 1.1X-ray fluorescence spectrometer: MXF-2400;

[0029] 1.2 Melting machine: TNRY-02A / C;

[0030] 1.3 Dryer: Use silica gel as desiccant;

[0031] 1.4 Electronic balance: BSA224S;

[0032] 1.5 Water bath: DZKW-4 220VAC 1500W double row six holes;

[0033] 1.6 Magnetic stirrer: adjustable speed;

[0034] 1.7 Vacuum pump: 2XZ-4A rotary vane type;

[0035] 1.8 Oven: DHG-9140A.

[0036] 2. Measurement conditions

[0037] 2.1 Sample particle size: less than 74 microns (200 mesh);

[0038] 2.2X-ray tube voltage 40KV, tube current 70mA;

[0039] 2.3 Water temperature: 90℃;

[0040] 2.4 Stirring speed: 300-400 rpm;

[0041] 2.5 Reaction time: 30 minutes;

[0042] 2.6 Washing times: 8 times;

[0043] 2.7 Drying temperature: 105℃;

[0044] 2.8 Melting furnace temperature: 1050℃;

[0045] 2.9 Sample melting time: 18 minutes, including 2 minutes of pre-melting, 15 minutes of melting, and 1 minute of standing;

[0046] 2.10x fluorescence stabilization time: 30min.

[0047] Table 1 Spectroscopic crystals and integration range

[0048]

[0049]

[0050] 3. Preparation of standard samples

[0051] A standard material library is established by combining the purchased bauxite national standard materials and the sodium aluminate clinker sent to the authoritative organization for calibration. The standard samples are made into glass pieces by the melting method, and the strength-concentration analysis curves are made according to the corresponding standard samples, and then the concentration of each standard sample is determined.

[0052] Table 2

[0053]

[0054] The determination range is as follows: Al2O3: 10.75~83.07%, SiO2: 1.73~21.36%, Fe2O3: 3.77~30.37%, CaO: 0.078~39.09%, Na2O: 0.092~35.00%. The standard curve is as follows Figure 1 shown.

[0055] IV. Sample preparation

[0056] The samples were sieved through a 200-mesh stainless steel sieve, ground to the specified particle size using a vibration mill, and stored for analysis;

[0057] 5. Sample dissolution

[0058] Turn on the water bath switch, set the water bath temperature to 90℃, add appropriate amount of water, put in 1-4 1000ml beakers with 625ml standard solution and 125ml water, where the standard solution is made by taking 194.0g analytical pure NaOH and 85.5g analytical pure Na2CO3 and dissolving and diluting to a constant volume of 10L, weigh 50.0g of sample and place it in a beaker, each beaker corresponds to a magnetic stirrer, the stirring blade is 3 cm below the liquid level, the speed is 350-400 rpm, and it is controlled at 85+5℃, and the dissolution reaction is 30 minutes. After dissolution, vacuum filtration is performed, and the beaker and filter cake are washed 8 times with boiling water, each time with 156.25ml of water, and the washed filter cake and filter paper are dried at 105℃ for 1 hour, cooled, ground and mixed with an agate mortar, and stored in a ziplock bag for analysis.

[0059] 6. Melt Analysis

[0060] Weigh 1.2g of sample and 6g of lithium tetraborate and lithium metaborate mixed flux, mix well, add 2-3 drops of 2:5 (ammonium bromide: water) ammonium bromide release agent, place the sample in a melting machine at 1050°C, pre-melt for 2min, melt for 15min, let stand for 1min, take out and cool, weigh and record the weight in the electronic balance room, and then analyze on the fluorescence instrument.

[0061] Table 3: Comparison of measured values ​​and standard values ​​of main elements in different samples determined by X-ray fluorescence spectrometry

[0062]

[0063] 7. Result Analysis and Accuracy

[0064] 7.1 Results of 5-10 parallel measurements in the laboratory

[0065] Table 4

[0066]

[0067] 7.2 Inter-laboratory comparison data

[0068] Table 5

[0069]

[0070] In summary, accurate determination of element content in sodium aluminate clinker is crucial to ensuring product quality and optimizing production processes. X-ray fluorescence spectrometry has become the preferred technology for the analysis of key elements in sodium aluminate clinker due to its advantages of high precision, rapid analysis, and simultaneous determination of multiple elements. By optimizing sample preparation and analysis curve construction, the accuracy and stability of the determination are effectively improved. Practical application examples have shown that XRF technology can not only meet the analysis needs of complex samples, but also achieve precise quality control in the production process, significantly improving product consistency and stability. Strict error control strategies further ensure the reliability of the measurement results and provide technical support for the high-quality production of sodium aluminate clinker. Overall, the application of X-ray fluorescence spectrometry in the determination of element content in sodium aluminate clinker has broad practical significance and promotion value, and has a positive role in improving the overall technical level of the industry.

[0071] The above is only an embodiment of the present invention, and the common knowledge such as the known specific structure and characteristics in the scheme is not described in detail here. It should be pointed out that for those skilled in the art, several deformations and improvements can be made without departing from the structure of the present invention, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicality of the patent. The scope of protection required by this application shall be based on the content of its claims, and the specific implementation methods and other records in the specification can be used to interpret the content of the claims.

Claims

1. A method for determining the element content of sodium aluminate clinker by X-ray fluorescence spectrometry, characterized in that: The following steps are involved: S1. Sample preparation: The sample is sieved through a stainless steel sieve, ground to a specified particle size using a vibration mill, and stored for analysis; S2. Establishing a standard curve: Establishing a standard substance library, using the melting method to make a glass piece from the standard sample, and making an intensity-concentration analysis curve based on the corresponding standard sample; S3, sample dissolution: weigh a certain amount of sample, put it in a beaker, add standard solution and water, stir and heat in a water bath, and perform dissolution reaction for a period of time; S4, filtration and washing: after dissolution, vacuum filtration is performed, and the beaker and filter cake are washed with boiling water for several times; S5. Sample drying and grinding: Dry the washed filter cake together with the filter paper, grind the dried sample into uniform fine powder using an agate mortar and store it for analysis; S6, preparation of fused sheet: weigh a certain amount of sample and a mixed flux of lithium tetraborate and lithium metaborate, mix them evenly, add a release agent, put them into a fusion machine for melting treatment, take out the fused sheet, weigh and record it after cooling; S7. X-ray fluorescence spectrometry analysis: Use an X-ray fluorescence spectrometer to analyze the molten sheet and determine the content of each element based on a pre-established standard curve; S8. Data recording and processing: record the X-ray fluorescence spectrum data of each sample, compare it with the standard value, and calculate the difference between the measured value and the standard value.

2. The method for determining the element content of sodium aluminate clinker by X-ray fluorescence spectrometry according to claim 1, characterized in that: In the step S1, the sample is screened with a 200-mesh stainless steel screen, and the standard substance library in the step S2 is established by combining the purchased national standard substance of bauxite and the sodium aluminate clinker sent to an authoritative institution for value determination.

3. The method for determining the element content of sodium aluminate clinker by X-ray fluorescence spectrometry according to claim 2, characterized in that: The standard solution in step S3 is prepared by dissolving and diluting 194.0 g of analytical pure NaOH and 85.5 g of analytical pure Na2CO3 to a constant volume of 10 L. 50 g of sample is weighed, 625 ml of standard solution and 125 ml of water are taken, the water bath temperature is 90°C, a magnetic stirrer with a rotation speed of 350-400 rpm is used, and the dissolution reaction time is 30 min.

4. The method for determining the element content of sodium aluminate clinker by X-ray fluorescence spectrometry according to claim 3, characterized in that: In the step S4, the beaker and the filter cake were washed 8 times with boiling water.

5. The method for determining the element content of sodium aluminate clinker by X-ray fluorescence spectrometry according to claim 4, characterized in that: In the step S5, the drying temperature is 105° C. and the drying time is 1 hour.

6. The method for determining the element content of sodium aluminate clinker by X-ray fluorescence spectrometry according to claim 5, characterized in that: In the step S6, 1.2 g of sample is weighed and mixed with 6 g of lithium tetraborate and lithium metaborate mixed flux, and 2-3 drops of 2:5 (ammonium bromide: water) ammonium bromide release agent are added. The temperature of the melting machine is 1050° C., pre-melting is 2 min, melting is 15 min, and standing is 1 min.

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