CN107656004A - A kind of horizontal large volume sample injection system and method for gas-chromatography - Google Patents
A kind of horizontal large volume sample injection system and method for gas-chromatography Download PDFInfo
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- CN107656004A CN107656004A CN201711093952.2A CN201711093952A CN107656004A CN 107656004 A CN107656004 A CN 107656004A CN 201711093952 A CN201711093952 A CN 201711093952A CN 107656004 A CN107656004 A CN 107656004A
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- 238000002347 injection Methods 0.000 title claims abstract description 78
- 239000007924 injection Substances 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000004817 gas chromatography Methods 0.000 title claims abstract description 31
- 238000007789 sealing Methods 0.000 claims abstract description 14
- 230000008859 change Effects 0.000 claims abstract description 9
- 230000005484 gravity Effects 0.000 claims abstract description 6
- 238000010926 purge Methods 0.000 claims abstract description 4
- 239000012159 carrier gas Substances 0.000 claims description 36
- 230000007246 mechanism Effects 0.000 claims description 30
- 239000002904 solvent Substances 0.000 claims description 27
- 238000005070 sampling Methods 0.000 claims description 24
- 239000007789 gas Substances 0.000 claims description 20
- 150000001875 compounds Chemical class 0.000 claims description 18
- 238000001514 detection method Methods 0.000 claims description 8
- 238000002309 gasification Methods 0.000 claims description 8
- 238000012360 testing method Methods 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 238000000935 solvent evaporation Methods 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000002390 rotary evaporation Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 8
- 230000004888 barrier function Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 6
- 230000035945 sensitivity Effects 0.000 description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000007123 defense Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 244000261422 Lysimachia clethroides Species 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000003965 capillary gas chromatography Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003891 environmental analysis Methods 0.000 description 1
- 238000004186 food analysis Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000008450 motivation Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
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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
- G01N30/24—Automatic injection systems
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Abstract
The invention provides a kind of gas-chromatography with horizontal large volume sample injection system and method, described gas-chromatography includes total flow control valve with horizontal large volume sample injection system, dottle pin nut and dottle pin, dottle pin purges control valve, flow divider, shunt discharge control valve, bushing pipe, post nut and sealing gasket, chromatographic column, temperature control modules, it is characterized in that, described bushing pipe is that bipyramid shunts bushing pipe, it is laterally disposed, placed parallel to ground, dottle pin nut and dottle pin, post nut and sealing gasket, chromatographic column, also corresponding change is done therewith in temperature control modules position, horizontal direction is followed successively by dottle pin nut and dottle pin from front to back, bushing pipe, post nut and sealing gasket and chromatographic column, temperature control modules laterally wrap up bushing pipe；Described gas-chromatography large volume sample injection method is applied to described large volume sample injection system.Overcome that to overcome bushing pipe be all the technology prejudice being disposed vertically, efficiently solve into bushing pipe solution under gravity easily from the technical barrier of immersed tube outflow.
Description
Technical field
The present invention relates to detecting instrument field, more particularly to a kind of gas-chromatography large volume sample injection system and method.
Background technology
Improve the eternal topic that sensitivity for analysis is almost analytical chemistry.With regard to GC analysis for, instrument manufacturers and
Analysis worker always tries the method for manufacturing highly sensitive instrument and developing high spirit degree of respecting.Especially in environmental analysis, medicine
In terms of analysis and food analysis, it is exactly this hair for requiring to promote instrument to have very high requirement to sensitivity about regulation method
Exhibition, and the development of instrument has the person that makes law making to propose that higher detection sensitivity requires, this interaction moves in circles.
Carrier of traditional gas chromatographic sample introduction mode using bushing pipe as solvent evaporation.Due to expansion rate when organic solvent vaporizes
Greatly, boiling point is relatively low, and the volume of bushing pipe can not increase substantially, therefore the sampling volume of gas-chromatography is generally limited by 5 μ L
Below.
Application of the large volume sample injection technology in capillary gas chromatography can reduce the test limit of analysis method, improve and divide
Analyse sensitivity and precision.Traditional large volume sample injection technology mainly has two classes, first, convenient cold on-column injection is based on, second, being based on program
Heat up vaporisation techniques (PTV technologies).Convenient cold on-column injection technology is applied to analysis thermally labile sample, mainly by entering with cold column cap
The connected chromatographic column pre-column of sample mouth realizes that solvent focuses on, and increases sample size, its shortcoming is that requirement sample substrate is clean, will not be polluted
Chromatographic column can just be analyzed.PTV input modes mainly realize large volume sample injection by temperature programming-solvent air defense pattern, i.e.,
Sample enters cold bushing pipe, solvent and part low boiling component with liquid condition and exports air defense from shunting with carrier gas).Work as major part
After solvent volatilization emptying, second of sample introduction can be carried out, above solvent vent process is repeated, until sample size needed for completion.Lining
After enough determinands are have accumulated in pipe, testing sample is transferred in chromatographic column by rise gasification room temperature, so as to reach
Large volume sample injection effect.Its advantage is that analyte vaporizes under minimum injector temperature rather than at a high temperature of constant, from
And the possibility of sample thermal cracking is minimized, while still allow a large amount of analytes to vaporize.Its shortcoming is due to the position of vaporization
Put and be still limited to bushing pipe, therefore the volume of sample introduction still is limited to the volume of bushing pipe.Further, since bushing pipe is all designed to hang down
Straight to place, upper end sample introduction and carrier gas, lower termination chromatographic column, due to being acted on by gravity and gas pressure, liquid is not easy serving as a contrast
Stopped in pipe.Then, each instrument manufacturer facility man have devised various schemes, solve the problems, such as Liquid sample introduction amount, Agilent company
Single or multiple baffle-walls are devised on bushing pipe（Agilent article No.：5183-2038、5183-2036、5183-2037）, Shimadzu it is public
Department devises the PTV bushing pipes of fine inner diameter, and internal diameter only has 1.25mm（Shimadzu article No.：221-49300-00）, platinum Elmer Co., Ltd
It set up fine inner diameter and add female gooseneck bushing pipe, internal diameter only has 1.0mm.But bushing pipe volume does not still have very big breakthrough, Agilent
The above-mentioned bushing pipe volume of company is 150 to 200 μ L, and Shimadzu is 100 μ L, the μ L of platinum Ai Ermo 70, and large volume sample injection is limited in ten
A few μ L even a few μ L, the purpose of real large volume sample injection it is not really achieved.
At present, liquid phase and the application that gas phase is online, GPC and gas phase are online are more and more, and interface problem is that a comparison is dashed forward
The problem of going out, the GPC-GCMSMS of Shimadzu Corporation's production is online, and injection port adds convenient cold on-column injection using PTV, just realizes
200 μ L sample size, has met requirement reluctantly.But which complex designing, cost are high, operation difficulty is big, are unfavorable for promoting
Use.
The content of the invention
All it is the technology that is disposed vertically it is an object of the invention to overcome bushing pipe in view of the above the shortcomings that prior art
Prejudice, there is provided a kind of horizontal large volume sample injection system and method for gas-chromatography, for solving the problems of the prior art.
In order to achieve the above objects and other related objects, the present invention provides a kind of gas-chromatography horizontal large volume sample injection system
System and method, a kind of gas-chromatography include total flow control valve, dottle pin nut and dottle pin, dottle pin with horizontal large volume sample injection system
Control valve, flow divider, shunting discharge control valve, bushing pipe, post nut and sealing gasket, chromatographic column, temperature control modules are purged, it is special
Sign is, described bushing pipe is that bipyramid shunts bushing pipe, laterally disposed, i.e., parallel to ground placement, dottle pin nut and every
Pad, post nut and sealing gasket, chromatographic column, temperature control modules position also do corresponding change therewith, horizontal direction from front to back according to
Secondary is dottle pin nut and dottle pin, bushing pipe, post nut and sealing gasket and chromatographic column, and temperature control modules laterally wrap up bushing pipe；It is a kind of
Gas-chromatography large volume sample injection method is applied to described large volume sample injection system, it is characterised in that comprises the following steps：
1. the preparatory stage before sample introduction：Temperature control modules cool, and are brought down below below 20 DEG C of solvent temperature；
2. the sample introduction stage：Inject in large volume fluid sample to the bushing pipe, under gravity, liquid is laid in bushing pipe bottom
On portion's tube wall, sampling system keeps low temperature, and shunting discharge control valve is opened；
3. solvent removes the stage：Temperature control modules are gradually heated up, and shunting discharge control valve is opened, the solvent in the presence of carrier gas
Evaporation, the solvent vapo(u)r for evaporating formation are discharged through flow divider and shunting discharge control valve from diffluence pass；
4. the high-temperature gasification stage：Temperature control modules are rapidly heated, and shunting discharge control valve is closed, sample quick air at high temperature
Change, enter chromatographic column with carrier gas, after chromatogram post separation, lead to detector；
5. cleansing phase：After target compound enters chromatographic column under the drive of carrier gas, shunting discharge control valve is opened, other
The material for being introduced into chromatographic column is discharged in the presence of carrier gas from shunting outlet.Shunting discharge control valve is closed, into carrier gas section
Province's pattern；
6. ending phase：When all target compounds flow out from chromatographic column, after testing after device detection, temperature control modules cool,
Wait next pin sample introduction.
Further, in addition to a triple valve and one section of chromatogram pre-column, triple valve respectively with pre-column, analytical column and carrier gas pipe
Road is connected, and forms blowback system, after target compound is by triple valve, inputs carrier gas to triple valve, the gas in analytical column
Flow detection device, pre-column gas flow sampling system, form blowback.Sample injection method, which is characterized in that, to be comprised the following steps：
1. the preparatory stage before sample introduction：Temperature control modules cool, and the input carrier gas of triple valve A mouths, form blowback；
2. the sample introduction stage：Large volume fluid sample is injected, sampling system keeps low temperature, keeps blowback；
3. solvent removes the stage：Sampling system is gradually heated up, and diffluence pass is opened, and solvent evaporates in the presence of carrier gas, evaporates shape
Into solvent vapo(u)r from diffluence pass discharge, keep blowback；
4. the high-temperature gasification stage：Sampling system is rapidly heated, and diffluence pass is closed, and blowback air is closed, sample quick air at high temperature
Change, enter chromatographic column pre-column with carrier gas, enter analytical column through triple valve, lead to detector；
5. the blowback stage：When target compound is after triple valve, opening blowback air, target compound continues the drive in carrier gas
Under separated in analytical column, other volatile-resistant substances return to sampling system in the presence of carrier gas, from shunting outlet discharge；
6. ending phase：When all target compounds flow out from analytical column, after testing after device detection, closing diffluence pass, closing is instead
Blow, wait next pin sample introduction.
Further, in addition to bearing, motor, O-ring, fixing nut, bushing pipe support ring, it is characterised in that described axle
The groove provided with internal thread is held, centre is provided with the hole that can pass through bushing pipe, and the O-ring described in described bushing pipe band passes through described axle
Hold, bushing pipe being fixed on bearing by described fixing nut in a manner of compressing O-ring, and described bearing is in described electricity
Rotated under the drive of motivation, bearing drives O-ring to rotate, and O-ring drives bushing pipe to rotate, and accelerates solvent evaporation, reaches rotation and steams
The effect of hair.
Further, in addition to a mechanical arm, automatic sample handling system and fixed plate, described mechanical arm, auto injection system
System and fixed plate are located at gas chromatograph injection port side, and described automatic sample handling system is by sample injection disc, automatic sampler, sample introduction
Device base is formed, and described automatic sampler is fixed on mechanical arm by fixed plate, and rotation is provided between fixed plate and mechanical arm
Rotation mechanism, fixed plate are provided with automatic sampler fixed mechanism, and up and down motion driving machine is provided between fixed mechanism and fixed plate
Structure, can make automatic sampler parallel to（Along）Automatic sampler direction moves up and down, and will can enter automatically in vertical direction
The lift-off of sample device and injector base is put back to, in the horizontal direction can be close by injector or leave injection port, be easy to sample introduction；Rotation
Mechanism can be rotated by 90 °, and automatic sampler is changed into horizontality from plumbness；Carrying out practically pattern is：
1. inhale the sample stage：Automatic sampler is in plumbness, on automatic sampler base, conventionally draws sample
Product.
2. revolving process：Up and down motion drive mechanism between fixed mechanism and fixed plate, by automatic sampler lift-off bottom
Seat, rotating mechanism driving mechanical arm are rotated by 90 °, and automatic sampler is changed into horizontality from plumbness, are directed at injection port,
Up and down motion drive mechanism between fixed mechanism and fixed plate is by automatic sampler close to injection port.
3. the sample introduction stage：Conventionally to injection port sample introduction.
4. return stage：Automatic sampler leaves injection port, and mechanical arm reversely rotates 90 degree, is changed into plumbness again,
Injector base is put back to, prepares next pin sample introduction.
Drive mechanism in the fixed plate docks automatic sampler with gas-chromatography large volume transverse direction injection port, enters
Sample, after the completion of sample introduction, then injector will be made by oneself and put back to injector base.
Further, automatic sampler is located above instrument, and mechanical arm is connected by rotary shaft with instrument, automatic sampler and
Mechanical arm is connected, and described rotating shaft can carry out 90 degree of rotations.
Further, to save the time, the 1-3 ranks of sample introduction next time can also after the 5th stage, before the 6th stage, be started
Section, after the 6th stage of previous pin terminates, starts the 4th stage of latter pin.
As described above, a kind of horizontal large volume sample injection system and method for gas-chromatography of the present invention, has beneficial below
Effect：
1. overcoming, to overcome bushing pipe be all the technology prejudice being disposed vertically, and is efficiently solved into bushing pipe solution under gravity
Easily from the technical barrier of immersed tube outflow, large volume sample injection is realized, sampling volume is changed from micro updating to milliliter level, improved
Sensitivity.
2. sample concentration process is organically combined with sampling system, the mistake concentrated in sample pre-treatments is eliminated
Journey, efficiency is improved, save cost.
3. blowback system, during solvent evaporation is carried out, solvent vapo(u)r will not enter chromatographic column, protect chromatographic column
And detector.
4. realizing " revolving " in bushing pipe, accelerate solvent volatilization.
5. being provided with mechanical arm, the injector of plumbness can be become horizontal state, realize horizontal large volume sample injection
The auto injection of system.
6. the present invention is simple in construction, easy to operation, it is easy to by the temperature programming multi-mode injection port of existing instrument（MMI）
It is transformed into horizontal large volume sample injection system.
Brief description of the drawings
Fig. 1 schematic structural views of the invention.
Fig. 2 has the horizontal large volume sample injection system of blowing function.
The rotatable horizontal large volume sample injection system of Fig. 3 bushing pipes.
The suction sample view of the rotatable automatic sample handling system of Fig. 4 automatic samplers.
The sample introduction view of the rotatable automatic sample handling system of Fig. 5 automatic samplers.
The suction sample view of automatic sample handling systems of the Fig. 6 with rotary shaft.
The sample introduction view of automatic sample handling systems of the Fig. 7 with rotary shaft.
In figure, 1. total flow control valves, 2 dottle pin nuts and dottle pin, 3 dottle pins purging control valve, 4 flow dividers, 5 shunting outlets
Control valve, 6 bushing pipes, 7 post nuts and sealing gasket, 8 chromatographic columns, 8-1 pre-columns, the temperature control modules of 8-2 analytical columns 9；10. threeway
Valve, 11 bearings, 12 motor, 13 grooves with internal thread, 14O type circles, 15 fixing nuts, 16 bushing pipe support rings, 17 mechanical arms, 18
Automatic sample handling system, sample injection disc 18-1, automatic sampler 18-2, injector base 18-3,19 fixed plates, 20 gas chromatographs,
21 injection ports, 22 rotating mechanisms, rotary shaft 23.
Embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book understands other advantages and effect of the present invention easily.
Embodiment one
The horizontal large volume sample injection system and method for a kind of gas-chromatography, as shown in figure 1, including total flow control valve 1, dottle pin spiral shell
Female and dottle pin 2, dottle pin purging control valve 3, flow divider 4, shunting discharge control valve 5, bushing pipe 6, post nut and sealing gasket 7, chromatogram
Post 8, temperature control modules 9, it is characterised in that described bushing pipe 6 is that bipyramid shunts bushing pipe, laterally disposed, i.e., parallel
Placed in ground, dottle pin nut and dottle pin 2, post nut and sealing gasket 3, chromatographic column 8, temperature control modules position 9 are also done therewith
Corresponding change, horizontal direction are followed successively by dottle pin nut and dottle pin 2, bushing pipe 6, post nut and sealing gasket 7 and chromatographic column from front to back
8, temperature control modules 9 laterally wrap up bushing pipe 6；Bushing pipe support ring 16 is also provided with, to keep bushing pipe to be in horizontality.Tool
Running body pattern is：
1. the preparatory stage before sample introduction：Temperature control modules 9 cool, and are brought down below below 20 DEG C of solvent temperature；
2. the sample introduction stage：Inject in large volume fluid sample to the bushing pipe 6, under gravity, liquid is laid in bushing pipe 6
On the tube wall of bottom, sampling system keeps low temperature, and shunting discharge control valve 5 is opened；
3. solvent removes the stage：Temperature control modules 9 are gradually heated up, and shunting discharge control valve 5 is opened, molten in the presence of carrier gas
Agent is evaporated, and the solvent vapo(u)r for evaporating formation is discharged through flow divider 4 and shunting discharge control valve 5 from diffluence pass；
4. the high-temperature gasification stage：Temperature control modules 9 are rapidly heated, and shunting discharge control valve 5 is closed, and sample is quick at high temperature
Gasification, enters chromatographic column 8 with carrier gas, after the separation of chromatographic column 8, leads to detector；
5. cleansing phase：After target compound enters chromatographic column 8 under the drive of carrier gas, shunting discharge control valve 5 is opened, its
The material that he is introduced into chromatographic column 8 is discharged in the presence of carrier gas from shunting outlet.Shunting discharge control valve 5 is closed, into load
Gas save mode；
6. ending phase：When all target compounds flow out from chromatographic column 8, after testing after device detection, temperature control modules 9 drop
Temperature, wait next pin sample introduction.
Embodiment two
A kind of horizontal large volume sample injection system and method for gas-chromatography as shown in embodiment one, further, as shown in Fig. 2
Also include a triple valve 10, chromatographic column 8 is divided and connects gas for pre-column 8-1 and analytical column 8-2, composition blowback system, triple valve A mouths
Road intake pipeline, B mouths connect analytical column, and C mouths connect pre-column, after target compound is by triple valve 10, inputs and carry to triple valve A mouths
Gas, B mouths and the output carrier gas of C mouths, the gas flow detector in analytical column, pre-column gas flow sampling system, when stopping passing through A
During mouth input carrier gas, carrier gas successively enters analytical column 8-2 from sampling system through pre-column 8-1, triple valve 10.Carrying out practically pattern
For：
1. the preparatory stage before sample introduction：Temperature control modules cool, and the input carrier gas of triple valve A mouths, form blowback；
2. the sample introduction stage：Large volume fluid sample is injected, sampling system keeps low temperature, keeps blowback；
3. solvent removes the stage：Sampling system is gradually heated up, and diffluence pass is opened, and solvent evaporates in the presence of carrier gas, evaporates shape
Into solvent vapo(u)r from diffluence pass discharge, keep blowback；
4. the high-temperature gasification stage：Sampling system is rapidly heated, and diffluence pass is closed, and blowback air is closed, sample quick air at high temperature
Change, enter chromatographic column pre-column with carrier gas, enter analytical column through triple valve, lead to detector；
5. the blowback stage：When target compound is after triple valve, opening blowback air, target compound continues the drive in carrier gas
Under separated in analytical column, other volatile-resistant substances return to sampling system in the presence of carrier gas, from shunting outlet discharge；
6. ending phase：When all target compounds flow out from analytical column, after testing after device detection, closing diffluence pass, closing is instead
Blow, wait next pin sample introduction.
Embodiment three
A kind of gas-chromatography large volume sample injection system and method as shown in embodiment one, further, as shown in figure 3, also including
Bearing 11, motor 12, O-ring 14, fixing nut 15, bushing pipe support ring 16, it is characterised in that described bearing is provided with band
The groove 13 of internal thread, centre are provided with the hole that can pass through bushing pipe, and described bushing pipe 6 passes through described bearing with described O-ring 14
11, described fixing nut 15 carries outer silk, can be screwed into the groove 13, in a manner of compressing O-ring 14 by bushing pipe 6
It is fixed on bearing 11, the other end of bushing pipe 6 is positioned in the support ring 16, with keep level laying state, described bearing
Being rotated under the drive of described motor, bearing drives O-ring to rotate, and O-ring drives bushing pipe to rotate, and accelerates solvent evaporation,
Reach the effect of rotary evaporation.Bearing 11 is in contact with the temperature adjustment module 9 of sampling system, is entered using end face seal mode
Row sealing, prevents gas leakage.
Example IV
A kind of gas-chromatography large volume sample injection system and method as shown in embodiment one, further, as shown in Figure 4,5, is also wrapped
Include a mechanical arm 17, automatic sample handling system 18 and fixed plate 19, described mechanical arm 17, automatic sample handling system 18 and fixed plate
19 are located at the side of 20 injection port of gas chromatograph 21, described automatic sample handling system by sample injection disc 18-1, automatic sampler 18-2,
Injector base 18-3 is formed, and described automatic sampler 18-2 is fixed on mechanical arm 17 by fixed plate 19, fixed plate 19
Rotating mechanism 22 is provided between mechanical arm 17, fixed plate is provided with automatic sampler fixed mechanism, fixed mechanism and fixed plate
Between be provided with up and down motion drive mechanism, can make automatic sampler parallel to（Along）Automatic sampler direction moves up and down,
By automatic sampler lift-off and injector base can be put back in vertical direction, in the horizontal direction can by injector close to or from
Injection port is opened, is easy to sample introduction；Rotating mechanism 22 can be rotated by 90 °, and automatic sampler 18-2 is changed into horizontal from plumbness
State；Sample state is inhaled as shown in figure 4, sample introduction state is as shown in Figure 5；Carrying out practically pattern is：
1. inhale the sample stage：Automatic sampler is in plumbness, on automatic sampler base, conventionally draws sample
Product.
2. revolving process：Up and down motion drive mechanism between fixed mechanism and fixed plate, by automatic sampler lift-off bottom
Seat, rotating mechanism driving mechanical arm are rotated by 90 °, and automatic sampler is changed into horizontality from plumbness, are directed at injection port,
Up and down motion drive mechanism between fixed mechanism and fixed plate is by automatic sampler close to injection port.
3. the sample introduction stage：Conventionally to injection port sample introduction.
4. return stage：Automatic sampler leaves injection port, and mechanical arm reversely rotates 90 degree, is changed into plumbness again,
Injector base is put back to, prepares next pin sample introduction.
Embodiment five
A kind of gas-chromatography large volume sample injection system and method as shown in example IV, it is further, as shown in Figure 6,7, described
Mechanical arm 17, automatic sample handling system 18 and fixed plate 19 be located at the one end of 20 top injection port of gas chromatograph 21, described machine
Tool arm 17 is connected by rotary shaft 23 with instrument 20, and described rotating shaft can carry out 90 degree of rotations.
Embodiment six
Any gas-chromatography large volume sample injection system and method in embodiment one to three, can also be the 5th to save the time
After stage, before the 6th stage, start the 1-3 stages of sample introduction next time, after the 6th stage of previous pin terminates, start latter pin
The 4th stage.
Claims (6)
1. a kind of horizontal large volume sample injection system and method for gas-chromatography, the horizontal large volume sample injection system of described gas-chromatography
System include total flow control valve, dottle pin nut and dottle pin, dottle pin purging control valve, flow divider, shunt discharge control valve, bushing pipe,
Post nut and sealing gasket, chromatographic column, temperature control modules, it is characterised in that described bushing pipe is that bipyramid shunts bushing pipe,
It is laterally disposed, i.e., placed parallel to ground, dottle pin nut and dottle pin, post nut and sealing gasket, chromatographic column, temperature control modules position
Put and also do corresponding change therewith, horizontal direction be followed successively by from front to back dottle pin nut and dottle pin, bushing pipe, post nut and sealing gasket and
Chromatographic column, temperature control modules laterally wrap up bushing pipe；Described gas-chromatography large volume sample injection method be applied to it is described substantially
Product sampling system, it is characterised in that comprise the following steps：
1. the preparatory stage before sample introduction：Temperature control modules cool, and are brought down below below 20 DEG C of solvent temperature；
2. the sample introduction stage：Inject in large volume fluid sample to the bushing pipe, under gravity, liquid is laid in bushing pipe bottom
On portion's tube wall, sampling system keeps low temperature, and shunting discharge control valve is opened；
3. solvent removes the stage：Temperature control modules are gradually heated up, and shunting discharge control valve is opened, the solvent in the presence of carrier gas
Evaporation, the solvent vapo(u)r for evaporating formation are discharged through flow divider and shunting discharge control valve from diffluence pass；
4. the high-temperature gasification stage：Temperature control modules are rapidly heated, and shunting discharge control valve is closed, sample quick air at high temperature
Change, enter chromatographic column with carrier gas, after chromatogram post separation, lead to detector；
5. cleansing phase：After target compound enters chromatographic column under the drive of carrier gas, shunting discharge control valve is opened, other
The material for being introduced into chromatographic column is discharged in the presence of carrier gas from shunting outlet；Shunting discharge control valve is closed, into carrier gas section
Province's pattern；
6. ending phase：When all target compounds flow out from chromatographic column, after testing after device detection, temperature control modules cool,
Wait next pin sample introduction.
A kind of 2. horizontal large volume sample injection system and method for gas-chromatography according to claim 1, it is characterised in that institute
The horizontal large volume sample injection system of the gas-chromatography stated also includes a triple valve and one section of chromatogram pre-column, triple valve respectively with advance
Post, analytical column are connected with gas-carrier pipeline, form blowback system, after target compound is by triple valve, inputs and carry to triple valve
Gas, the gas flow detector in analytical column, pre-column gas flow sampling system, form blowback；Described sample injection method application
In described large volume sample injection system, it is characterised in that comprise the following steps：
1. the preparatory stage before sample introduction：Temperature control modules cool, and the input carrier gas of triple valve A mouths, form blowback；
2. the sample introduction stage：Large volume fluid sample is injected, sampling system keeps low temperature, keeps blowback；
3. solvent removes the stage：Sampling system is gradually heated up, and diffluence pass is opened, and solvent evaporates in the presence of carrier gas, evaporates shape
Into solvent vapo(u)r from diffluence pass discharge, keep blowback；
4. the high-temperature gasification stage：Sampling system is rapidly heated, and diffluence pass is closed, and blowback air is closed, sample quick air at high temperature
Change, enter chromatographic column pre-column with carrier gas, enter analytical column through triple valve, lead to detector；
5. the blowback stage：When target compound is after triple valve, opening blowback air, target compound continues the drive in carrier gas
Under separated in analytical column, other volatile-resistant substances return to sampling system in the presence of carrier gas, from shunting outlet discharge；
6. ending phase：When all target compounds flow out from analytical column, after testing after device detection, closing diffluence pass, closing is instead
Blow, wait next pin sample introduction.
3. a kind of gas-chromatography according to claim 1 or 2 is existed with horizontal large volume sample injection system and method, its feature
In described gas-chromatography also includes bearing, motor, O-ring, fixing nut, bushing pipe branch with horizontal large volume sample injection system
Pushing out ring, it is characterised in that described bearing is provided with the groove of internal thread, and centre is provided with the hole that can pass through bushing pipe, described bushing pipe band
Described O-ring passes through described bearing, and described fixing nut by bushing pipe in a manner of compressing O-ring being fixed on bearing
On, described bearing rotates under the drive of described motor, and bearing drives O-ring to rotate, and O-ring drives bushing pipe to rotate,
Accelerate solvent evaporation, reach the effect of rotary evaporation.
4. a kind of gas-chromatography according to claim 1 or 2 is existed with horizontal large volume sample injection system and method, its feature
In gas-chromatography also includes a mechanical arm, automatic sample handling system and fixed plate, described machine with horizontal large volume sample injection system
Tool arm, automatic sample handling system and fixed plate are located at gas chromatograph injection port side, described automatic sample handling system by sample injection disc,
Automatic sampler, injector base composition, described automatic sampler are fixed on mechanical arm by fixed plate, fixed plate and machine
Rotating mechanism is provided between tool arm, fixed plate is provided with automatic sampler fixed mechanism, is provided between fixed mechanism and fixed plate
Up and down motion drive mechanism, can make automatic sampler parallel to（Along）Automatic sampler direction moves up and down, in Vertical Square
To by automatic sampler lift-off and injector base can be put back to, in the horizontal direction can be close by injector or sample introduction be left
Mouthful, it is easy to sample introduction；Rotating mechanism can be rotated by 90 °, and automatic sampler is changed into horizontality from plumbness；Applied to institute
The sample injection method for the large volume sample injection system stated, it is characterised in that comprise the following steps：
1. inhale the sample stage：Automatic sampler is in plumbness, on automatic sampler base, conventionally draws sample
Product；
2. revolving process：Up and down motion drive mechanism between fixed mechanism and fixed plate, by automatic sampler lift-off base, rotation
Rotation mechanism driving mechanical arm is rotated by 90 °, and automatic sampler is changed into horizontality from plumbness, is directed at injection port, fixed machine
Up and down motion drive mechanism between structure and fixed plate is by automatic sampler close to injection port；
3. the sample introduction stage：Conventionally to injection port sample introduction；
4. return stage：Automatic sampler leaves injection port, and mechanical arm reversely rotates 90 degree, is changed into plumbness again, puts back to
Injector base, prepare next pin sample introduction.
A kind of 5. horizontal large volume sample injection system and method for gas-chromatography according to claim 4, it is characterised in that gas
Phase chromatographic grade transverse direction large volume sample injection system automatic sampler is located above instrument, and mechanical arm is connected by rotary shaft with instrument,
Automatic sampler is connected with mechanical arm, and described rotating shaft can carry out 90 degree of rotations.
6. a kind of gas-chromatography according to claim 1 or 2 is existed with horizontal large volume sample injection system and method, its feature
In to save the time, the 1-3 stages of sample introduction next time after the 5th stage, before the 6th stage, being started, treat previous pin
After 6th stage terminated, start the 4th stage of latter pin.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108414644A (en) * | 2018-04-08 | 2018-08-17 | 西北民族大学 | A kind of preposition processing instrument of Drugs based on gas chromatographic detection technology |
| CN108426876A (en) * | 2018-03-29 | 2018-08-21 | 南通市第人民医院 | A kind of detection device of 2% glutaral disinfectant solution effective concentration |
| CN110361493A (en) * | 2019-08-07 | 2019-10-22 | 常州磐宇仪器有限公司 | A kind of multidigit automatic sampling apparatus |
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2017
- 2017-11-08 CN CN201711093952.2A patent/CN107656004A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108426876A (en) * | 2018-03-29 | 2018-08-21 | 南通市第人民医院 | A kind of detection device of 2% glutaral disinfectant solution effective concentration |
| CN108426876B (en) * | 2018-03-29 | 2020-04-21 | 南通市第一人民医院 | Detection apparatus for 2% glutaraldehyde antiseptic solution effective concentration |
| CN108414644A (en) * | 2018-04-08 | 2018-08-17 | 西北民族大学 | A kind of preposition processing instrument of Drugs based on gas chromatographic detection technology |
| CN110361493A (en) * | 2019-08-07 | 2019-10-22 | 常州磐宇仪器有限公司 | A kind of multidigit automatic sampling apparatus |
| CN110361493B (en) * | 2019-08-07 | 2024-05-10 | 常州磐宇仪器有限公司 | Multi-position automatic sample injection device |
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