CN113198637A - Spraying device and method for detecting multi-carbon alcohol in methanol gasoline - Google Patents
Spraying device and method for detecting multi-carbon alcohol in methanol gasoline Download PDFInfo
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- CN113198637A CN113198637A CN202110373419.1A CN202110373419A CN113198637A CN 113198637 A CN113198637 A CN 113198637A CN 202110373419 A CN202110373419 A CN 202110373419A CN 113198637 A CN113198637 A CN 113198637A
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- valve
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
- B05B9/00—Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour
- B05B9/03—Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour characterised by means for supplying liquid or other fluent material
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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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N2021/0106—General arrangement of respective parts
- G01N2021/0112—Apparatus in one mechanical, optical or electronic block
Abstract
A spraying device and a detection method for detecting multi-carbon alcohol in methanol gasoline belong to the technical field of multi-carbon alcohol detection, and can solve the problems that the existing detection method for detecting the content of the multi-carbon alcohol in the methanol gasoline consumes long time, is expensive in equipment, high in cost, not easy to operate and cannot be used for on-site determination. The detection method is simple, sensitive, high in detection speed, convenient to use, high in accuracy and convenient to carry.
Description
Technical Field
The invention belongs to the technical field of detection of multi-carbon alcohol, and particularly relates to a spraying device and a detection method for detecting the multi-carbon alcohol in methanol gasoline.
Background
With the reduction of oil reserves and the increase of environmental requirements, the development and utilization of new renewable energy sources has become a necessary trend. The methanol is mixed with a certain proportion of gasoline to be widely used as an energy source for vehicles. The methanol has the advantages that the octane value of the gasoline can be effectively improved, the gasoline can be completely combusted, the combustion efficiency is increased, the economy is improved, and the atmospheric pollution is reduced; the methanol has low heat value, and after a large amount of methanol is mixed into gasoline, gas resistance is easily generated to influence oil supply; methanol is easy to generate corrosion, abrasion and other adverse effects on sealing systems of engines, particularly piston rings, cylinder wall oil pumps and the like, but can be solved by adding a corrosion inhibitor into engine oil. A large body of data has demonstrated that methanol is one of the most promising and realistic clean alternative fuels in the near future.
Methanol is a highly polar organic substance, and gasoline is a nonpolar hydrocarbon mixture. Due to the large difference in polarity between molecules, methanol and gasoline are particularly not easily mixed directly, especially at lower temperatures. It is therefore necessary to add small amounts of co-solvent to the methanol gasoline. The multi-carbon alcohol (monohydric alcohol of C3-C8), especially monohydric alcohol of C4-C5, can improve the intersolubility of methanol and gasoline and improve the stability of the methanol and gasoline. In addition, because of abundant market raw materials and low price, the methanol gasoline additive is often used as a methanol gasoline cosolvent or a main component of a methanol gasoline additive, but the methanol gasoline additive has negative effects on automobiles when being used in large quantities. Therefore, the determination of the content of the multi-carbon alcohol has important significance when the methanol gasoline is prepared and used.
At present, the commonly used methods for measuring the content of the multi-carbon alcohol in the methanol gasoline industry comprise a gas chromatography-mass spectrometry method, a switching-back flushing gas chromatography method and the like. These methods can accurately measure the content of the polyhydric alcohol, but they have the disadvantages of long time consumption, expensive equipment, high cost, difficult operation and incapability of on-site measurement, so that a method which is simple to operate, low in cost, convenient to use, high in detection speed and high in accuracy is required to be constructed.
Disclosure of Invention
The invention provides a spraying device and a detection method for detecting the content of the multi-carbon alcohol in the methanol gasoline, aiming at the problems that the existing detection method for the content of the multi-carbon alcohol in the methanol gasoline has long time consumption, expensive equipment, higher cost, difficult operation and incapability of on-site measurement.
The invention adopts the following technical scheme:
the utility model provides a spraying device that is arranged in methanol gasoline many carbon alcohols to detect, including the stock solution bottle that has opening I and opening II, be equipped with hollow bottle plug I of taking valve II on the opening I, be equipped with bottle plug II on the opening II, be equipped with the three-way pipe that passes bottle plug II on the bottle plug II, the one end of pipe stretches into the stock solution bottle, one end is connected with the syringe, the other end is connected with the container, be equipped with valve I on the pipe, valve I is located the tee bend department of pipe and between the contact department with bottle plug II, be equipped with valve III on the container, the other end of container is equipped with the drain pipe, be equipped with valve IV on the drain pipe, the tip of drain pipe is equipped with the nozzle.
A method for detecting a multi-carbon alcohol in methanol gasoline comprises the following steps:
firstly, preparing a color developing solution, dissolving chromic anhydride in concentrated sulfuric acid according to 1.0g/mL, stirring to obtain a suspension, slowly adding the suspension into water with the volume 3 times that of the concentrated sulfuric acid, and cooling to room temperature;
step two, preparing a standard colorimetric plate: according to volume percentage, gasoline containing 15-25% of olefin, 30-40% of aromatic hydrocarbon and 35-55% of alkane is used as base oil; taking mixed alcohol containing 10% of n-propanol, 10% of isopropanol, 30% of mixed butanol, 30% of mixed pentanol, 5% of cyclohexanol, 5% of n-hexanol and 10% of sec-octanol as the multi-carbon alcohol;
preparing 13 parts of standard sample, wherein each part of base oil is 70-80 parts by volume, the content of the multi-carbon alcohol is 0.3, 0.5, 0.7, 0.9, 1.2, 1.5, 2.0, 2.5, 3.0, 3.5, 4.0, 4.5 or 5.0, and the balance is methanol; dripping 13 parts of standard samples on 13 silica gel chromatographic plates respectively, placing the plates in a container filled with ether, taking out the chromatographic plates to air dry when the ether is soaked upwards to a position of 0.3-0.5cm from the top end of the chromatographic plates, spraying a color developing solution by using a spraying device, and developing to obtain standard colorimetric plates;
thirdly, dripping a sample to be detected on the silica gel chromatographic plate, placing the silica gel chromatographic plate in a container filled with ether, taking out the chromatographic plate to air dry when the ether is soaked upwards to a position of 0.3-0.5cm from the top end of the chromatographic plate, spraying a color developing solution by using a spraying device, developing, and comparing with a standard colorimetric plate to obtain the content of the multi-carbon alcohol.
Further, the use method of the spraying device comprises the following steps:
firstly, opening a bottle stopper I of a liquid storage bottle, adding color developing liquid, and covering the bottle stopper I;
secondly, closing the valve I and the valve II, opening the valve III, lifting the injector piston to the maximum position, and closing the valve III;
thirdly, sucking 0.5mL of sample to be detected by using a 0.5mL suction tube, slowly placing the sample to be detected at the baseline of the silica gel plate, placing the sample in a chromatography bottle after the sample is half-dried until the front edge of the developing agent reaches 45mm of the silica gel plate, and taking out the silica gel plate until the sample is half-dried;
fourthly, placing the silica gel plate below the nozzle of the sprayer, unscrewing the valve IV, quickly pressing the plunger of the injector to the bottom end to finish spraying, comparing the silica gel plate with a standard colorimetric plate after 5 seconds, deducting the color band at the bottommost end during comparison, and determining the content of the multi-carbon alcohol.
The invention has the following beneficial effects:
the method utilizes a thin-layer chromatography plate to rapidly separate methanol from the polyhydric alcohol under the action of a developing agent, uses Jones reagent to rapidly develop color, and can rapidly analyze the content of the polyhydric alcohol by comparing with a standard colorimetric plate. The detection method is simple, sensitive, high in detection speed, convenient to use, high in accuracy and convenient to carry.
Drawings
FIG. 1 is a schematic view of the construction of the spray coating device of the present invention;
wherein: 1-liquid storage bottle; 2-opening I; 3-opening II; 4-valve II; 5-bottle stopper I; 6-a catheter; 7-a syringe; 8-a container; 9-valve I; 10-valve III; 11-a liquid outlet pipe; 12-valve iv; 13-nozzle.
Detailed Description
The invention is further explained with reference to the accompanying drawings.
Example 1
Ether (analytically pure)
Chromatography cup (with lid 1000mL wide-mouth bottle)
Silica gel chromatography plate: polypropylene substrate (thickness 1mm), H-type silica gel (200 mesh), silica gel coating thickness 0.5mm, area, 30mm x 50 mm.
Chromic anhydride (analytically pure)
Concentrated sulfuric acid (analytically pure 98%)
Distilled water
Preparing a color developing solution: adding 20g of chromic anhydride into 20mL of concentrated sulfuric acid, stirring to obtain a suspension, slowly adding the suspension into 60mL of water, and cooling to room temperature.
Preparing a standard colorimetric plate: gasoline containing 20% of olefin, 30% of aromatic hydrocarbon and 50% of alkane is used as base oil, and gasoline containing 10% of n-propanol, 10% of isopropanol, 30% of mixed butanol, 30% of mixed pentanol, 5% of cyclohexanol, 5% of n-hexanol and 10% of sec-octanol is used as multi-carbon alcohol; taking 13 parts of 75mL base oil, adding 0.3mL, 0.5mL, 0.7mL, 0.9mL, 1.2mL, 1.5mL, 2.0mL, 2.5mL, 3.0mL, 3.5mL, 4.0mL, 4.5mL and 5.0mL of polyhydric alcohol respectively, then supplementing the mixture to 100mL by methanol, dripping 13 parts of standard samples on 13 silica gel chromatographic plates respectively, placing the chromatographic plates in a container with ether, taking out the chromatographic plates to air dry when the ether is soaked to 0.5cm of the top end of the chromatographic plates upwards, spraying a color developing solution by a sprayer, and developing to obtain the standard colorimetric plates.
Self-prepared methanol gasoline (containing 4.5% methanol and 0.5% mixed butanol) is dripped on a silica gel chromatographic plate, the silica gel chromatographic plate is placed in a container filled with ether, when the ether is soaked upwards to a position which is just 0.5cm away from the top end of the chromatographic plate, the chromatographic plate is taken out and dried, a sprayer is used for spraying a color developing solution, and color development is carried out, and the standard colorimetric plate is compared, so that the content of the multi-carbon alcohol is 0.4%.
The sprayer comprises the following components: as shown in fig. 1, the sprayer is composed of a liquid storage bottle, 4 valves, a syringe (not less than 10mL), a 2mL small container, a nozzle and the like, and all the parts of the sprayer are connected by glass tubes. The nozzle is made of polypropylene plastics and is made of glass except the nozzle. The nozzle is inside by porous polyethylene board (thickness 2mm, diameter 10mm, the hole number 8~12, aperture diameter 1mm), and the outside comprises central authorities haplopore polypropylene plastic plate (external diameter 10mm, hole diameter 0.5mm, thickness 3mm), passes through polyethylene spiral external member with two subassemblies and fixes to with glass union coupling.
The using method of the sprayer comprises the following steps: opening the ground bottle stopper at the top of the center of the sprayer, adding color development liquid (the color development liquid can not contain mechanical impurities), and covering the bottle stopper. Firstly, unscrewing a valve I and a valve II, closing a valve III and a valve IV, and extracting an injector piston until a left small container is filled with color development liquid. And secondly, closing the valve I and the valve II, opening the valve III, lifting the injector piston to the maximum position, and closing the valve III. And thirdly, sucking 0.5mL of sample to be detected by using a 0.5mL suction pipe, and slowly pointing the sample to be detected at the baseline of the silica gel plate. After half-drying, placing the mixture in a chromatography bottle until the front edge of the developing agent reaches 45mm of the silica gel plate, and taking out the silica gel plate until the mixture is half-dried. Fourthly, the silica gel plate is arranged below the nozzle of the sprayer, the valve IV is unscrewed, and the plunger of the injector is quickly pressed to the bottom end to finish spraying. After 5 seconds, the silica gel plate was compared to a standard colorimetric plate (minus the bottom most color band, generally referred to as the methanol band) to determine the multicarbon alcohol content.
Example 2
Methanol gasoline (containing 14% methanol and 1% mixed butanol) was prepared by blending, and the remainder was the same as in example 1, except that the content of the polyhydric alcohol was 1.1%.
Example 3
The remainder of the example 1 was the same as the methanol gasoline (containing 25% methanol and 5% mixed pentanol) with a higher alcohol content of 4.5%.
Example 4
A self-prepared methanol gasoline (containing 10% methanol, 0.4% hexanol) was used as in example 1, except that the higher alcohol content was 0.3%.
Claims (2)
1. The utility model provides a spraying device that is arranged in many carbon alcohols of methanol gasoline to detect which characterized in that: including stock solution bottle (1) that has opening I (2) and opening II (3), be equipped with hollow bottle plug I (5) of taking valve II (4) on opening I (2), be equipped with bottle plug II on opening II (3), be equipped with tee bend pipe (6) of passing bottle plug II on the bottle plug II, the one end of pipe (6) stretches into stock solution bottle (1), one end is connected with syringe (7), the other end is connected with container (8), be equipped with valve I (9) on pipe (6), valve I (9) are located the tee bend department of pipe (6) and with between the contact department of bottle plug II, be equipped with valve III (10) on container (8), the other end of container (8) is equipped with drain pipe (11), be equipped with valve IV (12) on drain pipe (11), the tip of drain pipe (11) is equipped with nozzle (13).
2. A method for detecting a multi-carbon alcohol in methanol gasoline is characterized by comprising the following steps: the method comprises the following steps:
firstly, preparing a color developing solution, dissolving chromic anhydride in concentrated sulfuric acid according to 1.0g/mL, stirring to obtain a suspension, slowly adding the suspension into water with the volume 3 times that of the concentrated sulfuric acid, and cooling to room temperature;
step two, preparing a standard colorimetric plate: according to volume percentage, gasoline containing 15-25% of olefin, 30-40% of aromatic hydrocarbon and 35-55% of alkane is used as base oil; taking mixed alcohol containing 10% of n-propanol, 10% of isopropanol, 30% of mixed butanol, 30% of mixed pentanol, 5% of cyclohexanol, 5% of n-hexanol and 10% of sec-octanol as the multi-carbon alcohol;
preparing 13 parts of standard sample, wherein each part of base oil is 70-80 parts by volume, the content of the multi-carbon alcohol is 0.3, 0.5, 0.7, 0.9, 1.2, 1.5, 2.0, 2.5, 3.0, 3.5, 4.0, 4.5 or 5.0, and the balance is methanol; dripping 13 parts of standard samples on 13 silica gel chromatographic plates respectively, placing the plates in a container filled with ether, taking out the chromatographic plates to air dry when the ether is soaked upwards to a position of 0.3-0.5cm from the top end of the chromatographic plates, spraying a color developing solution by using a spraying device, and developing to obtain standard colorimetric plates;
thirdly, dripping a sample to be detected on a silica gel chromatographic plate, placing the silica gel chromatographic plate in a container filled with ether, taking out the chromatographic plate to air dry when the ether is soaked upwards to a position of 0.3-0.5cm from the top end of the chromatographic plate, spraying a color developing solution by using a spraying device, developing, and comparing with a standard colorimetric plate to obtain the content of the multi-carbon alcohol;
the using method of the spraying device comprises the following steps:
firstly, opening a bottle stopper I of a liquid storage bottle, adding color developing liquid, and covering the bottle stopper I;
secondly, closing the valve I and the valve II, opening the valve III, lifting the injector piston to the maximum position, and closing the valve III;
thirdly, sucking 0.5mL of sample to be detected by using a 0.5mL suction tube, slowly placing the sample to be detected at the baseline of the silica gel plate, placing the sample in a chromatography bottle after the sample is half-dried until the front edge of the developing agent reaches 45mm of the silica gel plate, and taking out the silica gel plate until the sample is half-dried;
fourthly, placing the silica gel plate below the nozzle of the sprayer, unscrewing the valve IV, quickly pressing the plunger of the injector to the bottom end to finish spraying, comparing the silica gel plate with a standard colorimetric plate after 5 seconds, deducting the color band at the bottommost end during comparison, and determining the content of the multi-carbon alcohol.
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| CN202110373419.1A CN113198637B (en) | 2021-04-07 | 2021-04-07 | Spraying device and method for detecting multi-carbon alcohol in methanol gasoline |
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| CN202110373419.1A CN113198637B (en) | 2021-04-07 | 2021-04-07 | Spraying device and method for detecting multi-carbon alcohol in methanol gasoline |
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| CN113198637B CN113198637B (en) | 2022-03-15 |
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2021
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| US20090280031A1 (en) * | 2008-05-07 | 2009-11-12 | Honeywell International Inc. | Methods for use of a sensitive layer for hydrogen sulphide detection with saw/baw devices |
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