CN202305291U - Device for analyzing and pretreating carbon isotope in organic matter sample - Google Patents

Device for analyzing and pretreating carbon isotope in organic matter sample Download PDF

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Publication number
CN202305291U
CN202305291U CN 201120433205 CN201120433205U CN202305291U CN 202305291 U CN202305291 U CN 202305291U CN 201120433205 CN201120433205 CN 201120433205 CN 201120433205 U CN201120433205 U CN 201120433205U CN 202305291 U CN202305291 U CN 202305291U
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valve
silver
cupric oxide
carbon isotope
trap
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李军杰
刘汉彬
金贵善
钟芳文
韩娟
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Beijing Research Institute of Uranium Geology
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Beijing Research Institute of Uranium Geology
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Abstract

The utility model relates to a device for analyzing and pretreating carbon isotope in an organic matter sample. The device for analyzing and pretreating the carbon isotope in the organic matter sample comprises an oxygen feeding system, a reaction system, a heating system and a collecting system, wherein the reaction system comprises two reaction tubes which are arranged in parallel; each reaction tube comprises an outer quartz tube connected with the oxygen feeding system in a sealing manner, and an inner quartz tube sleeved inside the outer quartz tube; the heating system comprises high-temperature furnaces which are arranged outside the two outer quartz tubes respectively; and a porcelain combustion boat, a copper oxide and silver metavanadate mixture filled into the inner quartz tube, a silver wire and a copper wire are sequentially arranged in each of the two inner quartz tubes. Through design of the two reaction tubes, time waste caused by changing the sample is avoided and the sampling efficiency is improved; through design of the inner quartz tube and the outer quartz tube, the systems are kept clean and chemical substances in the inner quartz tube can be periodically changed conveniently; and through design of an oxidizing part, a purifying part and a reducing part in the inner quartz tube, the complete combustion of the organic matter is ensured and pure carbon dioxide can be obtained.

Description

Carbon isotope analysis pretreatment unit in a kind of organic sample
Technical field
The utility model relates to carbon isotope analysis pretreatment unit in a kind of organic sample, particularly relates to a kind ofly can improving analysis efficiency, can also guarantee carbon isotope analysis pretreatment unit in the organic sample of precision of analysis.
Background technology
The ORGANIC CARBON ISOTOPES analysis is having very important use aspect the origin cause of formation of organic-fuels such as research oil, coal, and along with the continuous development and the improvement of stable carbon isotope analytical technology, its application aspect ground and environment is also increasingly extensive.Existing many scholars utilize source organic in organic carbon isotope research ocean, the lake, carry out environment tracer and rebuild paleoclimate and paleovegetation etc. through the soil organic carbon isotope, and the carbon isotope analysis method has great important in the visible research organic matter.
Constantly perfect along with high precision mass spectrometric analysis for isotope instrument, the factor of instrument own is more and more littler to sample determination result's influence, therefore The pretreatment has been determined its analytical accuracy to a great extent.The organic carbon isotope sample preparation methods mainly contains sealed-tube method, static calcination oxidizing process and continuous stream analytic approach etc.Sealed-tube method needs earlier sample to be mixed with cupric oxide to be put in sealing by fusing in the peace bottle, is put in then in the vacuum system, will pacify bottle under the hot conditions and smash; Collect its carbon dioxide; The carbon dioxide of this method preparation is very pure, but sealing by fusing process trouble, and efficient is not high; Static calcination method is sample and cupric oxide to be mixed be put in the quartz boat, then quartz boat is put into vacuum system, and carbon dioxide is collected in its heating then, this method employing at present commonplace; The method of continuous stream is that sample is put in the system, to the logical high-purity continuous Oxygen Flow of system, then sample is heated; Make itself and oxygen combustion, collect carbon dioxide, this method need not carried out the vacuum preparation; Thereby save the sample preparation time, thus continuous flow of oxygen can avoid atmosphere to sneak into system causing interference, and in continuous flow of oxygen; Can guarantee the abundant burning of sample, avoid fractionation.
But mainly there is following shortcoming in the method for the present continuous Oxygen Flow burning of adopting: at first be exactly that specimen preparation is slow; Sample of every reaction will be opened system and change next sample; Again aerating oxygen is driven the atmosphere of putting in the system away then; Could add hot preparation to next sample, so just waste the unnecessary time; Secondly, reacting pipe is owing to carry out the preparation of sample for a long time, and Oxygen Flow can more or less be taken away organic sample, will stick to inner-walls of duct like this, causes the pollution of pipeline; Once more, to removing the foreign gas that organic sample produces, also do not have detailed research at present, foreign gas can cause very big error; At last, the control problem of oxygen flow is because in the process of sample combustion; Will be used in cold-trap to sample and go out to put liquid nitrogen and collect, so after cold-trap adds liquid nitrogen, because system turns cold suddenly; Can form a negative pressure; Oxygen bottleneck oxygen flow is not just represented the flow of gas outlet like this, even possibly cause the air suck-back to be gone in the system, and analysis result is impacted.Therefore need badly carbon isotope analysis pretreatment unit in a kind of novel organic sample is provided.
Summary of the invention
The technical matters that the utility model will solve provides and a kind ofly can improve analysis efficiency, can also guarantee carbon isotope analysis pretreatment unit in the organic sample of analysis result accuracy.
For solving the problems of the technologies described above; Carbon isotope analysis pretreatment unit in a kind of organic sample of the utility model; The reactive system that comprises the oxygen gas handling system, is tightly connected with the oxygen gas handling system, the heating system that heats for reactive system and the collection system that is tightly connected with reactive system; Reactive system is two reaction tubes that laterally arrange, and each reaction tube comprises the quartz outer tube that is tightly connected with the oxygen gas handling system and is placed in the quartz inner pipe within the quartz outer tube; Heating system is for being arranged at two high temperature furnaces outside the quartz outer tube respectively.
Collection system comprises first cold-trap, second cold-trap, collection tube and mechanical pump; Between two quartz outer tubes and first cold-trap respectively sealing be provided with first valve and second valve; The other end of first valve and second valve is sealedly connected with the 3rd valve and the 4th valve; The other end of the 3rd valve first cold-trap that is tightly connected; First cold-trap, second cold-trap that is tightly connected, second cold-trap is sealedly connected with the 5th valve and the 6th valve respectively, and the other end of the other end of the 5th valve and the 4th valve is communicated with and is communicated with the gas outlet; The other end of the 6th valve is sealedly connected with the 7th valve, and the other end of the 7th valve is sealedly connected with the 8th valve and collection tube, and the other end of the 8th valve is sealedly connected with mechanical pump; Sealing is provided with vacuum degree measuring equipment between the 6th valve and the 7th valve; Seal respectively between the 4th valve, the 5th valve and the gas outlet and be provided with the sodium hydroxide trap and first gas meter.
The reduction valve that the oxygen gas handling system comprises welding bottle, is tightly connected with welding bottle, and second gas meter that is tightly connected with reduction valve; Second gas meter is sealedly connected with the 9th valve and the tenth valve respectively; The 9th valve seal is connected with the first rubber vacuum tube, and the tenth valve seal is connected with the second rubber vacuum tube, and the other end of the first rubber vacuum tube and the second rubber vacuum tube is tightly connected with two quartz outer tubes respectively.
Be connected through detachable flange seal between the first rubber vacuum tube and the second rubber vacuum tube and two quartz outer tubes.
First valve to the, ten valves are vacuum is not had the grease valve.
Vacuum degree measuring equipment adopts the ZJ-53B type vacuum gauge of Department of Electronics of Peking University, is equipped with DL-0 type vacuum meter, range 0~300Pa.
Be disposed with porcelain boat respectively in two quartz inner pipes and be filled in cupric oxide and the silver-colored potpourri of alum acid, filamentary silver, the copper wire in the quartz inner pipe.
Cupric oxide and the silver-colored potpourri of alum acid are evenly mixed with the alum acid silver that is adsorbed in zeolite surface by cupric oxide and form, and the mass ratio of cupric oxide and alum acid silver is 3: 1~5: 1, and the axial length of cupric oxide and the silver-colored potpourri of alum acid is 15~20cm.
The mass ratio of filamentary silver and copper wire is 1: 10~1: 15; Filamentary silver divides two parts to be arranged at the copper wire both sides; That part of filamentary silver of contiguous cupric oxide and the silver-colored potpourri of alum acid and the mass ratio of another part filamentary silver are 1: 1~1: 2, and the axial distance of that part of filamentary silver of contiguous cupric oxide and the silver-colored potpourri of alum acid and cupric oxide and the silver-colored potpourri of alum acid is 5~8cm.
Be provided with silica wool between porcelain boat and cupric oxide and the silver-colored potpourri of alum acid, be provided with silica wool between that part of filamentary silver of cupric oxide and the alum silver-colored potpourri of acid and contiguous cupric oxide and the silver-colored potpourri of alum acid.
The utility model has been avoided having improved sample preparation efficient because of changing the time waste that sample causes through the design of two reaction tubes.
Each reaction tube is all taked the design of internal and external casing in the utility model, makes total system to keep clean, and makes the chemical substance in the reaction tube be convenient to periodic replacement.
The utility model utilizes the design of oxidized portion unique in the reaction tube, purification part and reduction part, can guarantee organic burning fully, and obtain pure carbon dioxide.
The utility model is through the use of two flowmeters, makes system's Control Flow more easily, avoids because the atmosphere suck-back phenomenon that liquid nitrogen formation negative pressure causes.
The utility model has been avoided the interference of atmospheric carbon dioxide to made carbon dioxide in system's gas outlet design sodium hydroxide trap.
Whole system adopts no grease vacuum valve in the utility model, has avoided grease valve high temperature to produce the interference of carbon dioxide to sample down.
Description of drawings
Fig. 1 is the overall schematic of carbon isotope analysis pretreatment unit in a kind of organic sample that the utility model provided.
Fig. 2 is the synoptic diagram of the reaction tube of carbon isotope analysis pretreatment unit in a kind of organic sample that the utility model provided.
Among the figure: 1 is welding bottle, and 2 is reduction valve, and 3 is second gas meter, and 4 is the first rubber vacuum tube, and 5 is reaction tube, and 6 is first cold-trap; 7 is second cold-trap, and 8 is vacuum degree measuring equipment, and 9 is collection tube, and 10 is mechanical pump, and 11 is sodium hydroxide trap; 12 is the tenth valve, and 13 is the 9th valve, and 14 is first valve, and 15 is second valve, and 16 is the 3rd valve; 17 is the 4th valve, and 18 is the 5th valve, and 19 is the 6th valve, and 20 is the 8th valve, and 21 is the 7th valve; 22 is the second rubber vacuum tube, and 23 is first gas meter, and 24 is detachable flange, and 25 is porcelain boat, and 26 is high temperature furnace; 27 is silica wool, and 29 is filamentary silver, and 30 is copper wire, and 31 is quartz outer tube, and 32 is quartz inner pipe.
Embodiment
Below in conjunction with accompanying drawing and embodiment the utility model is done further detailed explanation.
Carbon isotope analysis pretreatment unit in a kind of organic sample of the utility model, the reactive system that comprises the oxygen gas handling system, is tightly connected with the oxygen gas handling system, the heating system that heats for reactive system and the collection system that is tightly connected with reactive system.
The reduction valve 2 that the oxygen gas handling system comprises welding bottle 1, is tightly connected with welding bottle 1, and second gas meter 3 that is tightly connected with reduction valve.Reduction valve 2 ranges 0~0.6MPa, second gas meter, 3 range 300ml/min.Welding bottle 1 adopts high purity oxygen gas, and is equipped with reduction valve 2 and carries out the gas outlet decompression, comes Control Flow through regulating second gas meter 3 then.Second gas meter 3 is sealedly connected with the 9th valve 13 and the tenth valve 12 respectively; The 9th valve 13 is sealedly connected with the first rubber vacuum tube, 4, the ten valves 12 and is sealedly connected with the second rubber vacuum tube 12.
Reactive system is two reaction tubes 5 that laterally arrange, and each reaction tube 5 comprises the quartz outer tube 31 that is tightly connected with the oxygen gas handling system and is placed in the quartz inner pipe 32 within the quartz outer tube 31.Quartz outer tube 31 is a long 95cm, external diameter 2.42cm, and the quartz ampoule of internal diameter 2.10cm, quartz inner pipe 32 are a 85cm, external diameter 1.90cm, the quartz ampoule of internal diameter 1.65cm.The other end of the first rubber vacuum tube 4 and the second rubber vacuum tube 22 is tightly connected through detachable flange 24 with two quartz outer tubes 4 respectively, preferably adopts the KF25 flange.
Heating system is for being arranged at two high temperature furnaces 26 outside the quartz outer tube 31 respectively.High temperature furnace 26 adopts tubular heater, adopts suspension type, can move in the horizontal direction.Temperature of reaction according to the various piece of reaction tube 5 adopts different high temperature furnaces 26, is controlled by different pressure regulators respectively.
The burning of sample and purifying etc. then mainly carry out in quartz inner pipe 32, are disposed with porcelain boat 25 respectively in two quartz inner pipes 32 and are filled in the silver-colored potpourri of cupric oxide and alum acid in the quartz inner pipe 32 28, filamentary silver 29, copper wire 30.
Alum acid silver is that the dissolving vanadium pentoxide precipitates and prepares in alkaline solution, and precipitate with deionized water is repeatedly cleaned, and is neutral with its solution of PH detection paper.The alum acid silver that is rich in moisture mixes with zeolite, and the zeolite granular size is 20~40 orders, and alum acid silver is adsorbed on zeolite surface, dries then.The mass ratio of cupric oxide and alum acid silver is 3: 1~5: 1, and the axial length of cupric oxide and the silver-colored potpourri 28 of alum acid is 15~20cm.
Filamentary silver 29 is for analyzing the fine silver silk, and filamentary silver 29 diameter 0.5mm~1mm, copper wire 30 are other copper wire of spectroscopic pure level.Filamentary silver 29 is 1: 10~1: 15 with the mass ratio of copper wire 30; 29 fens two parts of filamentary silver are arranged at copper wire 30 both sides; That part of filamentary silver 29 of contiguous cupric oxide and the silver-colored potpourri 28 of alum acid is 1: 1~1: 2 with the mass ratio of another part filamentary silver 29, and that part of filamentary silver 29 of contiguous cupric oxide and the silver-colored potpourri 28 of alum acid is 5~8cm with the radial distance of cupric oxide and the silver-colored potpourri 28 of alum acid.
Be provided with silica wool 27 between porcelain boat 25 and cupric oxide and the silver-colored potpourri 28 of alum acid, be provided with silica wool 27 between that part of filamentary silver 29 of cupric oxide and the alum silver-colored potpourri 28 of acid and contiguous cupric oxide and the silver-colored potpourri 28 of alum acid.
The silver-colored potpourri of porcelain boat 25 in the above-mentioned quartz inner pipe 32, cupric oxide and alum acid 28, filamentary silver 29, copper wire 30 are by being divided into combustion parts, oxidized portion, purification part and reduction part by function.
Combustion parts is made up of porcelain boat 25 and tubular heater, and the sample of handling well is positioned in the porcelain boat 25, is heated to corresponding temperature with corresponding tubular heater, under Oxygen Flow, burns.
Oxidized portion is made up of cupric oxide, when sample carries out combustion reaction, oxidized portion is heated to corresponding temperature, makes owing to the carbon monoxide that is not produced by perfect combustion is converted into carbon dioxide.Because oxygen is arranged often to its activation, cupric oxide can use repeatedly.
Purification part mainly is made up of alum acid silver and filamentary silver 29; Alum acid silver not only can remove foreign gases such as sulfide that dereaction produces and halogen; Can also improve the oxidation susceptibility of cupric oxide as catalyzer, filamentary silver then can further be removed foreign gas, guarantees the pure of carbon dioxide.
The reduction part mainly is made up of copper wire 30.Copper wire 30 is wanted regular replacing or is adopted hydrogen under hot conditions, to reduce.Owing to organic burning can produce a large amount of oxynitrides, especially nitrous oxide, because of itself and carbon dioxide have identical mass number, thus the serious interference analysis result of meeting, so restoring system mainly designs in order to remove oxynitrides.
Silica wool 27 can prevent that various materials mix more than under the situation of Oxygen Flow.
Collection system comprises first cold-trap 6, second cold-trap 7, collection tube 9 and mechanical pump 10.Between two quartz outer tubes 31 and first cold-trap 6 respectively sealing be provided with first valve 14 and second valve 15; The other end of first valve 14 and second valve 15 is sealedly connected with the 3rd valve 16 and the 4th valve 17; The other end of the 3rd valve 16 first cold-trap 6 that is tightly connected; Close 6 envelopes of first cold-trap connect the other end that second cold-trap, 7, the second cold-traps 7 are sealedly connected with the other end and the 4th valve 17 of the 5th valve 18 and the 6th valve 19, the five valves 18 respectively and are communicated with and are communicated with the gas outlet; The other end that the other end that the other end of the 6th valve 19 is sealedly connected with the 7th valve 21, the seven valves 21 is sealedly connected with the 8th valve 20 and collection tube 9, the eight valves 20 is sealedly connected with mechanical pump 10; Sealing is provided with vacuum degree measuring equipment 8 between the 6th valve 19 and the 7th valve 21; Between the 4th valve 17, the 5th valve 18 and the gas outlet respectively sealing be provided with the sodium hydroxide trap 11 and first gas meter 23.First valve, 14 to the tenth valves, the 12 preferred vacuum that adopt do not have the grease valve.The vacuum degree measuring equipment 8 preferred ZJ-53B type vacuum gauges that adopt Department of Electronics of Peking University are equipped with DL-0 type vacuum meter, range 0~300Pa.Put into analytically pure NaOH in the sodium hydroxide trap 11, and before making sample, heat the processing of degassing at every turn.Flowmeter respectively disposes one in welding bottle 1 gas outlet and total system gas outlet, with the instantaneous negative pressure that prevents to form because of at collection system interpolation liquid nitrogen, and the atmosphere suck-back phenomenon that causes.
The course of work of the utility model is following:
(1) sample preparation is got a certain amount of pedotheque, and granularity 200 orders are placed in the clean beaker, adds the hydrochloric acid of 1mol/L, and ultrasonic cleaning 0.5h with deionized water wash 6~8 times, removes carbonate impurity.120 ℃ of oven dry are for use in the placement baking oven.To the processing of porcelain boat, adopt 1: 1 nitric acid heated and boiled of volume ratio, use deionized water wash then 6~8 times, and 120 ℃ of oven dry are for use in the placement baking oven.
(2) reacting pipe degass: close the tenth valve 12, the 9th valve 13, the 4th valve 17 and the 5th valve 18; Open first valve 14, second valve 15, the 3rd valve 16, the 6th valve 19, the 8th valve 20 and the 7th valve 21; Open mechanical pump 10; And the high temperature furnace 26 through pressure regulator control reaction tube 5, make it be warming up to 200 ℃, to the reacting pipe processing of degassing.
(3) oxygen pipe blow-through: after the end of degassing; Get two parts of a certain amount of samples of having handled well; Be positioned in two porcelain boats 25; Open two quartz inner pipes 32 through detachable flange 24, porcelain boat 25 be positioned over respectively among two quartz inner pipes 32, then through detachable flange 24 with quartz inner pipe 32 and oxygen gas handling system sealed butt joint.Open welding bottle 1 and reduction valve 2; Open the tenth valve 12, the 9th valve 13, first valve 14, second valve 15, the 3rd valve 16, the 5th valve 18, close the 4th valve 17, the 6th valve 19, through regulating second gas meter 3; Controlling it, to go out airshed be 100ml/min; Reacting pipe is carried out the oxygen flushing, and the time is about 5min, and flushing is closed the tenth valve 12 and second valve 15 after finishing.
(4) example reaction: through regulating the reduction valve 2 and second gas meter 3; Making its flow is 300ml/min, and the phenomenon that causes system's gas outlet suck-back to prevent after putting liquid nitrogen on the cold-trap, to have formed a relative negative pressure puts dry ice-alcohol blend on first cold-trap 6; On second cold-trap 7, put liquid nitrogen; Through regulating second gas meter 3, make the registration of second gas meter 3 be about 60ml/min, transfer high temperature furnace 26 temperature to 800 ℃ with pressure regulator then; And it is heated to 600 ℃ to the silver-colored potpourri 28 of cupric oxide and alum acid; Copper wire 30 and filamentary silver 29 are heated to 400 ℃, high temperature furnace 26 are moved to porcelain boat 25 positions carry out combustion reaction, the reaction time is about 5min.
(5) collect gaseous sample: after reaction finishes, close the 9th valve 13, first valve 14, the 3rd valve 16 and the 5th valve 18, open second valve 15, first valve 14 and the 4th valve 17 simultaneously, another quartz inner pipe 32 is carried out the oxygen flushing.Open the 6th valve 19, the 8th valve 20 and the 7th valve 21, extract unnecessary oxygen, when treating that vacuum degree measuring equipment 8 readings are about 6Pa; Represent the end of bleeding, valve-off 20 puts liquid nitrogen on the collection tube 9; Remove the liquid nitrogen on second cold-trap 7; Change alcohol-dry ice rapidly, shift in carbon dioxide to the collection tube 9 in second cold-trap 7, confirm through vacuum degree measuring equipment 8 whether transfer finishes.
(6) reaction of next sample: after transfer finishes; Close the 8th valve 20 and the 7th valve 21, and the valve of collection tube 9, collection tube 9 taken off; And change next collection tube 9; Remove the alcohol-dry ice of first cold-trap 6 and second cold-trap 7, open the 8th valve 20 and the 7th valve 21, extract the foreign gases such as moisture in collection tube 9 and the residual system.Close the 4th valve 17 and the 6th valve 19 then, open the 3rd valve 16 and the 5th valve 18, repeating step (4) process.
(7) collect gaseous sample and change another quartz pipe sample: after reaction finishes, close the tenth valve 12, second valve 15, the 3rd valve 16 and the 5th valve 18; Through opening the detachable flange that is connected with rubber vacuum tube 4, change the sample in the quartz inner pipe 32 simultaneously; Open the 9th valve 13, first valve 14 and the 4th valve 17 then, another quartz inner pipe 32 is carried out the oxygen flushing; Open the 6th valve 19, the 8th valve 20 and the 7th valve 21, extract unnecessary oxygen, when treating vacuum degree measuring equipment 8 readings for 6Pa, the representative end of bleeding; Close the 8th valve 20, put liquid nitrogen on the collection tube 9, remove the liquid nitrogen on second cold-trap 7, change alcohol-dry ice rapidly, shift in carbon dioxide to the collection tube 9 in second cold-trap 7, confirm through vacuum degree measuring equipment 8 whether transfer finishes.
(8) repeating step (4), (5), (6), (7) get final product.
Reacting pipe need be handled quartz inner pipe 32 with after a period of time, causes mainly due to following reason:
(1) copper wire 30 is finally lost reducing power by the continuous oxidation of oxygen;
(2) organic sample is brought into pipeline by Oxygen Flow, sticks on quartz inner pipe 32 inwalls to pollute;
(3) silica wool is stopped up by organic sample, causes that Oxygen Flow is not smooth;
(4) alum acid silver is long-term uses, and catalytic performance descends.
For situation (1), then to copper wire 30 heat, and pass to continuous hydrogen, reduce.
For situation (2) (3) (4), then open detachable flange 24, take out quartz inner pipe 32; Take out each reactive material in the quartz inner pipe 32, quartz inner pipe 32 is cleaned with acetone earlier, and with deionized water rinsing 6~8 times; 120 ℃ of oven dry, and dress is put in the system with new chemical substance.

Claims (10)

1. carbon isotope analysis pretreatment unit in the organic sample; The reactive system that comprises the oxygen gas handling system, is tightly connected with the oxygen gas handling system, the heating system that heats for reactive system and the collection system that is tightly connected with reactive system; It is characterized in that: said reactive system is two reaction tubes that laterally arrange; Each reaction tube comprises the quartz outer tube that is tightly connected with said oxygen gas handling system and is placed in the quartz inner pipe within the said quartz outer tube; Said heating system is for being arranged at two high temperature furnaces outside the quartz outer tube respectively.
2. carbon isotope analysis pretreatment unit in a kind of organic sample according to claim 1 is characterized in that: said collection system comprises first cold-trap, second cold-trap, collection tube and mechanical pump; Seal respectively between said two quartz outer tubes and first cold-trap and be provided with first valve and second valve; The other end of said first valve and second valve is sealedly connected with the 3rd valve and the 4th valve; The other end of said the 3rd valve said first cold-trap that is tightly connected; Said first cold-trap second cold-trap that is tightly connected, said second cold-trap is sealedly connected with the 5th valve and the 6th valve respectively, and the other end of the other end of said the 5th valve and the 4th valve is communicated with and is communicated with the gas outlet; The other end of said the 6th valve is sealedly connected with the 7th valve, and the other end of said the 7th valve is sealedly connected with the 8th valve and said collection tube, and the other end of said the 8th valve is sealedly connected with mechanical pump; Sealing is provided with vacuum degree measuring equipment between said the 6th valve and the 7th valve; Seal respectively between said the 4th valve, the 5th valve and the gas outlet and be provided with the sodium hydroxide trap and first gas meter.
3. carbon isotope analysis pretreatment unit in a kind of organic sample according to claim 1; It is characterized in that: the reduction valve that said oxygen gas handling system comprises welding bottle, is tightly connected with said welding bottle, and second gas meter that is tightly connected with said reduction valve; Said second gas meter is sealedly connected with the 9th valve and the tenth valve respectively; Said the 9th valve seal is connected with the first rubber vacuum tube, and said the tenth valve seal is connected with the second rubber vacuum tube, and the other end of the said first rubber vacuum tube and the second rubber vacuum tube is tightly connected with two quartz outer tubes respectively.
4. carbon isotope analysis pretreatment unit in a kind of organic sample according to claim 3 is characterized in that: be connected through detachable flange seal between the said first rubber vacuum tube and the second rubber vacuum tube and said two quartz outer tubes.
5. according to carbon isotope analysis pretreatment unit in claim 2 or the 3 described a kind of organic samples, it is characterized in that: said first valve to the, ten valves are vacuum is not had the grease valve.
6. carbon isotope analysis pretreatment unit in a kind of organic sample according to claim 2 is characterized in that: said vacuum degree measuring equipment adopts the ZJ-53B type vacuum gauge of Department of Electronics of Peking University, is equipped with DL-0 type vacuum meter, range 0~300Pa.
7. carbon isotope analysis pretreatment unit in a kind of organic sample according to claim 1 is characterized in that: be disposed with porcelain boat respectively in said two quartz inner pipes and be filled in the silver-colored potpourri of cupric oxide and alum acid, filamentary silver, the copper wire in the said quartz inner pipe.
8. carbon isotope analysis pretreatment unit in a kind of organic sample according to claim 7; It is characterized in that: cupric oxide and the silver-colored potpourri of alum acid are evenly mixed with the alum acid silver that is adsorbed in zeolite surface by cupric oxide and form; The mass ratio of cupric oxide and alum acid silver is 3: 1~5: 1, and the axial length of said cupric oxide and the silver-colored potpourri of alum acid is 15~20cm.
9. carbon isotope analysis pretreatment unit in a kind of organic sample according to claim 7; It is characterized in that: the mass ratio of said filamentary silver and copper wire is 1: 10~1: 15; Said filamentary silver divides two parts to be arranged at the copper wire both sides; That part of filamentary silver of contiguous cupric oxide and the silver-colored potpourri of alum acid and the mass ratio of another part filamentary silver are 1: 1~1: 2, and the axial distance of that part of filamentary silver of contiguous cupric oxide and the silver-colored potpourri of alum acid and cupric oxide and the silver-colored potpourri of alum acid is 5~8cm.
10. carbon isotope analysis pretreatment unit in a kind of organic sample according to claim 9; It is characterized in that: be provided with silica wool between said porcelain boat and cupric oxide and the silver-colored potpourri of alum acid, be provided with silica wool between that part of filamentary silver of said cupric oxide and the alum silver-colored potpourri of acid and contiguous cupric oxide and the silver-colored potpourri of alum acid.
CN 201120433205 2011-11-04 2011-11-04 Device for analyzing and pretreating carbon isotope in organic matter sample Expired - Lifetime CN202305291U (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103091136A (en) * 2011-11-04 2013-05-08 核工业北京地质研究院 Device for analyzing and pretreating carbon isotope in organic matter sample
CN104048860A (en) * 2013-03-14 2014-09-17 核工业北京地质研究院 Sample preparation device and sample preparation method for sulfur isotope analysis
CN104181022A (en) * 2014-08-28 2014-12-03 中国科学院地质与地球物理研究所 System and method for preparing carbon dioxide gas needed by carbonate coupled isotope analysis
CN104483168A (en) * 2014-12-02 2015-04-01 中国科学院东北地理与农业生态研究所 Pretreatment method for carbon-nitrogen stable carbon isotope assay of liquid sample
CN104678047A (en) * 2015-03-18 2015-06-03 中国科学院上海应用物理研究所 Organic tritium oxidation combustion tube and organic tritium oxidation combustion method
CN109100413A (en) * 2018-09-13 2018-12-28 中国地质科学院矿产资源研究所 System and method for analyzing carbon and hydrogen isotopes oil-free valve of mineral fluid inclusion

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103091136A (en) * 2011-11-04 2013-05-08 核工业北京地质研究院 Device for analyzing and pretreating carbon isotope in organic matter sample
CN103091136B (en) * 2011-11-04 2015-04-29 核工业北京地质研究院 Device for analyzing and pretreating carbon isotope in organic matter sample
CN104048860A (en) * 2013-03-14 2014-09-17 核工业北京地质研究院 Sample preparation device and sample preparation method for sulfur isotope analysis
CN104181022A (en) * 2014-08-28 2014-12-03 中国科学院地质与地球物理研究所 System and method for preparing carbon dioxide gas needed by carbonate coupled isotope analysis
CN104483168A (en) * 2014-12-02 2015-04-01 中国科学院东北地理与农业生态研究所 Pretreatment method for carbon-nitrogen stable carbon isotope assay of liquid sample
CN104678047A (en) * 2015-03-18 2015-06-03 中国科学院上海应用物理研究所 Organic tritium oxidation combustion tube and organic tritium oxidation combustion method
CN109100413A (en) * 2018-09-13 2018-12-28 中国地质科学院矿产资源研究所 System and method for analyzing carbon and hydrogen isotopes oil-free valve of mineral fluid inclusion

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