CN111505136A - Method for testing harmful volatile matters of non-metallic materials of passenger vehicle - Google Patents
Method for testing harmful volatile matters of non-metallic materials of passenger vehicle Download PDFInfo
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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
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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
- G01N30/12—Preparation by evaporation
-
- 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
- G01N30/16—Injection
- G01N30/18—Injection using a septum or microsyringe
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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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
-
- 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
- G01N2030/042—Standards
- G01N2030/047—Standards external
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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
- G01N30/12—Preparation by evaporation
- G01N2030/125—Preparation by evaporation pyrolising
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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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
- G01N2030/326—Control of physical parameters of the fluid carrier of pressure or speed pumps
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
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- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a method for testing harmful volatile matters of non-metallic materials of passenger cars, which comprises the steps of loading the non-metallic materials into a sampling bag, preparing a blank sampling bag with the same specification, separating the harmful volatile matters from an adsorption object to be detected by heating, collecting benzene substances through a TENAX sampling tube, extracting the benzene substances in the TENAX sampling tube through a thermal desorption system, introducing the benzene substances into a gas chromatograph-mass spectrometer, obtaining the quantitative value of each benzene substance through a benzene substance analysis curve, collecting aldehyde ketone substances through a DNPH sampling tube, preparing an aldehyde ketone substance reagent through an acetonitrile elution DNPH sampling tube, introducing the aldehyde ketone substance reagent into a high performance liquid chromatograph-diode array detector, obtaining the quantitative value of each aldehyde ketone substance through the aldehyde ketone substance analysis curve, and finally calculating the concentration of each harmful volatile matter. According to the invention, the concentration of harmful substances volatilized from the non-metallic materials is detected, so that the unqualified interior trim assembly of the vehicle is locked, and targeted improvement is realized.
Description
Technical Field
The invention belongs to the technical field of detection of harmful volatile matters in the environment in an automobile, and particularly relates to a method for testing harmful volatile matters in a non-metallic material of a passenger car.
Background
With the rapid development of national economy, the living standard of people is constantly promoted, and passenger cars have become indispensable vehicles for people to go out. With the increasing popularity of passenger vehicles, the public has increasingly high demands on the dynamics, fuel economy, braking performance, steering stability, and ride comfort of passenger vehicles.
In recent years, with the increasing environmental awareness of the public, namely the increasing awareness of self-protection, the problem of pollution of the internal space of a passenger car is more and more exposed to the public, which begins as early as 2013, and the passenger car is complained continuously, and vehicles including a plurality of international high-grade vehicle systems have poor air quality in the car, contain sharp nose and eyes in the car and cause uncomfortable gas in the throat, so that children are used as high-frequency users of family passenger cars, and the health of the children is seriously threatened. Therefore, the public attention on toxic and harmful volatile matters in the interior of passenger cars is higher and higher, and the concern is also a problem which is heavily considered when people buy cars.
The poisonous and harmful volatile matters in the vehicle are mainly from non-metal materials, including materials used for manufacturing instrument panel assemblies, door guard plate assemblies, steering wheel assemblies, seat assemblies and the like, and the poisonous and harmful organic matters or aldehyde ketone substances emitted by the materials seriously pollute the environment in the vehicle and threaten the health of drivers and passengers.
At present, the state sets up an industry standard for environmental protection, and for the quality of the air of the whole automobile in the automobile industry, the state sets up an industry standard of HJ/T400-2007 'method for sampling and measuring volatile organic compounds and aldehydes and ketones in the automobile', and the industry standard is applicable to: the method comprises the steps of measuring the settings of sampling points of volatile organic compounds and aldehyde and ketone substances in the passenger compartment of the motor vehicle, the technical requirements of sampling environmental conditions, sampling methods and equipment, corresponding measuring methods and equipment, data processing, quality assurance and the like. According to the application range, the HJ/T400-2007 industrial standard is used for detecting the content of toxic and harmful substances volatilized into the interior space of the vehicle, but the content of the toxic and harmful substances of dozens of non-metal raw materials adopted by the interior parts of the vehicle cannot be determined, and whether the content is a main source for causing the indexes of the harmful substances in the vehicle to exceed the standard or not can not be determined; if the vehicle is unqualified, even if one or more harmful substances can be detected to be out of standard, the corresponding harmful substances cannot be judged from which material of which part in the vehicle comes. In addition, the contribution value of various non-metal raw materials adopted by the vehicle interior parts to toxic and harmful substances in the vehicle interior cannot be determined.
Further, even if it is determined that the detection result of a certain part in the vehicle is not acceptable, it is impossible to determine which kind of non-metallic material is specifically unacceptable because the material of which the part is made is different. In addition, even if the same material is used, the content of toxic and harmful substances can be significantly different due to different suppliers or different manufacturing and processing links.
In summary, according to the prior art, whether the air quality in the vehicle interior is qualified or not can be accurately detected, and the type of specific unqualified substances can also be detected, but the source of toxic and harmful substances cannot be locked, so that corresponding responsibility tracing or improvement measures cannot be taken in a targeted manner, and the problem of pollution to the air environment in the vehicle cannot be fundamentally solved.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the method for testing the harmful volatile matters in the passenger non-metal material, so that the concentration of different types of toxic and harmful substances volatilized from the non-metal material of the passenger car can be quickly and accurately detected, and the direction is pointed for fundamentally solving the problem of air environmental pollution in the passenger car. The technical scheme of the invention is as follows by combining the attached drawings of the specification:
a method for testing harmful volatile matters of non-metallic materials of passenger cars comprises the following steps:
s1: selecting qualified Tedlar sampling bags with the specification of 10 liters through leak detection and aging tests;
s2: loading a non-metal material sample into a sampling bag, preparing a blank sampling bag with the same specification, respectively filling 5 times of high-purity nitrogen into the non-metal material sample sampling bag and the blank sampling bag after the non-metal material sample is replaced with gas in the sampling bag by the high-purity nitrogen, heating to volatilize harmful substances in the non-metal material sample sampling bag and the blank sampling bag, respectively collecting benzene substances in harmful volatile substance mixed gas in the non-metal material sample sampling bag and the blank sampling bag by using a TENAX sampling tube at a preset sampling flow rate and sampling time, respectively collecting aldehyde ketone substances in the harmful volatile substance mixed gas in the non-metal material sample sampling bag and the blank sampling bag by using a DNPH sampling tube at a preset sampling flow rate and sampling time, and sealing and storing the collected TENAX sampling tube and DNPH sampling tube;
s3: introducing the gas mixed with benzene substances, which is heated and separated from the TENAX sampling tube by the thermal desorption system, into a gas chromatography-mass spectrometer, performing qualitative and quantitative analysis by an external standard method, generating and outputting a corresponding benzene substance analysis curve, and obtaining quantitative values of the benzene substances in the non-metal material sample sampling bag and the blank sampling bag; reacting aldehyde ketone substances in gas adsorbed by the DNPH sampling tube with 2.4-dinitrophenylhydrazine, eluting products obtained after the aldehyde ketone substances in the DNPH sampling tube react with the 2.4-dinitrophenylhydrazine through acetonitrile, qualitatively and quantitatively analyzing the reagent by using a high performance liquid chromatograph-diode array detector through an external standard method, generating and outputting corresponding aldehyde ketone substance analysis curves, and obtaining quantitative values of the aldehyde ketone substances in the non-metal material sample sampling bag and the blank sampling bag;
s4: the concentration of harmful volatile substances is obtained by calculation according to the following formula (1):
CVOC＝(A-BL)×1000/(V×T)·················(1)
in the above formula (1):
CVOCconcentration of harmful volatile substances, unit: microgram/cubic meter;
a is the quantitative value of harmful volatile substances in the non-metallic material sample sampling bag, and the unit is as follows: nanogram;
b L is the quantitative value of harmful volatile substance in the blank sampling bag, unit is nanogram;
v is the sampling flow rate in units of: ml/min;
t is the sampling time, unit: and (3) minutes.
Further, the non-metal material sample to be detected is a non-metal material sample with a constant plate thickness, which is cut at a flat position of a vehicle inner part, and the size of the non-metal material sample is 8 cm × 10 cm.
Further, the benzene-based substances include: benzene, toluene, ethylbenzene, xylene, and styrene;
the aldehyde ketone substances comprise: formaldehyde, acetaldehyde and acrolein.
Further, in step S1, the leak detection and aging process of the sampling bag is as follows:
s1.1 sampling bag leak detection
Pumping air in the sampling bag until the sampling bag is in a vacuum shriveled state, sealing the sampling bag, observing whether air enters the sampling bag after the sampling bag is placed for a preset time, if no air enters the sampling bag, detecting the leakage of the sampling bag to be qualified, and if air enters the sampling bag, detecting the leakage of the sampling bag to be unqualified;
s1.2 sampling bag aging detection
Turn out the sampling bag inside, through heating to predetermineeing the temperature to the sampling bag inner face to keep for a certain time, realize fully ageing the back to the sampling bag inner face, turn back the sampling bag inner face to clean the sampling bag inner face, gather the harmful substance concentration in the ageing back sampling bag through the mode of dashing into nitrogen gas and heating at last, and compare with harmful substance concentration limit value, the blank value limit value of sampling bag is specifically as following one:
watch 1
| Composition (I) | Sampling bag blank value limit (microgram/sampling bag) |
| Formaldehyde (I) | <0.075 |
| Acetaldehyde | <0.075 |
| Acrolein | <0.075 |
| Benzene and its derivatives | <0.05 |
| Toluene | <0.05 |
| Xylene | <0.05 |
| Ethylbenzene production | <0.05 |
| Styrene (meth) acrylic acid ester | <0.05 |
Further, in step S2, before filling 5 liters of nitrogen gas into each of the non-metal material sample bag and the blank sampling bag, the non-metal material sample bag and the blank sampling bag need to be cleaned, and the cleaning process is as follows: and respectively filling 5 liters of nitrogen into the non-metallic material sample sampling bag and the blank sampling bag, then pumping out the nitrogen, and repeatedly filling and pumping out the nitrogen for three times according to the same operation standard.
Further, in the step S2, in the process of heating to volatilize harmful substances in the non-metallic material sample sampling bag and the blank sampling bag, the heating temperature is 65 ℃, the heating time is 2 hours, and the non-metallic material sample sampling bag is kneaded before the heating is finished, so that the harmful volatile substances separated out from the non-metallic material sample sampling bag are uniformly distributed in the sampling bag.
Further, in step S2, first, 100 ml of the harmful volatile substance mixed gas is led out from the non-metallic material sample bag and the blank sample bag, and then the harmful volatile substance mixed gas is collected through the TENAX sample tube and the DNPH sample tube;
respectively collecting 1 liter of harmful volatile substance mixed gas in a non-metal material sample sampling bag and a blank sampling bag by using a TENAX sampling pipe at a sampling rate of 0.2 liter/minute;
at a sampling rate of 0.5 l/min, 3 l of the mixture of harmful volatiles in the non-metallic material sample bag and the blank sample bag were collected using DNPH sampling tubes, respectively.
Further, in step S3, the setting conditions of the thermal desorption system specifically include: the dry blowing time is 3 minutes, the desorption time is 10 minutes, the desorption temperature is 300 ℃, the cold trap temperature is minus 10 ℃, the temperature is kept for 3 minutes, and the outlet split ratio is 50: 1;
the set conditions of the gas chromatography-mass spectrometer are specifically that a chromatographic column Ultra2 is 50 m, × 320 m, × 0.52 m and 3926.52 m, the flow rate of the column is 1 ml/min, the temperature of a column box is kept at 40 ℃ for 3 min, then the temperature is increased to 90 ℃ at the heating rate of 10 ℃/min, the temperature of 90 ℃ is kept for 5 min, then the temperature is increased to 280 ℃ at the heating rate of 10 ℃/min, the temperature of 280 ℃ is kept for 6 min, the temperature of an ion source is 230 ℃, and the mass number is 35 amu-450 amu.
The set conditions of the high performance liquid chromatograph are specifically that a chromatographic column Syncronics C18 is 4.6 mm × 250 mm, a column box is 35 ℃, a detector DAD is arranged, a mobile phase is acetonitrile or water, the flow rate is 0.5 ml/min, and the sample injection amount is 15 microliters.
Further, when the emission amount of volatile organic compounds of the non-metallic material sample is large, the flow dividing ratio of the outlet of the thermal desorption system is adjusted to reduce the sample inlet amount of the gas chromatography-mass spectrometer and increase the high concentration point of the standard reagent when the benzene substance is analyzed by the gas chromatography-mass spectrometer;
when analyzing aldehyde ketone substances through a high performance liquid chromatograph, for a reagent containing aldehyde ketone substances with high concentration, the reagent is diluted so as to reduce the concentration of the reagent to be within the range of an analysis curve.
Further, according to the step S1 — the step S4, the concentrations of harmful volatile matters volatilized from the non-metallic materials are respectively obtained, and according to the concentrations of various harmful volatile matters emitted from the non-metallic materials, the non-metallic materials which are not qualified are locked, and the non-qualified non-metallic materials are improved in a targeted manner.
Compared with the prior art, the invention has the beneficial effects that:
the method for testing harmful volatile matters in the non-metallic materials of the passenger vehicles can realize the concentration of different types of harmful volatile matters released by the non-metallic materials of different types of passenger vehicles, can accurately lock the source of toxic and harmful substances causing the air environment of the whole vehicle not to reach the standard, and can take corresponding accountability or improvement measures in a targeted manner, thereby fundamentally solving the problem of air environment pollution in the passenger vehicles;
drawings
FIG. 1 is a schematic structural diagram of a testing and sampling device for non-metallic materials of passenger cars according to the invention.
FIG. 2 is a schematic diagram of an analysis curve of benzene substances generated and output by a gas chromatography-mass spectrometer in the testing method of the invention;
FIG. 3 is a schematic diagram of an analytical curve of aldehydes and ketones generated and outputted by a high performance liquid chromatograph-diode array detector in the testing method of the present invention;
in the figure:
1-oven, 2-sampling bag, 3-non-metallic material sample,
4-valves, 5-TENAX trap, 6-DNPH trap,
7-Teflon tube, 8-sampling pump, 9-flowmeter.
Detailed Description
For clearly and completely describing the technical scheme and the specific working process thereof, the specific implementation mode of the invention is as follows by combining the attached drawings of the specification:
before the description of the embodiments of the present invention, it should be noted that:
1. in the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
2. In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through an intermediate. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
3. In particular descriptions of the present specification, references to the description of the term "one embodiment," "some embodiments," "an example," "a particular example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
The invention discloses a method for testing harmful volatile matters in non-metallic materials of passenger cars, which adopts a bag method, puts the non-metallic materials with standard size into a sampling bag with the specification of 10 liters, adopts a thermal desorption method, separates the harmful volatile matters including benzene series substances and aldehyde ketone substances from the surface of the non-metallic materials by heating, and then detects the concentration of the harmful volatile matters. The test method comprises the following specific steps:
s1: selecting qualified sampling bags;
according to the testing method, a Tedlar bag is selected as a sampling bag, the Tedlar bag is produced by DuPont and made of a polyvinyl fluoride film, and the resistance and durability of the polyvinyl fluoride film to sunlight, chemical solvents, acid-base corrosion, moisture and oxidation are remarkably improved due to the fact that a fluorocarbon covalent bond in polyvinyl fluoride is far stronger than chemical bonds in other polymers; the surface repulsion of the polyvinyl fluoride film is large, so that dust can be prevented from being polluted, the cleaning and the maintenance are easy, and the polyvinyl fluoride film is not damaged even if the polyvinyl fluoride film is the strongest detergent; from 70 ℃ below zero to 110 ℃, the polyvinyl fluoride film can ensure excellent performance, and the instantaneous temperature peak value can not be damaged even when the temperature peak value reaches 200 ℃; according to the advantages of the characteristics, a Tedlar bag is preferably adopted as the sampling bag in the testing method.
S1.1 sampling bag leak detection
Taking a sampling bag, pumping air in the sampling bag by using a constant-flow air sampling pump until the sampling bag is in a vacuum shriveled state, sealing the sampling bag, standing for 10 minutes, observing whether air enters the sampling bag, if no air enters the sampling bag, detecting the leakage of the sampling bag, and if air enters the sampling bag, detecting the leakage of the sampling bag, and determining that the sampling bag is unqualified;
selecting a sampling bag qualified for leak detection to carry out the next step;
s1.2 sampling bag aging detection
S1.2.1, turning out the inner surface of a sampling bag, putting the sampling bag into an experimental box, and heating the sampling bag for aging at 78-82 ℃ for 10-12 hours;
s1.2.2, opening the door of the experiment box, replacing the air in the experiment box for 30 minutes, namely, exposing the sampling bag in the experiment box in a normal temperature environment for 30 minutes, realizing natural cooling of the sampling bag, then turning the sampling bag 180 degrees, turning the bottom surface of the sampling bag upwards in the step S1.2.1, closing the door of the experiment box, heating again to realize aging treatment, wherein the heating temperature is 78-82 ℃, the heating time is 2-3 hours, and finally, the inner surface of the sampling bag is uniformly aged through the step;
s1.2.3 turning the inner surface of the sampling bag back to the inner side, evacuating the gas in the sampling bag by a diaphragm vacuum pump, filling high-purity nitrogen with the volume of 30-40% of the volume of the sampling bag, pumping out the nitrogen, and repeating the same operation for three times to remove the pollutants attached to the inner wall of the sampling bag by nitrogen cleaning;
s1.2.4 filling 5L nitrogen gas into the sampling bag, and heating the sampling bag at 65 deg.C for 1 hr 50 min to 2 hr 10 min;
s1.2.5 detecting the concentration of benzene and aldehyde ketone in the sampling bag, wherein the benzene is collected by a TENAX sampling tube, and the benzene comprises: benzene, toluene, ethylbenzene, xylene, and styrene; the aldehyde ketone substances are collected by adopting a DNPH sampling tube, and the aldehyde ketone substances comprise: formaldehyde, acetaldehyde and acrolein;
in this step, the concentration of benzene substances and aldehyde ketone substances in the sampling bag is detected, that is, the blank value of the sampling bag is obtained, whether the sampling bag releases harmful volatile substances in the actual sampling process can be reflected through whether the blank value is qualified, and the accuracy of the detection result of the sample to be detected loaded in the sampling bag is affected, that is, whether the cleanliness of the sampling bag is qualified is detected through the aging detection step, if the blank value of the sampling bag is within the blank value limit value of the sampling bag, the cleanliness of the sampling bag is qualified, if the blank value of the sampling bag exceeds the blank value limit value of the sampling bag, the cleanliness of the sampling bag is unqualified, and the blank value limit values of the sampling bag are specifically as the following table one:
watch 1
| Composition (I) | Sampling bag blank value limit (microgram/sampling bag) |
| Formaldehyde (I) | <0.075 |
| Acetaldehyde | <0.075 |
| Acrolein | <0.075 |
| Benzene and its derivatives | <0.05 |
| Toluene | <0.05 |
| Xylene | <0.05 |
| Ethylbenzene production | <0.05 |
| Styrene (meth) acrylic acid ester | <0.05 |
S1.2.6 selecting the sampling bag with qualified cleanliness to carry out the next step, repeating the steps S1.2.3-S1.2.5 on the sampling bag with unqualified cleanliness, and cleaning the sampling bag again until the cleanliness is qualified or the sampling bag is discarded.
S2: sampling;
s2.1, preparing a non-metallic material sample sampling bag and a blank sampling bag of an assembly:
firstly, taking a uniform non-metallic material sample by using scissors at the flat position of an assembly in a vehicle, keeping the thickness of the non-metallic material sample unchanged, wherein the size of the non-metallic material sample is 8 cm × 10 cm, flatly placing the non-metallic material sample into a sampling bag with the size specification of 10 liters, and enabling the exposed surface of the assembly sample in the air environment of the vehicle to face upwards to form the non-metallic material sample sampling bag;
the purpose of adopting the blank sampling bag in the step is to avoid the inaccuracy of the detection result caused by the pollution of the detection equipment or the detection process. Namely, under the same operating specification, the content of the harmful substances in the non-metallic material sample sampling bag minus the content of the harmful substances in the blank sampling bag is the content of the harmful substances released by the real non-metallic material sample.
S2.2 cleaning the sampling bag:
respectively filling 5 liters of nitrogen into the non-metal material sample sampling bag and the blank sampling bag, then extracting the nitrogen, and repeatedly filling and extracting the nitrogen for three times according to the same operation standard so as to clean pollutants attached to the inner walls of the non-metal material sample sampling bag and the blank sampling bag by the nitrogen;
s2.3, heating to separate out harmful volatile substances:
respectively filling 5 liters of nitrogen into the non-metal material sample sampling bag and the blank sampling bag again, putting the non-metal material sample sampling bag and the blank sampling bag which are filled with the nitrogen into a sealed environment with the temperature of 65 ℃ for heating for 2 hours, and kneading the assembly non-metal material sample sampling bag in a constant temperature environment 10 minutes before the heating is finished so as to realize that harmful volatile substances separated out from the non-metal material sample sampling bag are uniformly distributed in the sampling bag;
s2.4, collecting harmful volatile substances by a sampling pipe:
under the constant temperature environment, respectively leading out 100 ml of harmful volatile substance mixed gas from a non-metal material sample sampling bag and a blank sampling bag, respectively collecting 1 l of harmful volatile substance mixed gas in the non-metal material sample sampling bag and the blank sampling bag by using a TENAX sampling pipe at a sampling rate of 0.2 l/min, and respectively collecting 3 l of harmful volatile substance mixed gas in the non-metal material sample sampling bag and the blank sampling bag by using a DNPH sampling pipe at a sampling rate of 0.5 l/min;
the mixed gas of the harmful volatile matters is the mixed gas of the harmful volatile matters and nitrogen;
s2.5, saving a sampling tube:
respectively wrapping and sealing the collected TENAX sampling tube and DNPH sampling tube by an aluminum foil or aluminum bag, placing the sealed packets into a zipper plastic bag, and marking;
the TENAX sampling tube is used for collecting benzene substances in harmful volatile matters, and the benzene substances comprise: benzene, toluene, ethylbenzene, xylene, and styrene;
the DNPH sampling tube is used for collecting aldehyde ketone substances in harmful volatile substances, and the aldehyde ketone substances comprise: formaldehyde, acetaldehyde and acrolein;
after the sampling of the TENAX sampling tube and the DNPH sampling tube is finished, quantitative analysis is carried out as soon as possible, if analysis cannot be carried out in time, the TENAX sampling tube and the DNPH sampling tube are stored in a refrigerator to be refrigerated, the refrigerating temperature is 4-10 ℃, and the longest storage life of the TENAX sampling tube and the DNPH sampling tube is one week.
S3: analyzing;
s3.1 the process of benzene substance analysis is as follows:
and (3) performing qualitative and quantitative analysis on benzene substances in the harmful volatile substances collected by the TENAX sampling tube in the step S2.4 by using a gas chromatography-mass spectrometer equipped with a thermal desorption system by adopting an analysis external standard method, wherein:
separating the benzene substances collected by the TENAX sampling tube from the TENAX sampling tube by the thermal desorption system by using a thermal desorption method to form a gas mixed with the benzene substances;
the set conditions of the thermal desorption system are specifically as follows: the dry blowing time is 3 minutes, the desorption time is 10 minutes, the desorption temperature is 300 ℃, the cold trap temperature is minus 10 ℃, the temperature is kept for 3 minutes, and the outlet split ratio is 50: 1;
inputting the gas mixed with benzene substances, which is heated and separated from a TENAX sampling tube in a thermal desorption system, into a gas chromatography-mass spectrometer, wherein the method comprises the following steps: generating and outputting a corresponding benzene substance analysis curve of a benzene substance standard reagent containing benzene, toluene, ethylbenzene, xylene and styrene by a gas chromatography-mass spectrometer, wherein the curve is shown in fig. 2; finally, respectively reading and obtaining quantitative values of benzene, toluene, ethylbenzene, xylene and styrene in the non-metal material sample sampling bag and the blank sampling bag of the assembly according to the corresponding benzene substance analysis curve;
the set conditions of the gas chromatography-mass spectrometer are specifically that a chromatographic column Ultra2 is 50 m, × 320 m, × 0.52 m and 3926.52 m, the flow rate of the column is 1 ml/min, the temperature of a column box is kept at 40 ℃ for 3 min, then the temperature is increased to 90 ℃ at the heating rate of 10 ℃/min, the temperature of 90 ℃ is kept for 5 min, then the temperature is increased to 280 ℃ at the heating rate of 10 ℃/min, and the temperature of 280 ℃ is kept for 6 min, the temperature of an ion source is 230 ℃, and the mass number is 35 amu-450 amu;
for a sample with large volatile organic compound emission amount, the flow split ratio of the outlet of the thermal desorption system can be adjusted to reduce the sample introduction amount of the gas chromatography-mass spectrometer and increase the high concentration point of the standard reagent for analysis;
s3.2 the analytical process of the aldehyde ketone substances is as follows:
firstly, reacting an aldehyde ketone substance in the gas adsorbed by the DNPH sampling tube in the step S2.4 with 2.4-dinitrophenylhydrazine, wherein the aldehyde ketone substance can be detected in the DNPH sampling tube in advance because the 2.4-dinitrophenylhydrazine and the aldehyde ketone substance can generate a color reaction; then, extracting a proper amount of chromatographic pure acetonitrile by using a glass syringe, connecting the glass syringe to a DNPH sampling tube, slowly extracting to elute the derivative obtained after the reaction of the 2, 4-dinitrophenylhydrazine and the aldehyde ketone substances by using the acetonitrile, and fixing the volume of the eluent as a reagent to a measuring flask or a similar container of 5 ml; finally, extracting 20 microliters of reagent, adopting an aldehyde-ketone-DNPH derivative mixed sample or equivalent manufactured by RADIAN company as an aldehyde and ketone substance standard reagent including formaldehyde, acetaldehyde and acrolein, and carrying out qualitative and quantitative analysis on the aldehyde and ketone substances in the reagent by using an external standard method through a high performance liquid chromatograph-diode array detector to generate and output a corresponding aldehyde and ketone substance analysis curve, as shown in FIG. 3; finally, according to the corresponding aldehyde ketone substance analysis curves, respectively reading and obtaining quantitative values of formaldehyde, acetaldehyde and acrolein in the non-metal material sample sampling bag and the blank sampling bag;
the set conditions of the high performance liquid chromatograph are that a chromatographic column Syncronics C18 is 4.6 mm × 250 mm, a column box is 35 ℃, a detector DAD is arranged, a mobile phase is acetonitrile or water, the flow rate is 0.5 ml/min, and the sample injection amount is 15 microliter;
for high concentrations of reagents, the reagents may be diluted to bring the concentration of the reagents down within the analytical curve;
the refrigerated storage period of the reagent eluted and extracted by acetonitrile is one week.
The instruction control requirements of the analysis process of the benzene substances and the aldehyde and ketone substances are as follows:
watch two
Under the specified analysis conditions, analyzing all harmful substances with retention time between the retention time of n-hexane (C6) and the retention time of n-hexadecane (C16) on the basis of the area with the minimum area rejection value of 0.01 g of toluene, and confirming the substance concentration corresponding to the peak area by using an analysis curve of toluene according to the response peak area of all harmful substances between the retention time of n-hexane (C6) and the retention time of n-hexadecane (C16) read by an analysis device;
the benzene substance analysis process S3.1 and the aldehyde ketone substance analysis process S3.2 can be performed simultaneously without being sequenced.
S4: calculating;
rounding off the quantitative values of benzene, toluene, ethylbenzene, xylene and styrene in the non-metal material sample sampling bag and the blank sampling bag obtained in the step S3 and the quantitative values of formaldehyde, acetaldehyde and acrolein in the non-metal material sample sampling bag and the blank sampling bag, respectively, taking the three decimal places, and calculating the concentration of the corresponding harmful volatile substances according to the following formula (1);
CVOC＝(A-BL)×1000/(V×T)·················(1)
in the above formula (1):
CVOCis the concentration of the corresponding harmful volatile substance, unit: microgram/cubic meter;
a is the quantitative value of the harmful volatile substances in the corresponding non-metallic material sample sampling bag, and the unit is as follows: nanogram;
b L is the quantitative value of harmful volatile substance in corresponding blank sampling bag, with unit of nanogram;
v is the sampling flow rate in units of: ml/min;
t is the sampling time, unit: and (3) minutes.
The concentrations of benzene, toluene, ethylbenzene, xylene, styrene, formaldehyde, acetaldehyde and acrolein volatilized from the corresponding samples are obtained through calculation in the steps.
The measurement results of the samples of the partial types of assemblies obtained by the above steps are shown in the following table three:
watch III
S5 locking unqualified non-metallic materials
According to the steps S1 to S4, different non-metal materials are tested respectively, the concentration of benzene substances and aldehyde ketone substances volatilized by each non-metal material is obtained, and the non-metal materials which are not qualified are locked according to the analysis of the test results shown in the third table.
According to the third table, it can be analyzed that if the formaldehyde of the whole vehicle is unqualified, the locking is related to the material 2, the material 3, the material 4 and the material 8, and the purpose of reducing the formaldehyde volatilization in the vehicle can be achieved by modifying the locked material.
In the method for testing harmful volatile matters in non-metallic materials of passenger cars, the structure of the sampling device adopted in the sampling step is as follows:
as shown in fig. 1, the sampling apparatus includes: oven 1, sampling bag 2, valve 4, TENAX trap 5, DNPH trap 6, Teflon tube 7, sampling pump 8 and flow meter 9.
The wall of the oven 1 is provided with a mounting hole, and the oven 1 is provided with an operation window, so that a tester can conveniently operate the internal device.
Two sampling bags 2 are arranged and are placed in the oven 1, wherein one sampling bag is used for containing a non-metal material sample 3, and the other sampling bag is empty;
the sampling bag 2 adopts a Tedlar bag.
The Teflon tube 7 penetrates through the sampling bin 1, and the length of the Teflon tube extending out of the sampling bin 1 is not more than 2 centimeters.
The number of the valves 4 is four, and the four valves are respectively and correspondingly installed at one end of the Teflon tube 7 connected with the sampling bag 2 so as to control the flow of the corresponding sampling bag 2 and the external air.
The two TENAX collecting pipes and the two DNPH collecting pipes are respectively and correspondingly detachably arranged at one end of a Teflon pipe 7 connected with a sampling pump 8, wherein one TENAX collecting pipe and one DNPH collecting pipe are correspondingly arranged on the Teflon pipe 7 correspondingly connected with each sampling bag 2;
the sampling pump 8 is connected with the flowmeter 9 through a pipeline, and the flowmeter 9 is used for measuring the sampling flow of the sampling pump 8 which is correspondingly connected;
the sampling pump 8 is respectively connected with a high-purity nitrogen source pipeline, so that high-purity nitrogen is pumped into the sampling bag 2 through the sampling pump 8 through the Teflon pipe 7;
The above-described embodiments of the present invention should not be construed as limiting the scope of the present invention. Any other corresponding changes and modifications made according to the technical idea of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. A method for testing harmful volatile matters of non-metallic materials of passenger vehicles is characterized by comprising the following steps:
the test method comprises the following steps:
s1: selecting qualified Tedlar sampling bags with the specification of 10 liters through leak detection and aging tests;
s2: loading a non-metal material sample into a sampling bag, preparing a blank sampling bag with the same specification, respectively filling 5 times of high-purity nitrogen into the non-metal material sample sampling bag and the blank sampling bag after the non-metal material sample is replaced with gas in the sampling bag by the high-purity nitrogen, heating to volatilize harmful substances in the non-metal material sample sampling bag and the blank sampling bag, respectively collecting benzene substances in harmful volatile substance mixed gas in the non-metal material sample sampling bag and the blank sampling bag by using a TENAX sampling tube at a preset sampling flow rate and sampling time, respectively collecting aldehyde ketone substances in the harmful volatile substance mixed gas in the non-metal material sample sampling bag and the blank sampling bag by using a DNPH sampling tube at a preset sampling flow rate and sampling time, and sealing and storing the collected TENAX sampling tube and DNPH sampling tube;
s3: introducing the gas mixed with benzene substances, which is heated and separated from the TENAX sampling tube by the thermal desorption system, into a gas chromatography-mass spectrometer, performing qualitative and quantitative analysis by an external standard method, generating and outputting a corresponding benzene substance analysis curve, and obtaining quantitative values of the benzene substances in the non-metal material sample sampling bag and the blank sampling bag; reacting aldehyde ketone substances in gas adsorbed by the DNPH sampling tube with 2.4-dinitrophenylhydrazine, eluting products obtained after the aldehyde ketone substances in the DNPH sampling tube react with the 2.4-dinitrophenylhydrazine through acetonitrile, qualitatively and quantitatively analyzing the reagent by using a high performance liquid chromatograph-diode array detector through an external standard method, generating and outputting corresponding aldehyde ketone substance analysis curves, and obtaining quantitative values of the aldehyde ketone substances in the non-metal material sample sampling bag and the blank sampling bag;
s4: the concentration of harmful volatile substances is obtained by calculation according to the following formula (1):
CVOC＝(A-BL)×1000/(V×T)·················(1)
in the above formula (1):
CVOCconcentration of harmful volatile substances, unit: microgram/cubic meter;
a is the quantitative value of harmful volatile substances in the non-metallic material sample sampling bag, and the unit is as follows: nanogram;
b L is the quantitative value of harmful volatile substance in the blank sampling bag, unit is nanogram;
v is the sampling flow rate in units of: ml/min;
t is the sampling time, unit: and (3) minutes.
2. The method for testing harmful volatile matters in the non-metallic materials of the passenger car as claimed in claim 1, wherein:
the non-metal material sample to be detected is a non-metal material sample with a constant plate thickness, which is cut at a flat position of a vehicle inner part, and the size of the non-metal material sample is 8 cm × 10 cm.
3. The method for testing harmful volatile matters in the non-metallic materials of the passenger car as claimed in claim 1, wherein:
the benzene substances comprise: benzene, toluene, ethylbenzene, xylene, and styrene;
the aldehyde ketone substances comprise: formaldehyde, acetaldehyde and acrolein.
4. The method for testing harmful volatile matters in the non-metallic materials of the passenger car as claimed in claim 1, wherein:
in step S1, the leak detection and aging process of the sampling bag is as follows:
s1.1 sampling bag leak detection
Pumping air in the sampling bag until the sampling bag is in a vacuum shriveled state, sealing the sampling bag, observing whether air enters the sampling bag after the sampling bag is placed for a preset time, if no air enters the sampling bag, detecting the leakage of the sampling bag to be qualified, and if air enters the sampling bag, detecting the leakage of the sampling bag to be unqualified;
s1.2 sampling bag aging detection
Turn out the sampling bag inside, through heating to predetermineeing the temperature to the sampling bag inner face to keep for a certain time, realize fully ageing the back to the sampling bag inner face, turn back the sampling bag inner face to clean the sampling bag inner face, gather the harmful substance concentration in the ageing back sampling bag through the mode of dashing into nitrogen gas and heating at last, and compare with harmful substance concentration limit value, the blank value limit value of sampling bag is specifically as following one:
watch 1
5. The method for testing harmful volatile matters in the non-metallic materials of the passenger car as claimed in claim 1, wherein:
in step S2, before 5 liters of nitrogen gas is filled into the non-metal material sample bag and the blank sampling bag, the non-metal material sample bag and the blank sampling bag need to be cleaned, and the cleaning process is as follows: and respectively filling 5 liters of nitrogen into the non-metallic material sample sampling bag and the blank sampling bag, then pumping out the nitrogen, and repeatedly filling and pumping out the nitrogen for three times according to the same operation standard.
6. The method for testing harmful volatile matters in the non-metallic materials of the passenger car as claimed in claim 1, wherein:
in the step S2, in the process of heating to volatilize harmful substances in the non-metallic material sample sampling bag and the blank sampling bag, the heating temperature is 65 ℃, the heating time is 2 hours, and the non-metallic material sample sampling bag is kneaded before the heating is finished, so that the harmful volatile substances separated out from the non-metallic material sample sampling bag are uniformly distributed in the sampling bag.
7. The method for testing harmful volatile matters in the non-metallic materials of the passenger car as claimed in claim 1, wherein:
in the step S2, first, 100 ml of mixed gas of harmful volatile matters is led out from the non-metallic material sample bag and the blank sample bag, and then the mixed gas of harmful volatile matters is collected through a TENAX sample tube and a DNPH sample tube;
respectively collecting 1 liter of harmful volatile substance mixed gas in a non-metal material sample sampling bag and a blank sampling bag by using a TENAX sampling pipe at a sampling rate of 0.2 liter/minute;
at a sampling rate of 0.5 l/min, 3 l of the mixture of harmful volatiles in the non-metallic material sample bag and the blank sample bag were collected using DNPH sampling tubes, respectively.
8. The method for testing harmful volatile matters in the non-metallic materials of the passenger car as claimed in claim 1, wherein:
in step S3, the setting conditions of the thermal desorption system are specifically: the dry blowing time is 3 minutes, the desorption time is 10 minutes, the desorption temperature is 300 ℃, the cold trap temperature is minus 10 ℃, the temperature is kept for 3 minutes, and the outlet split ratio is 50: 1;
the set conditions of the gas chromatography-mass spectrometer are specifically that a chromatographic column Ultra2 is 50 m, × 320 m, × 0.52 m and 3926.52 m, the flow rate of the column is 1 ml/min, the temperature of a column box is kept at 40 ℃ for 3 min, then the temperature is increased to 90 ℃ at the heating rate of 10 ℃/min, the temperature of 90 ℃ is kept for 5 min, then the temperature is increased to 280 ℃ at the heating rate of 10 ℃/min, the temperature of 280 ℃ is kept for 6 min, the temperature of an ion source is 230 ℃, and the mass number is 35 amu-450 amu.
The set conditions of the high performance liquid chromatograph are specifically that a chromatographic column Syncronics C18 is 4.6 mm × 250 mm, a column box is 35 ℃, a detector DAD is arranged, a mobile phase is acetonitrile or water, the flow rate is 0.5 ml/min, and the sample injection amount is 15 microliters.
9. The method for testing harmful volatile substances in non-metallic materials of passenger cars according to claim 1 or 8, characterized in that:
when the benzene substances are analyzed by the gas chromatography-mass spectrometer, when the volatile organic compound emission amount of the non-metallic material sample is large, the flow dividing ratio of the outlet of the thermal desorption system is adjusted to reduce the sample introduction amount of the gas chromatography-mass spectrometer and increase the high concentration point of the standard reagent;
when analyzing aldehyde ketone substances through a high performance liquid chromatograph, for a reagent containing aldehyde ketone substances with high concentration, the reagent is diluted so as to reduce the concentration of the reagent to be within the range of an analysis curve.
10. The method for testing harmful volatile matters in the non-metallic materials of the passenger car as claimed in claim 1, wherein:
according to the step S1-the step S4, the concentration of harmful volatile matters volatilized from each non-metal material is respectively obtained, and according to the concentration of various harmful volatile matters emitted from each non-metal material, unqualified non-metal materials are locked, and the unqualified non-metal materials are pertinently improved.
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| CN112595559A (en) * | 2020-12-04 | 2021-04-02 | 广东省测试分析研究所（中国广州分析测试中心） | Universal vehicle material volatile organic compound sampling system and detection method |
| 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 |
| CN115060825A (en) * | 2022-06-21 | 2022-09-16 | 奇瑞汽车股份有限公司 | Method for detecting phthalate ester in vehicle product |
| CN116087383A (en) * | 2023-02-16 | 2023-05-09 | 一汽奔腾轿车有限公司 | Method for analyzing VOC (volatile organic compound) component of plastic particle by using thermal desorption gas chromatography-mass spectrometer |
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