A device and method for detecting impurity elements in high-purity antimony

Abstract

The invention relates to a detection device and method for impurity elements in high-purity antimony applied to the technical field of analysis and detection. The detection device comprises an atomization chamber, an aerosol sample delivery tube, an injection atomizer, an adsorption tank, a conductive tube, a recovery tank and a waste liquid tube. The invention sequentially injects a test standard solution, a blank test liquid and a test liquid into an inductively coupled plasma mass spectrometer to detect the impurity elements in the high-purity antimony. The atomized test standard solution, the blank test liquid and the test liquid are mixed with an inert gas to perform a swirling motion in the atomization chamber. Large particle droplets are closer to the inner wall of the atomization chamber due to centrifugal force. The large particle droplets are attracted by the static electricity on the conductive tube, so that the large particle droplets adhere to the inner wall of the atomization chamber and the surface of the conductive tube, and the removal effect of the large particle droplets is achieved, so that small particle droplets with high ionization efficiency can enter the inductively coupled plasma mass spectrometer, thereby effectively improving the element detection quality of the inductively coupled plasma mass spectrometer.

Description

Technical Field

[0001] The present invention relates to a detection device and method, and in particular to a detection device and method for impurity elements in high-purity antimony applied in the field of analytical detection technology. Background Art

[0002] High-purity antimony is mainly used in the semiconductor industry. It is a doping element for semiconductor silicon and germanium and is the main raw material for producing semiconductor refrigeration chips. High-purity antimony is also used in alloys with other metals to produce various flame retardants, enamel, glass, rubber, coatings, pigments, ceramics, plastics, semiconductor components, fireworks, medicines, chemicals and other products. In the detection process of high-purity antimony, inductively coupled plasma mass spectrometer is mainly used for element detection.

[0003] The specification of Chinese invention patent CN202211743426.7 discloses "A method for detecting impurity elements in high-purity antimony and an online gas dilution device". A high-purity antimony sample is dissolved by mixed acid, and internal standard solutions of different mass numbers of low, medium and high are added. Argon gas is introduced online for dilution, and the sample solution is "crushed and atomized" by the nebulizer gas pressure to form an aerosol, and then the dilution gas pressure is adjusted to achieve quantitative dilution of the test sample.

[0004] The function of the atomization chamber is to select the droplets sprayed by the atomizer, remove large particle droplets with low ionization efficiency, and select small particle droplets (10μm) to enter the plasma. After screening in the atomization chamber, only 1% to 2% of the sample enters the plasma. The existing atomization method is not effective in removing large particle droplets. The above patent also lacks a method for removing large particle droplets, which will affect the element detection effect of the inductively coupled plasma mass spectrometer. Summary of the invention

[0005] In view of the above-mentioned prior art, the technical problem to be solved by the present invention is that the existing atomization method is not effective enough in removing large particle droplets, and there is also a lack of removal methods for large particle droplets, which will affect the element detection effect of the inductively coupled plasma mass spectrometer.

[0006] In order to solve the above problems, the present invention provides a detection device for impurity elements in high-purity antimony, comprising an inductively coupled plasma mass spectrometer and a corresponding sampling system, wherein the sampling system comprises a funnel-shaped atomization chamber, the contracted end of the atomization chamber is fixedly connected to an aerosol sample delivery tube connected to the inductively coupled plasma mass spectrometer, and the bottom of the expanded end of the atomization chamber is fixedly connected to a sampling atomizer;

[0007] An adsorption groove is fixedly connected to the middle of the atomization chamber. The adsorption groove is U-shaped and bent, and both ends of the adsorption groove extend out of the top of the atomization chamber. An electrostatic generating module is fixedly connected between the two ends of the adsorption groove. A conductive tube is sleeved inside the adsorption groove, and the conductive tube is fixedly connected to the output end of the electrostatic generating module.

[0008] A recovery tank is provided at the bottom of the atomization chamber, the top of the recovery tank is communicated with the adsorption tank, and the bottom of the recovery tank is fixedly connected with a waste liquid pipe.

[0009] A method for detecting impurity elements in high-purity antimony, using the above-mentioned device for detecting impurity elements in high-purity antimony, specifically includes the following method steps:

[0010] Step 1: dissolve the high-purity antimony sample in an acid solution, add a mixed internal standard solution and adjust the volume to obtain a test solution, and prepare a blank test solution and a standard solution at the same time;

[0011] Step 2: using an inductively coupled plasma mass spectrometer to test a standard solution, a blank test solution and a test solution in sequence, the test standard solution, the blank test solution and the test solution are sprayed into a spray chamber by an inert gas through a sample injection nebulizer in sequence, and the atomized test standard solution, the blank test solution and the test solution are mixed with the inert gas to perform a swirling motion in the spray chamber, and finally enter the inductively coupled plasma mass spectrometer through an aerosol sample delivery tube;

[0012] Step 3: The static electricity generated by the static electricity generating module is introduced into the adsorption tank through the conductive tube. The atomized droplets in swirling motion are affected by the static electricity on the conductive tube, and the atomized droplets are attracted to the adsorption tank, further removing large particle droplets with low ionization efficiency, so that more small particle droplets can enter the inductively coupled plasma mass spectrometer;

[0013] Step 4: The droplets attached to the inner wall of the atomization chamber and the droplets in the adsorption tank gather into waste liquid, which is recovered by the recovery tank and finally discharged through the waste liquid pipe.

[0014] In the above-mentioned device and method for detecting impurity elements in high-purity antimony, the atomized test standard solution, the blank test solution and the test solution mixed with the inert gas perform swirling motion in the atomization chamber. Large particle droplets are closer to the inner wall of the atomization chamber due to centrifugal force, and cooperate with the electrostatic adsorption on the conductive tube in the adsorption tank to effectively improve the removal effect of large particle droplets, thereby effectively improving the element detection quality of the inductively coupled plasma mass spectrometer.

[0015] As a further improvement of the present application, the standard solution is prepared by adding a mixed internal standard solution to a multi-element standard solution, and the blank test solution is prepared by adding a mixed internal standard solution to an acid solution, and the acid solution is one or two of concentrated hydrochloric acid, concentrated sulfuric acid and concentrated nitric acid.

[0016] As a further improvement of the present application, the inert gas used in step 2 is argon, and a pure water flushing process is inserted in the process of switching the test standard solution, blank test solution and test solution in step 2.

[0017] As a further improvement of the present application, a chamber tube is fixedly connected to the middle part of the flared end of the atomizing chamber, one end of the chamber tube extends into the atomizing chamber, and the extending end of the chamber tube is conically arranged corresponding to the atomizing chamber, and the outer end of the chamber tube is fixedly connected to an air inlet pipe, and an air outlet hole is provided on the surface of the extending end of the chamber tube. Inert gas is fed into the chamber tube through the air inlet pipe, and the inert gas is evenly blown out from the air outlet hole, thereby interfering with the outward diffusion of the swirling droplets inside the atomizing chamber, and further improving the removal effect of large particle droplets.

[0018] As another improvement of the present application, a capillary is fixedly connected to the outer end of the air outlet, the capillary is bent in an arc shape, and the capillary is made of elastic rubber material. The capillary is used to guide the blown inert gas to change the blowing direction of the inert gas.

[0019] As another improved supplement of the present application, a telescopic plug module is fixedly connected to the middle part of the chamber lumen tube, a guide needle is fixedly connected to the outside of the piston of the telescopic plug module, the guide needle passes through the air outlet, the capillary and the guide needle are sleeved, the air outlet is horizontally arranged, and the length of the guide needle extending into the capillary is adjusted by the telescopic movement of the telescopic plug module, that is, the bending angle of the capillary is adjusted to control the blowing direction of the inert gas.

[0020] As another improved supplement to the present application, the outer end of the chamber lumen tube is also fixedly connected to a flushing water pipe, and a connecting pipe is fixedly connected between the bottom of the outer end of the chamber lumen tube and the waste liquid pipe. The piston of the telescopic plug module corresponds to the connecting part of the connecting pipe and the chamber lumen tube. When the pure water flushing process is carried out, the pure water enters the chamber lumen tube through the flushing water pipe and is sprayed out through the air outlet, effectively improving the flushing effect of the atomization chamber. After the pure water flushing process is completed, the piston of the telescopic plug module opens the connecting pipe, so that the remaining flushing water in the chamber lumen tube enters the waste liquid pipe through the connecting pipe and is discharged, which is convenient for the chamber lumen tube to resume air intake operation.

[0021] In summary, the present invention realizes the detection of impurity elements in high-purity antimony by sequentially injecting a test standard solution, a blank test liquid and a test liquid through an inductively coupled plasma mass spectrometer, and the atomized test standard solution, the blank test liquid and the test liquid are mixed with an inert gas to perform a swirling motion in an atomization chamber, and large particle droplets are closer to the inner wall of the atomization chamber due to centrifugal force, and cooperate with the electrostatic adsorption on the conductive tube in the adsorption tank, that is, the electrostatic attraction on the conductive tube by the large particle droplets, so that the large particle droplets are attached to the inner wall of the atomization chamber and the surface of the conductive tube, and the removal effect of the large particle droplets is achieved, which facilitates the small particle droplets with high ionization efficiency to enter the inductively coupled plasma mass spectrometer, thereby effectively improving the element detection quality of the inductively coupled plasma mass spectrometer. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is a top-down perspective structural diagram of the first embodiment of the present application;

[0023] Figure 2 This is a bottom-up stereoscopic structural diagram of the first embodiment of the present application;

[0024] Figure 3 This is a sectional three-dimensional structural diagram of the first embodiment of the present application;

[0025] Figure 4 This is a demonstration diagram of the swirl motion of droplets in the first embodiment of the present application;

[0026] Figure 5 This is a cross-sectional three-dimensional structural diagram of the chamber tube according to the second embodiment of the present application;

[0027] Figure 6 This is a three-dimensional structural diagram of the chamber tube according to the second embodiment of the present application;

[0028] Figure 7 This is a three-dimensional structural diagram of the telescopic plug module and the guide needle in the second embodiment of the present application;

[0029] Figure 8 This is a demonstration diagram of the second embodiment of the present application, in which the guide needle is extended and retracted to change the capillary bending angle;

[0030] Fig. 9 This is a demonstration diagram of the telescopic plug module controlling the opening and closing of the connecting pipe in the second embodiment of the present application.

[0031] Description of the numbers in the figure:

[0032] 1. Atomization chamber; 101. Aerosol sample delivery tube; 102. Sample injection atomizer; 2. Adsorption tank; 201. Electrostatic generating module; 202. Conductive tube; 203. Recovery tank; 204. Waste liquid tube; 3. Chamber tube; 301. Air inlet pipe; 302. Air outlet; 303. Capillary tube; 304. Telescopic plug module; 305. Guide needle; 306. Flushing water pipe; 307. Connecting pipe. DETAILED DESCRIPTION

[0033] Two implementation modes of the present application are described in detail below with reference to the accompanying drawings.

[0034] The first implementation method:

[0035] Figures 1 to 4Shown is a device and method for detecting impurity elements in high-purity antimony, including an inductively coupled plasma mass spectrometer and a corresponding sampling system, wherein the sampling system includes a funnel-shaped atomization chamber 1, a contracted end of the atomization chamber 1 is fixedly connected to an aerosol sample delivery tube 101 connected to the inductively coupled plasma mass spectrometer, a sample injection atomizer 102 is fixedly connected to the bottom of the expanded end of the atomization chamber 1, an adsorption groove 2 is fixedly connected to the middle of the atomization chamber 1, the adsorption groove 2 is U-shaped, and both ends of the adsorption groove 2 extend out of the top of the atomization chamber 1, an electrostatic generating module 201 is fixedly connected between the two ends of the adsorption groove 2, a conductive tube 202 is sleeved inside the adsorption groove 2, and the conductive tube 202 is fixedly connected to the output end of the electrostatic generating module 201, a recovery groove 203 is provided at the bottom of the atomization chamber 1, the top of the recovery groove 203 is connected to the adsorption groove 2, and the bottom of the recovery groove 203 is fixedly connected to a waste liquid pipe 204.

[0036] A method for detecting impurity elements in high-purity antimony, using the above-mentioned device for detecting impurity elements in high-purity antimony, specifically includes the following method steps:

[0037] Step 1: dissolve the high-purity antimony sample in an acid solution, add a mixed internal standard solution and adjust the volume to obtain a test solution, and prepare a blank test solution and a standard solution at the same time;

[0038] Step 2: using an inductively coupled plasma mass spectrometer to test a standard solution, a blank test solution and a test solution in sequence, the test standard solution, the blank test solution and the test solution are sprayed into the atomization chamber 1 by an inert gas through the sample injection atomizer 102 in sequence, and the atomized test standard solution, the blank test solution and the test solution are mixed with the inert gas to perform a swirl motion in the atomization chamber 1, and finally enter the inductively coupled plasma mass spectrometer through the aerosol sample delivery tube 101;

[0039] Step 3: The static electricity generated by the static electricity generating module 201 is introduced into the adsorption tank 2 through the conductive tube 202. The atomized droplets in swirling motion are affected by the static electricity on the conductive tube 202, and the atomized droplets are attracted to the adsorption tank 2, further removing large particle droplets with low ionization efficiency, so that more small particle droplets can enter the inductively coupled plasma mass spectrometer;

[0040] Step 4: The droplets attached to the inner wall of the atomization chamber 1 and the droplets in the adsorption tank 2 are gathered into waste liquid, which is recovered by the recovery tank 203 and finally discharged through the waste liquid pipe 204;

[0041] The atomized test standard solution, the blank test solution and the test solution mixed with the inert gas perform swirling motion in the atomization chamber 1. Large particle droplets are closer to the inner wall of the atomization chamber 1 due to centrifugal force, and cooperate with the electrostatic adsorption on the conductive tube 202 in the adsorption tank 2, that is, the large particle droplets are attracted by the static electricity on the conductive tube 202, so that the large particle droplets are attached to the inner wall of the atomization chamber 1 and the surface of the conductive tube 202, and the large particle droplets are removed, so that small particle droplets with high ionization efficiency can enter the inductively coupled plasma mass spectrometer, thereby effectively improving the element detection quality of the inductively coupled plasma mass spectrometer. The attached droplets gather into waste liquid, and the droplets attached to the inner wall of the atomization chamber 1 and the droplets in the adsorption tank 2 gather into waste liquid, which is recovered by the recovery tank 203 and finally discharged through the waste liquid pipe 204.

[0042] The second implementation method:

[0043] Compared with the first embodiment, the main new addition is the chamber cavity tube 3, and the specific new structure is as follows, and the remaining structure is consistent with the first embodiment.

[0044] Figures 5 to 8 As shown, a chamber tube 3 is fixedly connected to the middle of the expanded end of the atomizing chamber 1, one end of the chamber tube 3 extends into the atomizing chamber 1, and the extending end of the chamber tube 3 is conically arranged corresponding to the atomizing chamber 1, and an air inlet pipe 301 is fixedly connected to the outer end of the chamber tube 3, and an air outlet hole 302 is provided on the surface of the extending end of the chamber tube 3. Inert gas is fed into the chamber tube 3 through the air inlet pipe 301, and the inert gas is evenly blown out from the air outlet hole 302, thereby interfering with the outward diffusion of the swirling droplets inside the atomizing chamber 1, further improving the removal effect of large particle droplets, and a capillary 303 is fixedly connected to the outer end of the air outlet hole 302, and the capillary 303 is curved in an arc shape. The capillary 303 is made of elastic rubber material, and the capillary 303 is used to guide the blown inert gas to change the blowing direction of the inert gas. A telescopic plug module 304 is fixedly connected to the middle of the chamber tube 3, and a guide needle 305 is fixedly connected to the piston of the telescopic plug module 304. The guide needle 305 passes through the gas outlet 302, and the capillary 303 is sleeved with the guide needle 305. The gas outlet 302 is horizontally arranged. Through the telescopic movement of the telescopic plug module 304, the length of the guide needle 305 extending into the capillary 303 is adjusted, that is, the bending angle of the capillary 303 is adjusted to control the blowing direction of the inert gas.

[0045] When the atomized test standard solution, the blank test liquid and the test liquid mixed with the inert gas perform a swirling motion in the atomization chamber 1, the chamber tube 3 also delivers the inert gas through the air inlet pipe 301, and the inert gas is evenly blown out from the air outlet 302. The blown inert gas is guided by the capillary 303, thereby disturbing the droplets of swirling motion to be closer to the inner wall of the atomization chamber 1, further improving the removal effect of large particle droplets, and the telescopic plug module 304 is telescopically adjusted, and the piston in the chamber tube 3 drives the guide needle 305 to extend and retract, and controls the length of the guide needle 305 inserted into the capillary 303, that is, adjusts the bending degree of the capillary 303, so as to control the blowing angle of the inert gas and adjust the interference degree of the droplets of swirling motion.

[0046] Figure 5 and Fig. 9 As shown, the outer end of the chamber tube 3 is also fixedly connected to a flushing water pipe 306, and a connecting pipe 307 is fixedly connected between the outer end bottom of the chamber tube 3 and the waste liquid pipe 204. The piston of the telescopic plug module 304 corresponds to the connecting part of the connecting pipe 307 and the chamber tube 3. When the pure water flushing process is performed, the pure water enters the chamber tube 3 through the flushing water pipe 306 and is sprayed out through the air outlet 302, which effectively improves the flushing effect of the atomization chamber 1. After the pure water flushing process is completed, the piston of the telescopic plug module 304 opens the connecting pipe 307, so that the remaining flushing water in the chamber tube 3 enters the waste liquid pipe 204 through the connecting pipe 307 and is discharged, which is convenient for the chamber tube 3 to re-perform the air intake operation;

[0047] When the pure water flushing process is performed, the air supply from the air inlet pipe 301 to the chamber tube 3 is closed, and the flushing water pipe 306 is opened. Pure water enters the chamber tube 3 through the flushing water pipe 306 and is ejected through the air outlet 302. The ejection of pure water is the same as the blowing method of inert gas, which effectively improves the flushing effect of the atomization chamber 1. After the pure water flushing process is completed, the piston of the telescopic plug module 304 retreats to the connecting part between the connecting pipe 307 and the chamber tube 3, so that the remaining flushing water in the chamber tube 3 enters the waste liquid pipe 204 through the connecting pipe 307 and is discharged, so that the chamber tube 3 can resume the air intake operation.

[0048] In view of current practical needs, the above-mentioned implementation mode adopted in this application is not limited to the scope of protection. Various changes made within the knowledge scope of technical personnel in this field without departing from the concept of this application still fall within the scope of protection of the present invention.

Claims

1. A device for detecting impurity elements in high-purity antimony, characterized in that: It comprises an inductively coupled plasma mass spectrometer and a corresponding sample injection system, wherein the sample injection system comprises a funnel-shaped atomization chamber (1), the contracted end of the atomization chamber (1) is fixedly connected to an aerosol sample delivery tube (101) connected to the inductively coupled plasma mass spectrometer, and the bottom of the expanded end of the atomization chamber (1) is fixedly connected to a sample injection atomizer (102); An adsorption groove (2) is fixedly connected to the middle of the atomization chamber (1); the adsorption groove (2) is bent in a U shape, and both ends of the adsorption groove (2) extend out of the top of the atomization chamber (1); an electrostatic generating module (201) is fixedly connected between the two ends of the adsorption groove (2); a conductive tube (202) is sleeved inside the adsorption groove (2), and the conductive tube (202) is fixedly connected to the output end of the electrostatic generating module (201); A recovery groove (203) is provided at the bottom of the atomization chamber (1), the top of the recovery groove (203) is communicated with the adsorption groove (2), the bottom end of the recovery groove (203) is fixedly connected to a waste liquid pipe (204), a chamber tube (3) is fixedly connected to the middle of the expanded end of the atomization chamber (1), one end of the chamber tube (3) extends into the atomization chamber (1), and the inlet end of the chamber tube (3) is arranged in a conical shape corresponding to the atomization chamber (1), the outer end of the chamber tube (3) is fixedly connected to an air inlet pipe (301), and the inlet end of the chamber tube (3) is provided with an outlet pipe (301). The air hole (302) is fixedly connected to a capillary (303) at the outer end of the air outlet hole (302), the capillary (303) is bent in an arc shape, and the capillary (303) is made of elastic rubber material. The middle part of the chamber tube (3) is fixedly connected to a telescopic plug module (304), the piston of the telescopic plug module (304) is fixedly connected to a guide needle (305) on the outside, the guide needle (305) passes through the air outlet hole (302), the capillary (303) is sleeved with the guide needle (305), and the air outlet hole (302) is horizontally arranged.

2. The device for detecting impurity elements in high-purity antimony according to claim 1, characterized in that: The outer end of the chamber tube (3) is also fixedly connected to a flushing water pipe (306), a connecting pipe (307) is fixedly connected between the bottom of the outer end of the chamber tube (3) and the waste liquid pipe (204), and the piston of the telescopic plug module (304) and the connecting pipe (307) correspond to the connecting part of the chamber tube (3).

3. A detection of impurity elements in high-purity antimony, using the detection device for impurity elements in high-purity antimony according to claim 1, characterized in that: The specific steps are as follows: Step 1: dissolve the high-purity antimony sample in an acid solution, add a mixed internal standard solution and adjust the volume to obtain a test solution, and prepare a blank test solution and a standard solution at the same time; Step 2: using an inductively coupled plasma mass spectrometer to test a standard solution, a blank test solution and a test solution in sequence, wherein the test standard solution, the blank test solution and the test solution are sprayed into the atomization chamber (1) by an inert gas through a sample injection atomizer (102) in sequence, and the atomized test standard solution, the blank test solution and the test solution are mixed with the inert gas to perform a swirling motion in the atomization chamber (1), and finally enter the inductively coupled plasma mass spectrometer through an aerosol sample delivery tube (101); Step 3: The static electricity generated by the static electricity generating module (201) is introduced into the adsorption tank (2) through the conductive tube (202), and the atomized droplets in swirling motion are affected by the static electricity on the conductive tube (202), and the atomized droplets are attracted to the adsorption tank (2), thereby further removing large particle droplets with low ionization efficiency, and allowing more small particle droplets to enter the inductively coupled plasma mass spectrometer; Step 4: The droplets attached to the inner wall of the atomization chamber (1) and the droplets in the adsorption tank (2) are aggregated into waste liquid, which is recovered by the recovery tank (203) and finally discharged through the waste liquid pipe (204).

4. The device and method for detecting impurity elements in high-purity antimony according to claim 3, characterized in that: The inert gas used in step 2 is argon. In step 2, a pure water flushing process is inserted in the process of switching the test standard solution, the blank test solution and the test solution in sequence.

5. The device and method for detecting impurity elements in high-purity antimony according to claim 3, characterized in that: The standard solution is prepared by adding a mixed internal standard solution to a multi-element standard solution, and the blank test solution is prepared by adding a mixed internal standard solution to an acid solution, wherein the acid solution is one or two of concentrated hydrochloric acid, concentrated sulfuric acid and concentrated nitric acid.

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