CN109459519A - The method for quickly measuring benzene homologues and aldehyde ketone substance in synthetic material simultaneously - Google Patents
The method for quickly measuring benzene homologues and aldehyde ketone substance in synthetic material simultaneously Download PDFInfo
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- CN109459519A CN109459519A CN201811649342.0A CN201811649342A CN109459519A CN 109459519 A CN109459519 A CN 109459519A CN 201811649342 A CN201811649342 A CN 201811649342A CN 109459519 A CN109459519 A CN 109459519A
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Abstract
The present invention relates to a kind of methods for quickly measuring benzene homologues and aldehyde ketone substance in synthetic material simultaneously, the parameter of this method set environment test chamber first, then sample is stablized, then gas in environmental test chamber is extracted using constant-temperature constant-current sampler, after gas extraction, sample is parsed and is eluted, is finally measured benzene homologues and aldehyde ketone substance using high performance liquid chromatograph.The problems such as present invention mainly solves that there are sampling steps in existing analytical technology is cumbersome, analysis needs different instruments, with high costs, solvent toxicity is strong；This method can be applied to the measurement of benzene homologues and aldehyde ketone substance in the fields such as artificial synthesized plate, plastic cement race track, automobile interior decoration, furniture.
Description
Technical field
The present invention relates to detection technique fields, in particular to a kind of quickly to measure benzene homologues and aldehyde ketone in synthetic material simultaneously
The method of substance.
Background technique
Synthetic material includes the materials such as synthetic plate, plastic cement race track, automobile interior decoration, furniture, is that people's life and work is necessary
The product of contact.As finishing causes " the malicious runway " of leukaemia, air quality in the vehicle is exceeded and initiation student's discomfort in recent years
Event occurs in succession, and people increasingly pay attention to the product quality of synthetic material.Synthetic material is past in production or process of deployment
Toward addition Macrodilution agent and adhesive, these raw materials can discharge a large amount of benzene homologues and aldehyde ketone substance is detrimental to health.
Currently, the research about benzene homologues and aldoketones substance detecting method reports that is be related to mainly has use both at home and abroad
Different solvents extract synthetic material；Using headspace sampling equipment or solid phase microextraction sampling device in not equality of temperature
It collects and is enriched under degree and time conditions；Using sampler bag or cabin formula method, and respectively select absorption activated carbon adsorption tube and
The method that DNPH adsorption tube is absorbed.The above pre-treating method for collecting benzene homologues and aldehyde ketone, in conjunction with gas chromatograph or
Person's gas chromatography mass spectrometer, high performance liquid chromatograph or efficient liquid phase mass spectrograph are measured.
However these method sampling steps are cumbersome, need successively to acquire benzene homologues and aldehyde ketone substance, the sampling period compared with
It is long；Interference of the free radical of sample generation to analysis is not considered；Without preferably illumination simulation, ventilation, temperature and humidity to examination
The influence of benzene homologues and aldoketones release in sample；Test uses different instrument and equipments, and the measurement of benzene homologues often uses gas phase color
Spectrometer or gas chromatography mass spectrometer, aldoketones detection use high performance liquid chromatograph or efficient liquid phase mass spectrograph, equipment cost
High, process is complicated；The stronger carbon disulfide of toxicity is used to the parsing of benzene homologues, is detrimental to health, it can not quickly, together
When, it is comprehensive analysis synthetic material release harmful substance.Therefore, effective system to benzene homologues in synthetic material and aldehyde ketone
Class content carries out analysis detection, and analysis method and the corresponding standard for establishing quick, sensitive, accurate save the cost are most important.
Summary of the invention
The purpose of the present invention is to provide a kind of sides for quickly measuring benzene homologues and aldehyde ketone substance in synthetic material simultaneously
Method.The present invention develops for the first time while acquiring benzene homologues and aldehyde ketone substance in synthetic material, utilizes liquid chromatogram comprehensive analysis
Method；This method can be applied to artificial synthesized plate, plastic cement race track, automobile interior decoration, furniture etc., and covering surface is wider, application
It is relatively strong；With preferable qualitative, quantitative effect.
In order to achieve the above object, the technical solution adopted by the present invention are as follows:
Quickly measure the method for benzene homologues and aldehyde ketone substance in synthetic material, comprising the following steps:
Step 1: equilibrium temperature, relative humidity, Air-cleaning technique, the intensity of illumination of environmental test chamber are set, by synthetic material
Sample is placed in environmental test chamber and is balanced.
Step 2: sample extracts gas in test chamber after balancing, using the constant-temperature constant-current sampler in comprehensively sampling device
Body passes the gas through comprehensively sampling device.
The comprehensively sampling device includes environmental test chamber, except ozone pillar, DNPH pillar, active carbon pillar and constant temperature
Constant flow sampler, one end JA(junction ambient) test chamber except ozone pillar, the other end by threeway respectively with DNPH pillar and
One end of active carbon pillar connects, and the other end of DNPH pillar and active carbon pillar is connect with constant-temperature constant-current sampler.
DNPH pillar and active carbon pillar after gas extraction should respectively be closed nozzle using seal cap, and 8 hours
The interior processing for carrying out next step.Otherwise, pillar Bao Yan is put into the closed appearance that low temperature (4 DEG C of <) is protected from light with tinfoil or aluminium foil
Device can be reserved for 3 days.
Step 3: after gas extraction, the DNPH pillar in comprehensively sampling device is eluted with leacheate, with parsing lyolysis
The active carbon pillar in comprehensively sampling device is analysed, leacheate and desorbed solution and constant volume are collected by filtration respectively；
Step 4: being measured using high performance liquid chromatograph, standard substance is qualitative, quantified by external standard method.
Further, the equilibrium temperature of environmental test chamber described in step 1 be 23 ± 2 DEG C, relative humidity be 5%~
90%, Air-cleaning technique is 1 ± 0.5 time/h, and intensity of illumination is 500~2000Lux, and the sample stable time is 18h or more.
Further, the flow of constant-temperature constant-current sampler described in step 2 is 0.2~1.0L/min；The extraction of gas
Volume is 1~20L.
Further, elution condition described in step 3 is respectively using acetonitrile normal pressure, reversed elution, and elution number is 3
More than secondary, leacheate after 0.45 μm of organic membrane filter constant volume in 5~10mL brown volumetric flask.
Further, analysis condition described in step 3 is to take out the adsorption stuffing in active carbon pillar, with N, N- bis-
Methylformamide room temperature parse 1~2h, desorbed solution after 0.45 μm of organic membrane filter constant volume in 5~10mL brown volumetric flask.
Further, chromatographic condition benzene homologues being measured using high performance liquid chromatograph in step 4 are as follows: chromatographic column
For C18Column 25cm × 4.6mm, 5 μm, column temperature is 20~35 DEG C, and UV detector wavelength is 260nm, 5~20 μ L of sample volume；Flowing
Phase A is water, and B is acetonitrile, and gradient elution program is 0~15min, 50%A；15~20min, 55%A；20~25min, 50%A；
Flow velocity is 1.0mL/min.The benzene homologues include benzene, toluene, ethylbenzene, paraxylene, ortho-xylene, isopropylbenzene and styrene.
Further, chromatographic condition aldehyde ketone substance being measured using high performance liquid chromatograph in step 4 are as follows: color
Spectrum column is C18Column 25cm × 4.6mm, 5 μm, column temperature is 20~35 DEG C, and UV detector wavelength is 360nm, 5~20 μ L of sample volume；
Mobile phase A is water, and B is acetonitrile, gradient elution program 60%B；Flow velocity is 1.0mL/min.The aldehyde ketone substance includes first
Aldehyde, acetaldehyde, acetone, propionic aldehyde, crotonaldehyde, butanone, n-butanal, methacrolein, benzaldehyde, valeral, o-tolualdehyde, to first
Benzaldehyde, cyclohexanone and hexanal.
The present invention also provides the methods of benzene homologues and aldehyde ketone substance in above-mentioned quick measurement synthetic material artificial
Synthetic plate, plastic cement race track, automobile interior decoration, the application in furniture in benzene homologues and aldoketones substance-measuring.
The beneficial effects of the present invention are:
Sample increases the adjusting of this parameter of intensity of illumination first in environmental test chamber stabilization process in the present invention, and optimizes
The parameters such as Air-cleaning technique, equilibrium temperature and relative humidity, in more real simulation actual environment in synthetic material free radical production
It is raw, and its influence discharged to benzene homologues in synthetic material and aldoketones is eliminated, and do not destroy sample.
Method that is provided by the invention while acquiring benzene homologues and aldehyde ketone substance, air exchange when eliminating sampling respectively
It is influenced caused by benzene homologues and aldehyde ketone constituents, stability is high；The time is saved, step is simple；The connection type of pillar is eliminated
The ozone etc. that free radical generates, strong antijamming capability can be preferably suitable for the synthetic material sample of substrate background complexity
Sampling.
Benzene homologues analytic method provided by the invention replaces two sulphur of severe toxicity using the n,N-Dimethylformamide of hypotoxicity
Change carbon, reduces the harm to personnel health；Method measurement accuracy is high, and method detection is limited to 0.3 × 10-4~1.2 × 10-3mg/m3,
Be below in national standard HJ 584-2010 is 1.5 × 10-3mg/m3Detection limit；Recovery of standard addition be 94.2%~
104.8%.
The method of the present invention eliminates thermal desorption instrument, gas chromatograph or gas chromatography mass spectrometer, has saved equipment cost；
Using the parsing solvent of hypotoxicity, the harm to human health is reduced；Eliminate the exploitation of correlation technique, fast and easy；It is high
Effect liquid phase chromatogram high sensitivity, detection limit are low, and standard substance is qualitative, quantified by external standard method, and method is stablized, and data are reliable；It is suitable for
Benzene homologues and group compounds of aldehydes and ketones in synthetic material are quickly measured simultaneously.
Detailed description of the invention
Fig. 1 is comprehensively sampling apparatus structure schematic diagram.
Fig. 2 is the liquid chromatogram of benzene homologues in the method for the present invention.
Fig. 3 is the liquid chromatogram of aldehyde ketone substance in the method for the present invention.
Influence of Fig. 4 equilibration time to benzene homologues in sample and aldoketones substance release.
Influence of Fig. 5 relative humidity to benzene homologues in sample and aldoketones substance release.
Influence of Fig. 6 intensity of illumination to benzene homologues in sample and aldoketones substance release.
Influence of Fig. 7 temperature to benzene homologues in sample and aldoketones substance release.
Influence of Fig. 8 desorbed solution to benzene homologues extraction efficiency.
Influence of Fig. 9 leacheate to aldoketones extracting substances efficiency.
It is marked in attached drawing, 1 environmental test chamber, 2 is, except ozone pillar, 3 are threeway, and 4 be DNPH pillar, and 5 be active carbon
Pillar, 6 be constant-temperature constant-current sampler.
Specific embodiment
The following examples are intended to illustrate the invention, but is not used to limit the scope of protection of the present invention.Unless otherwise specified, real
Apply the conventional means that technological means used in example is well known to those skilled in the art.
Embodiment 1
One, instrument and reagent
Aldoketones material mixing titer: formaldehyde, acetaldehyde, acetone, propionic aldehyde, crotonaldehyde, butanone, n-butanal, methacrolein, benzene
Formaldehyde, valeral, o-tolualdehyde, p-tolyl aldehyde, cyclohexanone, hexanal, each 100mg/L.
Benzene homologues Standard Stock solutions: weighing styrene 1mg respectively, benzene, toluene, ethylbenzene, paraxylene, ortho-xylene,
Each 10mg of isopropylbenzene, is placed in 100mL volumetric flask, with methanol dilution to scale and mixes.
Aldoketones standard of physical stock solution: taking aldoketones material mixing titer 1.00mL, be placed in 10mL volumetric flask,
With dilution in acetonitrile to scale and mix.
Benzene, toluene, ethylbenzene, paraxylene, ortho-xylene, isopropylbenzene, styrene, methanol, acetonitrile, N, N- dimethyl formyl
Amine is chromatographically pure, and water is tertiary effluent as defined in GB/T 6682.
Environmental test chamber model HJC-1-H type, Shanghai walk green experimental instruments and equipment limited production, and design parameter is shown in Table 1.
High performance liquid chromatograph model e2695 type, water generation Science and Technology Ltd., U.S. production, has UV detector or diode
Array detector.
1 environmental test chamber important technological parameters of table
Two, measuring method
1, environmental test chamber parameter setting: equilibrium temperature is 23 DEG C, relative humidity 45%, and Air-cleaning technique is 1 time/h, illumination
Intensity is 1000Lux；Then the plastic cement race track sample of 30cm × 30cm is intercepted in 1m3Environmental test chamber in be balanced, put down
The weighing apparatus time is 18 hours.
2, sample acquires
Gaseous sample in environmental test chamber is extracted at 25 DEG C using the constant-temperature constant-current sampler in comprehensively sampling device, constant temperature is permanent
Stream sampler flow is 0.5L/min；The extraction volume of gas is 10L.As shown in Figure 1, the comprehensively sampling device includes ring
Border test chamber 1 removes ozone pillar 2, DNPH pillar 4, active carbon pillar 5 and constant-temperature constant-current sampler 6, described to remove ozone pillar 2
One end JA(junction ambient) test chamber 1, the other end connect with one end of DNPH pillar 4 and active carbon pillar 5 respectively by threeway 3,
The other end of DNPH pillar 4 and active carbon pillar 5 is connect with constant-temperature constant-current sampler 6.
3, sample parses
Adsorption stuffing in active carbon pillar is taken out, is put into ground tool plug pipe, it is close that 1mL n,N-Dimethylformamide is added
Close, room temperature parse 1h, desorbed solution after 0.45 μm of organic membrane filter constant volume in 5mL brown volumetric flask.
DNPH pillar is used into 1mL acetonitrile normal pressure, reversed elution 3 times respectively, eluent is received after 0.45 μm of organic membrane filter
It combines in 5mL brown volumetric flask, acetonitrile constant volume is added.
3, high performance liquid chromatograph measures
3.1 chromatographic condition
Benzene homologues liquid phase chromatogram condition: chromatographic column C18Column (25cm × 4.6mm, 5 μm), column temperature are 20~35 DEG C, ultraviolet detection
Device wavelength is 260nm, 5~20 μ L of sample volume.Mobile phase A is water, and B is acetonitrile, and gradient elution program is 0~15min, 50%A；
15~20min, 55%A；20~25min, 50%A；Flow velocity is 1.0mL/min.Wherein 50%A represent 50% mobile phase A and
50% Mobile phase B, 55%A represent 55% mobile phase A and 45% Mobile phase B.
Aldehyde ketone substance liquid phase chromatogram condition: chromatographic column C18Column (25cm × 4.6mm, 5 μm), column temperature are 20~35 DEG C,
UV detector wavelength is 360nm, 5~20 μ L of sample volume.Mobile phase A is water, and B is acetonitrile, gradient elution program 60%B；
Flow velocity is 1.0mL/min.
3.2 the drafting of standard curve
The drafting of benzene homologues standard curve: being diluted benzene homologues Standard Stock solutions with methanol step by step, prepares mass concentration successively
For the hybrid standard working solution of 20,40,60,80,100mg/L.1 μ L of hybrid standard working solution is taken to be injected into active carbon respectively
In pillar, the flow of 100mL/min leads to N2In active carbon pillar 5 solvent is dried up, it is small to obtain standard curve series by 5min
Column.Standard curve series pillar is collected by analysis condition parsing, is measured by chromatographic condition sample introduction, according to each target component quality
Standard curve is drawn with response.Chromatogram is as shown in Figure 2.
The drafting of aldoketones standard of physical curve: being diluted aldoketones Standard Stock solutions with acetonitrile step by step, prepares quality
Concentration is followed successively by the hybrid standard working solution of 2,4,6,8,10mg/L.100 μ L of hybrid standard working solution is taken to be injected into respectively
In DNPH pillar, the flow of 100mL/min leads to N2Solvent in DNPH pillar is dried up, it is small to obtain standard curve series by 5min
Column.Standard curve series pillar is collected by the elution of elution condition, is measured by chromatographic condition sample introduction, according to each target component quality
Standard curve is drawn with response.Chromatogram is as shown in Figure 3.
3.3, it measures
Sample to be tested is measured, if the benzene homologues of detection and the chromatographic peak retention time of aldehyde ketone substance and standard items one
It causes, can tentatively assert that there are benzene homologues and aldehyde ketone substance in sample.Using standard curve quantified by external standard method.Benzene homologues and aldehyde ketone
Class content should be analyzed again within standard curve after should then diluting beyond the range of linearity.
3.4, blank test
In addition to not placing sample, carried out by said determination condition and step.
4, interpretation of result
As a result it calculates according to the following formula, calculated result should deduct blank value:
In formula:
W --- the release content of benzene homologues and aldehyde ketone substance in sample, unit are every cubic metre of milligram (mg/m3)；
M --- the quality of benzene homologues and aldehyde ketone substance from the sample solution found on standard working curve, unit are microgram
(μg)；V --- sampling volume, unit are to rise (L).
The optimization of 2 environmental test chamber operating condition of embodiment
It is analysis object, survey of optimizing the environment with benzene, toluene, styrene, ortho-xylene, isopropylbenzene, formaldehyde, acetaldehyde, acetone, butanone
The operating condition for trying cabin intercepts 30cm × 30cm's referring to standard GB/T/T 14833-2011 " synthetic material runway cover "
Plastic cement race track surface material is in 1m3Environmental test chamber in be balanced, the constant-temperature constant-current sampler of comprehensively sampling device is 25
Gaseous sample in environmental test chamber, flow 0.5L/min, sampling time 20min are extracted under the conditions of DEG C, sampling volume is
10L。
Equilibration time is too short, and the organic compound of material release is not yet uniform in environmental test chamber, benzene homologues and aldehyde ketone
Substance content is unstable；Equilibration time is too long, influences testing efficiency.The present embodiment has primarily looked at equilibration time in sample
The influence of benzene homologues and aldoketones substance release, experiment condition: equilibrium temperature is 23 DEG C, relative humidity 45%, intensity of illumination
For 1000Lux, equilibration time be respectively 2h, 4h, 6h, 8h, 10h, 12h, 14h, 16h, 18h, 20h, for 24 hours, 32h and 48h, as a result
See Fig. 4.As shown in Figure 4: when the time reach 16 it is small when, the release of all kinds of benzene homologues and aldehyde ketone substance starts to tend towards stability.Cause
This, selecting equilibration time of the sample in environmental test chamber is 18 hours.
The present embodiment has then investigated influence of the relative humidity to benzene homologues in sample and aldoketones substance release, tests item
Part: equilibrium temperature is 23 DEG C, intensity of illumination 1000Lux, and stablizing the time is 18h, relative humidity is respectively 10%, 20%,
30%, 40%, 50%, 60%, 70%, 80% and 90%, as a result see Fig. 5.From figure 5 it can be seen that with relative humidity
Increase, the release variation tendency of benzene homologues and aldehyde ketone substance is little in sample.
The present embodiment has also investigated influence of the illumination to benzene homologues in sample and aldoketones substance release.In environmental test chamber
Middle opening LED lamp tube, the illumination for changing material surface at a distance from material surface by change power of lamp tube and adjusting fluorescent tube are strong
Degree, experiment condition: equilibrium temperature be 23 DEG C, relative humidity 45%, stablize the time be 18h, intensity of illumination be respectively 0Lux,
100Lux, 300Lux, 500Lux, 700Lux, 1000Lux, 1300Lux, 1700Lux, 2000Lux, 2500Lux and 3000Lux,
As a result see Fig. 6.It will be appreciated from fig. 6 that the release of benzene homologues and aldehyde ketone substance becomes in growth in sample with the increase of intensity of illumination
Gesture, when intensity of illumination reaches 500Lux, classes of compounds tends towards stability, however when intensity of illumination is greater than 2000Lux, environment
Test chamber is not easy to reach stable, measurement result relative standard deviation >=5%.Therefore, light of the selection sample in environmental test chamber
It is 500~2000Lux according to intensity.
Temperature is to influence the key factor of benzene homologues and aldoketones substance release in sample.Temperature is higher, is more conducive to sample
The release of organic matter in product, but to reach the balance time used longer for environmental test chamber, gets over to the technical requirement of environmental test chamber
Height, the background values in environmental test chamber are also higher.The present embodiment has further investigated temperature to benzene homologues in sample and aldoketones
The influence of substance release, experiment condition: relative humidity 45%, intensity of illumination 1000Lux, stablizing the time is 18h, stablizes temperature
Degree is respectively 23 DEG C, 32 DEG C, 41 DEG C, 50 DEG C and 60 DEG C, as a result sees Fig. 7.As shown in Figure 7: as the temperature rises, benzene in sample
It is that the burst size of object accordingly increases, aldehyde material is increased slightly, and letones variation tendency is little, when temperature is more than 40 DEG C,
Measurement result relative standard deviation >=5% of aldehyde material burst size, when temperature is more than 60 DEG C, environmental test chamber has been difficult
To balance, it is longer that relative humidity reaches the stable time.Therefore, selecting equilibrium temperature of the sample in environmental test chamber is 23 DEG C.
The optimization of the parsing of embodiment 3 and elution condition
Select water, methanol, acetonitrile, acetone, ethyl acetate, n-hexane, hexamethylene, carbon disulfide and N,N-dimethylformamide
(DMF) it is used as desorbed solution, influence of the different solutions to benzene homologues extraction efficiency is investigated, as a result sees Fig. 8, as can be seen from Figure 8,
Carbon disulfide and DMF are greater than other solvents to the eluting power of benzene homologues, consider that the toxicity of DMF is smaller than carbon disulfide, therefore, choosing
The desorbed solution for selecting benzene homologues is DMF.
Select water, methanol, acetonitrile, ethyl acetate, n-hexane, hexamethylene, carbon disulfide and N,N-dimethylformamide
(DMF) it is used as leacheate, influence of the different leacheates to aldoketones extracting substances efficiency is investigated, as a result sees Fig. 9, it can be with from figure
Find out, water, methanol, acetonitrile eluting power be greater than low pole ethyl acetate, n-hexane, hexamethylene, carbon disulfide and DMF,
The extraction efficiency highest of acetonitrile.Therefore, select acetonitrile as the leacheate of aldehyde ketone substance.
Experiment advanced optimizes the volume of desorbed solution, parses volume and the time of time and leacheate, finally determines
Testing conditions are shown in embodiment 1.
The optimization of 4 chromatographic condition of embodiment
Liquid chromatogram detector wavelength, column model, flowing facies type and condition of gradient elution are investigated.It selects respectively
XbridgeC18 (25cm × 4.6mm, 5 μm), Atlantis T3 (25cm × 4.6mm, 5 μm), Xbridge Phenyl (25cm
× 4.6mm, 5 μm) and Waters PAH C18 (25cm × 4.6mm, 5 μm) chromatographic column, mobile phase methanol: water, acetonitrile: water and second
Nitrile: 0.1% formic acid solution；Benzene homologues liquid chromatogram detector 230~290nm of wavelength, aldoketones liquid chromatogram detector wavelength
354~370nm；According to testing result and in conjunction with the comfort level that benzene homologues and aldehyde ketone substance detect, the testing conditions of selection
See embodiment 1.
5 methodological study of embodiment
1, the linear relationship and detection limit of method
Series standard working solution is measured under chromatographic condition, its quality is linearly returned according to the peak area measured
Return, using peak area as Y-axis, maps by X-axis of quality, obtain equation of linear regression.The range of linearity of benzene homologues, linear regression side
Journey, related coefficient, detection limit and quantitative limit are shown in Table 2, the range of linearity of aldehyde ketone substance, equation of linear regression, related coefficient, inspection
Rising limit and quantitative limit are shown in Table 3.
Linear dimensions, detection limit and the quantitative limit of 2 benzene homologues of table
Linear dimensions, detection limit and the quantitative limit of 3 aldehyde ketone substance of table
2, the rate of recovery and precision of method
Methodology test, including rate of recovery examination have been carried out to the method for benzene homologues and aldoketones in measurement synthetic material of the invention
It tests and precision test.Basic, normal, high three additions concentration is set separately, measure the benzene homologues rate of recovery be 94.2%~
104.8%, relative standard deviation is 1.93%~4.84%；The aldoketones rate of recovery is 92.8%~108.0%, and relative standard is inclined
Difference is 1.77%~4.13%.It the results are shown in Table 4~table 5.
The 4 benzene homologues rate of recovery of table and Precision test result
The 5 aldoketones rate of recovery of table and Precision test result
6 sample detection of embodiment
Using the method that the present invention establishes, benzene homologues and aldehyde are carried out to plastic cement race track material, automotive interior part and Furniture panel
The measurement of letones burst size.It the results are shown in Table 6.
The measurement of 6 actual sample burst size of table
Note: "/" is indicated to be lower than quantitative limit, is not detected.
In summary situation, the rate of recovery of this method, all technicals such as detection limit and precision meet the requirements, side
Method is applied to synthetic material sample detection, and reproducibility is good.This method is easy to operate, facilitate stablize, solvent toxicity it is small, detection at
This is low, result is accurate, can be used for the measurement of benzene homologues and aldehyde ketone substance in synthetic material sample.
Finally, it is stated that preferred embodiment above is only used to illustrate the technical scheme of the present invention and not to limit it, although logical
It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (8)
1. quickly measuring the method for benzene homologues and aldehyde ketone substance in synthetic material, which comprises the following steps:
Step 1: equilibrium temperature, relative humidity, Air-cleaning technique, the intensity of illumination of environmental test chamber are set, by synthetic material
Sample is placed in environmental test chamber and is balanced；
Step 2: sample extracts gas in environmental test chamber after balancing, using the constant-temperature constant-current sampler in comprehensively sampling device
Body passes the gas through comprehensively sampling device；
The comprehensively sampling device includes environmental test chamber (1), except ozone pillar (2), DNPH pillar (4), active carbon pillar
(5) and constant-temperature constant-current sampler (6), one end JA(junction ambient) test chamber (1), the other end except ozone pillar (2) pass through three
Logical (3) are connect with one end of DNPH pillar (4) and active carbon pillar (5) respectively, DNPH pillar (4) and active carbon pillar (5)
The other end is connect with constant-temperature constant-current sampler (6)；
Step 3: after gas extraction, with the DNPH pillar (4) in leacheate elution comprehensively sampling device, being parsed with desorbed solution
Leacheate and desorbed solution and constant volume is collected by filtration in active carbon pillar (5) in comprehensively sampling device respectively；
Step 4: being measured using high performance liquid chromatograph, standard substance is qualitative, quantified by external standard method.
2. the method for benzene homologues and aldehyde ketone substance, feature exist in quick measurement synthetic material according to claim 1
In the equilibrium temperature of environmental test chamber 1 described in step 1 is 23 ± 2 DEG C, and relative humidity is 5%~90%, and Air-cleaning technique is
1 ± 0.5 time/h, intensity of illumination is 500~2000 Lux, and the sample stable time is 18h or more.
3. the method for benzene homologues and aldehyde ketone substance, feature exist in quick measurement synthetic material according to claim 1
In the flow of constant-temperature constant-current sampler 6 described in step 2 is 0.2~1.0 L/min；The extraction volume of gas is 1~20L.
4. the method for benzene homologues and aldehyde ketone substance, feature exist in quick measurement synthetic material according to claim 1
In elution condition described in step 3 is respectively using acetonitrile normal pressure, reversed elution, and elution number is 3 times or more, leacheate
Constant volume is in 5~10mL brown volumetric flask after 0.45 μm of organic membrane filter.
5. the method for benzene homologues and aldehyde ketone substance, feature exist in quick measurement synthetic material according to claim 1
In analysis condition described in step 3 is to take out in active carbon pillar 5 adsorption stuffing, normal with n,N-Dimethylformamide
Temperature parsing 1~2h, desorbed solution after 0.45 μm of organic membrane filter constant volume in 5~10mL brown volumetric flask.
6. the method for benzene homologues and aldehyde ketone substance, feature exist in quick measurement synthetic material according to claim 1
In the chromatographic condition being measured using high performance liquid chromatograph to benzene homologues in step 4 are as follows: chromatographic column C1825 cm of column ×
4.6 mm, 5 μm, column temperature is 20~35 DEG C, and UV detector wavelength is 260 nm, 5~20 μ L of sample volume；Mobile phase A is water,
B is acetonitrile, and gradient elution program is 0~15 min, 50%A；15~20 min, 55%A；20~25 min, 50%A；Flow velocity is
1.0 mL/min。
7. the method for benzene homologues and aldehyde ketone substance, feature exist in quick measurement synthetic material according to claim 1
In the chromatographic condition being measured using high performance liquid chromatograph to aldehyde ketone substance in step 4 are as follows: chromatographic column C18Column 25
The mm of cm × 4.6,5 μm, column temperature is 20~35 DEG C, and UV detector wavelength is 360 nm, 5~20 μ L of sample volume；Mobile phase A
For water, B is acetonitrile, gradient elution program 60%B；Flow velocity is 1.0 mL/min.
8. the method for benzene homologues and aldehyde ketone substance is in people in the described in any item quick measurement synthetic materials of claim 1~7
Work synthetic plate, plastic cement race track, automobile interior decoration, the application in furniture in benzene homologues and aldoketones substance-measuring.
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