CN105628683A - Method determining impurity content in stannic oxide electrode material - Google Patents
Method determining impurity content in stannic oxide electrode material Download PDFInfo
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- CN105628683A CN105628683A CN201511018541.8A CN201511018541A CN105628683A CN 105628683 A CN105628683 A CN 105628683A CN 201511018541 A CN201511018541 A CN 201511018541A CN 105628683 A CN105628683 A CN 105628683A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention discloses a method determining impurity content in a stannic oxide electrode material. The method comprises: adding the stannic oxide electrode into lithium tetraborate and lithium metaborate serving as a flux and mixed proportionally for melting, taking a fuse piece after cooling, adding water and inorganic strong acid to dissolve to obtain a solution to be determined, and then determining the solution to be determined by adopting an inductive coupling plasma emission spectrometer. By adopting the method disclosed by the invention, the high compactness stannic oxide electrode material can be fully dissolved, sampling is simple, various impurity elements in the stannic oxide electrode can be determined, a determined result is accurate and an analysis error is small.
Description
Technical field
The present invention relates to inorganic materials testing method, specifically, it relates to a kind of method measuring foreign matter content in tin oxide electrode materials.
Background technology
Tin oxide electrode is electric glass melting one of four large electrodes, at TFT glass furnace widely as electricity fusing-aid materials'use, for electrically heated glass liquid. Usual finding doped forms has, Sb2O3-CuO-ZnO��Sb2O3-CuO��Sb2O3-V2O3��Sb2O3-CuO-MnO2��ZnO-Nb2O3Deng. Compactness, resistance characteristic and corrosion resistance that different doped forms will directly affect tin oxide electrode. For this reason, it is necessary to carrying out analyzing mensuration to the doping component of tin oxide electrode, in the hope of obtaining the tin oxide electrode of excellent property, and its quality monitored, it is particularly necessary that this analysis is determined at the TFT glass production industry that product has high-quality requirement.
At present, the detection method of impurity content in tin oxide electrode is different, generally adopt flame atomic absorption spectrometry, spectrophotometry or inductively coupled plasma atomic emission spectrometry. And the problem adopting these methods first to be solved is that sample is prepared into solution. There is higher compactness and corrosion resistance due to tin oxide electrode materials, it is difficult to dissolve, the method of traditional dissolved oxygen tin is for adding strong acid or highly basic, but a large amount of experimental evidence shows, traditional acid-soluble or alkali solution technique all can not dissolve the tin oxide electrode of high fine and close body fully, and complex operation step, inefficiency. In addition, to the detection method of impurity element in tin oxide electrode can not compatible various impurity element simultaneously, analysis speed is slow, and accuracy of detection is low, it is difficult to meet the demand of modernization.
Summary of the invention
It is an object of the invention to provide the analytical procedure measuring foreign matter content in various model tin oxide electrode materials that a kind of sample dissolution is complete, quick, efficient, have general applicability.
In order to realize above-mentioned purpose, the present invention provides a kind of method measuring foreign matter content in tin oxide electrode materials, it is characterized in that comprising following step: tin oxide electrode is carried out molten sample by (1), the molten sheet of taking-up after cooling, adds water and inorganic acid is dissolved, and obtains liquid to be measured, it is characterized in that, also adding the lithium tetraborate as flux and lithium metaborate in the process of described molten sample, wherein, the mass ratio of described tin oxide electrode and flux is 1:(5-30); (2) typical curve for measuring foreign matter content is set up, and establishing criteria curve, adopt the liquid to be measured of inductive coupling plasma emission spectrograph determination step (1) gained.
Preferably, the mass ratio of the described lithium tetraborate in described step (1) and lithium metaborate is 1:(2-10). Further preferably, the mass ratio of described lithium tetraborate and lithium metaborate is 1:(5-8).
Preferably, the mass ratio of the described water in described step (1) and inorganic acid is (5-120): 1.
Preferably, also adding inorganic middle highly basic in the molten sample process of described step (1), the mass ratio of described tin oxide electrode and inorganic middle highly basic is 1:(2-10). Further preferably, the mass ratio of described inorganic middle highly basic and inorganic acid is 1:(5-20).
Preferably, described inorganic middle highly basic is at least one being selected from sodium hydroxide, potassium hydroxide, sodium carbonate, salt of wormwood and sodium peroxide.
Preferably, the described inorganic acid in described step (1) is at least one being selected from hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid and perchloric acid.
Preferably, in described step (1), the temperature of described molten sample is 800 DEG C-1000 DEG C, and the time of described molten sample is 10-20 minute.
Preferably, described impurity is at least one being selected from the elements such as Cu, Zn, Sb, Si, Zr, V, Nb, Mn, Al, Fe, Ca and Mg.
Compared with prior art, a kind of method tool measuring foreign matter content in tin oxide electrode materials provided by the invention has the following advantages:
(1) sample pretreatment process is simple, and the tin oxide electrode materials of high compactness can be completely dissolved, sample preparation success ratio height, and molten sample process temperature required lower, the molten sample time is shorter;
(2) detection efficiency height, it is possible to the Determination of Multi-Impurities in the various model tin oxide electrode of Simultaneously test, analyzes and realizes full-automaticization, fast, efficiently;
(3) measurement result is accurate, and analytical error is little.
In addition, the present inventor finds in an experiment unexpectedly, adopt lithium tetraborate and lithium metaborate to add according to the mixing of specific ratio and tin oxide electrode sample carries out molten sample, with do not add lithium tetraborate and compare with lithium metaborate, more easily molten sheet is spun off from platinum crucible after having founded cooling, the sample demoulding is complete, the errors of analytical results that the sample loss decreased in sample making course brings, and detected result is more accurately and reliably.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Embodiment
Hereinafter the specific embodiment of the present invention is described in detail. Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The present invention provides a kind of method measuring foreign matter content in tin oxide electrode materials, it is characterized in that comprising following step: tin oxide electrode is carried out molten sample by (1), molten sheet is taken out after cooling, add water and inorganic acid is dissolved, obtain liquid to be measured, it is characterised in that, the process of described molten sample also adds the lithium tetraborate as flux and lithium metaborate, wherein, the mass ratio of described tin oxide electrode and flux is 1:(5-30); (2) typical curve for measuring foreign matter content is set up, and establishing criteria curve, adopt the liquid to be measured of inductive coupling plasma emission spectrograph determination step (1) gained.
According to the present invention, the operation steps adopting ICP to carry out testing is well known to those skilled in the art, typical curve is set up according to ICP standard addition method, under the best conditions of instrument, bioassay standard liquid, the automatic Criterion curve of instrument, then measures liquid to be measured under same working conditions, and instrument calculates the content of each impurity in liquid to be measured automatically.
According to the present invention, described step (1) adds lithium tetraborate and lithium metaborate can make the tin oxide electrode materials of high compactness dissolve completely as flux, and molten sample complete cooling after molten sheet more easily depart from from platinum crucible, the sample demoulding is complete. The mass ratio of described lithium tetraborate and described lithium metaborate can be 1:(2-10). Preferably, the mass ratio of described lithium tetraborate and described lithium metaborate can be 1:(5-8).
According to the present invention, the object adding water and inorganic acid in described step (1) obtains clear liquor to make molten sheet dissolve, and after adding water and inorganic acid, the acidity of solution is at 2%-20%. Preferably, the mass ratio of the described water in described step (1) and inorganic acid can be (5-120): 1.
According to the present invention, in order to improve the dissolving situation of tin oxide electrode further and shorten the molten sample time, can also adding inorganic middle highly basic in the molten sample process of described step (1), the mass ratio of described tin oxide electrode and inorganic strongest's alkali can be 1:(2-10).
According to the present invention, the inorganic middle highly basic added in molten sample process should not affect the acidity that molten sheet dissolves described clear liquor when obtaining clear liquor, and the mass ratio of described inorganic middle highly basic and inorganic acid can be 1:(5-20);
According to the present invention, described inorganic middle highly basic and inorganic acid can select this area to commonly use material, as inorganic middle highly basic can at least one for being selected from sodium hydroxide, potassium hydroxide, sodium carbonate, salt of wormwood and sodium peroxide; Described inorganic acid can at least one for being selected from hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid and perchloric acid.
According to the present invention, in described step (1), by adding flux and inorganic middle highly basic in molten sample process, described molten sample process can complete in lower temperature with under the shorter time, the temperature of described molten sample can be 800 DEG C-1000 DEG C, and the time of described molten sample can be 10-20 minute.
Method according to mensuration tin oxide electrode materials provided by the invention, the Determination of Multi-Impurities in tin oxide electrode materials can be measured, preferably, described impurity can at least one for being selected from the elements such as Cu, Zn, Sb, Si, Zr, V, Nb, Mn, Al, Fe, Ca and Mg.
Come by the following examples the present invention is described further, but the present invention is not therefore subject to any restriction.
The embodiment of the present invention and comparative example adopt inductive coupling plasma emission spectrograph (ICP-OES) to be measured by foreign matter content in tin oxide electrode materials, and test condition is: RF power is 1000KW, plasma (orifice) gas: 12L/min; Atomization gas: 0.8L/min; Auxiliary gas: 0L/min; Sheath gas: 2L/min; Observed altitude 15mm, integral time 10s. , pump speed is 50r/min, and pump steady time is 0s.
Embodiment 1
(1) being ground to the tin oxide electrode sample of a known impurity level without, after granular sensation, being put in weighing bottle, be placed in 110 DEG C of baking ovens after dry 2 hours, taking-up is placed in moisture eliminator and is cooled to room temperature. Platinum crucible adds 1g lithium tetraborate, after 2g lithium metaborate, accurately takes 0.1000g (being accurate to 0.0001g) tin oxide electrode sample in wherein, then add 1g sodium hydrate solid and cover on it; Platinum crucible is placed in high frequency fusion stove at 1000 DEG C of temperature, heats 10min; Taking out platinum crucible, taken out by molten sheet after cooling, after being put in beaker to add 200g pure water, pipette the pure concentrated hydrochloric acid of excellent level that 15g concentration is 36.5%, being placed on electric furnace heating for dissolving obtains clear solution, is transferred in 250mL volumetric flask;
(2) prepare and needed for standard addition method, add mark sample series standardized solution, Criterion curve on ICP;
(3) sample solution step (1) obtained detects according to the typical curve built on ICP, and test result is such as table 1.
Embodiment 2
(1) being ground to the tin oxide electrode sample of a known impurity level without, after granular sensation, being put in weighing bottle, be placed in 110 DEG C of baking ovens after dry 2 hours, taking-up is placed in moisture eliminator and is cooled to room temperature. Platinum crucible adds 0.4g lithium tetraborate, after 2g lithium metaborate, accurately takes 0.1000g (being accurate to 0.0001g) tin oxide electrode sample in wherein, then add 0.5g sodium hydrate solid and cover on it, do sample blank test simultaneously; Platinum crucible is placed in high frequency fusion stove at 1000 DEG C of temperature, heats 15min; Taking out platinum crucible, taken out by molten sheet after cooling, after being put in beaker to add 230g pure water, pipette the pure concentrated nitric acid of excellent level that 8g concentration is 65%, being placed on electric furnace heating for dissolving obtains clear solution, is transferred in 250mL volumetric flask; Step (2), step (3) are consistent with embodiment 1, and test result is such as table 1.
Embodiment 3
(1) being ground to the tin oxide electrode sample of a known impurity level without, after granular sensation, being put in weighing bottle, be placed in 110 DEG C of baking ovens after dry 2 hours, taking-up is placed in moisture eliminator and is cooled to room temperature. Platinum crucible adds 0.1g lithium tetraborate, after 0.8g lithium metaborate, accurately takes 0.1000g (being accurate to 0.0001g) tin oxide electrode sample in wherein, then add 0.2g sodium hydrate solid and cover on it, do sample blank test simultaneously; Platinum crucible is placed in high frequency fusion stove at 1000 DEG C of temperature, heats 20min; Taking out platinum crucible, taken out by molten sheet after cooling, after being put in beaker to add 230g pure water, pipette the pure perchloric acid of excellent level that 5g concentration is 72%, being placed on electric furnace heating for dissolving obtains clear solution, is transferred in 250mL volumetric flask; Step (2), step (3) are consistent with embodiment 1, and test result is such as table 1.
Embodiment 4
Only being in step (1) to add 1g lithium tetraborate and 0.5g lithium metaborate with the difference of embodiment 1, other steps are all consistent with embodiment 1, and test result is such as table 1.
Embodiment 5
Only being in step (1) do not add sodium hydroxide with the difference of embodiment 1, other steps are all consistent with embodiment 1, and test result is such as table 1.
Comparative example 1
Only being in step (1) do not add lithium tetraborate and lithium metaborate with the difference of embodiment 1, other steps are all consistent with embodiment 1, and test result is such as table 1.
Comparative example 2
Only being in step (1) only add 1g lithium tetraborate with the difference of embodiment 1, other steps are all consistent with embodiment 1, and test result is such as table 1.
Table 1
By the experimental result of embodiment 1-5 and comparative example 1 and 2 it may be seen that the method adopting the present invention can accurately measure the foreign matter content in tin oxide electrode materials. By carrying out mixing as flux according to extra fine quality ratio with lithium metaborate using lithium tetraborate, with do not add lithium tetraborate and lithium metaborate, or only add lithium tetraborate and compare, effectively solve the problem that tin oxide electrode is difficult to dissolve, overcome the deficiency of traditional analysis, significantly improve the accuracy of measurement result. When the mass ratio of lithium tetraborate and lithium metaborate is 1:(2-10) time the solute effect of tin oxide electrode is better. The feature that in the mensuration tin oxide electrode materials of the present invention, the method for foreign matter content has fast, easy, accuracy is high, can meet the needs that glass production industry can control with quality product completely.
Claims (10)
1. measuring a method for foreign matter content in tin oxide electrode materials, wherein, the method comprises the following steps:
(1) tin oxide electrode is carried out molten sample, molten sheet is taken out after cooling, add water and inorganic acid is dissolved, obtain liquid to be measured, it is characterized in that, also adding the lithium tetraborate as flux and lithium metaborate in the process of described molten sample, wherein, the mass ratio of described tin oxide electrode and flux is 1:(5-30);
(2) typical curve for measuring foreign matter content is set up, and establishing criteria curve, adopt the liquid to be measured of inductive coupling plasma emission spectrograph determination step (1) gained.
2. method according to claim 1, wherein, described lithium tetraborate and the mass ratio of lithium metaborate in described step (1) are 1:(2-10).
3. method according to claim 2, wherein, the mass ratio of described lithium tetraborate and lithium metaborate is 1:(5-8).
4. method according to claim 1, wherein, described water and the mass ratio of inorganic acid in described step (1) are (5-120): 1.
5. method according to claim 1, wherein, also adds inorganic middle highly basic in the molten sample process of described step (1), and the mass ratio of described tin oxide electrode and inorganic strong alkali is 1:(2-10).
6. method according to claim 5, wherein, the mass ratio of described inorganic middle highly basic and inorganic acid is 1:(5-20).
7. method according to claim 5, wherein, described inorganic middle highly basic is at least one being selected from sodium hydroxide, potassium hydroxide, sodium carbonate, salt of wormwood and sodium peroxide.
8. method according to claim 1, wherein, the described inorganic acid in described step (1) is at least one being selected from hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid and perchloric acid.
9. method according to claim 1, wherein, in described step (1), the temperature of described molten sample is 800 DEG C-1000 DEG C, and the time of described molten sample is 10-20 minute.
10. the method for foreign matter content in mensuration tin oxide electrode materials according to claim 1, wherein, described impurity is at least one being selected from the elements such as Cu, Zn, Sb, Si, Zr, V, Nb, Mn, Al, Fe, Ca and Mg.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106568643A (en) * | 2016-11-09 | 2017-04-19 | 芜湖东旭光电科技有限公司 | Method for measuring impurity content in aluminium oxide sample and method of sample pretreatment |
| CN110455598A (en) * | 2019-09-02 | 2019-11-15 | 蚌埠中光电科技有限公司 | The sample treatment of impurity in a kind of detection stannic oxide |
| CN112179899A (en) * | 2020-10-09 | 2021-01-05 | 蒙自海关综合技术中心 | Method for detecting total iron content in iron ore |
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| GB2291184A (en) * | 1994-07-02 | 1996-01-17 | Natural Environment Res | Inductively-coupled plasma atomic emission spectrometer |
| CN102426122A (en) * | 2011-09-07 | 2012-04-25 | 河北钢铁股份有限公司邯郸分公司 | Sample preparation method by fusing medium-carbon ferrochrome and high-carbon ferrochrome |
| CN102564834A (en) * | 2011-12-19 | 2012-07-11 | 攀钢集团攀枝花钢铁研究院有限公司 | Digestion method of metallurgical materials and detection method |
| CN102998300A (en) * | 2012-11-19 | 2013-03-27 | 中国船舶重工集团公司第七二五研究所 | Analysis method for impurity elements in tin-oxide-containing nanopowder |
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- 2015-12-29 CN CN201511018541.8A patent/CN105628683A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| GB2291184A (en) * | 1994-07-02 | 1996-01-17 | Natural Environment Res | Inductively-coupled plasma atomic emission spectrometer |
| CN102426122A (en) * | 2011-09-07 | 2012-04-25 | 河北钢铁股份有限公司邯郸分公司 | Sample preparation method by fusing medium-carbon ferrochrome and high-carbon ferrochrome |
| CN102564834A (en) * | 2011-12-19 | 2012-07-11 | 攀钢集团攀枝花钢铁研究院有限公司 | Digestion method of metallurgical materials and detection method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106568643A (en) * | 2016-11-09 | 2017-04-19 | 芜湖东旭光电科技有限公司 | Method for measuring impurity content in aluminium oxide sample and method of sample pretreatment |
| CN110455598A (en) * | 2019-09-02 | 2019-11-15 | 蚌埠中光电科技有限公司 | The sample treatment of impurity in a kind of detection stannic oxide |
| CN112179899A (en) * | 2020-10-09 | 2021-01-05 | 蒙自海关综合技术中心 | Method for detecting total iron content in iron ore |
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