CN103134863A - Method of determining content of methanol, isobutanol, isoamylol of alcohol - Google Patents
Method of determining content of methanol, isobutanol, isoamylol of alcohol Download PDFInfo
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- CN103134863A CN103134863A CN2011103855987A CN201110385598A CN103134863A CN 103134863 A CN103134863 A CN 103134863A CN 2011103855987 A CN2011103855987 A CN 2011103855987A CN 201110385598 A CN201110385598 A CN 201110385598A CN 103134863 A CN103134863 A CN 103134863A
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Abstract
测定酒精中甲醇、正丙醇、异丁醇、异戊醇含量的方法，涉及测定酒精的方法。依次包括以下步骤：（1）酒精样品前处理步骤：移取样品酒精于容量瓶中，再加入内标溶液，用无水乙醇稀释并定容至刻度，混匀，作为待测液；（2）空白实验：不加样品，重复（1）步骤；（3）对所得样品和空白样品进行气相色谱-质谱联用分析。本发明的有益效果是：本发明通过改进方法，更改检测器，实现了酒精中甲醇、正丙醇、异丁醇、异戊醇含量的精确定量分析。本发明的方法操作简单、快速准确。The invention discloses a method for measuring the content of methanol, n-propanol, isobutanol and isoamyl alcohol in alcohol, relating to a method for measuring alcohol. Include the following steps in turn: (1) Alcohol sample pretreatment step: pipette the sample alcohol into a volumetric flask, then add the internal standard solution, dilute with absolute ethanol and set the volume to the mark, mix well, and use it as the solution to be tested; (2 ) Blank experiment: repeat step (1) without adding samples; (3) Perform gas chromatography-mass spectrometry analysis on the obtained samples and blank samples. The beneficial effects of the present invention are: the present invention realizes the precise quantitative analysis of the content of methanol, n-propanol, isobutanol and isoamyl alcohol in alcohol by improving the method and changing the detector. The method of the invention is easy to operate, fast and accurate.
Description
Technical field
The present invention relates to measure the method for alcohol, be specifically related to a kind of method of measuring methyl alcohol in alcohol, n-propanol, isobutyl alcohol, isoamylol content.
Background technology
chemical composition in alcohol is varied and very complicated, methyl alcohol, n-propanol, isobutyl alcohol, isoamylol is the harmful composition in alcohol, its assay method mostly is vapor-phase chromatography at present, and all adopt the single-stage standard model to calculate calibration factor and carry out again quantitative method, this method requires solvent for use not contain any methyl alcohol, n-propanol, isobutyl alcohol, isoamylol, require high especially to solvent, if contain the methyl alcohol of trace in solvent, n-propanol, isobutyl alcohol, isoamylol, the sample that calculates and the amount of blank sample deviation all can occur and cause final quantitative result relatively large deviation to occur.In addition, owing to being that the single-stage standard model calculates calibration factor, cause final quantitative result relatively large deviation to occur thereby very easily cause calibration factor large deviation to occur.Also having vapor-phase chromatography detecting device used is fid detector, selects ion quantitatively to compare with the mass spectrum detecting device, is from the sensitivity that detects or from aspects such as lock onto target compounds, gap is arranged all.
Summary of the invention
The objective of the invention is for top described weak point of the prior art, a kind of method of methyl alcohol, n-propanol, isobutyl alcohol, isoamylol content in the mensuration alcohol that can realize accurate quantitative test is provided.
The objective of the invention is to be achieved by the following technical programs.
Measure the method for methyl alcohol, n-propanol, isobutyl alcohol, isoamylol content in alcohol, it is characterized in that, comprise the following steps successively: (1) alcohol sample pre-treatments step: pipette sample alcohol in volumetric flask, add again inner mark solution, dilute and be settled to scale with absolute ethyl alcohol, mixing is as liquid to be measured; (2) blank assay: do not add sample, repeat (1) step; (3) gained sample and blank sample are carried out the gas chromatography-mass spectrography analysis.
In described step (1), the volume ratio of inner mark solution and sample alcohol is 1: 2-3.
Described inner mark solution refers to that normal butyl alcohol content is the ethanol solution of 0.05mg/ml.
The scale of the volumetric flask in described step (1) is 10ml.
Gas phase condition when described step (3) is carried out the gas chromatography-mass spectrography analysis is: chromatographic column: HP-INNOWax, 60m(length) * the 0.25mm(internal diameter) * 0.25 μ m(thickness), temperature programme: 70 ℃, keep 5min; Rise to 100 ℃ with 5 ℃/min speed; Rise to 150 ℃ with 30 ℃/min again, keep 10min.
Described alcohol is the alcohol of producing as raw material with sugarcane, corn, potato class, molasses etc.
Described gas chromatography-mass spectrography analysis adopts the multistage standard model calculating calibration factor to carry out quantitatively; Detecting device is mass detector, adopts characteristic ion that target compound is measured, and has not only satisfied quantitative requirement but also can carry out qualitative to target compound.
The invention has the beneficial effects as follows: the present invention is by improving one's methods, and the change detecting device has been realized the accurate quantification analysis of methyl alcohol, n-propanol, isobutyl alcohol, isoamylol content in alcohol.Method of the present invention is simple to operate, quick and precisely.
Embodiment
The present invention is further described below with reference to embodiment, but does not limit the present invention.
Embodiment 1.
A, accurately pipette alcohol sample that 5ml produces as raw material with sugarcane, corn, potato class, molasses etc. in the 10ml volumetric flask, then add the 2ml inner mark solution, to scale, mixing is as liquid to be measured with absolute ethyl alcohol dilution and constant volume.
B, the gained sample is carried out GC-MS analyze.Analysis result such as following table:
| Raw material | Methyl alcohol | N-propanol | Isobutyl alcohol | Isoamylol |
| Cane kind 1 | 35.4 | 31.1 | Do not detect | Do not detect |
| Cane kind 2 | 42.9 | 46.5 | 2.0 | Do not detect |
| Cane kind 3 | 30.6 | 282.7 | 20.8 | Do not detect |
| Potato class 1 | 271.2 | 180.6 | 10.3 | Do not detect |
| Potato class 2 | 77.1 | 109.6 | 11.7 | Do not detect |
| Potato class 3 | 19.2 | 24.5 | Do not detect | Do not detect |
| Corn class 1 | 87.6 | 126.5 | 8.8 | 3.6 |
| Corn class 2 | 22.6 | 5.9 | Do not detect | Do not detect |
| Corn class 3 | 253.9 | 13.8 | Do not detect | Do not detect |
| Molasses class 1 | 25.3 | 168.5 | 3.5 | Do not detect |
| Molasses class 2 | 69.7 | 480.6 | 7.0 | Do not detect |
| Molasses class 3 | 92.2 | 604.5 | 30.0 | Do not detect |
| Wheat class 1 | 74.3 | 143.4 | Do not detect | Do not detect |
Embodiment 2.
A, accurately pipette alcohol sample that 5ml different industrial enterprises use in the 10ml volumetric flask, then add the 2ml inner mark solution, to scale, mixing is as liquid to be measured with absolute ethyl alcohol dilution and constant volume.
B, the gained sample is carried out GC-MS analyze.Analysis result such as following table:
| Use enterprise | Methyl alcohol | N-propanol | Isobutyl alcohol | Isoamylol |
| Enterprise 1 | 32.1 | 59.4 | Do not detect | Do not detect |
| Enterprise 2 | 22.6 | 5.9 | Do not detect | Do not detect |
| Enterprise 3 | 74.3 | 143.4 | Do not detect | Do not detect |
| Enterprise 4 | 130.2 | 75.6 | 31.2 | 41.5 |
| Enterprise 5 | 75.5 | 194.3 | Do not detect | Do not detect |
| Enterprise 6 | 272.7 | 243.3 | 28.0 | Do not detect |
| Enterprise 7 | 77.1 | 109.6 | 11.7 | Do not detect |
| Enterprise 8 | 243.3 | 12.7 | Do not detect | Do not detect |
| Enterprise 9 | 16514.8 | 191.2 | 36.9 | 46.5 |
| Enterprise 10 | 36.8 | 47.6 | Do not detect | Do not detect |
Embodiment 3.
A, accurately pipette alcohol sample that the different alcohol of 5ml manufacturing enterprise produces in the 10ml volumetric flask, then add the 2ml inner mark solution, to scale, mixing is as liquid to be measured with absolute ethyl alcohol dilution and constant volume.
B, the gained sample is carried out GC-MS analyze.Analysis result such as following table:
| Manufacturing enterprise | Methyl alcohol | N-propanol | Isobutyl alcohol | Isoamylol |
| Enterprise 1 | 8.7 | 20.5 | Do not detect | Do not detect |
| Enterprise 2 | 44.6 | 97.5 | 10.6 | 17.4 |
| Enterprise 3 | 96.0 | 190.4 | 20.1 | 29.7 |
| Enterprise 4 | 154.3 | 78.9 | 5.7 | 4.1 |
| Enterprise 5 | 14.9 | 101.2 | Do not detect | Do not detect |
Claims (7)
1. the method for methyl alcohol, n-propanol, isobutyl alcohol, isoamylol content in mensuration alcohol, it is characterized in that: comprise the following steps successively: (1) alcohol sample pre-treatments step: pipette sample alcohol in volumetric flask, add again inner mark solution, dilute and be settled to scale with absolute ethyl alcohol, mixing is as liquid to be measured; (2) blank assay: do not add sample, repeat (1) step; (3) gained sample and blank sample are carried out the gas chromatography-mass spectrography analysis.
2. a kind of method of measuring methyl alcohol in alcohol, n-propanol, isobutyl alcohol, isoamylol content according to claim 1 is characterized in that: in described step (1), the volume ratio of inner mark solution and sample alcohol is 1: 2-3.
3. a kind of method of measuring methyl alcohol in alcohol, n-propanol, isobutyl alcohol, isoamylol content according to claim 1 and 2, it is characterized in that: described inner mark solution refers to that normal butyl alcohol content is the ethanol solution of 0.05mg/ml.
4. a kind of method of measuring methyl alcohol in alcohol, n-propanol, isobutyl alcohol, isoamylol content according to claim 1, it is characterized in that: the scale of the volumetric flask in described step (1) is 10ml.
5. a kind of method of measuring methyl alcohol in alcohol, n-propanol, isobutyl alcohol, isoamylol content according to claim 1, it is characterized in that: the gas phase condition when described step (3) is carried out the gas chromatography-mass spectrography analysis is: chromatographic column: HP-INNOWax, 60m(length) μ m(thickness * 0.25mm(internal diameter) * 0.25), temperature programme: 70 ℃, keep 5min; Rise to 100 ℃ with 5 ℃/min speed; Rise to 150 ℃ with 30 ℃/min again, keep 10min.
6. a kind of method of measuring methyl alcohol in alcohol, n-propanol, isobutyl alcohol, isoamylol content according to claim 1, is characterized in that: the alcohol of described alcohol for producing as raw material with sugarcane, corn, potato class, molasses.
7. a kind of method of measuring methyl alcohol in alcohol, n-propanol, isobutyl alcohol, isoamylol content according to claim 1 is characterized in that: described gas chromatography-mass spectrography analysis is adopted multistage standard model to calculate the calibration factor to carry out quantitatively; Detecting device is mass detector, adopts characteristic ion that target compound is measured.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104535701A (en) * | 2014-12-24 | 2015-04-22 | 青岛九龙生物医药有限公司 | Method for determining content of methanol in heparin sodium recovery ethanol |
| CN105445383A (en) * | 2014-08-14 | 2016-03-30 | 中粮生物化学（安徽）股份有限公司 | Amine-alcohol-kerosene extraction solvent quantitative analysis method |
| CN108760934A (en) * | 2018-07-13 | 2018-11-06 | 江苏力凡胶囊有限公司 | The assay method of residual solvent in a kind of carragheen |
| CN112526053A (en) * | 2020-12-29 | 2021-03-19 | 陕西延长石油（集团）有限责任公司 | Method for measuring mixed alcohol and mixed ester in industrial ethanol by gas chromatography internal standard method |
| CN113917013A (en) * | 2021-09-30 | 2022-01-11 | 山东省葡萄研究院 | Method for measuring methanol and 5 higher alcohols in fruit distilled liquor by internal standard method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105445383A (en) * | 2014-08-14 | 2016-03-30 | 中粮生物化学（安徽）股份有限公司 | Amine-alcohol-kerosene extraction solvent quantitative analysis method |
| CN104535701A (en) * | 2014-12-24 | 2015-04-22 | 青岛九龙生物医药有限公司 | Method for determining content of methanol in heparin sodium recovery ethanol |
| CN108760934A (en) * | 2018-07-13 | 2018-11-06 | 江苏力凡胶囊有限公司 | The assay method of residual solvent in a kind of carragheen |
| CN112526053A (en) * | 2020-12-29 | 2021-03-19 | 陕西延长石油（集团）有限责任公司 | Method for measuring mixed alcohol and mixed ester in industrial ethanol by gas chromatography internal standard method |
| CN113917013A (en) * | 2021-09-30 | 2022-01-11 | 山东省葡萄研究院 | Method for measuring methanol and 5 higher alcohols in fruit distilled liquor by internal standard method |
| CN113917013B (en) * | 2021-09-30 | 2024-02-02 | 山东省葡萄研究院 | Method for measuring methanol and 5 higher alcohols in fruit distilled liquor by internal standard method |
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Application publication date: 20130605 |