CN207717687U - 14C-AMS fast on-line analyzing instrument - Google Patents

Abstract

The utility model discloses one kind¹⁴C AMS fast on-line analyzing instrument comprising：Solid sample processing module, atmospheric sample acquisition and processing module, micrometeor control module, AMS modules and automatic control module.The utility model is beneficial in that：It has merged sample preparation to measure with AMS, not only can rapidly and efficiently analyze¹⁴C sample (including solid sample and atmospheric sample) reduces sample and gets dirty possibility, and interior in finite state machine can be substantially improved for the laboratories AMS¹⁴C sample analyzes power of test, while can also provide another stronger scheme of more quick and contamination resistance for the measurement of denier sample (content is in several micrograms)；Solid-state primary sample is not necessarily to chemical laboratory special disposal, is converted into CO₂Gas enters AMS measurements, and atmospheric sample can acquire in real time carries out AMS analyses, changes original specialty chemical laboratory elder generation sample preparation completely and carries out again¹⁴The flow that C AMS are measured.

Description

14C-AMS fast on-line analyzing instrument

Technical field

The utility model is related to one kind¹⁴C analyzers, and in particular to a kind of¹⁴C-AMS fast on-line analyzing instrument, belongs to analysis Equipment technical field.

Background technology

The development of AMS (Accelerator Mass Spectrometry, accelerator mass spectrometry) technology is with popularization so that length Service life radionuclide¹⁴C is widely used in geoscience, environmental science, archaeology, life science, Marine Sciences, cosmochemistry Equal fields.Currently, the laboratories AMS nearly various schools of thinkers in the world, when energy and machine in 90% or more nearly all laboratory, still throws Enter¹⁴In C researchs.Since AMS occur since, development always with¹⁴C with mutually promoting, the continuous development of AMS technologies Do not stop to push¹⁴C use field extension, scientists for¹⁴C frontiers developing or to have field deep-cut and Promoting AMS to have to will be original¹⁴C-AMS analytical technologies push forward.

In recent years, it is all polycyclic that national governments generally face the safety problems such as radionuclide contamination, social development is brought Border problem and the new cross discipline problem continued to bring out, these all promote the continuous development of AMS research directions.Flourishing state Family is planned to implement to be based on¹⁴The environmental monitoring and the fast slowdown monitoring of radioactive pollution and react that C-AMS is measured, to prevent possibility generation Core biochemical event (CBRN), the decision-making foundation of science is provided for government.With biomedical development,¹⁴C is as tracer quilt Extensive use, need quickly, large-scale basis data the characteristics of embody undoubtedly.Instantly, global warming and mankind's activity release CO₂Isothermal chamber gas is closely bound up, how many CO₂Be the discharge from fossil fuel it is current urgent environmental problem and important Problem in science, and emerging air Δ¹⁴C monitorings will annotate fossil fuel carbon emission amount pair with another independent visual angle CO₂Contribution amount, establish the fossil fuel carbon emission amount accounting method of science.

Above-mentioned completely new and unique research field is required to quick and a large amount of with direction¹⁴C measurement data provides for research In time, continuous basic data.

But it is conventional¹⁴Solid target sample sputtering mode used by C-AMS analysis methods far can not meet quickly With the demand of extensive sample test.Traditional¹⁴C unknown samples need unknown sample being sent to corresponding chemical pre-treatment before measuring With sample preparation laboratory, C contained therein is converted to CO by special chemical laboratory₂And purify, later again with one Longer time is by CO₂It is reduced to graphite (one convention amount sample H of reduction₂/ Fe methods at least 4 hours, and Zn/Fe rules are small up to 12 When or so), make¹⁴C measurement data obtains excessive cycle, and monocyte sample whole cycle is at least at 2 days or more.

In this case, it cannot be satisfied first and need quickly to analyze the research field according to result；Secondly many laboratories It is interior in limited machine to cannot be satisfied the scientific research demand for needing extensive sample to be supported as basic data；In another aspect, sample Contaminated possibility is greatly increased also with the increase of flow time and the reduction of sample size in longer flow.

As it can be seen that conventional sample chemical processing mode is entered plus solid ion sources using extraction after the bombardment of graphite target sample The pattern that AMS is measured cannot be satisfied quick or extensive or denier sample analysis test request completely.

Currently, it includes mainly following three type to explore the gas ion source drawn with the sputtering of gas target sample developed in the world Type：

The first, microwave plasma ion source is developed by the institutes of oceanography Woods Hole in the U.S..The CO prepared₂ After importing ion source by silicon capillary, C is generated⁺Line.In order to obtain anion line, measured for AMS, closely ion source Equipped with charge-exchange " channel ", C⁺It is converted into C here^-Line.It will be micro- using argon gas as carrier for minimum sample size Measure CO₂Ion source is imported, at charge-exchange channel, argon gas collects device (beam since charge-exchange occurs by line Dump it) collects, C^-Then measured in detector after accelerating, removing.This mode is utilized positive ion source and then converts For AMS measure needed for anion, it is excessively complicated in design and can not ensure final C^-The yield of line, meanwhile, other nucleic exist The measurement of this ion source receives restriction.Importantly, the program and be not implemented quickly it is succinct¹⁴C measurement schemes.Therefore, The ion source be one fine embody physical theory and thought device, but be not appropriate for practical scale and quickly¹⁴C is surveyed Examination.

Second, gas ion source is by the gas loading system of designed, designed by CO₂Ion source head is imported, this is System is that the solid/gas dual-purpose caesium plasma sputter source based on NEC MC-SNICS is transformed, CO₂By advanced combustion and seal up for safekeeping in 6mm In the Pyrex glass tubes of outer diameter, then glass tube is put into bellows, etc. vacuum degrees reduce after, pass through Curved Corrugated pipe will Equipped with CO₂The glass tube of gas fractures, by control valve, by CO₂Gas (with helium) injects ion source head with certain speed, Realize that sample measures.System solves the problem Cs plasma sputters sources for the basis of gas target sample analysis possibility, still, this side The processing of original sample and the test of AMS are still isolated and are come by formula, are not merged and achieve the purpose that quickly to analyze.But at the beginning of it Step establishes Cs⁺Sputter negative ion source can measure gas CO₂The theory and practice basis of target sample.

The third, gas ion source is to handle the design that the thinking based on solid sample carries out.Pass through elemental analyser (Elemental Analyzer) burning obtains CO₂, EA-AMS ion sources can be referred to as.The ion source is produced in NEC Corporation MC-SNICS and HVEE companies production the solid/gas dual-purpose caesium plasma sputter sources SO-110 on the basis of be transformed.Pass through member Plain analyzer obtains pure CO after realizing solid sample conflagration separation₂Gas, then using helium be carrier gas by CO₂It imports after improving Ion source target, special target head is sputtered by CO with caesium₂It is converted into C^-After draw, for AMS measure.Such ion source is current Newest probing direction in the research and development of gas class ion source, it would be possible to solve quick online burning and the AMS tests of a large amount of samples. More crucial is a little that such ion source directly generates pure CO mainly for solid sample with elemental analysis₂Gas it is quick Analysis is not directed to the direct analysis of atmospheric sample, therefore and unbonded CO₂Purification system so that need scale now The atmospheric sample of rapid batch can not be measured by it.

Utility model content

To solve the deficiencies in the prior art, it can both have been analyzed admittedly with direct-on-line the purpose of this utility model is to provide a kind of Body sample and atmospheric sample can be analyzed with direct-on-line¹⁴C-AMS fast on-line analyzing instrument.

In order to realize above-mentioned target, the utility model adopts the following technical scheme：

It is a kind of¹⁴C-AMS fast on-line analyzing instrument, which is characterized in that including：

Solid sample processing module：By elemental analysis submodule and CO₂Purified pool submodule forms, wherein element point Analysis submodule is for directly converting solid sample to CO₂, CO₂Purified pool submodule is used for CO₂It is purified and is collected, Solid sample is converted into CO via elemental analysis submodule₂After be directly entered CO₂Purified pool submodule；

Atmospheric sample acquires and processing module：Submodule and CO are acquired by atmospheric sample₂Sub-module stored composition is purified, In, atmospheric sample acquires submodule for acquiring the atmospheric sample at different height, CO in real time₂Purify sub-module stored for pair CO₂It is purified and is stored, atmospheric sample is directly entered CO after being acquired via atmospheric sample acquisition submodule₂Purifying storage submodule Block；

Micrometeor control module：For to from solid sample processing module and atmospheric sample acquisition and processing module come out CO₂Micrometeor control is carried out, CO is made₂Flow be maintained at 10 μ l/min or less；

AMS modules：For the CO to being come out from micrometeor control module₂Carry out the CO under Cs sputterings₂→C^-Line draws Go out, and gaseous sample is directly carried out¹⁴C-AMS is measured；

And automatic control module：For to solid sample processing module, atmospheric sample acquisition and processing module and miniflow The course of work of amount control module is controlled, with the online operation of AMS modules.

It is above-mentioned¹⁴C-AMS fast on-line analyzing instrument, which is characterized in that aforementioned elements analyze submodule using element Analyzer.

It is above-mentioned¹⁴C-AMS fast on-line analyzing instrument, which is characterized in that aforementioned CO₂Purified pool submodule includes：6 choosings Select valve, CO₂Molecular sieve, pressure gauge, pump, quantitative cold-trap and several solenoid valves, wherein

Aforementioned 6 selector valves are connected two-by-two, and 1^#Valve port connect with elemental analysis submodule, 2^#Valve port connects with miscellaneous gas discharge pipe Connect, 3^#Valve port and CO₂The input end connection of molecular sieve, 4^#Valve port connect with the input end of quantitative cold-trap, 5^#Valve port and He carrier gas pipes Connection, 6^#Valve port and CO₂The outlet end of molecular sieve connects；

Aforementioned CO₂Molecular sieve is to CO₂Desorption controlled by accurate temperature controlling electric furnace；

Aforementioned pressure meter and pump are arranged in the installation pipeline of quantitative cold-trap；

Aforementioned electromagnetic valve is arranged in the appropriate position of each installation pipeline, and module under automated control controls.

It is above-mentioned¹⁴C-AMS fast on-line analyzing instrument, which is characterized in that aforementioned CO₂It is filled in the front end pipeline of molecular sieve Drier.

It is above-mentioned¹⁴C-AMS fast on-line analyzing instrument, which is characterized in that aforementioned atmospheric sample acquires submodule and includes：Air inlet Pipe, air filter, solenoid valve and escape pipe, wherein

Air inlet pipe has several, acquires atmospheric sample from different height respectively, and air filter is mounted on every air inlet The outlet side of the inlet end of pipe, all air inlet pipe is connect with solenoid valve, and the atmospheric sample in air inlet pipe is converted via solenoid valve It is entered in escape pipe after inlet channel, aforementioned escape pipe and CO₂Purify sub-module stored connection.

It is above-mentioned¹⁴C-AMS fast on-line analyzing instrument, which is characterized in that aforementioned CO₂Purifying sub-module stored includes：Sample introduction Pipeline, two-stage purifying cold-trap, storage cold-trap, two determining volume branch pipes, out sample tube line, vacuum pump and several high vacuum Valve and vacuum meter/pressure sensor, wherein

Sample introduction pipeline, level-one purifying cold-trap, two level purifying cold-trap, first determining volume branch pipe, storage cold-trap, the Two determining volume branch pipes, out sample tube lines are sequentially connected in series, and vacuum pump is vacuumized by three pipelines pair, three cold-traps, high Vacuum valve and vacuum meter/pressure sensor are mounted on the appropriate position of entire submodule.

It is above-mentioned¹⁴C-AMS fast on-line analyzing instrument, which is characterized in that aforementioned CO₂Purifying sub-module stored further includes：It is standby With air sample introduction pipeline is not purified, which connect with sample introduction pipeline.

It is above-mentioned¹⁴C-AMS fast on-line analyzing instrument, which is characterized in that aforementioned CO₂Purifying sub-module stored further includes：It is standby With having purified CO₂Sample introduction pipeline, this is spare to have purified CO₂Sample introduction pipeline purifies cold-trap and first determining volume with two level is connect With the piping connection of branch pipe.

It is above-mentioned¹⁴C-AMS fast on-line analyzing instrument, which is characterized in that aforementioned micrometeor control module includes：4 selections Valve, 6 selector valves and accurate temperature controlling cold-trap, wherein

The 1 of aforementioned 4 selector valves^#Valve port and CO₂The outlet of purified pool submodule connects, and 2^#Valve port and CO₂Purifying is deposited The out sample tube line for storing up submodule connects, and 3^#Valve port and 4^#Valve port is spare valve port, and outlet is connect with 6 selector valves；

Aforementioned 6 selector valves are connected two-by-two, and 1^#Valve port connect with the outlet of 4 selector valves, 2^#Valve port and miscellaneous gas discharge pipe Connection, 3^#Valve port connect with one end of accurate temperature controlling cold-trap, 4^#Valve port connect with the ion source of AMS modules, 5^#Valve port and He carrier gas Pipe connection, 6^#Valve port is connect with the other end of accurate temperature controlling cold-trap.

The utility model is beneficial in that：The utility model¹⁴C-AMS fast on-line analyzing instrument, with gas CO₂Directly Based on connecing sputtering analytical technology, by gas CO₂Sample is directly analyzed¹⁴C technologies directly link with AMS, have merged sample preparation It measures with AMS, not only can rapidly and efficiently analyze¹⁴C sample (including solid sample and atmospheric sample) reduces sample and gets dirty possibility Property, and interior in finite state machine can be substantially improved for the laboratories AMS¹⁴C sample analyzes power of test, while can also be atomic The measurement of amount sample (content is in several micrograms) provides another stronger scheme of more quick and contamination resistance；Solid-state is original Sample is not necessarily to chemical laboratory special disposal, is converted into CO₂Gas enter AMS measurement, atmospheric sample can acquire in real time into Row AMS analyses, change original specialty chemical laboratory elder generation sample preparation and carry out again completely¹⁴The flow that C-AMS is measured.

Description of the drawings

Fig. 1 is the utility model¹⁴The composition schematic diagram of C-AMS fast on-line analyzing instrument；

Fig. 2 is the CO in Fig. 1₂The composition schematic diagram of purified pool submodule and micrometeor control module；

Fig. 3 is the composition schematic diagram of the atmospheric sample acquisition submodule in Fig. 1；

Fig. 4 is the CO in Fig. 1₂Purify the composition schematic diagram of sub-module stored.

The meaning of reference numeral in figure：11-6 selector valves, 12-CO₂Molecular sieve, 13- pressure gauges, 14- pumps, 15- are quantitative Cold-trap, 16- solenoid valves, 17- solenoid valves, 18- solenoid valves, 19- solenoid valves, 20- solenoid valves, 21-4 selector valves, 22-6 choosings Select valve, 23- accurate temperature controllings cold-trap, 24- air inlet pipe, 25- air filters, 26- solenoid valves, 27- escape pipes, 28- sample introductions pipeline, 29- level-ones purify cold-trap, 30- two levels purifying cold-trap, 31- storages cold-trap, the determining volume branch pipes of 32- first, 33- second A determining volume branch pipe, 34- out sample tubes line, 35- vacuum pumps, 36- be spare, and not purify air sample introduction pipeline, 37- spare pure Change CO₂Sample introduction pipeline.

Specific implementation mode

The utility model¹⁴C-AMS fast on-line analyzing instrument is based on gas ion source operating mode, is a synthesis Property¹⁴Online processing gaseous sample and solid sample may be implemented in C-AMS quick analysis systems, and then it is quick that AMS may be implemented Test analysis, fundamental design idea are " modularization, rapid, automation, versatility, opening ", and each module has opposite Independent function.

Specific introduce is made to the utility model below in conjunction with the drawings and specific embodiments.

Referring to Fig.1, the utility model¹⁴C-AMS fast on-line analyzing instrument includes：Solid sample processing module, big gas sample Product acquire and processing module, micrometeor control module, AMS modules and automatic control module.

One, solid sample processing module

Solid sample processing module obtains the CO of purifying for handling solid sample₂。

Solid sample processing module is by elemental analysis submodule and CO₂Purified pool submodule forms.

1, elemental analysis submodule

Elemental analysis submodule makes it be converted into CO for directly solid sample to burn₂Gas.

In the present invention, elemental analysis submodule we using elemental analyser.

Existing elemental analyser, offgas outlet are typically 6mm pipelines, we slightly change its offgas outlet It makes, first 6mm pipelines and 1/8 inch Copper tube is transferred, then 1/8 inch Copper tube and 1/4 inch of stainless steel tube are transferred, in this way Itself and CO can be facilitated₂Purified pool submodule connects, you can to facilitate CO₂Into CO later₂Purified pool submodule.

When using elemental analyser, first solid sample is crushed to powdered, is then wrapped with aluminium foil, and precise Sample is led to O by quality directly from the combustion tube that sample injection disc is sent into 950 DEG C later in combustion tube₂And it is aided with CuO and carries out completely Burning obtains CO₂, hereafter the gas of completely burned enter load Cu powder reduction tube carry out NO or NO₂Reduction obtains N₂, N₂、CO₂ Enter CO under the carrier band of carrier gas He with some miscellaneous gas₂Adsorption column, after after different time desorption successively enter TCD detect Device, it is last successively to be exported by offgas outlet, wherein N₂, miscellaneous gas and CO₂Carrier gas is discharged by vacuum system before peak, CO₂After then accessing Continuous CO₂Purified pool submodule, the process are switched over by multidigit selector valve.

In practical operation, we are to CO₂The desorption time is adjusted, and N is specifically adjusted to₂Postpone 30 seconds after appearance.

Solid sample is converted into CO via elemental analysis submodule₂After be directly entered CO₂Purified pool submodule.

2、CO₂Purified pool submodule

CO₂Purified pool submodule is used for the CO to being generated by elemental analysis submodule₂It is purified and is collected.

With reference to Fig. 2, CO₂Purified pool submodule includes：6 selector valves 11, CO₂Molecular sieve 12, pump 14, is determined pressure gauge 13 Measure cold-trap 15 and several solenoid valves.

(1) 6 selector valve

With reference to Fig. 2,6 selector valves 11 are connected two-by-two, wherein 1^#Valve port is connect with elemental analysis submodule, and 2^#Valve port with it is miscellaneous Gas discharge pipe connects, and 3^#Valve port and CO₂The input end of molecular sieve 12 connects, and 4^#Valve port is connect with the input end of quantitative cold-trap 14, and 5^# Valve port is connect with He carrier gas pipes, and 6^#Valve port and CO₂The outlet end of molecular sieve 12 connects.

Connection 1^#Valve port is equipped with solenoid valve 16 on the pipeline of elemental analysis submodule.

Connection 4^#Valve port is equipped with solenoid valve 17 on the pipeline of quantitative cold-trap 15, is installed on the fairlead of quantitative cold-trap 15 There is solenoid valve 20.

Connection 5^#Valve port is equipped with solenoid valve 18 on the pipeline of He carrier gas pipes.

The module control under automated control of solenoid valve 16, solenoid valve 17, solenoid valve 18, solenoid valve 20.

(2)CO₂Molecular sieve

CO₂Molecular sieve 12 is for absorbing and storing CO₂With release CO₂, to CO₂Desorption by accurate temperature controlling electric furnace Controlled, when need discharge CO₂Shi Liyong accurate temperature controlling electric furnaces carry out desorption, the CO after desorption₂Into quantitative cold-trap.

As a preferred solution, CO₂Drier is filled in the front end pipeline of molecular sieve 12, for drying steam.

(3) pressure gauge, pump

Pressure gauge 13 and pump 14 are arranged in the installation pipeline of quantitative cold-trap 15, wherein pressure gauge 13 is located at solenoid valve After 17, pump 14 is located at after pressure gauge 13, pumps and is equipped with solenoid valve 19 in 14 installation pipeline.

The also module control under automated control of solenoid valve 19.

(4) quantitative cold-trap

Quantitative cold-trap 15 is for purifying CO again₂, interim storage CO₂With determining CO₂Volume, carry pressure measurement Device.

CO₂The operation principle of purified pool submodule：

Solid sample is after elemental analysis submodule automatic business processing, miscellaneous gas (N₂And carrier gas) and under test gas (CO₂With Carrier gas) it is different when access 6 selector valves, 11,6 selector valves 11 be connected two-by-two：

When 1^#Valve port and 2^#(with reference to Fig. 2) when valve port is connected, miscellaneous gas discharge, and under test gas has stored in CO₂Molecular sieve In 12, CO is heated₂I.e. release CO after molecular sieve 12₂, at the same time, the He carrier gas in He gas tanks is by 5^#Valve port accesses the CO₂Purifying Collect submodule, the CO discharged under the carrier band of He carrier gas₂By 4^#Valve port enters subsequent quantitative cold-trap 15, and quantitative cold-trap 15 can By each valve complete closure, to determine CO₂Volume；

When switching to 1^#Valve port and 6^#Valve port conducting, 2^#Valve port and 3^#Valve port conducting, 4^#Valve port and 5^#When valve port is connected, to inhale Attached under test gas pattern, at this point, the CO drawn by elemental analysis submodule₂Via 1^#Valve port accesses the CO₂Purified pool submodule Block, He carrier gas and CO₂Simultaneously through 6^#Valve port enters CO₂Molecular sieve 12, wherein CO₂It is adsorbed, and He carrier gas is by 2^#Valve port is discharged.

6 selector valves 11 are with the N of the sample handled by elemental analysis submodule₂Peak occurs and terminates switching point in order to control.

CO₂Through CO₂Purified pool submodule is collected after purification in quantitative cold-trap 15, when needing to measure, is collected quantitative CO in cold-trap 15₂It is directly entered micrometeor control module.

Two, atmospheric sample acquisition and processing module

Atmospheric sample acquires and processing module is used to be acquired Real-Time Atmospheric sample and online processing, obtains purifying CO₂。

Atmospheric sample acquires and processing module acquires submodule and CO by atmospheric sample₂Purify sub-module stored composition.

1, atmospheric sample acquires submodule

Atmospheric sample acquires submodule for acquiring the atmospheric sample at different height in real time.

With reference to Fig. 3, atmospheric sample acquisition submodule includes：Air inlet pipe 24, air filter 25, solenoid valve 26 and escape pipe 27。

Air inlet pipe 24 have several (such as：Four), respectively from different height acquisition atmospheric sample (such as：Air inlet Height apart from ground is respectively 2m, 15m, 25m, 35m), air filter 25 is mounted on the inlet end of every air inlet pipe 24, institute There is the outlet side of air inlet pipe 24 to be connect with solenoid valve 26, the atmospheric sample in air inlet pipe 24 is converted air inlet via solenoid valve 26 and led to It is entered behind road in escape pipe 27.

Air inlet pipe 24 and the specification of escape pipe 27 can be：Outer diameter 6mm, internal diameter 4mm.

As a preferred solution, air inlet pipe 24 and escape pipe 27 are made of polytetrafluoroethylene (PTFE).

Atmospheric sample is directly entered CO after being acquired via atmospheric sample acquisition submodule₂Purify sub-module stored.

2、CO₂Purify sub-module stored

CO₂Sub-module stored is purified to be used for by the collected CO of atmospheric sample acquisition submodule₂It is purified and is stored.

With reference to Fig. 4, CO₂Purifying sub-module stored includes：Sample introduction pipeline 28, two-stage purifying cold-trap (level-one purify cold-trap 29, Two level purify cold-trap 30), storage 31, two determining volume branch pipe (first determining volume branch pipes 32, second of cold-trap Determine volume branch pipe 33), out sample tube line 34, vacuum pump 35 and several high vacuum valves and vacuum meter/pressure sensor.

Sample introduction pipeline 28, level-one purifying cold-trap 29 (remove CO for rejecting₂With the gas other than aqueous vapor), two level purify cold-trap 30 (for shifting CO₂Gas, to which aqueous vapor be discharged), first determining volume branch pipe 32, storage cold-trap 31 be (for storing CO₂Gas), second determining volume branch pipe 33, out sample tube line 34 be sequentially connected in series, vacuum pump 35 passes through three pipelines pair three Cold-trap is vacuumized, and high vacuum valve and vacuum meter/pressure sensor are suitably pacified on the appropriate location of entire submodule Dress.

As a preferred solution, CO₂Purifying sub-module stored further includes：It is spare not purify air sample introduction pipeline 36, The spare air sample introduction pipeline 36 that do not purify is connect with sample introduction pipeline 28, and the gaseous sample for accessing field acquisition is pacified thereon Equipped with high vacuum valve.

More preferably, CO₂Purifying sub-module stored further includes：It is spare to have purified CO₂Sample introduction pipeline 37, this is spare pure Change CO₂Sample introduction pipeline 37 purifies the piping connection of cold-trap 30 and first determining volume branch pipe 32 with two level is connect, for connecing Enter purified gaseous sample, high vacuum valve is also installed thereon.

Due to CO₂Purifying sub-module stored has sample introduction pipeline 28, the spare air sample introduction pipeline 36, spare of not purifying simultaneously CO is purified₂The pipeline of 37 3 kinds of sample introductions of sample introduction pipeline, it is achieved that atmospheric sample multimode sample introduction, uses extremely just It is prompt.

CO₂Through CO₂Purify the CO of sub-module stored after purification₂It is stored in storage cold-trap, when needing to measure, storage CO in storage cold-trap₂It is directly entered micrometeor control module.

Three, micrometeor control module

Micrometeor control module be used for from solid sample processing module and atmospheric sample acquisition and processing module come out CO₂Micrometeor control is carried out, CO is made₂Flow be maintained at 10 μ l/min hereinafter, in order to AMS modules carry out¹⁴C-AMS is measured.

With reference to Fig. 2, micrometeor control module includes：4 selector valves, 21,6 selector valves 22 and accurate temperature controlling cold-trap 23.

1,4 selector valves

The 1 of 4 selector valves 21^#Valve port and CO₂The outlet of purified pool submodule connects, and 2^#Valve port and CO₂Purifying storage The out sample tube line of submodule connects, and 3^#Valve port and 4^#Valve port is spare valve port, and 5^#Valve port (outlet) is connect with 6 selector valves.

The working method of 4 selector valves 21：1^#Valve port, 2^#Valve port, 3^#Valve port and 4^#It is cut between this four valve ports of valve port It changes, 5^#Valve port (outlet) always with 6 selector valves 22 1^#Valve port connects.

2,6 selector valves

6 selector valves 22 are connected two-by-two, and 1^#Valve port is connect with the outlet of 4 selector valves 21, and 2^#Valve port and miscellaneous gas discharge pipe Connection, 3^#Valve port is connect with one end of accurate temperature controlling cold-trap 23, and 4^#Valve port is connect with the ion source of AMS modules, and 5^#Valve port is carried with He Tracheae connects, and 6^#Valve port is connect with the other end of accurate temperature controlling cold-trap 23.

3, accurate temperature controlling cold-trap

Accurate temperature controlling cold-trap is the temperature for controlling gas.

Temperature-controlled precision of the accurate temperature controlling cold-trap when temperature is less than -150 DEG C is 1 DEG C, when temperature is -150 DEG C~-70 DEG C Temperature-controlled precision be 0.5 DEG C, the temperature-controlled precision when temperature is -70 DEG C~200 DEG C is 0.2 DEG C.

The operation principle of micrometeor control module：

When the 1 of 6 selector valves 22^#Valve port and 6^#Valve port conducting, 2^#Valve port and 3^#Valve port conducting, 4^#Valve port and 5^#Valve port is connected When (as shown in Figure 2), 4 selector valves 21 import gases, and gas enters accurate temperature controlling cold-trap 23 and first stores, and miscellaneous gas is by 6 The 3 of selector valve 22^#Valve port is through 2^#Valve port is discharged, and 4^#Valve port and 5^#Valve port is closed, and keeps ion source vacuum of this section with AMS modules Degree is always；

Wait for CO₂After the storage of accurate temperature controlling cold-trap 23,6 selector valves 22 switch to another conduction mode, i.e., 1^#Valve port and 2^# Valve port conducting, 3^#Valve port and 4^#Valve port conducting, 5^#Valve port and 6^#Valve port is connected, at this point, 4 selector valves 21 are without under test gas, other Miscellaneous gas is directly by the 2 of 6 selector valves 22^#Valve port is discharged, and 23 accurate temperature controlling of accurate temperature controlling cold-trap selects suitable CO₂Saturated vapor Pressure, slowly discharges CO very much₂, make CO₂Flow be maintained at 10 μ l/min hereinafter, simultaneously, control He carrier gas is by 6 selector valves 22 5^#Valve port enters micrometeor control module, and is conducted to 6^#Valve port, He carrier gas carry the CO in accurate temperature controlling cold-trap 23₂It is selected from 6 Select the 3 of valve 22^#Valve port is drawn, by 4^#Valve port enters the ion source of AMS modules.

Four, AMS modules

AMS modules are used for the CO to being come out from micrometeor control module₂Carry out the CO under Cs sputterings₂→C^-The extraction of line, And gaseous sample is directly carried out¹⁴C-AMS is measured.

As a preferred solution, AMS modules are using Xi ' an-AMS.

Five, automatic control module

Automatic control module is used to control solid sample processing module, atmospheric sample acquisition and processing module and micrometeor The course of work of module is controlled, with the online operation of AMS modules.

It can be seen that the utility model¹⁴C-AMS fast on-line analyzing instrument has the characteristics that and advantage：

1, sample analysis test is rapid, integrated

The utility model¹⁴The rapid of C-AMS fast on-line analyzing instrument is mainly reflected in what sample preparation was measured with AMS It integrates, that is, eliminates and take longest CO in conventional method₂Be reduced to the flow of graphite, this be greatly reduced analysis time, The possibility for improving efficiency, reducing sample pollution.

The utility model¹⁴C-AMS fast on-line analyzing instrument, the linking of each submodule is particularly critical, realizes each submodule The standardization of block physical interface/outlet can be linked simply and control break-make.

2, auto-control

The utility model¹⁴C-AMS fast on-line analyzing instrument realizes automation control substantially, changes traditional mould completely The mode of gas circuit is manually controlled under formula, each widget (such as pump group, valve group, cold-trap temperature control) realizes automation control, Real-time various state parameters can be directly acquired simultaneously to understand experiment process.

3, Universal joint

The utility model¹⁴C-AMS fast on-line analyzing instrument, Universal jointization are not only embodied in each submodule physics and connect The standardization (being embodied in the selection and control of each control element using current standard and data-interface) of mouth/outlet, But also it is embodied in the unified standard interface to existing conventional method of standard of each tie point of each submodule, it does so convenient for day Unify to safeguard afterwards and be accessed with sample.

4, there is high open and compatibility

The utility model¹⁴The above-mentioned design philosophy of C-AMS fast on-line analyzing instrument and feature ensure that its it is open with Compatibility, it is following be somebody's turn to do to improve with the interface (including physical interface and control interface) of standard and control model¹⁴C-AMS is quick The basis that in-line analyzer is expanded, developed again can increase the quick analysis submodule of other form samples in the future, quickly by this Analyzing submodule insertion should¹⁴C-AMS fast on-line analyzings instrument can carry out¹⁴C-AMS is analyzed, while can also be to other gases The long lived nuclides of form carry out corresponding submodule exploitation, which is embedded in¹⁴In C-AMS fast on-line analyzing instrument just AMS measurements can be carried out in real time.

5, other

It incorporates sample chemical pre-treatment to test with AMS, substantially reduces data acquisition flow, improve work efficiency, Reduce the contaminated possibility of sample.

It should be noted that above-described embodiment does not limit the utility model in any form, it is all to use equivalent replacement or wait The technical solution that the mode of effect transformation is obtained, all falls in the scope of protection of the utility model.

Claims (9)

1. a kind of¹⁴C-AMS fast on-line analyzing instrument, which is characterized in that including：

Solid sample processing module：By elemental analysis submodule and CO₂Purified pool submodule forms, wherein elemental analysis submodule Block is for directly converting solid sample to CO₂, CO₂Purified pool submodule is used for CO₂It is purified and is collected, solid-like Product are converted into CO via elemental analysis submodule₂After be directly entered CO₂Purified pool submodule；

Atmospheric sample acquires and processing module：Submodule and CO are acquired by atmospheric sample₂Purify sub-module stored composition, wherein big Gas sample collection submodule for acquiring the atmospheric sample at different height, CO in real time₂Sub-module stored is purified to be used for CO₂Into Row purifying and storage, atmospheric sample are directly entered CO after being acquired via atmospheric sample acquisition submodule₂Purify sub-module stored；

Micrometeor control module：For the CO to being come out from solid sample processing module and atmospheric sample acquisition and processing module₂Into Row micrometeor controls, and makes CO₂Flow be maintained at 10 μ l/min or less；

AMS modules：For the CO to being come out from micrometeor control module₂Carry out the CO under Cs sputterings₂→C^-The extraction of line, and Gaseous sample is directly carried out¹⁴C-AMS is measured；

And automatic control module：For to solid sample processing module, atmospheric sample acquisition and processing module and micrometeor control The course of work of molding block is controlled, with the online operation of AMS modules.

2. according to claim 1¹⁴C-AMS fast on-line analyzing instrument, which is characterized in that the elemental analysis submodule is adopted It is elemental analyser.

3. according to claim 1¹⁴C-AMS fast on-line analyzing instrument, which is characterized in that the CO₂Purified pool submodule Block includes：6 selector valves, CO₂Molecular sieve, pressure gauge, pump, quantitative cold-trap and several solenoid valves, wherein

6 selector valves are connected two-by-two, and 1^#Valve port connect with elemental analysis submodule, 2^#Valve port connect with miscellaneous gas discharge pipe, 3^# Valve port and CO₂The input end connection of molecular sieve, 4^#Valve port connect with the input end of quantitative cold-trap, 5^#Valve port connect with He carrier gas pipes, 6^#Valve port and CO₂The outlet end of molecular sieve connects；

The CO₂Molecular sieve is to CO₂Desorption controlled by accurate temperature controlling electric furnace；

The pressure gauge and pump are arranged in the installation pipeline of quantitative cold-trap；

The solenoid valve is arranged in the appropriate position of each installation pipeline, and module under automated control controls.

4. according to claim 3¹⁴C-AMS fast on-line analyzing instrument, which is characterized in that the CO₂The front end of molecular sieve Drier is filled in pipeline.

5. according to claim 1¹⁴C-AMS fast on-line analyzing instrument, which is characterized in that the atmospheric sample acquires submodule Block includes：Air inlet pipe, air filter, solenoid valve and escape pipe, wherein

Air inlet pipe has several, acquires atmospheric sample from different height respectively, and air filter is mounted on every air inlet pipe The outlet side of inlet end, all air inlet pipe is connect with solenoid valve, and the atmospheric sample in air inlet pipe converts air inlet via solenoid valve It is entered in escape pipe behind channel, the escape pipe and CO₂Purify sub-module stored connection.

6. according to claim 5¹⁴C-AMS fast on-line analyzing instrument, which is characterized in that the CO₂Purifying storage submodule Block includes：Sample introduction pipeline, two-stage purifying cold-trap, storage cold-trap, two determining volume branch pipes, out sample tube line, vacuum pump with And several high vacuum valves and vacuum meter/pressure sensor, wherein

Sample introduction pipeline, level-one purifying cold-trap, two level purifying cold-trap, first determining volume branch pipe, storage cold-trap, second Determine that volume branch pipe, out sample tube line are sequentially connected in series, vacuum pump is vacuumized by three pipelines pair, three cold-traps, high vacuum Valve and vacuum meter/pressure sensor are mounted on the appropriate position of entire submodule.

7. according to claim 6¹⁴C-AMS fast on-line analyzing instrument, which is characterized in that the CO₂Purifying storage submodule Block further includes：Spare not purify air sample introduction pipeline, which connect with sample introduction pipeline.

8. according to claim 6¹⁴C-AMS fast on-line analyzing instrument, which is characterized in that the CO₂Purifying storage submodule Block further includes：It is spare to have purified CO₂Sample introduction pipeline, this is spare to have purified CO₂Sample introduction pipeline purifies cold-trap and first with two level is connect The piping connection of a determining volume branch pipe.

9. according to claim 1¹⁴C-AMS fast on-line analyzing instrument, which is characterized in that the micrometeor control module packet It includes：4 selector valves, 6 selector valves and accurate temperature controlling cold-trap, wherein

The 1 of 4 selector valves^#Valve port and CO₂The outlet of purified pool submodule connects, and 2^#Valve port and CO₂Purifying storage The out sample tube line of module connects, and 3^#Valve port and 4^#Valve port is spare valve port, and outlet is connect with 6 selector valves；

6 selector valves are connected two-by-two, and 1^#Valve port connect with the outlet of 4 selector valves, 2^#Valve port connects with miscellaneous gas discharge pipe Connect, 3^#Valve port connect with one end of accurate temperature controlling cold-trap, 4^#Valve port connect with the ion source of AMS modules, 5^#Valve port and He carrier gas pipes Connection, 6^#Valve port is connect with the other end of accurate temperature controlling cold-trap.