Titanium tetrachloride test sample preparation device

By using a titanium tetrachloride test sample preparation device that mixes titanium tetrachloride and hydrochloric acid solution in a closed environment, the detection problem caused by the hydrolysis of titanium tetrachloride has been solved, achieving stable sample preparation and high-precision element detection.

CN224189669UActive Publication Date: 2026-05-01PANGANG GROUP VANADIUM & TITANIUM RESOURCES CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
PANGANG GROUP VANADIUM & TITANIUM RESOURCES CO LTD
Filing Date
2025-06-03
Publication Date
2026-05-01

AI Technical Summary

Technical Problem

Titanium tetrachloride is prone to hydrolysis during the detection process, producing corrosive white fumes and heat, which can lead to pipette blockage, sample insolubility, and corrosion of the detection environment, affecting the accuracy and safety of the detection.

Method used

A sample preparation device for titanium tetrachloride is designed. By mixing titanium tetrachloride with hydrochloric acid solution in a closed environment and using inert gas protection to avoid hydrolysis and heat generation, a stable sample solution is prepared.

Benefits of technology

It simplifies the detection process, avoids the hydrochloric acid mist and solid particles generated by exposing samples to air, and improves the accuracy and safety of element detection.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model relates to the field of titanium tetrachloride detection, in particular to a titanium tetrachloride test sample preparation device, which comprises a first container, a second container and a third container, the second container comprises a first liquid inlet and a gas outlet; and the U-shaped pipe comprises a second liquid inlet and a second liquid outlet which are respectively communicated with the first liquid outlet and the first liquid inlet in an airtight manner, and the second liquid inlet and the second liquid outlet of the U-shaped pipe are respectively close to the bottoms of the first container and the second container. According to the system disclosed by the utility model, titanium tetrachloride and a hydrochloric acid solution can be mixed in a closed environment, so that a stable titanium tetrachloride sample is prepared, and the titanium tetrachloride sample mixed with hydrochloric acid cannot generate hydrochloric acid mist, heat and solid particles after meeting air, so that the detection operation is greatly simplified, and the detection efficiency is improved. And carbon deposition cannot be generated during flame combustion detection, so that the element detection accuracy is greatly improved.
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Description

A sample preparation device for titanium tetrachloride testing Technical Field

[0001] This utility model relates to the field of titanium tetrachloride detection, and in particular to a sample preparation device for titanium tetrachloride testing. Background Technology

[0002] Titanium tetrachloride is an important raw material for the production of sponge titanium and titanium dioxide. Trace impurities such as Fe, Si, V, Al, Cr, Ni, Cu, and Co affect the quality of sponge titanium and titanium dioxide, necessitating monitoring of their content. The measurement of trace impurities in titanium tetrachloride is generally performed using a wet method with ICP (Inductively Coupled Plasma Emission Spectrometer). However, titanium tetrachloride is prone to hydrolysis upon contact with air, producing a large amount of corrosive white fumes and generating substantial white titanium hydrate solids. This reaction, accompanied by a significant heat release, can cause problems such as clogging of pipettes during sample transfer, insoluble solid particles during sample dissolution, and the generation of large amounts of heat and hydrochloric acid mist that corrode the testing environment and harm operators. It can also clog the ICP injection system during testing. Current industry practices employ inert gas operation protection and organic solvent protection, but these are inconvenient and introduce organic matter that can cause carbon buildup during ICP flame combustion, clogging the tube and affecting the test results. Summary of the Invention

[0003] To simplify the testing process and improve testing accuracy, this invention proposes a titanium tetrachloride test sample preparation device, comprising: a first container, the first container including an air inlet and a first liquid outlet; a second container, the second container including a first liquid inlet and an air outlet; and a U-shaped tube, the U-shaped tube including a second liquid inlet and a second liquid outlet, the second liquid inlet and the second liquid outlet being airtightly connected to the first liquid outlet and the first liquid inlet, respectively, and the second liquid inlet and the second liquid outlet being located near the bottom of the first container and the second container, respectively, and configured to receive a first solution pressed in by the first container and introduce it into the second container to mix with a second solution in the second container in an airtight environment to obtain a titanium tetrachloride test sample.

[0004] In one or more embodiments, the novel titanium tetrachloride test sample preparation apparatus further includes: an inlet pipe, which is in airtight communication with the inlet port; and an outlet pipe, which is in airtight communication with the outlet port.

[0005] In one or more embodiments, the novel titanium tetrachloride test sample preparation apparatus further includes: a one-way vent valve, wherein the one-way vent valve is airtightly connected to the vent end of the vent pipe.

[0006] In one or more embodiments, the novel titanium tetrachloride test sample preparation apparatus further includes: a gas storage bottle containing compressed inert gas; and a control valve connected between the gas storage bottle and the inlet end of the inlet pipe for controlling the amount of gas supplied to the first container.

[0007] In one or more embodiments, the novel titanium tetrachloride test sample preparation apparatus further includes: an air pump, wherein the outlet end of the air pump is airtightly connected to the inlet end of the air inlet pipe, for controllably supplying air into the first container.

[0008] In one or more embodiments, the novel titanium tetrachloride test sample preparation apparatus further includes a refiner connected to the second outlet of the U-shaped tube.

[0009] In one or more embodiments, the first container stores a titanium tetrachloride solution, and the second container stores a hydrochloric acid solution.

[0010] In one or more embodiments, the first container stores a hydrochloric acid solution, and the second container stores a titanium tetrachloride solution.

[0011] In one or more embodiments, both the first container and the second container include a test tube stopper, the first container defining the air inlet and the first liquid outlet by the test tube stopper, the second container defining the first liquid inlet and the air outlet by the test tube stopper, and the first container and the second container are test tubes.

[0012] In one or more embodiments, the test tube is a graduated test tube.

[0013] The beneficial effects of this invention include: This invention provides a titanium tetrachloride test sample preparation device. This device allows for the mixing of titanium tetrachloride with hydrochloric acid solution in a sealed environment to prepare a stable titanium tetrachloride sample, which is then used for testing. The titanium tetrachloride sample mixed with hydrochloric acid does not produce hydrochloric acid mist upon contact with air, nor does it generate heat or solid particles, thus greatly simplifying the testing operation. Furthermore, it does not produce carbon deposits during flame combustion testing, significantly improving the accuracy of elemental detection. Attached Figure Description

[0014] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other embodiments can be obtained based on these drawings without creative effort.

[0015] Figure 1 is a schematic diagram of the first embodiment of the titanium tetrachloride test sample preparation device of this utility model;

[0016] Figure 2 is a schematic diagram of the second embodiment of the titanium tetrachloride test sample preparation device of this utility model;

[0017] Figure 3 is a schematic diagram of the third embodiment of the titanium tetrachloride test sample preparation device of this utility model.

[0018] The meanings of the reference numerals in the attached drawings are as follows: first container 10, second container 20, U-shaped tube 30, air inlet pipe 40, air outlet pipe 50, one-way air outlet valve 60, air storage cylinder 70, control valve 80, air pump 90, and aerator 100. Detailed Implementation

[0019] To make the objectives, technical solutions, and advantages of this utility model clearer, the embodiments of this utility model will be further described in detail below with reference to specific examples and accompanying drawings.

[0020] It should be noted that all uses of "first" and "second" in the embodiments of this utility model are for the purpose of distinguishing two entities or parameters with the same name but different names. It is clear that "first" and "second" are only for the convenience of expression and should not be construed as limiting the embodiments of this utility model. Subsequent embodiments will not explain this in detail.

[0021] To simplify the detection process and improve accuracy, this invention proposes a titanium tetrachloride sample preparation device. This device first mixes titanium tetrachloride with hydrochloric acid solution in a sealed environment to prepare a stable titanium tetrachloride sample. Then, an elemental analyzer, such as an ICP (Inductively Coupled Plasma Emission Spectrometer), is used to perform elemental analysis on the prepared stable titanium tetrachloride sample. The titanium tetrachloride sample mixed with hydrochloric acid does not produce hydrochloric acid mist upon contact with air, nor does it generate heat or solid particles, thus greatly simplifying the detection process. Furthermore, it does not produce carbon deposits during flame combustion detection, significantly improving the accuracy of elemental analysis.

[0022] The structure of the titanium tetrachloride test sample preparation device of this utility model is shown in Figure 1, including: a first container 10, which includes an air inlet and a first liquid outlet; a second container 20, which includes a first liquid inlet and an air outlet; and a U-shaped tube 30, which includes a second liquid inlet and a second liquid outlet. The second liquid inlet and the second liquid outlet of the U-shaped tube 30 are respectively airtightly connected to the first liquid outlet of the first container 10 and the first liquid inlet of the second container 20. The second liquid inlet and the second liquid outlet of the U-shaped tube 30 are respectively close to the bottom of the first container 10 and the second container 20. The U-shaped tube 30 is configured to receive the first solution pressed in by the first container and introduce the first liquid into the second container to mix with the second solution in the second container in an airtight environment to obtain a titanium tetrachloride test sample.

[0023] Specifically, the titanium tetrachloride test sample preparation device in this embodiment is used to mix titanium tetrachloride solution and hydrochloric acid solution in a closed environment to prepare a sample solution for detection. During use, dry inert gas or air is introduced into the first container 10 through the air inlet to force the first solution in the first container 10 into the second container 20 through the U-tube 30, thus mixing the first solution with the second solution in the second container 20 and completing the sample preparation. For subsequent elemental detection, the prepared sample can be easily transferred from the second container for subsequent testing without exposing the sample to air.

[0024] In one embodiment, the titanium tetrachloride test sample preparation device of the present invention further includes: an air inlet pipe 40, which is in airtight communication with the air inlet of the first container 10; and an air outlet pipe 50, which is in airtight communication with the air outlet of the second container 20.

[0025] Specifically, the inlet pipe 40 and outlet pipe 50 are designed for easy assembly of the titanium tetrachloride test sample preparation device. The inlet pipe 40 and outlet pipe 50 can be made of transparent materials such as glass, PVC, or PET to facilitate observation of the flow and infusion status within the container.

[0026] In an optional embodiment, the first container 10 and the second container 20 can be test tubes, which may be graduated test tubes for easy observation and control of the mixing ratio of the solution. The first container 10 and the second container 20 may each include a test tube stopper. The test tube stopper facilitates opening the communicating vessel and adding the solution to be mixed. The first container 10 defines an air inlet and a first liquid outlet through the test tube stopper, and the second container 20 defines a first liquid inlet and an air outlet through the test tube stopper. In one embodiment, the air inlet and the first liquid outlet are respectively through holes formed on the test tube stopper of the first container 10; similarly, the first liquid inlet and the air outlet are respectively through holes formed on the test tube stopper of the second container 20.

[0027] In one embodiment, the titanium tetrachloride test sample preparation device of this invention further includes a one-way vent valve 60, which is airtightly connected to the vent end of the vent pipe 50. Specifically, the one-way vent valve 60 is used to discharge air from the second container 20 during the liquid infusion process from the first container 10 to the second container 20 to facilitate the smooth infusion process and to prevent external air from entering through the vent of the second container 20, thereby ensuring a sealed sample preparation environment.

[0028] In some embodiments, please refer to Figures 2 and 3. The gas delivery method of this invention includes the following two methods, which depend on the type of solution pre-placed in the first container:

[0029] In one embodiment, the titanium tetrachloride test sample preparation device of this invention further includes: a gas storage cylinder 70, which stores compressed inert gas; and a control valve 80, which is connected between the gas storage cylinder 70 and the inlet end of the inlet pipe 40, and is used to control the amount of gas supplied to the first container 10. Since the compressed inert gas is a dry gas, in this embodiment, a titanium tetrachloride solution or a hydrochloric acid solution can be pre-placed in the first container 10, and the amount of gas supplied to the first container 10 can be controlled by the control valve 80.

[0030] In another embodiment, the titanium tetrachloride test sample preparation apparatus further includes an air pump 90, the outlet of which is airtightly connected to the inlet of the air inlet pipe 40, for controllably supplying air into the first container 10. Specifically, since air is directly supplied into the first container 10 in this embodiment, the first container 10 can only be used to pre-fill the hydrochloric acid solution.

[0031] In one embodiment, the titanium tetrachloride test sample preparation device of this invention further includes a refiner 100, which is connected to the second liquid outlet of the U-shaped tube 30. Specifically, the refiner 100 is a hollow cavity with fine air vents on its surface, used to disperse the first solution pre-placed in the first container 10 and fully mix it with the second solution pre-placed in the second container 20.

[0032] In one embodiment, the titanium tetrachloride test sample preparation device of this invention further includes an elemental analyzer (ICP). Specifically, ICP is currently the main light source used for atomic emission spectroscopy. Its greatest advantage as an atomizer is that the atomizer has a very high temperature, and many elements can be well atomized. Its working principle is to use the photoelectric converted electrical signal, which is amplified and processed by a computer to report the analysis results of each element.

[0033] More specifically, compared to the traditional manual sample preparation process: Take 15 ml of hydrochloric acid (1:1) into a 50 ml volumetric flask. Using a 1 ml dry pipette, accurately transfer 1 ml of titanium tetrachloride solution into the 50 ml volumetric flask containing the 15 ml hydrochloric acid (1:1) solution. Suspend the pipette by inserting it into the neck of the flask, keeping the pipette tip at a distance from the hydrochloric acid surface. While adding the solution, gently shake the flask to ensure each drop of titanium tetrachloride solution is quickly dissolved by the molten salt in the hydrochloric acid, until all 1 ml of titanium tetrachloride solution is released and dissolved into the flask. During this process, the hydrochloric acid solution must not splash onto the pipette tip, otherwise hydrolysis will form solid hydrolysate that will clog the pipette. Make up to volume with 5% dilute hydrochloric acid, shake well, and prepare for analysis. The titanium tetrachloride test sample preparation device provided by this utility model can achieve the mixing of titanium tetrachloride and hydrochloric acid solution in a closed environment. By controlling the amount of gas supplied to the first container 10, the first solution in the first container 10 can be conveniently added to the second container 20 and fully mixed with the second solution without worrying about pipette blockage, acid mist generation and other problems.

[0034] The above are exemplary embodiments disclosed in this utility model. However, it should be noted that various changes and modifications can be made without departing from the scope of the embodiments of this utility model as defined by the claims. The functions, steps, and / or actions of the methods according to the disclosed embodiments described herein do not need to be performed in any particular order.

[0035] Those skilled in the art should understand that the discussion of any of the above embodiments is merely exemplary and is not intended to imply that the scope of the present invention (including the claims) is limited to these examples. Within the framework of the present invention, technical features of the above embodiments or different embodiments can also be combined, and many other variations of different aspects of the present invention exist, which are not provided in the details for the sake of brevity. Therefore, any omissions, modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A sample preparation apparatus for titanium tetrachloride testing, characterized in that, include: A first container, the first container including an air inlet and a first liquid outlet; The second container includes a first liquid inlet and a gas outlet; The U-shaped tube includes a second inlet and a second outlet, which are respectively in airtight communication with the first outlet and the first inlet. The second inlet and the second outlet are respectively located near the bottom of the first container and the second container. The U-shaped tube is configured to receive a first solution pressed in from the first container and introduce the first solution into the second container to mix with a second solution in the second container in an airtight environment to obtain a titanium tetrachloride test sample.

2. The titanium tetrachloride test sample preparation apparatus according to claim 1, characterized in that, Also includes: An air intake pipe, which is in airtight communication with the air inlet; and an air outlet pipe, which is in airtight communication with the air outlet.

3. The titanium tetrachloride test sample preparation apparatus according to claim 2, characterized in that, Also includes: A one-way vent valve is provided, which is airtightly connected to the vent end of the vent pipe.

4. The titanium tetrachloride test sample preparation apparatus according to claim 3, characterized in that, Also includes: A gas storage cylinder containing compressed inert gas; and a control valve connected between the gas storage cylinder and the inlet end of the inlet pipe for controlling the amount of gas supplied to the first container.

5. The titanium tetrachloride test sample preparation apparatus according to claim 3, characterized in that, Also includes: An air pump, the air outlet of which is airtightly connected to the air inlet of the air inlet pipe, is used to controllably supply air into the first container.

6. The titanium tetrachloride test sample preparation apparatus according to any one of claims 1-5, characterized in that, Also includes: A refiner, which is connected to the second liquid outlet of the U-shaped tube.

7. The titanium tetrachloride test sample preparation apparatus according to claim 4, characterized in that, The first container stores a titanium tetrachloride solution, and the second container stores a hydrochloric acid solution.

8. The titanium tetrachloride test sample preparation apparatus according to claim 5, characterized in that, The first container stores hydrochloric acid solution, and the second container stores titanium tetrachloride solution.

9. The titanium tetrachloride test sample preparation apparatus according to claim 1, characterized in that, Both the first container and the second container include a test tube stopper. The first container defines the air inlet and the first liquid outlet through the test tube stopper, and the second container defines the first liquid inlet and the air outlet through the test tube stopper. Both the first container and the second container are test tubes.

10. The titanium tetrachloride test sample preparation apparatus according to claim 9, characterized in that, The test tubes are graduated test tubes.