CN113777098A - Method for rapidly determining content of methanol in white spirit - Google Patents
Method for rapidly determining content of methanol in white spirit Download PDFInfo
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- CN113777098A CN113777098A CN202010218604.9A CN202010218604A CN113777098A CN 113777098 A CN113777098 A CN 113777098A CN 202010218604 A CN202010218604 A CN 202010218604A CN 113777098 A CN113777098 A CN 113777098A
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 238000000034 method Methods 0.000 title claims abstract description 22
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 45
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001514 detection method Methods 0.000 claims abstract description 19
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 11
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 9
- 239000011591 potassium Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 24
- 238000002835 absorbance Methods 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 239000012086 standard solution Substances 0.000 claims description 13
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 9
- 239000003153 chemical reaction reagent Substances 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 20
- 239000003638 chemical reducing agent Substances 0.000 description 9
- 239000000203 mixture Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 239000012286 potassium permanganate Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000007800 oxidant agent Substances 0.000 description 4
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 4
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 3
- 239000005695 Ammonium acetate Substances 0.000 description 3
- 229940043376 ammonium acetate Drugs 0.000 description 3
- 235000019257 ammonium acetate Nutrition 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000002203 pretreatment Methods 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 235000010288 sodium nitrite Nutrition 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- PYXRGWMIKFWVEE-UHFFFAOYSA-M N(=O)[O-].[Na+].C(C(=O)O)(=O)O Chemical compound N(=O)[O-].[Na+].C(C(=O)O)(=O)O PYXRGWMIKFWVEE-UHFFFAOYSA-M 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 239000012445 acidic reagent Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000035622 drinking Effects 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N2021/775—Indicator and selective membrane
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Abstract
The invention provides a method for rapidly determining methanol content in white spirit, which comprises the steps of adding potassium permanganate-phosphoric acid solution into a white spirit sample, adding acetylacetone color developing solution, adding oxalic acid after reaction, placing the treated sample in a cuvette, and determining by using a spectrophotometer. The detection method provided by the invention is used for detecting the content of methanol in the liquor sample, is quick, simple and easy to operate, and has high sensitivity for detecting the methanol in the liquor, and good repeatability data such as accuracy and precision.
Description
Technical Field
The invention relates to a method for rapidly determining the content of methanol in white spirit, belonging to the field of analysis and detection.
Background
China is the country with the largest consumption of white spirit in the world. The quality of the white spirit is related to the life and health of consumers, particularly, the content of methanol in the white spirit is extremely high, 5g of methanol is extremely toxic to human bodies, and if the drinking amount exceeds 12.5g, the human bodies can die. Therefore, it is necessary to establish an effective method for analyzing and detecting methanol in white spirit.
At present, the method for detecting the methanol in the wine mainly comprises two methods: gas chromatography and colorimetry. The gas chromatography has high detection accuracy, but has the defects of long detection time, high requirement on the professional performance of operators, high detection cost and the like. The method is characterized in that methanol is oxidized into formaldehyde by potassium permanganate under the acidic condition of phosphoric acid, then a colorless fuchsin-sulfurous acid reagent is added to react with the formaldehyde to generate a purple spread type pigment, and the content of the methanol in the white spirit is measured according to the shade of the color. The fuchsin-sulfurous acid solution adopts a grinding method, which has the problems of complicated operation, long time required, difficult complete dissolution during grinding, easy error of preparation concentration, and easy scald of operators due to frequent pouring of water with the temperature of 80 ℃ into a mortar in the operation process.
Disclosure of Invention
The invention aims to provide a method for rapidly determining the content of methanol in white spirit, which has the advantages of rapid and simple detection, high detection sensitivity, high accuracy and precision and suitability for detecting the content of methanol in a large batch of white spirit samples.
The invention discloses a method for rapidly determining the content of methanol in white spirit, which comprises the following steps:
1) preparation of standard solution: 0.5mL of methanol series standard solution 0, 0.05, 0.1, 0.2, 0.4 and 0.5mg/mL are taken, 0.5mL of potassium permanganate-phosphoric acid solution is added, 0.5mL of acetylacetone color developing solution is added, reaction is carried out for 10min at room temperature, 1mL of oxalic acid solution is added, color development is carried out for 10min in boiling water bath after uniform mixing, the mixture is taken out and cooled to the room temperature, deionized water is added to the room temperature to be 5mL, uniform mixing is carried out, and 0.5mL of uniform mixing solution is taken for detection.
2) And (3) zeroing with a blank reagent, namely 0.5mL of deionized water, placing 0.5mL of the uniformly mixed solution in a 1cm cuvette, measuring the absorbance value at the wavelength of 360-480 nm, and drawing a curve by taking the measured absorbance value as a vertical coordinate and the concentration of the methanol series standard solution as a horizontal coordinate.
3) And (3) replacing the formaldehyde standard solution in the step 1) with the liquor sample to be detected, detecting the absorbance value of the liquor sample to be detected in the same detection steps, comparing the absorbance value with the standard curve drawn in the step 2), and calculating the content of methanol in the liquor sample to be detected.
Preferably, the wavelength is 415nm as determined by a spectrophotometer.
Preferably, the standard curve equation is y 0.3672x +0.0025, y is methanol content, and x is the sample absorbance value.
Advantageous effects
The invention provides a method for rapidly determining methanol content in white spirit, which comprises the steps of adding potassium permanganate-phosphoric acid solution into a white spirit sample, adding acetylacetone color developing solution, adding oxalic acid after reaction, placing the treated sample in a 1cm cuvette, and determining by using a spectrophotometer. The method adopts acetylacetone as the color developing agent, the time required by the sample pretreatment method is short, the harm to operators is small, the whole detection process is rapid and easy to operate, the sensitivity of the detection method is high, and the repeatability data of the detection method, such as accuracy, precision and the like, are very good. The method can quickly, accurately and reliably measure the content of the methanol in the white spirit.
Drawings
FIG. 1 is a standard curve of the present invention;
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention illustrated in the accompanying examples, but it is to be understood that the description is intended to illustrate further features and advantages of the invention, rather than to limit the scope of the claims, and that the reagents of the invention, unless otherwise specified, are analytical grade.
Example sample Pre-treatment
Instruments and consumables: a liquid transfer device: 5mL, 1 mL; glass test tube: 10 mL; deionized or purified water; a visible light spectrophotometer.
Potassium permanganate-phosphoric acid solution: weighing 10g of potassium permanganate, placing the potassium permanganate in a 500mL volumetric flask, adding a proper amount of deionized water to dissolve the potassium permanganate, then adding 40mL of phosphoric acid, and using the deionized water to fix the volume to 400 mL.
Acetylacetone color developing solution: weighing 55g of ammonium acetate, placing the ammonium acetate in a 500mL volumetric flask, adding a proper amount of deionized water to dissolve the ammonium acetate, then adding 50mL of glacial acetic acid and 4mL of acetylacetone, using deionized water to fix the volume to 500mL, and transferring the mixture into a brown bottle to store the mixture at the temperature of 2-8 ℃.
Oxalic acid solution: 50g of oxalic acid is weighed and placed in a 500mL volumetric flask, a proper amount of deionized water is added for dissolution, and the volume is adjusted to 500mL by using the deionized water.
Sample pretreatment:
transferring 0.5mL of a white spirit sample into a 10mL glass test tube, adding 0.5mL of potassium permanganate-phosphoric acid solution and 0.5mL of acetylacetone color developing solution, uniformly mixing, reacting at room temperature for 10min, adding 1mL of oxalic acid solution, uniformly mixing, heating in a boiling water bath for 10min, taking out, cooling to room temperature, adding deionized water to 5mL, uniformly mixing, and detecting.
Selection of reactants and conditions for sample pretreatment according to the invention
1. The invention adopts potassium permanganate as an oxidant and oxalic acid as a reducing agent through multiple experiments, and the interference of the oxalic acid as the reducing agent on color development is obviously smaller than that of other reducing agents.
Under the condition of the same dosage of other test conditions, namely adding 0.5mL of potassium permanganate-phosphoric acid solution and 0.5mL of acetylacetone color developing solution, uniformly mixing, reacting at room temperature for 10min, taking deionized water as a reagent blank control, and respectively taking 1mL of sodium nitrite and oxalic acid as reducing agents to measure the absorbance value of the white spirit sample, which is shown in Table 1. The chromogenic interference of oxalic acid is significantly less than that of sodium nitrite, so oxalic acid was chosen as the reducing agent.
TABLE 1 Absorbance values determined for different reducing Agents
| Blank spaceControl | Sodium nitrite | Oxalic | |
| Absorbance value | |||
| 0 | 0.013 | 0.004 |
2. According to the invention, an oxidant and a color developing agent are simultaneously added into a sample to complete oxidation and absorption reactions, then a reducing agent is added to reduce redundant oxidants, and a standard curve is drawn according to the addition concentration and the absorbance value after multiple tests, so that a reagent sample addition scheme with good absorbance, small error and good linear coefficient is selected. Finally, the optimal sample adding scheme of 0.5mL of potassium permanganate-phosphoric acid solution, 0.5mL of acetylacetone color developing solution and 1mL of oxalic acid solution is selected. The results of the measurement of the amount of methanol added to 0, 0.05, 0.2, 0.4mg/mL of the samples of distilled spirit with different reagents are shown in Table 2.
TABLE 2 measurement results of different amounts of the oxidizing agent, the color-developing agent, and the reducing agent
3. The oxalic acid reducing agent is added, and then the reduction temperature is carried out for the maximum efficiency time, 120min, 45 ℃ (water bath) 90min, 80 ℃ (water bath) 30min and 100 ℃ (water bath) 10min at room temperature, so that the reaction time can be shortened to the maximum extent by adopting boiling water bath in the reduction process, and the reaction efficiency is improved. The maximum efficiency time of the oxidation reaction is hardly influenced by the room temperature, 45 ℃, 80 ℃ and 100 ℃, so the room temperature is directly selected from the energy-saving perspective for the oxidation reaction.
EXAMPLE two determination of methanol in white spirit
The method for measuring the methanol in the white spirit comprises the following steps:
respectively taking 0.5mL of methanol series standard solution to separate from 10mL of glassIn a core tube, the concentration of a methanol series standard solution is 0, 0.05, 0.1, 0.2, 0.4 and 0.5mg/mL, 0.5mL of a potassium permanganate-phosphoric acid solution is added, 0.5mL of an acetylacetone color developing solution is added, the reaction is carried out for 10min at room temperature, 1mL of an oxalic acid solution is added, the mixture is uniformly mixed and then is developed for 10min in a boiling water bath, the mixture is taken out and cooled to the room temperature by cold water, then deionized water is added to 5mL, and the mixture is uniformly mixed. A blank reagent, namely 0.5mL deionized water is used for zero setting, 0.5mL of the uniformly mixed solution is taken and placed in a 1cm cuvette, the absorbance value is measured at the wavelength of 415nm, the measured absorbance value is taken as the ordinate, the concentration of the methanol series standard solution is taken as the abscissa, a curve is drawn, and the standard curve equation is obtained: y is 0.3672x +0.0025, y is methanol content, x is sample absorbance value, r20.999, as shown in fig. 1.
EXAMPLE Effect of three wavelengths on the absorbance of the color reaction
The effect of different wavelengths on absorbance values was measured according to the method of example two, setting the wavelengths to 310nm, 345nm, 380nm, 415nm, 450nm, 485nm, showing the maximum absorbance value at the wavelength of 415 nm.
Examples of the experiments
Experiment of accuracy
By adopting the sample pretreatment method in the first embodiment and the methanol measurement method in the second embodiment, the blank samples of 42 ℃, 56 ℃ and 50 ℃ of Jiangjin in Niuban mountain are added with the methanol standard solution and then measured, and the results are shown in Table 3, and the sample detection accuracy range is 79-110%.
TABLE 3 sample detection accuracy experiment of the present invention
Precision experiment
The results of 7 times of measurement of the white spirit samples with methanol contents of 0.08 and 0.2mg/mL by the method are shown in Table 4, the standard deviation of the detection method is 2.0 percent and 4.6 percent respectively, and the detection method has better precision.
Table 4 precision verification of sample testing of the present invention
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention.
Claims (3)
1. A method for rapidly determining the content of methanol in white spirit comprises the following steps:
1) preparation of standard solution: taking 0.5mL of methanol series standard solution, 0.05 mL of potassium permanganate-phosphoric acid solution, 0.1 mL of acetylacetone color developing solution, 0.5mL of 0.5mg/mL of methanol series standard solution, reacting for 10min at room temperature, adding 1mL of oxalic acid solution, uniformly mixing, developing for 10min in a boiling water bath, taking out, cooling to room temperature, adding 5mL of deionized water, uniformly mixing, and taking 0.5mL of uniformly mixed solution for detection;
2) zeroing with a blank reagent, namely 0.5mL of deionized water, placing 0.5mL of the uniformly mixed solution in a 1cm cuvette, measuring an absorbance value at a wavelength of 360-480 nm, drawing a curve by taking the measured absorbance value as a vertical coordinate and the concentration of the methanol series standard solution as a horizontal coordinate, and obtaining a standard curve equation;
3) and (3) replacing the formaldehyde standard solution in the step 1) with the liquor sample to be detected, detecting the absorbance value of the liquor sample to be detected in the same detection steps, comparing the absorbance value with the standard curve drawn in the step 1), and calculating the content of methanol in the liquor sample to be detected.
2. The method for rapidly determining the content of methanol in white spirit according to claim 1, wherein the detection wavelength is set to 415 nm.
3. The method for rapidly determining the content of methanol in white spirit according to claim 2, wherein the standard curve equation is y =0.3672x +0.0025, y is the content of methanol, and x is the absorbance value of the sample.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050014213A1 (en) * | 2001-12-28 | 2005-01-20 | Kenji Nagakawa | Method of colorimetry and reagent for use therein |
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2020
- 2020-06-10 CN CN202010218604.9A patent/CN113777098A/en active Pending
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| US20050014213A1 (en) * | 2001-12-28 | 2005-01-20 | Kenji Nagakawa | Method of colorimetry and reagent for use therein |
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| CN103954619A (en) * | 2014-05-21 | 2014-07-30 | 江南大学 | Method for quickly quantifying cyanide in white spirit |
| TW201612503A (en) * | 2014-09-16 | 2016-04-01 | Taiwan Chuang Xing Co Ltd | Methanol inspection method and method for manufacturing methanol inspection dry reagent |
| CN105021600A (en) * | 2015-06-11 | 2015-11-04 | 上海理工大学 | Detection method for trace methanol in water |
| CN109342419A (en) * | 2018-12-07 | 2019-02-15 | 云南商测质量检验技术服务有限公司 | A kind of methanol in wine quick testing reagent and its application method |
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| Title |
|---|
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