CN102721678A - Solid acid tablet for quick field detection of portable atomic fluorescence and preparation method and application thereof - Google Patents
Solid acid tablet for quick field detection of portable atomic fluorescence and preparation method and application thereof Download PDFInfo
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- CN102721678A CN102721678A CN2012102380167A CN201210238016A CN102721678A CN 102721678 A CN102721678 A CN 102721678A CN 2012102380167 A CN2012102380167 A CN 2012102380167A CN 201210238016 A CN201210238016 A CN 201210238016A CN 102721678 A CN102721678 A CN 102721678A
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Abstract
The invention relates to a solid acid tablet for quick field detection of portable atomic fluorescence by adopting the chemical vapor generation and sample introduction technology. The solid acid tablet comprises the following components by weight percent: 1-10 parts of solid acid and 1-2 parts of molding agent, wherein the solid acid is sulfonamic acid and the molding agent is one or more of magnesium sulphate, oxalic acid, potassium chloride or sodium chloride. The technical scheme provided by the invention solves the problems that a concentrated acid is difficult to carry, the potential risk is high, and the quantitive weighing is difficult due to varied field environments during quick field detection of the atomic fluorescence; the solid acid tablet can be put into use so long as the solid acid tablet is resolved in water in proportion, the operation is simple, the use is safe, the performance is stable and the carrying is convenient; and therefore, the convenience and maneuverability in quick field detection of the portable atomic fluorescence is further improved, the analysis process is simplified, the analysis efficiency is improved and reference data can be quickly provided for emergency decision making of environmental pollution.
Description
Technical field
The present invention relates to the atomic fluorescence analysis technical field, especially relate to the required acidulant of steam generation sampling technique.
Background technology
The current atom XRF generally adopts the sample introduction means of steam generation sampling technique as atomic fluorescence.The essence of steam generation sampling technique is to make the acid solution and the reductant solution that contain element to be measured generate gaseous material through chemical reaction; After gas-liquid separation; Gaseous component is separated with sample matrices; Thereby reach efficient sample introduction and effectively eliminate the purpose that matrix disturbs, greatly improved the detectability of AFS.In Routine Test Lab was analyzed, all dilution obtained the employed acid of steam generation sampling technique through concentrated acid, and concentrated acid is generally hydrochloric acid and the nitric acid with extremely strong volatility, corrosivity and penetrating odor, perhaps has the sulfuric acid of extremely strong corrosivity and dehydration property.When stating acid in the use, need in vent cabinet, use transfer pipet quantitatively to pipette operation, need take strict safety prevention measure simultaneously.
What need particularly point out is, carries out the employed concentrated acid of atomic fluorescence analysis in the Routine Test Lab and is not suitable in the portable atomic fluorescence that needs the field condition fast detecting.Carry hydrochloric acid and nitric acid with strong volatility, corrosivity and penetrating odor and sulfuric acid and itself just have great difficulty and potential danger to analyzing the scene with extremely strong corrosivity and dehydration property; The scene also can't provide effective safeguard procedures such as vent cabinet simultaneously, adds complicated and changeable also quantitatively pipetting of concentrated acid operation of open-air analysis site environment and has caused certain difficulty.
In this field, also nobody proposes relevant patent, solution or special technology to the problems referred to above at present.
In view of this, for solving the deficiency in the above-mentioned technology, the design people is based on the research and development of association area, and constantly test and improvement of process, and then generation of the present invention is arranged.
Summary of the invention
In order to address the above problem, the objective of the invention is to carry out the requirement that the employed concentrated acid of atomic fluorescence analysis is not suitable for portable atomic fluorescence field condition fast detecting in the Routine Test Lab, there be very big potential safety hazard and non-operability; Designed a kind of solid acid compressing tablet; Use hydrochloric acid, nitric acid and the sulfuric acid of the alternative liquid of sulfaminic acid of solid, have portable, safe preferably; Use simply, can simplify analytic process greatly.
For achieving the above object, the invention provides a kind of solid acid compressing tablet of field quick detection atomic fluorescence chemical evapn generation sampling technique, it comprises following components in weight percentage: 1 ~ 10 part of solid acid, 1 ~ 5 part of forming agent; Wherein said solid acid is a sulfaminic acid, and said forming agent is one or more in magnesium sulphate, oxalic acid, potassium chloride or the sodium chloride.
Preferably, described solid acid compressing tablet comprises following components in weight percentage: 2 parts of sulfaminic acids, 1 part of forming agent.
Said forming agent is one or more in magnesium sulphate, oxalic acid, potassium chloride or the sodium chloride, and wherein preferred forming agent is an oxalic acid.
Said solid acid compressing tablet is preferably pie, column or bulk.More preferably, said compressing tablet is cylindrical, and diameter is 3 ~ 60mm, and height is 0.5 ~ 60mm.Wherein preferred diameter is 3 ~ 10mm, so that carry and pack into sample for analysis pipe and reagent bottle.
On the other hand, the present invention also provides the method for preparing above-mentioned solid acid compressing tablet, and it comprises the steps: to take by weighing in proportion solid acid and forming agent, with the two difference grind into powder, is pressed into said solid acid compressing tablet after mixing subsequently.The particle diameter of said powder is preferably less than 100 purpose powder.Wherein, taking by weighing the used device of solid acid and forming agent is ten thousand/electronic balance.XP204 type ten thousand/electronic balance like Mettler Toledo Inc.'s production.
Wherein, the used device of compacting compressing tablet is a sheeter, and the used pressure of sheeter is 1 ~ 10MPa, and preferred pressure is 5MPa.Said sheeter can be any sheeter that can buy on the market, like the 769YP-10D type powder compressing machine sheeter of device high and new technology company of Tianjin section production.
The invention provides the application in the fast detecting atomic fluorescence chemical evapn at the scene of said solid acid compressing tablet.
The solid acid compressing tablet is dissolved in the water of certain volume, can accomplishes the preparation process of acid solution after stirring.
Concentrated acid was difficult to carry when beneficial effect of the present invention had been to solve the atomic fluorescence field quick detection, potential danger is big and the changeable comparatively problem of difficulty that quantitatively pipettes of field environment; Only need dissolve in proportion and get final product with water; Simple to operate; Safe in utilization, stable in properties, be easy to carry, thereby further improved the convenience and the operability of portable atomic fluorescence field quick detection, further simplified analysis process; Improved analysis efficiency, can reference data be provided fast for the emergent decision-making of environmental pollution.
Embodiment
About the present invention is the application target that reaches above-mentioned and effect and the technological means that adopted, enumerate preferable feasible embodiment earlier, be described in detail.
Embodiment 1
With the mass ratio of preparation solid acid and forming agent is that 2/1 solid acid compressing tablet is an example, and details are as follows for its preparation process:
(1) is ready to solid acid sulfaminic acid and forming agent oxalic acid, pan paper, medicine spoon, agate mortar, ten thousand/electronic balance and sheeter;
(2) pan paper is placed on the weighing plate of electronic balance, deduct its weight, sulfaminic acid is transferred on the pan paper, quantitatively take by weighing 2.000g, use the agate mortar grind into fine powder then with the medicine spoon;
(3) brand-new pan paper is placed on the weighing plate of electronic balance, deduct its weight, oxalic acid is transferred on the pan paper, quantitatively take by weighing 1.000g, use the agate mortar grind into fine powder then with the medicine spoon;
(4) powder mixes that step (2) and step (3) is obtained is even, in the compacting tool set of the sheeter of packing into, to the powder pressurization, until 5MPa, keeps then 30 seconds gradually;
(5) release is taken out compressing tablet to the pressure of sheeter in mould, is kept in the reagent bottle of dry sealing.
When (6) analyzing this compressing tablet acidic reduction agent solution of scene use in the open air; Compressing tablet is dissolved in the 100mL pure water; The mass and size concentration (m/v) that promptly obtains solid acid after shaking up is 2%; Concentration of oxalic acid is that mass and size concentration (m/v) is 1% acid solution, can directly be used for the measurement of atomic fluorescence method.
Use the acid solution in the present embodiment, adopt flame method to measure detecting of arsenic and be limited to 0.01ng/mL, the repeatability of 7 measurements is 0.9%; Adopt the cold atom method to measure detecting of mercury and be limited to 0.001ng/mL, the repeatability of 7 measurements is 1%.
Embodiment 2
With the mass ratio of preparation solid acid and forming agent is that 5/2 solid acid compressing tablet is an example, and details are as follows for its preparation process:
(1) is ready to sulfaminic acid and forming agent oxalic acid, pan paper, medicine spoon, agate mortar, ten thousand/electronic balance and sheeter;
(2) pan paper is placed on the weighing plate of electronic balance, deduct its weight, sulfaminic acid is transferred on the pan paper, quantitatively take by weighing 5.000g, use the agate mortar grind into fine powder then with the medicine spoon;
(3) brand-new pan paper is placed on the weighing plate of electronic balance, deduct its weight, oxalic acid is transferred on the pan paper, quantitatively take by weighing 2.000g, use the agate mortar grind into fine powder then with the medicine spoon;
(4) powder mixes that step (2) and step (3) is obtained is even, in the compacting tool set of the sheeter of packing into, to the powder pressurization, until 10MPa, keeps then 30 seconds gradually;
(5) release is taken out compressing tablet to the pressure of sheeter in mould, is kept in the reagent bottle of dry sealing.
When (6) analyzing this compressing tablet acidic reduction agent solution of scene use in the open air; Compressing tablet is dissolved in the 100mL pure water; The mass and size concentration (m/v) that promptly obtains sulfaminic acid after shaking up is 5%; Concentration of oxalic acid is that mass and size concentration (m/v) is 2% acid solution, can directly be used for the measurement of atomic fluorescence method.
Use the acid solution in the present embodiment, adopt flame method to measure detecting of arsenic and be limited to 0.06ng/mL, the repeatability of 7 measurements is 1.5%; Adopt the cold atom method to measure detecting of mercury and be limited to 0.03ng/mL, the repeatability of 7 measurements is 1.9%.
Embodiment 3
With the mass ratio of preparation solid acid and forming agent is that 1/2 solid acid compressing tablet is an example, and details are as follows for its preparation process:
(1) is ready to sulfaminic acid and forming agent oxalic acid, pan paper, medicine spoon, agate mortar, ten thousand/electronic balance and sheeter;
(2) pan paper is placed on the weighing plate of electronic balance, deduct its weight, sulfaminic acid is transferred on the pan paper, quantitatively take by weighing 1.00g, use the agate mortar grind into fine powder then with the medicine spoon;
(3) brand-new pan paper is placed on the weighing plate of electronic balance, deduct its weight, oxalic acid is transferred on the pan paper, quantitatively take by weighing 2.000g, use the agate mortar grind into fine powder then with the medicine spoon;
(4) powder mixes that step (2) and step (3) is obtained is even, in the compacting tool set of the sheeter of packing into, to the powder pressurization, until 8MPa, keeps then 30 seconds gradually;
(5) release is taken out compressing tablet to the pressure of sheeter in mould, is kept in the reagent bottle of dry sealing.
When (6) analyzing this compressing tablet acidic reduction agent solution of scene use in the open air; Compressing tablet is dissolved in the 100mL pure water; The mass and size concentration (m/v) that promptly obtains sulfaminic acid after shaking up is 1%; Concentration of oxalic acid is that mass and size concentration (m/v) is 2% acid solution, can directly be used for the measurement of atomic fluorescence method.
Use the acid solution in the present embodiment, adopt flame method to measure detecting of arsenic and be limited to 0.13ng/mL, the repeatability of 7 measurements is 2.1%; Adopt the cold atom method to measure detecting of mercury and be limited to 0.08ng/mL, the repeatability of 7 measurements is 2.7%.
Embodiment 4
With the mass ratio of preparation solid acid and forming agent is that 10/2 solid acid compressing tablet is an example, and details are as follows for its preparation process:
(1) is ready to sulfaminic acid and forming agent potassium chloride and sodium chloride, pan paper, medicine spoon, agate mortar, ten thousand/electronic balance and sheeter;
(2) pan paper is placed on the weighing plate of electronic balance, deduct its weight, sulfaminic acid is transferred on the pan paper, quantitatively take by weighing 10.00g, use the agate mortar grind into fine powder then with the medicine spoon;
(3) brand-new pan paper is placed on the weighing plate of electronic balance, deduct its weight, potassium chloride and sodium chloride are transferred on the pan paper, quantitatively take by weighing potassium chloride 1.000g and sodium chloride 1.000g, use the agate mortar grind into fine powder then with the medicine spoon;
(4) powder mixes that step (2) and step (3) is obtained is even, in the compacting tool set of the sheeter of packing into, to the powder pressurization, until 4MPa, keeps then 30 seconds gradually;
(5) release is taken out compressing tablet to the pressure of sheeter in mould, is kept in the reagent bottle of dry sealing.
When (6) analyzing this compressing tablet acidic reduction agent solution of scene use in the open air; Compressing tablet is dissolved in the 100mL pure water; The mass and size concentration (m/v) that promptly obtains sulfaminic acid after shaking up is 10%; The mass and size concentration (m/v) of potassium chloride is 1%, and the mass and size concentration (m/v) of sodium chloride is 2% acid solution, can directly be used for the measurement of atomic fluorescence method.
Use the acid solution in the present embodiment, adopt flame method to measure detecting of arsenic and be limited to 0.23ng/mL, the repeatability of 7 measurements is 2.9%; Adopt the cold atom method to measure detecting of mercury and be limited to 0.15ng/mL, the repeatability of 7 measurements is 3.1%.
Embodiment 5
With the mass ratio of preparation solid acid and forming agent is that 1/1 solid acid compressing tablet is an example, and details are as follows for its preparation process:
(1) is ready to sulfaminic acid and forming agent magnesium sulphate, pan paper, medicine spoon, agate mortar, ten thousand/electronic balance and sheeter;
(2) pan paper is placed on the weighing plate of electronic balance, deduct its weight, sulfaminic acid is transferred on the pan paper, quantitatively take by weighing 1.00g, use the agate mortar grind into fine powder then with the medicine spoon;
(3) brand-new pan paper is placed on the weighing plate of electronic balance, deduct its weight, magnesium sulphate is transferred on the pan paper, quantitatively take by weighing 1.000g, use the agate mortar grind into fine powder then with the medicine spoon;
(4) powder mixes that step (2) and step (3) is obtained is even, in the compacting tool set of the sheeter of packing into, to the powder pressurization, until 9MPa, keeps then 30 seconds gradually;
(5) release is taken out compressing tablet to the pressure of sheeter in mould, is kept in the reagent bottle of dry sealing.
When (6) analyzing this compressing tablet acidic reduction agent solution of scene use in the open air; Compressing tablet is dissolved in the 100mL pure water; The mass and size concentration (m/v) that promptly obtains sulfaminic acid after shaking up is 1%; Magnesium sulfate concentration is that mass and size concentration (m/v) is 1% acid solution, can directly be used for the measurement of atomic fluorescence method.
Use the acid solution in the present embodiment, adopt flame method to measure detecting of arsenic and be limited to 0.32ng/mL, the repeatability of 7 measurements is 1.9%; Adopt the cold atom method to measure detecting of mercury and be limited to 0.14ng/mL, the repeatability of 7 measurements is 1.5%.
In the foregoing description 1 ~ 5, the mass ratio of solid acid and forming agent is 2/1 o'clock, and steam reacts can be complete; And the course of reaction pressure surge is less; The gaseous material vapour content that generates is lower, and signal is the most stable, and noise is minimum; Therefore cold atom method and flame method can obtain best analytical effect, and the mass ratio of preferred solid acid and forming agent is 2/1.
The above description of this invention is illustrative, and nonrestrictive, and those skilled in the art is understood, and within spirit that claim limits and scope, can carry out many modifications, variation or equivalence to it, but they will fall in protection scope of the present invention all.
Claims (10)
1. the solid acid compressing tablet of a portable atomic fluorescence field quick detection chemical evapn generation sampling technique is characterized in that it comprises following components in weight percentage: 1 ~ 10 part of solid acid, 1 ~ 2 part of forming agent; Wherein said solid acid is a sulfaminic acid, and said forming agent is one or more in magnesium sulphate, oxalic acid, potassium chloride or the sodium chloride.
2. solid acid compressing tablet as claimed in claim 1 is characterized in that, it comprises following components in weight percentage: 2 parts of solid acids, 1 part of forming agent.
3. solid acid compressing tablet as claimed in claim 1 is characterized in that, said forming agent is an oxalic acid.
4. like any described solid acid compressing tablet of claim 1 ~ 3, it is characterized in that said compressing tablet is pie, column or bulk.
5. solid acid compressing tablet as claimed in claim 4 is characterized in that, said compressing tablet is cylindrical, and diameter is 3 ~ 60mm, and height is 0.5 ~ 60mm.
6. solid acid compressing tablet as claimed in claim 5 is characterized in that, the diameter of said compressing tablet is 3 ~ 10mm.
7. the method for preparing any said solid acid compressing tablet of claim 1 ~ 6, it comprises the steps: to take by weighing in proportion solid acid and forming agent, with the two difference grind into powder, is pressed into said solid acid compressing tablet after mixing subsequently.
8. method as claimed in claim 7 is characterized in that, the used device of compacting compressing tablet is a sheeter, and the used pressure of sheeter is 1 ~ 10MPa.
9. method as claimed in claim 8 is characterized in that, the used pressure of said sheeter is 5MPa.
10. any said solid acid compressing tablet of claim 1 ~ 6 application in the portable atomic fluorescence chemical evapn of the fast detecting generation sampling technique at the scene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210238016.7A CN102721678B (en) | 2012-07-09 | 2012-07-09 | Solid acid tablet for quick field detection of portable atomic fluorescence and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210238016.7A CN102721678B (en) | 2012-07-09 | 2012-07-09 | Solid acid tablet for quick field detection of portable atomic fluorescence and preparation method and application thereof |
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| Publication Number | Publication Date |
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| CN102721678A true CN102721678A (en) | 2012-10-10 |
| CN102721678B CN102721678B (en) | 2014-09-10 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201210238016.7A Active CN102721678B (en) | 2012-07-09 | 2012-07-09 | Solid acid tablet for quick field detection of portable atomic fluorescence and preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104655598A (en) * | 2013-11-25 | 2015-05-27 | 北京瑞利分析仪器有限公司 | Hydride generation and sample introduction method of germanium |
| CN104655597A (en) * | 2013-11-25 | 2015-05-27 | 北京瑞利分析仪器有限公司 | Hydride generation and sample introduction method of seleninic acid radical ions |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH01248058A (en) * | 1988-03-29 | 1989-10-03 | Shibata Kagaku Kikai Kogyo Kk | Solid reagent for quantitative determination of phosphoric acid ion and arsenic acid ion |
| US20050118722A1 (en) * | 2002-08-21 | 2005-06-02 | Geen Alexander V. | Reagents for arsenic meter |
| CN202029413U (en) * | 2011-03-30 | 2011-11-09 | 南通赛孚机械设备有限公司 | Stearic acid tablet press |
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2012
- 2012-07-09 CN CN201210238016.7A patent/CN102721678B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01248058A (en) * | 1988-03-29 | 1989-10-03 | Shibata Kagaku Kikai Kogyo Kk | Solid reagent for quantitative determination of phosphoric acid ion and arsenic acid ion |
| US20050118722A1 (en) * | 2002-08-21 | 2005-06-02 | Geen Alexander V. | Reagents for arsenic meter |
| CN202029413U (en) * | 2011-03-30 | 2011-11-09 | 南通赛孚机械设备有限公司 | Stearic acid tablet press |
Non-Patent Citations (2)
| Title |
|---|
| B. RAJITHA等: "Sulfamic acid: a novel and efficient catalyst for the synthesis of aryl-14H-dibenzo[a.j]xanthenes under conventional heating and microwave irradiation", 《TETRAHEDRON LETTERS》 * |
| 吴艳霞等: "中间包涂料中镁质骨料所用的酸性和碱性结合剂", 《耐火与石灰》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104655598A (en) * | 2013-11-25 | 2015-05-27 | 北京瑞利分析仪器有限公司 | Hydride generation and sample introduction method of germanium |
| CN104655597A (en) * | 2013-11-25 | 2015-05-27 | 北京瑞利分析仪器有限公司 | Hydride generation and sample introduction method of seleninic acid radical ions |
| CN104655597B (en) * | 2013-11-25 | 2018-09-25 | 北京瑞利分析仪器有限公司 | A kind of hydride generation sample injection method of selenite radical ion |
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| CN102721678B (en) | 2014-09-10 |
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Effective date of registration: 20210906 Address after: 100094 160 Beiqing Road, Haidian District, Beijing Patentee after: BEIJING BEIFEN-RUILI ANALYTICAL INSTRUMENT (Group) Co.,Ltd. Address before: 100015 A5 / F, 9 Jiuxianqiao East Road, Chaoyang District, Beijing Patentee before: BEIJING RAYLEIGH ANALYTICAL INSTRUMENT Co.,Ltd. |
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