CN209247664U - Instillation micro-extraction device for thermal analyzer evolution component analysis - Google Patents
Instillation micro-extraction device for thermal analyzer evolution component analysis Download PDFInfo
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- CN209247664U CN209247664U CN201821669451.4U CN201821669451U CN209247664U CN 209247664 U CN209247664 U CN 209247664U CN 201821669451 U CN201821669451 U CN 201821669451U CN 209247664 U CN209247664 U CN 209247664U
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Abstract
The utility model relates to micro-extraction fields of instiling, more particularly to a kind of instillation micro-extraction device for thermal analyzer evolution component analysis, including for control droplet size and periodically collect drop drop control unit, for carry out instillation micro-extraction and by instillation micro-extraction unit that object is enriched in drop, the thermal analyzer unit for being used to carry sample and carrying out heat analysis, be used to add the internal standard adding unit of volatility internal standard compound for carrier gas all the way, be used to hold the micro-collection bottle of drop；Liquid replenisher in drop control unit is communicated by liquid capillary road with the extracting head in instillation micro-extraction unit, and switching valve is connect with micro-collection bottle, and the extraction chamber in instillation micro-extraction unit is separately connected thermal analyzer unit and internal standard adding unit.The utility model has the characteristics that easy, quick, stable, efficient, high degree of automation, provides reliable and stable technical guarantee for application of the instillation micro-extraction technique in terms of thermal analyzer escapes component qualitative and quantitative analysis.
Description
Technical field
The utility model relates to micro-extraction fields of instiling, and in particular to a kind of drop for thermal analyzer evolution component analysis
Infuse micro-extraction device.
Background technique
Liquid-phase micro extraction technique is a kind of novel sample proposed in mid-term the 1990s, and rapidly developing
Pretreatment technology.Liquid-phase micro extraction technique integrates sampling, separation, purifying, concentration, sample introduction, and adapts to complex dielectrics, trace
Measure the analysis of ingredient, special nature ingredient；It is easy to operate, quick, it is not necessarily to special instruments and equipment；Extraction mode is more, available
Organic solvent type is more and dosage is about several to tens microlitres few, provides very large space to optimize the condition of liquid-phase micro-extraction.
In today of building resource-efficient and environment friendly society, use is environmentally protective, consumption of organic solvent is small and inexpensive sample
Product pre-treating method has important practical significance.
Single drop micro-extraction (SDME) technology is a kind of novel, environmental-friendly Sample Pretreatment Technique, it collects extraction, enrichment
In one, have the characteristics that at low cost, device is simple, easily operated, consumption of organic solvent is few and bioaccumulation efficiency is high.Single drop is micro-
Extraction is that a drop extractant is suspended from conventional GC micro syringe needle tip, is then dipped in sample solution or is suspended from sample
Product headspace makes analyte be transferred to organic phase (extractant) from water phase, and organic droplet is drawn back injection through certain time
Device is simultaneously transferred to GC or other analysis systems are analyzed.But the drop for carrying out under the conditions of flowing gas automatically continuously supplements
Instillation micro-extraction device but rarely have correlative study and document report.
Utility model content
The utility model provides that a kind of easy to operate, rate of extraction is fast and the drop of high degree of automation regarding to the issue above
Infuse micro-extraction device.
The utility model uses following technical proposal in order to achieve the above objectives:
For the instillation micro-extraction device of thermal analyzer evolution component analysis, including for controlling droplet size and periodically receiving
The drop control unit of collection drop, the instillation micro-extraction list for carrying out instillation micro-extraction and being enriched in object in drop
Member, for carry sample and carry out heat analysis thermal analyzer, for for carrier gas all the way addition volatility internal standard compound internal standard add
Add unit, the micro-collection bottle for holding drop；Liquid replenisher in the drop control unit by liquid capillary road with
Extracting head in instillation micro-extraction unit communicates, and the switching valve in drop control unit is connect with micro-collection bottle, and instil micro- extraction
The extraction chamber in unit is taken to be separately connected thermal analyzer and internal standard adding unit.
Further, the drop control unit includes liquid getting device, liquid replenisher, controller, fibre-optical probe and switching valve, described
Controller is separately connected and controls liquid getting device, liquid replenisher and fibre-optical probe, and the switching valve is equipped with active tunnel, collects and lead to
Three channels in road and taking liquid passage, the liquid getting device are connected with switching valve by liquid capillary road and by switching valves
Active tunnel is according to circumstances communicated with collection channel or taking liquid passage, and the liquid replenisher passes through liquid capillary road and micro- extraction that instils
It takes and is communicated at the top of the extracting head of unit, and fluid infusion operation is carried out to maintain the big of drop according to the feedback signal of fibre-optical probe
Small, the fibre-optical probe is located at drop, and for the size and feedback signal for incuding drop to controller, the activity is logical
Road one end is fixedly connected with liquid getting device, and the other end can individually be connected to collection channel by the rotation process of switching valve or take liquid logical
The other end in road, taking liquid passage is connected with extracting head, and the other end of collection channel is connect with micro-collection bottle, so as to liquid getting device
It is pipetted in drop to micro-collection bottle in due course or periodically according to experimental program.
Further, the instillation micro-extraction unit is made of the extraction chamber extracting head intracavitary with extraction is arranged in, described
Extracting head be back taper, the top of extracting head is enclosed construction and the outside for extending to extraction chamber, and the bottom of extracting head is contracting
Mouthful, the top of extracting head is connected to by liquid capillary road with liquid replenisher, the top of extracting head also pass through liquid capillary road and
Taking liquid passage communicates, and the liquid capillary road lower end communicated with taking liquid passage extends at the necking of extracting head, the extraction
Chamber is taken to be separately connected thermal analyzer and internal standard adding unit, the rear positions that drop is located on extraction chamber are used equipped with offgas outlet
In the tail gas of discharge evolution.
Further, the internal standard adding unit includes conical flask, inner mark solution, magnetic stirring apparatus, stirring rod, conical flask
It is placed on magnetic stirring apparatus, inner mark solution, stirring rod are placed in conical flask, the rotation that the magnetic stirring apparatus passes through control stirring rod
Rotary speed adjusts the mixing speed of inner mark solution in conical flask, achievees the purpose that make inner mark solution normalization everywhere；Institute
It states conical flask top and external carrier gas N is separately connected by gas piping2With instillation micro-extraction unit, external carrier gas N2Into taper
The internal standard compound that bottle post-purge inner mark solution surface and carrying volatilize leaves conical flask, enters instillation micro-extraction along gas piping
Unit.
Further, the lower part of the micro-collection bottle inner surface be V-arrangement, convenient for small volume drop in late detection
It is middle to be extracted by sample introduction needle.
Further, the liquid getting device and liquid replenisher are syringe pump.
Further, spiral liquid support is equipped at the necking of the extracting head, the inner end of the spiral liquid support is located at extracting head
In necking, the outer end of spiral liquid support is extended to outside extracting head necking.
The utility model has the advantage that compared with prior art
1, the utility model realizes the combination of thermal analyzer Yu instillation micro-extraction technique, escapes component point for thermal analyzer
Analysis research field provides a kind of effective and feasible automatic device, facilitates thermal analyzer and gas-chromatography-mass spectrum, liquid chromatogram-
A variety of analysis and detecting instrument combinations such as mass spectrum, Capillary Electrophoresis.
2, the utility model has the characteristics that easy, quick, stable, efficient, high degree of automation, for instillation micro-extraction skill
Application of the art in terms of thermal analyzer escapes component qualitative and quantitative analysis provides reliable and stable technical guarantee.
Detailed description of the invention
Fig. 1 is the instillation micro-extraction device structural schematic diagram of the utility model.
Wherein A-drop control unit, B-instillation micro-extraction unit, C- thermal analyzer, D- internal standard adding unit, 1-takes
Liquid device, 2-liquid replenishers, 3- controller, 4- fibre-optical probe, 5-conical flasks, 6- inner mark solution, 7-magnetic stirring apparatus, 8-stirrings
Stick, 9-switching valves, 10-active tunnels, 11- collection channel, 12- taking liquid passage, 13-micro-collection bottles, 14- extract liquor,
15-drops, 16-furnace bodies, 17-crucibles, 18-balance arms, 19-offgas outlets, 20-extraction chambers, 21-extracting heads,
22-spiral liquid supports.
Specific embodiment
In order to which the technical solution of the utility model is further described, the utility model is carried out with reference to the accompanying drawing further
Explanation.
Embodiment 1
As shown in Figure 1, the instillation micro-extraction device for thermal analyzer evolution component analysis, including for controlling drop 15
Size simultaneously periodically collects the drop control unit A of drop 15, for carrying out instillation micro-extraction and object being enriched in drop 15
In instillation micro-extraction unit B, for carrying sample and carrying out the Switzerland Mettler Toledo brand TGA/DSC 3 of heat analysis
The thermal analyzer C of+model, for for carrier gas all the way add volatility internal standard compound internal standard adding unit D, for holding drop 15
Micro-collection bottle 13；10 milliliters of syringe pumps 2 of moist fluid board in the drop control unit A by liquid capillary road with
Extracting head 21 in instillation micro-extraction unit B communicates, and the switching valve 9 in drop control unit A is connect with micro-collection bottle 13,
Extraction chamber 20 in instillation micro-extraction unit B is separately connected the heat of Switzerland's Mettler Toledo brand TGA/DSC 3+ model
Analyzer C and internal standard adding unit D.The drop control unit A includes moist 100 microlitres of syringe pumps 1 of fluid board, moist stream
10 milliliters of syringe pumps 2 of body board, controller 3, Luo Shida board m3 diffuse fiber sensor 4 and switching valve 9, and the controller 3 divides
It is unrestrained anti-that 100 microlitres of syringe pumps 1 of moist fluid board, moist 10 milliliters of syringe pumps 2 of fluid board and Luo Shida board m3 are not connected and controlled
Fibre optical sensor 4 is penetrated, the switching valve 9 is equipped with 12 3 active tunnel 10, collection channel 11 and taking liquid passage channels, institute
100 microlitres of syringe pumps 1 of moist fluid board are stated to be connected by liquid capillary road with switching valve 9 and by the work in switching valve 9
Dynamic channel 10 is according to circumstances communicated with collection channel 11 or taking liquid passage 12, and described 10 milliliters of syringe pumps 2 of moist fluid board pass through
Liquid capillary road is communicated with the top of the extracting head 21 of instillation micro-extraction unit B, and according to Luo Shida board m3 diffusing reflection optical fiber
The feedback signal of sensor 4 carries out fluid infusion operation to maintain the size of drop 15, and the Luo Shida board m3 diffusing reflection optical fiber passes
Sensor 4 is located at the drop 15, and the size and feedback signal for incuding drop 15 are to controller 3, the active tunnel 10
One end is fixedly connected with 100 microlitres of syringe pumps 1 of moist fluid board, and the other end can be individually connected to by the rotation process of switching valve 9
The other end of collection channel 11 or taking liquid passage 12, taking liquid passage 12 is connected with extracting head 21, collection channel 11 it is another
One end is connect with micro-collection bottle 13, so that 100 microlitres of syringe pumps 1 of fluid board of moistening are moved according to experimental program in due course or periodically
It takes in drop 15 to micro-collection bottle 13.The instillation micro-extraction unit B is by extraction chamber 20 and the extraction being arranged in extraction chamber 20
First 21 composition is taken, the extracting head 21 is back taper, and the top of extracting head 21 is enclosed construction and extends to extraction chamber 20
Outside, the bottom of extracting head 21 are necking, and the top of extracting head 21 passes through liquid capillary road and 10 milliliters of moist fluid board notes
2 connection of pump is penetrated, the top of extracting head 21 also passes through liquid capillary road and communicates with taking liquid passage 12, described and taking liquid passage 12
The liquid capillary road lower end communicated extends at the necking of extracting head 21, and spiral liquid support is equipped at the necking of the extracting head 21
22, the inner end of the spiral liquid support 22 is located in 21 necking of extracting head, and the outer end of spiral liquid support 22 extends to 21 necking of extracting head
It is external.The extraction chamber 20 is separately connected the thermal analyzer C of Switzerland's Mettler Toledo brand TGA/DSC 3+ model and interior
Adding unit D is marked, the rear positions that drop 15 is located on extraction chamber 20 are equipped with the tail that offgas outlet 19 is used to discharge evolution
Gas.It include furnace body 16, balance arm in the thermal analyzer C of the Switzerland Mettler Toledo brand TGA/DSC 3+ model
18 and crucible 17；The balance arm 18 and crucible 17 are placed in furnace body 16, and the crucible 17 is placed on balance arm 18, the furnace body
16 have Program for precision temperature controlling function；The balance arm 18 is for detecting the mass change of sample in Temperature Programmed Processes and leading to
Cross embedded thermocouple test sample thermal change, the heat of the Switzerland Mettler Toledo brand TGA/DSC 3+ model
Analyzer C can measure sample quality and temperature change relationship by balance arm 18 under programed temperature, provide specific load
Under the conditions of gas in Temperature Programmed Processes sample thermal decomposition information；The Switzerland Mettler Toledo brand TGA/DSC 3+ type
Number the carrier gas of thermal analyzer C can carry the thermal decomposition product evolution furnace body 16 that sample volatilizes in temperature-rise period, along gas
Body pipeline enters instillation micro-extraction unit B.The internal standard adding unit D include conical flask 5, inner mark solution 6, magnetic stirring apparatus 7,
Stirring rod 8, conical flask 5 are placed on magnetic stirring apparatus 7, and inner mark solution 6, stirring rod 8 are placed in conical flask 5, the magnetic agitation
Device 7 adjusts the mixing speed of inner mark solution 6 in conical flask 5 by controlling the rotation speed of stirring rod 8, and reaching makes inner mark solution
The purpose of 6 normalizations everywhere；5 top of conical flask is separately connected external carrier gas N by gas piping2With micro- extraction that instils
Take unit B, external carrier gas N2Into 5 post-purge inner mark solution of conical flask, 6 surface and carries the internal standard compound that volatilizes and leave taper
Bottle 5, enters instillation micro-extraction unit B along gas piping.The lower part of 13 inner surface of micro-collection bottle is V-arrangement, is convenient for body
The lesser drop 15 of product is extracted in late detection by sample introduction needle.
Carry out the instillation micro-extraction experimental procedure of paper pyrolysis evolution component using the present invention:
A. Cigarette paper sample to be measured is collected first and is shredded；
B. 200mL extract liquor 14 is prepared according to volume ratio 1:9 with acetone and ethyl alcohol, is vacuumized through 0.22 μm of organic phase filter membrane
It is added to after filtering in 10 milliliters of syringe pumps 2 of moist fluid board；
C. 100 microlitres of syringe pumps 1 of moist fluid board are removed to be cleaned with extract liquor and dried up with pure air, accessed after emptying
System, rotating transfer valve 9 make active tunnel 10 be connected to taking liquid passage 12；
D. start drop control unit A, moist 10 milliliters of syringe pumps 2 of fluid board is promoted to make instillation micro-extraction unit B top
Full of extract liquor 14 and complete moist 10 milliliters of syringe pumps 2 of fluid board of pause propulsion after excluding gas；
E. 1000mL inner mark solution 6 is prepared according to volume ratio 1:999 with isopropanol and ethyl alcohol, pipettes 100mL and is added to cone
In shape bottle 5；
F. it is passed through high pure nitrogen 99.999% for conical flask 5, nitrogen flow 500mL/min is set, start magnetic stirring apparatus
7, setting speed 300r/min；
G. the thermal analyzer C for starting Switzerland Mettler Toledo brand TGA/DSC 3+ model, is added in crucible 17
100mg outturn, setting heat analysis temperature program(me) are heated to 600 DEG C from 40 DEG C with 10 DEG C/min heating rate, and carrier gas is arranged
For pure air, flow 200mL/min；
H. after the starting of sample temperature program, controller 3 controls moist 10 milliliters of syringe pumps 2 of fluid board in instillation micro-extraction list
First B automatically forms drop 15；
I. with the progress that instillation micro-extraction is tested, when drop 15 by carrier gas purge and volume become smaller when, drop control is single
First 15 size of A automatic sensing drop and automatic liquid supply, make drop 15 remain full state；
J. when sample is warming up to 60 DEG C, 10 milliliters of syringe pumps 2 of moist fluid board is paused immediately and start moist fluid board
100 microlitres of syringe pumps 1 extract drop 15, and then rotating transfer valve 9 makes active tunnel 10 be connected to collection channel 11, controller 3
Moist 100 microlitres of syringe pumps 1 of fluid board are controlled to be discharged in 15 to No. I micro-collection bottles 13 of drop；
K. 15 process time-consuming 5s of drop is extracted, immediately starts moist 10 milliliters of syringe pumps 2 of fluid board and generates drop 15
Continue the instillation micro-extraction test of second segment, and rotating transfer valve 9 makes active tunnel 10 be connected to taking liquid passage again
12；
L. the control process for repeating i step, j step, k step, every drop 15 of 20 DEG C of collections, until sample temperature is super
It crosses and no longer collects drop 15 after 500 DEG C；
M.40 23 drops 15 are collected into altogether in DEG C -500 DEG C of sample temperature-rise periods to be sub-packed in 23 micro-collection bottles 15,
Then with gas chromatograph-mass spectrometer (GC-MS) to each 15 analysis detection of drop.
The instillation micro-extraction is to carry the carrier gas continuously flowed of component to be measured constantly to purge drop 15, be component to be measured
The micro-extraction process that dynamic equilibrium is realized between carrier gas and drop 15, is that a drop 15 is constantly purged and persistently volatilized by carrier gas
And incuded and the volume dynamic changing process of continuous supplementation by the drop control unit A moment.
Embodiment 2
As shown in Figure 1, the instillation micro-extraction device for thermal analyzer evolution component analysis, including for controlling drop 15
Size simultaneously periodically collects the drop control unit A of drop 15, for carrying out instillation micro-extraction and object being enriched in drop 15
In instillation micro-extraction unit B, for carrying sample and carrying out the Switzerland Mettler Toledo brand TGA/DSC 3 of heat analysis
The thermal analyzer C of+model, for for carrier gas all the way add volatility internal standard compound internal standard adding unit D, for holding drop 15
Micro-collection bottle 13；10 milliliters of syringe pumps 2 of moist fluid board in the drop control unit A by liquid capillary road with
Extracting head 21 in instillation micro-extraction unit B communicates, and the switching valve 9 in drop control unit A is connect with micro-collection bottle 13,
Extraction chamber 20 in instillation micro-extraction unit B is separately connected the heat of Switzerland's Mettler Toledo brand TGA/DSC 3+ model
Analyzer C and internal standard adding unit D.The drop control unit A includes moist 100 microlitres of syringe pumps 1 of fluid board, moist stream
10 milliliters of syringe pumps 2 of body board, controller 3, Luo Shida board m3 diffuse fiber sensor 4 and switching valve 9, and the controller 3 divides
It is unrestrained anti-that 100 microlitres of syringe pumps 1 of moist fluid board, moist 10 milliliters of syringe pumps 2 of fluid board and Luo Shida board m3 are not connected and controlled
Fibre optical sensor 4 is penetrated, the switching valve 9 is equipped with 12 3 active tunnel 10, collection channel 11 and taking liquid passage channels, institute
100 microlitres of syringe pumps 1 of moist fluid board are stated to be connected by liquid capillary road with switching valve 9 and by the work in switching valve 9
Dynamic channel 10 is according to circumstances communicated with collection channel 11 or taking liquid passage 12, and described 10 milliliters of syringe pumps 2 of moist fluid board pass through
Liquid capillary road is communicated with the top of the extracting head 21 of instillation micro-extraction unit B, and according to Luo Shida board m3 diffusing reflection optical fiber
The feedback signal of sensor 4 carries out fluid infusion operation to maintain the size of drop 15, and the Luo Shida board m3 diffusing reflection optical fiber passes
Sensor 4 is located at the drop 15, and the size and feedback signal for incuding drop 15 are to controller 3, the active tunnel 10
One end is fixedly connected with 100 microlitres of syringe pumps 1 of moist fluid board, and the other end can be individually connected to by the rotation process of switching valve 9
The other end of collection channel 11 or taking liquid passage 12, taking liquid passage 12 is connected with extracting head 21, collection channel 11 it is another
One end is connect with micro-collection bottle 13, so that 100 microlitres of syringe pumps 1 of fluid board of moistening are moved according to experimental program in due course or periodically
It takes in drop 15 to micro-collection bottle 13.The instillation micro-extraction unit B is by extraction chamber 20 and the extraction being arranged in extraction chamber 20
First 21 composition is taken, the extracting head 21 is back taper, and the top of extracting head 21 is enclosed construction and extends to extraction chamber 20
Outside, the bottom of extracting head 21 are necking, and the top of extracting head 21 passes through liquid capillary road and 10 milliliters of moist fluid board notes
2 connection of pump is penetrated, the top of extracting head 21 also passes through liquid capillary road and communicates with taking liquid passage 12, described and taking liquid passage 12
The liquid capillary road lower end communicated extends at the necking of extracting head 21, and spiral liquid support is equipped at the necking of the extracting head 21
22, the inner end of the spiral liquid support 22 is located in 21 necking of extracting head, and the outer end of spiral liquid support 22 extends to 21 necking of extracting head
It is external.The extraction chamber 20 is separately connected the thermal analyzer C of Switzerland's Mettler Toledo brand TGA/DSC 3+ model and interior
Adding unit D is marked, the rear positions that drop 15 is located on extraction chamber 20 are equipped with the tail that offgas outlet 19 is used to discharge evolution
Gas.It include furnace body 16, balance arm in the thermal analyzer C of the Switzerland Mettler Toledo brand TGA/DSC 3+ model
18 and crucible 17；The balance arm 18 and crucible 17 are placed in furnace body 16, and the crucible 17 is placed on balance arm 18, the furnace body
16 have Program for precision temperature controlling function；The balance arm 18 is for detecting the mass change of sample in Temperature Programmed Processes and leading to
Cross embedded thermocouple test sample thermal change, the heat of the Switzerland Mettler Toledo brand TGA/DSC 3+ model
Analyzer C can measure sample quality and temperature change relationship by balance arm 18 under programed temperature, provide specific load
Under the conditions of gas in Temperature Programmed Processes sample thermal decomposition information；The Switzerland Mettler Toledo brand TGA/DSC 3+ type
Number the carrier gas of thermal analyzer C can carry the thermal decomposition product evolution furnace body 16 that sample volatilizes in temperature-rise period, along gas
Body pipeline enters instillation micro-extraction unit B.The internal standard adding unit D include conical flask 5, inner mark solution 6, magnetic stirring apparatus 7,
Stirring rod 8, conical flask 5 are placed on magnetic stirring apparatus 7, and inner mark solution 6, stirring rod 8 are placed in conical flask 5, the magnetic agitation
Device 7 adjusts the mixing speed of inner mark solution 6 in conical flask 5 by controlling the rotation speed of stirring rod 8, and reaching makes inner mark solution
The purpose of 6 normalizations everywhere；5 top of conical flask is separately connected external carrier gas N by gas piping2With micro- extraction that instils
Take unit B, external carrier gas N2Into 5 post-purge inner mark solution of conical flask, 6 surface and carries the internal standard compound that volatilizes and leave taper
Bottle 5, enters instillation micro-extraction unit B along gas piping.The lower part of 13 inner surface of micro-collection bottle is V-arrangement, is convenient for body
The lesser drop 15 of product is extracted in late detection by sample introduction needle.
Carry out the instillation micro-extraction experimental procedure of glucose pyrolysis evolution component using the present invention:
A. prepare glucose sample first and pulverized with mortar；
B. 200mL alcohol extraction liquid 14 is used, moist fluid board is added to after 0.22 μm of organic phase filter membrane vacuumizing filtration
In 10 milliliters of syringe pumps 2；
C. 100 microlitres of syringe pumps 1 of moist fluid board are removed to be cleaned with extract liquor and dried up with pure air, accessed after emptying
System, rotating transfer valve 9 make active tunnel 10 be connected to taking liquid passage 12；
D. start drop control unit A, moist 10 milliliters of syringe pumps 2 of fluid board is promoted to make instillation micro-extraction unit B top
Full of extract liquor 14 and complete moist 10 milliliters of syringe pumps 2 of fluid board of pause propulsion after excluding gas；
E. 1000mL inner mark solution 6 is prepared according to volume ratio 1:999 with acetone and ethyl alcohol, pipettes 120mL and is added to taper
In bottle 5；
F. it is passed through high pure nitrogen 99.999% for conical flask 5, nitrogen flow 600mL/min is set, start magnetic stirring apparatus
7, setting speed 200r/min；
G. the thermal analyzer C for starting Switzerland Mettler Toledo brand TGA/DSC 3+ model, is added in crucible 17
Glucose sample, setting heat analysis temperature program(me) are heated to 900 DEG C from 40 DEG C with 10 DEG C/min heating rate, and setting carrier gas is
Pure air, flow 100mL/min；
H. after the starting of sample temperature program, controller 3 controls moist 10 milliliters of syringe pumps 2 of fluid board in instillation micro-extraction list
First B automatically forms drop 15；
I. with the progress that instillation micro-extraction is tested, when drop 15 by carrier gas purge and volume become smaller when, drop control is single
First 15 size of A automatic sensing drop and automatic liquid supply, make drop 15 remain full state；
J. when sample is warming up to 100 DEG C, 10 milliliters of syringe pumps 2 of moist fluid board is paused immediately and start moist fluid board
100 microlitres of syringe pumps 1 extract drop 15, and then rotating transfer valve 9 makes active tunnel 10 be connected to collection channel 11, controller 3
Moist 100 microlitres of syringe pumps 1 of fluid board are controlled to be discharged in 15 to No. I micro-collection bottles 13 of drop；
K. it is 5 seconds time-consuming to extract 15 process of drop, immediately starts moist 10 milliliters of syringe pumps 2 of fluid board and generates drop
15 continue the instillation micro-extractions operation of second segment, and rotating transfer valve 9 makes active tunnel weigh 10 to be newly connected to taking liquid passage
12；
L. the control process for repeating i step, j step, k step, every drop 15 of 20 DEG C of collections, until sample temperature is super
Stop collecting drop 15 when crossing 600 DEG C；
M.100 it is collected into 26 drops 15 altogether in DEG C -600 DEG C of sample temperature-rise periods and is sub-packed in 26 micro-collection bottles 13
In, then each drop 15 is tested and analyzed with liquid chromatogram-triple tandem quadrupole mass spectrograph.
The instillation micro-extraction is to carry the carrier gas continuously flowed of component to be measured constantly to purge drop 15, be component to be measured
The micro-extraction process that dynamic equilibrium is realized between carrier gas and drop 15, is that a drop 15 is constantly purged and persistently volatilized by carrier gas
And incuded and the volume dynamic changing process of continuous supplementation by the drop control unit A moment.
Claims (7)
1. the instillation micro-extraction device for thermal analyzer evolution component analysis, it is characterised in that: including for controlling drop
(15) size and periodically collect drop (15) drop control unit (A), for carrying out instillation micro-extraction and being enriched with object
Instillation micro-extraction unit (B) in drop (15), for carry sample and carry out heat analysis thermal analyzer (C), for for
The internal standard adding unit (D) of carrier gas addition volatility internal standard compound, the micro-collection bottle (13) for holding drop (15) all the way；Institute
The liquid replenisher (2) stated in drop control unit (A) passes through the extracting head in liquid capillary road and instillation micro-extraction unit (B)
(21) it communicates, the switching valve (9) in drop control unit (A) is connect with micro-collection bottle (13), in instillation micro-extraction unit (B)
Extraction chamber (20) be separately connected thermal analyzer (C) and internal standard adding unit (D).
2. the instillation micro-extraction device according to claim 1 for thermal analyzer evolution component analysis, it is characterised in that:
The drop control unit (A) includes liquid getting device (1), liquid replenisher (2), controller (3), fibre-optical probe (4) and switching valve (9),
The controller (3) is separately connected and controls liquid getting device (1), liquid replenisher (2) and fibre-optical probe (4), in the switching valve (9)
Equipped with (12) three active tunnel (10), collection channel (11) and taking liquid passage channels, the liquid getting device (1) passes through liquid capillary
Pipeline be connected with switching valve (9) and by the active tunnel (10) on switching valve (9) according to circumstances with collection channel (11) or
Taking liquid passage (12) communicates, and the liquid replenisher (2) passes through the extracting head (21) on liquid capillary road and instillation micro-extraction unit (B)
Top communicate, and carry out according to the feedback signal of fibre-optical probe (4) fluid infusion operation to maintain the size of drop (15), it is described
Fibre-optical probe (4) is located at drop (15), and the size and feedback signal for incuding drop (15) are to controller (3), institute
It states active tunnel (10) one end to be fixedly connected liquid getting device (1), the other end can be individually connected to by the rotation process of switching valve (9)
The other end of collection channel (11) or taking liquid passage (12), taking liquid passage (12) is connected with extracting head (21), collection channel
(11) the other end is connect with micro-collection bottle (13), so that liquid getting device (1) pipettes liquid according to experimental program in due course or periodically
It drips in (15) to micro-collection bottle (13).
3. the instillation micro-extraction device according to claim 1 for thermal analyzer evolution component analysis, it is characterised in that:
The instillation micro-extraction unit (B) is made of the extracting head (21) of extraction chamber (20) and setting in extraction chamber (20), described
Extracting head (21) is back taper, and the top of extracting head (21) is enclosed construction and the outside for extending to extraction chamber (20), extracting head
(21) bottom is necking, and the top of extracting head (21) is connected to by liquid capillary road with liquid replenisher (2), extracting head (21)
Top also passes through liquid capillary road and communicates with taking liquid passage (12), the liquid capillary road communicated with taking liquid passage (12)
Lower end extends at the necking of extracting head (21), and the extraction chamber (20) is separately connected thermal analyzer (C) and internal standard adding unit
(D), the rear positions that drop (15) are located in extraction chamber (20) are equipped with the tail gas that offgas outlet (19) are used to discharge evolution.
4. the instillation micro-extraction device according to claim 1 for thermal analyzer evolution component analysis, it is characterised in that:
The internal standard adding unit (D) includes conical flask (5), inner mark solution (6), magnetic stirring apparatus (7), stirring rod (8), conical flask
(5) it is placed on magnetic stirring apparatus (7), inner mark solution (6), stirring rod (8) are placed in conical flask (5), the magnetic stirring apparatus (7)
The mixing speed of inner mark solution (6) in conical flask (5) is adjusted by controlling the rotation speed of stirring rod (8), reaching makes internal standard
The purpose of solution (6) normalization everywhere；Conical flask (5) top is separately connected external carrier gas N by gas piping2With
Instillation micro-extraction unit (B), external carrier gas N2It is volatilized into conical flask (5) post-purge inner mark solution (6) surface and carrying
Internal standard compound leaves conical flask (5), enters instillation micro-extraction unit (B) along gas piping.
5. the instillation micro-extraction device according to claim 1 for thermal analyzer evolution component analysis, it is characterised in that:
The lower part of micro-collection bottle (13) inner surface be V-arrangement, convenient for small volume drop (15) in late detection by sample introduction
Needle extracts.
6. the instillation micro-extraction device according to claim 2 for thermal analyzer evolution component analysis, it is characterised in that:
The liquid getting device (1) and liquid replenisher (2) are syringe pump.
7. the instillation micro-extraction device according to claim 3 for thermal analyzer evolution component analysis, it is characterised in that:
Spiral liquid support (22) is equipped at the necking of the extracting head (21), the inner end of the spiral liquid support (22) is located at extracting head (21) contracting
In mouthful, the outer end of spiral liquid support (22) is extended to outside extracting head (21) necking.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109060869A (en) * | 2018-10-15 | 2018-12-21 | 海南红塔卷烟有限责任公司 | Instillation micro-extraction device and method for thermal analyzer evolution component analysis |
| WO2023284346A1 (en) * | 2021-07-15 | 2023-01-19 | 长视科技股份有限公司 | Method for detecting polycyclic musks in water body |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109060869A (en) * | 2018-10-15 | 2018-12-21 | 海南红塔卷烟有限责任公司 | Instillation micro-extraction device and method for thermal analyzer evolution component analysis |
| WO2023284346A1 (en) * | 2021-07-15 | 2023-01-19 | 长视科技股份有限公司 | Method for detecting polycyclic musks in water body |
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