CN109358671A - One kind being suitable for the mass spectrometric temperature control method of rare gas - Google Patents
One kind being suitable for the mass spectrometric temperature control method of rare gas Download PDFInfo
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- CN109358671A CN109358671A CN201811028631.9A CN201811028631A CN109358671A CN 109358671 A CN109358671 A CN 109358671A CN 201811028631 A CN201811028631 A CN 201811028631A CN 109358671 A CN109358671 A CN 109358671A
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- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D23/00—Control of temperature
- G05D23/19—Control of temperature characterised by the use of electric means
- G05D23/30—Automatic controllers with an auxiliary heating device affecting the sensing element, e.g. for anticipating change of temperature
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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Abstract
The invention discloses one kind to be suitable for the mass spectrometric temperature control method of rare gas, and steps are as follows: A-1, heating, and A-2, constant temperature are kept, A-3, cooling.There are the two kinds of heating modes of mode and constant heating rates sintering mode that are rapidly heated in A-1 step, keep temperature constant by heater in A-2 step, there are air-cooled mode, fast-refrigerating mode and constant speed refrigerating mode Three models in A-3 step, keep cooling velocity constant by heater under constant speed refrigerating mode；In three steps, heater all has two control models of pressure regulation mode and timing mode when heating.It is respectively arranged with various control mode in heating process and temperature-fall period, corresponding control model can be selected according to the difference of process object, by control heater during constant temperature is kept, reach accurate constant temperature.
Description
Technical field
The present invention relates to geological sample analysis Instrument technology fields, in particular to a kind of mass spectrometric suitable for rare gas
Temperature control method.
Background technique
Rare gas have stability is good, have different characteristics the characteristics such as isotopic ratio in earth layers,
It is widely used in the every field of earth science research as a kind of natural food essence agent.To the geological sample containing rare gas at
Its argon isotope can be analyzed after reason, for determining specific geological age, this is to determine year in geoscience research and show
The important method of track.
Rare gas analysis instrument is generally made of sample preparation system and Mass Spectrometer Method system, and in addition there are electric systems
With vacuum system as support.When carrying out rare gas analysis, first by the methods of crushing or heating by gas from sample
It is released in product, subsequently enters purification system.Existing sample preparation system generally comprises the activity of Zr-Al asepwirator pump and low temperature
Charcoal cold-trap, gas after purification enter ion source, and the gas molecule of sample to be tested ionizes, and accelerate and focus bunchy.Wait divide
After beamlet of isolating passes through special slit, focuses again and fall on the ion acceptor of detection system and collect, ion connects
It receives device to be connected with measurement by magnification device, the various isotopes of rare gas can be obtained by the application facility that computer etc. matches
Ratio or content.In order to improve measurement accuracy, it is desirable that alternately measurement adds to the isotopic ratio of test sample and standard sample and by the two
To compare.It is analyzed when measurement using static schema, therefore low system background is the important guarantee of rare gas test.
System background can be reduced by the baking and purifying of system, thus must to associated conduit and outgassing component into
Row heating outgassing, the air of entrained with as far as possible discharged and taken away.Baking is the mass spectrometric important process of rare gas,
Before and after carrying out sample test, require to toast corresponding component.But in the entire system, the baking of different components requires not
Together, therefore unified roasting mode cannot be used.For example having glass window in sample disc, glass window is in rapidly heating or suddenly
When prompt drop temperature, glass window easily ruptures, and leads to whole system exposure atmosphere, causes destructive damage to instrument.For another example cold
Trap freezes according to refrigerating fluid, alcohol is contained in refrigerating fluid, therefore when carrying out outgassing to cold-trap, if failing to beat in time
Gas bleeder valve is opened, and temperature is rapidly heated, it would be possible to which ignite remaining alcohol, and dangerous situation occurs.Therefore it is required to associated components
Combined operation is set, and carries out slow heating and cooling setting.Metal valve baking temperature may not exceed design value for another example, otherwise
Gas leakage will be will lead to.Heat-activated for scarvenger and with rear outgassing, needs step-up temperature, avoids scarvenger from capturing a large amount of
Gas is fast released, and influences the molecular pump service life.And it is generally heated to 750 DEG C or so and activates to it, belongs to very
The heating of high temperature, and need persistently several hours even several days, it is necessary to monitor heated condition and the variation of relevant vacuum in real time.
Therefore, establishing a set of control system that is full-automatic, remotely can monitoring and operate is to realize high-precision40Ar/39Ar
Determine year and high-precision rare gas and analyze indispensable component part, be one for rare gas mass spectrograph efficiently, safety and
Automatically working plays vital improvement.
Summary of the invention
Technical problem to be solved by the invention is to provide one kind to be suitable for the mass spectrometric temperature control device of rare gas and temperature
Prosecutor method, the temperature control device and temperature control method operation are convenient, control is accurate, high degree of automation is, it can be achieved that rare gas mass spectrum
Instrument toasts the automatic control of outgassing, can effectively protect the mass spectrometric all parts of rare gas.
Used technical solution to solve above-mentioned technical problem:
One kind being suitable for the mass spectrometric temperature control method of rare gas, includes the following steps: that A-1, heating, A-2, constant temperature are protected
It holds, A-3, cooling；There are the two kinds of heating modes of mode and constant heating rates sintering mode that are rapidly heated in A-1 step, pass through in A-2 step
Heater keeps temperature constant, has air-cooled mode, fast-refrigerating mode and constant speed refrigerating mode Three models in A-3 step,
Keep cooling velocity constant by heater under constant speed refrigerating mode；In three steps, heater all has pressure regulation mode when heating
With two control models of timing mode.
Further, when handling sample disc or purifying pump, A-1 step uses constant heating rates sintering mode, and A-3 step is cold using constant speed
But mode is all made of pressure regulation scheme control heater when needing to heat in each step.
Further, when process instrumentation pipeline, A-1 step is adopted when needing to heat in each step using the mode that is rapidly heated
With timing scheme control heater.
Further, when handling cold-trap, if set temperature is higher than room temperature, tri- steps of A-1, A-2 and A-3 are successively carried out,
And identical processing mode is pumped using with purifying；If set temperature is lower than room temperature, A-3 step is directly carried out, and using quick
Refrigeration mode is cooled to set temperature.
Further, under pressure regulation mode, according to the difference of the actual temperature of process object and set temperature, by adjusting correspondence
The load voltage of heater, so as to adjust heating power.
Further, under timing mode, according to the difference of the actual temperature of process object and set temperature, by adjusting correspondence
The make-and-break time of the relay of heater, to adjust the operating time of the heater, so as to adjust temperature.
Further, under fast-refrigerating mode, temperature is reduced by the way that liquid nitrogen is added.
Further, sample disc and the temperature-control range of instrument pipeline are 0.0 to 350.0 DEG C.
Further, the temperature-control range of cold-trap and purifying pump is -200 DEG C to 1300 DEG C.
The utility model has the advantages that the temperature control method in the present invention, is respectively arranged with various control in heating process and temperature-fall period
Mode can select the corresponding rate of heat addition and control model according to the difference of process object, pass through control during constant temperature is kept
Heater processed reaches accurate constant temperature；The temperature-control range for setting sample disc and instrument pipeline is smaller, is that excessive temperature is led in order to prevent
Cause sample disc and instrument pipeline impaired；The temperature-control range for setting cold-trap and purifying pump is larger, is to make cold-trap and pure as far as possible
Change pump outgassing.It the composite can be widely applied to geological sample analysis Instrument technology field.
Detailed description of the invention
Fig. 1 is the schematic diagram of temperature control method in the present invention；
Fig. 2 is temperature curve when heating sample disc.
Specific embodiment
Below with reference to Fig. 1 and Fig. 2, the present invention is described further.
One kind being suitable for the mass spectrometric temperature control method of rare gas, and used temperature control device includes computer, PLC control
Device processed, pipeline heater, sample dish warmer, purifying pump heater, cold-trap heater and liquid nitrogen loader are compiled in computer
With control program, control program is by sending instruction different components mass spectrometric to rare gas using not to PLC controller
Same temperature control step, control program have the function of each heater of control, actual temperature of each component of real-time monitoring etc..
The tool of rare gas mass spectrograph employed in the present embodiment there are two sample disc, one group of purifying pump, a cold-trap with
And two groups of instrument pipelines, corresponding, the quantity of sample dish warmer and pipeline heater is two, purifying pump heater and
The quantity of cold-trap heater is one.
PLC controller controls pipeline heater by relay control panel and liquid nitrogen loader, PLC controller pass through digital-to-analogue
Conversion module controls sample dish warmer, purifying pump heater and cold-trap heater, D/A converter module and passes through pressure regulation relay
Device controls the heating power of sample dish warmer, purifying pump heater and cold-trap heater.
PLC controller monitors the temperature of sample disc and pipeline by the first thermal module, and PLC controller passes through second temperature
The temperature of module monitors purifying pump and cold-trap.The temperature that first thermal module passes through different thermocouple monitoring sample disc and pipeline
Degree, the temperature that second temperature module passes through different thermocouple monitoring purifying pump and cold-trap.
The temperature control method includes the following steps: A-1, heating, rises with the mode that is rapidly heated and two kinds of constant heating rates sintering mode
Warm mode；A-2, constant temperature are kept, and set constant temperature duration, and keep temperature constant by controlling heater；A-3, cooling have air-cooled
Mode, fast-refrigerating mode and constant speed refrigerating mode Three models, and make temperature by the way that liquid nitrogen is added under fast-refrigerating mode
It is rapidly reached target value, keeps cooling velocity constant by controlling heater under constant speed refrigerating mode.
In above three step, heater all has two control models of pressure regulation mode and timing mode when heating, and
One is set, and is all using same control model in three steps.That is in three steps or all using pressure regulation mode or
All use timing mode.
Under pressure regulation mode, according to the difference of the actual temperature of process object and set temperature, by adjusting corresponding heater
Load voltage, so as to adjust heating power, so that actual temperature is as close possible to target temperature；Under timing mode, according to place
The actual temperature of object and the difference of set temperature are managed, by adjusting the make-and-break time of the relay of corresponding heater, with adjustment
The operating time of the heater, so as to adjust temperature, so that actual temperature is as close possible to target temperature.
In above-mentioned steps, the load voltage of corresponding heater is adjusted by adjusting the output valve of D/A converter module, is led to
Relay control panel is crossed to adjust the make-and-break time of the relay of corresponding heater.
In A-1 step, under constant heating rates sintering mode, when passing through timer, such as set heating rate as 1 DEG C/min, then plus
Target temperature when hot increases by 1 DEG C per minute, until when consistent with the target temperature of setting, into A-2 step.Be rapidly heated mould
Under formula, then median is not set, directly heated to the target temperature of setting.
In A-2 step, when using timing mode, if temperature is lower than target temperature, elevated the temperature by heater, to
After reaching target temperature, by controlling the operating time of heater, to keep constant temperature；When using pressure regulation mode, if temperature is low
When target temperature, then increase the output power of heater, so that actual temperature is increased to target temperature, if temperature is higher than target
When temperature, then the output power for reducing heater is even switched off heater, so that actual temperature is reduced to target temperature.Work as constant temperature
When duration reaches setting duration, into A-3 step or terminate heating.
In A-3 step: air-cooled mode is to close natural cooling after heater；Under fast-refrigerating mode, by the way that liquid is added
Nitrogen reduces temperature；Under constant speed refrigerating mode, if rate of temperature fall is higher than setting speed, rate of temperature fall can be slowed down by heating, work as drop
When warm rate is lower than setting speed, then cooled down by the way of natural cooling；When not requiring rate of temperature fall, that is, can be used
The mode of natural cooling.
In the present embodiment, the temperature-control range of sample disc and instrument pipeline is 0 to 350 DEG C, the temperature control model of cold-trap and purifying pump
Enclose is -200 DEG C to 1300 DEG C.
When handling sample disc or purifying pump, A-1 step uses constant heating rates sintering mode, and A-3 step uses constant speed refrigerating mode.
And in three steps, if desired heating is all made of pressure regulation scheme control heater.In A-3 step, when target temperature is down to 30
DEG C when, illustrate to complete entire temperature control process, can close sample dish warmer or purifying pump heater.
When process instrumentation pipeline, A-1 step uses air-cooled mode using the mode that is rapidly heated, A-3 step.If in each step
It needs to heat and is all made of timing scheme control heater.
Handle cold-trap when, if set temperature be higher than room temperature, successively carry out tri- steps of A-1, A-2 and A-3, and using with
Purifying pumps identical processing mode；If set temperature is lower than room temperature, A-3 step is directly carried out, and use fast-refrigerating mode,
So that temperature is reached set temperature, in this case, cooling, constant temperature, heating is substantially to the treatment process of cold-trap.
In the present embodiment, room temperature is generally 20 to 25 DEG C.
In above-mentioned steps, slow heating-constant temperature holding-Slow cooling temperature is used to sample disc, purifying pump and cold-trap
Prosecutor method, the effective protection glass window of sample disc are effectively prevented because of sharply outgassing caused by being rapidly heated, to instrument
Pipeline is handled in lesser temperature-control range, protects metal valve.
Illustrate by taking the processing to sample disc as an example below:
Baking outgassing temperature needs to reach 150 DEG C, therefore using the lower range mode and thermocouple of degree of precision to heating
Device carries out accurate thermometric.To protect the glass window in sample disc, using slow heating-constant temperature holding-Slow cooling temperature control
Method, and its heating rate (such as being set greater than or be equal to 1min/ DEG C) can be set according to actual needs, heater is disk
Formula heater.
After installing heater, for the first time using needing first adjust its pid parameter, obtain pid parameter be respectively 6,
1052,159, therefore the pid parameter for heating up and cooling down is set as 6,1052,159.In constant temperature, in order to reach more accurately
Thermostatic control sets pid parameter as 8,1052,159.
Sample disc realizes temperature-controllable in heating, constant temperature and temperature-fall period as a result, and variation range is at ± 1 DEG C, heating
Curve such as Fig. 2, ordinate of orthogonal axes numerical value is followed successively by 20,55,90,125 and 160 in figure, and target temperature is linearity curve, target temperature
That is set temperature, and actual temperature is the curve stirred up and down along target temperature profile.
In conjunction with attached drawing, the embodiments of the present invention are described in detail above, but the present invention is not limited to above-mentioned embodiment party
Formula within the scope of knowledge possessed by those of ordinary skill in the art can also be before not departing from present inventive concept
Put that various changes can be made.
Claims (9)
1. one kind is suitable for the mass spectrometric temperature control method of rare gas, which comprises the steps of: A-1, heating, A-
2, constant temperature is kept, A-3, cooling；There is the two kinds of heating modes of mode and constant heating rates sintering mode that are rapidly heated, A-2 step in A-1 step
Keep temperature constant by heater in rapid, with air-cooled mode, fast-refrigerating mode and three kinds of constant speed refrigerating mode in A-3 step
Mode keeps cooling velocity constant under constant speed refrigerating mode by heater；In three steps, heater all has tune when heating
Two control models of die pressing type and timing mode.
2. according to claim 1 a kind of suitable for the mass spectrometric temperature control method of rare gas, it is characterised in that: processing sample
When product disk or purifying pump, A-1 step uses constant heating rates sintering mode, and A-3 step uses constant speed refrigerating mode, needs to add in each step
Pressure regulation scheme control heater is all made of when hot.
3. according to claim 2 a kind of suitable for the mass spectrometric temperature control method of rare gas, it is characterised in that: processing instrument
When device pipeline, A-1 step is all made of timing scheme control heater using the mode that is rapidly heated when needing to heat in each step.
4. according to claim 2 a kind of suitable for the mass spectrometric temperature control method of rare gas, it is characterised in that: processing is cold
When trap, if set temperature is higher than room temperature, tri- steps of A-1, A-2 and A-3 are successively carried out, and pump identical place using with purifying
Reason mode；If set temperature is lower than room temperature, A-3 step is directly carried out, and set temperature is cooled to using fast-refrigerating mode.
5. according to claim 1 a kind of suitable for the mass spectrometric temperature control method of rare gas, it is characterised in that: pressure regulation mould
Under formula, according to the difference of the actual temperature of process object and set temperature, by adjusting the load voltage of corresponding heater, thus
Adjust heating power.
6. according to claim 1 a kind of suitable for the mass spectrometric temperature control method of rare gas, it is characterised in that: timing mould
Under formula, according to the difference of the actual temperature of process object and set temperature, by adjusting the on-off of the relay of corresponding heater
Time, to adjust the operating time of the heater, so as to adjust temperature.
7. according to claim 1 a kind of suitable for the mass spectrometric temperature control method of rare gas, it is characterised in that: quickly system
Under cold mode, temperature is reduced by the way that liquid nitrogen is added.
8. according to claim 3 a kind of suitable for the mass spectrometric temperature control method of rare gas, it is characterised in that: sample disc
Temperature-control range with instrument pipeline is 0.0 to 350.0 DEG C.
A kind of be suitable for the mass spectrometric temperature control method of rare gas 9. according to claim 4, it is characterised in that: cold-trap and
The temperature-control range of purifying pump is -200 DEG C to 1300 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114709128A (en) * | 2022-03-22 | 2022-07-05 | 厦门大学 | Heating temperature control device of miniaturized mass spectrum ion source |
| CN114840040A (en) * | 2022-04-20 | 2022-08-02 | 天津国科医工科技发展有限公司 | ESI source auxiliary air temperature control system based on controllable silicon |
| CN117804056A (en) * | 2024-02-29 | 2024-04-02 | 成都千麦医学检验所有限公司 | Temperature-changing incubator for enzyme-linked immunosorbent assay |
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| CN114709128A (en) * | 2022-03-22 | 2022-07-05 | 厦门大学 | Heating temperature control device of miniaturized mass spectrum ion source |
| CN114840040A (en) * | 2022-04-20 | 2022-08-02 | 天津国科医工科技发展有限公司 | ESI source auxiliary air temperature control system based on controllable silicon |
| CN117804056A (en) * | 2024-02-29 | 2024-04-02 | 成都千麦医学检验所有限公司 | Temperature-changing incubator for enzyme-linked immunosorbent assay |
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