CN1796983A - Method for analyzeing carbon, sulphur and phosphor in rare metal through emission spectrum, and new light source device - Google Patents
Method for analyzeing carbon, sulphur and phosphor in rare metal through emission spectrum, and new light source device Download PDFInfo
- Publication number
- CN1796983A CN1796983A CNA2004101025144A CN200410102514A CN1796983A CN 1796983 A CN1796983 A CN 1796983A CN A2004101025144 A CNA2004101025144 A CN A2004101025144A CN 200410102514 A CN200410102514 A CN 200410102514A CN 1796983 A CN1796983 A CN 1796983A
- Authority
- CN
- China
- Prior art keywords
- light source
- rare metal
- sulphur
- power supply
- carbon
- 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.)
- Granted
Links
Images
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention is a method for analyzing C, S and P in a rare-earth metal by emission spectrum, firstly putting a to-be-detected sample in electrode cavity; selecting a large capacitor with a corresponding value and connecting the large capacitor in parallel to a control circuit; charging argon gas and starting up a light source generating device to excite high energy a large spark with high energy so as to excite the radiation of the sample; a new light source device for implementing the method, comprises a light source generating device and a pair of emission electrodes, where a control circuit in the light source generating device comprises: a power supply, where one output of the power supply is connected to one end of each of two high frequency-blocking protective inductances and the two ends of a large capacitor is connected with the other two ends of them, respectively; the other output of the power supply is connected with a high voltage transformer, the secondary coil of the high voltage transformer is connected to an adjustable inductance high frequency transformer, and the two ends of the secondary coil of the high frequency transformer is connected through a protective circuit to those of an analytical gap, respectively. The device is also provided with a spin chamber with upper and lower air holes, where the two opposite sides of the spin chamber are made with a gas inlet each.
Description
Technical field
The present invention relates to the method and the new light sources equipment thereof of carbon, sulphur, phosphorus in a kind of emission spectrographic analysis rare metal.
Background technology
For the spectroscopic analysis methods of carbon, sulphur, phosphorus (C, S, P) in the rare metal, up to this point, main method is to analyze in the steel or oil with the vacuum quantorecorder spark both at home and abroad
(2)In C, S, P, its defective is relatively low for C, S, P sensitivity for analysis in the coloured and rare metal, and often is subjected to the interference of multiline and overall background and influences.
The normal cover system equipment that adopts in having now to rare infusibility and rare-earth spectrum analysis; as shown in Figure 4: the spark discharge light supply apparatus 201 ' exciting electrode 202 ' by light source produces electric arc, spark; plasma in the measured matter in the exciting electrode cave 2021 '; by spectroanalysis instrument 4 ' it is taken, adds up, analyzes; Ar gas (can provide by Ar gas tank 3 ') is provided in the work simultaneously electric arc, spark and peripheral oxygen are isolated, in spark excitation, to be used as anti-oxidation atmosphere protection.Common way is to adopt through type atmosphere control box 1 ' about in the of, directly by feeding Ar gas flatly, another mouthful gives vent to anger (the arrow indication moves towards for gas circuit among the figure), and formation is to the encirclement of spark, but comparatively speaking, this through type atmosphere control box air consumption is big, and the per minute gas consumption is 20 liters/minute, and limited to condensed spark discharge prevention dynamics; Continuous working is poor, and every detection once needs to shut down behind the measured matter of changing in the electrode cave to wash with the Ar air purge restarts.
The spark discharge light supply apparatus 202 ' of above-mentioned existing light source is that the electric cabinet by built-in control circuit constitutes, control circuit generally adopts the classic travel route of arc spark, wherein used electric capacity is 0.01-6.0uuF, the spark energy that produces is lower, to legibility in some rare metals from infusibility main body (comprising the spectral analysis of carbon in the rare metal, sulphur, phosphorus) then analyze ineffective, sensitivity is low, can not satisfy the analysis requirement.
Summary of the invention
The method that the purpose of this invention is to provide carbon, sulphur, phosphorus in a kind of emission spectrographic analysis rare metal, adopt this method can commonly used analyze wave band analyze coloured and rare metal in C, S, P.
Another object of the present invention provides the new light sources equipment of carbon, sulphur, phosphorus method in a kind of emission spectrographic analysis rare metal, adopts this device can produce high-octane spark light source, makes highly sensitive to the spectral analysis of carbon, sulphur, phosphorus in the rare metal.
For achieving the above object, the present invention takes following design proposal:
The method of carbon, sulphur, phosphorus in a kind of emission spectrographic analysis rare metal, its method is as follows:
1) tested rare metal sample is inserted in the electrode cave;
2) incorporate in the control circuit of light source generating means according to the big electric capacity of the selected respective value of determination object;
3) air intake opening by the atmosphere pulpit charges into argon gas and starts the light source generating means simultaneously, excites the big condensed spark of high-energy under the argon gas atmosphere protection, and the excitation sample makes it radiation under the big spark of high-energy.
Described argon gas by be positioned at the atmosphere pulpit not two air intake openings of homonymy charge into, form the eddy current type argon gas atmosphere, the flow velocity that argon gas charges into is 3～4 liters/minute.
In the above-mentioned steps 2, when in the emission spectrographic analysis rare metal during carbon, selected big capacitance is 50 μ F; When in the emission spectrographic analysis rare metal when sulphur, phosphorus, selected big capacitance is that 5 μ F are good.
The new light sources equipment of the method for carbon, sulphur, phosphorus in a kind of emission spectrographic analysis rare metal, the a pair of emitting electrode that comprises light source generating means and output control thereof, described light source generating means is made of the electric cabinet of built-in control circuit, and described control circuit comprises:
One power supply, power supply one tunnel output are connected to an end of two obstruct carrier current protection power supply inductance, and two other ends that intercept carrier current protection power supply inductance are incorporated a big electric capacity into;
Another road output of power supply connects high-tension transformer; the secondary coil of high-tension transformer is connected to the adjustable high-frequency transformer of inductance again; secondary coil one end of high-frequency transformer is connected to an end of analytical gap through electric capacity, the resistance of holding circuit, and the other end is connected to the other end of analytical gap.
Also be furnished with an atmosphere pulpit in this new light sources equipment, comprise having the swirl air chamber of pore up and down, respectively open an air intake opening in the two opposite sides of swirl air chamber.
Advantage of the present invention is:
1, sensitivity for analysis height: the high-energy spark light source of generation can improve several times to the sensitivity for analysis of carbon, sulphur, phosphorus in the rare metal than prior art.
2, Ar gas control system effect is good: can further reduce the influence of main body, improve the launching efficiency of carbon, sulphur, phosphorus in the rare metal.Reduce on the one hand the overall background radiation that the big fire lace comes, improve letter one sensitivity for analysis when of making an uproar, can reduce electrode temperature on the other hand, improve the degree and the spark stability of sputter vaporization.
Description of drawings
Fig. 1 is the electrical schematic diagram of new light sources equipment spark discharge light supply apparatus of the present invention
Fig. 2 is the swirl air chamber structural representation of new light sources equipment of the present invention
Fig. 3 is A-A cross-sectional view among Fig. 2 (the arrow indication is that gas circuit is moved towards among the figure)
Fig. 4 constitutes synoptic diagram for total system equipment in the existing spectral analysis
Fig. 5 is analytic curve figure of the present invention
Fig. 6 is analytic curve figure of the present invention
Embodiment
The new light sources equipment of the method for carbon, sulphur, phosphorus in the emission spectrographic analysis rare metal of the present invention, also roughly the same prior art equipment is provided with, the a pair of emitting electrode (can with reference to shown in the figure 4) that comprises light source generating means and output control thereof, its unique point are the transformation to the atmosphere control box of the built-in control circuit of light source generating means and electric arc, spark periphery.
As shown in Figure 1, described light source generating means is made of the electric cabinet of built-in control circuit, and built-in control circuit comprises:
One power supply, power supply one tunnel output are connected to the end of two obstruct carrier current protection power supply inductance L 1, L2, and two other ends that intercept carrier current protection power supply inductance L 1, L2 are incorporated a big capacitor C into;
Another road output of power supply meets high-tension transformer T1; the secondary coil of high-tension transformer T1 is connected to the adjustable high-frequency transformer T4 of inductance again; secondary coil one end of high-frequency transformer T4 is through the capacitor C 3 of holding circuit, the end that resistance R 3 is connected to analytical gap K, and the other end is connected to the other end of analytical gap K.
In the built-in control circuit of above-mentioned light source generating means, the big capacitor C of incorporating into can adopt 5～100 μ F electric capacity adjustable.
The characteristics of above-mentioned light source are: discharge current is bigger, and maximum can reach I0A (effective value), thereby the excitation energy height, and excitation temperature can reach 10000 ° more than the K.
Big condensed spark excitation source can provide technical foundation preferably.Yet, it still is not enough eliminating the influence of sample main body in electric arc, another big characteristic of the present invention is to utilize the swirl air chamber of design voluntarily, make big condensed spark discharge obtain more excellent results with pure Ar gas control system, can further reduce the influence of main body, improve the launching efficiency of high excitation potential impurity.Reduce on the one hand the overall background radiation that the big fire lace comes, improved letter one sensitivity for analysis when of making an uproar, reduced electrode temperature on the other hand, improved the degree and the spark stability of sputter vaporization.For not evaporable infusibility material, the sputter of the big condensed spark of cause makes its even evaporation, the electronegative potential of the main body launching efficiency of the high excitation potential impurity of influence greatly that dissociates is controlled by the launching efficiency of big condensed spark and the environment of motive high ionization current potential, reduce.
The structure of above-mentioned swirl air chamber constitutes and can comprise having the atmosphere control box body 1 of pore 101 up and down referring to Fig. 2, shown in Figure 3, respectively opens an air intake opening 21,22 in the two opposite sides of atmosphere control box.
Above-mentioned two air intake openings are the duct type gas port, and wherein the extensions angle theta of a duct type gas port and another duct type gas port is 12～18 °.
Establish a quartz window 3 at the non-air inlet side of atmosphere control box.This quartz window can be made into the buckle closure formula of ground, and during work, buckle closure 301 is buckled, and only plays the form effect, and during off working state, buckle closure 301 can be taken down, and with convenient the atmosphere control box is cleared up.
Adopt spectral analysis of the present invention to carry out pure Ar gas control system with swirl air chamber, its principle of work and process are: use vortex air intake, give vent to anger by around the electrode, it is big to have eliminated in the past in the through type atmosphere control box flow velocity, air pressure is little and cause entering of surrounding air, thereby controlled atmospher is effective, and the article on plasma body has heat hoop Shu Xiaoying, thereby improves the temperature and the launching efficiency of plasma.Measure by experiment, allow the meeting in a certain angle of two duct type gas ports make atmosphere control better effects if.
The big capacitance of incorporating in the above-mentioned light source generating means can be incorporated into as required flexibly, is the result who adopts experiment to measure below:
1, the spectrum experiment condition is as shown in table 1
Table 1 spectrum experiment condition
| Spectrometer light source atmosphere electrode exposure sense plate | The PGS-2 grating spectrograph, three lighting system of lens, center wave band 240.0nm～350.0nm, the electric arc of the big spark of intercept 3.2m. the spark combined light source.Electric capacity is adjustable, and 5～100uF argon gas is controlled at swirl air chamber is lathed o4 * 4 with red copper electrode cave dress sample, to electrode is taper 1min Tianjin II type, standardization |
2, measure the influence of electric capacity to sensitivity:
With the listed condition of table 1 electric capacity is changed, observe best analytical line, usefulness log ((I/ φ)=log (I (A+ φ)-I φ)/I φ)=log (((I (
A+ φ)/I φ)-I)) and with the button background and with the characterization value that the signal-to-noise of detaining background likens sensitivity to test.Result such as table 2.
Table 2 electric capacity is to the influence of sensitivity for analysis
Wherein: S
I (A+ Φ)---analytical line blackness and background blackness sum;
S
I Φ---the background blackness
LogR---calculated value, the logarithm of analytical line intensity and the ratio of background intensity;
C
247.8nm, P
330.8nm, S
349.7nmBe respectively the analytical line of carbon (C), phosphorus (P), sulphur (S).
3, result:
Analyze carbon (C) and select 247.8 for use, electric capacity 50uF uses 330.8nm and analyze phosphorus (P), and sulphur (S) 349.7nm, electric capacity 5uF are good.
So when in the emission spectrographic analysis rare metal during carbon, selected big capacitor C value is 50 μ F; When in the emission spectrographic analysis rare metal when sulphur, phosphorus, selected big capacitance C is that 5 μ F are good.
The present invention is further described below by specific embodiment:
Embodiment 1:
1) but to join among the Cu preparation one cover content with simple substance C by the element wt proportion by subtraction be 1%, 0.3%, 0.1%, 0.03%, 0.01% standard.
2) by testing requirements, each unit of debugging spectroscopic analysis system is a normal operating conditions, incorporates the big electric capacity of 50 μ F into light source generating means control circuit;
3) the tested rare metal sample of above-mentioned configuration is inserted in the electrode cave, open argon bottle, charge into argon gas by the air intake opening of atmosphere pulpit to swirl air chamber, the control flow velocity is 3～4 liters/minute, and starts the light source generating means simultaneously;
4) the big condensed spark of high-energy is seted out, and the rare metal sample excites under the big spark of high-energy, and spectrometer is taken;
5) numerical value measured in record, usefulness logC-log ((I (
A+ φ)/I
φ)) workmanship's curve.
The C analytic curve is referring to table 3 among the Cu
The analytic curve of C in the table 3 Cu powder
| LogC | 0.01 | 0.03 | 0.1 | 0.3 | 1.0 |
| LogR | -1.46 | -1.10 | -0.61 | -0.09 | 0.40 |
Embodiment 2:
But adding preparation one cover content in the Si powder with sodium phosphate by the element wt proportion by subtraction is 1%, 0.3%, 0.1%, 0.03%, 0.01% standard.Concrete experimental procedure is with embodiment 1, and difference is: the big electric capacity of 5 μ F is incorporated in the light source generating means control circuit; With logC-log ((I (
A+ φ)/I
φ)) workmanship's curve, the P analytic curve is referring to table 4 among the Si.
The analytic curve of P in the table 4 Si powder
| LogC | 0.025 | 0.05 | 0.1 | 0.3 | 1.0 |
| LogR | -1.85 | -1.66 | -1.49 | -1.20 | -0.95 |
Embodiment 3:
But adding preparation one cover content in the Si powder with simple substance S by the element wt proportion by subtraction is 1%, 0.3%, 0.1%, 0.03%, 0.01% standard.Concrete experimental procedure is with embodiment 1, and difference is: the big electric capacity of 5 μ F is incorporated in the light source generating means control circuit; With logC-log ((I (
A+ φ)/I
φ)) workmanship's curve, the S analytic curve is referring to table 5 among the Si.
The analytic curve of S in the table 5 Si powder
| LogC | 0.025 | 0.05 | 0.1 | 0.3 | 1.0 |
| LogR | -1.76 | -1.62 | -1.46 | -1.22 | -1.01 |
For convenience of explanation, the data that embodiment 1～3 experiment is recorded are made Fig. 5, Fig. 6.By Fig. 5 explanation, to the analysis of C, strengthening booster dose is favourable to sensitivity, and curve a slope is higher.Under existence conditions S, P sensitivity is not good enough, and high background influence is bigger, curve b, curve c slope lower (referring to Fig. 6) improves evaporation or separates main body and could further improve sensitivity.
Claims (8)
1, the method for carbon, sulphur, phosphorus in a kind of emission spectrographic analysis rare metal is characterized in that method is as follows:
1) tested rare metal sample is inserted in the electrode cave;
2) incorporate in the control circuit of light source generating means according to the big electric capacity of the selected respective value of determination object;
3) air intake opening by the atmosphere pulpit charges into argon gas and starts the light source generating means simultaneously, excites the big condensed spark of high-energy under the argon gas atmosphere protection, and the excitation sample makes it radiation under the big spark of high-energy.
2, the method for carbon, sulphur, phosphorus in the emission spectrographic analysis rare metal according to claim 1, it is characterized in that: described argon gas by be positioned at the atmosphere pulpit not two air intake openings of homonymy charge into, form the eddy current type argon gas atmosphere, the flow velocity that argon gas charges into is 3～4 liters/minute.
3, the method for carbon, sulphur, phosphorus in the emission spectrographic analysis rare metal according to claim 1 is characterized in that: when in the emission spectrographic analysis rare metal during carbon, selected big capacitance is 50 μ F; When in the emission spectrographic analysis rare metal when sulphur, phosphorus, selected big capacitance is 5 μ F.
4, the new light sources equipment of the method for carbon, sulphur, phosphorus in a kind of emission spectrographic analysis rare metal, the a pair of emitting electrode that comprises light source generating means and output control thereof, described light source generating means is made of the electric cabinet of built-in control circuit, it is characterized in that described control circuit comprises:
One power supply, power supply one tunnel output is connected to an end of two obstruct carrier current protection power supply inductance (L1, L2), and two other ends that intercept carrier current protection power supply inductance (L1, L2) are incorporated a big electric capacity (C) into;
Another road output of power supply connects high-tension transformer (T1); the secondary coil of high-tension transformer (T1) is connected to the adjustable high-frequency transformer of inductance (T4) again; secondary coil one end of high-frequency transformer (T4) is through the electric capacity (C3) of holding circuit, the end that resistance (R3) is connected to analytical gap (K), and the other end is connected to the other end of analytical gap (K).
5, new light sources equipment according to claim 4 is characterized in that: it also is furnished with an atmosphere pulpit, comprises having the swirl air chamber of pore up and down, respectively opens an air intake opening in the two opposite sides of swirl air chamber.
6, new light sources equipment according to claim 5 is characterized in that: two air intake openings are the duct type gas port, and wherein the extensions angle theta of a duct type gas port and another duct type gas port is 12～18 °.
7, new light sources equipment according to claim 5 is characterized in that: the non-air inlet side in the atmosphere pulpit is established a quartz window.
8, new light sources equipment according to claim 7 is characterized in that: described quartz window has the fastening lid of ground.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004101025144A CN100447556C (en) | 2004-12-24 | 2004-12-24 | Method for analyzeing carbon, sulphur and phosphor in rare metal through emission spectrum, and new light source device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004101025144A CN100447556C (en) | 2004-12-24 | 2004-12-24 | Method for analyzeing carbon, sulphur and phosphor in rare metal through emission spectrum, and new light source device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1796983A true CN1796983A (en) | 2006-07-05 |
| CN100447556C CN100447556C (en) | 2008-12-31 |
Family
ID=36818193
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004101025144A Expired - Fee Related CN100447556C (en) | 2004-12-24 | 2004-12-24 | Method for analyzeing carbon, sulphur and phosphor in rare metal through emission spectrum, and new light source device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100447556C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101294905B (en) * | 2008-05-22 | 2011-05-04 | 浙江沃尔达铜业有限公司 | Method for fast detecting metal composition |
| WO2012028484A1 (en) | 2010-09-03 | 2012-03-08 | Thermo Fisher Scientific (Ecublens) Sarl | Improved spark chamber for optical emission analysis |
| CN102608104A (en) * | 2011-09-06 | 2012-07-25 | 北京瑞利分析仪器有限公司 | Direct-reading spectrometer based on combination of alternating current/direct current arc and concave grating beam splitting system |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2603998B2 (en) * | 1987-11-30 | 1997-04-23 | 株式会社島津製作所 | Emission spectrometer |
| JP2004003988A (en) * | 2002-03-15 | 2004-01-08 | Matsushita Electric Ind Co Ltd | System and method for identifying metal |
| CN1160552C (en) * | 2002-04-01 | 2004-08-04 | 钢铁研究总院 | In-situ metal analyzer |
-
2004
- 2004-12-24 CN CNB2004101025144A patent/CN100447556C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101294905B (en) * | 2008-05-22 | 2011-05-04 | 浙江沃尔达铜业有限公司 | Method for fast detecting metal composition |
| WO2012028484A1 (en) | 2010-09-03 | 2012-03-08 | Thermo Fisher Scientific (Ecublens) Sarl | Improved spark chamber for optical emission analysis |
| CN102608104A (en) * | 2011-09-06 | 2012-07-25 | 北京瑞利分析仪器有限公司 | Direct-reading spectrometer based on combination of alternating current/direct current arc and concave grating beam splitting system |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100447556C (en) | 2008-12-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US6750449B2 (en) | Sampling and analysis of airborne particulate matter by glow discharge atomic emission and mass spectrometries | |
| Okamoto | High-sensitivity microwave-induced plasma mass spectrometry for trace element analysis | |
| CN105115959B (en) | The liquid phase cathodic discharge plasma spectrometry rapid detection system and detection method of metallic element | |
| US7381973B2 (en) | Analyzer system and method incorporating excimer UV fluorescence detection | |
| Zheng et al. | A pulsed atmospheric-pressure discharge generated in contact with flowing electrolyte solutions for metal element analysis by optical emission spectrometry | |
| CN109904056B (en) | Chemical ionization-vacuum ultraviolet single photon ionization composite ionization source device based on air discharge | |
| JP2013532349A (en) | Oxidation resistance induction device | |
| CN109887833A (en) | A kind of combined type ion source bipolarity linear ion trap mass analyzer | |
| CN105632871A (en) | Mass spectrum chemical ionization source based on UV light emitting diode | |
| CN1796983A (en) | Method for analyzeing carbon, sulphur and phosphor in rare metal through emission spectrum, and new light source device | |
| Minnich et al. | Direct injection high efficiency nebulization in inductively coupled plasma mass spectrometry under cool and normal plasma conditions | |
| CN1811408A (en) | Internal photo ionization ion trap quality analyzer and method thereof | |
| CN106206239B (en) | High-efficient combination formula atmospheric pressure ionization source | |
| CN112378986A (en) | Mass spectrometry method | |
| CN207719138U (en) | A kind of portable mass spectrometer | |
| Hayashi et al. | Determination of traces of phosphorus in steels by laser ablation/low-pressure helium-ICP-MS | |
| Oskolok et al. | X-ray fluorescence and atomic emission determination of cobalt in water using polyurethane foam sorbents | |
| CN212517113U (en) | Radio frequency discharge excited methylene dichloride induced proton transfer reaction ion source | |
| JP2006071492A (en) | Apparatus and method for measuring particulate component in gas | |
| Goleb | Near Ultraviolet-Visible Atomic Absorption Spectra of the Noble Gases. | |
| Winefordner et al. | Status of and perspectives on microwave and glow discharges for spectrochemical analysis. Plenary lecture | |
| Cousins et al. | High-voltage spark spectra: utility as a function of temporal and spatial resolution | |
| CN219319921U (en) | Integrated sample leading-in detection device | |
| CN210037726U (en) | Liquid chromatography-mass spectrometer for detecting veterinary drug residues in meat products | |
| Vallance Jones et al. | Indirect excitation processes in aurora |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20160530 Address after: Yang Yanlu 101407 Beijing city Huairou District Yanqi Economic Development Zone No. 88 Patentee after: National standard (Beijing) inspection & Certification Co., Ltd. Address before: 100088, 2, Xinjie street, Beijing Patentee before: General Research Institute for Nonferrous Metals |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20081231 Termination date: 20161224 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |