CN109142566A - The separation method and measuring method of automotive upholstery volatile matter methacrylaldehyde and acetone - Google Patents
The separation method and measuring method of automotive upholstery volatile matter methacrylaldehyde and acetone Download PDFInfo
- Publication number
- CN109142566A CN109142566A CN201810852178.7A CN201810852178A CN109142566A CN 109142566 A CN109142566 A CN 109142566A CN 201810852178 A CN201810852178 A CN 201810852178A CN 109142566 A CN109142566 A CN 109142566A
- Authority
- CN
- China
- Prior art keywords
- acetone
- methacrylaldehyde
- dnph
- mobile phase
- proportion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 title claims abstract description 289
- STNJBCKSHOAVAJ-UHFFFAOYSA-N Methacrolein Chemical compound CC(=C)C=O STNJBCKSHOAVAJ-UHFFFAOYSA-N 0.000 title claims abstract description 202
- 238000000926 separation method Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 62
- 150000001299 aldehydes Chemical class 0.000 claims abstract description 45
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 37
- 238000010586 diagram Methods 0.000 claims abstract description 34
- 230000000694 effects Effects 0.000 claims abstract description 34
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 72
- 239000012071 phase Substances 0.000 claims description 46
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 9
- 239000007791 liquid phase Substances 0.000 claims description 8
- 239000012074 organic phase Substances 0.000 claims description 8
- 238000003556 assay Methods 0.000 claims description 4
- 239000003085 diluting agent Substances 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 8
- 238000012360 testing method Methods 0.000 abstract description 4
- ZTQMSNSOJSROMU-UHFFFAOYSA-N CC(C)=O.CC(=C)C=O Chemical compound CC(C)=O.CC(=C)C=O ZTQMSNSOJSROMU-UHFFFAOYSA-N 0.000 abstract description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- -1 aldehyde ketone Chemical class 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- 238000004128 high performance liquid chromatography Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 150000002894 organic compounds Chemical class 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- HORQAOAYAYGIBM-UHFFFAOYSA-N 2,4-dinitrophenylhydrazine Chemical compound NNC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O HORQAOAYAYGIBM-UHFFFAOYSA-N 0.000 description 3
- 238000007445 Chromatographic isolation Methods 0.000 description 3
- 238000003915 air pollution Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- MLUCVPSAIODCQM-NSCUHMNNSA-N crotonaldehyde Chemical compound C\C=C\C=O MLUCVPSAIODCQM-NSCUHMNNSA-N 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 208000002173 dizziness Diseases 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 239000002649 leather substitute Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229960002715 nicotine Drugs 0.000 description 1
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 210000005239 tubule Anatomy 0.000 description 1
Classifications
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses the separation method and measuring method of a kind of automotive upholstery volatile matter methacrylaldehyde and acetone, separation method includes: that the aldehyde ketone-DNPH that configuration concentration is 1mg/L mixes standard liquid, and injects the chromatographic column of liquid chromatograph；According to the appearance time of chromatography waveform diagram and peak shape and methacrylaldehyde acetone separation effect, under the conditions of identical sample volume, detector wavelength, column temperature and proportion of mobile phase, selection target flow velocity；Under the conditions of identical sample volume, detector wavelength, flow velocity and proportion of mobile phase, selection target column temperature；Under the conditions of identical sample volume, detector wavelength, flow velocity and column temperature, selection target proportion of mobile phase；According to target flow rate, target column temperature, target proportion of mobile phase, methacrylaldehyde is separated with acetone.The present invention just uses the separating effect of liquid chromatogram acetone and methacrylaldehyde to test, and according to the factors such as the appearance time of substance, peak shape, resolution under different condition, determines optimal separation detection condition.
Description
Technical field
The present invention relates to vapour to examine field, in particular to a kind of separation method of automotive upholstery volatile matter methacrylaldehyde and acetone
And measuring method.
Background technique
In recent years, with the fast development of domestic automobile industry and automobile industry, automobile interior part materials are more and more extensive,
In-car air quality gradually attracts people's attention.In-vehicle air pollution source mainly includes material for car interior trim parts, such as artificial
Leather, textile fabric, a series of pollution sources such as plastics.The formaldehyde that these pollution sources are discharged, acetaldehyde, methacrylaldehyde, etc. volatility have
Amine, the nicotine that machine object (VOC) and air conditioning for automobiles operation generate.Wherein the organic compound (VOC) of car room volatilization is shadow
The main reason for ringing the quality of in-vehicle air, this can lead to, and driver is dizzy, has a headache, the central nervous system uncomfortable in chest, out of strength for making people
System is suppressed, and serious that driver is caused to faint and be poisoned, this will cause the life property safety of driver and passenger
Great security risk.For this purpose, the content of the organic compound of monitoring material for car interior trim parts volatilization, is conducive to monitor in automobile
Gadget material is more environmentally protective.
As the research of automotive air pollution object harm to the human body is goed deep into China, specify that automotive upholstery volatilizees
Organic compound include a series of organic compounds such as formaldehyde, acetaldehyde, methacrylaldehyde, acetone, benzene homologues, publication is " interior empty
Makings amount evaluation guide " and provide the substances such as formaldehyde, acetaldehyde, methacrylaldehyde, benzene homologues be can quantitative detection pollutant, it is " interior
Volatile organic matter and aldehyde ketone substance sampling determination method " it is middle using in high performance liquid chromatography (HPLC) measurement in-vehicle air
Group compounds of aldehydes and ketones.By the gas containing aldehyde ketone by coating 2,4-dinitrophenylhydrazine (DNPH) sampling tubule, aldehyde ketone with
2,4-dinitrophenylhydrazine generates stable hydrazone compounds, carries out qualitative, quantitative after being eluted with acetonitrile on high performance liquid chromatograph
Analysis.It finds in the analysis process, acetone and methacrylaldehyde molecular weight are close, ketone carbonyl (- CO-) and aldehyde radical (- CHO) functional group
Polarity is close, and when efficient liquid phase chromatographic analysis aldehyde ketone pollutant is difficult to separate in acetone and methacrylaldehyde, and then cannot be well
Determine the content of acetone and methacrylaldehyde.
Summary of the invention
In order to solve problems in the prior art, the present invention provides a kind of automotive upholstery volatile matter methacrylaldehyde and acetone
Separation method and measuring method can efficiently separate methacrylaldehyde and acetone, and testing result is accurate, and the technical solution is as follows:
The present invention provides the separation methods of a kind of automotive upholstery volatile matter methacrylaldehyde and acetone, comprising:
Using acetonitrile as diluent, the aldehyde ketone-DNPH that configuration concentration is 1mg/L mixes standard liquid；
Configured aldehyde ketone-DNPH is mixed to the chromatographic column of standard liquid injection liquid chromatograph；
Under the conditions of identical sample volume, detector wavelength, column temperature and proportion of mobile phase, flow velocity is adjusted, observes liquid phase color
The methacrylaldehyde of spectrometer output and the chromatography waveform diagram of acetone, according to the appearance time of the chromatography waveform diagram and peak shape and to third
The separating effect of olefine aldehydr and acetone, selection target flow velocity；
Under the conditions of identical sample volume, detector wavelength, flow velocity and proportion of mobile phase, column temperature is adjusted, observes liquid phase color
The methacrylaldehyde of spectrometer output and the chromatography waveform diagram of acetone, according to the appearance time of the chromatography waveform diagram and peak shape and to third
The separating effect of olefine aldehydr and acetone, selection target column temperature；
Under the conditions of identical sample volume, detector wavelength, flow velocity and column temperature, proportion of mobile phase is adjusted, observes liquid phase color
The methacrylaldehyde of spectrometer output and the chromatography waveform diagram of acetone, according to the appearance time of the chromatography waveform diagram and peak shape and to third
The separating effect of olefine aldehydr and acetone, selection target proportion of mobile phase；
According to the target flow rate, target column temperature, target proportion of mobile phase, methacrylaldehyde is separated with acetone.
Further, the aldehyde ketone-DNPH mixing standard liquid includes formaldehyde, acetaldehyde, methacrylaldehyde and acetone.
Further, the appearance time and peak shape according to the chromatography waveform diagram and methacrylaldehyde and acetone are divided
From effect, selection target flow velocity includes:
Meeting within the scope of preset appearance time, and under the conditions of the peak shape of methacrylaldehyde and acetone is independent, selection
Maximum flow rate is as target flow rate.
Further, the appearance time and peak shape according to the chromatography waveform diagram and methacrylaldehyde and acetone are divided
From effect, selection target column temperature includes:
Meeting within the scope of preset appearance time, and under the conditions of the peak shape of methacrylaldehyde and acetone is independent, pre-
If safe temperature range in select maximum value as target column temperature.
Further, the appearance time and peak shape according to the chromatography waveform diagram and methacrylaldehyde and acetone are divided
From effect, selection target proportion of mobile phase includes:
Meeting within the scope of preset appearance time, and under the conditions of the peak shape of methacrylaldehyde and acetone is independent, selection
The maximum target proportion of mobile phase of organic phase accounting is as target proportion of mobile phase.
Optionally, the aldehyde ketone-DNPH mixing standard liquid is that 4 kinds of aldehyde ketone-DNPH mix standard liquid, 7 kinds of aldehyde ketone-DNPH mixing marks
Liquid, 13 kinds of aldehyde ketone-DNPH mixing standard liquids or 16 kinds of aldehyde ketone-DNPH mix standard liquid.
Further, the initial concentration of the aldehyde ketone-DNPH mixing standard liquid is 100mg/L, and the configuration concentration is 1mg/L
Aldehyde ketone-DNPH mixing standard liquid include:
Aldehyde ketone-DNPH mixing the standard liquid for pipetting 500 μ l using the liquid-transfering gun of 1000 μ l is determined into the first volumetric flask with acetonitrile
Hold the aldehyde ketone-DNPH mixing standard liquid that 10mg/L is obtained to 5ml graduation mark；
Standard liquid is mixed using the aldehyde ketone-DNPH that the liquid-transfering gun of 1000 μ l pipettes 500 μ l from first volumetric flask again
Into the second volumetric flask, it is settled to 5ml graduation mark with acetonitrile, obtains the aldehyde ketone-DNPH mixing standard liquid of 1mg/L.
Further, the target proportion of mobile phase includes initial flow matched, intermediate flow matching when final stream
Dynamic matched, the intermediate flow matched in methacrylaldehyde and increase stream relative to initial flow matched in the acetone appearance period
The ratio of organic phase in dynamic phase.
On the other hand, the present invention also provides the measuring method of a kind of automotive upholstery volatile matter methacrylaldehyde and acetone, benefits
Methacrylaldehyde and acetone are separated with separation method as described above, and to after separation methacrylaldehyde and acetone carry out containing measure
It is fixed, obtain respective assay result.
Technical solution bring provided by the invention has the beneficial effect that: using high performance liquid chromatography (HPLC) to propylene
When aldehyde and acetone carry out quantitative analysis, by different in flow rate, different column temperatures, the chromatographies column condition such as different proportion of mobile phase it is excellent
Change, finally determines sample volume: 10 μ l, detector wavelength: 360nm, 35 DEG C of column temperature, flow velocity 1.0ml/min, 60% water 40 of mobile phase
Acetonitrile is in vehicle or automotive upholstery VOC detection, and the quantitative detection condition of formaldehyde, acetaldehyde, methacrylaldehyde, acetone can be to propylene
Aldehyde and acetone efficiently separated, and eliminate superposition of the acetone to methacrylaldehyde in quantitative detection, provide more effective, quasi-
Really, scientific vehicle VOC testing result, provides effective technical support for the improvement of vehicle VOC.
Detailed description of the invention
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing.
Fig. 1 is that the process of the separation method of automotive upholstery volatile matter methacrylaldehyde and acetone provided in an embodiment of the present invention is shown
It is intended to；
Fig. 2 is the methacrylaldehyde and acetone of the liquid chromatograph output under 0.6ml/min flow velocity provided in an embodiment of the present invention
Chromatography waveform diagram；
Fig. 3 is the methacrylaldehyde and acetone of the liquid chromatograph output under 0.8ml/min flow velocity provided in an embodiment of the present invention
Chromatography waveform diagram；
Fig. 4 is the methacrylaldehyde and acetone of the liquid chromatograph output under 1.0ml/min flow velocity provided in an embodiment of the present invention
Chromatography waveform diagram；
Fig. 5 is the methacrylaldehyde and acetone of the liquid chromatograph output under 1.2ml/min flow velocity provided in an embodiment of the present invention
Chromatography waveform diagram；
Fig. 6 is the methacrylaldehyde of the liquid chromatograph output under 25 DEG C of column temperatures provided in an embodiment of the present invention and the chromatography of acetone
Waveform diagram；
Fig. 7 is the methacrylaldehyde of the liquid chromatograph output under 30 DEG C of column temperatures provided in an embodiment of the present invention and the chromatography of acetone
Waveform diagram；
Fig. 8 is the methacrylaldehyde of the liquid chromatograph output under 35 DEG C of column temperatures provided in an embodiment of the present invention and the chromatography of acetone
Waveform diagram；
Fig. 9 is that the liquid chromatograph under 60% acetonitrile provided in an embodiment of the present invention/40% water flowing matched exports
The chromatography waveform diagram of methacrylaldehyde and acetone；
Figure 10 is that the liquid chromatograph under 55% acetonitrile provided in an embodiment of the present invention/35% water flowing matched exports
The chromatography waveform diagram of methacrylaldehyde and acetone.
Specific embodiment
In order to enable those skilled in the art to better understand the solution of the present invention, below in conjunction in the embodiment of the present invention
Attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is only
The embodiment of a part of the invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill people
The model that the present invention protects all should belong in member's every other embodiment obtained without making creative work
It encloses.
It should be noted that description and claims of this specification and term " first " in above-mentioned attached drawing, "
Two " etc. be to be used to distinguish similar objects, without being used to describe a particular order or precedence order.It should be understood that using in this way
Data be interchangeable under appropriate circumstances, so as to the embodiment of the present invention described herein can in addition to illustrating herein or
Sequence other than those of description is implemented.In addition, term " includes " and " having " and their any deformation, it is intended that cover
Covering non-exclusive includes to be not necessarily limited to for example, containing the process, method of a series of steps or units, device, product or equipment
Step or unit those of is clearly listed, but may include be not clearly listed or for these process, methods, product
Or other step or units that equipment is intrinsic.
In one embodiment of the invention, the separation side of a kind of automotive upholstery volatile matter methacrylaldehyde and acetone is provided
Method, referring to Fig. 1, including following below scheme:
S1, using acetonitrile as diluent, configuration concentration be 1mg/L aldehyde ketone-DNPH mix standard liquid.
Specifically, the aldehyde ketone-DNPH mixing standard liquid includes at least formaldehyde, acetaldehyde, methacrylaldehyde and acetone.Optionally, institute
Stating aldehyde ketone-DNPH mixing standard liquid is that 4 kinds of aldehyde ketone-DNPH mix standard liquid, 7 kinds of aldehyde ketone-DNPH mix standard liquid, 13 kinds of aldehyde ketone-DNPH
It mixes standard liquid or 16 kinds of aldehyde ketone-DNPH mixes standard liquid.In embodiments of the present invention, by taking 7 kinds of aldehyde ketone-DNPH mix standard liquid as an example,
Verifying for methacrylaldehyde and acetone HPLC separation condition.Concrete configuration process is as follows:
Aldehyde ketone-DNPH mixing the standard liquid for pipetting 500 μ l using the liquid-transfering gun of 1000 μ l is determined into the first volumetric flask with acetonitrile
Hold the aldehyde ketone-DNPH mixing standard liquid that 10mg/L is obtained to 5ml graduation mark；
Standard liquid is mixed using the aldehyde ketone-DNPH that the liquid-transfering gun of 1000 μ l pipettes 500 μ l from first volumetric flask again
Into the second volumetric flask, it is settled to 5ml graduation mark with acetonitrile, obtains the aldehyde ketone-DNPH mixing standard liquid of 1mg/L.
S2, the chromatographic column that configured aldehyde ketone-DNPH is mixed to standard liquid injection liquid chromatograph.
In a preferred embodiment of the invention, the liquid chromatograph uses high performance liquid chromatograph, such as (Sai Mo
Fly Ultimate3000) Syncronis C18, Dim (mm) 250 × 4.6, Particle Sz (μ) 5.
S3, under the conditions of identical sample volume, detector wavelength, column temperature and proportion of mobile phase, adjust flow velocity, observe liquid phase
The methacrylaldehyde of chromatograph output and the chromatography waveform diagram of acetone, according to the appearance time of the chromatography waveform diagram and peak shape and right
The separating effect of methacrylaldehyde and acetone, selection target flow velocity.
One of an important factor for flow velocity is influence chromatographic isolation, different flow velocitys will affect appearance time.Set sample volume
For 10 μ l, detector wavelength 360nm, mobile phase is 40% water, 60% acetonitrile, and column temperature is 30 DEG C, and (the above primary condition is only to lift
Example, and it is not limited to this).Meeting within the scope of preset appearance time, and the independent item of the peak shape of methacrylaldehyde and acetone
Under part, select maximum flow rate as target flow rate.In the present embodiment, it by taking following four flow velocity as an example, is said in conjunction with spectrogram
It is bright:
Fig. 2 represents flow velocity as 0.6ml/min, and Fig. 3 represents flow velocity as 0.8ml/min, and Fig. 4 represents flow velocity as 1.0ml/min,
Fig. 5 represents flow velocity as 1.2ml/min, in the separating effect of lower verifying methacrylaldehyde and acetone different in flow rate, wherein 1 in spectrogram
Formaldehyde is represented, 2 represent acetaldehyde, and 3 represent methacrylaldehyde, and 4 represent acetone, it is analyzed as follows:
By Fig. 2 to Fig. 5 it is found that sample introduction flow rate set be 0.6ml/min when formaldehyde appearance time at 11 minutes or so, and
The appearance time of methacrylaldehyde acetone is then at 15 minutes or so, with the continuous increase of flow velocity, formaldehyde, and acetaldehyde, methacrylaldehyde, acetone
Appearance time constantly shifts to an earlier date.But flow velocity is unobvious on the influence of the separating effect of methacrylaldehyde and acetone, it is contemplated that when high flow rate
Column pressure is higher, and column pressure maintains the service life that will affect chromatographic column quaternary pump under higher level for a long time, and in view of doing
Sample duration is unsuitable too long.Therefore select flow velocity for 1.0ml/min, and optimize on other factors for influencing separating effect.
That is Fig. 2-4 meets preset appearance time range, and the independent condition of the peak shape of methacrylaldehyde and acetone, but schemes
Shown in 5, the appearance time of formaldehyde is 5.748min, and too short appearance time will affect column effect.Above-mentioned preset appearance time model
It encloses and examines a time range obtained from field compares column effect according to many experiments for vapour.Therefore, it is excluding to be unsatisfactory for condition
Other than 1.2ml/min, select the maximum 1.0ml/min of flow velocity as target flow rate.
It should be noted that not only selecting this four flow velocitys, above four data are only for example in experiment
Bright, (excessively slow flow velocity makes column pressure maintain higher level for a long time to other flow velocitys being actually also tested in safe range
Under will affect the service life of chromatographic column quaternary pump, it is too early that too fast flow velocity will lead to appearance time).
S4, under the conditions of identical sample volume, detector wavelength, flow velocity and proportion of mobile phase, adjust column temperature, observe liquid phase
The methacrylaldehyde of chromatograph output and the chromatography waveform diagram of acetone, according to the appearance time of the chromatography waveform diagram and peak shape and right
The separating effect of methacrylaldehyde and acetone, selection target column temperature.
One of an important factor for column temperature is influence chromatographic isolation, different column temperatures will affect column effect, retention time, separation choosing
Selecting property and peak type.Sample volume is set as 10 μ l, detector wavelength 360nm, mobile phase is 40% water, 60% acetonitrile, and flow velocity is
1.0ml/min (the above primary condition is only for example, and is not limited to this).
Meeting within the scope of preset appearance time, and under the conditions of the peak shape of methacrylaldehyde and acetone is independent, pre-
If safe temperature range in select maximum value as target column temperature.In the present embodiment, by taking following three column temperatures as an example, in conjunction with
Spectrogram is illustrated:
It is 25 DEG C that Fig. 6, which represents column temperature, and it is 30 DEG C that Fig. 7, which represents column temperature, and it is 35 DEG C that Fig. 8, which represents column temperature, is tested under different column temperatures
Demonstrate,prove the separating effect of methacrylaldehyde and acetone, wherein 1 in spectrogram represents formaldehyde, and 2 represent acetaldehyde, and 3 represent methacrylaldehyde, and 4 represent third
Ketone is analyzed as follows:
Column effect is directly proportional to theoretical cam curve N, is inversely proportional with height equivalent to a theoretical plate H.According to formula:AndWherein, N is theoretical cam curve, and L is column length, and H is height equivalent to a theoretical plate, and T is temperature,
A, b, c are constant under certain linear velocity, it is known that, when heating up in a certain range, it can be obtained one of height equivalent to a theoretical plate H most
Small value obtains the minimum value of height equivalent to a theoretical plate and then obtains highest column effect.Heating, needs to consider in described a certain range
It is excessively high to temperature, there is extreme influence to the service life of chromatographic column, so being preset with a safe temperature high temperature limit is 35 DEG C.
When Fig. 6 column temperature is set in 25 DEG C, appearance time the latest, although and methacrylaldehyde and acetone there are two apparent peak,
But the separating effect of methacrylaldehyde and acetone is bad, it can be seen that there is apparent overlapping phenomenon at the peak of methacrylaldehyde and acetone；Fig. 7 institute
30 DEG C of setting compares as the temperature rises with 35 DEG C set by Fig. 3, the appearance time of various substances and retention time time
In advance, but also higher column effect is better for temperature in Fig. 2 and Fig. 3 zone of reasonableness that compares；Therefore selecting column temperature is 35 DEG C, and to flowing
The selection of matched optimizes.
It should be noted that not only selecting these three column temperatures, three above data are only for example in experiment
Other column temperatures bright, be actually also tested in safe range.
S5, under the conditions of identical sample volume, detector wavelength, flow velocity and column temperature, adjust proportion of mobile phase, observe liquid phase
The methacrylaldehyde of chromatograph output and the chromatography waveform diagram of acetone, according to the appearance time of the chromatography waveform diagram and peak shape and right
The separating effect of methacrylaldehyde and acetone, selection target proportion of mobile phase.
One of an important factor for proportion of mobile phase is influence chromatographic isolation, different proportion of mobile phase can shadow separating effect.
Sample volume is set as 10 μ l, detector wavelength 360nm, flow velocity 1.0ml/min, column temperature is 35 DEG C, and (the above primary condition is only
To illustrate, and it is not limited to this).
Meeting within the scope of preset appearance time, and under the conditions of the peak shape of methacrylaldehyde and acetone is independent, selection
The maximum target proportion of mobile phase of organic phase accounting is as target proportion of mobile phase.In the present embodiment, it is flowed with following two
For matched, it is illustrated in conjunction with spectrogram:
Fig. 9 represents proportion as 40% water/60% acetonitrile, and Figure 10 represents proportion 45% water/55% acetonitrile, in different mobile phases
The separating effect of proportion lower verifying methacrylaldehyde and acetone, wherein 1 in spectrogram represents formaldehyde, and 2 represent acetaldehyde, and 3 represent propylene
Aldehyde, 4 represent acetone, are analyzed as follows:
First set 40% water/60% acetonitrile proportion:
As seen from Figure 9, when flowing is matched than for 60% 40% water of acetonitrile, formaldehyde appearance time was on 6.7 minutes left sides
At 10.2 minutes or so, the substance peak of methacrylaldehyde and acetone was essentially totally separated the appearance time of the right side, methacrylaldehyde and acetone, was reached
Separate the effect of optimization.
Secondly 45% water/55% acetonitrile is set:
The appearance of formaldehyde known to Figure 10 at 7.5 minutes or so, the appearance time of methacrylaldehyde and acetone at 11.2 minutes or so,
But there is overlapping at methacrylaldehyde and two peak of acetone substance at the lowest point, acetone generates overlaying influence to the quantitative detection of methacrylaldehyde.When
The appropriate ratio for reducing organic phase in methacrylaldehyde and the mobile phase of acetone appearance period, will cause the substance peak weight of methacrylaldehyde acetone
It is folded, it can not separate.
The appropriate ratio for increasing organic phase in methacrylaldehyde and the mobile phase of acetone appearance period, then increase the elution of mobile phase
Ability makes methacrylaldehyde and acetone reach better separating effect.Therefore finally determine that proportion of mobile phase is 60% acetonitrile, 40% water, and
And in methacrylaldehyde and the ratio appropriate for increasing organic phase in mobile phase in the acetone appearance period, i.e., the described target proportion of mobile phase
Match when final proportion of mobile phase including initial flow matched, intermediate flow, the intermediate flow matched is in methacrylaldehyde
With in the acetone appearance period relative to initial flow matched increase mobile phase in organic phase ratio, such as the present invention implement
In example, it is 70% that when the time is 8min, acetonitrile proportion is increased by 60%, and when the time is 10-14min, acetonitrile proportion, which is increased, is
90%, and final proportion of mobile phase is returned to initial flow matched.It finds during the experiment, if in initial flow matched
Acetonitrile is matched more than 60%, then formaldehyde appearance time exceeds preset appearance time range.
S6, according to the target flow rate, target column temperature, target proportion of mobile phase, methacrylaldehyde is separated with acetone.
In another embodiment of the present invention, the survey of a kind of automotive upholstery volatile matter methacrylaldehyde and acetone is additionally provided
Determine method, methacrylaldehyde and acetone are separated using separation method as described above, and to the methacrylaldehyde and acetone after separation
Carry out assay, obtain respective assay as a result, the content assaying method of the methacrylaldehyde and acetone be the prior art,
Details are not described herein.
The present invention just uses the separating effect of high performance liquid chromatography separation acetone and methacrylaldehyde to test, and passes through not cocurrent flow
Speed, the proportion of different mobile phase gradients, detection of the chromatographies such as the different column temperatures column condition to methacrylaldehyde and acetone separation effect,
According to the factors such as the appearance time of substance, peak shape, resolution under different condition, optimal separation detection condition is determined.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of separation method of automotive upholstery volatile matter methacrylaldehyde and acetone characterized by comprising
Using acetonitrile as diluent, the aldehyde ketone-DNPH that configuration concentration is 1mg/L mixes standard liquid；
Configured aldehyde ketone-DNPH is mixed to the chromatographic column of standard liquid injection liquid chromatograph；
Under the conditions of identical sample volume, detector wavelength, column temperature and proportion of mobile phase, flow velocity is adjusted, observes liquid chromatograph
The methacrylaldehyde of output and the chromatography waveform diagram of acetone, according to the appearance time of the chromatography waveform diagram and peak shape and to methacrylaldehyde
With the separating effect of acetone, selection target flow velocity；
Under the conditions of identical sample volume, detector wavelength, flow velocity and proportion of mobile phase, column temperature is adjusted, observes liquid chromatograph
The methacrylaldehyde of output and the chromatography waveform diagram of acetone, according to the appearance time of the chromatography waveform diagram and peak shape and to methacrylaldehyde
With the separating effect of acetone, selection target column temperature；
Under the conditions of identical sample volume, detector wavelength, flow velocity and column temperature, proportion of mobile phase is adjusted, observes liquid chromatograph
The methacrylaldehyde of output and the chromatography waveform diagram of acetone, according to the appearance time of the chromatography waveform diagram and peak shape and to methacrylaldehyde
With the separating effect of acetone, selection target proportion of mobile phase；
According to the target flow rate, target column temperature, target proportion of mobile phase, methacrylaldehyde is separated with acetone.
2. separation method according to claim 1, which is characterized in that the aldehyde ketone-DNPH mixing standard liquid includes formaldehyde, second
Aldehyde, methacrylaldehyde and acetone.
3. separation method according to claim 1, which is characterized in that the appearance time according to the chromatography waveform diagram
With peak shape and to the separating effect of methacrylaldehyde and acetone, selection target flow velocity includes:
Meeting within the scope of preset appearance time, and under the conditions of the peak shape of methacrylaldehyde and acetone is independent, selection is maximum
Flow velocity is as target flow rate.
4. separation method according to claim 1, which is characterized in that the appearance time according to the chromatography waveform diagram
With peak shape and to the separating effect of methacrylaldehyde and acetone, selection target column temperature includes:
Meeting within the scope of preset appearance time, and under the conditions of the peak shape of methacrylaldehyde and acetone is independent, preset
Select maximum value as target column temperature in safe temperature range.
5. separation method according to claim 1, which is characterized in that the appearance time according to the chromatography waveform diagram
With peak shape and to the separating effect of methacrylaldehyde and acetone, selection target proportion of mobile phase includes:
Meeting within the scope of preset appearance time, and under the conditions of the peak shape of methacrylaldehyde and acetone is independent, is selecting organic
The maximum target proportion of mobile phase of phase accounting is as target proportion of mobile phase.
6. separation method according to claim 2, which is characterized in that the aldehyde ketone-DNPH mixing standard liquid is 4 kinds of aldehyde ketones-
DNPH mixes standard liquid, 7 kinds of aldehyde ketone-DNPH mixing standard liquids, 13 kinds of aldehyde ketone-DNPH mixing standard liquids or 16 kinds of aldehyde ketone-DNPH mixing marks
Liquid.
7. separation method according to claim 1, which is characterized in that the initial concentration of the aldehyde ketone-DNPH mixing standard liquid
For 100mg/L, the aldehyde ketone-DNPH that the configuration concentration is 1mg/L mixes standard liquid and includes:
Aldehyde ketone-DNPH mixing the standard liquid for pipetting 500 μ l using the liquid-transfering gun of 1000 μ l is settled into the first volumetric flask with acetonitrile
5ml graduation mark obtains the aldehyde ketone-DNPH mixing standard liquid of 10mg/L；
Standard liquid is mixed to the using the aldehyde ketone-DNPH that the liquid-transfering gun of 1000 μ l pipettes 500 μ l from first volumetric flask again
In two volumetric flasks, it is settled to 5ml graduation mark with acetonitrile, obtains the aldehyde ketone-DNPH mixing standard liquid of 1mg/L.
8. separation method according to claim 5, which is characterized in that the target proportion of mobile phase includes initial liquid phase
Proportion, intermediate flow match when final proportion of mobile phase, and the intermediate flow matched is in methacrylaldehyde and acetone appearance period
The interior ratio for increasing organic phase in mobile phase relative to initial flow matched.
9. a kind of measuring method of automotive upholstery volatile matter methacrylaldehyde and acetone, which is characterized in that using such as claim 1-8
Any one of described in separation method methacrylaldehyde and acetone are separated, and to after separation methacrylaldehyde and acetone contain
It is fixed to measure, and obtains respective assay result.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810852178.7A CN109142566A (en) | 2018-07-30 | 2018-07-30 | The separation method and measuring method of automotive upholstery volatile matter methacrylaldehyde and acetone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810852178.7A CN109142566A (en) | 2018-07-30 | 2018-07-30 | The separation method and measuring method of automotive upholstery volatile matter methacrylaldehyde and acetone |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109142566A true CN109142566A (en) | 2019-01-04 |
Family
ID=64798352
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810852178.7A Pending CN109142566A (en) | 2018-07-30 | 2018-07-30 | The separation method and measuring method of automotive upholstery volatile matter methacrylaldehyde and acetone |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109142566A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113252817A (en) * | 2021-06-23 | 2021-08-13 | 长春汽车检测中心有限责任公司 | Method for simultaneously detecting acetone and acrolein by adopting liquid chromatography and special mobile phase thereof |
| CN114252533A (en) * | 2021-12-10 | 2022-03-29 | 一汽奔腾轿车有限公司 | Method for detecting aldehyde and ketone substance content in passenger car |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140147926A1 (en) * | 2012-11-23 | 2014-05-29 | Samsung Electro-Mechanics Co., Ltd. | Method of analyzing aldehyde compound in metal plating solution |
| CN106018635A (en) * | 2016-08-12 | 2016-10-12 | 福建中烟工业有限责任公司 | Method for pre-processing tobacco or tobacco product and detection method thereof |
| CN107255688A (en) * | 2017-05-04 | 2017-10-17 | 东华大学 | The detection method of aldoketones organic volatile in a kind of in-car textile |
-
2018
- 2018-07-30 CN CN201810852178.7A patent/CN109142566A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140147926A1 (en) * | 2012-11-23 | 2014-05-29 | Samsung Electro-Mechanics Co., Ltd. | Method of analyzing aldehyde compound in metal plating solution |
| CN106018635A (en) * | 2016-08-12 | 2016-10-12 | 福建中烟工业有限责任公司 | Method for pre-processing tobacco or tobacco product and detection method thereof |
| CN107255688A (en) * | 2017-05-04 | 2017-10-17 | 东华大学 | The detection method of aldoketones organic volatile in a kind of in-car textile |
Non-Patent Citations (2)
| Title |
|---|
| 何海峰等: "整车VOC检测中丙烯醛和丙酮分离条件的优化", 《广东化工》 * |
| 赵永刚等: "2, 4 -二硝基苯肼固相吸附/高效液相色谱法测定车内空气中醛酮类物质", 《环境监测管理与技术》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113252817A (en) * | 2021-06-23 | 2021-08-13 | 长春汽车检测中心有限责任公司 | Method for simultaneously detecting acetone and acrolein by adopting liquid chromatography and special mobile phase thereof |
| CN114252533A (en) * | 2021-12-10 | 2022-03-29 | 一汽奔腾轿车有限公司 | Method for detecting aldehyde and ketone substance content in passenger car |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101858897B (en) | Detection method of phthalate plasticizer | |
| CN106338568B (en) | A kind of method for detecting automobile and automotive trim odoring substance | |
| Faber et al. | Air Pollution in New Vehicles as a Result of VOC Emissions from Interior Materials. | |
| CN109142566A (en) | The separation method and measuring method of automotive upholstery volatile matter methacrylaldehyde and acetone | |
| Huang et al. | Rapid and sensitive detection of trace malachite green and its metabolite in aquatic products using molecularly imprinted polymer-coated wooden-tip electrospray ionization mass spectrometry | |
| EP3137889A1 (en) | Fluidic analysis and separation | |
| CN109459519B (en) | Method for rapidly and simultaneously determining benzene series and aldehyde ketone substances in synthetic material | |
| Miller et al. | Review of analytical measurements facilitated by drop formation technology | |
| CN105486794B (en) | The detection method of prohibitive dye in a kind of ink | |
| CN104359997B (en) | Head space-GC-MS is measured the method for the low boiling halogenated hydrocarbons in solvent-borne type woodwork coating | |
| CN112345682B (en) | Detection method for benzene volatile organic components and application thereof | |
| CN111707770B (en) | Method for measuring isoprene content in butyl rubber liquid by gas chromatography internal standard method | |
| CN107037151B (en) | A kind of measuring method of transfer volume of epoxy chloropropane in food contact material | |
| CN101456866A (en) | Thioester in rhodamine B as well as preparation method and application thereof | |
| CN105823841B (en) | One grow tobacco and tobacco product in a variety of chloroanisoles detection method | |
| Komazaki et al. | The development of an automated continuous measurement system for the monitoring of HCHO and CH3CHO in the atmosphere by using an annular diffusion scrubber coupled to HPLC | |
| CN112748210A (en) | Method for determining aldehyde ketone content in polyether modified organic silicon | |
| CN115792009A (en) | Method for determining aldehyde ketone volatile organic compounds in automotive interior parts | |
| CN106872629B (en) | A kind of method of three nitrogen amidine contents in measurement dairy products | |
| CN111983129B (en) | Method for synchronously analyzing content of acid radical ions in heteropoly acid by ion chromatography | |
| CN114252533A (en) | Method for detecting aldehyde and ketone substance content in passenger car | |
| CN113176363A (en) | Method for measuring total volatile organic compounds in recycled plastics | |
| CN112595800A (en) | Quantitative analysis method for 7-class fine chemicals | |
| CN114062572A (en) | Detection method and application of polyol | |
| CN1538169A (en) | Method of quantitative analysing glutaruldehyde by internal cabel method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190104 |