TW202022341A - The reaction gas supply equipment of an inductive coupled plasma mass spectrometer comprises an ammonia supply end and a helium supply end and a reaction gas supply equipment - Google Patents

Abstract

The reaction gas supply equipment of an inductive coupled plasma mass spectrometer comprises an ammonia supply end and a helium supply end and a reaction gas supply equipment, which is supplied with an ammonia supply end and the helium supply end, and the reaction gas supply equipment is provided with an ammonia mass flowmeter to adjust the flow of ammonia and helium, Helium mass flowmeter; The ammonia mass flowmeter and helium mass flowmeter are adjusted by the proportion of reaction gas specified by the inductive coupled Plasma spectrometer, and the reaction gas is formed by mixing ammonia gas with helium, which is then provided to the inductive coupled Plasma mass spectrometer, which can be used to protect the detection instrument and reduce the cost of reaction gas through the technical means of the invention.

Description

Reactive gas supply equipment and deployment method of inductively coupled plasma mass spectrometer

The present invention relates to the reactive gas supply module of detection equipment, and in particular refers to a reactive gas supply device and deployment method of an inductively coupled plasma mass spectrometer; the reactive gas supply device and reactive gas deployment method provided by the present invention allow inspection The unit uses the correct reaction gas for element detection, which can increase the detection rate of elements and protect the product advantages of inductively coupled plasma mass spectrometers.

Inductively coupled plasma mass spectrometer for measurement and analysis, analysis technology can quantitatively measure the element content of the material, the range is ppt to wt%. Only C (carbon), H (hydrogen), O (oxygen), N (nitrogen) and halogen are not applicable.

The application method is to spray the sample solution into the core of inductively coupled plasma. The plasma temperature is as high as 8000°C. Under such high temperature, all analytical species will be atomized, ionized and thermally excited, and then the test object can be Be detected and quantified.

Among them, the inductively coupled plasma mass spectrometer mainly measures the mass of element ions produced by high temperature argon ion plasma; the ions produced in the plasma are separated according to their charge-to-mass ratio, so that unknown materials can be identified and quantified.

Therefore, industries such as aerospace industry, sputtering targets, chemicals, alloy manufacturers, food/beverage, geology, pharmacy, environmental water, wastewater, and water treatment industries will pass through the testing unit when they need to submit related reports such as material certification. Inductively coupled plasma mass spectrometer for element content, concentration and other related data analysis.

Among them, the Agilent 8900 series of inductively coupled plasma mass spectrometers from Agilent Technologies are used by major domestic inspection units or semiconductor high-tech companies. Because in the semiconductor manufacturing process, in order to determine specific elements, inductively coupled electrical The plasma mass spectrometer has detected elements such as those contained in the wafer; the reaction gas specifications provided by the company are 10% NH ₃ (ammonia) and 90% He (helium), but the inventor of this case found that all major domestic manufacturers The ammonia cylinder was purchased from the gas company, and the element test was performed with 100% NH ₃ (ammonia), which caused the following problems:

1. The corrosive nature of NH ₃ (ammonia gas) is destructive to inductively coupled plasma mass spectrometers. Therefore, major domestic inspection units often report for repairs, which not only delays the inspection progress, but also the suppliers of inductively coupled plasma mass spectrometers. distressed.

2. The inventor found that the aforementioned problem lies in the fact that the domestic testing unit cannot adjust the proportion of the reaction gas by itself, and the inspector directly uses ammonia as the reaction gas for the detection.

3. In addition, the aforementioned reaction gas (ammonia, ammonia) is not used in a large amount, which causes the inspection unit to directly use ammonia in order to save costs, which indirectly causes damage to the inspection equipment.

4. The maintenance cost of the inductively coupled plasma mass spectrometer is high, resulting in a significant increase in the unit cost of inspection.

5. Since the reaction gas is ammonia, if pure ammonia is used as the reaction gas, it may cause pipeline damage and ammonia leakage. Ammonia is harmful to the human body and is likely to cause industrial safety problems.

Therefore, how to solve the problems and deficiencies of the above-mentioned conventional knowledge is a topic that the related industry urgently wants to develop.

The main purpose of the present invention is to provide a reactive gas supply device and a deployment method for an inductively coupled plasma mass spectrometer, which mainly connects an ammonia gas supply terminal and a helium gas supply terminal through a reactive gas supply device to combine the two reactions The gas is in the mixing pipeline, and then the pipeline pressure in the mixing pipeline is controlled to allow the reaction gas to be fully mixed, and the reaction gas is output to the inductively coupled plasma mass spectrometer for inspection. The technical means of the present invention can achieve protection detection Many advantages such as instrument, lower reaction gas cost, etc.

For this reason, the reactive gas supply device of the inductively coupled plasma mass spectrometer of the present invention is achieved through the following technical means. An ammonia supply end can provide ammonia; a helium supply end can provide helium; and it is characterized by: The reactive gas supply device is respectively connected to the ammonia gas supply end and the helium gas supply end, and the reactive gas supply device is provided with an output end connected to the inductively coupled plasma mass spectrometer, and the reactive gas supply device includes a Ammonia gas pipeline and a helium gas pipeline; the aforementioned ammonia gas pipeline further includes a first ammonia gas pressure regulating valve, an ammonia gas mass flow meter and a second ammonia gas pressure regulating valve; the aforementioned helium gas pipeline further includes a first A helium gas pressure regulating valve, a helium gas mass flow meter and a second helium gas pressure regulating valve; the ammonia gas pipeline is pulled up on the side of the ammonia gas supply end, and the helium gas pipeline is pulled up on the side of the helium gas supply end A mixing pipeline connected with the ammonia pipeline and the helium pipeline; the mixing pipeline is connected with the output end to supply reaction gas to the inductively coupled plasma mass spectrometer.

Through the above-mentioned equipment, the reaction gas deployment method of the present invention is as follows: Step 1: Open the aforementioned ammonia supply end and helium supply end, so that ammonia and helium flow into the ammonia pipeline and the Helium gas pipeline; Step 2: Adjust the aforementioned first ammonia gas pressure regulating valve, second ammonia gas pressure regulating valve, first helium gas pressure regulating valve, and second helium gas pressure regulating valve to 10-20 psi, and connect in this state The internal pressure of the mixing pipeline will also be maintained at 10~20psi; Step 3: Adjust the supply parameter of the aforementioned ammonia mass flowmeter to 0.1L/min, and the supply parameter of the helium mass flowmeter to 0.9L/min; Thereby, ammonia gas and helium gas are thoroughly mixed under a pressure state of 10-20 psi to form a reaction gas for the inductively coupled plasma mass spectrometer.

In the embodiment of the reaction gas supply device of the present invention, a check valve is provided between the aforementioned ammonia gas pipeline and the aforementioned mixing pipeline, and between the aforementioned helium gas pipeline and the aforementioned mixing pipeline to prevent gas backflow.

In the embodiment of the reactive gas supply device of the present invention, if ammonia gas penetrates into water vapor, it will become ammonia water (NH4OH). Ammonia water is a strong alkali compound, and its physical and chemical properties are corrosive to the human body and pipelines. Therefore, the present invention A heating module is connected to the ammonia pipeline, the mixing pipeline, and the output end for heating. The heating module is wound with a plurality of metal heating tapes on the pipeline, and the heating module adds the metals In the tropical zone, the temperature rises to about 70~80℃ to prevent the occurrence of ammonia water mixed with water vapor in the pipeline.

In the embodiment of the reaction gas supply device of the present invention, the mixing pipeline is further connected to a gas storage unit, by which a large amount of reaction gas can be stored, so that when a large amount of reaction gas is required, the gas The storage unit supplies reactive gas to increase the convenience of detection.

Through the equipment and technical means of the present invention, it can be understood that: 1. The present invention can indeed provide the correct gas ratio for the inductively coupled plasma mass spectrometer inspection; the inspection unit does not need to order special specifications of reaction gas from the gas supplier, which can reduce the inspection Unit inspection cost; 2. Prevent the use of pure Ammonia is used as a reaction gas to cause damage to the inductively coupled plasma mass spectrometer.

1‧‧‧Ammonia supply side

11‧‧‧Purifier

12‧‧‧Water filter

2‧‧‧Helium supply side

21‧‧‧Water Filter

3‧‧‧Reactive gas supply equipment

31‧‧‧Output

32‧‧‧body

33‧‧‧Ammonia pipeline

331‧‧‧First Ammonia Pressure Regulator

332‧‧‧Ammonia Mass Flowmeter

333‧‧‧Second Ammonia Pressure Regulator

334‧‧‧One-way valve

335‧‧‧Ammonia Pressure Gauge

34‧‧‧Helium pipeline

341‧‧‧The first helium pressure regulator

342‧‧‧Helium mass flow meter

343‧‧‧The second helium pressure regulator

344‧‧‧One-way valve

345‧‧‧Helium Pressure Gauge

35‧‧‧Mixed pipeline

36‧‧‧Heating Module

37‧‧‧Metal heating belt

38‧‧‧Gas storage unit

4‧‧‧Inductively coupled plasma mass spectrometer

Fig. 1 is a schematic diagram of the structure of the reactive gas supply equipment of the present invention; Fig. 2 is a schematic diagram of the pipe wrapped with a metal heating tape; Fig. 3 is a schematic diagram of the structure of the present invention including a gas storage unit; Fig. 4 is the application of the present invention The flow chart of the method for configuring the reactant gas; Figure 5 is a schematic structural diagram of another embodiment of the present invention.

In order to enable your reviewer to have a further understanding and recognition of the features and characteristics of the present invention, the following preferred embodiments are listed and illustrated as follows: Please refer to Figures 1 to 3, the inductively coupled plasma mass spectrometer of the present invention The reaction gas supply equipment of the instrument includes: an ammonia gas supply port 1, a helium gas supply port 2 and a reaction gas supply device 3; the aforementioned ammonia gas supply port 1 can provide ammonia gas, wherein the purity of the ammonia gas It needs to be close to 100% to produce better analytical data and reduce environmental impurities; as shown in Figures 1 and 3, the ammonia supply end 1 is provided with a purifier 11 that can filter impurities in the ammonia gas.

The aforementioned helium gas supply terminal 2 provides helium gas, where the purity of the helium gas needs to be close to 100% to produce better analysis data and reduce environmental impurities.

The aforementioned reactive gas supply device 3 is respectively connected to the ammonia gas supply port 1 and the helium gas supply port 2, and the reactive gas supply device 3 is provided with an output port 31 which is connected to the inductively coupled plasma mass spectrometer 4 ; As shown in Figures 1 and 3, the reactive gas supply device 3 is equipped with a machine Body 32, most of the equipment described later is installed in the fuselage 3. The reactive gas supply equipment 3 includes an ammonia pipe 33 and a helium pipe 34; the aforementioned ammonia pipe 33 sequentially includes a first ammonia pressure regulator Valve 331, an ammonia mass flow meter 332, and a second ammonia pressure regulating valve 333; the aforementioned helium pipeline 34 includes a first helium pressure regulating valve 341, a helium mass flow meter 342, and a The second helium pressure regulating valve 343.

Please continue to refer to Figures 1 and 3, the ammonia gas pipeline 33 is opposite to the ammonia gas supply end 1 side, and the helium gas pipeline 34 is opposite to the helium gas supply end 2 side. The pipeline 35 is connected with the ammonia pipeline 33 and the helium pipeline 34; the mixing pipeline 35 is connected with the output end 31 to supply reaction gas to the inductively coupled plasma mass spectrometer 4.

In addition, between the aforementioned ammonia pipe 33 and the aforementioned mixing pipe 35, and between the helium pipe 34 and the aforementioned mixing pipe 35, one-way valves 334 and 344 are respectively provided to prevent gas backflow; in addition, the ammonia pipe A heating module 36 is connected to the circuit 33, the mixing pipe 35 and the output end 31 for heating. The aforementioned heating module 36 is connected to the aforementioned ammonia pipe 33, the mixing pipe 35, and the output end 31. There are two metal heating belts 37, and the heating module 36 raises the temperature of the metal heating belts 37 to a range of about 70-80°C to prevent the pipeline from mixing with water vapor to form ammonia.

Through the above equipment, the inspection unit can purchase ammonia cylinders and helium cylinders from the gas supplier as the ammonia supply port 1 and helium supply port 2 of the present invention; connect the ammonia gas pipeline 33 to the ammonia supply port 1. The helium gas pipeline 34 is connected to the helium gas supply end 2 and can be mixed through the aforementioned reaction gas supply device 3 to form the reaction gas for the inductively coupled plasma mass spectrometer 4.

As shown in Figure 3, the structure is basically the same as that in Figure 1, except that the mixing pipe 35 is further connected to a gas storage unit 38, which can store a large amount of reaction gas. When a large amount of reaction gas is needed, the gas storage unit 38 Supply of reactive gas increases the convenience of detection.

As shown in Figure 4, through the above-mentioned equipment, the present invention further includes a reaction gas preparation method as follows: Step 1: Open the aforementioned ammonia supply port 1 and helium supply port 2 to allow ammonia and helium to flow in The ammonia gas pipeline 33 and the helium gas pipeline 34; Step 2: Adjust the aforementioned first ammonia pressure regulating valve 331, second ammonia pressure regulating valve 333, first helium pressure regulating valve 341, and second helium pressure regulating valve The valve 343 is 10-20 psi. In this state, the internal pressure of the mixing pipeline 35 connected will also be maintained at 10-20 psi; among them, in order to facilitate the operator to adjust the pressure, the ammonia supply port 1 and the ammonia pipeline 33 An ammonia gas pressure gauge 335 is provided between the helium gas supply end 2 and the helium gas supply pipe 34, and a helium gas pressure gauge 345 is installed between the helium gas supply end 2 and the helium gas supply pipe 34. Adjust the ammonia gas pipeline 33 and the helium gas pipeline 34 to 10-20 psi.

Step 3: Adjust the supply parameter of the aforementioned ammonia mass flow meter 332 to 0.1L/min, and the aforementioned supply parameter of helium mass flow meter 342 to 0.9L/min; thereby, the ammonia and helium can pass through 10-20 psi The reaction gas is fully mixed to form the reaction gas for the inductively coupled plasma mass spectrometer 4 under the pressure state.

Therefore, the reaction gas preparation method of the present invention makes the reaction gas exactly match the correct ratio of the reaction gas when the inductively coupled plasma mass spectrometer 4 performs the test. Since the reaction gas provided by the present invention can reduce the amount of ammonia used, it is not easy to cause induction. The coupling plasma mass spectrometer 4 equipment has corrosion and damage problems, and can reduce environmental impurities so that the detected substance can correctly determine the elements contained, the element content and even the element concentration.

As shown in Figure 5, it is the second embodiment of the reactive gas supply device 3 of the present invention In this embodiment, the feature is that a water filter is added to the ammonia supply end 1 and the helium supply end 2, which can prevent the aforementioned ammonia pipe 33 or helium pipe 34 from being frozen by water. In other words, the aforementioned ammonia gas pipeline 33 or helium gas pipeline 34 does not need to be additionally provided with a heating module 36 and a metal heating belt 37, and the specific implementation of this embodiment is to provide an ammonia gas supply port 1 and a helium gas supply Terminal 2, the aforementioned ammonia supply terminal 1 and the aforementioned helium supply terminal 2 are connected to a reactive gas supply device 3, wherein the ammonia supply terminal 1 is provided with a water filter 12, and the helium supply terminal is also provided with a Water filter 21. The water filters 12 and 21 are used to filter ammonia and helium to prevent icing of the pipeline; the reactive gas supply device 3 is basically the same as that provided in Figures 1 to 3 The structure is the same, it has an ammonia gas pipeline 33 and a helium gas pipeline 34. The ammonia gas pipeline 33 sequentially includes a first ammonia gas pressure regulating valve 331, an ammonia gas mass flow meter 332, and a second ammonia gas pressure regulating valve. Valve 333; the aforementioned helium gas pipeline 34 includes a first helium pressure regulating valve 341, a helium mass flow meter 342 and a second helium pressure regulating valve 343 in sequence; the ammonia gas pipeline 33 is opposite to the ammonia gas A mixing pipe 35 is pulled up on the side of the supply end 1 and the helium gas pipeline 34 opposite to the helium supply end 2, and the mixing pipeline 35 is connected to the ammonia pipeline 33 and the helium pipeline 34; the mixing pipe The circuit 35 is connected to the output terminal 31 to supply reaction gas to the inductively coupled plasma mass spectrometer 4. However, the principle of this embodiment is the same as that of Figs. 1 to 3, so it will not be repeated.

To sum up, the structure of the present invention has not been seen in books and periodicals or used publicly, and it meets the requirements of an invention patent application. I sincerely ask Jun Bureau to approve the patent as soon as possible.

If it needs to be clarified, the above is the technical principle immediately used in the implementation of the present invention. If the changes made according to the concept of the present invention, the functions produced by it still do not exceed the spirit covered by the specification and drawings, All should be within the scope of the present invention and should be disclosed.

1‧‧‧Ammonia supply side

11‧‧‧Purifier

2‧‧‧Helium supply side

3‧‧‧Reactive gas supply equipment

31‧‧‧Output

32‧‧‧body

33‧‧‧Ammonia pipeline

331‧‧‧First Ammonia Pressure Regulator

332‧‧‧Ammonia Mass Flowmeter

333‧‧‧Second Ammonia Pressure Regulator

334‧‧‧One-way valve

335‧‧‧Ammonia Pressure Gauge

34‧‧‧Helium pipeline

341‧‧‧The first helium pressure regulator

342‧‧‧Helium mass flow meter

343‧‧‧The second helium pressure regulator

344‧‧‧One-way valve

345‧‧‧Helium Pressure Gauge

35‧‧‧Mixed pipeline

36‧‧‧Heating Module

37‧‧‧Metal heating belt

4‧‧‧Inductively coupled plasma mass spectrometer

Claims (8)

A reactive gas supply device for an inductively coupled plasma mass spectrometer, comprising: an ammonia gas supply end which can provide ammonia gas; a helium gas supply end which provides helium gas; and is characterized in that: a reactive gas supply device, which is respectively Connected to the ammonia supply end and the helium supply end, and the reaction gas supply device is provided with an output end connected to an inductively coupled plasma mass spectrometer. The reaction gas supply device includes an ammonia pipe and a helium pipe The aforementioned ammonia gas pipeline further includes a first ammonia gas pressure regulating valve, an ammonia gas mass flow meter and a second ammonia gas pressure regulating valve; the aforementioned helium gas pipeline further comprises a first helium gas pressure regulating valve, A helium mass flow meter and a second helium pressure regulating valve; the ammonia gas pipeline is opposite to the ammonia gas supply end side, and the helium gas pipeline is opposite to the helium gas supply end side. The pipeline is connected with the ammonia pipeline and the helium pipeline; the mixing pipeline is connected with the output end to supply reaction gas to the inductively coupled plasma mass spectrometer. The method of preparing the reaction gas generated by the reaction gas supply equipment of the inductively coupled plasma mass spectrometer described in the first item of the scope of patent application is: Step 1: Turn on the aforementioned ammonia gas supply port and helium gas supply port, so that the ammonia gas and helium gas Flow into the ammonia gas pipeline and the helium gas pipeline; Step 2: Adjust the aforementioned first ammonia gas pressure regulating valve, second ammonia gas pressure regulating valve, first helium gas pressure regulating valve, and second helium gas pressure regulating valve to 10 ~20psi. In this state, the internal pressure of the connected mixing pipeline will also be maintained at 10~20psi; Step 3: Adjust the supply parameters of the aforementioned ammonia mass flowmeter to 0.1L/min, and the helium mass flowmeter The supply parameter is 0.9L/min; by this, ammonia and helium can pass through the pressure state of 10~20psi Mix thoroughly to form a reaction gas for the inductively coupled plasma mass spectrometer. According to the reactive gas supply equipment of the inductively coupled plasma mass spectrometer according to the first item of the patent application, the ammonia gas pipeline and the mixing pipeline, the helium gas pipeline and the mixing pipeline are more separate A one-way valve to prevent gas backflow is provided. According to the reactive gas supply equipment of the inductively coupled plasma mass spectrometer described in the first item of the scope of patent application, a heating module is connected to the ammonia gas pipeline, the mixing pipeline, and the output end for heating. The group is wound with multiple metal heating tapes on the pipeline. According to the reactive gas supply equipment of the inductively coupled plasma mass spectrometer described in item 4 of the scope of patent application, the heating module heats the metals to a temperature range of about 70~80℃ to prevent the pipeline from being mixed with water vapor. Ammonia situation occurs. According to the reactive gas supply device of the inductively coupled plasma mass spectrometer according to the first item of the patent application, the mixing pipeline is further connected to a gas storage unit. According to the reactive gas supply device of the inductively coupled plasma mass spectrometer described in the scope of the patent application, an ammonia gas pressure gauge is arranged between the ammonia gas supply end and the ammonia gas pipeline, the helium gas supply end and the helium gas A helium pressure gauge is arranged between the supply pipelines, and the pipeline pressures of the ammonia pipeline and the helium pipeline are quickly adjusted by the ammonia pressure gauge and the helium pressure gauge. A reactive gas supply device for an inductively coupled plasma mass spectrometer, comprising: an ammonia gas supply end which can supply ammonia gas, the ammonia gas supply end is provided with a water filter; a helium gas supply end which supplies helium gas, the The helium gas supply end is also provided with a water filter; it is characterized in that: the aforementioned ammonia gas pipeline further includes a first ammonia gas pressure regulating valve, an ammonia gas mass flow meter, and a second ammonia gas pressure regulating valve; The gas pipeline further includes a first helium pressure regulating valve, a helium mass flow meter and a The second helium pressure regulating valve; the ammonia gas pipeline is opposite to the ammonia gas supply end side, the helium gas pipeline is opposite to the helium gas supply end side, pull up a mixing pipeline, the mixing pipeline and the ammonia gas pipeline, The helium gas pipeline is connected; the mixing pipeline is connected with the output end to supply reaction gas to an inductively coupled plasma mass spectrometer.

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