CN107255688A - The detection method of aldoketones organic volatile in a kind of in-car textile - Google Patents
The detection method of aldoketones organic volatile in a kind of in-car textile Download PDFInfo
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- CN107255688A CN107255688A CN201710309178.8A CN201710309178A CN107255688A CN 107255688 A CN107255688 A CN 107255688A CN 201710309178 A CN201710309178 A CN 201710309178A CN 107255688 A CN107255688 A CN 107255688A
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- aldoketones
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
Abstract
The present invention relates to a kind of detection method of aldoketones organic volatile in in-car textile, including：(1) blank fabric is taken, aldehyde ketone monomer solution is added as needed on, is put into hermetic bag and empties；Nitrogen is subsequently filled, seals to isolate unsteered ambient air；Baking oven heating, a length of 2h ± 5min during heating, to simulate environment inside car are put under the conditions of 65~68 DEG C；(2) with the gas in DNPH sampling pipes absorption hermetic bag, DNPH sampling pipes is eluted using the acetonitrile of addition hydrochloric acid, eluent is obtained, is placed in high performance liquid chromatograph and is detected, obtain the volatile quantity of aldoketones organic volatile.
Description
Technical field
The invention belongs to standardized fiber samples detection field, aldoketones organic volatile in more particularly to a kind of in-car textile
The detection method of thing.
Background technology
Aldoketones organic volatile includes formaldehyde, acetaldehyde, acetone, methacrylaldehyde, propionic aldehyde, crotonaldehyde, butanone, butyraldehyde, methyl
Methacrylaldehyde, benzaldehyde, valeral, tolyl aldehyde, cyclohexanone, hexanal etc..It can be used in the production process of in-car textile a lot
Auxiliary agent, these auxiliary agents usually contain aldehyde material, the persistence to keep stamp and dyeing, obtain wrinkle resistant, shrinkproof and fire-retardant
And other effects；In order to improve the durability of fabric, can be used during textile dyeing and finishing antiaging agent, antistatic additive, waterproofing agent,
Softening agent etc., these auxiliary agents are all much hydro carbons and silicone product.Research shows that aldoketones organic volatile has certain
Toxicity, can be to the infringement of the healthy generation of people seriously.State Environmental Protection Administration once promulgated GB27630-2011 in 2011
《Air Quality Evaluation guide in passenger car》, define the content difference of these three aldoketones materials of formaldehyde, acetaldehyde and methacrylaldehyde
It must not exceed 0.10,0.05 and 0.5mgm-3。
Door and window is closed in vehicle traveling process, and seal is stronger, and pernicious gas is difficult to external diffusion, and pollution level is big.When
Automobile long run is parked in the sun, due to glass door and window in automobile construction the larger area of occupation ratio, vehicle interior temperature
There can be change by a relatively large margin.Under high temperature, harmful substance is more volatile in in-car textile.The aldoketones evaporated is organic
Thing can be raised with the rise of vehicle interior temperature, the parked car especially under burning sun, and its concentration inside can be in the short time drastically
Rise, bigger injury is caused to human body.
The detection method of aldoketones organic volatile includes gas chromatography, high performance liquid chromatography etc..But determine empty
Content is relatively low in gas aldoketones organic volatile needs noiseless and sensitive detection technique, in addition, as formaldehyde and acetone this
Class compound and 2,4 dinitrophenyl hydrazine (under strong acid condition) reacted derivative have higher on high performance liquid chromatography
Sensitivity.U.S. EPA-TO-11《Determination of Formaldehyde in Ambient Air using
Adsorbant Cartridge followed by High Performance Liquid Chromatography(HPLC)》
Middle regulation, for the aldoketones organic volatile in air, is detected using liquid chromatography.The shortcoming of above-mentioned existing method
It is：A kind of method for detecting to aldoketones material is only proposed, is not the detection method specifically designed for in-car textile, to aldehyde
The volatilization condition of ketone organic matter does not simulate in-car actual conditions strictly, while sampling process is more bothered, being unsuitable for industry should
With.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of detection of aldoketones organic volatile in in-car textile
Method, this method is suitable to commercial Application, and sample introduction concentration is high, detection time is few, is conducive to further research；Aldehydes and ketones
Volatilization condition strictly simulate in-car actual conditions, improve the accuracy and practicality of result.
The detection method of aldoketones organic volatile in a kind of in-car textile of the present invention, including：
(1) blank fabric is taken (not consider the aldehyde ketone content of fabric in itself in experiment, the mark of injection is only included as carrier
Sample), aldehyde ketone monomer solution is added as needed on, is put into hermetic bag and empties；Nitrogen is subsequently filled, sealing is not controlled to isolate
Ambient air；Baking oven heating, a length of 2h ± 5min during heating, to simulate environment inside car are put under the conditions of 65~68 DEG C；
(2) with the gas in DNPH sampling pipes absorption hermetic bag, DNPH sampling pipes is eluted using the acetonitrile of addition hydrochloric acid, obtained
To eluent, it is placed in high performance liquid chromatograph and is detected, obtains the volatile quantity of aldoketones organic volatile.
The material of hermetic bag in the step (1) is PVF, is purged in advance using the nitrogen of clean dry.PVF materials are lazy
It is property, airtight and do not adsorb.
The addition of hydrochloric acid in the step (2) is the 0.1~0.2% of acetonitrile volume.
Testing conditions in the step (2) are：The C18 chromatographic columns of 250mm × 4.6mm × 5 μm, the μ L of sample size 25；Stream
Dynamic phase：Water 45%, acetonitrile tetrahydrofuran 55%；Flow velocity：1mL/min, 25 DEG C of column temperature；DAD Detection wavelengths：360nm, spectrum is swept
Retouch 190~400nm of scope.
When being detected in the step (2) with high performance liquid chromatograph, advanced pin standard specimen compares, according to blank car
The ratio calculation rate of recovery of the area at the peak of the area at corresponding peak and standard specimen in the spectrogram of interior textile.
The preparation method of the standard specimen is：0.05g sterlings liquid is taken in 50ml volumetric flasks, acetonitrile is poured into by solution constant volume
To 50ml, the aldehyde ketone solution that concentration is 1000 μ g/ml is obtained；It is diluted again as needed.
Beneficial effect
(1) present invention is suitable to commercial Application, and sample introduction concentration is high, detection time is few, is conducive to further research.
(2) the volatilization condition of aldehydes and ketones of the present invention strictly simulates in-car actual conditions, improves the accurate of result
Property and practicality.(3) in the present invention detection blank fabric while aldoketones organic volatile, also by standard sample efficient
The detected level of aldoketones organic volatile is variable, difference, the temperature/humidity of random device in sample introduction in liquid spectrometer, standard sample
Seasonal variety and change, in blank fabric the detected level of aldehydes and ketones be with standard sample test detected level oppose
Than under same external condition, being carried out on same instrument, it is to avoid because instrument is different, environment temperature/humidity is not on an equal basis to experiment
As a result influence；As long as ensureing testing sample and standard sample under the same period, same external condition, in same efficient liquid
Detected on chromatography, there will be the higher rate of recovery.
(4) work for needing testing crew to do in detection experiment is exactly mainly sample preparation and the elution process of early stage, not
It is related to the numerical examination of detected level, the main part of detection experiment is completed by high performance liquid chromatograph, is reduced experimental error, is contracted
The difference of the small result being likely to result in by different tests personnel, is more suitable for industrial application.
(5) present invention takes the derivative stage in the method that micro hydrochloric acid is added in acetonitrile, optimization pretreatment process, carries
The detected level of high aldoketones organic volatile, strengthens the accuracy of detection.
Brief description of the drawings
Fig. 1 is the standard curve of formaldehyde；
Fig. 2 is the standard curve of hexanal；
Fig. 3 is the standard curve of butanone；
Fig. 4 is the standard curve of cyclohexanone.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
Take the formaldehyde sterling of market sale to prepare required solution, detected, specific detecting step is as follows：
(1) formalin is prepared, its compound method is：0.05g sterlings liquid is taken in 50ml volumetric flasks, pouring into acetonitrile will
Solution is settled to 50ml, and the concentration of gained formaldehyde monomers solution is about 1000 μ g/ml；Under the conditions of optional test, acetonitrile is dilute
Release and 3.75 μ g/mL are made；1.875μg/mL；0.9375μg/mL；0.4688μg/mL；0.2344μg/mL；0.0586μg/mL；
0.0293 μ g/mL standard working solution, obtains Fig. 1 standard curves；10 sample blanks are chosen, addition concentration is C's (mg/kg)
Standard substance is detected, is computed, and the detection limit (LOD) and quantitative limit (LOQ) of formaldehyde are shown in Table 1 in this method；Blank is taken to knit
Thing, size is 10cm × 10cm, thickness no requirement (NR).100 μ l formaldehyde monomers solution are added, it is quickly put into 10L hermetic bags,
And empty hermetic bag.The nitrogen of 5L clean dries is filled afterwards, seals to isolate unsteered ambient air.Under the conditions of 65 DEG C
Baking oven heating is put into, duration 2h ± 5min are heated, to simulate environment inside car.
(2) heating terminates, and the gas in hermetic bag is adsorbed with DNPH sampling pipes after cooling, and adsorption volume is respectively 1L, 2L,
Obtain the formaldehyde of varying level concentration.200 μ l hydrochloric acid elution DNPH sampling pipes are added in 100ml acetonitriles, eluent is obtained, puts
Detected in high performance liquid chromatograph, obtain the volatile quantity of formaldehyde, after detection terminates, 50 μ l are added in blank fabric
Formaldehyde monomers solution, continue above-mentioned steps (to obtain the rate of recovery under varying level concentration).Entered with high performance liquid chromatograph
During row detection, advanced pin standard specimen compares, by the area at the peak of the area at corresponding peak and standard specimen in the spectrogram of blank fabric
Ratio calculate the rate of recovery, obtain table 2.The formalin that the first step is prepared, as standard specimen solution.
Embodiment 2
Take the hexanal sterling of market sale to prepare required solution, detected, specific detecting step is as follows：
(1) hexanal solution is prepared, its compound method is：0.05g sterlings liquid is taken in 50ml volumetric flasks, pouring into acetonitrile will
Solution is settled to 50ml, and the concentration of gained hexanal monomer solution is about 1000 μ g/ml；Under the conditions of optional test, acetonitrile is dilute
Release and 3.75 μ g/mL are made；1.875μg/mL；0.9375μg/mL；0.4688μg/mL；0.2344μg/mL；0.0586μg/mL；
0.0293 μ g/mL standard working solution, obtains Fig. 2 standard curves；10 sample blanks are chosen, addition concentration is C's (mg/kg)
Standard substance is detected, is computed, and the detection limit (LOD) and quantitative limit (LOQ) of hexanal are shown in Table 1 in this method；Blank is taken to knit
Thing, size is 10cm × 10cm, thickness no requirement (NR).100 μ l hexanal monomer solutions are added, it is quickly put into 10L hermetic bags,
And empty hermetic bag.The nitrogen of 5L clean dries is filled afterwards, seals to isolate unsteered ambient air.Under the conditions of 65 DEG C
Baking oven heating is put into, duration 2h ± 5min are heated, to simulate environment inside car.
(2) heating terminates, and the gas in hermetic bag, adsorption volume difference are adsorbed with DNPH sampling pipes after cooling a period of time
For 1L, 2L, the hexanal of varying level concentration is obtained.200 μ l hydrochloric acid elution DNPH sampling pipes are added in 100ml acetonitriles, are obtained
Eluent, is placed in high performance liquid chromatograph and is detected, the volatile quantity of hexanal is obtained, after detection terminates, then at blank fabric
50 μ l of middle addition hexanal monomer solution, continues above-mentioned steps.When being detected with high performance liquid chromatograph, advanced pin standard specimen
Compare, the ratio of the area at the peak of the area at corresponding peak and standard specimen in the spectrogram of blank fabric is calculated into the rate of recovery, obtained
To table 3.The hexanal solution that the first step is prepared, as standard specimen solution.
Embodiment 3
Take the butanone sterling of market sale to prepare required solution, detected, specific detecting step is as follows：
(1) butanone solution is prepared, its compound method is：0.05g sterlings liquid is taken in 50ml volumetric flasks, pouring into acetonitrile will
Solution is settled to 50ml, and the concentration of gained butanone monomer solution is about 1000 μ g/ml；
Under the conditions of optional test, 3.75 μ g/mL are made in dilution in acetonitrile；1.875μg/mL；0.9375μg/mL；
0.4688μg/mL；0.2344μg/mL；0.0586μg/mL；0.0293 μ g/mL standard working solution, obtains Fig. 3 standard curves；
10 sample blanks are chosen, addition concentration is detected for C (mg/kg) standard substance, is computed, the inspection of butanone in this method
Rising limit (LOD) and quantitative limit (LOQ) are shown in Table 1；Blank fabric is taken, size is 10cm × 10cm, thickness no requirement (NR).Add 100 μ l
Butanone monomer solution, it is quickly put into 10L hermetic bags, and empty hermetic bag.The nitrogen of 5L clean dries is filled afterwards, it is close
Seal to isolate unsteered ambient air.Baking oven heating is put under the conditions of 65 DEG C, duration 2h ± 5min are heated, to simulate in-car
Environment.
(2) heating terminates, and the gas in hermetic bag, adsorption volume difference are adsorbed with DNPH sampling pipes after cooling a period of time
For 1L, 2L, the butanone of varying level concentration is obtained.200 μ l hydrochloric acid elution DNPH sampling pipes are added in 100ml acetonitriles, are obtained
Eluent, is placed in high performance liquid chromatograph and is detected, the volatile quantity of butanone is obtained, after detection terminates, then at blank fabric
50 μ l of middle addition butanone monomer solution, continues above-mentioned steps.When being detected with high performance liquid chromatograph, advanced pin standard specimen
Compare, the ratio of the area at the peak of the area at corresponding peak and standard specimen in the spectrogram of blank fabric is calculated into the rate of recovery, obtained
To table 4.The butanone solution that the first step is prepared, as standard specimen solution.
Embodiment 4
Take the cyclohexanone sterling of market sale to prepare required solution, detected, specific detecting step is as follows：
(1) cyclohexanone solution is prepared, its compound method is：Take 0.05g sterlings liquid in 50ml volumetric flasks, pour into acetonitrile
Solution is settled to 50ml, the concentration of gained cyclohexanone monomer solution is about 1000 μ g/ml；Under the conditions of optional test, second
3.75 μ g/mL are made in nitrile dilution；1.875μg/mL；0.9375μg/mL；0.4688μg/mL；0.2344μg/mL；0.0586μg/
mL；0.0293 μ g/mL standard working solution, obtains Fig. 4 standard curves；10 sample blanks are chosen, addition concentration is C (mg/
Kg standard substance) is detected, is computed, and the detection limit (LOD) and quantitative limit (LOQ) of cyclohexanone are shown in Table 1 in this method；Take
Blank fabric, size is 10cm × 10cm, thickness no requirement (NR).100 μ l cyclohexanone monomer solutions are added, it is quickly put into 10L
In hermetic bag, and empty hermetic bag.The nitrogen of 5L clean dries is filled afterwards, seals to isolate unsteered ambient air.
Baking oven heating is put under the conditions of 65 DEG C, duration 2h ± 5min are heated, to simulate environment inside car.
(2) heating terminates, and the gas in hermetic bag, adsorption volume difference are adsorbed with DNPH sampling pipes after cooling a period of time
For 1L, 2L, the cyclohexanone of varying level concentration is obtained.200 μ l hydrochloric acid elution DNPH sampling pipes are added in 100ml acetonitriles, are obtained
To eluent, it is placed in high performance liquid chromatograph and is detected, the volatile quantity of cyclohexanone is obtained, after detection terminates, then at blank
50 μ l cyclohexanone monomer solution is added in fabric, continues above-mentioned steps.When being detected with high performance liquid chromatograph, advanced one
Pin standard specimen is compared, and the ratio of the area at the peak of the area at corresponding peak and standard specimen in the spectrogram of blank fabric is calculated to recovery
Rate, obtains table 5.The cyclohexanone solution that the first step is prepared, as standard specimen solution.
The detection limit of the in-car textile aldoketones organic volatile of table 1
The recovery of standard addition and precision (n=6) of the formaldehyde of table 2
The recovery of standard addition and precision (n=6) of the hexanal of table 3
The recovery of standard addition and precision (n=6) of the butanone of table 4
The recovery of standard addition and precision (n=6) of the cyclohexanone of table 5
Claims (6)
1. the detection method of aldoketones organic volatile in a kind of in-car textile, including：
(1) blank fabric is taken, aldehyde ketone monomer solution is added as needed on, is put into hermetic bag and empties；Nitrogen is subsequently filled, it is close
Seal to isolate unsteered ambient air；Baking oven heating, a length of 2h ± 5min during heating, with mould are put under the conditions of 65~68 DEG C
Intend environment inside car；
(2) with the gas in DNPH sampling pipes absorption hermetic bag, DNPH sampling pipes is eluted using the acetonitrile of addition hydrochloric acid, washed
De- liquid, is placed in high performance liquid chromatograph and is detected, obtain the volatile quantity of aldoketones organic volatile.
2. the detection method of aldoketones organic volatile in a kind of in-car textile according to claim 1, its feature exists
In：The material of hermetic bag in the step (1) is PVF, is purged in advance using the nitrogen of clean dry.
3. the detection method of aldoketones organic volatile in a kind of in-car textile according to claim 1, its feature exists
The addition of hydrochloric acid in the step (2) is the 0.1~0.2% of acetonitrile volume.
4. the detection method of aldoketones organic volatile in a kind of in-car textile according to claim 1, its feature exists
In：Testing conditions in the step (2) are：The C18 chromatographic columns of 250mm × 4.6mm × 5 μm, the μ L of sample size 25；Mobile phase：
Water 45%, acetonitrile tetrahydrofuran 55%；Flow velocity：1mL/min, 25 DEG C of column temperature；DAD Detection wavelengths：360nm, spectral scan model
Enclose 190~400nm.
5. the detection method of aldoketones organic volatile in a kind of in-car textile according to claim 1, its feature exists
In：When being detected in the step (2) with high performance liquid chromatograph, advanced pin standard specimen compares, and is spun according to blank in-car
The ratio calculation rate of recovery of the area at the peak of the area at corresponding peak and standard specimen in the spectrogram of fabric.
6. the detection method of aldoketones organic volatile in a kind of in-car textile according to claim 1, its feature exists
In：The preparation method of the standard specimen is：Take 0.05g sterlings liquid in 50ml volumetric flasks, pour into acetonitrile and be settled to solution
50ml, obtains the aldehyde ketone solution that concentration is 1000 μ g/ml；It is diluted again as needed.
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| CN108344820A (en) * | 2018-03-07 | 2018-07-31 | 苏州艾驰博特检测科技有限公司 | A kind of detection method of down toy organic volatile |
| CN108508127A (en) * | 2018-02-02 | 2018-09-07 | 厦门鉴科检测技术有限公司 | The high performance liquid chromatography of Carbonyl compounds in a kind of measurement air |
| CN109142566A (en) * | 2018-07-30 | 2019-01-04 | 苏州中汽检测技术服务有限公司 | The separation method and measuring method of automotive upholstery volatile matter methacrylaldehyde and acetone |
| CN109342601A (en) * | 2018-11-14 | 2019-02-15 | 上海帕卡兴产化工有限公司 | A kind of test method of rust-proofing wax VOC content |
| CN109596758A (en) * | 2018-11-24 | 2019-04-09 | 合肥谱尼测试科技有限公司 | Separate the liquid chromatogram mobile phase system of ten kinds of group compounds of aldehydes and ketones in plastic cement race track |
| CN110261516A (en) * | 2019-07-30 | 2019-09-20 | 安徽江淮汽车集团股份有限公司 | A kind of vehicle glass sealant volatile organic matter sample preparation device and detection method |
| CN114894933A (en) * | 2022-05-09 | 2022-08-12 | 台州市产品质量安全检测研究院 | Method for measuring volatile aldehyde ketone substances of automotive interior parts by environment test cabin method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108508127A (en) * | 2018-02-02 | 2018-09-07 | 厦门鉴科检测技术有限公司 | The high performance liquid chromatography of Carbonyl compounds in a kind of measurement air |
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| CN109142566A (en) * | 2018-07-30 | 2019-01-04 | 苏州中汽检测技术服务有限公司 | The separation method and measuring method of automotive upholstery volatile matter methacrylaldehyde and acetone |
| CN109342601A (en) * | 2018-11-14 | 2019-02-15 | 上海帕卡兴产化工有限公司 | A kind of test method of rust-proofing wax VOC content |
| CN109596758A (en) * | 2018-11-24 | 2019-04-09 | 合肥谱尼测试科技有限公司 | Separate the liquid chromatogram mobile phase system of ten kinds of group compounds of aldehydes and ketones in plastic cement race track |
| CN110261516A (en) * | 2019-07-30 | 2019-09-20 | 安徽江淮汽车集团股份有限公司 | A kind of vehicle glass sealant volatile organic matter sample preparation device and detection method |
| CN114894933A (en) * | 2022-05-09 | 2022-08-12 | 台州市产品质量安全检测研究院 | Method for measuring volatile aldehyde ketone substances of automotive interior parts by environment test cabin method |
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Application publication date: 20171017 |