CN111272896B - Method for detecting content of hexacarboxaldehyde in n-propanol serving as n-propyl acetate raw material - Google Patents
Method for detecting content of hexacarboxaldehyde in n-propanol serving as n-propyl acetate raw material Download PDFInfo
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Abstract
The method for detecting the content of the hexaldehyde in the n-propanol serving as the raw material of the n-propyl acetate comprises the following steps of S1, selecting a chromatographic column; s2, adjusting parameters of a chromatograph; s3, detecting the analytically pure propanol; s4, taking 100ml of analytically pure propanol, dropwise adding 1-2 drops of analytically pure 2-methyl valeraldehyde, shaking up, and detecting; s5, dropwise adding 1-2 drops of analytically pure 2-methyl-2-pentenal into the solution of the S5, shaking up, and detecting the analytically pure 2-methyl-2-pentenal; s6, detecting a correction factor; and S7, taking the n-propanol solution to be detected, detecting the n-propanol solution, and recording the peak area of the hexacarboxaldehyde. The invention finds a chromatographic column and obtains a specific detection method by debugging parameters, and can accurately measure the content of the hexaldehyde in the n-propanol serving as the raw material of the n-propyl acetate; and the detection method is simple and reliable, and the conventional laboratory or factory conditions can meet the test requirements.
Description
Technical Field
The invention belongs to the technical field of impurity content determination, and particularly relates to a method for detecting the content of hexaldehyde in n-propanol serving as an n-propyl acetate raw material.
Background
The n-propyl acetate is generated by esterifying acetic acid and n-propanol, is a colorless transparent liquid, has soft fruit fragrance, presents pear fragrance like the fragrance after being diluted, is mutually soluble with alcohol, ether, ketone and hydrocarbon, and is slightly soluble in water; the product can be used as excellent solvent for paint, ink, nitro lacquer, varnish and various resins, and is also used as colorless transparent liquid with pleasant fruity smell in the industries of essence and perfume. The lower homologues are poorly soluble in water; is mixed and dissolved with organic solvents such as alcohol, ether, ketone and the like, is an excellent organic solvent, and is widely used in industries such as paint, curing agent, polyester resin and the like.
But the n-propyl acetate can generate an off-flavor during the storage process, and the generated off-flavor can influence the original taste of the n-propyl acetate and influence the normal use of the n-propyl acetate, so that the requirement of the customer on the odor of the n-propyl acetate can not be met.
Disclosure of Invention
The inventor finds that the substance generating the peculiar smell is generated by the carbohexaaldehyde in the n-propanol which is a raw material of the n-propyl acetate, the carbohexaaldehyde (2-methylpentanal and 2-methyl-2-pentenal) is generated as a byproduct in the production process of the n-propanol, the carbohexaaldehyde enters an n-propyl acetate production system along with the n-propanol and partially remains in the n-propyl acetate, and an aldehyde functional group in the carbohexaaldehyde plays a determining role in the main chemical property of the carbohexaaldehyde, and under the conditions of no nitrogen protection, higher storage temperature and longer storage time, the carbohexaacid (2-methylpentanic acid and 2-methyl-2-pentenoic acid) is generated through oxidation to generate the peculiar smell of the n-propyl acetate product, so that the peculiar smell influencing normal use of the n-propyl acetate product can be avoided when the content of the 2-methylpentanic acid is less than 10 ppm.
Therefore, in order to control the odor of n-propyl acetate, the content of the carbon hexaldehyde in n-propanol needs to be controlled, and therefore, a method for detecting the content of the carbon hexaldehyde in n-propanol serving as a raw material of n-propyl acetate is continuously sought so as to accurately detect the content of the carbon hexaaldehyde. Finally, a chromatographic column is found and a specific detection method is obtained by adjusting parameters.
Therefore, in order to solve the problem that the normal use of n-propyl acetate cannot meet the requirement of a customer on the smell of n-propyl acetate due to the generation of peculiar smell in the storage process of the n-propyl acetate product, a detection method which starts from the control of the content of the carbon hexaaldehyde in the n-propyl acetate raw material and can accurately determine the content of the carbon hexaaldehyde in the n-propyl acetate raw material is provided, so that the generation of peculiar smell affecting the normal use of the n-propyl acetate product in the storage process is avoided.
The method for detecting the content of the hexaldehyde in the n-propanol serving as the raw material of the n-propyl acetate comprises the following steps:
s1, mounting a chromatographic column, wherein the thickness of the chromatographic column is 28-32m × 300-350 um, and the thickness of the chromatographic column is 0.2-0.3 um;
s2, adjusting parameters during detection of the gas chromatograph, wherein a sample inlet: the temperature is 180-220 ℃, the split ratio is 28; column flow rate: constant current mode 1.5ml/min; a detector: the temperature is 180-220 ℃, the air flow is 330-360 ml/min, the hydrogen flow is 30-40 ml/min, and the tail blowing flow is 20-30 ml/min; temperature rising procedure: keeping the temperature at 420-460 ℃ for 4-6 min, heating the temperature to 145-155 ℃ at the heating rate of 14-16 ℃/min, and keeping the temperature for 4-6 min;
s3, after setting all parameters in the S2, detecting the analytically pure propanol;
s4, taking 100ml of analytically pure propanol, dropwise adding 1-2 drops of analytically pure 2-methyl valeraldehyde, shaking up, and detecting;
s5, dripping 1-2 drops of analytically pure 2-methyl-2-pentenal into the solution of the S5, shaking up and detecting the analytically pure 2-methyl-2-pentenal;
s6, detecting a correction factor;
and S7, taking the n-propanol solution to be detected, detecting the n-propanol solution, and recording the peak area of the hexacarboxaldehyde.
In one embodiment, the chromatographic column is a non-polar chromatographic column and the stationary phase is (5% -phenyl) -methylpolysiloxane.
In one embodiment, after the parameters in S3 are set, the aging of the chromatographic column is further required.
In one embodiment, when the chromatographic column is aged, the chromatographic column is installed, and the chromatographic instrument is adjusted to have the following parameters: the flow rate and constant flow mode of the column is 2.0-2.5ml/min; a sample inlet: the temperature is 230-250 ℃, the flow splitting ratio is 10; the carrier gas is selected from nitrogen; a detector: the temperature is 230-250 ℃, the air flow is 350-400 ml/min, the hydrogen flow is 35-40 ml/min, and the tail blowing flow is 25-30 ml/min; temperature rising procedure: keeping the temperature at 180-200 ℃ for 30-40 min.
In one embodiment, the detection sample amount of the gas chromatograph is 1 to 2ul.
In one embodiment, the carrier gas is a high purity carrier gas.
In one embodiment, the step of detecting the correction factor includes S61, accurately measuring 100xml of analytically pure propanol, and then accurately weighing 1xg each of 2-methylpentanal and 2-methyl-2-pentenal in the analytically pure propanol; s62, shaking up, and diluting step by step according to the sequence of 100 times, 10 times and 2 times; s63, taking the sample 1 (2-methylpentanal 10Xmg/L, 2-methyl-2-pentenal 10 Xmg/L) and the sample 2 (2-methylpentanal 5Xmg/L, 2-methyl-2-pentenal 5 Xmg/L) obtained after dilution, detecting the samples, and repeating the steps for at least 3 times; and S64, taking the peak area average value, and calculating to obtain a correction factor.
The method for detecting the content of the hexacarboxaldehyde in the n-propanol serving as the n-propyl acetate raw material has the beneficial effects that:
1. the invention finds a chromatographic column and obtains a specific detection method by debugging parameters, and can accurately measure the content of the hexaldehyde in the n-propanol serving as the raw material of the n-propyl acetate.
2. The method for detecting the content of the hexacarboxaldehyde in the n-propanol serving as the n-propyl acetate raw material is simple and reliable, and the conventional laboratory or factory conditions can meet the test requirements.
Drawings
FIG. 1 is a chromatogram obtained after detection by the method for detecting the content of the hexaldehyde in the n-propanol which is a raw material of n-propyl acetate.
Detailed Description
The embodiments in the description are only for illustrating the present invention and do not limit the scope of the present invention. The scope of the present invention is defined only by the appended claims, and any omissions, substitutions, or modifications made based on the embodiments disclosed herein will fall within the scope of the present invention.
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
As used herein, the term "consisting of 8230; preparation" is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of 8230comprises" excludes any non-specified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of 8230title" appears in a clause of the subject matter of the claims and not immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or range defined by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when the range "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5"
And the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise.
"optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein in the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes equivalent parts that are acceptable for use in a generic sense without departing from the spirit and scope of the invention. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise numerical value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In the specification, x represents a coefficient, and the value of the coefficient ranges from 1 to 100.
The method for detecting the content of the hexaldehyde in the n-propanol serving as the raw material of the n-propyl acetate comprises the following steps:
s1, mounting a chromatographic column, wherein the thickness of the chromatographic column is 28-32m × 300-350 um, and the thickness of the chromatographic column is 0.2-0.3 um;
s2, adjusting parameters during detection of the gas chromatograph, wherein a sample inlet: the temperature is 180-220 ℃, the split ratio is 28; column flow rate: constant current mode 1.5ml/min; a detector: the temperature is 180-220 ℃, the air flow is 330-360 ml/min, the hydrogen flow is 30-40 ml/min, and the tail blowing flow is 20-30 ml/min; temperature rising procedure: keeping the temperature at 420-460 ℃ for 4-6 min, heating the temperature to 145-155 ℃ at the heating rate of 14-16 ℃/min, and keeping the temperature for 4-6 min;
s3, after setting all parameters in the S2, detecting the analytically pure propanol;
s4, taking 100ml of analytically pure propanol, dropwise adding 1-2 drops of analytically pure 2-methyl valeraldehyde, shaking up, and detecting;
s5, dropwise adding 1-2 drops of analytically pure 2-methyl-2-pentenal into the solution of the S5, shaking up, and detecting the analytically pure 2-methyl-2-pentenal;
s6, detecting a correction factor;
and S7, taking the n-propanol solution to be detected, detecting the n-propanol solution, and recording the peak area of the hexacarboxaldehyde.
Firstly, installing a chromatographic column, then adjusting various parameters of a chromatograph, entering a detection stage, detecting analytically pure propanol to obtain a reference chromatogram, namely a chromatogram 2 in fig. 1, after detection, and observing the peak emergence time of each substance peak; then 100ml of analytically pure propanol is taken, 1-2 drops of analytically pure 2-methyl valeraldehyde are added dropwise, the mixture is shaken up and detected, a sample chromatogram 1 is obtained after detection, the peak-off time of each substance peak is observed, and the peak-off time of the 2-methyl valeraldehyde is marked; and then dropwise adding 1-2 drops of analytically pure 2-methyl-2-pentenal into the solution of S5, shaking uniformly, detecting the solution, detecting to obtain a chromatogram of a sample 2, namely a chromatogram 1 in figure 1, observing the peak-off time of each substance peak, marking the peak-off time of 2-methyl-valeraldehyde and 2-methyl-2-pentenal, wherein A1 is the peak of 2-methyl-valeraldehyde, A2 is the peak of 2-methyl-2-pentenal, obtaining a correction factor by using an external standard method, detecting the to-be-detected liquid of the n-propanol, detecting to obtain the chromatogram of the to-be-detected liquid, namely a chromatogram 3 in figure 1, finding the peaks of 2-methyl-valeraldehyde and 2-methyl-2-pentenal, wherein A1 is the peak of 2-methyl-valeraldehyde, and A2 is the peak of 2-methyl-2-pentenal, recording the peak area, and then calculating. It should be noted that the calibration factor obtained by the external standard method in the invention is single-point calibration, the obtained calibration factor is input into a computer, and then the liquid to be detected is continuously detected on the basis; the spacer purging is to blow a gas flow transversely under the spacer of the sample inlet, and aims to blow volatile matters of the spacer at high temperature out as much as possible and vent the volatile matters from the spacer purging outlet so as to prevent the volatile matters of the spacer from entering the chromatographic column.
The invention finds a chromatographic column and obtains a specific detection method by debugging parameters, and can accurately measure the content of the hexaldehyde in the n-propanol serving as the raw material of the n-propyl acetate; and the detection method is simple and reliable, and the conventional laboratory or factory conditions can meet the test requirements.
The chromatographic column is a nonpolar chromatographic column, and the stationary phase is (5% -phenyl) -methyl polysiloxane.
The chromatographic column has the specification of 28-32mx 300-350 um, the film thickness of 0.2-0.3 um and (5% -phenyl) -methyl polysiloxane, has extremely low loss of the chromatographic column, is an ideal chromatographic column for GC, has excellent inertia to active compounds, including acidic and alkaline compounds, improves the signal-to-noise ratio, has higher sensitivity and mass spectrum integrity, is bonded and crosslinked, and can be cleaned by a solvent.
Thus, the content of the carbon hexaldehyde in the n-propanol can be accurately measured, so that the problem that the normal use of the n-propyl acetate product is influenced in the storage process is avoided.
And after the parameters in the S3 are set, aging of the chromatographic column is required.
The effect of aging is to remove residual solvent and make the stationary liquid film more uniform and the baseline more stable.
In this way, it is further ensured that the amount of the hexaldehyde in the n-propanol is accurately measured to avoid the generation of an off-flavor in the n-propyl acetate product during storage that would interfere with normal use.
When the chromatographic column is aged, the chromatographic column is well installed, and the parameters of the chromatograph are adjusted as follows: the flow rate and constant flow mode of the column is 2.0-2.5ml/min; a sample inlet: the temperature is 230-250 ℃, the flow division ratio is 10-1, and the shock insulator is purged for 6-10 ml/min; the carrier gas is selected from any one of hydrogen, nitrogen, helium and argon; a detector: the temperature is 230-250 ℃, the air flow is 350-400 ml/min, the hydrogen flow is 35-40 ml/min, and the tail blowing flow is 25-30 ml/min; temperature rising procedure: keeping the temperature at 180-200 ℃ for 30-40 min.
The setting of each parameter mainly depends on the requirement on sensitivity and the acceptable loss degree of an operator, under the aging condition, the obtained loss curve smoothly rises along with the rise of temperature without obvious mixed peaks, and the loss curve is a chromatogram obtained by running temperature programming without sample injection.
This ensures that residual solvent can be removed and that the stationary liquid film is more uniform and the baseline is more even.
The detection sample amount of the gas chromatograph is 1-2 ul.
In gas chromatograph analysis, various sample introduction systems are required because of differences in sample state, sample composition, sample performance, sample content, chromatographic column, analysis purpose, analysis requirements, and the like. The structure of the sample introduction system, the material of the sample introduction system, the sample introduction method, the temperature during sample introduction, the sample introduction time, the sample introduction amount, the sample introduction tool, the accuracy and the repeatability of sample introduction and the like can directly influence the qualitative and quantitative results of the gas chromatograph, and the sample introduction system is one of the main sources of errors in the analysis of the gas chromatograph, and influences the separation effect of the chromatograph and the accuracy and the repeatability of the analysis result according to the quantity of the sample introduction, the length of the sample introduction time, the gasification speed of the sample and the like. And the detection sample amount is 1-2 ul, so that the requirements on the separation effect and the accuracy and the repeatability of the analysis result can be met.
Thus, the content of the carbon hexaldehyde in the n-propanol can be accurately measured, so that the problem that the normal use of the n-propyl acetate product is influenced in the storage process is avoided.
The carrier gas is high-purity carrier gas.
The purity requirements of the carrier gas depend primarily on the requirements of the chromatography column, the detector and the sample being analyzed. The purity requirement of the carrier gas in the invention is very high, the carrier gas needs to enter a gas chromatographic system after purification, pressure stabilization, flow control and measurement, the high-purity nitrogen is inert gas, and the high-purity nitrogen has the advantages of small diffusion coefficient, large relative molecular mass, relatively high column efficiency, safety and low price.
In this way, a better separation of the substances to be detected is ensured and the accuracy of the detection is improved.
The step of detecting the correction factors comprises S61, accurately measuring 100xml of analytically pure propanol, and then accurately weighing 1xg of 2-methylpentanal and 2-methyl-2-pentenal respectively in the analytically pure propanol; s62, shaking up, and diluting step by step according to the sequence of 100 times, 10 times and 2 times; s63, taking the sample 1 (2-methylpentanal 10Xmg/L, 2-methyl-2-pentenal 10 Xmg/L) and the sample 2 (2-methylpentanal 5Xmg/L, 2-methyl-2-pentenal 5 Xmg/L) obtained after dilution, detecting the samples, and repeating the steps for at least 3 times; and S64, taking the peak area average value, and calculating to obtain a correction factor.
The function of the correction factor is to reflect the relationship between the object to be measured and the response of the detector, and the calculation formula of the correction factor is as follows: correction factor = sample concentration ÷ sample peak area, the carbon hexaaldehyde content is calculated as: and C = f multiplied by A (C is the content of the carbon hexaldehyde, f is a correction factor, and A is the peak area of the carbon hexaldehyde), and the content of the carbon hexaldehyde can be more accurately measured by performing calibration.
Therefore, the measured experimental value can be more accurate and is closer to the true value.
Some specific examples are listed below, but it should be noted that the following examples are not exhaustive of all possible cases. And the materials used in the following examples are commercially available unless otherwise specified.
Example 1
Detecting a correction factor, comprising the steps of:
s61, accurately measuring 100ml of analytically pure propanol, and then accurately weighing 1g of 2-methylpentanal and 1g of 2-methyl-2-pentenal in the analytically pure propanol respectively;
s62, shaking up, and diluting step by step according to the sequence of 100 times, 10 times and 2 times;
s63, taking the sample 1 (10 mg/L of 2-methylpentanal, 10mg/L of 2-methyl-2-pentenal) and the sample 2 (5 xmg/L of 2-methylpentanal, 5xmg/L of 2-methyl-2-pentenal) obtained after dilution, detecting the samples, and repeating the steps for at least 3 times;
and S64, taking the peak area average value, and calculating to obtain a correction factor.
Example 2
Aging of the chromatographic column: the chromatographic column is installed, but not connected with the detector, and the parameters of the chromatograph are adjusted as follows: the flow rate and constant flow mode of the column is 2.2ml/min; a sample inlet: the temperature is 240 ℃, the split ratio is 12, and the isolation pad purging is 8ml/min; the carrier gas is selected from nitrogen; a detector: the temperature is 240 ℃, the air flow is 380ml/min, the hydrogen flow is 38ml/min, and the tail blowing flow is 28ml/min; temperature rising procedure: keeping the temperature at 190 ℃ for 35min.
Example 3
The method for detecting the content of the hexaldehyde in the n-propanol serving as the raw material of the n-propyl acetate comprises the following steps:
s1, selecting a chromatographic column 28-32m, 300-350 um, and a film thickness of 0.2-0.3 um, (5% -phenyl) -methyl polysiloxane; the column was aged as in example 2;
s2, continuously adjusting parameters during detection of the gas chromatograph, wherein a sample inlet: the temperature is 200 ℃, the flow distribution ratio is 30; column flow rate: constant current mode 1.5ml/min; a detector: the temperature is 200 ℃, the air flow is 350ml/min, the hydrogen flow is 35ml/min, and the tail blowing flow is 25ml/min; temperature rising procedure: keeping the temperature at 45 ℃ for 6min, increasing the temperature at the rate of 15 ℃/min to 150 ℃, and keeping the temperature for 10min;
s3, after setting all parameters in the S2, detecting the analytically pure propanol;
s4, taking 100ml of analytically pure propanol, dropwise adding 1 drop of analytically pure 2-methyl valeraldehyde, shaking up, and detecting;
s5, dropwise adding 1 drop of analytically pure 2-methyl-2-pentenal into the solution of the S5, shaking up, and detecting the analytically pure 2-methyl-2-pentenal;
s6, detecting a correction factor according to the embodiment 1;
and S7, taking the n-propanol solution to be detected, detecting the n-propanol solution, and recording the peak area of the hexacarboxaldehyde.
Example 4
The method for detecting the content of the hexaldehyde in the n-propanol serving as the raw material of the n-propyl acetate comprises the following steps of:
s1, selecting a chromatographic column of 28-32m, 300-350 um, and a film thickness of 0.2-0.3 um, (5% -phenyl) -methyl polysiloxane; the column was aged as in example 2;
s2, continuously adjusting parameters during detection of the gas chromatograph, wherein a sample inlet: the temperature is 210 ℃, the split ratio is 35, the spacer is used for purging 4ml/min, and the carrier gas is selected from nitrogen; column flow rate: constant current mode 1.8ml/min; a detector: the temperature is 210 ℃, the air flow is 380ml/min, the hydrogen flow is 38ml/min, and the tail blowing flow is 28ml/min; temperature rising procedure: keeping the temperature at 48 ℃ for 6min, increasing the temperature at the rate of 18 ℃/min to 160 ℃, and keeping the temperature for 8min;
s3, after setting all parameters in the S2, detecting the analytically pure propanol;
s4, taking 100ml of analytically pure propanol, dropwise adding 2 drops of analytically pure 2-methyl valeraldehyde, shaking up, and detecting;
s5, dropwise adding 2 drops of analytically pure 2-methyl-2-pentenal into the solution of the S5, and detecting the analytically pure 2-methyl-2-pentenal after shaking up;
s6, detecting a correction factor according to the embodiment 1;
and S7, taking the n-propanol solution to be detected, detecting the n-propanol solution, and recording the peak area of the hexacarboxaldehyde.
Example 5
The method for detecting the content of the hexaldehyde in the n-propanol serving as the raw material of the n-propyl acetate comprises the following steps:
s1, selecting a chromatographic column of 28-32m, 300-350 um, and a film thickness of 0.2-0.3 um, (5% -phenyl) -methyl polysiloxane; the column was aged as in example 2;
s2, continuously adjusting parameters during detection of the gas chromatograph, wherein a sample inlet: the temperature is 220 ℃, the flow distribution ratio is 40; column flow rate: constant current mode 2.0ml/min; a detector: the temperature is 220 ℃, the air flow is 400ml/min, the hydrogen flow is 40ml/min, and the tail blowing flow is 30ml/min; temperature rising procedure: keeping the temperature at 50 ℃ for 5min, heating the temperature to 160 ℃ at the heating rate of 20 ℃/min, and keeping the temperature for 5min;
s3, after setting all parameters in the S2, detecting the analytically pure propanol;
s4, taking 200ml of analytically pure propanol, dropwise adding 3 drops of analytically pure 2-methyl valeraldehyde, shaking up, and detecting;
s5, dropwise adding 3 drops of analytically pure 2-methyl-2-pentenal into the solution of the S5, shaking up, and detecting the analytically pure 2-methyl-2-pentenal;
s6, detecting a correction factor according to the embodiment 1;
and S7, taking the n-propanol solution to be detected, detecting the n-propanol solution, and recording the peak area of the hexacarboxaldehyde.
The following are the results of the recording and calculation of examples 3 to 5, and the specific results are shown in Table 1:
TABLE 1
It should be noted that the concentrations of 2-methylpentanal and 2-methyl-2-pentenal in the sample to be tested are 10.00mg/L, 5.00mg/L and 3.00mg/L, respectively, f1 is the correction factor (average value) of 2-methylpentanal, f2 is the correction factor (average value) of 2-methyl-2-pentenal, A1 is the peak area of 2-methylpentanal, A2 is the peak area of 2-methyl-2-pentenal, C1 is the concentration of 2-methylpentanal, and C2 is the concentration of 2-methyl-2-pentenal.
The results show that the difference between the concentration of the carbon hexaldehyde obtained by the detection result and the actual concentration of the carbon hexaldehyde is almost the same, which indicates that the content of the carbon hexaldehyde can be accurately detected by adopting the method for detecting the content of the carbon hexaldehyde in the n-propanol serving as the n-propyl acetate raw material, so that the peculiar smell influencing normal use of the n-propyl acetate product in the storage process is avoided.
The technical features of the above embodiments can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, but should be considered as the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above embodiments are described in more detail and specifically, but should not be construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (6)
1. A method for detecting the content of hexacarboxaldehyde in n-propanol serving as a raw material of n-propyl acetate is characterized by comprising the following steps:
s1, installing a chromatographic column, wherein the thickness of the chromatographic column is 28 to 32mx 300 to 350 mu m, and the thickness of the chromatographic column is 0.2 to 0.3 mu m;
s2, adjusting parameters during detection of the gas chromatograph, wherein a sample inlet: the temperature is 200 to 220 ℃, the split ratio is 30 to 1, the cushion blowing is carried out for 3 to 5ml/min, and the carrier gas is selected from nitrogen gas; column flow rate: constant current mode is 1.5 to 2.0ml/min; a detector: the temperature is 200 to 220 ℃, the air flow is 350 to 400ml/min, the hydrogen flow is 35 to 40ml/min, and the tail blowing flow is 25 to 30ml/min; temperature rising procedure: keeping the temperature at 45-50 ℃ for 5-6 min, heating the temperature to 150-160 ℃ at the heating rate of 15-20 ℃/min, and keeping the temperature for 5-10 min;
s3, after setting all parameters in the S2, detecting the analytically pure propanol;
s4, taking 100ml of analytically pure propanol, dropwise adding 1-2 drops of analytically pure 2-methyl valeraldehyde, shaking up, and detecting;
s5, dripping 1-2 drops of analytically pure 2-methyl-2-pentenal into the solution of the S5, shaking up and detecting the analytically pure 2-methyl-2-pentenal;
s6, detecting a correction factor;
s7, taking the n-propanol solution to be detected, detecting the n-propanol solution, and recording the peak area of the hexacarboxaldehyde;
wherein the chromatographic column is a nonpolar chromatographic column, and the stationary phase is (5% -phenyl) -methyl polysiloxane.
2. The method for detecting the content of the hexaldehyde in the n-propanol as a raw material of n-propyl acetate according to claim 1, wherein after the parameters in S3 are set, the aging of the chromatographic column is further required.
3. The method for detecting the content of the hexaldehyde in the n-propanol which is a raw material of n-propyl acetate according to claim 2, wherein when the chromatographic column is aged, the chromatographic column is installed, and the parameters of the chromatographic instrument are adjusted as follows: the flow rate and constant flow mode of the column is 2.0-2.5ml/min; a sample inlet: the temperature is 230 to 250 ℃, the split ratio is 10; the carrier gas is selected from nitrogen; a detector: the temperature is 230 to 250 ℃, the air flow is 350 to 400ml/min, the hydrogen flow is 35 to 40ml/min, and the tail blowing flow is 25 to 30ml/min; temperature rising procedure: keeping the temperature at 180 to 200 ℃ for 30 to 40min.
4. The method for detecting the content of the hexaldehyde in the n-propanol serving as a raw material of n-propyl acetate according to claim 1, wherein the detection sample size of the gas chromatograph is 1 to 2 μ l.
5. The method for detecting the content of the hexaldehyde in the n-propanol which is a raw material of n-propyl acetate according to claim 1, wherein the carrier gas is a high-purity carrier gas.
6. The method for detecting the content of hexanal in n-propanol, which is a raw material of n-propyl acetate, according to claim 1, wherein the step of detecting the correction factor comprises the steps of:
s61, accurately measuring 100ml of analytically pure propanol, and accurately weighing 1g of 2-methylpentanal and 1g of 2-methyl-2-pentenal in the analytically pure propanol respectively;
s62, shaking up, and diluting step by step according to the sequence of 100 times, 10 times and 2 times;
s63, taking a sample 1 and a sample 2 obtained after dilution, wherein the sample 1 comprises 10mg/L of 2-methylpentanal and 10mg/L of 2-methyl-2-pentenal, and the sample 2 comprises 5mg/L of 2-methylpentanal and 5mg/L of 2-methyl-2-pentenal, detecting the samples, and repeating the steps for at least 3 times;
and S64, taking the peak area average value, and calculating to obtain a correction factor.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1015911A (en) * | 1962-07-09 | 1966-01-05 | Union Carbide Corp | 2,3-dimethyl-4-pentenal |
| CN104011218A (en) * | 2011-07-21 | 2014-08-27 | 帝斯曼知识产权资产管理有限公司 | Microbial oils enriched in polyunsaturated fatty acids |
| CN109991113A (en) * | 2019-03-12 | 2019-07-09 | 泰兴金江化学工业有限公司 | Rapid detection method for quality of n-butyl acetate |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| GB2563524B (en) * | 2016-03-28 | 2021-09-01 | Procter & Gamble | Long lasting and stable freshening compositions and methods of freshening the air |
-
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1015911A (en) * | 1962-07-09 | 1966-01-05 | Union Carbide Corp | 2,3-dimethyl-4-pentenal |
| CN104011218A (en) * | 2011-07-21 | 2014-08-27 | 帝斯曼知识产权资产管理有限公司 | Microbial oils enriched in polyunsaturated fatty acids |
| CN109991113A (en) * | 2019-03-12 | 2019-07-09 | 泰兴金江化学工业有限公司 | Rapid detection method for quality of n-butyl acetate |
Non-Patent Citations (3)
| Title |
|---|
| Tharun Jose等.Amino functionalized chitosan as a catalyst for selective solvent-free self-condensation of linear aldehydes.《Journal of Molecular Catalysis A: Chemical》.2010,第333卷 * |
| Trung T. Pham等.Hydrogenation and Hydrodeoxygenation of 2-methyl-2-pentenal on supported metal catalysts.《Journal of Catalysis》.2009,第266卷 * |
| 静玮 等.澳洲坚果焙烤过程中挥发性成分的特征分析.《热带作物学报》.2016,第37卷(第6期), * |
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