Method for rapidly determining content of carbon and sulfur in aluminum wires and aluminum particles

Abstract

The invention discloses a method for rapidly determining the content of carbon and sulfur in an aluminum wire and an aluminum particle, which comprises the following steps: introducing oxygen into a high-frequency induction furnace in the presence of a fluxing agent, combusting the sample at high temperature, generating carbon monoxide and carbon dioxide gas when carbon meets oxygen, and generating sulfur dioxide gas by sulfur; the mixed gas enters a sulfur infrared pool to measure the sulfur content; sulfur dioxide is subjected to catalytic oxidation to generate sulfur trioxide and is absorbed; and the residual gas enters a carbon infrared pool to measure the carbon content. The invention aims to provide an analysis method for determining the content of carbon and sulfur in aluminum wires and aluminum particles by a high-frequency-infrared absorption method, which is a rapid, accurate and economical method for determining the content of carbon and sulfur in aluminum wires and aluminum particles.

Description

Technical Field

[0001] The invention relates to the technical field of metallurgical analysis, and in particular to a method for rapidly determining carbon and sulfur contents in aluminum wires and aluminum particles. Background Art

[0002] With the smelting of clean steel, the cleanliness control of steel runs through the entire steelmaking process. In order to control the sulfur and oxygen content in steel during the steelmaking process, aluminum wire and aluminum particles are used as deoxidizers to achieve the purpose of deoxidation and sulfur control. Therefore, it is very important to quickly and accurately determine the components of carbon and sulfur. At present, the high-frequency combustion-infrared absorption method is widely used in the analysis of carbon and sulfur in various materials due to its simple and rapid operation, accurate and reliable methods. Ren Xudong et al. described the use of tungsten, tin, iron, molybdenum, and nickel five-element flux in the document "Determination of Carbon and Sulfur Content in Ferrosilicon by High-Frequency Combustion-Infrared Absorption Method Based on Five-element Flux". The method uses a large amount of flux, which will splash violently when the sample burns, causing blockage of the pipeline, reducing the accuracy of the analysis, and wasting materials. So far, all literature has rarely reported on the carbon and sulfur content in aluminum wire and aluminum particles.

[0003] Since aluminum wire and aluminum particles have weak magnetic conductivity and high melting temperature, the plate flow is low during high-frequency induction, the combustion effect is poor, and a large amount of flux is required for analysis. This patent is aimed at the selection of the amount of flux used, and establishes a method for quickly, accurately and economically determining the carbon and sulfur content in aluminum wire and aluminum particles, which has important practical significance. Summary of the invention

[0004] In order to solve the above technical problems, the purpose of the present invention is to provide an analytical method for determining the carbon and sulfur content in aluminum wire and aluminum particles by high-frequency-infrared absorption method, which is a fast, accurate and economical method for determining the carbon and sulfur content in aluminum wire and aluminum particles.

[0005] In order to solve the above technical problems, the present invention adopts the following technical solutions:

[0006] The invention discloses a method for rapidly determining the carbon and sulfur contents in aluminum wires and aluminum particles, comprising: introducing oxygen into a sample in a high-frequency induction furnace in the presence of a flux, the sample burning at a high temperature, carbon generating carbon monoxide and carbon dioxide gas when meeting oxygen, and sulfur generating sulfur dioxide gas; the mixed gas entering a sulfur infrared cell to determine the sulfur content; sulfur dioxide generating sulfur trioxide through catalytic oxidation and absorbing; and the remaining gas entering a carbon infrared cell to determine the carbon content.

[0007] Further, the specific steps include:

[0008] Collect the carbon and sulfur in a special crucible, place it in a muffle furnace at 1050-1150℃ and burn it for 1.5-2.5h. After the muffle furnace cools naturally, place it in a dryer for later use;

[0009] Step 1: Blank determination: Add 0.5g of tin flux, 1.2g of pure iron flux and 1.3g of tungsten flux to the carbon-sulfur crucible, manually input the sample weight as 1.000g and place it in the infrared carbon-sulfur instrument for determination. Measure in the same channel, repeat the measurement enough times to obtain low and relatively consistent readings, record the minimum three readings, calculate the average value, and input it into the instrument. The instrument will perform electronic compensation for the blank value when measuring the sample;

[0010] Step 2: Calibrate the working curve. Weigh 0.1-0.2g of aluminum iron or silicon iron standard sample with high carbon and sulfur content into a carbon-sulfur crucible, automatically input the actual weight of the sample, evenly cover the sample with 0.5g of tin flux, 1.2g of pure iron flux and 1.3g of tungsten flux, and place it in an infrared carbon-sulfur analyzer for measurement. Record the sulfur analysis value. Repeat the measurement three times. The three measurement values ​​are within the tolerance of each other. Input the certified value of the standard sample into the carbon-sulfur analyzer for calibration curve and calculation of the correction factor.

[0011] Step 3: Weigh two standard samples with different carbon and sulfur contents of 0.1-0.2g into the carbon-sulfur crucible, input the actual weight of the sample automatically, evenly cover the sample with 0.5g tin flux, 1.2g pure iron flux and 1.3g tungsten flux, and place it in the infrared carbon-sulfur instrument for measurement. The measured value and the certified value are within the allowable error range.

[0012] Step 4: Weigh 0.1-0.2g of aluminum wire and aluminum granule samples into a regeneration crucible, automatically input the actual weight of the sample, and evenly cover the sample with 0.5g of tin flux, 1.2g of pure iron flux and 1.3g of tungsten flux. The carbon and sulfur analysis values ​​displayed on the instrument are the measurement results of the sample.

[0013] Further, it was placed in a muffle furnace at 1100°C for 2 h.

[0014] Furthermore, in step 1, the measurement is repeated 5 to 6 times to obtain a low and relatively consistent reading.

[0015] Furthermore, the method is accurate and fast in measurement.

[0016] Compared with the prior art, the beneficial technical effects of the present invention are:

[0017] The present invention is used for the determination of carbon and sulfur in aluminum wire and aluminum particles. The aluminum wire and aluminum particles are burned at high temperature with a tungsten flux, and a small amount of 0.5g of tin flux and 1.2g of pure iron flux are used to completely decompose the aluminum wire and aluminum particles, and the carbon and sulfur release rate in the sample is high. The present invention uses a high-frequency-infrared absorption method to determine the carbon and sulfur content in aluminum wire and aluminum particles and provides accurate data. The present invention can be used for detection and analysis in the metallurgical industry and related scientific research institutes, and provides an accurate and rapid analysis and detection method for personnel engaged in the detection and analysis of carbon and sulfur in aluminum wire and aluminum particles. DETAILED DESCRIPTION

[0018] The present invention will be further described below in conjunction with specific embodiments.

[0019] Place the carbon-sulfur professional crucible in a muffle furnace at 1100°C and burn it for 2 hours. After natural cooling in the muffle furnace, place it in a dryer for later use.

[0020] Weigh the sample 0.1~0.2g.

[0021] Blank determination: Add the same amount of flux as required for analyzing the sample into an empty crucible, set the sample weight to 1.0000g, perform the determination in the same channel, repeat the determination 5 times, and record the carbon and sulfur analysis values ​​as the blank values ​​of the flux. Enter the blank values ​​of carbon and sulfur into the instrument, and they will be automatically deducted in the subsequent analysis operations.

[0022] Calibration working curve: Weigh standard samples of medium and low alloy steel (or ferrosilicon) with high carbon and sulfur content into a crucible, automatically input the actual weight of the sample, add flux and place it in an infrared carbon-sulfur analyzer for measurement, record the sulfur analysis value, repeat the measurement three times, and the three measurement values ​​should be within the tolerance of each other. The certified value of the standard sample is input into the carbon-sulfur analyzer for calibration curve and calculation of the correction factor.

[0023] Weigh 0.1-0.2g of aluminum particles and aluminum wire samples into a regeneration crucible, automatically input the actual weight of the sample, add tungsten flux and place it in an infrared carbon-sulfur analyzer for measurement. The carbon and sulfur analysis values ​​displayed by the instrument are the measurement results of the sample.

[0024] Example 1

[0025] According to the above method, the standard sample ferrosilicon (GBW01432, C: 0.024%, S: 0.0037%) was weighed to calibrate the sulfur standard curve, and then the ferrosilicon standard (BH0301-4), industrial pure iron standard (BH1502-1), carbon sulfur special steel standard (YSBC11114-94) and aluminum wire and aluminum grain samples were measured. The results are shown in Table 1. 12 portions of aluminum wire sample 1# were weighed and precision tested according to the experimental method. The test results are shown in Table 2.

[0026] Table 1 Sample measurement results (%)

[0027]

[0028] Table 2 Determination results of carbon and sulfur content in aluminum wire (%)

[0029]

[0030] Therefore, through the verification of the above-mentioned implementation examples, it can be seen that the present invention is used for the determination of carbon and sulfur in aluminum particles and aluminum wires. The alloy generated by the high-temperature combustion of aluminum particles and aluminum wires with suitable tin and pure iron flux and tungsten has strong high-frequency induction, can quickly increase the melting temperature of the sample, make the sample burn completely, and has a high carbon and sulfur release rate. The sample can be completely decomposed using a small amount of flux.

[0031] The method of using different standards to calibrate carbon and sulfur curves is used to determine the carbon and sulfur contents in aluminum particles and aluminum wires, which solves the difficulties in daily analysis caused by the lack of suitable standard substances for aluminum particles and aluminum wires, thereby accurately determining the carbon and sulfur contents in samples and providing accurate data for scientific research and production.

[0032] The embodiments described above are only descriptions of the preferred modes of the present invention, and are not intended to limit the scope of the present invention. Without departing from the design spirit of the present invention, various modifications and improvements made to the technical solutions of the present invention by ordinary technicians in this field should all fall within the protection scope determined by the claims of the present invention.

Claims

1. A method for rapidly determining the carbon and sulfur content in aluminum wire and aluminum particles, characterized in that: include: In the presence of flux, oxygen is introduced into the sample in a high-frequency induction furnace. The sample burns at high temperature, and carbon generates carbon monoxide and carbon dioxide gas when it meets oxygen, and sulfur generates sulfur dioxide gas. The mixed gas enters the sulfur infrared cell to determine the sulfur content. Sulfur dioxide is catalytically oxidized to generate sulfur trioxide and is absorbed. The remaining gas enters the carbon infrared cell to determine the carbon content.

2. The method for rapidly determining the carbon and sulfur content in aluminum wire and aluminum particles according to claim 1, characterized in that: The specific steps include: Collect the carbon and sulfur in a special crucible, place it in a muffle furnace at 1050-1150℃ and burn it for 1.5-2.5h. After the muffle furnace cools naturally, place it in a dryer for later use; Step 1: Blank determination: Add 0.5g of tin flux, 1.2g of pure iron flux and 1.3g of tungsten flux to the carbon-sulfur crucible, manually input the sample weight as 1.000g and place it in the infrared carbon-sulfur instrument for determination. Measure in the same channel, repeat the measurement enough times to obtain low and relatively consistent readings, record the minimum three readings, calculate the average value, and input it into the instrument. The instrument will perform electronic compensation for the blank value when measuring the sample; Step 2: Calibrate the working curve. Weigh 0.1-0.2g of aluminum iron or silicon iron standard sample with high carbon and sulfur content into a carbon-sulfur crucible, automatically input the actual weight of the sample, evenly cover the sample with 0.5g of tin flux, 1.2g of pure iron flux and 1.3g of tungsten flux, and place it in an infrared carbon-sulfur analyzer for measurement. Record the sulfur analysis value. Repeat the measurement three times. The three measurement values ​​are within the tolerance of each other. Input the certified value of the standard sample into the carbon-sulfur analyzer for calibration curve and calculation of the correction factor. Step 3: Weigh two standard samples with different carbon and sulfur contents of 0.1-0.2g into the carbon-sulfur crucible, input the actual weight of the sample automatically, evenly cover the sample with 0.5g tin flux, 1.2g pure iron flux and 1.3g tungsten flux, and place it in the infrared carbon-sulfur instrument for measurement. The measured value and the certified value are within the allowable error range. Step 4: Weigh 0.1-0.2g of aluminum wire and aluminum granule samples into a regeneration crucible, automatically input the actual weight of the sample, and evenly cover the sample with 0.5g of tin flux, 1.2g of pure iron flux and 1.3g of tungsten flux. The carbon and sulfur analysis values ​​displayed on the instrument are the measurement results of the sample.

3. The method for rapidly determining the carbon and sulfur content in aluminum wire and aluminum particles according to claim 2, characterized in that: Place it in a muffle furnace at 1100℃ and burn it for 2h.

4. The method for rapidly determining the carbon and sulfur content in aluminum wire and aluminum particles according to claim 2, characterized in that: In step 1, the measurement is repeated 5 to 6 times to obtain low and relatively consistent readings.

5. The method for rapidly determining the carbon and sulfur content in aluminum wire and aluminum particles according to claim 2, characterized in that: This method is accurate and fast.

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