CN110416040B - Method for automatically processing graphite electrode - Google Patents
Method for automatically processing graphite electrode Download PDFInfo
- Publication number
- CN110416040B CN110416040B CN201910618256.1A CN201910618256A CN110416040B CN 110416040 B CN110416040 B CN 110416040B CN 201910618256 A CN201910618256 A CN 201910618256A CN 110416040 B CN110416040 B CN 110416040B
- Authority
- CN
- China
- Prior art keywords
- current
- graphite electrode
- stage
- voltage
- automatically processing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/02—Manufacture of electrodes or electrode systems
- H01J9/04—Manufacture of electrodes or electrode systems of thermionic cathodes
- H01J9/042—Manufacture, activation of the emissive part
- H01J9/045—Activation of assembled cathode
Abstract
The invention relates to a method for automatically processing a graphite electrode, which inserts an untreated graphite electrode (1) on a cathode tungsten wire (3) of a hollow cathode lamp (2), and applies high voltage between the cathode tungsten wire (3) and an anode (5) through a control system (4) to enable the graphite electrode (1) to emit light; the control system (4) is used for setting the initial voltage, the voltage superposition step number and the current fluctuation range, and the graphite electrode (1) is processed by adopting a step-type current increasing method, so that the method can effectively release manpower, improve the efficiency, avoid human errors, is simple to operate, and ensures the stable discharge of the graphite electrode during detection.
Description
Technical Field
The invention relates to a method for automatically processing a graphite electrode, belonging to the technical field of detection.
Background
Since the trace element content has an important influence on the material performance, the trace analysis of the material has become the most remarkable frontline field of analytical chemistry research, especially in steel, high-temperature alloy, pure metal, high-purity alloy, electronic devices, ceramics, medicines and foods, the trace elements required to be analyzed and controlled are as much as more than 60, the minimum requirement is less than 0.00001%, and even the trace elements have a trend of gradually extending to lower content.
The commonly used solid sample introduction trace element detection methods at present mainly comprise a secondary ion mass spectrometry, a glow discharge mass spectrometry and a hollow cathode emission spectrometry. The secondary ion mass spectrometry method is used for locally sampling micro-areas on the surface of a sample and can only carry out low-concentration semi-quantitative analysis on elements. Although glow discharge mass spectrometers are an advanced instrument for direct solid sample introduction trace and ultra trace element analysis, they are quite expensive. The hollow cathode emission spectrometer is a high-sensitivity and high-accuracy instrument capable of detecting trace impurity elements in a solid sample, and has the advantages of simplicity in operation, low price and the like. The graphite electrode is used as the cathode of the excitation light source of the hollow cathode emission spectrometer, and the graphite has high adsorption capacity, is easy to adsorb impurity gas and moisture, and the graphite powder remained in the tube after processing can seriously affect the discharge stability, so thatBefore detection, the graphite electrode needs to be treated to remove impurity gas, moisture and residual graphite powder in the tube, so as to ensure stable discharge. C is also formed in the discharge chamber2When N, O, H-containing samples are analyzed, CN, CO, NO and OH molecules are also formed, molecular spectral bands are generated, and the analysis work is influenced.
Disclosure of Invention
The invention provides a method for automatically processing a graphite electrode, aiming at automatically processing the graphite electrode, having simple operation, saving labor, improving efficiency and avoiding human error caused by manually determining whether the graphite electrode is stable or not under current at the stage by observing the stability of a light source of a hollow cathode lamp.
The purpose of the invention is realized by the following technical scheme:
the method for automatically processing the graphite electrode is characterized by comprising the following steps: the method comprises the following steps:
inserting an untreated graphite electrode 1 on a cathode tungsten wire 3 of a hollow cathode lamp 2, and applying high voltage between the cathode tungsten wire 3 and an anode 5 through a control system 4 to enable the graphite electrode 1 to emit light;
setting initial voltage, voltage superposition steps and a current fluctuation range through a control system 4, and processing the graphite electrode 1 by adopting a step-type current increasing method, wherein the specific process is as follows;
the first step is as follows: after the graphite electrode 1 is treated for 20-40 s by using initial voltage and corresponding initial current, the initial voltage is increased by one voltage superposition step every 5s until the current reaches the first-stage current;
the initial voltage is 0.08-0.2V, the corresponding initial current is 100-200 mA, and the voltage superposition step number is 0.005-0.009V;
the second step is that: after the first-stage current floats in the current fluctuation range and is stabilized for 20-40 s, continuing increasing the voltage superposition step number once every 5s by the voltage corresponding to the first-stage current until the second-stage current is reached;
thirdly, after the current in the second stage floats in the current fluctuation range and is stable for 20-40 s, continuing increasing the voltage superposition step number for every 5s by the voltage corresponding to the current in the second stage until the current in the third stage is reached;
fourthly, after the current in the third stage floats in the current fluctuation range and is stable for 20-40 s, continuing increasing the voltage superposition step number once every 5s by the voltage corresponding to the current in the third stage until the current in the fourth stage is reached;
step three, after the current in the fourth stage floats in the current fluctuation range and is continuously stable for 20-40 s, the graphite electrode 1 is processed, and the current is returned to the initial current;
the current fluctuation range in the steps is 3% -7%.
In one implementation, when the current suddenly increases and exceeds the upper limit value of the current during the treatment of the graphite electrode 1, returning to the step two, and restarting the treatment process of the graphite electrode 1; the upper limit value of the current is 1400 mA.
Further, in the second step of the second step, when the current fluctuation is out of the range, the process returns to the first step of the second step, and the process of the graphite electrode 1 is restarted.
Further, in the third step of the second step, when the current fluctuation is out of range, the process returns to the second step of the second step, and the process of the graphite electrode 1 is restarted.
Further, in the fourth step of the second step, when the current fluctuation is out of range, the process returns to the third step of the second step, and the process of the graphite electrode 1 is restarted.
Further, in the treatment process of the third step, when the current fluctuation is out of the range, the fourth step of the second step is returned to, and the treatment process of the graphite electrode 1 is restarted.
In one embodiment, the first stage current is 300-450 mA, the second stage current is 450-650 mA, the third stage current is 650-850 mA, and the fourth stage current is 850-1000 mA.
In one embodiment, the graphite electrode 1 has a cavity with a bore diameter of 3-6 mm and a bore depth of 10-30 mm.
Drawings
FIG. 1 is a schematic view of the shape and structure of a graphite electrode
FIG. 2 is a schematic view showing the structure of an apparatus for automatically processing a graphite electrode by the method of the present invention
FIG. 3 is a schematic diagram of a current step-wise increase mode
FIG. 4 is a schematic diagram of a linear current increasing mode
Detailed Description
The invention will be further described in detail with reference to the following figures and examples:
referring to the attached drawing 1, the graphite electrode 1 is provided with a cavity with the aperture of 3-6 mm and the hole depth of 10-30 mm, a sample to be detected is placed in the cavity during detection, a deeper hole can be used for volatile elements, and a shallower hole can be used for low volatile elements, and 20-50 g of the sample is filled in the cavity.
Referring to fig. 2, an untreated graphite electrode 1 was inserted on a cathode tungsten wire 3 of a hollow cathode lamp 2; the outer cavity of the hollow cathode lamp 3 is filled with cooling water and circulates in the outer cavity; the control system 4 pumps out the air in the hollow cathode lamp 2, then carries in carrier gas, works after the vacuum and the carrier gas are in dynamic balance, the control system 4 applies high voltage between the cathode tungsten wire 3 and the anode 5, and the graphite electrode 1 emits light.
Setting an initial voltage, a voltage superposition step number and a current fluctuation range in the control system 4; the initial voltage is 0.2V, the corresponding initial current is 200mA, the control system 4 adjusts the voltage of the silicon controlled signal input end to provide the current for processing the graphite electrode, the minimum voltage of the silicon controlled signal input end is the initial voltage, and the voltage superposition step number is 0.007V. The graphite electrode is processed by adopting a method of increasing current in a stepwise manner, the current in the first stage is 400mA, the current in the second stage is 600mA, the current in the third stage is 800mA, the current in the fourth stage is 1000mA, and the current in each stage can be set randomly. As shown in fig. 3.
The graphite electrode was treated continuously for 30s at an initial current of 200mA, and then the initial voltage was increased by 0.007V every 5s until the initial current reached a first-stage current of 400 mA; when the first-stage current 300mA floats within 5% of the current fluctuation range and the graphite electrode is continuously and stably processed for 30s, if the first-stage current floats within 5% of the current fluctuation range within 30s, the current returns to the initial current, and the previous step is repeated; conversely, the voltage corresponding to the first-stage current continues to increase by 0.007V every 5s until the first-stage current reaches the second-stage current of 600 mA; when the current 600mA at the second stage floats within 5% of the current fluctuation range and is continuously stable for 30s, if the current floating at the second stage within 30s is not within 5% of the current fluctuation range, the current returns to the current at the first stage, and the previous step is repeated; on the contrary, the voltage corresponding to the second-stage current is continuously increased by 0.007V every 5s until the second-stage current reaches the third-stage current of 800 mA; when the current 800mA in the third stage floats within 5% of the current fluctuation range and is continuously stable for 30s, if the current in the third stage floats within 5% of the current fluctuation range within 30s, the current returns to the current in the second stage, and the previous step is repeated; on the contrary, the voltage corresponding to the current in the third stage is continuously increased by 0.007V every 5s until the current in the third stage reaches 1000mA in the fourth stage; when the current of the fourth stage floats within 5% of the current fluctuation range and is continuously stable for 30s, if the current of the fourth stage floats within 5% of the current fluctuation range within 30s, the current returns to the current of the third stage, and the previous step is repeated; and conversely, the graphite electrode 1 is processed completely, and the current returns to the initial current.
When the current suddenly increases to be larger than the upper current limit of 1400mA during the automatic processing of the graphite electrode 1, the current returns to the initial current and restarts from the initial current until the current is stabilized in the fourth stage.
The method has the advantages that the voltage superposition steps are too many, the current fluctuation range is too wide, the current stabilization time is too short, the stabilization time is easily too short, the graphite electrode is unstable to process, the current of the next stage cannot be stabilized and returns to the current of the previous stage, the processing time is too long repeatedly, and the graphite electrode processing efficiency is low; the current fluctuation range is too narrow, so that the current at the stage cannot be continuously stabilized; thereby causing low efficiency of processing the graphite electrode; the current stabilization time is too long, so that the whole graphite electrode processing time is too long, and the efficiency is low.
As shown in fig. 4, the current increased in a linear fashion, the graphite electrode was treated at an initial current of 200mA, the current fluctuated within 5% and continued to stabilize for 30s, and then the initial voltage was increased by 0.007V every 5s until the initial current reached the termination current; and after the current is stopped to float within 5% of the current fluctuation range and is continuously stable for 30s, the graphite electrode 1 is processed, and the current returns to the initial current.
And returning to the current minus 200mA current when the current floats within 5% of the current fluctuation range or the terminating current cannot be stabilized continuously for 30s from the initial current to the terminating current, and continuously increasing the corresponding current voltage by one voltage superposition step every 5s until the current reaches the terminating current.
When the current suddenly increases more than the upper current limit of 1200 mA-1400 mA during the automatic processing of the graphite electrode 1, the current returns to the initial current and increases from the initial current to the termination current again.
Compared with the prior art, the method effectively releases manpower, improves efficiency, avoids artificial errors caused by the fact that whether the graphite electrode is processed perfectly at the current stage is determined by observing whether the light source of the hollow cathode lamp is stable or not manually, is simple to operate, and ensures stable discharge of the graphite electrode during detection.
Claims (8)
1. A method for automatically processing a graphite electrode is characterized by comprising the following steps: the method comprises the following steps:
inserting an untreated graphite electrode (1) on a cathode tungsten wire (3) of a hollow cathode lamp (2), and applying high voltage between the cathode tungsten wire (3) and an anode (5) through a control system (4) to enable the graphite electrode (1) to emit light;
setting initial voltage, voltage superposition steps and a current fluctuation range through a control system (4), and processing the graphite electrode (1) by adopting a step-type current increasing method, wherein the specific process is as follows;
the first step is as follows: after the graphite electrode (1) is treated for 20-40 s by using initial voltage and corresponding initial current, the initial voltage is increased by one voltage superposition step every 5s until the current reaches the first-stage current;
the initial voltage is 0.08-0.2V, the corresponding initial current is 100-200 mA, and the voltage superposition step number is 0.005-0.009V;
the second step is that: after the first-stage current floats in the current fluctuation range and is stabilized for 20-40 s, continuing increasing the voltage superposition step number once every 5s by the voltage corresponding to the first-stage current until the second-stage current is reached;
thirdly, after the current in the second stage floats in the current fluctuation range and is stable for 20-40 s, continuing increasing the voltage superposition step number for every 5s by the voltage corresponding to the current in the second stage until the current in the third stage is reached;
fourthly, after the current in the third stage floats in the current fluctuation range and is stable for 20-40 s, continuing increasing the voltage superposition step number once every 5s by the voltage corresponding to the current in the third stage until the current in the fourth stage is reached;
step three, after the current in the fourth stage floats in the current fluctuation range and is continuously stable for 20-40 s, the graphite electrode (1) is processed, and the current is returned to the initial current;
the current fluctuation range in the steps is 3% -7%.
2. The method of automatically processing graphite electrodes of claim 1, wherein: during the treatment of the graphite electrode (1), when the current suddenly increases and exceeds the upper limit value of the current, returning to the step two, and restarting the treatment process of the graphite electrode (1);
the upper limit value of the current is 1400 mA.
3. The method for automatically processing a graphite electrode according to claim 1 or 2, wherein: and in the second step of the second step, when the current fluctuation exceeds the range, returning to the first step of the second step, and restarting the treatment process of the graphite electrode (1).
4. The method for automatically processing a graphite electrode according to claim 1 or 2, wherein: and in the third step of the second step, when the current fluctuation exceeds the range, returning to the second step of the second step, and restarting the treatment process of the graphite electrode (1).
5. The method for automatically processing a graphite electrode according to claim 1 or 2, wherein: and in the fourth step of the second step, when the current fluctuation exceeds the range, returning to the third step of the second step, and restarting the treatment process of the graphite electrode (1).
6. The method for automatically processing a graphite electrode according to claim 1 or 2, wherein: and in the treatment process of the third step, when the current fluctuation exceeds the range, returning to the fourth step of the second step, and restarting the treatment process of the graphite electrode (1).
7. The method for automatically processing a graphite electrode according to claim 1 or 2, wherein: the first stage current is 300-450 mA, the second stage current is 450-650 mA, the third stage current is 650-850 mA, and the fourth stage current is 850-1000 mA.
8. The method of automatically processing graphite electrodes of claim 1, wherein: the graphite electrode (1) is provided with a cavity with the aperture of 3-6 mm and the hole depth of 10-30 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910618256.1A CN110416040B (en) | 2019-07-09 | 2019-07-09 | Method for automatically processing graphite electrode |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910618256.1A CN110416040B (en) | 2019-07-09 | 2019-07-09 | Method for automatically processing graphite electrode |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110416040A CN110416040A (en) | 2019-11-05 |
| CN110416040B true CN110416040B (en) | 2021-07-16 |
Family
ID=68360843
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910618256.1A Active CN110416040B (en) | 2019-07-09 | 2019-07-09 | Method for automatically processing graphite electrode |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110416040B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1336783A (en) * | 2000-05-03 | 2002-02-20 | 皇家菲利浦电子有限公司 | Method and arrangement for operating gas discharge lamp |
| US7262564B2 (en) * | 2002-07-03 | 2007-08-28 | Kronos Advanced Technologies, Inc. | Electrostatic fluid accelerator for and a method of controlling fluid flow |
| CN102921761A (en) * | 2012-11-08 | 2013-02-13 | 西安诺博尔稀贵金属材料有限公司 | Method for preparing niobium-zirconium alloy wire for electric light source |
| CN103943437A (en) * | 2014-04-18 | 2014-07-23 | 北京大学 | Shaping device and method for field emission electron source emitter tip |
| CN105023820A (en) * | 2014-04-29 | 2015-11-04 | 安徽华东光电技术研究所 | Vacuum treatment method of multi-injection cathode assembly |
-
2019
- 2019-07-09 CN CN201910618256.1A patent/CN110416040B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1336783A (en) * | 2000-05-03 | 2002-02-20 | 皇家菲利浦电子有限公司 | Method and arrangement for operating gas discharge lamp |
| US7262564B2 (en) * | 2002-07-03 | 2007-08-28 | Kronos Advanced Technologies, Inc. | Electrostatic fluid accelerator for and a method of controlling fluid flow |
| CN102921761A (en) * | 2012-11-08 | 2013-02-13 | 西安诺博尔稀贵金属材料有限公司 | Method for preparing niobium-zirconium alloy wire for electric light source |
| CN103943437A (en) * | 2014-04-18 | 2014-07-23 | 北京大学 | Shaping device and method for field emission electron source emitter tip |
| CN105023820A (en) * | 2014-04-29 | 2015-11-04 | 安徽华东光电技术研究所 | Vacuum treatment method of multi-injection cathode assembly |
Non-Patent Citations (1)
| Title |
|---|
| "称量定容-ICP-AES法测定纯铁中痕量铝、铬、铜、锰、镍和硅";丁妍等;《分析试验室》;20190415;第542-547页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110416040A (en) | 2019-11-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US8173960B2 (en) | Low pressure electrospray ionization system and process for effective transmission of ions | |
| US7671344B2 (en) | Low pressure electrospray ionization system and process for effective transmission of ions | |
| US9269551B2 (en) | Tandem quadrupole mass spectrometer | |
| JP6202103B2 (en) | Mass spectrometer and mass spectrometry method | |
| EP3509086A1 (en) | Elemental analysis device and elemental analysis method | |
| Zheng et al. | A pulsed atmospheric-pressure discharge generated in contact with flowing electrolyte solutions for metal element analysis by optical emission spectrometry | |
| CN109243964A (en) | Dielectric barrier discharge ion source, analysis instrument and ionization method | |
| Page et al. | Automatic gain control in mass spectrometry using a jet disrupter electrode in an electrodynamic ion funnel | |
| CN110416040B (en) | Method for automatically processing graphite electrode | |
| CN105185688A (en) | Mass spectrograph for automatically regulating air pressure inside ion trap and operation method of mass spectrograph | |
| CN112683991A (en) | Organic matter quality detection device and method based on arc plasma | |
| Page et al. | An electrodynamic ion funnel interface for greater sensitivity and higher throughput with linear ion trap mass spectrometers | |
| CN112420479B (en) | Miniature mass spectrometer | |
| CN111199862B (en) | Capillary micro-area ionization source | |
| CN213752623U (en) | Miniature mass spectrometer | |
| CN106770144B (en) | Solid sample chemical vapor generation and sample injection method based on hydrogen plasma | |
| EP3503161A1 (en) | Method for producing gaseous ammonium for ion-molecule-reaction mass spectrometry | |
| CN219642781U (en) | Photoelectric ion source capable of continuously adjusting air pressure | |
| CN113630950B (en) | Liquid anode glow discharge micro-plasma excitation source and excitation method | |
| Kreschollek et al. | Dry analyte introduction system for ICP-MS optimization utilizing a dry plasma | |
| RU2487434C1 (en) | Mass-spectral device for quick and direct analysis of samples | |
| CN106561447A (en) | Radio frequency source high density low energy ion beam biological modification equipment | |
| CN108091546B (en) | Discharge gas assisted windowless radio frequency lamp mass spectrum ionization source | |
| CN117832043A (en) | Ion source device based on direct current hollow electrode discharge | |
| CN106561446A (en) | Microwave source high-density low-energy ion beam biological modification equipment |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |