Test method for evaluating smell of synthetic ester

Abstract

The invention belongs to the field of synthetic ester smell testing, and particularly relates to a testing method for evaluating synthetic ester smell. The same sample to be tested is divided into a plurality of identical samples, then gas passes through the samples in sequence, the volatilization speed of the volatile substances in the samples passing through the gas can be reduced or the volatile substances are enriched due to the fact that the volatile components of the samples passing through the gas in sequence are changed, and the volatile components of the samples passing through the gas in sequence are changed. Then, multiple testers are used for carrying out odor evaluation on the samples to determine qualified samples, and subsequent product odor evaluation can be compared according to qualified products to determine whether the products are qualified or not.

Description

Technical Field

[0001] This invention belongs to the field of synthetic ester odor testing, and specifically relates to a test method for evaluating the odor of synthetic esters. Background Technology

[0002] Isonononyl isononate (ININ) and other synthetic esters used in cosmetic raw materials require strict requirements on odor. If a product contains a large amount of odorous raw material acids, raw material alcohols or other byproducts, even if the product meets the purity requirements, it will still not meet the delivery requirements due to the presence of other odors.

[0003] Currently, odor testing of synthetic ester products still relies on the subjective judgment of quality inspectors. However, different people have different odor thresholds, which may lead to the risk of products with unacceptable odors being released.

[0004] To address this issue, it is particularly important to provide a test method for evaluating the odor of synthetic esters, which can reduce experimental errors caused by manual measurement and provide a stable assessment of product odor. Summary of the Invention

[0005] The present invention aims to at least solve one of the technical problems existing in the prior art. To this end, the present invention proposes a test method for evaluating the odor of synthetic esters; the apparatus and method can reduce experimental errors caused by manual measurement and can stably evaluate the odor of products.

[0006] The concept of this invention is as follows: the same product is divided into multiple identical samples, and then gas is passed through the samples sequentially. Since the gas will carry volatile substances after passing through the online samples, the evaporation rate of volatile substances in the samples that pass through the gas later will decrease or the volatile substances will be enriched, resulting in changes in the composition of the samples that pass through the gas successively. Then, multiple testers are used to evaluate the odor of the samples to determine the qualified samples. The odor evaluation of subsequent products can be compared with the qualified products (such as odor, liquid phase, gas phase) to determine whether the product is qualified.

[0007] The first aspect of the present invention provides a test method for evaluating the odor of synthetic esters.

[0008] Specifically, a test method for evaluating the odor of synthetic esters; The test method utilizes a test apparatus, which includes a sample bottle and an adsorption bottle. The sample bottle includes a first inlet pipe and a first outlet pipe, with the height of the end of the first inlet pipe inside the sample bottle lower than the height of the end of the first outlet pipe inside the sample bottle. The adsorption bottle includes a second inlet pipe and a second outlet pipe, with the height of the end of the second inlet pipe inside the sample bottle lower than the height of the end of the second outlet pipe inside the sample bottle. The first outlet pipe and the second inlet pipe are connected. The testing method includes the following steps: Step 1: The sample bottle and the adsorption bottle contain the same batch of test samples; Step 2: At 20-35℃, gas is introduced into the first inlet tube, and the odor assessment and chromatographic test are performed on the samples in the sample bottle and the adsorption bottle every 30-60 minutes; the odor assessment includes using multiple assessors to assess the odor of the samples and record the intensity level; Step 3: Statistically analyze the odor assessment data and determine the chromatographic test data corresponding to the passing standard.

[0009] Compared with the prior art, the beneficial effects of the test method for odor evaluation of synthetic esters provided by the first aspect are as follows: the gas first passes through the sample bottle and carries the volatile substances in the sample to be tested. When it passes through the adsorption bottle, less of the volatile substances in the sample volatilizes or more volatile substances are adsorbed. After a period of time, there will be a difference in the volatile substances in the two bottles. At this time, the odor evaluation of the samples in the two bottles is more accurate and can accurately find the passing standard.

[0010] Preferably, in the testing device, the adsorption bottles are a plurality of sequentially connected to each other, and the second exhaust pipe of each adsorption bottle is connected to the second air inlet pipe of the next adsorption bottle. By setting multiple adsorption bottles, after blowing air, the volatile substances in the samples in different adsorption bottles can show a gradient change, which is beneficial for evaluating the product odor and determining whether the product is qualified.

[0011] Preferably, in the testing device, the end of the second air inlet pipe is a cone with a gradually increasing diameter. The conical design of the second air inlet pipe is more conducive to the absorption of volatile substances in the gas by the sample in the adsorption bottle.

[0012] Preferably, in the testing device, the sample bottle further includes a magnetic stirrer, and the adsorption bottle further includes a magnetic stirrer.

[0013] Preferably, in the testing device, the sample bottle is further provided with a thermometer, and the adsorption bottle also includes a thermometer.

[0014] Preferably, in step 1, the volume of the sample to be tested contained in the sample bottle and the adsorption bottle is the same.

[0015] Preferably, in step 2, the temperature of the gas is 20-35°C. 2. -35°C helps prevent the synthetic ester from deteriorating.

[0016] Preferably, in step 2, the flow rate of the introduced gas is 1-10 cm³. 3 / s, the diameter of the first intake pipe is 2-10mm.

[0017] Preferably, in step 2, the gas introduction time is 2-48 hours.

[0018] Preferably, in step 2, the intensity level is one of three levels: no odor, slight odor, and odor.

[0019] Compared with the prior art, the beneficial effects of the present invention are as follows: The gas first passes through the sample bottle, carrying the volatile substances from the sample to be tested. When it passes through the adsorption bottle, less of the volatile substances in the sample volatilizes or more volatile substances are adsorbed. After a period of time, there will be a difference in the volatile substances in the two bottles. At this time, it is more accurate to evaluate the odor of the samples in the two bottles and to accurately find the passing standard. Attached Figure Description

[0020] Figure 1 This is a schematic diagram of the test apparatus in some embodiments; Figure 2 This is a schematic diagram of the testing apparatus in Example 1; Figure 3 The gas chromatogram of the sample to be tested in the sample vial after being blown with gas for 2.5 hours; Figure label: Sample bottle 100, first air inlet pipe 110, first exhaust pipe 120, magnetic stirrer 130, adsorption bottle 200, second air inlet pipe 210, second exhaust pipe 220. Detailed Implementation

[0021] To enable those skilled in the art to more clearly understand the technical solutions described in this invention, the following embodiments are provided for illustration. Examples of the embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. It should be noted that the following embodiments do not constitute a limitation on the scope of protection claimed by this invention.

[0022] like Figure 1 , Figure 1 This is a schematic diagram of the testing apparatus in some embodiments, and a testing method for evaluating the odor of synthetic esters; The test method uses a test apparatus, which includes a sample bottle 100 and an adsorption bottle 200. The sample bottle 100 includes a first inlet pipe 110 and a first outlet pipe 120. The height of the end of the first inlet pipe 110 inside the sample bottle 100 is lower than the height of the end of the first outlet pipe 120 inside the sample bottle 100. The adsorption bottle 200 includes a second inlet pipe 210 and a second outlet pipe 220. The height of the end of the second inlet pipe 210 inside the sample bottle 100 is lower than the height of the end of the second outlet pipe 220 inside the sample bottle 100. The first outlet pipe 120 and the second inlet pipe 210 are connected. The testing method includes the following steps: Step 1: The same sample to be tested is placed in sample bottle 100 and adsorption bottle 200; Step 2: At 20-35℃, gas is introduced into the first inlet tube 110, and the odor assessment and chromatographic test are performed on the samples in the sample bottle 100 and adsorption bottle 200 every 30 minutes. The odor assessment includes using multiple assessors to assess the odor of the samples and record the intensity level. Step 3: Compile the odor assessment data and determine the chromatographic test data corresponding to the passing standard.

[0023] Compared with the prior art, the beneficial effects of the test method for evaluating the odor of synthetic esters provided in this first aspect are as follows: the gas first passes through the sample bottle 100 and carries the volatile substances in the sample to be tested. When it passes through the adsorption bottle 200, less of the volatile substances in the sample volatilizes or more volatile substances are adsorbed. After a period of time, there will be a difference in the volatile substances in the two bottles. At this time, it is more accurate to evaluate the odor of the samples in the two bottles and can accurately find the passing standard.

[0024] Preferably, in the testing apparatus, there are multiple adsorption bottles 200 connected sequentially to each other, and the second exhaust pipe 220 of each adsorption bottle 200 is connected to the second air inlet pipe 210 of the next adsorption bottle 200. By setting multiple adsorption bottles 200, after blowing air, the volatile substances of the samples in different adsorption bottles 200 can show a gradient change, which is beneficial for evaluating the product odor and determining whether the product is qualified.

[0025] Preferably, in the testing apparatus, the end of the second inlet pipe 210 is a cone with a gradually increasing diameter. The conical design of the second inlet pipe 210 is more conducive to the absorption of volatile substances in the gas by the sample in the adsorption bottle 200.

[0026] Preferably, in the testing apparatus, the sample bottle 100 further includes a magnetic stirrer 130, and the adsorption bottle 200 further includes a magnetic stirrer 130.

[0027] Preferably, the sample bottle 100 in the testing device is also equipped with a thermometer, and the adsorption bottle 200 is also equipped with a thermometer.

[0028] Preferably, in step 2, the temperature of the gas is 20-35℃.

[0029] Preferably, in step 2, the flow rate of the introduced gas is 1-10 cm3 / s, and the diameter of the first air inlet pipe 110 is 2-10 mm.

[0030] Preferably, in step 2, the gas is introduced for 2-48 hours.

[0031] Preferably, in step 2, the strength level is divided into three levels: no odor, slight odor, and odor. Example 1

[0032] A test method for evaluating the odor of synthetic esters, the method using a test apparatus, such as... Figure 2 , Figure 2 This is a schematic diagram of the testing apparatus of Example 1. The testing apparatus includes a sample bottle 100 and an adsorption bottle 200. The sample bottle 100 includes a first inlet pipe 110 (3mm in diameter) and a first exhaust pipe 120. The height of the end of the first inlet pipe 110 inside the sample bottle 100 is lower than the height of the end of the first exhaust pipe 120 inside the sample bottle 100. The adsorption bottle 200 includes a second inlet pipe 210 and a second exhaust pipe 220. The height of the end of the second inlet pipe 210 inside the sample bottle 100 is lower than the height of the end of the second exhaust pipe 220 inside the sample bottle 100. The first exhaust pipe 120 is connected to the second inlet pipe 210. The end of the second inlet pipe 210 is a cone with a gradually increasing diameter. The sample bottle 100 also includes a magnetic stirrer 130. The samples to be tested are isononyl isononanoate (ININ) produced in the same batch. The test method includes the following steps: Step 1: The same 50mL sample to be tested is placed in sample bottle 100 and adsorption bottle 200. The magnetic stirrer 130 in sample bottle 100 rotates at 3r / s. Step 2: At 30°C, inject 2cm of air into the first intake pipe 110. 3 Air at 30°C was introduced at a rate of / s for 3 hours. Odor assessment and gas chromatography tests were performed on the samples in sample bottle 100 and adsorption bottle 200 every 30 minutes. The odor assessment included 5 evaluators assessing the odor of the samples and recording the intensity level. Step 3: Compile the odor assessment data in Table 1 and determine the chromatographic test data corresponding to the passing standard.

[0033] No odor is scored as 0 points, slight odor as 1 point, and odor as 2 points. The sum of the scores given by the five evaluators is recorded as the odor evaluation score.

[0034] Table 1. Odor assessment scores.

[0035] Sample bottle odor assessment score Odor assessment score of adsorption bottle 0h 7 7 0.5h 6 8 1h 4 6 1.5h 2 5 2h 1 5 2.5h 0 4 3h 0 3 This testing method allows for the simultaneous comparison of test samples with different odors, eliminating the need for evaluators to rely on odor memory for assessment. It accurately determines whether a test sample is an odorless, qualified product, thereby precisely identifying the corresponding liquid chromatography data for the qualification standard. Clearly, in this method, blowing air for 2.5 hours is sufficient to reduce the product's odor, thus making it a qualified product.

[0036] Figure 3 The image shows the gas chromatogram of the sample in the sample vial after purging for 2.5 h. The relative peak area of ​​isononyl isononanoate (ININ) with a retention time of 7.385 min is 99.96%.

Claims

1. A test method for evaluating the odor of synthetic esters, characterized in that, The test method uses a test device, which includes a sample bottle and an adsorption bottle. The sample bottle includes a first inlet pipe and a first outlet pipe, and the height of the end of the first inlet pipe inside the sample bottle is lower than the height of the end of the first outlet pipe inside the sample bottle. The adsorption bottle includes a second inlet pipe and a second outlet pipe, and the height of the end of the second inlet pipe inside the sample bottle is lower than the height of the end of the second outlet pipe inside the sample bottle. The first exhaust pipe is connected to the second intake pipe; The testing method includes the following steps: Step 1: The sample bottle and the adsorption bottle contain the same batch of test samples; Step 2: At 20-35℃, gas is introduced into the first inlet tube, and the odor assessment and chromatographic test are performed on the samples in the sample bottle and the adsorption bottle every 30 minutes; the odor assessment includes using multiple assessors to assess the odor of the samples and record the intensity level; Step 3: Statistically analyze the odor assessment data and determine the chromatographic test data corresponding to the passing standard.

2. The test method according to claim 1, characterized in that, In the testing apparatus, a plurality of adsorption bottles are sequentially connected to each other, and the second exhaust pipe of each adsorption bottle is connected to the second air inlet pipe of the next adsorption bottle. By setting up multiple adsorption bottles, after blowing air, the volatile substances in the samples in different adsorption bottles can show a gradient change, which is beneficial for evaluating the product odor and determining whether the product is qualified.

3. The test method according to claim 1, characterized in that, In the testing apparatus, the end of the second inlet pipe is a cone with a gradually increasing diameter. The conical design of the second inlet pipe is more conducive to the absorption of volatile substances in the gas by the sample in the adsorption bottle.

4. The test method according to claim 1, characterized in that, The testing device further includes a magnetic stirrer in the sample bottle and a magnetic stirrer in the adsorption bottle.

5. The test method according to claim 1, characterized in that, In the testing device, a thermometer is also provided in the sample bottle, and a thermometer is also provided in the adsorption bottle.

6. The test method according to claim 1, characterized in that, In step 1, the sample to be tested contained in the sample bottle and the adsorption bottle have the same volume.

7. The test method according to claim 1, characterized in that, In step 2, the temperature of the gas is 20-35℃.

8. The test method according to claim 1, characterized in that, In step 2, the flow rate of the introduced gas is 1-10 cm³ / s, and the diameter of the first air inlet pipe is 2-10 mm.

9. The test method according to claim 1, characterized in that, In step 2, the gas is introduced for 2-48 hours.

10. The test method according to claim 1, characterized in that, In step 2, the intensity level is divided into three levels: no odor, slight odor, and odor.

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