CN105588895A - Detecting method for methyl alcohol content in acid - Google Patents
Detecting method for methyl alcohol content in acid Download PDFInfo
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- CN105588895A CN105588895A CN201510939871.4A CN201510939871A CN105588895A CN 105588895 A CN105588895 A CN 105588895A CN 201510939871 A CN201510939871 A CN 201510939871A CN 105588895 A CN105588895 A CN 105588895A
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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Abstract
The invention provides a detecting method for methyl alcohol content in acid. A gas chromatography is adopted for detection, acid to be detected is neutralized through liquid caustic soda, internal standard substance isopropanol is added after the pH of the solution is adjusted to be neutral, ethyl alcohol is used for achieving constant volume of the solution, then an internal standard method is used for detecting a sample on a chromatographic instrument, and the methyl alcohol content is calculated through correction factors calculated through the internal standard method. The detecting method analyzes the methyl alcohol content in acid, has the advantages of being rapid and accurate, and has remarkable social benefits and economic benefits.
Description
Technical field
The present invention relates to methanol content analysis in acid, feature is after acid-conditioning solution pH to be measured is neutrality, adds interior markThing isopropyl alcohol, and use ethanol to carry out constant volume to solution, on chromatograph, use thereafter internal standard method to sample detection, calculate firstAlcohol content.
Background technology
Methyl alcohol is one of basic organic. Mainly for the manufacture of formaldehyde, acetic acid, chloromethanes, methylamine and dimethyl suflfate etc.Multiple organic products. Can be used as coating, varnish, shellac, ink, adhesive, dyestuff, alkaloid, cellulose acetate,The solvent of celluloid, ethyl cellulose, polyvinyl butyral resin etc., can be used as that analytical reagent is clear, motor vehicle antifreeze fluid,Metal surface cleaning agent and alcotate, for organic synthesis etc. Methyl alcohol is important fuel, can mix gasoline and substituteFuel uses. Methyl alcohol uses as the fuel additive of F1 racing car, is also widely used in methanol fuel cell. BeManufacture agricultural chemicals, medicine, plastics, synthetic fibers and Organic chemical products as formaldehyde, methylamine, chloromethanes, dimethyl suflfate etc.Raw material. It is one of important industrial chemicals. In recent years, along with the development of C1 chemical industry, methyl alcohol has become manufacture etheneImportant source material with propylene.
Organosilicon by-product is chloromethanes synthesis tail gas absorption product containing diluted acid, wherein contains a small amount of methyl alcohol. Its production technology is for makingWater absorbs unreacted hydrogen chloride and methyl alcohol. In acid the high low reaction of methanol content the degree of synthetic reaction and material benzenemethanolUtilization rate. Owing to lacking the method for methanol content in a kind of fast detecting acid, can not adjust production work according to methanol content in timeSkill.
In view of the above, the invention provides the analytical method of methanol content in fast detecting diluted acid.
Summary of the invention
The object of the present invention is to provide the gas-chromatography inspection that in a kind of acid, methanol content directly fast, detection sensitivity is highMethod. The inventive method is measured methanol content in acid solution, does not need that sample is carried out to complexity and processes early stage. Adopt ethanolThe solution dilution aqueous solution, reduces water and the damage of salinity to chromatograph sampling system, column system. Use PoraBondU lookSpectrum post, methyl alcohol, ethanol, isopropyl alcohol are effectively separated, and do not affect measurement result. Adopt internal standard method, expansion methyl alcohol detectsScope.
The object of the present invention is achieved like this:
1, set instrument condition of work: set instrument condition of work as following table 1.
Table 1 chromatographiccondition
2, preparing standard solution: in the dry 50ml volumetric flask of weighing, add 5ml methyl alcohol and weigh, accurate to 0.0001g.Be diluted to scale and weigh with ethanol, mixing, as mother liquor. Divide in 4 clean, dry 50ml volumetric flasks, respectivelyAdd 0ml, 5ml, the above-mentioned mother liquor of 10ml, 20ml, then add 25 μ L isopropyl alcohols as interior mark, be diluted to quarter with ethanolDegree, mixes.
3, measure relative correction factor: start gas chromatograph, set instrument by table 1 condition. After instrument stabilizer, pointOther sample introduction analysis. Relative correction factor is calculated and is calculated as follows.
In formula:
ms---the quality of methyl alcohol;
me---the quality of isopropyl alcohol;
As---the peak area of methyl alcohol;
Ae---the peak area of isopropyl alcohol.
4, sample solution processing: add a certain amount of sodium hydroxide solution to be neutralized to pH in a certain amount of diluted acid and equal 7.Add deionized water constant volume to 50ml volumetric flask, quality after weighing constant volume. From 1 solution, take about 1g solution, addTo 50ml volumetric flask, then add about 20ug isopropyl alcohol as interior mark, with chromatographically pure ethanol constant volume. Adopt following formula meterCalculate dilution gfactor D:
In formula:
W2---the quality of solution after constant volume;
W3---pipette the quality of solution.
5, sample determination: after processing with microsyringe, sample solution injects chromatogram. Record methyl alcohol peak area, isopropyl alcoholPeak area, adopts following formula to calculate methanol content in ethanolic solution:
In formula:
X1---the quality of methyl alcohol;
A1---methyl alcohol peak area;
A2---isopropyl alcohol peak area;
W4---the quality of isopropyl alcohol;
The correction factor of f---isopropyl alcohol to methyl alcohol.
6, calculate methanol content in acid solution: adopt following formula to calculate methanol content in acid solution:
In formula:
X---the quality of methyl alcohol in acid solution;
X1---the quality of methyl alcohol;
W1---the quality of dilute acid soln.
Instrument and equipment of the present invention and reagent:
Gas-chromatography (hydrogen ion flame detector), pH meter, beaker, glass bar, pipette, 50ml volumetric flaskTrace, micro syringe, 1mol/l sodium hydroxide solution, 0.01mol/l sodium hydroxide solution.
Good effect of the present invention is:
1 provides the analytical method of methyl alcohol in a kind of diluted acid.
2 the present invention can be used for the analysis of methanol content in other acid and carbinol mixture.
The impetus that 3 the present invention play containing the quality control of alcohol diluted acid organosilicon.
Detailed description of the invention
Embodiment 1
Methanol content measuring in watery hydrochloric acid
1, set instrument condition: press table 1 condition and set instrument.
2, preparing standard solution: in the dry 50ml volumetric flask of weighing, add 5ml methyl alcohol and weigh, the quality of titleFor 3.9107g. Be diluted to scale and weigh with ethanol, mixing, as mother liquor. Divide 4 clean, dry 50ml to holdIn measuring bottle, add respectively 0ml, 5ml, the above-mentioned mother liquor of 10ml, 20ml, then add 25 μ L isopropyl alcohols as interior mark, useEthanol is diluted to scale, mixes.
3, measure correction factor: measure relative correction factor: start gas chromatograph, set instrument by table 1 condition. TreatAfter instrument stabilizer, sample introduction analysis respectively. After integration, obtain methyl alcohol peak area and isopropyl alcohol peak area. Calculate relative correction factorBe 1.4.
4, take 5.0549 grams of watery hydrochloric acid in 500 ml beakers, drip 1mol/l sodium hydroxide solution and neutralize pH etc.In 7. Solution is transferred to 50 milliliters of volumetric flasks, adds ultra-pure water constant volume, weigh and show that solution gross mass is 50.1762Gram. From volumetric flask, take 1.0398 grams and add volumetric flask, take 0.0197 gram of isopropyl alcohol and add after volumetric flask, use ethanolBe settled to 50 milliliters, calculate dilution gfactor 48.256.
5, sample determination: after instrument stabilizer, by sample chromatogram instrument after above-mentioned processing, sample size 2 μ l. After integration, obtainMethyl alcohol peak area 3015 and isopropyl alcohol peak area 11089. Adopting formula to calculate methanol quality is 0.0075 gram,
6, calculate methanol content in acid solution: in diluted acid, methanol content is 7.1%.
Embodiment 2
Methanol content measuring in slightly acidic water
1, set instrument condition: press table 1 condition and set instrument.
2, preparing standard solution: in the dry 50ml volumetric flask of weighing, add 5ml methyl alcohol and weigh, the quality of titleFor 3.8995g. Be diluted to scale and weigh with ethanol, mixing, as mother liquor. Divide 4 clean, dry 50ml to holdIn measuring bottle, add respectively 0ml, 5ml, the above-mentioned mother liquor of 10ml, 20ml, then add 25 μ L isopropyl alcohols as interior mark, useEthanol is diluted to scale, mixes.
3, measure correction factor: measure relative correction factor: start gas chromatograph, set instrument by table 1 condition. TreatAfter instrument stabilizer, sample introduction analysis respectively. After integration, obtain methyl alcohol peak area and isopropyl alcohol peak area. Calculate relative correction factorBe 1.4.
4, take 4.9924g slightly acidic water solution constant volume in 50 milliliters of volumetric flasks, drip 0.01mol/l sodium hydroxide solutionNeutralization equals 7 to pH. Weighing obtains 49.6825 grams of solution qualities. From volumetric flask, take 1.0116 grams and add volumetric flask,Take after 0.0196 gram of isopropyl alcohol adds volumetric flask and use ethanol constant volume, calculate dilution gfactor 49.113.
5, sample determination: after instrument stabilizer, by sample chromatogram instrument after above-mentioned processing, sample size 2 μ l. After integration, obtainMethyl alcohol peak area 2194 and isopropyl alcohol peak area 11152. Adopting formula to calculate methanol quality is 0.0054 gram,
6, calculate methanol content in acid solution: in water, methanol content is 5.3%.
Embodiment 3
Methanol content measuring in dilute sulfuric acid
1, set instrument condition: press table 1 condition and set instrument.
2, preparing standard solution: in the dry 50ml volumetric flask of weighing, add 5ml methyl alcohol and weigh, the quality of titleFor 3.8995g. Be diluted to scale and weigh with ethanol, mixing, as mother liquor. Divide 4 clean, dry 50ml to holdIn measuring bottle, add respectively 0ml, 5ml, the above-mentioned mother liquor of 10ml, 20ml, then add 25 μ L isopropyl alcohols as interior mark, useEthanol is diluted to scale, mixes.
3, measure correction factor: measure relative correction factor: start gas chromatograph, set instrument by table 1 condition. TreatAfter instrument stabilizer, sample introduction analysis respectively. After integration, obtain methyl alcohol peak area and isopropyl alcohol peak area. Calculate relative correction factorBe 1.4.
4, take 2.0125g dilution heat of sulfuric acid constant volume in 50 milliliters of volumetric flasks, drip the neutralization of 1.0mol/l sodium hydroxide solutionEqual 7 to pH. Weighing obtains 50.0121 grams of solution qualities. From volumetric flask, take 1.0058 grams and add volumetric flask, claimGet after 0.0197 gram of isopropyl alcohol adds volumetric flask and use ethanol constant volume, calculate dilution gfactor 49.724.
5, sample determination: after instrument stabilizer, by sample chromatogram instrument after above-mentioned processing, sample size 2 μ l. After integration, obtainMethyl alcohol peak area 1548 and isopropyl alcohol peak area 11201. Adopting formula to calculate methanol quality is 0.0038 gram,
6, calculate methanol content in dilution heat of sulfuric acid: in dilute sulfuric acid, methanol content is 9.4%.
Claims (3)
1. a detection method for methanol content in acid, is characterized in that: adopt gas-chromatography to detect, acid to be measured is usedLiquid caustic soda neutralizes, and after regulator solution pH is neutrality, adds internal standard compound isopropyl alcohol, and uses ethanol to carry out constant volume to solution,Thereafter on chromatograph, use internal standard method to sample detection, the correction factor calculating according to internal standard method calculates methanol content.
2. the detection method of methanol content in acid according to claim 1, is characterized in that: described acid refers to contain methyl alcoholThe solution of hydrochloric acid, sulfuric acid or nitric acid.
3. the detection method of methanol content in acid according to claim 1, is characterized in that: adopt gas-chromatography to examineWhen survey, chromatographic column is PoraBondU; Column length, column internal diameter, thickness of liquid film are respectively 25,0.32,7; Column temperature is adjusted to 110 DEG CKeep 1min, be warming up to 160 DEG C with the heating rate of 10 DEG C/min afterwards, keep 2min; Temperature of vaporization chamber is 150 DEG C; InspectionSurveying room temperature is 200 DEG C; Air mass flow 350mL/min; Nitrogen flow 35mL/min; Carrier gas flux 1.0mL/min; ShuntingThan being 25:1.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101210909A (en) * | 2007-12-24 | 2008-07-02 | 山西省国家煤及煤化工产品质量监督检验中心 | Methanol fuel methanol content measuring method |
| WO2012019134A2 (en) * | 2010-08-06 | 2012-02-09 | Brown University | Functionalized chromatographic materials and methods of making and using therefor |
| 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 |
| CN104749271A (en) * | 2015-03-06 | 2015-07-01 | 沈阳石蜡化工有限公司 | Determination method for content of methanol in water of methanol cracking device |
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- 2015-12-16 CN CN201510939871.4A patent/CN105588895B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101210909A (en) * | 2007-12-24 | 2008-07-02 | 山西省国家煤及煤化工产品质量监督检验中心 | Methanol fuel methanol content measuring method |
| WO2012019134A2 (en) * | 2010-08-06 | 2012-02-09 | Brown University | Functionalized chromatographic materials and methods of making and using therefor |
| 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 |
| CN104749271A (en) * | 2015-03-06 | 2015-07-01 | 沈阳石蜡化工有限公司 | Determination method for content of methanol in water of methanol cracking device |
Non-Patent Citations (4)
| Title |
|---|
| 刘百战等: "香精香料中溶剂及水分含量的气相色谱分析", 《烟草科技》 * |
| 叶建晨等: "顶空毛细管气相色谱法测定葡萄酒中甲醇残留量", 《中国卫生检验杂志》 * |
| 李小娟等: "Plot-U毛细管柱气相色谱测定工作场所空气中的甲醇", 《光谱实验室》 * |
| 王少锋: "工业浓盐酸中微量甲醇的测定", 《河南化工》 * |
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