Preparation method and detection method of total carbon content test solution in titanium tetrachloride

Abstract

The invention discloses a preparation method and a detection method of a total carbon content test solution in titanium tetrachloride, and belongs to the technical field of component detection and analysis. The preparation method and the detection method comprise the following steps: adding water into a titanium tetrachloride sample to fully react, and heating and evaporating the obtained product to dryness at the temperature of not higher than 90 DEG C; then adding a hydrofluoric acid solution and a proper amount of water, heating and dissolving at the temperature of not higher than 80 DEG C to obtain a clear and transparent solution, and adding water to dilute and fix the volume to obtain the solution for testing the total carbon content in the titanium tetrachloride. And fully shaking up the test solution, and then immediately determining the total carbon content in the solution by adopting ICP-MS or ICP-OES (Inductively Coupled Plasma-Mass Spectrometry). The method disclosed by the invention is simple and rapid to operate, small in reagent dosage and low in test solution acidity, and can effectively solve the problems that coexisting components such as high-concentration Cl <-> and H < + > in the TiCl4 sample solution interfere a detection result and corrode an instrument.

Description

Technical Field

[0001] The present invention belongs to the technical field of component detection and analysis, and relates to a preparation method and a detection method of a test solution for total carbon content in titanium tetrachloride, and specifically to a preparation method and an analysis method of a sample test solution for detecting the total carbon content in organic and inorganic carbon-containing compounds in titanium tetrachloride. Background Art

[0002] Currently, the mainstream production process for titanium metal and titanium dioxide uses a chlorination process to produce crude TiCl4 from high-titanium slag. This crude TiCl4 is then refined to obtain refined TiCl4. The refined TiCl4 is then reduced with active magnesium to produce titanium sponge, which is then used to manufacture various titanium metal and titanium alloy materials. Because impurities contained in refined TiCl4 after reduction to titanium sponge are difficult to remove, and impurities in refined TiCl4 are enriched and transferred to titanium sponge at a four-fold ratio, the quality of refined TiCl4 determines the quality of the titanium sponge product.

[0003] During the distillation and rectification process to produce refined TiCl4, impurities in crude TiCl4, with a separation coefficient close to 1, remain in the refined TiCl4, significantly impacting the quality of the end-product, titanium sponge. Therefore, appropriate impurity removal processes must be implemented to remove the impurities contained in crude TiCl4. Currently, the development of mineral oil-based impurity removal to produce high-quality refined TiCl4 is a hot topic of research both domestically and internationally. However, the key to this technology lies in resolving the problem of excessive carbon content in titanium sponge due to residual organic impurities in the TiCl4 when using various mineral oils.

[0004] In order to effectively monitor the quality of TiCl4 and guide the removal of organic impurities, it is necessary to study and master the detection and analysis technology of the total carbon content in organic and inorganic carbon-containing compounds in TiCl4. The analytical technology for detecting organic impurities in TiCl4 is still in the exploratory research stage both at home and abroad, and there is no mature and reliable analytical method. Currently, organic analysis methods such as infrared spectroscopy, gas chromatography, headspace extraction / gas chromatography-mass spectrometry are mainly used to detect individual carbon-containing components such as CCl4 and CO2 in TiCl4. Alternatively, the content of each organic molecule is determined by infrared spectroscopy, gas chromatography-mass spectrometry, etc., and the carbon content of each substance is calculated one by one according to its molecular formula. Finally, the carbon content of each component is added together to obtain the total carbon content in TiCl4. However, these methods are very complicated to operate, have many interfering factors, long inspection cycles, and large analytical errors.

[0005] For example, the document "Determination of Impurity Elements in Titanium Tetrachloride Liquid by Inductively Coupled Plasma Atomic Emission Spectrometry" dilutes the TiCl4 sample solution with relatively high concentrations of dilute hydrochloric acid or dilute nitric acid, and uses inductively coupled plasma atomic emission spectrometry (ICP-OES) to determine inorganic impurity elements such as Si, Fe, V, and Al. However, the ICP-OES detection method used in this method is limited by its performance indicators such as the lower limit of detection and cannot meet the requirements for the determination of trace and micro carbon content. In addition, the sample pretreatment method of using a large amount of high-concentration dilute hydrochloric acid solution to dilute TiCl4 will cause the concentration of hydrogen ions and chloride ions in the test solution to be far higher than the upper limit that the ICP-OES can tolerate, resulting in a significant impact of matrix effects and mass spectrometry interference on the accuracy of the results, and serious corrosion of valuable components such as the interface cone of the ICP-MS instrument.

[0006] Therefore, developing a method that can accurately, quickly and simply detect the total carbon content in TiCl4 has important practical significance and application value for improving the quality of refined TiCl4 and thus improving the quality of sponge titanium products. Summary of the Invention

[0007] The technical problem to be solved by the present invention is that during the TiCl4 detection process, high concentration Cl - 、H + The reliability of the test results is affected by matrix effects, acidity effects, mass spectrometry interference, etc., as well as the corrosion of the detection instrument caused by strong acidic medium solutions.

[0008] To achieve the above application objectives, the technical solutions adopted in this application are as follows:

[0009] First, in order to completely eliminate the high concentration of Cl in the TiCl4 sample solution - 、H + The present invention provides a method for preparing a solution for testing the total carbon content in titanium tetrachloride, comprising the following steps:

[0010] S1. Add an appropriate amount of water to the titanium tetrachloride sample to be tested and allow to react at room temperature until a large amount of thick white smoke is no longer produced;

[0011] S2. The product obtained in step S1 is heated and evaporated to dryness at a temperature not higher than 90°C to obtain a titanium-based solid mainly composed of anatase-type titanium dioxide;

[0012] S3. Add hydrofluoric acid solution and an appropriate amount of water to the titanium-based solid obtained in step S2, and heat at a temperature not higher than 80 ° C until the titanium matrix is ​​completely dissolved to obtain a clear and transparent solution;

[0013] S4. After the solution obtained in step S3 is cooled, water is added to dilute the solution to a fixed volume to obtain a test solution for the total carbon content in titanium tetrachloride with a hydrofluoric acid concentration of less than 1%.

[0014] First, the present invention makes full use of the property that TiCl4 is easily hydrolyzed in water to generate titanium precipitate and a large amount of HCl smoke, providing a simple, fast and efficient method for removing Cl in TiCl4. - 、H + The sample test solution pretreatment preparation method of coexisting components is as follows. By adding water to the TiCl4 sample and controlling the hydrolysis reaction conditions, Cl - and H + It escapes in the form of volatile HCl; then it is heated at low temperature until the solution evaporates to dryness, further promoting the Cl - and H + At the same time, by controlling the hydrolysis temperature and reaction extent, the generated titanium dioxide precipitates into an anatase crystal structure, facilitating its rapid and complete dissolution by a small amount of hydrofluoric acid. Studies have found that anatase titanium dioxide has a high solubility, but high temperature or prolonged hydrolysis can cause it to transform into rutile. Therefore, the present invention chooses to carry out the hydrolysis reaction at room temperature, stop the reaction immediately after no large amount of thick white smoke is produced, and heat and evaporate to dryness at a low temperature to avoid changes in the titanium dioxide crystal structure.

[0015] In the above step S1, the volume ratio of the titanium tetrachloride sample to be tested to water is 1:1 to 1:5.

[0016] In step S1 above, adding water to the titanium tetrachloride sample triggers a vigorous hydrolysis reaction, resulting in the rapid release of a large amount of HCl gas. To avoid an excessively vigorous reaction, water should be added dropwise to the titanium tetrachloride slowly to control the reaction rate and prevent safety issues caused by the release of large amounts of HCl gas. This also prevents volatile carbon impurities from escaping and being lost along with the HCl gas during the vigorous hydrolysis process.

[0017] In the above step S2, the heating temperature is 60-90°C.

[0018] In the above step S3, the volume ratio of the titanium tetrachloride sample to be tested to the hydrofluoric acid solution is 1:1 to 2:1.

[0019] In the above step S3, the concentration of the hydrofluoric acid solution is ≥40%.

[0020] In the above step S3, the amount of water added should ensure that the titanium-based solid is completely dissolved.

[0021] In the above step S3, the heating temperature is 50-80°C.

[0022] In the above step S4, the volume ratio of the titanium tetrachloride sample to be tested to the total carbon content test solution in titanium tetrachloride is 1:50 to 1:200.

[0023] In the early experiments, the present invention tried to use reagents such as nitric acid to dissolve the titanium-based precipitate. The results showed that the titanium-based precipitate was not completely dissolved and the acid-insoluble particles needed to be removed by centrifugation or filtration. This will inevitably lead to the loss of the component to be tested due to inclusion, encapsulation or adsorption in the insoluble particles, thereby affecting the accuracy of the test results. At the same time, in order to avoid the high concentration of titanium matrix that is re-dissolved from being hydrolyzed again during the dilution process to form a precipitate, it is necessary to dilute the constant volume test solution with a dilute nitric acid solution. The principle is to maintain a high H + This method is essentially to replace the hydrochloric acid in TiCl4 with reagents such as nitric acid, eliminating Cl - The interference of ions was eliminated, but the acidity of the test solution was not effectively reduced, so the corrosion effect on the instrument still existed. In addition, the incomplete dissolution of the hydrolysis precipitate can lead to the loss of the components to be tested, and the large amount of reagents such as nitric acid increases the analysis cost and the background contamination of the reagent blank interferes with the test results.

[0024] In addition, the present invention reduces the volatilization loss of HF by controlling the temperature of the dissolution reaction, and - With Ti 4 + The titanium matrix is ​​fully complexed to achieve rapid dissolution of the titanium-based precipitate, so that the titanium matrix exists in the low-acidity medium solution in the form of a stable complex ion. At the same time, the high-concentration titanium matrix can remain stable in a low-acidity environment, effectively inhibiting the occurrence of hydrolysis reactions. The use of low-concentration, small-dose hydrofluoric acid can quickly and completely dissolve the titanium-based precipitate, and the resulting solution is clear and transparent, without acid-insoluble residues and suspended or settled insoluble particles. The loss caused by the insoluble precipitate encapsulating and entangling the components to be tested is avoided, and there is no need to separate the insoluble particles by means of filtration or centrifugation, which fundamentally solves the problem of clogging of the detection instrument. In addition to the titanium matrix, the prepared sample test solution contains only less than 1% HF, which significantly reduces the acidity, purifies the coexisting medium system, effectively eliminates the interference of chloride ions, and reduces the corrosion of the instrument by the strong acid medium. At the same time, the evaporation temperature and solution temperature set by the present invention are both lower than the volatilization temperature of the carbon compound, preventing the carbon-containing compound from escaping during the evaporation and dissolution process, thereby ensuring the accuracy of the carbon content determination.

[0025] In a second aspect, the present invention provides a method for detecting a total carbon content test solution in titanium tetrachloride. The test solution is prepared according to the above-mentioned method for preparing a total carbon content test solution in titanium tetrachloride, the solution is thoroughly shaken, and then the total carbon content in the solution is immediately determined using ICP-MS or ICP-OES; the total carbon content includes the dissolved carbon content in the solution and the uniformly dispersed insoluble organic carbon content.

[0026] In addition to the soluble titanium matrix and soluble carbon compounds, the test solution prepared using the above-described method for preparing a solution for testing total carbon content in titanium tetrachloride may also contain water- or acid-insoluble organic carbon compounds. Therefore, prior to ICP-MS or ICP-OES analysis, the solution must be thoroughly shaken to ensure that the water- or acid-insoluble organic carbon compounds are evenly distributed throughout the solution, allowing them to be converted into a detectable form during the ICP-MS or ICP-OES analysis.

[0027] The present invention introduces the concept of detecting the total carbon content in organic and inorganic carbon-containing compounds, indirectly characterizing the content levels of organic impurities and inorganic carbon-containing compounds in TiCl4. By adopting a more rapid elemental analysis method, the problem of detecting organic components is solved, and a method for quickly determining trace total carbon using ICP-MS and ICP-OES is established, achieving the goal of determining the quality of TiCl4. Compared with the traditional method of using organic analysis methods such as infrared spectroscopy, gas chromatography, and gas chromatography-mass spectrometry to detect the content of each single organic molecule in the organic mixture contained in the sample, then calculating the carbon content one by one based on its molecular formula, and finally adding the carbon content of each component to obtain the total carbon content in TiCl4, the method of directly determining the total carbon content is simpler and faster, with a shorter analysis process and smaller errors.

[0028] Furthermore, when the total carbon content in titanium tetrachloride is less than or equal to 1 mg / L, ICP-MS is used for detection; the detection parameters are: 12 C is the analytical isotope, No gas mode, 103 Rh was the internal standard calibration element, and the radio frequency power was 1350W.

[0029] Furthermore, when the total carbon content in titanium tetrachloride is greater than 1 mg / L, ICP-OES detection is adopted; the detection parameters are: C 193.091 nm as the analysis spectrum line, and radio frequency power 1350 W.

[0030] Compared with the prior art, the present invention has the following beneficial effects:

[0031] When TiCl4 comes into contact with moisture in the air, it undergoes a hydrolysis reaction, generating titanium precipitates and large amounts of HCl fumes. In traditional TiCl4 test solution preparation, to avoid interference from the hydrolysis reaction of the high-concentration titanium matrix, exposure to moisture is typically minimized to prevent the occurrence of hydrolysis. However, the present invention exploits this hydrolysis property of TiCl4, employing a technical approach that differs radically from conventional methods. This invention involves slowly adding an appropriate amount of water dropwise to the TiCl4 sample, inducing a controlled hydrolysis reaction of the TiCl4. This reaction produces a large amount of HCl gas that escapes in a volatile form, effectively removing chloride and hydrogen ions from the sample. Subsequently, a small amount of HF is added dropwise to the reacted solids to redissolve the generated titanium-based precipitate. The resulting test solution, excluding the titanium matrix, contains only HF at a concentration of less than 1%, resulting in extremely low chloride and hydrogen ion contents. This effectively eliminates chloride ion interference with test results and significantly reduces hydrogen ion corrosiveness to the detection instrument, meeting the test medium requirements of ICP-MS and ICP-OES.

[0032] The method for rapid total carbon determination using ICP-MS or ICP-OES established in this paper not only covers the preparation of the sample test solution but also includes the determination of the total carbon content. The entire process takes only 15 to 30 minutes, significantly shortening the detection cycle compared to traditional methods. The detection scheme of the present invention is simple to operate, efficient and fast, providing a new, simpler, accurate and reliable method for determining the total carbon content in TiCl4, effectively improving the detection efficiency and the accuracy of the test results. DETAILED DESCRIPTION

[0033] In order to make the technical problems, technical solutions and beneficial effects to be solved in the present application clearer, the present application will be further described in detail below in conjunction with the embodiments. It will be understood by those skilled in the art that the following examples are only used to illustrate the present invention and should not be considered as limiting the scope of the present invention. Unless otherwise defined, all scientific and technological terms used herein have the same meanings understood by those of ordinary skill in the art.

[0034] A method for preparing and detecting a solution for testing the total carbon content in titanium tetrachloride comprises the following steps: adding an appropriate amount of water to a titanium tetrachloride sample to be tested, allowing the solution to react fully at room temperature until no more thick white smoke is generated; heating the resulting product to dryness at a temperature not exceeding 90°C to obtain a titanium-based solid primarily composed of anatase-type titanium dioxide; adding a hydrofluoric acid solution and an appropriate amount of water to the titanium-based solid, heating the solution at a temperature not exceeding 80°C until the titanium matrix is ​​completely dissolved, thereby obtaining a clear and transparent solution; after the solution is cooled, diluting the solution with water to a constant volume, thereby obtaining a solution for testing the total carbon content in titanium tetrachloride having a hydrofluoric acid concentration of less than 1%. The solution for testing the total carbon content in titanium tetrachloride is thoroughly shaken, and then the total carbon content in the solution is immediately determined using ICP-MS or ICP-OES; the total carbon content includes the dissolved carbon content in the solution and the uniformly dispersed insoluble organic carbon content.

[0035] In one embodiment of the present invention, the volume ratio of the titanium tetrachloride sample to be tested to the water added during hydrolysis is 1:1 to 1:5. As a non-limiting example, the volume ratio of the titanium tetrachloride sample to be tested to the water added during hydrolysis can be 1:1, 1:2, 1:3, 1:4, 1:5, or any ratio therebetween.

[0036] In one embodiment of the present invention, the temperature of the heating and evaporation is 60-90° C. As a non-limiting example, the temperature of the heating and evaporation is 60° C., 70° C., 80° C., 90° C., or a range consisting of any two of the above values.

[0037] In one embodiment of the present invention, the volume ratio of the titanium tetrachloride sample to be tested to the hydrofluoric acid solution is 1:1 to 2:1. As a non-limiting example, the volume ratio of the titanium tetrachloride sample to be tested to the hydrofluoric acid solution can be 1:1, 2:1, or any ratio therebetween.

[0038] In one embodiment of the present invention, the temperature of the heating and dissolving is 50-80° C. As a non-limiting example, the temperature of the heating and dissolving is 50° C., 60° C., 70° C., 80° C., or a range consisting of any two of the above values.

[0039] In one embodiment of the present invention, the volume ratio of the titanium tetrachloride sample to be tested to the total carbon content in titanium tetrachloride test solution is 1:50 to 1:200. As a non-limiting example, the volume ratio of the titanium tetrachloride sample to be tested to the total carbon content in titanium tetrachloride test solution can be 1:50, 1:60, 1:70, 1:80, 1:90, 1:100, 1:110, 1:120, 1:130, 1:140, 1:150, 1:160, 1:170, 1:180, 1:190, 1:200, or any ratio therebetween.

[0040] Example 1

[0041] (1) 1.0 mL of TiCl4 sample solution (sample 1#) was taken in a 100 mL beaker, 1 mL of water was slowly added dropwise, and the mixture was allowed to react fully at room temperature until no more thick white smoke was produced in the beaker; the beaker was placed on a 60°C low-temperature electric hot plate and heated until the solution evaporated to dryness; 1 mL of 40% HF solution and 15 mL of water were added dropwise, and the mixture was placed on a 50°C low-temperature electric hot plate and heated until the precipitate dissolved to obtain a clear and transparent solution, which was diluted to 100 mL with water to obtain a test solution; the total carbon content in the test solution was determined by ICP-MS, and the detection parameters were: 12 C is the analytical isotope, No gas mode, 103 Rh was the internal standard calibration element, and the radio frequency power was 1350W.

[0042] (2) 1.0 mL of the TiCl4 sample solution (sample 2#) was taken into a 100 mL beaker, and 2.5 mL of water was slowly added dropwise. The mixture was allowed to react fully at room temperature until no more thick white smoke was produced in the beaker. The beaker was placed on a 75°C low-temperature electric hot plate and heated until the solution evaporated to dryness. 0.5 mL of 40% HF solution and 20 mL of water were added dropwise. The mixture was placed on a 70°C low-temperature electric hot plate and heated until the precipitate dissolved, obtaining a clear and transparent solution. The solution was diluted with water to a constant volume of 150 mL to obtain a test solution. The total carbon content in the test solution was determined by ICP-MS using the following detection parameters: 12 C is the analytical isotope, No gas mode, 103 Rh was the internal standard calibration element, and the radio frequency power was 1350W.

[0043] The test solution preparation and total carbon content determination were repeated 8 times according to the above (1) and (2), and the average value and relative standard deviation (RSD) of the 8 measurement results were statistically calculated to evaluate the detection precision level of the method of the present invention. The results are shown in Table 1.

[0044] Table 1 Precision test (n=8)

[0045]

[0046] Example 2

[0047] (3) 1.5 mL of the TiCl4 sample solution (sample 3#) was taken in a 100 mL beaker, and 4.0 mL of water was slowly added dropwise. The mixture was allowed to react fully at room temperature until no more thick white smoke was produced in the beaker. The beaker was placed on an 80°C low-temperature electric hot plate and heated until the solution evaporated to dryness. 1.0 mL of 40% HF solution and 25 mL of water were added dropwise. The mixture was placed on a 70°C low-temperature electric hot plate and heated until the precipitate dissolved, obtaining a clear and transparent solution. The solution was diluted to 100 mL with water to obtain a test solution. The total carbon content in the test solution was determined by ICP-MS using the following detection parameters: 12C is the analytical isotope, No gas mode, 103 Rh was the internal standard calibration element, and the radio frequency power was 1350W.

[0048] (4) 1.0 mL of the TiCl4 sample solution (sample 4#) was taken into a 100 mL beaker, and 3.0 mL of water was slowly added dropwise. The mixture was allowed to react fully at room temperature until no more thick white smoke was produced in the beaker. The beaker was placed on a 60°C low-temperature electric hot plate and heated until the solution was evaporated to dryness. 1.0 mL of HF solution (40%) and 20 mL of water were added dropwise, and the mixture was placed on an 80°C low-temperature electric hot plate and heated until the precipitate dissolved to obtain a clear and transparent solution. The solution was diluted to a constant volume of 200 mL with water to obtain a test solution. The total carbon content in the test solution was determined by ICP-OES using the following detection parameters: C 193.091 nm as the analytical line and RF power 1350 W.

[0049] The test solution preparation and total carbon content determination were repeated 8 times according to the above (3) and (4), and the average value and relative standard deviation (RSD) of the 8 measurement results were statistically calculated to evaluate the detection precision level of the method of the present invention. The results are shown in Table 2.

[0050] Table 2 Precision test (n=8)

[0051]

[0052] As can be seen from Tables 1 and 2, the relative standard deviation (RSD) of the determination results of the method of the present invention is less than 10.0%, indicating that the results of multiple repeated determinations are consistent, the repeatability and reproducibility of the method are good, and the method has a high level of precision.

[0053] Example 3

[0054] The effectiveness of the method of the present invention in solving the problem of chloride ions and hydrogen ions affecting the detection results and causing corrosion to the detection instrument during the detection process of titanium tetrachloride was evaluated.

[0055] 1. Targeting chloride ions

[0056] Determine the chloride ion content in the test solution prepared according to (1) to (4) above by comparing it with the solution without removing Cl - Cl in the test solution - The theoretical concentration of 200 μg / ml was used to evaluate the removal rate of chloride ions by the method of the present invention. The results are shown in Table 3.

[0057] Table 3 Chloride ion removal effect verification test

[0058]

[0059] As can be seen from Table 3, the rate of chloride ion removal by the method of the present invention is greater than 80%, which effectively reduces the corrosion to instruments and equipment and the interference effect on the determination of the components to be treated.

[0060] 2. Targeting hydrogen ions

[0061] The original mother liquor of titanium tetrachloride contains almost no hydrogen ions. In traditional methods, to prevent titanium tetrachloride from hydrolyzing in low-acidity media to form titanium oxide precipitates, large amounts of acid must be added during dilution, introducing a large number of hydrogen ions. These hydrogen ions not only affect the accuracy of test results but can also corrode the testing equipment. The method of the present invention requires only minimal addition of acid during the dilution process, significantly reducing the concentration of introduced hydrogen ions. Compared to traditional methods that use higher acid concentrations for dilution, the method of the present invention reduces hydrogen ion concentration by orders of magnitude.

[0062] Calculations show that the hydrogen ion concentration in the test solution prepared by methods (1) to (4) above is significantly lower than that obtained by conventional methods. This indicates that the method of the present invention can effectively control and significantly reduce the hydrogen ion concentration in the test solution, thereby reducing its interference with the test results and the risk of corrosion to the instrument.

Claims

1. A method for preparing a solution for testing total carbon content in titanium tetrachloride, characterized in that: The steps include: S1. Add an appropriate amount of water to the titanium tetrachloride sample to be tested and allow to react at room temperature until a large amount of thick white smoke is no longer produced; S2. The product obtained in step S1 is heated and evaporated to dryness at a temperature not higher than 90°C to obtain a titanium-based solid mainly composed of anatase-type titanium dioxide; S3. Add hydrofluoric acid solution and an appropriate amount of water to the titanium-based solid obtained in step S2, and heat at a temperature not higher than 80 ° C until the titanium matrix is ​​completely dissolved to obtain a clear and transparent solution; S4. After the solution obtained in step S3 is cooled, water is added to dilute the solution to a fixed volume to obtain a test solution for the total carbon content in titanium tetrachloride with a hydrofluoric acid concentration of less than 1%.

2. The method for preparing a total carbon content test solution in titanium tetrachloride according to claim 1, wherein: In step S1, the volume ratio of the titanium tetrachloride sample to be tested to water is 1:1 to 1:

5.

3. The method for preparing a total carbon content test solution in titanium tetrachloride according to claim 1, wherein: In step S2, the heating temperature is 60-90°C.

4. The method for preparing a total carbon content test solution in titanium tetrachloride according to claim 1, wherein: In step S3, the volume ratio of the titanium tetrachloride sample to be tested to the hydrofluoric acid solution is 1:1 to 2:

1.

5. The method for preparing a total carbon content test solution in titanium tetrachloride according to claim 1, wherein: In step S3, the concentration of the hydrofluoric acid solution is ≥40%.

6. The method for preparing a total carbon content test solution in titanium tetrachloride according to claim 1, wherein: In step S3, the heating temperature is 50-80°C.

7. The method for preparing a total carbon content test solution in titanium tetrachloride according to claim 1, wherein: In step S4, the volume ratio of the titanium tetrachloride sample to be tested to the total carbon content test solution in titanium tetrachloride is 1:50 to 1:

200.

8. A method for detecting the total carbon content in a test solution of titanium tetrachloride, characterized in that: Prepare a total carbon content test solution in titanium tetrachloride according to the preparation method according to any one of claims 1 to 7, shake the solution thoroughly, and then immediately measure the total carbon content in the solution using ICP-MS or ICP-OES; The total carbon content includes the dissolved carbon content in the solution and the uniformly dispersed insoluble organic carbon content.

9. The method for detecting the total carbon content in the titanium tetrachloride test solution according to claim 8, wherein: When the total carbon content in titanium tetrachloride is less than or equal to 1 mg / L, ICP-MS is used for detection; The detection parameters are: 12 C is the analytical isotope, No gas mode, 103 Rh was the internal standard calibration element, and the radio frequency power was 1350W.

10. The method for detecting the total carbon content in titanium tetrachloride according to claim 8, wherein: When the total carbon content in titanium tetrachloride is greater than 1 mg / L, ICP-OES is used for detection; The detection parameters are: C 193.091nm as the analysis line, and radio frequency power 1350W.

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