CN104150482B - A kind of device that prepared by required carbon dioxide during for carbonate carbon, oxygen isotope analysis - Google Patents
A kind of device that prepared by required carbon dioxide during for carbonate carbon, oxygen isotope analysis Download PDFInfo
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- CN104150482B CN104150482B CN201410429376.4A CN201410429376A CN104150482B CN 104150482 B CN104150482 B CN 104150482B CN 201410429376 A CN201410429376 A CN 201410429376A CN 104150482 B CN104150482 B CN 104150482B
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Abstract
The invention discloses a kind of device that prepared by required carbon dioxide during for carbonate carbon, oxygen isotope analysis, comprise for splendid attire carbonate samples powder and ortho-phosphoric reaction vessel, for vacuum extractor that described reaction vessel is vacuumized and the sealing device for the reaction vessel after described vacuumizing is sealed, described reaction vessel, for vertically tubular, is provided with on the top of this VERTICAL TUBE shaped reaction container the sealing and connecting device coordinating with described sealing device; Be provided with the accommodating storehouse of carbonate samples powder and the accommodating storehouse of orthophosphoric acid that mutually separate in the bottom of this VERTICAL TUBE shaped reaction container; When described VERTICAL TUBE shaped reaction container lean is during to predetermined angular, in the accommodating storehouse of orthophosphoric acid Implantation hydrochlorate sample powder in the accommodating storehouse of described orthophosphoric acid and with the carbonate samples powder in the accommodating storehouse of carbonate samples powder, mix.
Description
Technical field
The present invention relates to a kind of device of preparing carbon dioxide, relate in particular to a kind of for carbonate carbon,The device that when oxygen isotope analysis prepared by required carbon dioxide.
Background technology
In the time of carbonate carbon, oxygen isotope analysis, researcher adopts phosphoric acid method to carry out carbon dioxide conventionallyThe preparation of gas.
Existing phosphoric acid method is to adopt to carry out sample preparation with the glass reaction container of vacuum grease. This glassGlass reaction vessel is divided into two parts, props up tubular container and the grease with bistrique with " Y " font of groundSeal valve (as shown in Figure 1).
Its main preparation flow is as follows: first, pack carbonate samples powder into " Y " font and prop up tubular containerMain pipe bottom, and extract a certain amount of 100% orthophosphoric acid with syringe and add in the branched pipe of side; Secondly,Prop up Tu on the ground of tubular container in " Y " font and smear vacuum grease, and connect and compose one with grease seal valveIndividual closed container; Again, this closed container is received in vacuum system and vacuumized, by the sky of internal tankGas is discharged, valve-off after vacuum reaches pre-provisioning request, and reaction vessel is taken off; Finally, willSide branches pipe tilts to make the orthophosphoric acid slowly inject the main pipe that sample is housed, and then puts into 25 DEG CIn water-bath, reaction is spent the night (general 16 hours), and by the carbon dioxide process purifying, the collection that produceRear examination with computer.
There is following shortcoming in the above-mentioned device of preparing carbon dioxide:
The first, due to band vacuum grease, can only be used for the reaction preparation process under low temperature (as 25 DEG C),Reaction time is grown (approximately 16 hours), and preparation efficiency is low;
The second, add orthophosphoric acid in the arm of side time, acquire a certain degree of difficulty, if careless, haveOrthophosphoric acid drop is fallen in main pipe, causes sample loss;
The 3rd, after each sample preparation completes, all need the vacuum grease to installing each position to carry out wipingAnd cleaning, process is loaded down with trivial details, loses time.
Summary of the invention
The present invention is directed to the drawback of prior art, when one is provided for carbonate carbon, oxygen isotope analysisDevice prepared by required carbon dioxide.
The dress that prepared by required carbon dioxide during for carbonate carbon, oxygen isotope analysis of the present inventionPut, comprise for splendid attire carbonate samples powder and ortho-phosphoric reaction vessel, for described reaction is heldThe vacuum extractor that device vacuumizes and close for what the reaction vessel after described vacuumizing was sealedSeal apparatus,
Described reaction vessel, for vertically tubular, is provided with described on the top of this VERTICAL TUBE shaped reaction containerThe sealing and connecting device that sealing device coordinates;
Be provided with the upright dividing plate of predetermined altitude in the bottom of described VERTICAL TUBE shaped reaction container, described uprightThe bottom zone of described VERTICAL TUBE shaped reaction container is divided into the accommodating storehouse of carbonate samples powder and orthophosphoric acid by dividing plateAccommodating storehouse;
When described VERTICAL TUBE shaped reaction container lean is during to predetermined angular, in the accommodating storehouse of described orthophosphoric acid justIn the accommodating storehouse of phosphoric acid Implantation hydrochlorate sample powder and with the accommodating storehouse of carbonate samples powder in carbonateSample powder is mixed.
The dress that prepared by required carbon dioxide during for carbonate carbon, oxygen isotope analysis of the present inventionIn putting, described sealing device comprises bend pipe and is communicated with the arm that is arranged at this bend pipe middle part;
Wherein, one end of described bend pipe and described VERTICAL TUBE shaped reaction container are undertaken by sealing and connecting deviceConnect, the other end of this bend pipe is provided with without grease vacuum seal valve;
The openend of described arm is connected with described vacuum extractor.
The dress that prepared by required carbon dioxide during for carbonate carbon, oxygen isotope analysis of the present inventionIn putting, the openend of described arm is provided with the glass ground joint or the O type circle that coordinate with described vacuum extractorJoint.
The dress that prepared by required carbon dioxide during for carbonate carbon, oxygen isotope analysis of the present inventionIn putting, described sealing and connecting device comprises the nut that is sheathed on described bend pipe one end;
Top at described VERTICAL TUBE shaped reaction container is also provided with external screw thread;
Described nut coordinates and described VERTICAL TUBE shaped reaction container is connected in to described sealing with described external screw threadDevice.
The dress that prepared by required carbon dioxide during for carbonate carbon, oxygen isotope analysis of the present inventionIn putting, also comprise the sealing polytetrafluoroethylene gasket that is arranged at nut inside;
In the time that described nut screws in described external screw thread, described sealing polytetrafluoroethylene gasket be extruded distortion andMake top and the formation of described bend pipe one end of described VERTICAL TUBE shaped reaction container be tightly connected.
The dress that prepared by required carbon dioxide during for carbonate carbon, oxygen isotope analysis of the present inventionIn putting, realize the process of carbonate samples in the lower preparation of high temperature (as more than 70 DEG C), can make systemThe standby time foreshortened to 30 minutes by 16 hours, thereby had greatly improved preparation efficiency. Meanwhile, when reactionBetween shortening can also avoid reaction to produce the interior trace water of carbon dioxide and reaction vessel between oxygenExchange, thereby improve the accuracy of Determination of Oxygen Isotopes. Owing to adopting VERTICAL TUBE shaped reaction container, makeOrthophosphoric acid must be added more convenient. Owing to not using vacuum grease, the cleaning of whole container and assembling all tenIt is simple, convenient to divide; Meanwhile, owing to not needing to clean grease, saved a large amount of cleaning solvents (as stoneOil ether and liquid detergent etc.) and wiping paper using, certain economic benefit there is.
Brief description of the drawings
Fig. 1 is the structural representation of the device of preparing carbon dioxide of the prior art;
Fig. 2 is required carbon dioxide gas system during for carbonate carbon, oxygen isotope analysis of the present inventionThe structural representation of standby device.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is described in further detail, to make those skilled in the art's referenceDescription word can be implemented according to this.
As shown in Figure 2, required titanium dioxide during for carbonate carbon, oxygen isotope analysis of the present inventionThe device of carbon gas generation, comprise for splendid attire carbonate samples powder and ortho-phosphoric reaction vessel 1,For vacuum extractor 2 that described reaction vessel 1 is vacuumized and for to after described vacuumizingThe sealing device 3 that reaction vessel 1 seals.
Wherein, described reaction vessel 1, for vertically tubular, is established on the top of this VERTICAL TUBE shaped reaction container 1Be equipped with the sealing and connecting device 11 coordinating with described sealing device 3. At this VERTICAL TUBE shaped reaction container 1Bottom is provided with the accommodating storehouse 13 of the carbonate samples powder mutually separating and the accommodating storehouse 12 of orthophosphoric acid. Work as instituteWhen stating VERTICAL TUBE shaped reaction container 1 and tilting to predetermined angular, the orthophosphoric acid in the accommodating storehouse 12 of described orthophosphoric acidIn the accommodating storehouse 13 of Implantation hydrochlorate sample powder, and with carbonate samples powder accommodating 13 in carbonateSample powder is mixed. By means of conditions such as high temperature bath heating, can produce carbon dioxide. Here instituteThe concrete angle that the VERTICAL TUBE shaped reaction container 1 of saying tilts, during according to real reaction in the accommodating storehouse 12 of orthophosphoric acidOrthophosphoric acid can be injected into the accommodating storehouse 13 of carbonate samples powder and be as the criterion.
In the present invention, for the bottom zone at VERTICAL TUBE shaped reaction container 1 is every forming carbonate samples powderThe accommodating storehouse 12 of accommodating storehouse 13 and orthophosphoric acid, spy is provided with in the bottom of described VERTICAL TUBE shaped reaction container 1The upright dividing plate 14 of predetermined altitude, described upright dividing plate 14 is by the end of described VERTICAL TUBE shaped reaction container 1Portion separates as the accommodating storehouse 13 of carbonate samples powder and the accommodating storehouse 12 of orthophosphoric acid. Described upright dividing plate 14Highly according to concrete carbonate samples powder and ortho-phosphoric use amount and determine, when carbonate samples powder withWhen ortho-phosphoric use amount is large, relatively high upright dividing plate 14 should be set; If carbonate samples powder andOrtho-phosphoric use amount is little, and relatively low upright dividing plate 14 can be set.
In the present invention, described sealing device 3 comprises bend pipe 31 and is communicated with and is arranged at these bend pipe 31 middle partsArm 32. Wherein, one end of described bend pipe 31 and described VERTICAL TUBE shaped reaction container 1 connect by sealingConnection device 11 connects, and the other end of this bend pipe 31 is provided with without grease vacuum seal valve 33; InstituteThe openend of stating arm 32 is connected with described vacuum extractor 2. Particularly, at described arm 32Openend the glass ground joint or the O type circle joint that coordinate with described vacuum extractor 2 can be set, to realizeBe tightly connected.
In the present invention, described sealing and connecting device 11 specifically comprises the spiral shell that is sheathed on described bend pipe 31 one endCap 111; Top at described VERTICAL TUBE shaped reaction container 1 is also provided with external screw thread 112; Described nut 111Coordinate and described VERTICAL TUBE shaped reaction container 1 is connected in to described sealing device 3 with described external screw thread 112.Further, sealing polytetrafluoroethylene (PTFE) (PTFE) packing ring 113 also can be set in described nut 111 inside;In the time that described nut 111 screws in described external screw thread 112, described sealing polytetrafluoroethylene gasket 113 is squeezedCompressive strain and make the top of described VERTICAL TUBE shaped reaction container 1 and described bend pipe 31 one end form sealing connectingConnect.
Applying device of the present invention, to prepare the detailed process of carbon dioxide as follows:
First, pack carbonate samples powder into carbonate samples powder accommodating storehouse 13, and take out with syringeGet a certain amount of 100% orthophosphoric acid and add the accommodating storehouse 12 of orthophosphoric acid;
Then, VERTICAL TUBE shaped reaction container 1 and sealing device 3 are connected and composed to a closed container;
Again, this closed container is received on vacuum extractor 2 and vacuumized, with by this closed container insideBas Discharged is closed without grease vacuum seal valve 33 after vacuum reaches requirement, and by whole airtightPreparing container is set up and takes off from vacuum means;
Finally, VERTICAL TUBE shaped reaction container 1 is tilted, make the orthophosphoric acid in the accommodating storehouse 12 of described orthophosphoric acidIn the accommodating storehouse 13 of Implantation hydrochlorate sample powder, then put into 90 DEG C of water-baths and react 30 minutes, institute producesRaw carbon dioxide is examination with computer after purifying, collection again.
Apply the device of preparing carbon dioxide of the present invention and there is following beneficial effect:
(1) realized the process of carbonate samples in the lower preparation of high temperature (as more than 70 DEG C), can makePreparation time foreshortened to 30 minutes by 16 hours, thereby had greatly improved preparation efficiency. Meanwhile, reactionBetween the interior trace water of carbon dioxide and reaction vessel that the shortening of time can also avoid reaction to produceThe exchange of oxygen, thereby the accuracy of raising Determination of Oxygen Isotopes;
(2) owing to adopting VERTICAL TUBE shaped reaction container, make to add orthophosphoric acid more convenient;
(3), owing to not using vacuum grease, the cleaning of whole container and assembling are all very simple, convenient;Meanwhile, owing to not needing to clean grease, saved a large amount of cleaning solvent (as benzinum and liquid detergent etc.)With wiping paper using, there is certain economic benefit.
Although embodiment of the present invention are open as above, it is not restricted to description and enforcement sideListed utilization in formula, it can be applied to various applicable the field of the invention completely, for being familiar with abilityThe personnel in territory, can easily realize other amendment, therefore do not deviate from claim and etc. homotypeEnclose under limited universal, the present invention is not limited to specific details and illustrates here and the figure describingExample.
Claims (5)
1. the device that during for carbonate carbon, oxygen isotope analysis prepared by required carbon dioxide,Comprise for splendid attire carbonate samples powder and ortho-phosphoric reaction vessel, for described reaction vessel is taken outThe vacuum extractor of vacuum and the sealing dress for the reaction vessel after described vacuumizing is sealedPut, it is characterized in that,
Described reaction vessel, for vertically tubular, is provided with described on the top of this VERTICAL TUBE shaped reaction containerThe sealing and connecting device that sealing device coordinates;
Be provided with the upright dividing plate of predetermined altitude in the bottom of described VERTICAL TUBE shaped reaction container, described uprightThe bottom zone of described VERTICAL TUBE shaped reaction container is divided into the accommodating storehouse of carbonate samples powder and orthophosphoric acid by dividing plateAccommodating storehouse;
When described VERTICAL TUBE shaped reaction container lean is during to predetermined angular, in the accommodating storehouse of described orthophosphoric acid justIn the accommodating storehouse of phosphoric acid Implantation hydrochlorate sample powder and with the accommodating storehouse of carbonate samples powder in carbonateSample powder is mixed.
2. required carbon dioxide gas during for carbonate carbon, oxygen isotope analysis as claimed in claim 1The device that system is standby, is characterized in that, described sealing device comprises that bend pipe and connection are arranged in this bend pipeThe arm of portion;
Wherein, one end of described bend pipe and described VERTICAL TUBE shaped reaction container are undertaken by sealing and connecting deviceConnect, the other end of this bend pipe is provided with without grease vacuum seal valve;
The openend of described arm is connected with described vacuum extractor.
3. required carbon dioxide gas during for carbonate carbon, oxygen isotope analysis as claimed in claim 2The device that system is standby, is characterized in that, the openend of described arm is provided with described vacuum extractor joinsThe glass ground joint closing or O type circle joint.
4. required carbon dioxide gas during for carbonate carbon, oxygen isotope analysis as claimed in claim 2The device that system is standby, is characterized in that, described sealing and connecting device comprises and is sheathed on described bend pipe one endNut;
Top at described VERTICAL TUBE shaped reaction container is also provided with external screw thread;
Described nut coordinates and described VERTICAL TUBE shaped reaction container is connected in to described sealing with described external screw threadDevice.
5. required carbon dioxide gas during for carbonate carbon, oxygen isotope analysis as claimed in claim 4The device that system is standby, is characterized in that, also comprises the sealing polytetrafluoroethylene gasket that is arranged at nut inside;
In the time that described nut screws in described external screw thread, described sealing polytetrafluoroethylene gasket be extruded distortion andMake top and the formation of described bend pipe one end of described VERTICAL TUBE shaped reaction container be tightly connected.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410429376.4A CN104150482B (en) | 2014-08-28 | 2014-08-28 | A kind of device that prepared by required carbon dioxide during for carbonate carbon, oxygen isotope analysis |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410429376.4A CN104150482B (en) | 2014-08-28 | 2014-08-28 | A kind of device that prepared by required carbon dioxide during for carbonate carbon, oxygen isotope analysis |
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| CN104150482A CN104150482A (en) | 2014-11-19 |
| CN104150482B true CN104150482B (en) | 2016-05-18 |
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| CN112229691B (en) * | 2020-10-21 | 2022-03-04 | 中国科学院广州地球化学研究所 | Device and method for acidolysis by using I-shaped glass tube |
| CN112305058A (en) * | 2020-10-30 | 2021-02-02 | 上海化工研究院有限公司 | Method for determining deuterium isotope abundance in water sample |
| CN112986453B (en) * | 2021-05-11 | 2021-07-20 | 中国科学院地质与地球物理研究所 | Method and system for high-resolution determination of organic carbon isotopes in stalagmite |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6491890B1 (en) * | 1999-04-30 | 2002-12-10 | Soechting Klaus | Method and set for continuous long-term dosing of CO2 |
| CN101474583A (en) * | 2008-12-05 | 2009-07-08 | 华南理工大学 | Plastic reaction bottle |
| CN201470295U (en) * | 2009-07-13 | 2010-05-19 | 核工业北京地质研究院 | Collecting device of carbon dioxide generated by carbonate and phosphoric acid |
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2014
- 2014-08-28 CN CN201410429376.4A patent/CN104150482B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6491890B1 (en) * | 1999-04-30 | 2002-12-10 | Soechting Klaus | Method and set for continuous long-term dosing of CO2 |
| CN101474583A (en) * | 2008-12-05 | 2009-07-08 | 华南理工大学 | Plastic reaction bottle |
| CN201470295U (en) * | 2009-07-13 | 2010-05-19 | 核工业北京地质研究院 | Collecting device of carbon dioxide generated by carbonate and phosphoric acid |
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