CN114252533A - Method for detecting aldehyde and ketone substance content in passenger car - Google Patents
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- 239000000126 substance Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 28
- 150000001299 aldehydes Chemical class 0.000 title claims abstract description 24
- 150000002576 ketones Chemical class 0.000 title claims abstract description 18
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 66
- -1 aldehyde ketone Chemical class 0.000 claims abstract description 33
- 238000000926 separation method Methods 0.000 claims abstract description 29
- 238000010828 elution Methods 0.000 claims abstract description 22
- 238000012360 testing method Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
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- 239000002904 solvent Substances 0.000 claims abstract description 4
- 238000004458 analytical method Methods 0.000 claims description 6
- HORQAOAYAYGIBM-UHFFFAOYSA-N 2,4-dinitrophenylhydrazine Chemical compound NNC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O HORQAOAYAYGIBM-UHFFFAOYSA-N 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 3
- 230000000536 complexating effect Effects 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 9
- 238000010812 external standard method Methods 0.000 abstract description 3
- 238000010790 dilution Methods 0.000 abstract 1
- 239000012895 dilution Substances 0.000 abstract 1
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- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 description 22
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 16
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- 239000012855 volatile organic compound Substances 0.000 description 8
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- 238000002474 experimental method Methods 0.000 description 6
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- 238000011002 quantification Methods 0.000 description 3
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
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- 238000013441 quality evaluation Methods 0.000 description 2
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- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
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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
-
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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Abstract
The invention relates to a method for detecting the content of aldehyde ketone substances in a passenger vehicle, which comprises the steps of taking acetonitrile as a solvent, carrying out gradient dilution on 14 aldehyde ketone mixed standard solutions, and selecting 0.5 mu g/mL aldehyde ketone-DNPH mixed standard solution as a test sample to be detected; analyzing a sample to be detected by using a liquid chromatograph, selecting 4 factors of mobile phase proportion, flow rate, sample injection amount and column temperature as variables, setting a contrast test, obtaining a rule according to chromatogram peak separation conditions and determining optimal conditions of homogeneous elution; and carrying out gradient elution on the basis of the conclusion of the homogeneous elution experimental conditions to obtain the experimental conditions meeting the preset requirements. The method can realize the separation of 14 common and commercially available aldehyde ketone standard substances, and meets the quantitative requirement by using an external standard method; the common 14 types of aldehyde and ketone standard substances sold in the market can be resolved within 25 minutes, and the detection efficiency is higher compared with the prior art; the mobile phase only contains acetonitrile and water, and other mobile phases are not introduced, so that the method is relatively environment-friendly and healthy.
Description
Technical Field
The invention belongs to the technical field of automobile interior decoration detection, and particularly relates to a method for detecting the content of aldehydes and ketones in a passenger car.
Background
With the rapid development of the automobile manufacturing industry, the non-metallic materials of the automobile interior are also greatly changed. The release of harmful substances contained in the interior materials of the passenger cars comprises volatile components such as organic solvents, auxiliary agents, additives and the like contained in materials such as plastic and rubber parts, fabrics, paint coatings, heat insulation materials, adhesives and the like used by the cars, and the harmful substances are released to the environment in the cars in the using process of the cars to cause air pollution in the cars. The formaldehyde, acetaldehyde, acrolein and other aldehydes and ketones contained in Volatile Organic Compounds (VOC) in the automobile can cause physiological discomfort of passengers, and even cause carcinogenic risks when the automobile is in an environment with high concentration of the substances for a long time.
For the problem, a recommended standard GB/T27630 plus 2011 passenger vehicle interior air quality evaluation guideline and a national mandatory standard GB 18352.6-2016 light vehicle pollutant emission limit and measurement method (the sixth stage of China) are set by the country, and an industry standard HJ/T400 plus 2007 sampling and measurement method for volatile organic compounds and aldehyde ketone substances in a vehicle interior and a certification and approval industry standard dynamic sampling and measurement method for volatile organic compounds and aldehyde ketone substances in a vehicle passenger compartment (a levee suggestion). Meanwhile, each automobile host factory also sets enterprise standards to manage the air quality in the automobile. In the industry standard HJ/T400-2007 method for sampling and measuring volatile organic compounds and aldehyde ketone substances in vehicles, different aldehyde ketone substances are measured by using a standard specific liquid chromatography analysis method, and the problems that the peaks are overlapped so that quantification cannot be performed and the experimental period is long exist are shown in FIG. 1.
The prior art discloses a method for detecting the content of aldehyde ketone compounds in materials in an automobile cabin, which comprises the steps of pretreatment of substances to be detected, derivatization reaction and quantitative analysis by a high performance liquid chromatograph, wherein the specific parameters are as follows: the temperature of the column incubator is 30-50 ℃; the elution mode is gradient elution, and the elution conditions are as follows: 0-10min of mobile phase-water A is 30-60%, mobile phase-acetonitrile B is 20-40%, mobile phase-tetrahydrofuran C is 10-30%, and the flow rate is 1.0-1.5 mL/min; the gradient of the mobile phase-water A is reduced to 20-40% in a gradient of 30-60% in 5-30 min, the gradient of the mobile phase-acetonitrile B is increased to 60-80% in a gradient of 20-40%, the gradient of the mobile phase-tetrahydrofuran C is reduced to 0% in a gradient of 20%, and the flow rate is reduced to 0.5-0.8mL/min in a gradient of 1.0 mL/min; the mobile phase-water A is decreased to 0-10% in 10-30% in 15-40min, the mobile phase-acetonitrile B is increased to 90-100% in gradient in 60-80%, the mobile phase-tetrahydrofuran C is increased to 0-10% in gradient in 0.5-0.8mL/min to 1.0-1.5 mL/min; the sample injection volume is 10-30 mu L, the detection wavelength is 350-380nm, and the operation time is 5-10min later; and quantifying by adopting an external standard method, and determining standard curves of 13 aldehyde ketone standard substances. However, the above method has the following disadvantages: 1. 3 mobile phases are used, namely water, acetonitrile and tetrahydrofuran, and the long-term contact of tetrahydrofuran can harm the physical health of experimenters, especially has great harm to reproductive health; 2. the time of 30 minutes is required for completely resolving 13 aldehyde ketone substances, and the experimental period is long.
The prior art also discloses a separation method and a determination method of volatile acrolein and acetone of automotive upholstery, which are characterized in that aldehyde ketone-DNPH mixed standard solution with the concentration of 1mg/L is prepared and injected into a chromatographic column of a liquid chromatograph; selecting a target flow rate under the conditions of the same sample introduction amount, detector wavelength, column temperature and flow matching ratio according to the peak time and peak shape of a chromatographic waveform diagram and the acrolein-acetone separation effect; selecting a target column temperature under the conditions of the same sample introduction amount, the same detector wavelength, the same flow velocity and the same flow matching ratio; selecting a target mobile phase ratio under the conditions of the same sample introduction amount, the same detector wavelength, the same detector flow rate and the same column temperature; and (3) separating the acrolein from the acetone according to the target flow rate, the target column temperature and the target mobile phase ratio. The invention tests the separation effect of separating acetone and acrolein by adopting liquid chromatography, determines the optimal separation detection condition according to factors such as the peak emergence time, the peak shape, the separation degree and the like of substances under different conditions, enables the acrolein-acetone peak to be separated within the range of the specific detection condition, and has the advantages that the 3 rd peak and the 4 th peak from left to right in figure 2 are acrolein-acetone two substances respectively, the peak emergence time is 10-10.5min, and the separation degree is better. However, the above method has the following disadvantages: 1. the peak separation method is developed only aiming at two substances of acrolein and acetone, and the peak separation of each substance in 14 common commercial aldehyde ketone standard substances is not expanded, because the volatile aldehyde ketone substances of the interior materials of the passenger car are many, although the national standard only requires the limit values of three substances of formaldehyde, acetaldehyde and acrolein, some automobile detection mechanisms have the requirement for quantification of other aldehyde ketone substances, and therefore the peak separation method is developed to take more aldehyde ketone substances into account; 2. the detection period is long, the cost of the experiment time is high, and the consumption of the flow cancellation is large.
Disclosure of Invention
The invention aims to provide a method for detecting the content of aldehyde and ketone substances in a passenger car, and aims to solve the problems that in an industry standard HJ/T400-2007 method for sampling and determining volatile organic compounds and aldehyde and ketone substances in the car, different aldehyde and ketone substances are determined by using a standard specific liquid chromatography analysis method, peaks are overlapped so that quantification cannot be performed, and the experiment period is long.
The purpose of the invention is realized by the following technical scheme:
a method for detecting the content of aldehydes and ketones in a passenger car comprises the following steps:
A. taking acetonitrile as a solvent, diluting 14 aldehyde ketone mixed standard solutions to 1 mu g/mL, 0.5 mu g/mL, 0.1 mu g/mL, 0.05 mu g/mL and 0.01 mu g/mL in a gradient manner, and selecting 0.5 mu g/mL aldehyde ketone-DNPH mixed standard solution as a test sample to be tested;
B. analyzing a sample to be detected by using a liquid chromatograph, selecting 4 factors of mobile phase proportion, flow rate, sample injection amount and column temperature as variables, setting a contrast test, obtaining a rule according to chromatogram peak separation conditions and determining optimal conditions of homogeneous elution;
C. and carrying out gradient elution on the basis of the conclusion of the homogeneous elution experimental conditions to obtain the experimental conditions meeting the preset requirements.
Further, in step A, the aldehyde ketone mixed standard solution is complexed with DNPH, and the concentration is 2 mu g/mL.
Further, the step B specifically includes the following steps: on the basis that a mobile phase is acetonitrile/water, elution is equal gradient, 60% of acetonitrile/40% of water, the flow rate is 1mL/min, the sample injection amount is 25 mu L, 4 factors of the proportion of the mobile phase, the flow rate, the sample injection amount and the column temperature are selected as variables, a contrast test is set, 3 factors are respectively fixed and unchanged, the 4 th factor is changed as a test condition, a liquid chromatogram of a sample to be tested is obtained through analysis, and the test condition is set through observing the separation condition of peaks of 14 aldehyde ketone standard substances.
Further, the separation condition includes a peak time, a peak shape, and a separation degree.
Further, the experimental conditions are: the proportion of the mobile phase is 55 percent of acetonitrile/45 percent of water-80 percent of acetonitrile/20 percent of water; the flow rate is 0.6mL/min-1.2 mL/min; the sample amount is 10-25 μ L; the column temperature is 25-35 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the method for detecting the content of the aldehyde ketone substances in the passenger car can provide specific liquid chromatography detection conditions, realize the liquid phase peak separation of 14 commercially common aldehyde ketone standard substances, meet the quantitative requirement by utilizing an external standard method, ensure that the separation degree reaches more than 1.5, ensure that the total peak time is within 25min, ensure that the linear coefficients of standard curves of 6 different concentration points in the concentration range of 0.01-2 mu g/mL of the 14 aldehyde ketone substances are all more than 0.999 and the relative standard deviation of a quality control sample is less than 1 percent, and meet the quantitative determination requirement of 3 aldehyde ketone substances in the field of cars based on the national standard GB/T27630 plus 2011 'passenger car interior air quality evaluation guideline' and the extension requirement of quantitative determination of other aldehyde ketone substances; the common 14 types of aldehyde and ketone standard substances sold in the market can be resolved within 25 minutes, and the detection efficiency is higher compared with the prior art; the mobile phase only contains acetonitrile and water, and other mobile phases are not introduced, so that the method is relatively environment-friendly and healthy.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1A typical chromatogram for analysis of an aldehyde ketone component by a DNPH tube;
FIG. 2 is a chromatogram of a DNPH tube analysis of the aldehyde ketone component under specific conditions;
FIG. 3 is a flow chart illustrating the steps of the method for detecting the content of aldehydes and ketones in a passenger car according to the present invention;
FIG. 4 is a liquid chromatogram of the sample to be detected;
FIG. 5 is a liquid chromatogram of a control experiment;
FIG. 6 liquid chromatogram of standard solution after gradient elution;
FIG. 7-FIG. 86 are standard curves of 14 aldone-DNPH mixtures of different concentrations.
Detailed Description
The invention is further illustrated by the following examples:
the present invention will be described in further detail with reference to the accompanying drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting of the invention. It should be noted that, for convenience of description, only a part of the structures related to the technical solution of the present invention, not all of the structures, are shown in the drawings.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures. Meanwhile, in the description of the present invention, the terms "first", "second", and the like are used only for distinguishing the description, and are not to be construed as indicating or implying relative importance.
As shown in FIG. 1, the method for detecting the content of aldehydes and ketones in a passenger car comprises the following steps:
s1: using acetonitrile as a solvent, diluting 14 commercially available aldehyde-ketone mixed standard solutions (which are complexed with DNPH and have the concentration of 2 mu g/mL) in a gradient manner to 1 mu g/mL, 0.5 mu g/mL, 0.1 mu g/mL, 0.05 mu g/mL and 0.01 mu g/mL, and selecting 0.5 mu g/mL aldehyde-ketone-DNPH mixed standard solution as a test sample to be tested;
s2: using a liquid chromatograph (Agilent 1260, column type)
C18-5 μm-4.6 × 250mm, deuterium lamp light source) to analyze the sample to be tested.
On the basis of a liquid chromatography detection method (mobile phase: acetonitrile/water; elution: an equal gradient, 60% acetonitrile/40% water; a flow rate: 1 mL/min; a sample introduction amount: 25 muL) specified in an industrial standard HJ/T400-2007 sampling and measuring method for volatile organic compounds and aldehyde ketone substances in vehicles, 4 factors of the proportion of the mobile phase, the flow rate, the sample introduction amount and the column temperature are selected as variables, and a comparison test is set: and respectively fixing 3 factors unchanged, changing the 4 th factor as a test condition, and analyzing to obtain the liquid chromatogram of the sample to be tested. By observing the separation condition (factors such as peak time, peak shape and separation degree) of 14 kinds of aldehyde ketone standard substance peaks, the experimental conditions are set as the mobile phase proportion: 55% acetonitrile/45% water-80% acetonitrile/20% water; flow rate: 0.6mL/min-1.2 mL/min; sample introduction amount: 10-25 μ L; column temperature: 25-35 ℃.
Examples are: in the above experimental condition range, a liquid chromatogram shown in fig. 4 is obtained, which is different from a standard liquid chromatogram (fig. 1) in the "in-vehicle volatile organic compound and aldehyde ketone substance sampling and measuring method" of the industry standard HJ/T400-2007, in that an acrolein peak and an acetone peak can be separated, which correspond to the 3 rd peak and the 4 th peak in fig. 4, respectively, the separation degree reaches 1.2, and the total peak output time can be reduced to be within 25 min. This example is only one of many control experiments and does not represent optimal experimental conditions. The following conclusions were obtained during the control experiment: firstly, with the increase of the acetonitrile ratio, the retention time of each aldehyde ketone is reduced, the peak height/peak width is increased, but the peak height/peak width is not too large, so that adjacent peaks are overlapped, and as shown in figure 5, the 8 th peak and the 9 th peak are overlapped; secondly, along with the increase of the flow velocity of the mobile phase, the retention time of each aldehyde ketone is reduced, but the retention time is not too long, so that the service lives of a pump and a chromatographic column are shortened; with the increase of the sample injection amount, the peak area can be increased, and the separation degree can be reduced; fourthly, with the rising of the column temperature, the total peak output time is reduced, but the service life of the chromatographic column is influenced by overhigh temperature; the amount of sample injection has little influence on the retention time but influences the degree of separation of adjacent peaks, and the smaller the amount of sample injection, the greater the degree of separation, but the smaller the amount of sample injection, the larger the error.
S3: gradient elution is carried out on the basis of the conclusion of the conditions of the homogeneous elution experiment.
Examples are: as shown in fig. 5, acrolein (peak 3) and acetone (peak 4) are relatively well separated, but two standard substance peaks are contained in the retention time of 9.105min, so that the 2 peaks are separated by gradient elution, and the experimental conditions of the gradient elution are shown in table 1:
TABLE 1
The liquid chromatogram of the standard solution after gradient elution can separate 2 peaks of acrolein and acetone (the separation degree reaches more than 1.5), meet the quantitative requirement of the acrolein in GB/T27630-2011, simultaneously can relatively separate other aldehyde and ketone substances, and can control the total peak output time within 25min, taking the example shown in FIG. 6, and taking the 6 mixed standard solutions of 14 aldehyde ketone-DNPH with different concentrations configured in the step 1 as the standard curve, as shown in FIGS. 7 and 8, the linear coefficients of the acrolein and the acetone can reach more than 0.999, and the quality control relative deviation of the 14 mixed standard solutions of aldehyde ketone-DNPH is within 1%.
The mobile phase only contains water and acetonitrile, and other organic solvents are not introduced; the method realizes the liquid phase peak separation of 14 commercially common aldone standard substances by adjusting 4 variables of mobile phase proportion, mobile phase flow rate, sample introduction amount and column temperature and adopting a gradient elution mode; the total peak time of the 14 aldehyde ketone standard substances is within 25 min.
It is to be noted that the foregoing is only illustrative of the preferred embodiments of the present invention and the technical principles employed. It will be understood by those skilled in the art that the present invention is not limited to the particular embodiments described herein, but is capable of various obvious changes, rearrangements and substitutions as will now become apparent to those skilled in the art without departing from the scope of the invention. Therefore, although the present invention has been described in greater detail by the above embodiments, the present invention is not limited to the above embodiments, and may include other equivalent embodiments without departing from the spirit of the present invention, and the scope of the present invention is determined by the scope of the appended claims.
Claims (5)
1. A method for detecting the content of aldehydes and ketones in a passenger car is characterized by comprising the following steps: the method comprises the following steps:
A. taking acetonitrile as a solvent, diluting 14 aldehyde ketone mixed standard solutions to 1 mu g/mL, 0.5 mu g/mL, 0.1 mu g/mL, 0.05 mu g/mL and 0.01 mu g/mL in a gradient manner, and selecting 0.5 mu g/mL aldehyde ketone-DNPH mixed standard solution as a test sample to be tested;
B. analyzing a sample to be detected by using a liquid chromatograph, selecting 4 factors of mobile phase proportion, flow rate, sample injection amount and column temperature as variables, setting a contrast test, obtaining a rule according to chromatogram peak separation conditions and determining optimal conditions of homogeneous elution;
C. and carrying out gradient elution on the basis of the conclusion of the homogeneous elution experimental conditions to obtain the experimental conditions meeting the preset requirements.
2. The method for detecting the content of the aldehydes and ketones in the passenger car as claimed in claim 1, wherein: and step A, complexing the aldehyde ketone mixed standard solution with DNPH, wherein the concentration is 2 mu g/mL.
3. The method for detecting the content of the aldehydes and ketones in the passenger car as claimed in claim 1, wherein: the step B specifically comprises the following steps: on the basis that a mobile phase is acetonitrile/water, elution is equal gradient, 60% of acetonitrile/40% of water, the flow rate is 1mL/min, the sample injection amount is 25 mu L, 4 factors of the proportion of the mobile phase, the flow rate, the sample injection amount and the column temperature are selected as variables, a contrast test is set, 3 factors are respectively fixed and unchanged, the 4 th factor is changed as a test condition, a liquid chromatogram of a sample to be tested is obtained through analysis, and the test condition is set through observing the separation condition of peaks of 14 aldehyde ketone standard substances.
4. The method for detecting the content of the aldehydes and ketones in the passenger car as claimed in claim 3, wherein: the separation conditions include the time to peak, the shape of the peak and the degree of separation.
5. The method for detecting the content of the aldehydes and ketones in the passenger car as claimed in claim 3, wherein: the experimental conditions are that the proportion of the mobile phase is 55% acetonitrile/45% water-80% acetonitrile/20% water; the flow rate is 0.6mL/min-1.2 mL/min; the sample amount is 10-25 μ L; the column temperature is 25-35 ℃.
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Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2425380C1 (en) * | 2010-06-25 | 2011-07-27 | Федеральное государственное учреждение науки "Федеральный научный центр медико-профилактических технологий управления рисками здоровью населения" Федеральной службы по надзору в сфере защиты прав потребителей и благополучия человека (ФГУН "ФНЦ МПТ УРЗН" РОСПОТРЕБНАДЗОРА) | Method of quantitative analysis of urine dimethyl terephthalate by liquid chromatography |
| CN103728381A (en) * | 2012-10-15 | 2014-04-16 | 深圳出入境检验检疫局工业品检测技术中心 | Liquid chromatographic analysis method of aldehyde ketone compounds |
| CN105738520A (en) * | 2016-02-29 | 2016-07-06 | 广西中烟工业有限责任公司 | Sample liquid preparation method for detecting squalene in cigarette fume based on high performance liquid chromatography |
| CN108732264A (en) * | 2018-04-12 | 2018-11-02 | 中国检验认证集团湖北有限公司 | A method of content of group compounds of aldehydes and ketones in material in detection automobile seat cabin |
| 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 |
| CN109459519A (en) * | 2018-12-30 | 2019-03-12 | 国家建筑装修材料质量监督检验中心 | The method for quickly measuring benzene homologues and aldehyde ketone substance in synthetic material simultaneously |
| CN109781901A (en) * | 2019-03-11 | 2019-05-21 | 山东新华制药股份有限公司 | The efficient liquid phase chromatographic analysis detection method of impurity in a kind of 3,4- dimethoxy benzaldehyde |
| US20200182840A1 (en) * | 2017-08-16 | 2020-06-11 | Henan Taloph Pharmaceutical Co., Ltd. | Identification method and content measurement method for pediatric compound endothelium corneum gigeriae galli chewable tablet |
| CN111505136A (en) * | 2020-04-23 | 2020-08-07 | 一汽奔腾轿车有限公司 | Method for testing harmful volatile matters of non-metallic materials of passenger vehicle |
| CN111505137A (en) * | 2020-04-23 | 2020-08-07 | 一汽奔腾轿车有限公司 | Method for testing harmful volatile matters of interior trim assembly of passenger car |
| CN112684040A (en) * | 2020-12-15 | 2021-04-20 | 山东欧陆检测有限公司 | Method for detecting residual quantity of tolterone in milk and milk powder |
| CN112857925A (en) * | 2021-01-27 | 2021-05-28 | 暨南大学 | Method and device for collecting and analyzing aldehyde and ketone substances in biogas sample |
-
2021
- 2021-12-10 CN CN202111505475.2A patent/CN114252533A/en active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2425380C1 (en) * | 2010-06-25 | 2011-07-27 | Федеральное государственное учреждение науки "Федеральный научный центр медико-профилактических технологий управления рисками здоровью населения" Федеральной службы по надзору в сфере защиты прав потребителей и благополучия человека (ФГУН "ФНЦ МПТ УРЗН" РОСПОТРЕБНАДЗОРА) | Method of quantitative analysis of urine dimethyl terephthalate by liquid chromatography |
| CN103728381A (en) * | 2012-10-15 | 2014-04-16 | 深圳出入境检验检疫局工业品检测技术中心 | Liquid chromatographic analysis method of aldehyde ketone compounds |
| CN105738520A (en) * | 2016-02-29 | 2016-07-06 | 广西中烟工业有限责任公司 | Sample liquid preparation method for detecting squalene in cigarette fume based on high performance liquid chromatography |
| US20200182840A1 (en) * | 2017-08-16 | 2020-06-11 | Henan Taloph Pharmaceutical Co., Ltd. | Identification method and content measurement method for pediatric compound endothelium corneum gigeriae galli chewable tablet |
| CN108732264A (en) * | 2018-04-12 | 2018-11-02 | 中国检验认证集团湖北有限公司 | A method of content of group compounds of aldehydes and ketones in material in detection automobile seat cabin |
| 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 |
| CN109459519A (en) * | 2018-12-30 | 2019-03-12 | 国家建筑装修材料质量监督检验中心 | The method for quickly measuring benzene homologues and aldehyde ketone substance in synthetic material simultaneously |
| CN109781901A (en) * | 2019-03-11 | 2019-05-21 | 山东新华制药股份有限公司 | The efficient liquid phase chromatographic analysis detection method of impurity in a kind of 3,4- dimethoxy benzaldehyde |
| CN111505136A (en) * | 2020-04-23 | 2020-08-07 | 一汽奔腾轿车有限公司 | Method for testing harmful volatile matters of non-metallic materials of passenger vehicle |
| CN111505137A (en) * | 2020-04-23 | 2020-08-07 | 一汽奔腾轿车有限公司 | Method for testing harmful volatile matters of interior trim assembly of passenger car |
| CN112684040A (en) * | 2020-12-15 | 2021-04-20 | 山东欧陆检测有限公司 | Method for detecting residual quantity of tolterone in milk and milk powder |
| CN112857925A (en) * | 2021-01-27 | 2021-05-28 | 暨南大学 | Method and device for collecting and analyzing aldehyde and ketone substances in biogas sample |
Non-Patent Citations (1)
| Title |
|---|
| 纪然等: "液相色谱法测定空气中17种醛酮类化合物", 《化工环保》, vol. 29, no. 02, 15 April 2009 (2009-04-15), pages 188 - 192 * |
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