CN207081656U - A kind of volatile matter prepares collection device - Google Patents
A kind of volatile matter prepares collection device Download PDFInfo
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- CN207081656U CN207081656U CN201721028539.3U CN201721028539U CN207081656U CN 207081656 U CN207081656 U CN 207081656U CN 201721028539 U CN201721028539 U CN 201721028539U CN 207081656 U CN207081656 U CN 207081656U
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Abstract
The utility model discloses a kind of volatile matter to prepare collection device, including volatile matter preparation facilities and volatile matter collection device；The volatile matter preparation facilities includes volatile matter and prepares container and the heater for preparing container heating to the volatile matter, the volatile matter prepares the container lid that container includes vessel, is adapted with the vessel, the container lid is provided with volatiles outlet and inert gas entrance, inert gas input pipe is connected with the inert gas entrance, the lower end of the inert gas input pipe is passed through and extends to the bottom of the vessel；The volatiles outlet is connected to one end of volatile matter escape pipe, and the other end of the volatile matter escape pipe is connected with the volatile matter collection device.Device described in the utility model have device is simple, cost is low, exploitativeness is strong, analysis sample size is big, prepare and collection efficiency is high, the volatile component collected comprehensively, the strong advantage of scope can be expanded.
Description
Technical field
It the utility model is related to a kind of volatile matter and prepare collection device, produced by especially a kind of polymer processing
Volatile matter prepares collection device.
Background technology
Polymeric material understands residual monomer and catalyst in preparation process or adds some function additives, such as fire-retardant
Agent, antioxidant etc., molecular weight is smaller, and the monomer or function additive of residual and low-molecular weight polymer etc. add in polymer twin-screw
It in work or injection molding process, can evaporate, run into the relatively low metal die meeting condensation of temperature, stick in die surface,
As processing modulus increases, slowly mold deposit is formed, it is necessary to periodic cleaning, not only have impact on the efficiency of material processing, but also
The outward appearance of polymeric material shaping can be influenceed.
Evaluation for similar volatile matter, there are the TVOC of some test total carbon contents Static Headspace methods at present, using adding
Under heat to specified temp, after constant temperature special time, solid and gas reaches balance, then carries out test analysis to the admixture of gas of volatilization,
It is generally used for the polypropylene material that automobile uses；But because heated temperature conditionss (conventional 120 DEG C of temperature) influence, for adding
The volatile matter evaluation of the higher engineering plastics of work temperature is related to less, and the sample size evaluated only has 1.2g, and is heated to gas-solid
Balance, take longer；Similar atomization measure in addition, due to the influence of heated carrier silicone oil, heating-up temperature is difficult adjustment
To higher processing temperature, and the method can only collect a certain degree of volatile component, and for incondensible gas group
Dividing to collect.
Publication No. CN 102514158A patent, Publication No. CN202412592U patent individually discloses one kind
The collection method of injection mold and slide to the volatile matter of polymeric material, but both approaches are utilized in injection molding process
There is following weak point：First, needing to be collected by injection mold in injection moulding process, polymeric material is not carried out
The injection molding of evaluation before to(for) polymeric material volatile matter is less applicable；Two be due to that mould gas port is smaller and slide
Area is smaller to cause the sample size for collecting volatile matter less；Comparatively practicality and enforcement difficulty are easily limited by condition
System.Publication No. CN106501426A patent discloses a kind of Seedling Stage soya bean plant volatiles for feeling poisonous insect damage induction and received
Diversity method, be collected primarily directed to the volatile matter of plant, and need be collected by solid phase micro-extraction device, and temperature compared with
Low, preparation and collection for volatile matter condensed components in polymeric material process are less applicable.
Produced volatile matter in polymer processing is collected, and carries out qualitative and quantitative analysis, can be polymerization
Abnormal cause lookup in thing process is given a clue and direction, further improves formula and technique, processability are more preferable
Material.
Utility model content
In consideration of it, the purpose of this utility model is to overcome above-mentioned the deficiencies in the prior art part and provide a kind of volatile matter
Collection device is prepared, described device is simple, cost is low, volatile matter collection is accurate fully, can be to the volatilization under different processing temperatures
Thing is collected.
To achieve the above object, technical solution adopted in the utility model is：A kind of volatile matter prepares collection device, bag
Include volatile matter preparation facilities and volatile matter collection device；
The volatile matter preparation facilities includes volatile matter and prepares container and for preparing container heating to the volatile matter
Heater, the volatile matter prepare the container lid that container includes vessel, is adapted with the vessel, the appearance
Device lid is provided with volatiles outlet and inert gas entrance, and inert gas input pipe is connected with the inert gas entrance,
The lower end of the inert gas input pipe is passed through and extends to the bottom of the vessel；
The volatiles outlet is connected to one end of volatile matter escape pipe, the other end of the volatile matter escape pipe with it is described
Volatile matter collection device connects.
The utility model provides a kind of condition and preparation method that volatile matter can be produced with replica polymerization thing process
With the device of caused volatile matter in comprehensive collection polymeric material process；Solves other method analysis sample size not
Foot, volatile matter collect the problem of incomplete, preparation efficiency is relatively low, and not equality of temperature can be collected by temperature regulating device in the utility model
The condensate and gas component of the lower volatile matter of degree, the volatile matter of collection is carried out with instrumental method to the composition of volatile matter qualitative
Quantitative analysis, the lookup for abnormal cause is given a clue and direction, further improves formula and technique, the more preferable material of processability
Material.The utility model can be widely applied in the process of various most of macromolecule polymer materials produce the system of volatile matter
Standby and collection, further completes the constituent analysis of volatile matter according to the component of collection.
The bottom that the lower end of the inert gas input pipe was passed through and extended to the vessel is passed through to utilize
Inert gas, preferably discharge vessel in volatile matter.
Furthermore it is noted that the utility model can use torque rheometer to prepare the volatile component under dynamic,
And the collection of volatile matter is completed using similar device.
Sample in the utility model can be ABS and its alloy sample, and engineering plastics and its engineering plastic alloy
The polymeric materials such as sample；Sample size typically needs 5-100g, and the testing time need to typically keep 50min- at processing temperatures
150min, ensure that volatile matter fully evaporates.
Container lid described in the utility model needs and the vessel bore matches, and ensures preferable sealing, makes
Volatile matter completely passes through the container lid as far as possible, and then collects the condensed components of volatile matter, and uncondensed components are by volatilization
Thing escape pipe is flowed into volatile matter collection device.
Preferably, the container lid is ground container lid.
Preferably, the container lid is provided with temperature control device.
It is highly preferred that the temperature control device is water-circulating pipe, the water-circulating pipe is in the container lid from the appearance
The side of device lid extends to the opposite side of the container lid.
The design of the water-circulating pipe, temperature that can accurately at control container lid make the condensed components of sample more
Good condensation, reduces the loss of volatile matter and condensate, further ensures the accuracy of collection.
Preferably, the heater includes heating plate and the heating mantle in the heating plate；The volatile matter system
Standby container is in the heating mantle of the heater.
It is highly preferred that contain one kind in water, oil, sand in the heating mantle.
Heater described in the utility model need to be can be with the electric heating cover of precise control of temperature, electric boiling plate etc., temperature
Scope is wide, and water-bath, oil bath, sand-bath can be needed to use to carry out the condensation group of the volatile matter under preparation different temperatures according to difference
Point and gas component；Temperature range is 30-550 DEG C, can suitably be adjusted according to the scope of processing temperature.
Preferably, the volatile matter collection device is at least one of gas collector, fluid collection device；
The gas collector includes gas collection bag, and the gas collection bag connects with the volatile matter escape pipe；
The fluid collection device includes at least two liquid collecting containers, between at least two liquid collecting container
Connected by connecting tube, volatile matter import is equipped with least two liquid collecting container；The volatile matter escape pipe
One end is passed through the bottom of one of liquid collecting container by its volatile matter import.
Collection device of the present utility model is divided into two kinds of fluid collection device and gas collector, and every kind of collection device is all
There is control valve control, two kinds of collection devices can be used alone, can also be used together, and can specifically be set according to different analyses
The different control valve of standby opening is selected.
Preferably, the liquid collecting container includes polar solvent collection vessel and non-polar solution collection vessel.
Liquid collecting container described in the utility model, using rule of similarity, fully absorb caused by uncooled wave
Stimulating food；General liquid collecting container is respectively provided to 2 less, deposits polar solvent respectively and the collection vessel of non-polar solven is each
Place one, can also polar solvent place two collection vessels, non-polar solven place two collection vessels, ensure it is uncooled
Volatile component sufficiently absorbed.
Preferably, the gas collector includes the adsorption tube being connected with the gas collection bag and the adsorption tube
The flow pump of connection, filler is provided with the adsorption tube.
Gas collection bag in the utility model gas collector is collected to gas, and the gas being collected into can be straight
Tap into and analyzed into gas chromatography, after can also being adsorbed by the adsorption tube of specific filler, then filled by thermal desorption
Qualitative and quantitative analysis is carried out in putting into gaschromatographic mass spectrometry, this has expanded comprehensive analysis method of volatile matter.
It is highly preferred that the gas collector includes at least two adsorption tubes, one end of at least two adsorption tube
It is connected respectively with the gas collection bag, the other end of at least two adsorption tube is connected to flow pump.
There is different adsorption stuffings in the adsorption tube according to different volatile gases, by flow pump below, enter
One step adsorbed gas.Because absorption of the filler in adsorption tube to volatilization gas often has targetedly, therefore, multiple suctions
Attached pipe can targetedly be absorbed for different volatile gases, be easy to follow-up qualitative and quantitative analysis.
Preferably, the volatile matter collection device includes gas collector and fluid collection device, the gas collection
Device, the fluid collection device connect with the volatile matter escape pipe.
Preferably, the outer surface of the volatile matter escape pipe is provided with muff.The setting of muff can be reduced further
Volatile matter is due to loss caused by condensation.
Preferably, the heating mantle of the heater, the gas collection bag of gas collector, the liquid of fluid collection device
Body collection vessel is fixed by iron stand.
Preferably, the vessel is glass container, and the volatile matter escape pipe is glass tube or polyfluortetraethylene pipe.
Liquid collecting container described in the utility model is generally ground silica ware, and can not have with sample chemical action or
Interference etc.；Described volatile matter escape pipe, inert gas input pipe are glass or polytetrafluoro tubes of material, will not be with volatilization produce
Raw effect, and volatile matter will not be produced under other circumstances.
Relative to prior art, the beneficial effects of the utility model are：
1) device is simple, and cost is low, and exploitativeness is strong, and analysis sample size is big, prepares and collection efficiency is high, the volatilization of collection
Thing component is comprehensive；
2) it is abundant to collect volatile constituent, condenses and gas component collects；
3) volatile matter under different processing temperatures can be prepared using the method；
4) volatile component obtained can carry out different types of qualitative and quantitative analysis, and it is strong can to expand scope.
Brief description of the drawings
Fig. 1 is a kind of structural representation that volatile matter described in the utility model prepares collection device；
Fig. 2 is a kind of structural representation of gas collection bag described in the utility model；
Fig. 3 is a kind of structural representation of gas collector described in the utility model；
Fig. 4 is a kind of structural representation that volatile matter described in the utility model prepares container；
Fig. 5 is the FTIR spectrum figure of the volatile matter condensed components of the utility model embodiment 1；
Fig. 6 is the GC-MS spectrograms of the volatile matter uncondensed components of the utility model embodiment 1；
Fig. 7 is the FTIR spectrum figure of the volatile matter condensed components of the utility model embodiment 2；
Fig. 8 is the GC-MS spectrograms of the volatile matter uncondensed components of the gas collection of the utility model embodiment 2；
Fig. 9 is the GC-MS spectrograms for the volatile matter uncondensed components that the liquid of the utility model embodiment 2 is collected；
Wherein, 1, heating plate；2nd, testing sample；3rd, vessel；4th, container lid；5th, volatile matter escape pipe；6th, threeway
One of them of pipe and the connector of gas collector；7th, connecting tube；8th, liquid collecting container；9th, polarity lyosoption；10、
Nonpolar lyosoption；11st, gas collection bag；12nd, gas collection bag support frame；13rd, the adsorption tube with filler；14th, threeway
Pipe；15th, flow pump；16th, inert gas input pipe；17th, heating mantle；18th, volatiles outlet；19th, inert gas entrance；20th, water
Circulation pipe；A, B, C, D represent iron stand.
Embodiment
To better illustrate the purpose of this utility model, technical scheme and advantage, below in conjunction with specific embodiment and attached
The utility model is described in further detail for figure.
Embodiment 1
Volatile matter described in the utility model prepares a kind of embodiment of collection device, and prepared by volatile matter described in the present embodiment receives
The structural representation of acquisition means is as shown in accompanying drawing 1 (closing the connector at 6 using control valve in accompanying drawing 1) and accompanying drawing 4：
Including volatile matter preparation facilities and volatile matter collection device (as shown in Figure 1)；
Volatile matter preparation facilities (as shown in Figure 4) prepares container including volatile matter and added for preparing container to volatile matter
The heater of heat, volatile matter prepare the container lid 4 that container includes vessel 3, is adapted with vessel 3, container cover
Son 4 is provided with volatiles outlet 18 and inert gas entrance 19, and it is defeated that inert gas (pure nitrogen gas) porch is connected with inert gas
Enter pipe (polyfluortetraethylene pipe) 16, the lower end of inert gas input pipe 16 is passed through and extends to the bottom of vessel 3；Volatile matter
Outlet is connected to one end of volatile matter escape pipe 5, and the other end of volatile matter escape pipe 5 is connected with volatile matter collection device, volatilizees
The outer surface of thing escape pipe 5 is provided with muff；
Container lid 4 is provided with temperature control device, is water-circulating pipe 20, water-circulating pipe is in container lid 4 from container lid 4
Side extend to the opposite side of container lid 4；
Heater includes heating plate 1 and the heating mantle 17 in heating plate 1；Volatile matter prepares container and filled located at heating
In the heating mantle 17 put, one kind in water, oil, sand is contained in heating mantle 17；
Volatile matter collection device is fluid collection device；Fluid collection device includes two liquid collecting containers 8, wherein one
Individual liquid collecting container is equipped with polarity lyosoption, and another liquid collecting container is equipped with nonpolar lyosoption, two liquid
Connected between collection vessel 8 by connecting tube 7, volatile matter import is equipped with two liquid collecting containers 8；Volatile matter escape pipe
5 one end is passed through the bottom of one of liquid collecting container 8 by its volatile matter import；
The heating mantle 17 of heater, the liquid collecting container 8 of fluid collection device are carried out by iron stand A, C, D respectively
It is fixed.
In certain modified ABS injection molding forming process is carried out, it is found that the open defect of spray occurs in product；Surveyed by the present apparatus
Try the volatile constituent of modified ABS at the process conditions.
Implementation process：
Volatile matter equipped with testing sample (12g flame-proof ABSs sample) is prepared container (ground quartz container) and is positioned over and is added
In thermal, the heating-up temperature of heater is adjusted to 240 DEG C, heated at constant temperature 60min, and volatile matter prepares container and prepares gained volatilization
Thing is divided into two parts, and the larger volatile component of molecular weight is agglomerated to container lid 4 (ground container lid) surface, and molecular weight is smaller
Uncooled volatile component fluid collection device is entered by volatile matter escape pipe 5, wherein, polarity volatile matter enters
Equipped with (the acetone liquid of polarity lyosoption 9：In liquid collecting container 8 80mL), nonpolar volatile matter is entered equipped with non-
(the n-hexane absorbing liquid of polarity lyosoption 10：In liquid collecting container 8 80mL).
After test terminates, 3-5min is cooled down, puts on protective gloves while hot by container lid 4 (ground container lid) and sample
Separated with vessel 3, liquid collecting container 8 and connecting tube 7 are separated, and be marked, in case other surveys below
Examination, can carry out the volatile matter being collected into infrared test analysis, and concrete analysis process is as follows：
1) condensed components are separated from container lid 4 (ground container lid) first, specifically from suitable
Solvent elutes to container lid 4 (ground container lid), condensed components is eluted into clean glass container, if container
Undissolved solid is still remained on lid 4 (ground container lid), then is taken the undissolved condensate using suitable spoon
Getting off, it is standby in clean culture dish to be placed in.
2) infrared spectrum analysis
2.1 weigh appropriate order of spectrum KBr into glass culture dish, are placed under infrared baking lamp, KBr is done
Dry processing；
2.2 take appropriate dried KBr to be placed in the agate ware of dried and clean, with grinding rod by the bromine in agate ware
It is levigate to change k particle；
2.3 take out KBr sample preparation tools, and are cleaned and drying process, reuse KBr sample preparation tool prepare it is empty
White kbr tablet is used for deducting the background infrared spectrum of KBr；
The preparation of 2.4 condensed components sample salt pieces：If condensed components can be completely dissolved, a blank bromine is prepared in addition
Change potassium piece, the solution dissolved with condensed components is added drop-wise on this blank bromination sylvite piece, dry, it is stand-by；If condensed components are deposited
In solid sample, then need to grind the solid sample and appropriate potassium bromide powder uniformly together, utilize KBr sample preparation tool system
The bromination sylvite piece of standby testing sample；
The test of 2.5 testing sample salt pieces：Fourier infrared spectrograph device parameter and sample ID are set, take out drying
Next the bromination sylvite piece of testing sample is placed in FTIR spectrum by blank bromination sylvite piece to deduct air background
Tested in instrument, you can obtain the infrared spectrum of sample condensed components；
According to above-mentioned steps, the test result of the condensed components measured using Fourier infrared spectrograph is as shown in Figure 5；
2.6 data analysis：It was found from infrared spectrum is obtained：Wave number is 551cm-1、683cm-1Locate to shake for the flexible of C-Br
It is dynamic；700cm-1、760cm-1、813cm-1、858cm-1For C-H on phenyl ring after the substitutions of phenyl ring 1,2,3,5- tetra- of tribromophenoxy
Deformation vibration；1043cm-1、1157cm-1、1229cm-1For C-O stretching vibration；1273cm-1、1313cm-1Vibrate and inhale for C-N
Receive peak；1380cm-1For-CH3Scissoring vibration, 1457cm-1、1614cm-1Vibrated for the framework deformation of phenyl ring；1273cm-1、
1491cm-1、1550cm-1For the skeletal vibration of triazine ring；1659cm-1、1709cm-1For C=O stretching vibration；2925cm-1For
C-H stretching vibration；3077cm-1For the stretching vibration of C-H on phenyl ring；3486cm-1For O-H stretching vibrations；It is infrared more than
The analysis result of spectral signature absworption peak understands that the main component of condensed components is brominated triazine class material.
3) absorbing liquid-GC-MS is analyzed
The concentration of 3.1 absorbing liquids：The polarity lyosoption of two liquid collecting containers 8, nonpolar lyosoption are distinguished
It is transferred in round-bottomed flask, then carries out being concentrated into 10-15mL on a rotary evaporator；
3.2GC-MS test：The polarity lyosoption after 1.5-2.0mL concentrations, nonpolar lyosoption are taken in sample bottle
In, and prepare corresponding blank solution；It is placed on auto injection specimen holder, calls suitable analysis method, auto injection is set
Program, clicking on operation can be tested automatically, can obtain corresponding analysis result, as shown in Figure 6；
The analysis of 3.3 data
Obtained gaschromatographic mass spectrometry result is analyzed：Retention time is 7.511min, and mass-to-charge ratio m/z is 198, warp
Retrieval is understood, is C14 alkane；Retention time is 8.834min, and mass-to-charge ratio m/z is 226, is understood through retrieval, is C16 alkane
Hydrocarbon；Retention time is 9.99min, and mass-to-charge ratio m/z is 254.0, is understood through retrieval, is C18 alkane；Retention time is
12.691min, mass-to-charge ratio m/z are 281.0, are understood through retrieval, are erucyl amide composition；Retention time is 17.134min, matter lotus
It is 646.0 than m/z, is understood through analysis, be organic phosphite composition.
Embodiment 2
Volatile matter described in the utility model prepares a kind of embodiment of collection device, and prepared by volatile matter described in the present embodiment receives
The structural representation of acquisition means is as shown in accompanying drawing 1~4：
Including volatile matter preparation facilities and volatile matter collection device (as shown in Figure 1)；
Volatile matter preparation facilities (as shown in Figure 4) prepares container including volatile matter and added for preparing container to volatile matter
The heater of heat, volatile matter prepare the container lid 4 that container includes vessel 3, is adapted with vessel 3, container cover
Son 4 is provided with volatiles outlet 18 and inert gas entrance 19, and inert gas input pipe 16 is connected with inert gas entrance 19,
The lower end of inert gas input pipe 16 is passed through and extends to the bottom of vessel 3；Volatiles outlet is connected to volatile matter outlet
One end of pipe 5, the other end of volatile matter escape pipe 5 are connected with volatile matter collection device, and the outer surface of volatile matter escape pipe 5 is provided with
Muff；
Container lid 4 is provided with temperature control device, is water-circulating pipe 20, water-circulating pipe is in container lid 4 from container lid 4
Side extend to the opposite side of container lid 4；
Heater includes heating plate 1 and the heating mantle 17 in heating plate 1；Volatile matter prepares container and filled located at heating
In the heating mantle 17 put, one kind in water, oil, sand is contained in heating mantle 17；
Volatile matter collection device (as shown in Figure 1) includes gas collector and fluid collection device, gas collection dress
Put and connected with fluid collection device by three-way pipe 14 with volatile matter escape pipe 5, three connectors of three-way pipe 14 respectively with gas
Body collection device, fluid collection device connection；Gas collector (as shown in Figure 3) includes gas collection bag 11 and gas
Adsorption tube 13 that collecting bag 11 connects, the flow pump 15 that is connected with adsorption tube 13, filler, gas collection bag are provided with adsorption tube 13
11 are connected with volatile matter escape pipe 5 by one of them of three-way pipe with the connector 6 of gas collector；Fluid collection device
Including two liquid collecting containers 8, connected between two liquid collecting containers 8 by connecting tube 7, two liquid collecting containers 8
On be equipped with volatile matter import；One end of volatile matter escape pipe 5 is passed through one of liquid and collected by its volatile matter import to hold
The bottom of device 8；
The heating mantle 17 of heater, the gas collection bag 11 of gas collector, the liquid of fluid collection device are collected
Container 8 is fixed by iron stand A, B, C, D respectively.
In certain modified engineered plastic injection molding process is carried out, after finding shaping certain amount product, die surface is residual
Stay more mold deposit；Certain modified engineered plastic volatile matter at the process conditions is tested by the present apparatus and condenses composition and uncooled
Volatile gas composition.
Implementation process：
Volatile matter equipped with testing sample (the fire-retardant PPE samples of 62g) is prepared container (ground quartz container) and is positioned over and is added
In thermal, the heating-up temperature of heater is adjusted to 300 DEG C, heated at constant temperature 50-60min, and volatile matter prepares container and prepares gained
Volatile matter is divided into two parts, and the larger volatile component of molecular weight is agglomerated to container lid 4 (ground container lid) surface, molecular weight
Less volatile component is entered in gas collection bag 11 by the junction 6 of volatile matter escape pipe and gas collector；
Meanwhile the less uncooled volatile component of molecular weight can also enter fluid collection device by volatile matter escape pipe 5,
Wherein, polarity volatile matter is entered equipped with (the acetone liquid of polarity lyosoption 9：In liquid collecting container 8 80mL), non-pole
Property volatile matter is entered equipped with nonpolar (the n-hexane absorbing liquid of lyosoption 10：In liquid collecting container 8 80mL).
1) volatile matter condensation constituent analysis
After test terminates, 3-5min is cooled down, puts on protective gloves while hot by container lid 4 (ground container lid) and container
Body 3 is separated, and liquid collecting container 8 and connecting tube 7 are separated, gas collection bag 11 and three-way pipe one of them with
The connector 6 of gas collector separates, and is marked, in case other tests below, volatile matter condensation composition is entered
Row infrared spectrum analysis, specific analytical method are as shown in Figure 7 with the method in embodiment 1, analysis result：
It was found from infrared spectrum is obtained：Wave number is 700cm-1Locate to absorb for the out-of-plane bending vibration of C-H on phenyl ring；903cm-1、1026cm-1For P-O-C absorption of vibrations；966cm-1、1162cm-1、1188cm-1For P-O vibration absorption peak；1225cm-1
For C-P vibration absorption peaks；1362cm-1For CH3Deformation vibration the absworption peak；1267cm-1、1295cm-1For P=O absworption peak；
1455cm-1、1490cm-1For the upper C-C stretching vibrations of phenyl ring；1511cm-1、1552cm-1For phenyl ring skeleton C=C stretching vibrations；
1491cm-1、1592cm-1For C-H vibration absorption peaks on phenyl ring；1708cm-1For C=O stretching vibration；2858cm-1、2929cm-1、2959cm-1For-CH2- the stretching vibration with-CH；3026cm-1、3061cm-1For the stretching vibration of C-H on phenyl ring；According to
The analysis result of upper ft-ir characteristic absorption peak understands that the main component of condensed components is phosphenylic acid esters material.
2) gas collection analysis-GC-MS is analyzed
The absorption of 2.1 gases：By flow pump 15, the adsorption tube 13 with filler is set to adsorb 500mL gases, and use lid
Seal adsorption tube 13；
2.2GC-MS test：Take the adsorption tube of adsorption sample to carry out examination with computer, and prepare corresponding blank；It is placed in certainly
On dynamic sample introduction sample frame, suitable analysis method is called, auto injection program is set, clicking on operation can be tested automatically,
Corresponding analysis result can be obtained, as shown in Figure 8；
The analysis of 2.3 data：
Analyze obtaining gaschromatographic mass spectrometry result：Retention time is 6.817min, and mass-to-charge ratio m/z is 90.9, warp
Retrieval is understood, is toluene composition；Retention time is 7.632min, and mass-to-charge ratio m/z is 103.9, is understood through retrieval, be styrene into
Point；Retention time is 8.114min, and mass-to-charge ratio m/z is 94.0, is understood through retrieval, is phenol component.
3) absorbing liquid-GC-MS is analyzed
The concentration of 3.1 absorbing liquids：The polarity lyosoption of two liquid collecting containers 8, nonpolar lyosoption are distinguished
It is transferred in round-bottomed flask, then carries out being concentrated into 10-15mL on a rotary evaporator；
3.2GC-MS test：The polarity lyosoption after 1.5-2.0mL concentrations, nonpolar lyosoption are taken in sample bottle
In, and prepare corresponding blank solution；It is placed on auto injection specimen holder, calls suitable analysis method, auto injection is set
Program, clicking on operation can be tested automatically, can obtain corresponding analysis result, as shown in Figure 9；
The analysis of 3.3 data：
Analyze obtaining gaschromatographic mass spectrometry result：Retention time is 6.817min, and mass-to-charge ratio m/z is 90.9, warp
Retrieval is understood, is toluene composition；Retention time is 7.632min, and mass-to-charge ratio m/z is 103.9, is understood through retrieval, be styrene into
Point；Retention time is 8.120min, and mass-to-charge ratio m/z is 94.0, is understood through retrieval, is phenol component；Retention time is
18.165min, mass-to-charge ratio m/z are 325.7, are understood through retrieval, are phosphenylic acid esters chemical composition；Retention time is
18.886min, mass-to-charge ratio m/z are 311.9, are understood through retrieval, are phenyl oxaza class chemical composition.
Finally, it should be noted that above example is only illustrating the technical solution of the utility model rather than to this reality
With the limitation of novel protected scope, although being explained in detail with reference to preferred embodiment to the utility model, this area it is common
It will be appreciated by the skilled person that the technical solution of the utility model can be modified or equivalent substitution, without departing from this reality
With the spirit and scope of new technique scheme.
Claims (10)
1. a kind of volatile matter prepares collection device, it is characterised in that including volatile matter preparation facilities and volatile matter collection device；
The volatile matter preparation facilities includes volatile matter and prepares container and the heating for preparing container heating to the volatile matter
Device, the volatile matter prepare the container lid that container includes vessel, is adapted with the vessel, the container cover
Son is provided with volatiles outlet and inert gas entrance, and inert gas input pipe is connected with the inert gas entrance, described
The lower end of inert gas input pipe is passed through and extends to the bottom of the vessel；
The volatiles outlet is connected to one end of volatile matter escape pipe, the other end and the volatilization of the volatile matter escape pipe
Thing collection device connects.
2. volatile matter as claimed in claim 1 prepares collection device, it is characterised in that the container lid fills provided with temperature control
Put.
3. volatile matter as claimed in claim 2 prepares collection device, it is characterised in that the temperature control device is water-circulating pipe,
The water-circulating pipe extends to the opposite side of the container lid in the container lid from the side of the container lid.
4. volatile matter as claimed in claim 1 prepares collection device, it is characterised in that the heater include heating plate and
Heating mantle in the heating plate；The volatile matter prepares container in the heating mantle of the heater.
5. volatile matter as claimed in claim 4 prepares collection device, it is characterised in that contains water, oil, sand in the heating mantle
In one kind.
6. volatile matter as claimed in claim 1 prepares collection device, it is characterised in that the volatile matter collection device is gas
At least one of collection device, fluid collection device；
The gas collector includes gas collection bag, and the gas collection bag connects with the volatile matter escape pipe；
The fluid collection device includes at least two liquid collecting containers, passes through between at least two liquid collecting container
Connecting tube is connected, and volatile matter import is equipped with least two liquid collecting container；One end of the volatile matter escape pipe
The bottom of one of liquid collecting container is passed through by its volatile matter import.
7. volatile matter as claimed in claim 6 prepares collection device, it is characterised in that the gas collector include with it is described
Adsorption tube, the flow pump that is connected with the adsorption tube of gas collection bag connection, filler is provided with the adsorption tube.
8. volatile matter as claimed in claim 7 prepares collection device, it is characterised in that the gas collector includes at least two
Individual adsorption tube, one end of at least two adsorption tube are connected with the gas collection bag respectively, at least two adsorption tube
The other end be connected to flow pump.
9. the volatile matter as described in claim 6,7 or 8 prepares collection device, it is characterised in that the volatile matter collection device
Including gas collector and fluid collection device, the gas collector, the fluid collection device with the volatilization
Thing escape pipe connects.
10. the volatile matter as described in claim 1 or 6 prepares collection device, it is characterised in that outside the volatile matter escape pipe
Surface is provided with muff.
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| CN107356697A (en) * | 2017-08-16 | 2017-11-17 | 金发科技股份有限公司 | A kind of volatile matter prepares collection device |
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| CN107356697A (en) * | 2017-08-16 | 2017-11-17 | 金发科技股份有限公司 | A kind of volatile matter prepares collection device |
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