Detection method for measuring carbon content in ferrotitanium by using infrared carbon-sulfur instrument

Abstract

The invention relates to the technical field of physical and chemical detection, in particular to a method for detecting the content of carbon in ferrotitanium through an infrared carbon and sulfur instrument. The method mainly comprises the following steps: 1) crucible pretreatment: putting a crucible in a muffle furnace, preserving heat at 800-1400 DEG C for 1-3 hours, and then putting the crucible in a dryer for storage for no more than 24 hours; (2) pretreating the ferrotitanium sample, namely crushing the ferrotitanium sample to 80-120 meshes by using grinding equipment; and 3) detection by an infrared carbon-sulfur analyzer: adding part of the fluxing agent into the crucible pretreated in the step 1), putting a to-be-detected sample, uniformly covering the to-be-detected sample with the remaining fluxing agent, and putting the to-be-detected sample on the infrared carbon-sulfur analyzer for analysis. According to the detection method, the carbon content in ferrotitanium can be rapidly and accurately measured, the analysis result is stable and reliable, the labor intensity of post personnel is relieved, and the working efficiency is improved; according to the method, the ferrotitanium sample is crushed to 80-120 meshes, so that the particles are uniform, and the determination result is ensured.

Description

Technical Field

[0001] This invention relates to the field of physicochemical testing technology, and in particular to a method for determining the carbon content in ferrotitanium using an infrared carbon-sulfur analyzer. Background Technology

[0002] Ferrotitanium is an alloy with a titanium content between 25% and 75%, and it is one of the most widely used binary ferroalloys. Currently, ferrotitanium alloys are important raw materials for the production of chain steel, anchor chain steel, shipbuilding steel, stainless steel, welding electrodes, and electronic and military products. Ferrotitanium is mainly used as a deoxidizer and degassing agent in steelmaking. Besides the titanium content, the carbon content is a crucial and mandatory indicator for the quality of ferrotitanium.

[0003] Currently, conventional methods for determining the carbon content in ferrotitanium suffer from large fluctuations in values, poor accuracy, and inadequate precision. There is a need to research a new method for determining the carbon content in ferrotitanium, optimize detection parameters, and provide faster and more accurate analytical results. Summary of the Invention

[0004] To overcome the shortcomings of existing technologies, the technical problem solved by this invention is to provide a detection method for determining the carbon content in ferrotitanium using an infrared carbon-sulfur analyzer, thereby solving the problems of large fluctuations in the carbon content values, poor accuracy, and poor precision in the determination of ferrotitanium.

[0005] To achieve the above objectives, the present invention employs the following technical solution:

[0006] A method for determining the carbon content in ferrotitanium using an infrared carbon-sulfur analyzer mainly includes the following steps:

[0007] 1) Crucible pretreatment:

[0008] Place the crucible in a muffle furnace and keep it at 800–1400℃ for 1–3 hours. Then store it in a desiccator for no more than 24 hours.

[0009] 2) Pretreatment of titanium-iron samples:

[0010] The ferrotitanium sample was pulverized to 80–120 mesh using a grinding device;

[0011] 3) Infrared carbon and sulfur analyzer detection:

[0012] Add some flux to the pretreated crucible in step 1), place the test sample in it, evenly cover it with the remaining flux, and place it on an infrared carbon-sulfur analyzer for analysis.

[0013] In step 1), the crucible is placed in a muffle furnace and kept at 1200℃ for 2 hours, and then dried and stored for 15 hours.

[0014] The grinding equipment mentioned in step 2) is a vertical spiral stirred mill or a vibrating ball mill.

[0015] The flux mentioned in step 3) is one or a mixture of two or more of tungsten granules, tin granules, and industrial pure iron.

[0016] The flux is a mixture of tungsten granules, tin granules and industrial pure iron in a mass ratio of (10-12):(1-3):(3-5).

[0017] In step 3), the operating conditions for the infrared carbon-sulfur analyzer are: carrier flow rate 2-4 L / min, carrier gas pressure 25-45 psi, and power gas pressure 30-50 psi.

[0018] In step 3), the analysis time is 20–60 s, and the comparison level is 1–3.

[0019] Compared with the prior art, the beneficial effects of the present invention are:

[0020] The detection method of the present invention can quickly and accurately determine the carbon content in ferrotitanium, and the analysis results are stable and reliable, reducing the labor intensity of personnel and improving work efficiency; the ferrotitanium sample of the present invention is crushed to 80-120 mesh to ensure uniform particle size and guarantee the measurement results. Detailed Implementation

[0021] The specific embodiments of the present invention will be further described below:

[0022] Example

[0023] This invention provides a method for determining the carbon content in ferrotitanium using an infrared carbon-sulfur analyzer, which mainly includes the following steps:

[0024] 1) Crucible pretreatment:

[0025] The crucible was placed in a muffle furnace and kept at 1200℃ for 2 hours, and then stored in a desiccator for 15 hours. This treatment effectively avoids secondary contamination and results in a low and relatively stable blank value.

[0026] 2) Pretreatment of titanium-iron samples:

[0027] The ilmenite sample was pulverized to 80-120 mesh using a vertical spiral stirred mill or a vibrating ball mill.

[0028] 3) Infrared carbon and sulfur analyzer detection:

[0029] ①The operating conditions of the infrared carbon-sulfur analyzer are shown in Table 1 below:

[0030] Table 1 Working Conditions

[0031]

[0032] ② Selection of cosolvents

[0033] The role of flux in carbon and sulfur analysis is to lower the melting point of the sample, increase the combustion temperature, and prevent sample splashing. Commonly used fluxes include one or more of tungsten granules, tin granules, and pure iron. Multiple analyses were performed on a standard sample YSBC19605-05 with a carbon content of 0.032% using these fluxes, and the average value was taken.

[0034] The experimental procedure was as follows: standard samples were weighed and placed in a crucible that had been kept in a muffle furnace at 1200℃ for 2 hours. Then, 2g of tungsten granules, 2g of tin granules, 1g of tungsten granules + 1g of tin granules, and 1.2g of tungsten granules + 0.3g of tin granules + 0.5g of pure iron were added. The samples were analyzed on an infrared carbon-sulfur analyzer. The results are shown in Table 2.

[0035] Table 2. Flux Experimental Results

[0036]

[0037] This shows that the measured values ​​are low and the stability is poor when using tungsten granules, tin granules or tungsten-tin mixed flux. Therefore, industrial pure iron is added as a flux when using tungsten-tin mixed flux.

[0038] ③ Selection of sample weight for ferrotitanium samples

[0039] The sample weight of ferrotitanium has a certain impact on the accuracy of the analytical results. The main reason is that if the sample weight is too low, the sample will have low representativeness, while if the sample weight is too high, the analytical results will be lower due to the poor melting of the sample. The following are the results of the symmetrical sample weight test using the standard sample YSBC19605-05 with a carbon content of 0.032%, as shown in Table 3.

[0040] Table 3 shows the results of the test on the sample size.

[0041]

[0042]

[0043] By comparing the average value and the relative standard deviation, a sample weight of 0.5g is preferred.

[0044] ④ Selection of analysis time and comparison level

[0045] The analysis time of the sample is determined by both the analysis time and the comparison level in the analytical method, generally ranging from 20 to 60 seconds. In actual testing, the integral curve on the computer screen should be observed. If tailing occurs, the comparison level should be appropriately increased to avoid affecting the analytical results due to excessive blank levels. Table 4 shows the results of experiments using the standard sample QD16-251 with a carbon content of 0.047% at analysis times of 20, 30, 40, 50, and 60 seconds to test the comparison level.

[0046] Table 4. Results of the analysis time and comparison level test

[0047]

[0048] Based on the above data and integral curve analysis, an analysis time of 50 seconds and a comparison level of 2 were selected.

[0049] ⑤ Accuracy Experiment

[0050] Accuracy tests were conducted using standard samples YSBC19605-05, QD17-265, YSBC19604-05, and QD16-251. 0.5g of the sample was weighed and placed in a crucible that was kept at 1200℃ for 2 hours. 1.2g of tungsten granules, 0.3g of tin granules, and 0.5g of pure iron were added. The instrument analysis time was set to 50s, and the comparison level was 2. The experimental results are shown in Table 5.

[0051] Table 5. Accuracy Experiment Results

[0052]

[0053] Based on the experimental data above, it can be seen that the method has good accuracy.

[0054] ⑥ Determination of carbon content in ferrotitanium samples

[0055] Three pretreated ferrotitanium samples, numbered 1#, 2#, and 3#, were weighed, each weighing 0.5g. 1.2g of tungsten granules, 0.3g of tin granules, and 0.5g of pure iron were added as flux. The analysis time was set to 50s, the comparison level to 2, and the analysis was performed using a CS-600 infrared carbon-sulfur analyzer. The results are shown in Table 6.

[0056] Table 6. Results of carbon content determination in ferrotitanium samples

[0057]

[0058]

[0059] As can be seen from the table, the sample analysis results are good and the precision is relatively good.

[0060] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited to the specific details of the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solutions of the present invention, and these simple modifications all fall within the protection scope of the present invention. Furthermore, it should be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. To avoid unnecessary repetition, the present invention will not describe the various possible combinations separately. In addition, various different embodiments of the present invention can also be arbitrarily combined, as long as they do not violate the spirit of the present invention, they should also be considered as the content disclosed by the present invention.

Claims

1. A method for determining the carbon content in ferrotitanium using an infrared carbon-sulfur analyzer, characterized in that, The main steps include the following: 1) Crucible pretreatment: Place the crucible in a muffle furnace and keep it at 800–1400℃ for 1–3 hours. Then store it in a desiccator for no more than 24 hours. 2) Pretreatment of titanium-iron samples: The ferrotitanium sample was pulverized to 80–120 mesh using a grinding device; 3) Infrared carbon and sulfur analyzer detection: Add some flux to the pretreated crucible in step 1), place the test sample in it, evenly cover it with the remaining flux, and place it on an infrared carbon-sulfur analyzer for analysis.

2. The method for determining the carbon content in ferrotitanium using an infrared carbon-sulfur analyzer according to claim 1, characterized in that, In step 1), the crucible is placed in a muffle furnace and kept at 1200℃ for 2 hours, and then dried and stored for 15 hours.

3. The method for determining the carbon content in ferrotitanium using an infrared carbon-sulfur analyzer according to claim 1, characterized in that, The grinding equipment mentioned in step 2) is a vertical spiral stirred mill or a vibrating ball mill.

4. The method for determining the carbon content in ferrotitanium using an infrared carbon-sulfur analyzer according to claim 1, characterized in that, The flux mentioned in step 3) is one or a mixture of two or more of tungsten granules, tin granules, and industrial pure iron.

5. The method for determining the carbon content in ferrotitanium using an infrared carbon-sulfur analyzer according to claim 4, characterized in that, The flux is a mixture of tungsten granules, tin granules and industrial pure iron in a mass ratio of (10-12):(1-3):(3-5).

6. The method for determining the carbon content in ferrotitanium using an infrared carbon-sulfur analyzer according to claim 1, characterized in that, In step 3), the operating conditions for the infrared carbon-sulfur analyzer are: carrier flow rate 2-4 L / min, carrier gas pressure 25-45 psi, and power gas pressure 30-50 psi.

7. The method for determining the carbon content in ferrotitanium using an infrared carbon-sulfur analyzer according to claim 1, characterized in that, In step 3), the analysis time is 20–60 s, and the comparison level is 1–3.

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