CN108226322A - A kind of low temperature concentrating instrument and control method - Google Patents
A kind of low temperature concentrating instrument and control method Download PDFInfo
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- CN108226322A CN108226322A CN201711318589.XA CN201711318589A CN108226322A CN 108226322 A CN108226322 A CN 108226322A CN 201711318589 A CN201711318589 A CN 201711318589A CN 108226322 A CN108226322 A CN 108226322A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
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Abstract
The present invention is suitable for volatile organic compounds sample gas and concentrates field, disclose a kind of low temperature concentrating instrument and control method, including gas chromatography mass spectrometer, it further includes for the sample injection unit for sample gas sample introduction, for detaching the processing unit of volatile organic compounds in sample gas impurity and concentrating sample gas, purge unit for the monitoring unit for detecting pipeline gas flow rate and manifold pressure and for shifting volatile organic compounds, processing unit includes the first cold-trap for removing moisture in sample gas, third cold-trap for the second cold-trap for removing carbon dioxide in sample gas and for concentrating volatile organic compounds, first cold-trap, second cold-trap connects setting with third cold-trap.Provided by the present invention a kind of low temperature concentrating instrument and control method, may separate out impurity in sample gas, and the volatile organic compounds component in enriched sample gas carries out concentration to sample gas, improves detection and analysis speed, promote working efficiency.
Description
Technical field
The invention belongs to volatile organic compounds sample gas concentration field more particularly to a kind of low temperature concentrating instrument and controls
Method processed.
Background technology
Volatile organic compounds (VOCs) is the important component of air, passes through VOCs during studying different pollutions
There is significant meaning in level of pollution, contamination characteristics and source etc., so to big to urban air-quality and gray haze contamination control
Volatile organic compounds is monitored particularly important in real time in gas.At present, it is mainly completed by chromatography in air
The detection of volatile organic compounds, the volatile organic compounds type in air is various, and concentration is low, if high and low dense
When degree sample flows through same path, concentration samples need pre-concentration 100,000 times, can be only achieved expected detection result, so as to make
Into temporal waste, therefore in order to promote working efficiency, enrichment concentration need to be carried out to sample.
Invention content
It is an object of the invention to which above-mentioned the deficiencies in the prior art is overcome to provide a kind of low temperature concentrating instrument and control method,
It may separate out impurity component in sample gas, and pass through volatile organic in the selectable enriched sample gas of temperature action
Polymer component carries out concentration to sample gas, improves detection and analysis speed, promotes working efficiency.
The technical scheme is that：A kind of low temperature concentrating instrument, including gas chromatography mass spectrometer, further includes and is connected by pipeline
What is connect is used for the sample injection unit for sample gas sample introduction, has for detaching volatility in sample gas impurity and concentrating sample gas
The processing unit of machine compound volatilizees for the monitoring unit that detects pipeline gas flow rate and manifold pressure and for shifting
The purge unit of property organic compound, is provided with parts more than first, the place between the sample injection unit and the processing unit
Multiple-way valve is provided between reason unit and the gas chromatography mass spectrometer, is set between the monitoring unit and the processing unit
There are a parts more than second, the processing unit is included for removing the first cold-trap of moisture in sample gas, for removing sample gas
Second cold-trap of carbon dioxide and the third cold-trap for concentrating volatile organic compounds in body, it is first cold-trap, described
Second cold-trap connects setting with the third cold-trap.
Specifically, the sample injection unit includes injection port and sampling valve, and the injection port is provided at least two, it is described into
One end of sample valve is connected with the injection port, and the other end of the sampling valve is communicated in the parts more than first.
Specifically, the first metal tube to circulate for supplied gas, first metal tube are provided in first cold-trap
Winding setting, second cold-trap are provided with the second metal tube to circulate for supplied gas, and the second metal tube winding is set,
The third metal tube to circulate for supplied gas is provided in the third cold-trap, the third metal tube bending is provided with deformation knot
Structure.
Specifically, it tells in the second metal tube and fills filled with silica gel powder or/and bead in first metal tube
There is not adsorption moisture but there are the Tenax adsorbents of adsorption capacity to volatile organic compounds.
Specifically, the first heating member is provided in first cold-trap, first metal tube is around on the heating member,
The second heating member is provided in second cold-trap, second metal tube is around on second heating member, and the third is cold
It being provided in trap for the heating tube for heat gas circulation, the heating pipe diameter is more than the diameter of the third metal tube,
And it is placed on the heating tube in the third metal tube.
Specifically, the multiple-way valve includes the first multiple-way valve and the second multiple-way valve, and first multiple-way valve is set on described the
Between parts more than one and first cold-trap, second multiple-way valve is set between first cold-trap and second cold-trap,
First multiple-way valve and described cold-trap valve is additionally provided with more than first between parts.
Specifically, in first multiple-way valve and the external setting having heaters of second multiple-way valve.
Specifically, the monitoring unit includes pressure sensor and mass flowmenter, the pressure sensor and the matter
The inlet parallel of amount flowmeter is communicated in the parts more than second, and the outlet of the mass flowmenter is connected with vacuum pump.
Specifically, the purge unit is included for the gas washing source of scavenging pipeline and for low temperature concentrating instrument interior change
It does the standard gas air source of detection compensation, the gas washing source and described is provided with gas washing valve more than first between parts and for adjusting flow
Flow valve, the standard gas air source and it is described be provided between parts more than first for control internal standard standard gas switch internal standard valve..
The present invention also provides a kind of for controlling the control method of above-mentioned low temperature concentrating instrument, include the following steps：
S1:Injection port is chosen, starts to freeze the first cold-trap, when the temperature of the first cold-trap is chilled to set point and stablizes one
After the section time, purge unit is blown into pipeline by the flow velocity and time of setting；
S2：After the completion of purging, by sample inlet be loaded into internal standard, purge unit by setting flow velocity enter the first cold-trap until
Stop after reaching aim parameter；
S3:Sample gas is by the flow velocity of setting and time purging filling line；
S4：After the completion of sample purge pipeline, sample gas is loaded into the first cold-trap by the flow velocity of setting, until the sample being loaded into
Gas stops after reaching scheduled aim parameter；
S5：Purge unit is removed sample remaining in pipeline, then, is purged by the flow velocity of setting and time scavenging pipeline
Unit purges the first cold-trap by the flow velocity of setting and time, empties empty gas and water remaining in the first cold-trap and carbon dioxide, and same
When freeze second cold-trap；
S6：After purging, after the second cold-trap is chilled to specified range and keeps stablizing, the first cold-trap is preheated；
S7:After the completion of the first cold-trap preheating, the first multiple-way valve is adjusted, purge unit is blown by the flow velocity and time of setting
It sweeps, volatile organic compounds is transferred to the second cold-trap, and before volatile organic compounds transfer terminates from the first cold-trap
Two minutes, third cold-trap is freezed, and freezing state is kept to stablize；
S8:Set temperature is heated to the second cold-trap, purge unit purges the second cold-trap by the flow velocity of setting and time, will
Carbon dioxide separation in second cold-trap in sample gas, the second cold-trap continues to heat after carbon dioxide separation, and volatility is had
Machine compound is transferred to from the second cold-trap in third cold-trap, the first cold-trap is toasted by the temperature and time of setting, simultaneously
Purge unit purges the first cold-trap；
S9:In second cold-trap after the completion of volatile organic compounds transfer, start gas chromatography mass spectrometer, third cold-trap exists
Volatile organic compounds is injected gas chromatography mass spectrometer by transient heating in the time specified according to set time；
S10:After volatile organic compounds has been injected, sample introduction terminates, cold by the temperature and time baking second of setting
Trap, while purge unit purges the second cold-trap；
S11:Gas chromatography mass spectrometer delay start, purge unit purging sample introduction pipeline simultaneously empty, and make low temperature concentrating instrument pipe
The state of temperature and gas flow paths and state consistency when not working in road；
S12:Out of service after gas chromatography mass spectrometer delay start, system is by next sample in automatic running sequence
Product sample introduction, repeats the above steps, until the last one sample end of run.
A kind of low temperature concentrating instrument provided by the present invention and control method can carry out at effective early period sample gas
Reason, is carried out dehydrating sample gas using vapour pressure, the carbon dioxide in sample gas is isolated using temperature difference, is avoided
Influence of the impurity to sample gas testing result improves the accuracy of sample gas testing result, and to waving in sample gas
Hair property organic compound is concentrated, and improves the detection and analysis speed of sample gas, promotes working efficiency.
Description of the drawings
It to describe the technical solutions in the embodiments of the present invention more clearly, below will be to needed in the embodiment
Attached drawing is briefly described, it should be apparent that, the accompanying drawings in the following description is only some embodiments of the present invention, for ability
For the those of ordinary skill of domain, without creative efforts, it can also be obtained according to these attached drawings other attached
Figure.
Fig. 1 is a kind of structure diagram of low temperature concentrating instrument provided in an embodiment of the present invention；
Fig. 2 is a kind of right view of low temperature concentrating instrument provided in an embodiment of the present invention；
Fig. 3 is a kind of left view of low temperature concentrating instrument provided in an embodiment of the present invention；
Fig. 4 is the structure diagram of the first cold-trap in a kind of low temperature concentrating instrument provided in an embodiment of the present invention；
Fig. 5 is the structure diagram of the second cold-trap in a kind of low temperature concentrating instrument provided in an embodiment of the present invention；
Fig. 6 is the structure diagram of third cold-trap in a kind of low temperature concentrating instrument provided in an embodiment of the present invention.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, it is right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
It should be noted that when element is referred to as " being fixed on " or " being set to " another element, it can be directly another
On one element or it may be simultaneously present centering elements.When an element is known as " being connected to " another element, it can
To be directly to another element or may be simultaneously present centering elements.
Only it is relative concept each other it should also be noted that, the orientation term such as left and right, upper and lower in the embodiment of the present invention
Or using the normal operating condition of product as reference, and should not be regarded as restrictive.
As shown in Figures 1 to 6, a kind of low temperature concentrating instrument provided in an embodiment of the present invention, including gas chromatography mass spectrometer 5,
It further includes and is used for the sample injection unit 1 for sample gas sample introduction, by what pipeline connected for detaching sample gas impurity and concentration
The processing unit 2 of volatile organic compounds, the monitoring for detecting pipeline gas flow rate and manifold pressure in sample gas
Unit 3 and the purge unit 4 for shifting volatile organic compounds, between the sample injection unit 1 and the processing unit 2
Parts 6 more than first are provided with, multiple-way valve 7, the prison are provided between the processing unit 2 and the gas chromatography mass spectrometer 5
Parts 8 more than second are provided between control unit 3 and the processing unit 2, the processing unit 2 includes removing sample gas
It is first cold-trap 21 of middle moisture, organic for the second cold-trap 22 for removing carbon dioxide in sample gas and for concentrating volatility
The third cold-trap 23 of compound, first cold-trap 21, the second cold-trap 22 connect setting with third cold-trap 23.During work, first
Cold-trap 21 captures water, carbon dioxide and the volatile organic compounds condensation in sample gas simultaneously under the action of refrigerant
Absorption has different steam on silica gel powder or/and bead, using water, carbon dioxide and volatile organic compounds three
Pressure is dehydrated sample gas, then carbon dioxide and volatile organic compounds are transferred in the second cold-trap 22, passes through system
The effect of cryogen makes carbon dioxide and volatile organic compounds be condensed to capture and adsorb in Tenax adsorbents, utilizes temperature difference
Carbon dioxide is made to become gaseous state, carbon dioxide is isolated, then volatile organic compounds is transferred in third cold-trap 23, is passed through
The effect of refrigerant carries out concentration to volatile organic compounds, after the completion of concentration, to the volatile organic after concentration
The heating heating of object moment is closed, volatile organic compounds is injected into gas chromatography mass spectrometer 5, is detected analysis.The low temperature is dense
Contracting instrument can effectively carry out sample gas processing early period, remove water and carbon dioxide in sample gas, avoid depositing for impurity
Testing result is being influenced, while concentration can also be carried out to volatile organic compounds, to refrigerant when reducing freezing
Energy consumption when consumption and heating, reduces production cost, improves gas chromatography mass spectrometer 5 and tests and analyzes speed, promotes work
Efficiency.
Specifically, the third cold-trap 23 can carry out cryogenic refrigeration.
Specifically, the sample injection unit 1 includes injection port 11 and sampling valve 12, and the injection port 11 is provided at least two
A, one end of the sampling valve 12 is connected with the injection port 11, and the other end parallel communication of each sampling valve 12 is in described
Parts 6 more than first.
In the embodiment of the present invention, there are four the settings of injection port 11, and parts more than first 6 are logical for circle eight, and parts more than second 8 are circle
Five is logical.
Specifically, first cold-trap 21 has the first refrigerating chamber 211, and the second cold-trap 22 has the second refrigerating chamber 212, the
Three cold-traps 23 have third refrigerating chamber 213, and the first refrigerating chamber 211, the second refrigerating chamber 212 and third refrigerating chamber 213 are sealing
Refrigerating chamber.
Specifically, first cold-trap 21, which has, is used to arrange for the first inlet 212 of refrigerant injection and for refrigerant
The first discharge port 213 gone out, the second cold-trap 22, which has, to be used to arrange for the second inlet 222 of refrigerant injection and for refrigerant
The second outlet 223 gone out, third cold-trap 23, which has, to be used to discharge for the third inlet 232 of refrigerant injection and for refrigerant
Third outlet 233.
Specifically, the first temperature-sensing element 216 for detecting temperature, the second cold-trap 22 are provided in first cold-trap 21
Inside it is provided with the third sense being provided in the second temperature-sensing element 226 and third cold-trap 23 for detecting temperature for detecting temperature
Warm element 236 detects the temperature of the first refrigerating chamber 211 by the first temperature-sensing element 216, by the second temperature-sensing element 226 come
The second refrigerating chamber 212 is detected, the temperature of third refrigerating chamber 213 is detected by third temperature-sensing element 236, then via control
Software controls refrigerant stream according to the temperature for collecting the first refrigerating chamber 211, the second refrigerating chamber 212 and third refrigerating chamber 213
The size of amount is to maintain the first refrigerating chamber 211, temperature is stablized in the second refrigerating chamber 212 and third refrigerating chamber 213, practical application
In, refrigerant can be liquid nitrogen, liquid helium or liquid oxygen etc..
Specifically, it is provided in first cold-trap 21 for the first metal tube 215 for sample gas circulation, described the
The winding setting of one metal tube 215, second cold-trap 22 are provided with for the second metal tube 225 for sample gas circulation, institute
The winding setting of the second metal tube 225 is stated, is provided in the third cold-trap 23 for the third metal tube for sample gas circulation
235, the bending of third metal tube 235 is provided with deformation structure.
In practical application, in order to ensure that the early period of sample gas, processing work effectively carried out, the first metal tube 215, second
Metal tube 225 and third metal tube 235 need to possess enough length, and are to reduce the first metal tube 215, the second metal tube
225 and the space of third metal tube 235, reduce the first refrigerating chamber 211, the second refrigerating chamber 212 and third refrigerating chamber 213
First metal tube 215 and the second metal tube 225 are made winding design by volume, and third metal tube 235 is made curved design, can be reduced
The consumption of first refrigerating chamber 211, the second refrigerating chamber 212 and third refrigerating chamber 213 in freezing to refrigerant, can also reduce first
Refrigerating chamber 211, the energy consumption of the second refrigerating chamber 212 and third refrigerating chamber 213 when heated.
In the embodiment of the present invention, as shown in Figures 4 and 5, the first metal tube 215 and the second metal tube 225 are set in " helical form "
It puts, as shown in fig. 6, the deformation structure of third metal tube 235 is set in " U-shaped shape ".
Specifically, 215 and second metal tube 225 of the first metal tube be silanization metal tube, 215 He of the first metal tube
The caliber of second metal tube 225 is 1/8 inch, and the third metal tube 235 is capillary column.
Specifically, in first metal tube 215 the second metal tube 225 is told filled with silica gel powder or/and bead
The interior Tenax adsorbents for being filled with not adsorption moisture but having adsorption capacity to volatile organic compounds, can be according to detection sample
The volatile organic compounds of various concentration determines the dosage of Tenax adsorbents in gas, silica gel powder, bead and
Tenax adsorbents are common agents, can be easy to purchase.
Specifically, the first heating member 214 is provided in first cold-trap 21, first metal tube 215 is around in described
On first heating member 214, the second heating member 224 is provided in second cold-trap 22, second metal tube 225 is around in described
On second heating member 224, it is provided in the third cold-trap 23 for the heating tube 234 for heat gas circulation, the heating
234 diameter of pipe is more than the diameter of the third metal tube 235, and the heating tube 234 is placed in the third metal tube 235.
First metal tube 215 is wound on the first heating member 214, the second metal tube 225 is wound on the second heating member 224, the
Three metal tubes 235 are set in heating tube 234, ensure heating process the first metal tube 215, the second metal tube 225 and third metal
Pipe 235 is heated evenly.
In the embodiment of the present invention, as shown in Figs. 4-6, is provided between the first metal tube 215 and the first heating member 214
One asbestos insulating layer 218 is provided with the second asbestos insulating layer 228 between second metal tube 225 and the second heating member 224, make
One metal tube 215 and the first metal tube 225 are heated evenly in heating process, are provided in third cold-trap 23 by 237 He of thermal insulation board
The incubation cavity that insulation cover 238 is combined into, it is ensured that temperature in third refrigerating chamber 213 can be kept to put down during third 23 cryogenic refrigeration of cold-trap
Weighing apparatus.
In the embodiment of the present invention, the heating tube 234 is tetrafluoroethene pipe, and caliber is 1/8 inch, and the heating tube 234 is logical
Enter to have the resolution gas of heating can be heated to third metal tube 235.
Specifically, first heating member 214 can be heating board, heat-generating pipe or heat coil etc., and the second heating member 224 can
For heating board, heat-generating pipe or fever circle etc..
In the embodiment of the present invention, the first heating member 214 and the second heating member 224 are heat coil, and set in " helical form "
It puts, it is made to possess enough power in certain space.
Specifically, first cold-trap 21 is also provided with the first temperature controller 217 for disconnecting protection, the second cold-trap 22
The second temperature controller 227 for disconnecting protection is also provided with, when temperature is excessively high in the first refrigerating chamber 211, the second refrigerating chamber 212
When stop heating, silica gel powder, bead and Tenax adsorbents can be prevented because temperature is excessively high so as to cause failure.
Specifically, the multiple-way valve 7 includes the first multiple-way valve 71 and the second multiple-way valve 72, and first multiple-way valve 71 is set on
Between 6 and first cold-trap 21 of parts more than first, second multiple-way valve 72 is set on 21 and second cold-trap of the first cold-trap
Between 22, make the low temperature concentrating instrument that can form multiple accesses, can also be set between first multiple-way valve 71 and parts more than first 6
There is cold-trap valve 9.
In the embodiment of the present invention, as shown in Figure 1, the first multiple-way valve 71 and the second multiple-way valve 72 are six-way valve.
Specifically, heater is may be provided in the outside of 71 and second multiple-way valve 72 of the first multiple-way valve (not mark in figure
Note), by being heated to the first multiple-way valve 71 and the second multiple-way valve 72, the absorption to sample gas can be reduced, conducive to removing
Sample gas remains.
Specifically, the monitoring unit 3 includes pressure sensor 31 and mass flowmenter 32,31 He of pressure sensor
The inlet parallel of mass flowmenter 32 is communicated in parts 8 more than second, and the outlet of the mass flowmenter 32 is connected with vacuum
Pump 33, pressure sensor 31 in real time read low temperature concentrating instrument in pressure change, mass flowmenter 32 be used for sample into
Metering when sample and sample shift, convenient for understanding the working condition of low temperature concentrating instrument.Vacuum pump 33 can be used for the low temperature concentrating instrument
Leak test, vacuumize, the transfer of sample feeding, sample and the work such as scavenging pipeline.
Specifically, the purge unit 4 is included for the gas washing source 411 of scavenging pipeline and for inside to low temperature concentrating instrument
The standard gas air source 421 of detection compensation is done in variation.
Specifically, the gas in the gas washing source 411 can be nitrogen, helium or zero level air etc..
Specifically, as shown in Figure 1, the parts more than second 8 can also be connected with the drain 10 for discharge gas, this is put
It eats dishes without rice or wine to may be provided with blow valve 101 between the parts more than second 8.
In the embodiment of the present invention, as shown in Figure 1, may be provided with to adjust between the first multiple-way valve 71 and parts more than second 8
The MFC valves 11 of throttle body flow.
Specifically, gas washing valve 412 is provided between the gas washing source 411 and the parts more than first 6 and is flowed for adjusting
The flow valve 413 of amount is provided with that internal standard standard gas is controlled to switch between the standard gas air source 421 and the parts more than first 6
Internal standard valve 422.
The present invention also provides a kind of control methods, for controlling above-mentioned low temperature concentrating instrument, include the following steps：
S1:Injection port 11 is chosen, starts to freeze the first cold-trap 21, when the temperature of the first cold-trap 21 is chilled to set point simultaneously
After a period of stabilisation, the first multiple-way valve 71 and the second multiple-way valve 72 are adjusted, opens internal standard valve 422, internal standard standard gas is by setting
Flow velocity and time are blown into pipeline, and for the range of the cryogenic temperature of the first cold-trap 21 in -250 DEG C to -100 DEG C, preferred value is -150
DEG C, it is possible to understand that ground, the cryogenic temperature of the first cold-trap 21 may be other suitable values.
In the step, the flow velocity that internal standard standard gas is set as 100 ml/mins, the purge time that internal standard standard gas is set as 10s,
If 20% of the actual flow velocity of internal standard standard gas less than setting flow velocity, and do not reach aim parameter, then in the monitoring of control software
Under, low temperature concentrating instrument is out of service.
S2：After the completion of internal standard purging, the first multiple-way valve 71 is adjusted, is loaded into internal standard standard gas, internal standard standard gas is by the flow velocity set
Stop after into the first cold-trap 21 until reaching aim parameter, target effect is to be turned into compensation inspection to the change of low temperature concentration systems in addition
It surveys, can significantly reduce error, without correcting data.
S3:The first multiple-way valve 71 and the second multiple-way valve 72 are adjusted, sample gas is by the flow velocity of setting and time purging purging
Pipeline excludes the influence of other factors, ensures the precision of the testing result of sample gas.
In the step, the flow velocity that sample gas is set as 100 ml/mins, the purge time that sample gas is set as 10s,
If 20% of the actual flow velocity of sample gas less than setting flow velocity, and do not reach aim parameter, then in the monitoring of control software
Under, low temperature concentrating instrument is out of service.
S4：After the completion of sample purge pipeline, the first multiple-way valve 71 is adjusted, sample gas is cold by the flow velocity loading first of setting
Trap 21, until the sample gas being loaded into stops after reaching scheduled aim parameter, sample gas is condensed in the first cold-trap 21 and catches
It catches.
S5：The first multiple-way valve 71 is adjusted, the gas in gas washing source 411 removes pipe by the flow velocity of setting and time scavenging pipeline
Remaining sample in road then, adjusts the first multiple-way valve 71 again, and the gas in gas washing source 411 is blown by the flow velocity and time of setting
The first cold-trap 21 is swept, empties empty gas and water remaining in the first cold-trap 21 and carbon dioxide, and freeze second cold-trap simultaneously
22；
S6：After purging, after the second cold-trap 22 is chilled to specified range and keeps stablizing, the first cold-trap 21 is heated,
The range of the cryogenic temperature of second cold-trap 22 can be in -25 DEG C to -3 DEG C, and preferred value is -10 DEG C, it is possible to understand that ground, the second cold-trap
22 cryogenic temperature may be other suitable values.
S7:The heating temperature range of first cold-trap 21 can be in 15 DEG C to 40 DEG C, and preferred value is 30 DEG C, it is possible to understand that ground,
The heating temperature of first cold-trap 21 may be other suitable values, after the completion of the heating of the first cold-trap 21, adjust the first multiple-way valve
71 and second multiple-way valve 72, the gas in gas washing source 411 is by the flow velocity of setting and time purging, by volatile organic compounds from the
One cold-trap 21 is transferred to the second cold-trap 22, and two minutes before volatile organic compounds transfer terminates, to third cold-trap 23
It is freezed, and freezing state is kept to stablize, if volatile organic compounds transfer time is less than two minutes, stopped to third
Cold-trap 23 is freezed.
In the step, the third cold-trap 23 is cold focusing, the range of cryogenic temperature can in -220 DEG C to -60 DEG C,
Preferred value is -165 DEG C, it is possible to understand that ground, the cryogenic temperature of third cold-trap 23 may be other suitable values.
S8:Set temperature is heated to the second cold-trap 22, the heating temperature range of the second cold-trap 22 can be at -25 DEG C to -3 DEG C
Interior, preferred value is -10 DEG C, it is possible to understand that ground, the heating temperature of the second cold-trap 22 may be other suitable values, adjust first
71 and second multiple-way valve 72 of multiple-way valve, the gas in gas washing source 411 purges the second cold-trap 22 by the flow velocity of setting and time, by second
Carbon dioxide separation in cold-trap 22 in sample gas, the second cold-trap 22 continues to heat after carbon dioxide separation, and volatility is had
Machine compound is transferred to from the second cold-trap 22 in third cold-trap 23, and the first cold-trap 21 is dried by the temperature and time of setting
It is roasting, while the gas in gas washing source 411 purges the first cold-trap 21, and the first cold-trap 21 is cleaned.
S9:In second cold-trap 22 after the completion of volatile organic compounds transfer, it is logical to adjust the first multiple-way valve more than 71 and second
Valve 72 starts gas chromatography mass spectrometer 5, the interior transient heating at the appointed time of third cold-trap 23, while the gas in gas washing source 411
Third cold-trap 23 is purged, volatile organic compounds is injected to gas chromatography mass spectrometer 5 according to set time.
S10:After volatile organic compounds has been injected, sample introduction terminates, and adjusts the first multiple-way valve 71 and the second multiple-way valve
72, the second cold-trap 22 is toasted, while the gas in gas washing source 411 purges the second cold-trap 22 by the temperature and time of setting, to second
Cold-trap 22 is cleaned.
S11:5 delay start of gas chromatography mass spectrometer adjusts the first multiple-way valve 71 and the second multiple-way valve 72, gas washing source 411
Gas purge pipeline in the low temperature concentrating instrument, pipeline is cleaned, makes temperature and gas stream in the pipeline of low temperature concentrating instrument
The state in dynamic path and state consistency when not working.
S12:Out of service after 5 delay start of gas chromatography mass spectrometer, system will be next in automatic running sequence
Sample feeding repeats the above steps, until the last one sample end of run.
A kind of control method of low temperature concentrating instrument provided by the present invention can effectively carry out at early period sample gas
Reason, the water in sample gas is removed using vapour pressure, is removed the carbon dioxide in sample gas using temperature difference, is avoided impurity
In the presence of testing result is influenced, while concentration can also be carried out to volatile organic compounds, accelerate gas chromatography mass spectrometer
Speed is tested and analyzed, improves working efficiency.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modification, equivalent replacement or improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of low temperature concentrating instrument, including gas chromatography mass spectrometer, which is characterized in that further include and be used to supply by what pipeline connected
The sample injection unit of sample gas sample introduction, for detaching volatile organic compounds in sample gas impurity and concentrating sample gas
Processing unit, for the monitoring unit that detects pipeline gas flow rate and manifold pressure and for shifting volatile organic compound
The purge unit of object is provided with parts more than first, the processing unit and institute between the sample injection unit and the processing unit
It states and is provided with multiple-way valve between gas chromatography mass spectrometer, be provided with second more and lead between the monitoring unit and the processing unit
Part, the processing unit are included for removing the first cold-trap of moisture in sample gas, for removing titanium dioxide in sample gas
Second cold-trap of carbon and the third cold-trap for concentrating volatile organic compounds, first cold-trap, second cold-trap and
The third cold-trap connection setting.
2. a kind of low temperature concentrating instrument as described in claim 1, which is characterized in that the sample injection unit includes injection port and sample introduction
Valve, the injection port are provided at least two, and one end of the sampling valve is connected with the injection port, the sampling valve it is another
End is communicated in the parts more than first.
3. a kind of low temperature concentrating instrument as described in claim 1, which is characterized in that be provided with to supply in first cold-trap
First metal tube of body circulation, the first metal tube winding setting, second cold-trap are provided with what is circulated for supplied gas
Second metal tube, the second metal tube winding are set, and the third gold to circulate for supplied gas is provided in the third cold-trap
Belong to pipe, the third metal tube bending is provided with deformation structure.
4. a kind of low temperature concentrating instrument as claimed in claim 3, which is characterized in that silica white is filled in first metal tube
Grain or/and bead are told and not adsorption moisture are filled in the second metal tube but has adsorption capacity to volatile organic compounds
Tenax adsorbents.
5. a kind of low temperature concentrating instrument as claimed in claim 3, which is characterized in that be provided with the first heating in first cold-trap
Part, first metal tube are around on the heating member, and the second heating member, second metal are provided in second cold-trap
Pipe is around on second heating member, is provided in the third cold-trap for the heating tube for heat gas circulation, described to add
Heat pipe diameter is more than the diameter of the third metal tube, and is placed on the heating tube in the third metal tube.
6. a kind of low temperature concentrating instrument as described in claim 1, which is characterized in that the multiple-way valve includes the first multiple-way valve and the
Two multiple-way valves, first multiple-way valve are set between the parts more than first and first cold-trap, and second multiple-way valve is set
Between first cold-trap and second cold-trap, first multiple-way valve and it is described be additionally provided between parts more than first it is cold
Trap valve.
7. a kind of low temperature concentrating instrument as claimed in claim 6, which is characterized in that in first multiple-way valve and described more than second
The external setting having heaters of port valve.
8. a kind of low temperature concentrating instrument as described in claim 1, which is characterized in that the monitoring unit include pressure sensor and
The inlet parallel of mass flowmenter, the pressure sensor and the mass flowmenter is communicated in the parts more than second, described
The outlet of mass flowmenter is connected with vacuum pump.
9. a kind of low temperature concentrating instrument as described in claim 1, which is characterized in that the purge unit is included for scavenging pipeline
Gas washing source and for low temperature concentrating instrument interior change do detection compensation standard gas air source, the gas washing source and more than described first
It is provided with gas washing valve and the flow valve for adjusting flow between parts, the standard gas air source and described is set between parts more than first
It is equipped with the internal standard valve for internal standard standard gas to be controlled to switch.
A kind of a kind of 10. control method, which is characterized in that control low temperature concentration as in one of claimed in any of claims 1 to 9
Instrument includes the following steps：
S1:Injection port is chosen, starts to freeze the first cold-trap, when the temperature of the first cold-trap is chilled to set point and stablizes one section
Between after, purge unit is blown into pipeline by the flow velocity and time of setting；
S2：After the completion of purging, internal standard is loaded by sample inlet, purge unit enters the first cold-trap until reaching by the flow velocity of setting
Stop after aim parameter；
S3:Sample gas is by the flow velocity of setting and time purging filling line；
S4：After the completion of sample purge pipeline, sample gas is loaded into the first cold-trap by the flow velocity of setting, until the sample gas being loaded into
Stop after reaching scheduled aim parameter；
S5：Purge unit removes sample remaining in pipeline, then, purge unit by the flow velocity of setting and time scavenging pipeline
The first cold-trap is purged by the flow velocity of setting and time, empties empty gas and water remaining in the first cold-trap and carbon dioxide, and cold simultaneously
Freeze second cold-trap；
S6：After purging, after the second cold-trap is chilled to specified range and keeps stablizing, the first cold-trap is preheated；
S7:After the completion of the first cold-trap preheating, the first multiple-way valve is adjusted, purge unit is purged by the flow velocity of setting and time,
Volatile organic compounds is transferred to the second cold-trap, and two before volatile organic compounds transfer terminates from the first cold-trap
Minute, third cold-trap is freezed, and freezing state is kept to stablize；
S8:Set temperature is heated to the second cold-trap, purge unit purges the second cold-trap by the flow velocity of setting and time, by second
Carbon dioxide separation in cold-trap in sample gas, the second cold-trap continues to heat after carbon dioxide separation, by volatile organic
It closes object to be transferred in third cold-trap from the second cold-trap, the first cold-trap by the temperature and time of setting is toasted, is purged simultaneously
Unit purges the first cold-trap；
S9:In second cold-trap after the completion of volatile organic compounds transfer, start gas chromatography mass spectrometer, third cold-trap is specified
Time in transient heating, purge unit purging third cold-trap, volatile organic compounds is injected into gas phase according to set time
Chromatographic mass spectrometry instrument；
S10:After volatile organic compounds has been injected, sample introduction terminates, and toasts the second cold-trap by the temperature and time of setting, together
When purge unit purge the second cold-trap；
S11:Gas chromatography mass spectrometer delay start, purge unit purging sample introduction pipeline are simultaneously emptied, are made in low temperature concentrating instrument pipeline
The state of temperature and gas flow paths and state consistency when not working；
S12:It is out of service after gas chromatography mass spectrometer delay start, system by next sample in automatic running sequence into
Sample repeats the above steps, until the last one sample end of run.
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| CN201711318589.XA CN108226322A (en) | 2017-12-12 | 2017-12-12 | A kind of low temperature concentrating instrument and control method |
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| CN201711318589.XA CN108226322A (en) | 2017-12-12 | 2017-12-12 | A kind of low temperature concentrating instrument and control method |
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| CN110095575A (en) * | 2019-05-08 | 2019-08-06 | 中国科学技术大学 | The enriching and purifying equipment of pure gas in mixed gas |
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