CN110749559A - Rapid detection method for low-content silicon in aluminum and aluminum alloy - Google Patents
Rapid detection method for low-content silicon in aluminum and aluminum alloy Download PDFInfo
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Abstract
The invention relates to a method for rapidly detecting low-content silicon in aluminum and aluminum alloy, which comprises the following steps: 1) sample weighing and dissolving: weighing aluminum and aluminum alloy samples, and adding hydrogen peroxide and hydrochloric acid to dissolve the samples; 2) removing hydrogen peroxide: heating and boiling the aluminum and aluminum alloy sample solution obtained in the step 1) at low temperature to decompose hydrogen peroxide in the solution; 3) diluting: diluting the aluminum and aluminum alloy sample solution obtained in the step 2) after the hydrogen peroxide removal with water according to the requirements of the detection method; 4) and finally, detecting the silicon content. The invention adopts the hydrogen peroxide-hydrochloric acid to dissolve the aluminum and aluminum alloy samples, and combines chemical kinetics factors, thereby effectively overcoming the problems in the prior art, and the whole method has simple operation, high detection speed and stable result.
Description
Technical Field
The invention belongs to the technical field of analysis and detection, and particularly relates to a rapid detection method for low-content silicon in aluminum and aluminum alloy.
Background
Compared with other alloy materials, the aluminum alloy has the characteristics of small density, corrosion resistance, plasticity, thermal conductivity and good electrical conductivity, and is widely applied to the fields of aerospace, ships, vehicles, electric power, electronics, chemical industry and the like at present. The silicon element added into the aluminum alloy is mainly used for improving the casting performance of the alloy, and the silicon and the aluminum can form a solid solution, thereby improving the high-temperature mouldability of the alloy, reducing the shrinkage rate and having no hot cracking tendency. However, when the silicon content in the alloy exceeds the eutectic composition, i.e., hard particles of free silicon are present, cutting work becomes difficult; silicon is associated with aluminum and has similar properties, silicon of other materials can also invade in the smelting and casting processes to become common main impurities in aluminum and most aluminum alloys, and the coexistence of silicon, particularly silicon and iron obviously influences the tissues and the performances of the aluminum and the aluminum alloys, so that the content of silicon in the aluminum and the aluminum alloys needs to be strictly controlled, and the requirement is to accurately detect the content of silicon in the aluminum and the aluminum alloys.
The content of silicon element in the most commonly used aluminum and aluminum alloy at present is generally less than 0.50 percent. In the existing method, sodium hydroxide or hydrofluoric acid is generally adopted to dissolve aluminum and aluminum alloy, and then detection is carried out. However, the sodium hydroxide or hydrofluoric acid is adopted to dissolve aluminum and aluminum alloy, so that a large amount of salt is introduced, subsequent determination and the like are influenced, or an apparatus which is easy to corrode and pollutes the environment are influenced, and the operation is complicated. And the adoption of sodium hydroxide or hydrofluoric acid to dissolve aluminum and aluminum alloy can also introduce silicon in the forms of sodium silicate and fluosilicic acid respectively, which leads to the blank value of the solution to be increased and seriously influences the accuracy of the detection result. The reagent with higher silicon content influences the determination of low-content silicon, and whether the dosages are consistent with each other directly influences the determination result.
Disclosure of Invention
The invention provides a method for rapidly detecting low-content silicon in aluminum and aluminum alloy aiming at the technical problems in the prior art, the problems in the prior art can be effectively overcome by adopting hydrogen peroxide-hydrochloric acid to dissolve aluminum and aluminum alloy samples and combining chemical kinetics factors, and the whole method is simple to operate, high in detection speed and stable in result.
The technical scheme for solving the technical problems is as follows: a method for rapidly detecting low-content silicon in aluminum and aluminum alloy comprises the following steps:
1) sample weighing and dissolving: weighing 0.0500-0.3000 g of aluminum and aluminum alloy samples, adding 0.5-3.0 mL of hydrogen peroxide and 15-50 mL of hydrochloric acid (1+3) to dissolve the samples until the reaction stops, and obtaining aluminum and aluminum alloy sample solution;
2) removing hydrogen peroxide: heating the aluminum and aluminum alloy sample solution obtained in the step 1) at a low temperature to boil, decomposing hydrogen peroxide in the solution, and then cooling to room temperature to obtain the aluminum and aluminum alloy sample solution without hydrogen peroxide;
3) diluting: adding water to dilute the solution of the aluminum and aluminum alloy samples subjected to the hydrogen peroxide removal in the step 2) to 100.00mL according to the requirements of the detection method, and uniformly mixing to obtain a solution to be detected of the aluminum and aluminum alloy samples;
4) and (3) detecting the silicon content: taking the solution to be detected of the aluminum and aluminum alloy samples obtained in the step 3), and detecting the silicon content by using an inductively coupled plasma atomic emission spectrometry, an atomic absorption spectrometry or a molecular absorption spectrophotometry to obtain a detection result.
The invention has the beneficial effects that: the method adopts the mixed solvent of hydrogen peroxide and hydrochloric acid to dissolve the aluminum and aluminum alloy samples, has high dissolving speed, does not introduce a large amount of salt and new silicon elements into the solution to be detected, has simple and quick pretreatment on the samples, and has accurate detection result of the treated samples; the method decomposes the hydrogen peroxide by heating and boiling at low temperature, effectively removes the hydrogen peroxide, ensures that silicon compounds in the solution are not evaporated and polymerized, keeps the acidity between the solutions basically consistent, and further ensures the detection accuracy.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, in the step 1), the content of silicon in the aluminum and aluminum alloy samples is less than 1.0%.
The method has the advantages that the method limits the sample to further ensure the accuracy of the detection result, and the method has higher detection accuracy on low-content silicon.
Further, in the step 1), the hydrogen peroxide is rho 1.10 g/mL.
Further, in the step 1), hydrochloric acid with rho 1.19g/mL is selected.
Further, in the step 1), dilute hydrochloric acid is selected as hydrochloric acid, and the volume ratio of the hydrochloric acid diluted by water is 1: 0-5.
The beneficial effect of adopting the above-mentioned further scheme is that can effectively improve the dissolution rate of sample.
Further, in the step 1), hydrogen peroxide and hydrochloric acid are added in sequence or added after premixing.
Preferably, in the step 1), the hydrogen peroxide and the hydrochloric acid are added in a manner of adding the hydrogen peroxide and then adding the hydrochloric acid in batches.
The further scheme has the beneficial effects that the dissolving speed of the sample can be further effectively improved, and the generation of silane can be effectively inhibited.
Further, the reagent is selected from a reagent with superior purity, analytical purity or chemical purity.
The method has the advantage that the practicability of the method can be effectively improved.
Further, in the step 2), the temperature adopted for low-temperature heating and boiling is less than 280 ℃.
The beneficial effect of adopting the further scheme is that the temperature parameter can ensure that the hydrogen peroxide can be rapidly removed, and simultaneously, the silicon compound in the solution can be ensured not to be evaporated and polymerized, thereby further improving the processing speed.
Further, in the step 3), the water for dilution is primary or secondary deionized water or distilled water.
The beneficial effects of adopting above-mentioned further scheme are that can effectively improve the precision of detection and the stability of testing result, avoid introducing other impurity in the dilution process, influence the testing result.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
The invention discloses a method for rapidly detecting low-content silicon in aluminum and aluminum alloy, which comprises the following steps:
1) sample weighing and dissolving: weighing 0.0500-0.3000 g of aluminum and aluminum alloy samples, adding 0.5-3.0 mL of hydrogen peroxide and 15-50 mL of hydrochloric acid (1+3) to dissolve the samples until the reaction stops, and obtaining aluminum and aluminum alloy sample solution;
2) removing hydrogen peroxide: heating the aluminum and aluminum alloy sample solution obtained in the step 1) at a low temperature to boil, decomposing hydrogen peroxide in the solution, and then cooling to room temperature to obtain the aluminum and aluminum alloy sample solution without hydrogen peroxide;
3) diluting: adding water to dilute the solution of the aluminum and aluminum alloy samples subjected to the hydrogen peroxide removal in the step 2) to 100.00mL according to the requirements of the detection method, and uniformly mixing to obtain a solution to be detected of the aluminum and aluminum alloy samples;
4) and (3) detecting the silicon content: taking the solution to be detected of the aluminum and aluminum alloy samples obtained in the step 3), and detecting the silicon content by using an inductively coupled plasma atomic emission spectrometry, an atomic absorption spectrometry or a molecular absorption spectrophotometry to obtain a detection result.
The silicon detection sensitivity of the invention is high, and the invention is more suitable for the determination of low-content silicon, therefore, the detection sample is preferably a sample with the silicon content less than 1.0%.
The core of the invention lies in the pretreatment of the sample, and the invention adopts hydrogen peroxide and hydrochloric acid as solvents to dissolve the sample to prepare the solution to be detected. This is based on the study of the inventors on the method of measuring silicon. After the inventor intensively studies the method for detecting the silicon content in the aluminum alloy, the inventor finds that the general acid, especially the reducing acid dissolves the aluminum and the aluminum alloy, the general acid is easy to react with intermetallic compounds in a sample to generate silane, the silane is volatilized in a variable amount to lose silicon, and the measurement result is unstable or low, so the method is not suitable for measuring the silicon.
The existing detection method is to dissolve aluminum and aluminum alloy by using sodium hydroxide or hydrofluoric acid, so that the dosage of reagents is large, instruments are easy to corrode, the environment is polluted, the operation is complex, and the like. Based on the above findings, the inventors have conducted experimental studies to dissolve aluminum and aluminum alloy samples with a mixed solvent of hydrogen peroxide and hydrochloric acid. Not only has faster dissolving speed, but also has small reagent dosage and simple and convenient operation, and is more beneficial to subsequent determination. The technical problem of the existing detection method is obviously solved.
Further, in the step 1), the hydrogen peroxide is rho 1.10 g/mL.
Further, in the step 1), hydrochloric acid with rho 1.19g/mL is selected.
Further, in the step 1), dilute hydrochloric acid is selected as hydrochloric acid, and the volume ratio of the hydrochloric acid diluted by water is 1: 0-5.
Such a selection can further improve the dissolution efficiency.
Further, in the step 1), hydrogen peroxide and hydrochloric acid are added in sequence or added after premixing.
Preferably, in the step 1), the hydrogen peroxide and the hydrochloric acid are added in a manner of adding the hydrogen peroxide and then adding the hydrochloric acid in batches.
Such selection can further effectively increase the dissolution rate and effectively suppress the generation of silane.
Further, the reagent is selected from a reagent with superior purity, analytical purity or chemical purity.
The method has the advantage that the practicability of the method can be effectively improved.
Further, in the step 2), the temperature adopted for low-temperature heating and boiling is less than 280 ℃.
The beneficial effect of adopting the further scheme is that the temperature parameter can ensure that the hydrogen peroxide can be rapidly removed, and simultaneously, the silicon compound in the solution can be ensured not to be evaporated and polymerized, thereby further improving the processing speed.
Further, in the step 3), the water for dilution is primary or secondary deionized water or distilled water.
The beneficial effects of adopting above-mentioned further scheme are that can effectively improve the precision of detection and the stability of testing result, avoid introducing other impurity in the dilution process, influence the testing result.
Example 1
1) Sample weighing and dissolving: weighing 0.0500g of aluminum and aluminum alloy samples, placing the samples in a 150mL conical flask, adding 0.5mL of rho 1.10g/mL of hydrogen peroxide, adding 15mL of hydrochloric acid (1+3), dissolving the samples until the reaction stops to obtain an aluminum and aluminum alloy sample solution, wherein a detection reagent is a chemically pure reagent;
2) removing hydrogen peroxide: heating and boiling the aluminum and aluminum alloy sample solution obtained in the step 1) below 280 ℃, decomposing hydrogen peroxide in the solution, and then cooling to room temperature to obtain the aluminum and aluminum alloy sample solution without hydrogen peroxide;
3) diluting: diluting the aluminum and aluminum alloy sample solution obtained in the step 2) after removing the hydrogen peroxide with water according to the requirements of the detection method, and uniformly mixing to obtain a solution to be detected of the aluminum and aluminum alloy sample;
4) and (3) detecting the silicon content: and (3) taking the solution to be detected of the aluminum and aluminum alloy samples obtained in the step 3), and detecting the silicon content by using an inductively coupled plasma atomic emission spectrometry to obtain a detection result.
Example 2
1) Sample weighing and dissolving: weighing 0.1000g of aluminum and aluminum alloy sample, placing the sample in a 150mL conical flask, uniformly mixing 1.5mL of rho 1.10g/mL of hydrogen peroxide and 25mL of hydrochloric acid (1+3), adding the mixture into the conical flask, dissolving the sample until the reaction is stopped to obtain an aluminum and aluminum alloy sample solution, wherein the detection reagent is an analytical pure reagent;
2) removing hydrogen peroxide: heating and boiling the aluminum and aluminum alloy sample solution obtained in the step 1) below 280 ℃, decomposing hydrogen peroxide in the solution, and then cooling to room temperature to obtain the aluminum and aluminum alloy sample solution without hydrogen peroxide;
3) diluting: diluting the aluminum and aluminum alloy sample solution obtained in the step 2) after removing the hydrogen peroxide with water and the like according to the requirements of the detection method, and uniformly mixing to obtain a solution to be detected of the aluminum and aluminum alloy sample;
4) and (3) detecting the silicon content: and (3) taking the solution to be detected of the aluminum and aluminum alloy samples obtained in the step 3), and detecting the silicon content by using an atomic absorption spectrometry to obtain a detection result.
Example 3
1) Sample weighing and dissolving: weighing 0.2000g of aluminum and aluminum alloy sample, placing the sample in a 150mL conical flask, adding 2.5mL of rho 1.10g/mL of hydrogen peroxide, adding 25mL of hydrochloric acid (1+3), dissolving the sample until the reaction is stopped to obtain an aluminum and aluminum alloy sample solution, wherein the detection reagent is an analytical pure reagent;
2) removing hydrogen peroxide: heating and boiling the aluminum and aluminum alloy sample solution obtained in the step 1) below 280 ℃, decomposing hydrogen peroxide in the solution, slightly cooling, adding 15mL of hydrochloric acid (1+3), and cooling to room temperature to obtain the aluminum and aluminum alloy sample solution without hydrogen peroxide;
3) diluting: diluting the aluminum and aluminum alloy sample solution obtained in the step 2) after removing the hydrogen peroxide with water according to the requirements of the detection method, and uniformly mixing to obtain a solution to be detected of the aluminum and aluminum alloy sample;
4) and (3) detecting the silicon content: taking the solution to be detected of the aluminum and aluminum alloy samples obtained in the step 3), and detecting the silicon content by using a molecular absorption spectrophotometry method to obtain a detection result.
Example 4
1) Sample weighing and dissolving: weighing 0.3000g of aluminum and aluminum alloy samples, placing the samples in a 150mL conical flask, adding 3.0mL of rho 1.10g/mL of hydrogen peroxide, then adding 20mL of hydrochloric acid (1+1), dissolving the samples until the reaction is stopped to obtain an aluminum and aluminum alloy sample solution, wherein the detection reagent is a high-grade pure reagent;
2) removing hydrogen peroxide: heating and boiling the aluminum and aluminum alloy sample solution obtained in the step 1) below 280 ℃, decomposing hydrogen peroxide in the solution, and then cooling to room temperature to obtain the aluminum and aluminum alloy sample solution without hydrogen peroxide;
3) diluting: adding secondary deionized water to dilute the aluminum and aluminum alloy sample solution subjected to hydrogen peroxide removal in the step 2) according to the requirements of the detection method, and uniformly mixing to obtain a solution to be detected of the aluminum and aluminum alloy sample;
4) and (3) detecting the silicon content: and (3) taking the solution to be detected of the aluminum and aluminum alloy samples obtained in the step 3), and detecting the silicon content by using an inductively coupled plasma atomic emission spectrum to obtain a detection result.
The aluminum and aluminum alloy standard samples with different silicon contents are selected as detection samples, the detection method of the national standard GB/T20975.5-2008 is used as a reference method, the detection methods of the embodiments 1-4 are used as experimental methods, and the detection samples are detected, so that the obtained results are shown in Table 1.
| Serial number | When it is used for detection | The result of the detection | Setting value |
| National standard method 1 | 109min | The silicon content is 0.195% | 0.185％ |
| National standard method two | 363min | The silicon content is 0.463% | 0.476％ |
| Example 1 | 31min | The silicon content is 1.00 percent | 0.99％ |
| Example 2 | 32min | The silicon content is 0.468% | 0.476％ |
| Example 3 | 61min | The silicon content is 0.177% | 0.185％ |
| Example 4 | 31min | The silicon content is 0.084% | 0.082％ |
TABLE 1 data List of the results of the experiment
As can be seen from the results in Table 1, the detection method of the present invention has much shorter detection time than the detection method using the national standard method, and has the advantages of greatly reduced chemical reagent consumption and waste liquid amount, low energy consumption, and simple operation.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A method for rapidly detecting low-content silicon in aluminum and aluminum alloy is characterized by comprising the following steps:
1) sample weighing and dissolving: weighing 0.0500-0.3000 g of aluminum and aluminum alloy samples, adding 0.5-3.0 mL of hydrogen peroxide and 15-50 mL of hydrochloric acid (1+3) to dissolve the samples until the reaction stops, and obtaining aluminum and aluminum alloy sample solution;
2) removing hydrogen peroxide: heating the aluminum and aluminum alloy sample solution obtained in the step 1) at a low temperature to boil, decomposing hydrogen peroxide in the solution, and then cooling to room temperature to obtain the aluminum and aluminum alloy sample solution without hydrogen peroxide;
3) diluting: adding water to dilute the solution of the aluminum and aluminum alloy samples subjected to the hydrogen peroxide removal in the step 2) to 100.00mL according to the requirements of the detection method, and uniformly mixing to obtain a solution to be detected of the aluminum and aluminum alloy samples;
4) and (3) detecting the silicon content: taking the solution to be detected of the aluminum and aluminum alloy samples obtained in the step 3), and detecting the silicon content by using an inductively coupled plasma atomic emission spectrometry, an atomic absorption spectrometry or a molecular absorption spectrophotometry to obtain a detection result.
2. The method for rapidly detecting low-content silicon in aluminum and aluminum alloys according to claim 1, wherein the method comprises the following steps: in the step 1), the content of silicon in the aluminum and aluminum alloy samples is less than 1.0%.
3. The method for rapidly detecting low-content silicon in aluminum and aluminum alloys according to claim 1, wherein the method comprises the following steps: in the step 1), the hydrogen peroxide is rho 1.10 g/mL.
4. The method for rapidly detecting low-content silicon in aluminum and aluminum alloys according to claim 1, wherein the method comprises the following steps: in the step 1), hydrochloric acid with rho 1.19g/mL is selected.
5. The method for rapidly detecting low-content silicon in aluminum and aluminum alloys according to claim 1, wherein the method comprises the following steps: in the step 1), dilute hydrochloric acid is selected as hydrochloric acid, and the volume ratio of the hydrochloric acid diluted by water is 1: 0-5.
6. The method for rapidly detecting low-content silicon in aluminum and aluminum alloys according to claim 1, wherein the method comprises the following steps: in the step 1), hydrogen peroxide and hydrochloric acid are added in sequence or added after premixing.
7. The method for rapidly detecting low-content silicon in aluminum and aluminum alloys according to claim 6, wherein the method comprises the following steps: in the step 1), the hydrogen peroxide and the hydrochloric acid are added in a mode of adding the hydrogen peroxide firstly and then adding the hydrochloric acid in batches.
8. The method for rapidly detecting low-content silicon in aluminum and aluminum alloys according to claim 1, wherein the method comprises the following steps: the reagent is selected from a reagent with superior purity, analytical purity or chemical purity.
9. The method for rapidly detecting low-content silicon in aluminum and aluminum alloys according to claim 1, wherein the method comprises the following steps: in the step 2), the low-temperature heating and boiling temperature is less than 280 ℃.
10. The method for rapidly detecting low-content silicon in aluminum and aluminum alloys according to claim 1, wherein the method comprises the following steps: in the step 3), the water for dilution is primary or secondary deionized water or distilled water.
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