CN109521127B - Qualitative and quantitative analysis method for evaluating odor of single odor substance - Google Patents
Qualitative and quantitative analysis method for evaluating odor of single odor substance Download PDFInfo
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- CN109521127B CN109521127B CN201811593232.7A CN201811593232A CN109521127B CN 109521127 B CN109521127 B CN 109521127B CN 201811593232 A CN201811593232 A CN 201811593232A CN 109521127 B CN109521127 B CN 109521127B
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
Abstract
The invention discloses a qualitative and quantitative analysis method for evaluating odor of a single odor substance, which comprises the following steps: s1, determining a sniffing threshold: determining the olfactory threshold value of a single odorant by a bag method; s2, GCO analysis: collecting gases of S1 bags with different strengths, separating the materials by gas chromatography, dividing the separated gases into two paths, acquiring a material concentration-time spectrogram of one path by a mass spectrometer, manually distinguishing odor intensity of the other path by an odor distinguishing instrument, and recording the odor intensity-time spectrogram to obtain the relationship between the odor intensity and the odor concentration; and S3, matching the odor intensity recorded by the odor identification instrument with the intensity recorded by a bag method, and correcting the relationship between the odor intensity and the intensity recorded by the bag method on the basis of the intensity recorded by the bag method, so that the corresponding relationship between the odor intensity and the odor concentration is directly obtained through GCO, and the odor type and the odor intensity of a single odor substance are evaluated. The method can be used for quantitatively analyzing the relation between the odor intensity and the odor concentration of a single odor substance. Through the method, the source tracing of the odor can be carried out, and the quantification and the control of the odor substance can also be carried out.
Description
Technical Field
The invention belongs to the technical field of odor evaluation, and particularly relates to a qualitative and quantitative analysis method for performing odor evaluation on a single odor substance.
Background
Due to the demands for weight reduction and energy saving of automobiles, the application of polymer materials in automotive interior parts is becoming more and more extensive. Research shows that main parts in a vehicle, such as an instrument panel, a sub-instrument panel assembly, a seat assembly and the like, and other leather or plastic ornaments, can release organic volatile substances (VOC) such as formaldehyde, benzene, toluene, xylene and the like in the using process. These VOCs are primarily a result of the use of many small molecules of solvents and adjuvants in the production and processing of polymeric materials and the degradation or aging of the materials during use. Because the automobile has good sealing performance, narrow internal space and limited air flow, the harm to human bodies caused by the excessive VOC in the automobile is larger. Odor perception is the most intuitive psychological perception of the human body, and more people begin to pay attention to odor research and continuously develop low-VOC and low-odor materials.
At present, the odor evaluation of automotive upholsteries at home and abroad is mainly based on various sensory evaluation methods, namely a three-point odor bag comparison method, a part bag method and a bottle method. Subjective evaluation of odor by a specialized odor evaluator is a form of odor evaluation that is mainly recognized at the present stage. The source of the odor is many and different materials and processes result in different final odors. The daily smelling smell is the integration of a plurality of smell substances, and the subjective evaluation method cannot carry out qualitative and quantitative analysis on a single smell substance. Patent CN201710994372.4 discloses a man-machine combined method for evaluating odor sources in an automobile, which can qualitatively determine a single odor substance by using a gas chromatography-mass spectrometry combined method and olfaction detection (GC-MS/O), and can screen the sources of the odor in the air in the automobile by using the method, but only uses a GCO method to screen the odor substances in the air in the automobile, and does not combine a subjective odor evaluation method of a human body and does not quantitatively analyze the relationship between the odor concentration and the odor intensity of the single odor substance. Due to the difference of the sniffing modes, the evaluation results of human body by sniffing instrument do not conform to the results of bottle method, bag method, etc. The results obtained based solely on GCO are not consistent with the results of odor evaluations used on a daily basis. Moreover, the research only simply qualitatively identifies the single odor substance, further research is needed on how the single odor substance affects the subjective evaluation of people, and further analysis and discussion are needed on how to establish the quantitative relation between the odor intensity and the odor concentration of the single odor substance.
Disclosure of Invention
The invention aims to solve the technical problem that the existing GCO method does not combine with a subjective odor evaluation method of a human body and cannot carry out quantitative analysis on the relationship between the odor concentration and the odor intensity of a single odor substance; the method for evaluating the odor of the single odor substance is provided by combining the GCO technology with the human subjective evaluation method, and the quantitative relation between the odor concentration and the odor intensity of the single odor substance is established, so that the odor substance is better quantified and controlled.
The invention aims to provide a qualitative and quantitative analysis method for evaluating the odor of a single odor substance.
The above object of the present invention is achieved by the following technical solutions:
a qualitative and quantitative analysis method for evaluating the odor of a single odor substance comprises the following steps:
s1, determining a sniffing threshold: determining the olfactory threshold value of a single odorant by a bag method;
s2, GCO analysis: collecting gases of S1 bags with different intensities, separating the materials by gas chromatography, dividing the separated gases into two paths, acquiring a material concentration-time spectrogram by a mass spectrometer on one path, manually distinguishing odor intensity by an odor distinguishing instrument on the other path, and recording the odor intensity-time spectrogram to obtain the relationship between the odor intensity and the odor concentration recorded by the odor distinguishing instrument;
and S3, matching the odor intensity recorded by the sniffing instrument with the intensity recorded by a bag method, and correcting the relationship between the odor intensity and the intensity recorded by the bag method on the basis of the intensity recorded by the bag method, so that the corresponding relationship between the odor intensity recorded by the bag method and the odor concentration is directly obtained through GCO, and the odor type and the odor intensity of a single odor substance are evaluated.
The invention combines the GCO technology with the subjective evaluation of human body to establish a qualitative and quantitative analysis method for evaluating the odor of a single odor substance, and solves the problem that the GCO method cannot be applied to daily odor evaluation results due to different odor modes and different standards. The invention firstly determines the olfactory threshold value of a single odor substance by using the traditional bag method and other methods; then testing the gas with different strength odor threshold values (odor strength) through GCO to obtain the relationship between the odor strength and the odor concentration under the GCO testing method; finally, the relation between the strength of the single gas substance and the strength of the single gas substance is corrected on the basis of the strength of the single gas substance measured by the traditional bag method and the like, so that the corresponding relation between the strength of the odor and the concentration of the odor can be directly obtained by the GCO method, and the type of the odor and the strength of the odor of the single odor substance can be evaluated.
Preferably, S1 is to dilute the substance concentration step by the triple point olfactory method, and the evaluator performs odor intensity and odor type evaluation on the odorants of different concentrations by subjective evaluation, thereby determining the human body' S threshold for single substance olfactory discrimination.
Preferably, the intensity of S2 is three intensities of perception (1.5-2), cognition (2.5-3) and discomfort (3.5-4).
Specifically, in the GCO test, a part of gas enters the GC-MS and another part of gas enters the sniffer according to a certain flow-dividing ratio, so that a certain difference exists between the concentration measured in the GCO and the actual concentration of the gas, and therefore the concentration of the substance in the GCO test needs to be corrected, and the corrected concentration is the outlet concentration of the sniffer.
The correction formula C is m/s 1000 wherein: c-exit concentration of the sniffer in mg/m3(ii) a m-actual content of substance in the adsorption tube, unit μ g; s-outlet flow of sniffer in mL.
Preferably, the single-odor substance is n-butanol, 2-butanone or acetophenone.
The invention also claims the application of any one of the qualitative and quantitative analysis methods for evaluating the odor of the single odor substance in the traceability, quantification and management of the odor substance.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a qualitative and quantitative analysis method for evaluating the odor of a single odor substance, which combines the GCO test of the single substance with the subjective evaluation of human body by a bag method and adopts the correction of the gas concentration of GCO to realize the quantitative analysis of the odor concentration of the single substance in the bag and determine the odor intensity of the substance in the bag. In addition, the problem that the source of the odor substance cannot be determined in the existing mixed gas can be solved, so that the source tracing and quantitative control of the odor substance are realized.
Drawings
FIG. 1 is a substance concentration-time spectrum and an odor intensity-time spectrum of a n-butanol GCO test; in fig. 1, curve 1 represents the concentration-time spectrum of the substance, and curve 2 represents the odor intensity-time spectrum.
FIG. 2 is a spectrum of the concentration of acetophenone in GCO test and the odor intensity, wherein the gas concentrations are 40ppm, 300ppm and 1000ppm respectively.
Detailed Description
The invention is further described with reference to the drawings and the following detailed description, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
Example 1
A qualitative and quantitative analysis method for evaluating the odor of a single odor substance comprises the following steps:
(1) bag method for determining threshold value of olfactory discrimination
For a certain single odor substance, the odor substance with known concentration is injected into the PVF bag, the substance concentration is diluted step by a three-point odor discrimination method, and the odor intensity and odor type of the odor substance with different concentration are evaluated by an evaluator through subjective evaluation, so that the odor discrimination threshold of a human body to the single substance is determined, the odor discrimination threshold can truly reflect the subjective feeling of people on the odor, and the odor discrimination threshold is also an important basis for odor control. The odor intensity was evaluated with reference to VDA 270 and the corresponding rating criteria are shown in table 1.
TABLE 1 evaluation criteria for odor intensity
| Odor intensity rating | Description of |
| 1 | Has no odor |
| 2 | Inconspicuous odor |
| 3 | Clearly distinguishable odor |
| 4 | Clearly perceptible interfering odor |
| 5 | Strong interfering odor |
| 6 | Intolerable odor |
The specific operation of the bag method for sniffing the threshold is as follows:
1) preparing: preparing a series of PVF bags which are numbered in sequence and injecting known high-concentration odor substance samples (with sharp concentration content for the first time) into any PVF bag;
2) and (3) inflating: accurately filling 50% high-purity nitrogen into the PVF bag filled with the standard;
3) heating: placing the PVF bag in a constant-temperature oven or a VOC test chamber with a set temperature, and balancing for 2 hours;
4) evaluation: after the odor bag is placed at room temperature, an evaluator needs to dilute the PVF bags filled with the high-concentration standard articles one by one according to a specified proportion until the evaluator cannot perceive the odor, the evaluator describes the odor type and the odor intensity, and three types of PVF bags with the odor discrimination thresholds of perception (1.5-2), cognition (2.5-3) and discomfort (3.5-4) are selected from the odor type and the odor intensity.
Taking n-butanol as an example, injecting n-butanol standard solution into the bag to make n-butanol gas concentration in the bag be 10mg/m3The odor intensity in the bag was evaluated by the sniffer; then, the concentration of the gas in the bag was diluted stepwise, and the odor intensity was evaluated in turn. The bag odor threshold of 2-butanone and acetophenone was studied according to the method, and the results of the relevant tests are shown in Table 2. The labeling concentration in the bags at the same odor intensity is significantly different for different substances due to the different olfactory thresholds.
TABLE 2 bag method labeling concentration vs. odor intensity relationship
(2) GCO analysis
And (3) carrying out data acquisition on a PVF bag with three intensities of perception (1.5-2), cognition (2.5-3) and discomfort (3.5-4) as an odor evaluation result, carrying out material separation on an acquired sample by using a Gas Chromatography (GC), dividing the separated gas into two paths, obtaining a material concentration-time spectrogram through a Mass Spectrometer (MS) on one path, manually smelling and distinguishing odor intensity through an olfactory recognizer on the other path, and recording the odor intensity-time spectrogram. At this time, the relationship between the odor intensity and the odor concentration recorded by the sniffer can be obtained.
FIG. 1 is a substance concentration-time spectrogram and an odor intensity-time spectrogram of a n-butanol GCO test, and the substance concentration and odor intensity spectrograms can be obtained by overlapping the concentration-time spectrogram and the odor intensity-time spectrogram.
FIG. 2 is a spectrum of the concentration of acetophenone in GCO test and the odor intensity, with gas concentrations of 40ppm, 300ppm and 1000ppm, respectively. As can be seen from fig. 2, as the concentration of the substance increases, the intensity of the odor increases.
(3) Comparison of results of GCO analysis and subjective evaluation
The odor types obtained by the two methods are the same, and in order to match the odor intensity recorded by the sniffing instrument with the intensity recorded by the bag method, the relationship between the odor intensity recorded by the bag method and the intensity recorded by the bag method is taken as the basis, so that the corresponding relationship between the odor intensity (the intensity recorded by the bag method) and the odor concentration can be directly obtained through GCO, and the odor type and the odor intensity of a single odor substance can be evaluated.
In the GCO test, a part of gas enters the GC-MS and the other part of gas enters the olfactory analyzer according to a certain flow-dividing ratio, so that the concentration measured in the GCO is different from the actual concentration of the gas to a certain extent, the concentration of a substance in the GCO test needs to be corrected, and the corrected concentration is the outlet concentration of the olfactory analyzer.
And (3) correcting the formula: c1000 m/s
Wherein: c-exit concentration of the sniffer in mg/m3；
m-actual content of substance in the adsorption tube, unit μ g;
s-outlet flow of sniffer in mL.
The labeling concentration of n-butanol, 2-butanone and acetophenone in the bag method and the outlet concentration of the modified sniffer for different odor intensities are summarized in table 3, and it can be seen that the odor intensities are evaluated by the bag method and GCO, and when the odor intensities are the same, the labeling concentration of the bag method and the outlet concentration of the modified sniffer are approximately 10 times of each other, and of course, the multiple relationship needs to be further studied for different substances.
TABLE 3 relationship between the concentration at the outlet of the sniffer and the concentration of the label in the bag method for the same odor intensity
According to the research, the single substance GCO test is combined with the subjective evaluation of human body by a bag method, and the correction of the GCO gas concentration is adopted, so that the quantitative analysis of the odor concentration of the single substance in the bag can be realized, and the odor intensity of the substance in the bag can be determined. In addition, the problem that the source of the odor substance cannot be determined in the existing mixed gas can be solved, so that the source tracing and quantitative control of the odor substance are realized.
Claims (5)
1. A qualitative and quantitative analysis method for evaluating the odor of a single odor substance is characterized by comprising the following steps:
s1, determining a sniffing threshold: determining the olfactory threshold value of a single odorant by a bag method;
s2, GCO analysis: collecting gases of S1 bags with different intensities, separating the materials by gas chromatography, dividing the separated gases into two paths, acquiring a material concentration-time spectrogram by a mass spectrometer on one path, manually distinguishing odor intensity by an odor distinguishing instrument on the other path, and recording the odor intensity-time spectrogram to obtain the relationship between the odor intensity and the odor concentration recorded by the odor distinguishing instrument;
s3, matching the odor intensity recorded by the odor identification instrument with the intensity recorded by a bag method, and correcting the relationship between the odor intensity and the intensity recorded by the bag method on the basis of the intensity recorded by the bag method, so that the corresponding relationship between the odor intensity recorded by the bag method and the odor concentration is directly obtained through GCO (general packet access), and the odor type and the odor intensity of a single odor substance are evaluated; the odor concentration of the GCO test was modified by C = m/s 1000 by the following formula: c-exit concentration of the sniffer in mg/m 3; m-actual content of substance in the adsorption tube, unit μ g; s-outlet flow of sniffer in mL.
2. The method of claim 1, wherein the step S1 is that the substance concentration is diluted step by a three-point olfactive method, and the odor intensity and the odor type of the odor substance with different concentrations are evaluated subjectively by an evaluator, so that the human body' S threshold for single substance olfaction is determined.
3. The method according to claim 1, wherein the intensity of S2 is three intensities of perception 1.5-2, cognition 2.5-3, and discomfort 3.5-4.
4. The method according to claim 1, characterized in that the single odorant is n-butanol, 2-butanone or acetophenone.
5. Use of the method according to any one of claims 1 to 4 for the traceability and/or quantification and control of odorants.
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| CN110658305A (en) * | 2019-09-12 | 2020-01-07 | 中汽研汽车检验中心（天津）有限公司 | Method for positively designing grade of odor substance in vehicle |
| CN111397996B (en) * | 2020-06-08 | 2020-10-13 | 中汽研汽车零部件检验中心(宁波)有限公司 | Odor standard gas preparation method based on odor intensity concentration relation |
| CN111812239A (en) * | 2020-07-10 | 2020-10-23 | 广电计量检测（天津）有限公司 | Method for determining key odor substances in shoes |
| CN114441650B (en) * | 2020-10-30 | 2023-06-06 | 海宁森德皮革有限公司 | Genuine leather smell tracing analysis and control method |
| CN113125509A (en) * | 2021-04-15 | 2021-07-16 | 浙江大学 | Human body odor detection and masking effect evaluation method based on biological mixing system |
| CN114264770A (en) * | 2021-08-23 | 2022-04-01 | 中汽研汽车检验中心（天津）有限公司 | Odor evaluation method based on map matching |
| CN113984960A (en) * | 2021-09-24 | 2022-01-28 | 中汽研汽车检验中心（天津）有限公司 | Method for researching odor characteristics of multi-component gas in dynamic mixing mode |
| CN114487223A (en) * | 2022-01-19 | 2022-05-13 | 青岛科大新橡塑检测服务有限公司 | Method for measuring VOC content in EPS foam |
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