CN105588895B - The detection method of methanol content in a kind of acid - Google Patents
The detection method of methanol content in a kind of acid Download PDFInfo
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- CN105588895B CN105588895B CN201510939871.4A CN201510939871A CN105588895B CN 105588895 B CN105588895 B CN 105588895B CN 201510939871 A CN201510939871 A CN 201510939871A CN 105588895 B CN105588895 B CN 105588895B
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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 present invention provides a kind of detection method of methanol content in acid, detected using gas-chromatography, acid to be measured is neutralized with liquid caustic soda, after pH value of solution is adjusted for neutrality, add internal standard compound isopropanol, and constant volume is carried out to solution using ethanol, use internal standard method to sample detection on chromatograph thereafter, the correction factor calculated according to internal standard method is calculated methanol content.Methanol content in detection method analysis acid, with fast and accurately feature, with significant Social benefit and economic benefit.
Description
Technical field
Analyzed the present invention relates to methanol content in acid, be characterized in after to acid-conditioning solution pH to be measured for neutrality, to add interior
Thing isopropanol is marked, and constant volume is carried out to solution using ethanol, uses internal standard method to sample detection on chromatograph thereafter, calculates first
Alcohol content.
Background technology
Methanol is one of basic organic.Mainly for the manufacture of formaldehyde, acetic acid, chloromethanes, methylamine and dimethyl suflfate
Etc. a variety of organic products.It can be used as coating, varnish, shellac, ink, adhesive, dyestuff, alkaloid, cellulose acetate, nitric acid fine
Tie up the solvent of element, ethyl cellulose, polyvinyl butyral resin etc., can be used as analytical reagent clearly, motor vehicle antifreeze fluid, metal surface it is clear
Lotion and alcotate, for organic synthesis etc..Methanol is important fuel, can mix gasoline and be used as alternative fuel.First
Alcohol is used as the fuel additive of F1 racing cars, is also widely used in methanol fuel cell.Be manufacture agricultural chemicals, medicine,
The raw material of plastics, synthetic fibers and Organic chemical products such as formaldehyde, methylamine, chloromethanes, dimethyl suflfate etc..It is important chemical industry
One of raw material.In recent years, with the development of C1 chemical industry, methanol has become the important source material of manufacture ethene and propylene.
Organosilicon by-product is chloromethanes synthesis tail gas absorption product containing diluted acid, wherein containing a small amount of methanol.Its production technology
To absorb unreacted hydrogen chloride and methanol using water.The high low reaction of the methanol content degree and raw material first of synthetic reaction in acid
The utilization rate of alcohol.Method due to lacking methanol content in a kind of quick detection acid, it is impossible to adjusted give birth to according to methanol content in time
Production. art.
In view of the above, the invention provides the analysis method of methanol content in quick detection diluted acid.
The content of the invention
It is an object of the invention to provide a kind of directly high gas-chromatography of quick, detection sensitivity of methanol content in acid
The method of inspection.The inventive method determines methanol content in acid solution, it is not necessary to complicated early stage is carried out to sample and is handled.Using second
Alcoholic solution dilute aqueous solution, reduces the damage of water and salinity to chromatograph sampling system, column system.Use PoraBond U chromatograms
Post, methanol, ethanol, isopropanol are efficiently separated, and do not influence measurement result.Using internal standard method, methanol inspection range is extended.
The object of the present invention is achieved like this：
1st, instrument condition of work is set：Set instrument condition of work such as table 1 below.
The chromatographiccondition of table 1
2nd, preparing standard solution：In dry 50ml volumetric flasks of having weighed, add 5ml methanol and weigh, standard is extremely
0.0001g.Scale is diluted to ethanol and is weighed, mixes, is used as mother liquor.In the 50ml volumetric flasks for divide 4 cleanings, drying, point
Not Jia Ru the above-mentioned mother liquor of 0ml, 5ml, 10ml, 20ml, add 25 μ L isopropanols as internal standard, scale be diluted to ethanol, mix
It is even.
3rd, relative correction factor is determined：Start gas chromatograph, instrument is set by the condition of table 1.After after instrument stabilizer, distinguish
Sample introduction is analyzed.Relative correction factor is calculated and is calculated as follows.
In formula：
ms--- the quality of methanol；
me--- the quality of isopropanol；
As--- the peak area of methanol；
Ae--- the peak area of isopropanol.
4th, sample solution is handled：A certain amount of sodium hydroxide solution is added in a certain amount of diluted acid and is neutralized to pH equal to 7.
Deionized water constant volume is added to 50ml volumetric flasks, quality after constant volume is weighed.About 1g solution is weighed from 1 solution, 50ml is added to
Volumetric flask, adds about 20ug isopropanols as internal standard, with chromatogram straight alcohol constant volume.Using equation below dilution factor calculated D：
In formula：
W2--- the quality of solution after constant volume；
W3--- pipette the quality of solution.
5th, sample is determined：Sample solution injection chromatogram after being handled with microsyringe.Record methanol peak area, isopropanol
Peak area, methanol content in ethanol solution is calculated using equation below：
In formula：
X1--- the quality of methanol；
A1--- methanol peak area；
A2--- isopropanol peak area；
W4--- the quality of isopropanol；
Correction factor of f --- the isopropanol to methanol.
6th, methanol content in acid solution is calculated：Methanol content in acid solution is calculated using equation below：
In formula：
X --- the quality of methanol in acid solution；
X1--- the quality of methanol；
W1--- the quality of dilute acid soln.
The instrument and equipment and reagent of the present invention：
Gas-chromatography (hydrogen ion flame detector), pH meter, beaker, glass bar, pipette, 50ml volumetric flasks are micro, micro-
Measure syringe, 1mol/l sodium hydroxide solutions, 0.01mol/l sodium hydroxide solutions.
The positive effect of the present invention is：
1 provides a kind of analysis method of methanol in diluted acid.
Analysis of 2 present invention available for methanol content in other acid and carbinol mixture.
The impetus that quality control of 3 present invention to organosilicon containing alcohol diluted acid is played.
Embodiment
Embodiment 1
Methanol content measuring in watery hydrochloric acid
1st, instrument condition is set：Instrument is set by the condition of table 1.
2nd, preparing standard solution：In dry 50ml volumetric flasks of having weighed, add 5ml methanol simultaneously weigh, quality be called
3.9107g.Scale is diluted to ethanol and is weighed, mixes, is used as mother liquor.In the 50ml volumetric flasks for divide 4 cleanings, drying, point
Not Jia Ru the above-mentioned mother liquor of 0ml, 5ml, 10ml, 20ml, add 25 μ L isopropanols as internal standard, scale be diluted to ethanol, mix
It is even.
3rd, correction factor is determined：Determine relative correction factor：Start gas chromatograph, instrument is set by the condition of table 1.Treat instrument
After device is stable, sample introduction analysis respectively.Methanol peak area and isopropanol peak area are obtained after integration.Calculating relative correction factor is
1.4。
4th, 5.0549 grams of watery hydrochloric acid are weighed in 500 milliliters of beakers, the neutralization of 1mol/l sodium hydroxide solutions is added dropwise and arrives pH etc.
In 7.Solution is transferred to 50 milliliters of volumetric flasks, ultra-pure water constant volume is added, weighing show that solution gross mass is 50.1762 grams.From
1.0398 grams of addition volumetric flasks are weighed in volumetric flask, 0.0197 gram of isopropanol is weighed and adds after volumetric flask, 50 are settled to ethanol
Milliliter, calculates dilution gfactor 48.256.
5th, sample is determined：After after instrument stabilizer, by sample chromatogram instrument after above-mentioned processing, the μ l of sample size 2.First is obtained after integration
Alcohol peak area 3015 and isopropanol peak area 11089.Formula is used to calculate methanol quality for 0.0075 gram,
6th, methanol content in acid solution is calculated：Methanol content is 7.1% in diluted acid.
Embodiment 2
Methanol content measuring in slightly acidic water
1st, instrument condition is set：Instrument is set by the condition of table 1.
2nd, preparing standard solution：In dry 50ml volumetric flasks of having weighed, add 5ml methanol simultaneously weigh, quality be called
3.8995g.Scale is diluted to ethanol and is weighed, mixes, is used as mother liquor.In the 50ml volumetric flasks for divide 4 cleanings, drying, point
Not Jia Ru the above-mentioned mother liquor of 0ml, 5ml, 10ml, 20ml, add 25 μ L isopropanols as internal standard, scale be diluted to ethanol, mix
It is even.
3rd, correction factor is determined：Determine relative correction factor：Start gas chromatograph, instrument is set by the condition of table 1.Treat instrument
After device is stable, sample introduction analysis respectively.Methanol peak area and isopropanol peak area are obtained after integration.Calculating relative correction factor is
1.4。
4th, 4.9924g slightly acidic water solution constant volumes are weighed in 50 milliliters of volumetric flasks, 0.01mol/l sodium hydroxide solutions are added dropwise
PH is neutralized equal to 7.Weighing obtains 49.6825 grams of solution quality.1.0116 grams of addition volumetric flasks are weighed from volumetric flask, are weighed
0.0196 gram of isopropanol uses ethanol constant volume after adding volumetric flask, calculates dilution gfactor 49.113.
5th, sample is determined：After after instrument stabilizer, by sample chromatogram instrument after above-mentioned processing, the μ l of sample size 2.First is obtained after integration
Alcohol peak area 2194 and isopropanol peak area 11152.Formula is used to calculate methanol quality for 0.0054 gram,
6th, methanol content in acid solution is calculated：Methanol content is 5.3% in water.
Embodiment 3
Methanol content measuring in dilute sulfuric acid
1st, instrument condition is set：Instrument is set by the condition of table 1.
2nd, preparing standard solution：In dry 50ml volumetric flasks of having weighed, add 5ml methanol simultaneously weigh, quality be called
3.8995g.Scale is diluted to ethanol and is weighed, mixes, is used as mother liquor.In the 50ml volumetric flasks for divide 4 cleanings, drying, point
Not Jia Ru the above-mentioned mother liquor of 0ml, 5ml, 10ml, 20ml, add 25 μ L isopropanols as internal standard, scale be diluted to ethanol, mix
It is even.
3rd, correction factor is determined：Determine relative correction factor：Start gas chromatograph, instrument is set by the condition of table 1.Treat instrument
After device is stable, sample introduction analysis respectively.Methanol peak area and isopropanol peak area are obtained after integration.Calculating relative correction factor is
1.4。
4th, 2.0125g dilution heat of sulfuric acid constant volume is weighed in 50 milliliters of volumetric flasks, is added dropwise in 1.0mol/l sodium hydroxide solutions
It is equal to 7 with to pH.Weighing obtains 50.0121 grams of solution quality.1.0058 grams of addition volumetric flasks are weighed from volumetric flask, are weighed
0.0197 gram of isopropanol uses ethanol constant volume after adding volumetric flask, calculates dilution gfactor 49.724.
5th, sample is determined：After after instrument stabilizer, by sample chromatogram instrument after above-mentioned processing, the μ l of sample size 2.First is obtained after integration
Alcohol peak area 1548 and isopropanol peak area 11201.Formula is used to calculate methanol quality for 0.0038 gram,
6th, methanol content in dilution heat of sulfuric acid is calculated：Methanol content is 9.4% in dilute sulfuric acid.
Claims (1)
1. the detection method of methanol content in a kind of acid, it is characterised in that：Detected using gas-chromatography, by acid liquid to be measured
Alkali is neutralized, after regulation pH value of solution is neutrality, adds internal standard compound isopropanol, and carries out constant volume to solution using ethanol, thereafter
Using internal standard method to sample detection on chromatograph, the correction factor calculated according to internal standard method is calculated methanol content；Adopt
When being detected with gas-chromatography, chromatographic column is Pora Bond U；Column length, column internal diameter, thickness of liquid film be respectively 25m,
0.32mm、7μm；Column temperature is adjusted to 110 DEG C of holding 1min, is warming up to 160 DEG C, holding afterwards with 10 DEG C/min heating rate
2min；Temperature of vaporization chamber is 150 DEG C；It is 200 DEG C to detect room temperature；Air mass flow 350mL/min；Nitrogen flow 35mL/min；
Carrier gas flux 1.0mL/min；Split ratio is 25:1, described acid refers to the solution of the hydrochloric acid containing methanol, sulfuric acid or nitric acid.
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