KR20140137626A - Identification of odor-causing components occurred from odor sources - Google Patents

Abstract

The present invention relates to a method for identifying an odor-causing component from an odor source and, more specifically, to a method for identifying an odor-causing component from an odor source comprising a sample collecting step which collects odor substances occurred from an odor source in a plastic bag; a sensory test step which checks kinds of odor substances using an organic functions test; an instrumental analysis step which checks detected elements by different kinds of odor substances through the instrumental analysis; and an odor threshold assessment step which checks the odor threshold value for the detected elements; and a reproducibility evaluation step which produces sample gas for the sensory test, which is identical with concentration checked in the sample, from matters selected as the odor substances, and evaluates odor identities through a comparative sensory test with the produced gas.

Description

Identification of Odor-causing Causes for Odor Generation Sources {Identification of odor-causing components from odor sources}

The present invention relates to an odor evaluation method for more accurately and easily discriminating an odor causing component that affects the actual odor of components generated from an odor generating source.

Smells have unpleasant smells such as incense and smell like sewer. These unpleasant smells are generally called stinks. In Korea 's Anti - Odor Law, odor is defined as the smell of hydrogen sulfide, mercaptans, amines, and other irritating gaseous substances acting on the human' s smell, giving it discomfort and disgust.

Odorous substances are a kind of air pollutants and they are similar to volatile organic compounds (VOCs) and tend to be treated similarly, but the biggest difference is that odor causes discomfort.

At present, the designated odor substances according to the Korean Society of Odor Control Law are total 22 kinds, namely, ammonia, methyl mercaptan, hydrogen sulfide, dimethyl sulfide, dimethyl disulfide, trimethylamine, acetaldehyde, styrene, propionaldehyde, , n-valeric aldehyde, i-valeraldehyde, toluene, xylene, methyl ethyl ketone, methyl isobutyrate ketone, butylacetate, propionic acid, n-butyric acid, n- It is managed by le alcohol.

On the other hand, odorous substances are sensory pollutants that cause mental and physiological stress that is not visually identifiable and dependent on human olfactory sense. Odorogenic sources are also very diverse and are mostly caused by the complex nature of several compounds rather than a single substance. It is also a pollutant that is very difficult to objectively measure and evaluate because it is influenced by various factors such as weather conditions and human senses. Therefore, it is necessary to objectively measure and evaluate the odorous substances generated from the odor source through the reproducibility of odor substances generated from the odor source.

Accordingly, it is an object of the present invention to provide an evaluation method for more accurately and easily discriminating causal elements that have a direct and direct effect on each odor generation source, and it is an object of the present invention to provide an evaluation method for odor reduction by accurately identifying what constitutes an odor- To improve environmental pollution and product quality.

In order to achieve the above object, the present invention provides a sensory evaluation method, comprising: a sensory evaluation step of identifying a kind of odorous substance using a direct sensory method; A gas sample preprocessing step of collecting the gas generated from the odor generating source into a plastic bag and then adsorbing and absorbing the odor type or adsorbing and absorbing the gas generated from the odor source directly according to the type of odor; A device analyzing step of confirming the detected components by analyzing the devices according to the types of odorous substances; A minimum sensing method evaluation step of confirming a minimum sensing value for the detected component; A smell reproducibility evaluation step of preparing a standard gas which is the same as the concentration determined in the sample only for the substance selected as the smell substance and judging whether or not the standard gas is identical to the smell through the comparative sensory evaluation with the sample gas Provides an evaluation method for the odor causing agent selection process.

The vinyl bag may be a vinyl bag made of polyester.

Wherein the sensory evaluation includes a judge selecting step; A circle sample evaluation step; An odorless air production step; A sample gas production step; Sample sensory evaluation stage; And a result calculating step.

The equipment used for the above equipment analysis can be temperature controlled by a gas chromatograph and temperature of the oven can be adjusted by adjusting the flow rate of the pipe.

The minimum sensing method evaluation is a primary gas manufacturing step in which a reagent of a single substance is injected into a glass bottle for gas production and vaporized to a component detected through a device analysis; Preparing a sample for sensory evaluation in which a predetermined amount of the primary gas is injected and diluted only in one of a plurality of bags containing odorless gas; A sample sensory evaluation step in which a plurality of judges smell to evaluate the lowest sensed concentration until the highest result is obtained; And a minimum sensing value confirming step of confirming a result of the determination source having the lowest detection concentration and excluding the highest determination source. If the reagent of the detection component is a gaseous component, a sample for sensory evaluation can be prepared by omitting the primary gas production step and immediately diluting it in a bag containing an odorless gas.

The odor reproducibility evaluation step includes a quantitative analysis for each detected component using instrumental analysis and a cause tracking step for tracking the cause of odor generation by confirming the minimum sensed value; A sensory fluid manufacturing step of identifying the cause of the actual odor generation and producing a sensory fluid using the concentration of each sensing component; A sample gas production step of producing a sample gas in a range of the predetermined amount of the sensory solution in a range similar to the concentration generated in the cause of odor generation; And a step of identifying the causative component of the odor causing physical odor causing component by comparing the cause of the actual odor with the produced sample gas sensually.

According to the present invention, there is provided a method for identifying a causative element causing odor in an odor generating source, comprising the steps of establishing an odor reduction method according to the type of odor generated in the odor generating source, Thereby improving the product efficiency, thereby preventing environmental pollution.

Figure 1 shows the sensory evaluation step,
FIG. 2 shows a minimum sensing method evaluation step,
3 shows the reproducibility evaluation step.

Hereinafter, the odor reproducibility evaluation method according to the present invention will be described in detail with reference to the detailed process.

1. Sampling step

To pick up the odor origins and ingredients from the raw materials, use a plastic bag made of polyester with no odor or VOC. The bag that can be used for the evaluation should have very little reaction with various odor components. The sample collecting bag used in the present invention has a thickness of only 38 microns but does not tear easily and does not deteriorate when the sample is not a strong acid or a strong base. Further, various gases constituting the odor, organic solvent vapor, nitrogen, oxygen , Carbon dioxide, and the like.

2. Sensory Evaluation Step

The overall process is shown in FIG. 1, which is a method applied to measure odor intensity and odor quality, in which a gaseous substance stimulates the nose of a person to give offensive and repulsive effects. Although there is an advantage that it can be evaluated in a short time compared with the instrumental analysis method, the sensitivity of the result to the same sample may be large because the sensitivity is different depending on the type of odor of each odorant participating in the odor test, have.

3. Instrument Analysis Phase

The selection of the evaluation items is based on the 22 designated odor substances regulated by Korea's Anti-Odor Control Act, and identifies the detected components of ammonia, amines, sulfur compounds, aldehydes, volatile organic compounds, and lower fatty acids. The evaluation methods for each component are shown in Table 1 below.

Analytical component Sampling Pretreatment Detector ammonia Plastic bag Boric acid absorption method UV / VIS Amines Sulfuric acid absorption method MSD Sulfur compounds Low temperature enrichment FPD Aldehydes After DNPH cartridge reaction, acetonitrile solvent extraction HPLC Volatile organic compounds Low temperature enrichment MSD Lower fatty acids Alkali absorption method MSD

1) Ammonia

Ammonia analysis was performed by adding 5 ml of phenol-pentacyano nitrosyl iron (III) sodium salt solution and 5 ml of sodium hypochlorite solution to the sample solution for analysis, allowing to stand in a water bath at 25 to 30 ° C for 1 hour and then reacting with ammonium ion The absorbance of the resulting indanthrene phenols is measured and blue color is developed using the indophenol method, which is a method of quantifying ammonia, and then analyzed at a wavelength of 640 nm using UV / vis (CARY-50, USA). A UV / vis spectrophotometer is used for ammonia analysis.

2) Trimethylamine

Trimethylamine analysis was performed by adding 5 ml of 50% KOH to the vial containing the sample solution for analysis. After 5 minutes of stirring using the SPME auto sampler (MH01-00B) as a pretreatment device, trimethylamine was eluted into the upper layer of the vial, After adsorption (15 min), it is analyzed by gas chromatography (GC / MSD). GC / MSD is used for the trimethylamine analysis.

3) Sulfur compounds

Sulfur compounds are measured using a vacuum suction box (Model 1062, Film Science) and a Tedlar bag (5 L, 10 L, JAPAN) with built-in pump. The Tedlar bag used in the measurement of sulfur compounds was washed with high purity nitrogen (99.999%) three or more times before the measurement. Fill the sample bag with at least one sample, exhaust the sample, and collect the sample. After collection of samples, bags should be kept at room temperature (15 ~ 25 ℃) and kept away from direct sunlight. Analysis should be done within 24 hours.

Analyze with a GC (CP3800, Varian, U.S.A) equipped with a selective flame photometric detector (PFPD) for sulfur compounds. GC / PFPD is used for the analysis of sulfur compounds.

4) Aldehyde

The aldehydes are 2,4-DNPH derivatives that react with carbonyl compounds and 2,4-DNPH (Dinitrophenylhydrazine) to produce DNPH derivatives, which react with not only aldehydes but also ketones to form stable derivatives. .

Through derivatization of the carbonyl compound with 2,4-DNPH, the carbonyl compound is converted to a stable 2,4-DNPH hydrazone derivative form and H ₂ O is produced as a by-product. The 2,4-DNPH cartridge coated with 2,4-DNPH purified in a high-purity polypropylene tube and the 2,4-DNPH cartridge to remove ozone, which acts as an obstacle in the measurement of aldehydes, Use an ozone scrubber filled with KI at the front end.

After the measurement is completed, the sample is individually packaged in a container coated with aluminum. The sample is refrigerated at 4 ° C or lower before solvent extraction. Extract at very slow rate (1 ml / min) using 2.5 ml of acetonitrile. For analysis of aldehydes, liquid chromatography (HPLC) is used.

5) Volatile Organic Compounds (VOCs)

Toluene, xylene, methyl ethyl ketone (MEK), methyl isobutyrate ketone (MIBK), butylacetate (Butyl acetate), which are managed as odor substances in volatile organic compounds, , And isobutyl alcohol (i-butyl alcohol) are measured using a Tenax-TA adsorption tube (Supelco, USA) filled with 200 mg or more of Tenax-TA adsorbent.

The Tenax-TA adsorption tubes are stored at 4 ° C or lower and analyzed by GC / MSMS (3800 GC / 1200 L, Varian, U.S.A). GC / MS is used for VOCs analysis.

6) Organic acid

For the analysis of organic acids, 2.3 g of NaCl was added to the vial containing analytical sample solution, and 1 ml of 2% sulfuric acid was added. After thorough mixing, the mixture was stirred (90 ° C., 20 minutes) using SPME auto sampler (MH01-00B) When the organic acid is eluted into the upper layer of the gas layer, it is adsorbed by SPME (15 minutes) and analyzed by gas chromatography (GC / MSD). GC / MSD is used for organic acid analysis.

4. Minimum Sensing Method Evaluation Step

By analyzing the equipment, the emission discrimination component is evaluated, and the component that directly affects the actual odor is selected by confirming the minimum sensed value that can be sensed by the judge for these components. At this time, the overall process is shown in FIG.

5. Reproducibility Evaluation Step

The odor reproducibility evaluation method as shown in Fig. 3 is applied in order to ensure the reliability of whether the selected components are true odor substances. That is, a standard gas is prepared at a concentration equal to the concentration detected in the sample, and the odor is compared with the sample odor to evaluate whether or not the odor types are similar. Thus, only the actual odor inducing components among the components detected in the device analysis are presented.

Finally, based on these results, it can be used as the basic data for securing the most effective smell reducing method.

While the present invention has been described in connection with certain exemplary embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, It is to be understood that various changes and modifications may be made without departing from the scope of the appended claims.

Claims (5)

A sample collecting step of collecting the odor substance generated in the odor generating source in a plastic bag; A sensory evaluation step of confirming the type of odorous substance using a direct sensory method; A device analyzing step of confirming the detected components by analyzing the devices according to the types of odorous substances; A minimum sensing method evaluation step of confirming a minimum sensing value for the detected component; And a reproducibility evaluation step of preparing a standard gas whose concentration is the same as the concentration determined in the sample for only the substance selected as the odor substance and evaluating the odor identity through comparative sensory evaluation of the standard gas with the sample How to Identify the Causing Components of Odor. The method according to claim 1, wherein the vinyl bag is a vinyl bag made of polyester. The method according to claim 1, wherein the sensory evaluation comprises: a judge selecting step; A circle sample evaluation step; An odorless air production step; A sample gas production step; Sample sensory evaluation stage; And a result calculating step of calculating the odor causing component of the odor generating source. The apparatus according to claim 1, wherein the apparatus used for analyzing the apparatus is a gas chromatograph capable of raising the temperature of the separator tube oven, and can be adjusted by adjusting the flow rate of the separator tube. Method of identification. [2] The method of claim 1, wherein the minimum sensing method comprises: a first high concentration gas producing step of injecting a standard solution into a standard sample bottle and vaporizing the same to produce a primary gas; A step of preparing a sample gas for sensory evaluation in which the primary high concentration gas is injected and diluted in a certain amount only in one of a plurality of bags containing odorless gas; A sample sensory evaluation step in which a plurality of judges smell to evaluate the lowest sensed concentration until the highest result is obtained; And a minimum sensed value confirming step of confirming the result of the judgment on the other judgment sources except for the highest judgment source, which has the lowest detection concentration, and identifying the cause component of the odor causing substance to the odor generating source.

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