CN108008034B - Method for detecting purity of N, N, N' -trimethylethylenediamine by gas chromatography - Google Patents
Method for detecting purity of N, N, N' -trimethylethylenediamine by gas chromatography Download PDFInfo
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Abstract
The invention discloses a method for detecting the purity of N, N, N' -trimethylethylenediamine by adopting a gas chromatography, which adopts DB-624 capillary chromatographic column for detection, adopts a peak area normalization method to calculate the purity, and sets the detection conditions as follows: the injection port temperature is 200-250 ℃, the detection port temperature is 250-300 ℃, the carrier gas is high-purity nitrogen, the fuel gas is hydrogen, the combustion-supporting gas is compressed air, the column flow is 1.0ml/min, split-flow injection is adopted, the split-flow ratio is 50:1, the detector is a hydrogen flame ionization detector, and the column temperature adopts program temperature rise. The gas chromatography detection method is stable, reliable, accurate, high in repeatability and stable in peak-out time and peak value of the material, and the quality of the N, N, N' -trimethylethylenediamine can be well controlled by the detection method.
Description
Technical Field
The invention relates to the technical field of substance purity analysis, in particular to a method for detecting the purity of N, N, N '-trimethylethylenediamine, and more particularly to a method for detecting the purity, unknown single impurities and total impurities of N, N, N' -trimethylethylenediamine by adopting a gas chromatography.
Background
N, N '-trimethylethylenediamine is a main production raw material for tens of products such as 4-chloro-2-methylbenzaldehyde and N- (2-dimethylaminoethyl) -N-methylformamide, and when the content of impurities in N, N' -trimethylethylenediamine is high, the quality of the produced product is affected. Therefore, it is important to establish a stable, reliable and accurate method for detecting the purity of N, N, N' -trimethylethylenediamine.
The gas chromatography detection method has the advantages of high separation efficiency, high analysis speed, small sample consumption, high detection sensitivity, good selectivity and the like, so the method is widely applied to the fields of petrochemical industry, medicine and health, environmental monitoring, biochemistry, food detection and the like.
At present, no report related to the purity detection method of N, N, N '-trimethylethylenediamine is found, and in order to enhance the quality control of N, N, N' -trimethylethylenediamine, it is necessary to establish a stable, reliable and accurate gas chromatography detection method for the purity of N, N, N '-trimethylethylenediamine so as to rapidly analyze the purity, unknown single impurities and total impurities of N, N, N' -trimethylethylenediamine.
Disclosure of Invention
The invention aims to provide a stable, reliable and accurate gas chromatography detection method for the purity of N, N, N ' -trimethylethylenediamine, which is used for rapidly analyzing the purity, unknown single impurities and total impurities of the N, N, N ' -trimethylethylenediamine and provides a simple, accurate, rapid and reliable detection method for the industrial production of the N, N, N ' -trimethylethylenediamine.
The technical scheme adopted by the invention is as follows: a method for detecting the purity of N, N, N' -trimethylethylenediamine by adopting gas chromatography comprises the following steps:
1) setting the working conditions of the instrument: the temperature of the sample inlet is 200-250 ℃, the temperature of the detection port is 250-300 ℃, the carrier gas is high-purity nitrogen, the fuel gas is hydrogen, the combustion-supporting gas is compressed air, the flow rate of the column is 1.0ml/min, and split-flow sample injection is adopted;
2) sample introduction detection: precisely measuring 0.2 μ l of test product N, N, N' -trimethylethylenediamine, injecting into a gas chromatograph, recording the chromatogram, analyzing the chromatogram, and calculating the purity.
Preferably, a micro-sampler can be used for sampling.
The gas chromatography adopts a medium-polarity gas chromatographic column and a hydrogen flame ionization detector for detection, and is qualitative in retention time and quantitative in peak area.
Preferably, when the operating conditions of the apparatus are set in step 1), the column used is a DB-624 capillary column, and the specification of the column is 30m (length) 320 μm (inner diameter) 1.8 μm (packing particle size).
Preferably, the detector used in setting the working condition of the apparatus in step 1) is a hydrogen flame ionization detector. The hydrogen flame ionization detector has the advantages of simple structure, good stability, high sensitivity, quick response and high sensitivity.
Preferably, when the working condition of the instrument is set in the step 1), the column temperature is programmed to rise, the initial temperature is maintained at 48-52 ℃ for 1-3min, then raised to 118-125 ℃ at 18-25 ℃/min, then raised to 152-165 ℃ at 3-8 ℃/min, and maintained for 1-3min, and finally raised to 210-225 ℃ at 3-6 ℃/min.
More preferably, when the working conditions of the instrument are set in the step 1), the column temperature is programmed to rise, the initial temperature is maintained at 50 ℃ for 2min, then the temperature is raised to 120 ℃ at 20 ℃/min, then the temperature is raised to 160 ℃ at 5 ℃/min, the temperature is maintained for 2min, and finally the temperature is raised to 220 ℃ at 5 ℃/min.
Preferably, in the step 1), the split ratio of the split injection is 50: 1.
Preferably, in step 2), the purity is calculated by peak area normalization.
The invention has the beneficial effects that:
the method adopts a gas chromatography detection method to rapidly analyze the purity, unknown single impurities and total impurities of the N, N, N '-trimethylethylenediamine, the gas chromatography detection method is stable, reliable, accurate and high in repeatability, the peak-producing time and the peak value of the material are stable, and the quality of the N, N, N' -trimethylethylenediamine can be well controlled by adopting the detection method.
Drawings
FIG. 1 is a gas phase spectrum of N, N, N' -trimethylethylenediamine detected in example 1;
FIG. 2 is a gas phase diagram of N, N, N' -trimethylethylenediamine detected in example 2;
FIG. 3 is a gas phase diagram of N, N, N' -trimethylethylenediamine detected in example 3.
Detailed Description
Taking 3 batches of N, N, N' -trimethylethylenediamine products produced by the same production specification instruction, detecting according to the detection method described in the embodiment 1-3, and calculating the purity, unknown single impurities and total impurities by adopting an area normalization method.
Example 1
A method for detecting the purity of N, N, N' -trimethylethylenediamine by adopting gas chromatography comprises the following steps:
1) setting the working conditions of the instrument: the temperature of a sample inlet is 200 ℃, the temperature of a detection port is 250 ℃, carrier gas is high-purity nitrogen, fuel gas is hydrogen, combustion-supporting gas is compressed air, the flow rate of a column is 1.0ml/min, split-flow sample injection is adopted, and the split-flow ratio of the split-flow sample injection is 50: 1; wherein, the adopted chromatographic column is a DB-624 chromatographic column, the specification of the chromatographic column is 30m 320 μm 1.8 μm, the adopted detector is a hydrogen flame ionization detector, the temperature of the column is programmed to rise, the initial temperature is kept for 1min at 48 ℃, the initial temperature is kept to rise to 118 ℃ at 18 ℃/min, then rises to 152 ℃ at 3 ℃/min, the initial temperature is kept for 3min, and finally the initial temperature is kept to rise to 210 ℃ at 3 ℃/min;
2) sample introduction detection: precisely measuring 0.2 μ l of test sample N, N, N' -trimethylethylenediamine, injecting into a gas chromatograph, recording the chromatogram, analyzing the chromatogram, and calculating the purity by adopting a peak area normalization method.
The gas phase spectrum of the detected N, N, N '-trimethylethylenediamine is shown in figure 1, and the purity, unknown single impurities and total impurities of the detected N, N, N' -trimethylethylenediamine are shown in table 1.
Example 2
A method for detecting the purity of N, N, N' -trimethylethylenediamine by adopting gas chromatography comprises the following steps:
1) setting the working conditions of the instrument: the temperature of a sample inlet is 220 ℃, the temperature of a detection port is 280 ℃, carrier gas is high-purity nitrogen, fuel gas is hydrogen, combustion-supporting gas is compressed air, the flow rate of a column is 1.0ml/min, split-flow sample injection is adopted, and the split-flow ratio of the split-flow sample injection is 50: 1; wherein, the adopted chromatographic column is a DB-624 chromatographic column, the specification of the chromatographic column is 30m 320 μm 1.8 μm, the adopted detector is a hydrogen flame ionization detector, the temperature of the column is programmed to rise, the initial temperature is maintained at 50 ℃ for 2min, the temperature is raised to 120 ℃ at 20 ℃/min, then raised to 160 ℃ at 5 ℃/min, the temperature is maintained for 2min, and finally the temperature is raised to 220 ℃ at 5 ℃/min;
2) sample introduction detection: precisely measuring 0.2 μ l of test sample N, N, N' -trimethylethylenediamine, injecting into a gas chromatograph, recording the chromatogram, analyzing the chromatogram, and calculating the purity by adopting a peak area normalization method.
The gas phase spectrum of the detected N, N, N '-trimethylethylenediamine is shown in figure 2, and the purity, unknown single impurities and total impurities of the detected N, N, N' -trimethylethylenediamine are shown in table 1.
Example 3
A method for detecting the purity of N, N, N' -trimethylethylenediamine by adopting gas chromatography comprises the following steps:
1) setting the working conditions of the instrument: the temperature of a sample inlet is 250 ℃, the temperature of a detection port is 300 ℃, carrier gas is high-purity nitrogen, fuel gas is hydrogen, combustion-supporting gas is compressed air, the flow rate of a column is 1.0ml/min, split-flow sample injection is adopted, and the split-flow ratio of the split-flow sample injection is 50: 1; wherein, the adopted chromatographic column is a DB-624 chromatographic column, the specification of the chromatographic column is 30m 320 μm 1.8 μm, the adopted detector is a hydrogen flame ionization detector, the temperature of the column is programmed to rise, the initial temperature is 52 ℃ for 2min, the temperature is raised to 125 ℃ at 22 ℃/min, then raised to 162 ℃ at 6 ℃/min, the temperature is maintained for 2min, and finally raised to 225 ℃ at 6 ℃/min;
2) sample introduction detection: precisely measuring 0.2 μ l of test sample N, N, N' -trimethylethylenediamine, injecting into a gas chromatograph, recording the chromatogram, analyzing the chromatogram, and calculating the purity by adopting a peak area normalization method.
The gas phase spectrum of the detected N, N, N '-trimethylethylenediamine is shown in figure 3, and the purity, unknown single impurities and total impurities of the detected N, N, N' -trimethylethylenediamine are shown in Table 1.
TABLE 1 purity, unknown Mono-and Total hetero measured in examples 1-3
| Purity of | Unknown simple impurity | Total miscellaneous | |
| Example 1 | 98.2％ | 0.87％ | 1.8％ |
| Example 2 | 98.1％ | 0.95％ | 1.9％ |
| Example 3 | 98.9％ | 0.72％ | 1.1％ |
The gas chromatography detection method is stable, reliable, accurate and high in repeatability, the peak time and the peak value of the material are stable, the detection can be finished within about 20min, and the quality of the N, N, N' -trimethylethylenediamine can be well controlled by the detection method.
Claims (5)
1. A method for detecting the purity of N, N, N' -trimethylethylenediamine by adopting gas chromatography is characterized by comprising the following steps:
1) setting the working conditions of the instrument: the temperature of the sample inlet is 200-250 ℃, the temperature of the detection port is 250-300 ℃, the carrier gas is high-purity nitrogen, the fuel gas is hydrogen, the combustion-supporting gas is compressed air, the flow rate of the column is 1.0mL/min, and split-flow sample injection is adopted;
2) sample introduction detection: precisely measuring 0.2 mul of test sample N, N, N' -trimethylethylenediamine, injecting into a gas chromatograph, recording the map, analyzing the map, and calculating the purity;
when the working conditions of the instrument are set in the step 1), the adopted chromatographic column is a DB-624 chromatographic column, and the specification of the chromatographic column is 30m x 320 μm x 1.8 μm;
when the working conditions of the instrument are set in the step 1), the column temperature is raised by a program, the initial temperature is kept at 48-52 ℃ for 1-3min, is raised to 118-125 ℃ at 18-25 ℃/min, is raised to 152-165 ℃ at 3-8 ℃/min, is kept for 1-3min, and is finally raised to 210-225 ℃ at 3-6 ℃/min.
2. The method for detecting the purity of N, N, N' -trimethylethylenediamine by gas chromatography as claimed in claim 1, wherein the detector used in the step 1) is a hydrogen flame ionization detector when the operating conditions of the apparatus are set.
3. The method for detecting the purity of N, N, N' -trimethylethylenediamine by gas chromatography as claimed in claim 1, wherein the column temperature is programmed to 50 ℃ for 2min, 20 ℃/min to 120 ℃ for 2min, 5 ℃/min to 160 ℃ for 2min, and 5 ℃/min to 220 ℃ for 5 ℃/min when the working conditions of the apparatus are set in step 1).
4. The method for detecting the purity of N, N, N' -trimethylethylenediamine by using the gas chromatography as claimed in claim 1, wherein the split ratio of the split sample injection in the step 1) is 50: 1.
5. The method for detecting the purity of N, N, N' -trimethylethylenediamine by gas chromatography as claimed in claim 1, wherein in the step 2), the purity is calculated by a peak area normalization method.
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