A method for the gas phase detection of 3-amino-4'-nitrodiphenyl ether

Abstract

The present application relates to the technical field of chemical analysis, in particular to a gas phase detection method of 3-amino-4'-nitro diphenyl ether, characterized in that the detection method comprises the following steps: S1, preparation of standard solution: taking 3-amino-4'-nitro diphenyl ether standard product, and preparing a series of standard solutions with different concentrations by using acetonitrile; sample solution preparation: taking 3-amino-4'-nitro diphenyl ether sample, and preparing sample solution by using solvent acetonitrile; S2, gas chromatography detection of standard solution and sample solution according to the following gas chromatography conditions: detector: hydrogen flame ionization detector; chromatographic column: high-temperature chromatographic column; column temperature: programmed temperature; injection port temperature: 280-300 DEG C; detector temperature: 300-310 DEG C; split ratio: (80-100):1. The detection method has the advantages of smooth baseline, no tailing, good peak shape, low instrument operation cost, simple and convenient detection process, and good repeatability.

Description

Technical Field

[0001] This invention relates to a gas-phase detection method for 3-amino-4'-nitrodiphenyl ether, belonging to the field of chemical analysis technology. Background Technology

[0002] 3-Amino-4'-nitrodiphenyl ether is an important organic synthetic intermediate with wide applications in the chemical and related industries. This compound appears as a pale yellow crystalline powder, sparingly soluble in water but soluble in many common organic solvents. Its chemical structure combines amino and nitro-substituted diphenyl ether skeletons, thus exhibiting good modifying activity and functionality in reactions. The structural formula of 3-amino-4'-nitrodiphenyl ether is: .

[0003] As a versatile intermediate, 3-amino-4'-nitrodiphenyl ether is frequently used in polymer synthesis processes, particularly in the preparation of certain diphenyl ether herbicides, high-performance dyes, and functional material monomers, where it can serve as a key precursor or structural unit. The amino and nitro groups introduced into its molecule provide important reaction sites for subsequent functional group transformations and polymerization reactions.

[0004] In the synthesis of 3,4'-dinitrodiphenyl ether, 3-amino-4'-nitrodiphenyl ether is an important intermediate. For example, in the preparation method of 3,4'-dinitrodiphenyl ether disclosed in patent application CN118791390A, 3-amino-4'-nitrodiphenyl ether is the key intermediate. Quality control of 3-amino-4'-nitrodiphenyl ether is crucial for its synthesis. Currently, a systematic method for rapid and intuitive chromatographic monitoring of this intermediate is lacking. Furthermore, because this compound is easily decomposed under high temperature and light, samples in the reaction system often cannot be accurately determined directly by conventional gas chromatography. Therefore, developing a gas chromatographic detection method suitable for this compound to achieve rapid, accurate, and efficient analysis of its content has become a critical issue urgently needing to be addressed by those skilled in the art. Summary of the Invention

[0005] To address the shortcomings of existing technologies, this invention provides a gas-phase detection method for 3-amino-4'-nitrodiphenyl ether. The detection method features a stable baseline, no tailing, good peak shape, low instrument operating cost, simple and convenient detection process, and good repeatability.

[0006] The technical solution of this invention to solve the above-mentioned technical problems is as follows: a gas-phase detection method for 3-amino-4'-nitrodiphenyl ether, wherein the detection method is as follows:

[0007] S1. Preparation of standard solutions and sample solutions:

[0008] Preparation of standard solutions: Take 3-amino-4'-nitrodiphenyl ether standard and prepare a series of standard solutions of different concentrations with acetonitrile;

[0009] Sample solution preparation: Take the 3-amino-4'-nitrodiphenyl ether sample and prepare a sample solution using acetonitrile as the solvent;

[0010] S2. Standard solutions and sample solutions were subjected to gas chromatographic detection under the following gas chromatographic conditions:

[0011] Detector: Hydrogen flame ionization detector;

[0012] Chromatographic column: High-temperature chromatographic column;

[0013] Column temperature: programmed temperature rise;

[0014] Inlet temperature: 280℃-300℃;

[0015] Detector temperature: 300℃-310℃;

[0016] Split ratio: (80-100):1.

[0017] Furthermore, the concentration of 3-amino-4'-nitrodiphenyl ether in the sample solution is 4.5-5.5 mg / mL.

[0018] Furthermore, the chromatographic column is an HP-5 with dimensions of 30m × 320μm × 0.25μm.

[0019] Furthermore, the column temperature conditions for the programmed temperature rise are: 210℃-240℃ for 8min-12min, then increase the temperature to 260℃-300℃ at a rate of 15℃ / min-25℃ / min and hold for 6min-10min.

[0020] Preferably, the column temperature conditions for programmed temperature rise are: 230°C for 8 minutes, then increased to 280°C at a rate of 20°C / min and held for 8 minutes.

[0021] Furthermore, the carrier gas for gas chromatography detection is nitrogen, and the flow rate is 0.8 mL / min-1.2 mL / min.

[0022] Furthermore, the injection volume during the detection process is 0.8-1.2 μL.

[0023] Preferably, the injection port temperature is 300℃ and the detector temperature is 310℃.

[0024] Preferably, the injection volume is 1.0 μL and the split ratio is 100:1.

[0025] Furthermore, when preparing the standard solutions, the concentrations of the series of standard solutions with different concentrations are 60±1 mg / mL, 50±1 mg / mL, 20±1 mg / mL, 10±1 mg / mL, 5±0.5 mg / mL, 2±0.5 mg / mL, and 1±0.5 mg / mL.

[0026] The beneficial effects of this invention are:

[0027] The gas chromatography detection method for 3-amino-4'-nitrodiphenyl ether described in this invention, by selecting a suitable chromatographic column and combining it with specific gas chromatography conditions such as programmed temperature rise, injection port temperature, and split ratio, enables accurate quantitative detection of the purity of 3-amino-4'-nitrodiphenyl ether. This method is more conducive to truly reflecting the quality of 3-amino-4'-nitrodiphenyl ether purity and is of great significance for controlling and improving the quality of 3-amino-4'-nitrodiphenyl ether products.

[0028] The gas-phase detection method for 3-amino-4'-nitrodiphenyl ether provided by this invention has been validated by methodology and shows high specificity, accuracy, sensitivity, repeatability, and stability. It is also simple to operate and can achieve qualitative and quantitative analysis of the purity of 3-amino-4'-nitrodiphenyl ether in a single detection. This fills the gap in existing technologies that cannot accurately detect the purity of 3-amino-4'-nitrodiphenyl ether, facilitating quality control of its purity and reducing quality risks associated with its purity. Therefore, this method has high potential for widespread application.

[0029] The gas chromatography detection method for 3-amino-4'-nitrodiphenyl ether described in this invention provides suitable detection conditions that result in good peak shapes for 3-amino-4'-nitrodiphenyl ether and its impurities, and improve the separation between the main component and the impurities. Automatic injection ensures accurate sample volume, and programmed heating and a suitable carrier gas flow rate enable effective separation of the components. Samples can be detected in approximately 20.5 minutes. Content analysis is performed based on peak area results. This method can rapidly, accurately, and efficiently determine the content of 3-amino-4'-nitrodiphenyl ether, with a stable baseline, no tailing, good peak shape, low instrument operating costs, a simple and convenient detection process, and good repeatability. Attached Figure Description

[0030] Figure 1 The gas chromatogram of the 3-amino-4'-nitrodiphenyl ether standard solution in Example 1;

[0031] Figure 2 for Figure 1 Enlarged image;

[0032] Figure 3The gas chromatogram of the 3-amino-4'-nitrodiphenyl ether sample solution in Example 1;

[0033] Figure 4 for Figure 3 Enlarged image;

[0034] Figure 5 The standard curve is for the standard solution of 3-amino-4'-nitrodiphenyl ether. Detailed Implementation

[0035] The specific embodiments of the present invention will be described in detail below. The present invention can be implemented in many other ways different from those described herein, and those skilled in the art can make similar modifications without departing from the spirit of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed.

[0036] Unless otherwise defined, 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 pertains. The terminology used is for describing particular embodiments only and is not intended to limit the invention.

[0037] A gas-phase detection method for 3-amino-4'-nitrodiphenyl ether, wherein the detection method is as follows:

[0038] S1. Preparation of standard solutions and sample solutions:

[0039] Preparation of standard solutions: Take 3-amino-4'-nitrodiphenyl ether standard and prepare a series of standard solutions of different concentrations with acetonitrile;

[0040] Sample solution preparation: Take the 3-amino-4'-nitrodiphenyl ether sample and prepare a sample solution using acetonitrile as the solvent;

[0041] S2. Standard solutions and sample solutions were subjected to gas chromatographic detection under the following gas chromatographic conditions:

[0042] Detector: Flame Ionization (FID) detector;

[0043] Chromatographic column: High-temperature chromatographic column;

[0044] Column temperature: programmed temperature rise;

[0045] Inlet temperature: 280℃-300℃;

[0046] Detector temperature: 300℃-310℃;

[0047] Split ratio: (80-100):1.

[0048] Specifically, the concentration of 3-amino-4'-nitrodiphenyl ether in the sample solution is 4.5-5.5 mg / mL.

[0049] Preferably, the concentration of 3-amino-4'-nitrodiphenyl ether in the sample solution is 5.0 mg / mL.

[0050] Preferably, the chromatographic column is an Agilent HP-5 with dimensions of 30m × 320μm × 0.25μm.

[0051] Specifically, the column temperature conditions for programmed temperature rise are: 210℃-240℃ for 8min-12min, then increase the temperature to 260℃-300℃ at a rate of 15℃ / min-25℃ / min and hold for 6min-10min.

[0052] Preferably, the column temperature conditions for programmed temperature rise are: 230°C for 8 minutes, then increased to 280°C at a rate of 20°C / min and held for 8 minutes.

[0053] Specifically, the carrier gas for gas chromatography detection is nitrogen, and the flow rate is 0.8 mL / min-1.2 mL / min.

[0054] Preferably, the carrier gas for gas chromatography detection is nitrogen, and the flow rate is 1.0 mL / min.

[0055] Specifically, the injection volume for the detection process is 0.8-1.2 μL.

[0056] Preferably, the injection port temperature is 300℃ and the detector temperature is 310℃.

[0057] Preferably, the injection volume is 1.0 μL and the split ratio is 100:1.

[0058] Specifically, when preparing standard solutions, the concentrations of the series of standard solutions with different concentrations are 60±1 mg / mL, 50±1 mg / mL, 20±1 mg / mL, 10±1 mg / mL, 5±0.5 mg / mL, 2±0.5 mg / mL, and 1±0.5 mg / mL.

[0059] Preferably, when preparing the standard solutions, the concentrations of the series of standard solutions of different concentrations are 60 mg / mL, 50 mg / mL, 20 mg / mL, 10 mg / mL, 5 mg / mL, 2 mg / mL, and 1 mg / mL.

[0060] Example 1

[0061] A gas-phase detection method for 3-amino-4'-nitrodiphenyl ether is described below:

[0062] (1) The gas chromatography detection conditions are set as follows:

[0063] Detector: Flame Ionization (FID) detector;

[0064] Chromatographic column: HP-5, 30m × 320μm × 0.25μm;

[0065] Column temperature: 230℃ for 10 min, then increase to 280℃ at a rate of 20℃ / min and hold for 8 min;

[0066] Inlet temperature: 300℃;

[0067] Detector temperature: 310℃;

[0068] Carrier gas: High-purity nitrogen (99.99% purity), flow rate 1 mL / min;

[0069] Flow split ratio: 100:1;

[0070] Injection volume: 1.0 μL;

[0071] Take 1 mL of standard solution and 1 mL of sample solution and place them into 2.0 mL gas chromatograph sample vials for injection and detection.

[0072] (2) Solution preparation:

[0073] Blank solvent: acetonitrile.

[0074] Standard solution: Accurately weigh 5.0 g of 3-amino-4'-nitrodiphenyl ether standard, accurate to 0.0001 g, dissolve in acetonitrile, and dilute to 100 mL. The concentration of the standard solution at this point is 50 g / L. Serially dilute the standard solutions to obtain concentrations of 60 mg / mL, 50 mg / mL, 20 mg / mL, 10 mg / mL, 5 mg / mL, 2 mg / mL, and 1 mg / mL.

[0075] (3) Plotting the standard curve:

[0076] Based on the peak area of ​​the standard solution of 3-amino-4'-nitrodiphenyl ether under the above chromatographic conditions, the linear regression equation was obtained: y = 151.25x - 3.372, with a linear correlation coefficient of R² = 0.9999. Relevant data are shown in Table 1 and... Figure 5 As shown. The gas chromatogram of the 50 mg / mL standard solution is shown below. Figure 1 and Figure 2 As shown in Table 2, the specific test data is as follows.

[0077] Table 1 Test data of standard solutions

[0078]

[0079] Table 2 Gas chromatographic detection data of standard solutions

[0080]

[0081] The elution times of 3-amino-4'-nitrodiphenyl ether in the standard solution and sample solution in this embodiment are shown in Table 3.

[0082] Table 3 Peak Time

[0083]

[0084] (4) Sample testing:

[0085] Preparation of the test sample solution: Accurately weigh 5.0 g of the 3-amino-4'-nitrodiphenyl ether test sample, accurate to 0.0001 g, dissolve it in acetonitrile, and dilute it to a 100 mL volumetric flask.

[0086] The sample solution was injected and tested three times under the above chromatographic conditions. The peak area of ​​3-amino-4'-nitrodiphenyl ether was recorded and the average value was taken. The content of 3-amino-4'-nitrodiphenyl ether in the sample solution was calculated by substituting the average value into the standard curve formula. As shown in Table 4, the gas phase detection data of the sample solution is shown in Table 5.

[0087] Table 4 Results of Calculation of Sample Solution Content Using Standard Curve Formula

[0088]

[0089] Table 5 Gas chromatographic detection data of the sample solution to be tested

[0090]

[0091] Example 2

[0092] Methodological validation:

[0093] (1) Stability test:

[0094] Standard solution and sample solution were taken and placed at room temperature. Samples were taken at 0h, 12h and 24h for testing. Stability was investigated according to the testing conditions of Example 1. The results are shown in Table 6 below.

[0095] Table 6 Stability Test

[0096]

[0097] The above results demonstrate that the reference solution and the test solution exhibit good stability when left at room temperature for 24 hours.

[0098] (2) Precision test

[0099] The reference solution was prepared according to the method in Example 1. The reference solution was injected continuously for 6 injections under the detection conditions in Example 1, and the peak area was recorded. The results are shown in Table 7.

[0100] Table 7 Precision Test

[0101]

[0102] The above results demonstrate that with six consecutive injections, the peak area RSD of 3-amino-4'-nitrodiphenyl ether in the standard solution was 0.672%, indicating good precision.

[0103] Example 2

[0104] A gas-phase detection method for 3-amino-4'-nitrodiphenyl ether is described below:

[0105] (1) The gas chromatography detection conditions are set as follows:

[0106] Detector: Flame Ionization (FID) detector;

[0107] Chromatographic column: HP-5, 30m × 320μm × 0.25μm;

[0108] Column temperature: 210℃ for 12 min, then increase to 260℃ at a rate of 15℃ / min and hold for 10 min;

[0109] Inlet temperature: 280℃;

[0110] Detector temperature: 300℃;

[0111] Carrier gas: High-purity nitrogen (99.99% purity), flow rate 0.8 mL / min;

[0112] Flow split ratio: 80:1;

[0113] Injection volume: 1.0 μL.

[0114] (3) Preparation of the sample solution to be tested:

[0115] Accurately weigh 4.5 g of the 3-amino-4'-nitrodiphenyl ether sample to be tested, accurate to 0.0001 g, dissolve it in acetonitrile, and dilute it to a 100 mL volumetric flask.

[0116] The sample solution to be tested was injected into a gas chromatograph for detection. The peaks in the spectrum were well shaped, and the separation between the main component and the impurities was good.

[0117] Example 3

[0118] A gas-phase detection method for 3-amino-4'-nitrodiphenyl ether is described below:

[0119] (1) The gas chromatography detection conditions are set as follows:

[0120] Detector: Flame Ionization (FID) detector;

[0121] Chromatographic column: HP-5, 30m × 320μm × 0.25μm;

[0122] Column temperature: 240℃ for 8 min, then increase to 300℃ at a rate of 25℃ / min and hold for 6 min;

[0123] Inlet temperature: 290℃;

[0124] Detector temperature: 305℃;

[0125] Carrier gas: High-purity nitrogen (99.99% purity), flow rate 1.2 mL / min;

[0126] Flow split ratio: 90:1;

[0127] Injection volume: 1.0 μL.

[0128] (2) Preparation of the sample solution to be tested:

[0129] Accurately weigh 5.5 g of the 3-amino-4'-nitrodiphenyl ether sample to be tested, accurate to 0.0001 g, dissolve it in acetonitrile, and dilute it to a 100 mL volumetric flask.

[0130] The sample solution to be tested was injected into a gas chromatograph for detection. The peaks in the spectrum were well shaped, and the separation between the main component and the impurities was good.

[0131] Comparative Example 1

[0132] In Comparative Example 1, the gas chromatographic conditions for the gas chromatography detection of 3-amino-4'-nitrodiphenyl ether were the same as in Example 1, except that the split ratio was reduced (60:1). The specific process is as follows:

[0133] (1) The gas chromatography detection conditions are set as follows:

[0134] Detector: Flame Ionization (FID) detector;

[0135] Chromatographic column: HP-5, 30m × 320μm × 0.25μm;

[0136] Column temperature: 230℃ for 10 min, then increase to 280℃ at a rate of 20℃ / min and hold for 8 min;

[0137] Inlet temperature: 300℃;

[0138] Detector temperature: 310℃;

[0139] Carrier gas: High-purity nitrogen (99.99% purity), flow rate 1 mL / min;

[0140] Flow split ratio: 60:1;

[0141] Injection volume: 1.0 μL.

[0142] (2) Preparation of the sample solution to be tested:

[0143] Same as Example 1.

[0144] The experimental process of Comparative Example 1 shows that if the split ratio decreases, it will lead to damage to the gas chromatograph split outlet trap, blockage of the split outlet pipeline, and consequently damage to the solenoid valve.

[0145] Comparative Example 2

[0146] In Comparative Example 2, the gas chromatographic conditions for the gas chromatography detection of 3-amino-4'-nitrodiphenyl ether were the same as in Example 1, except that the split ratio was increased to 120:1. The specific process is as follows:

[0147] (1) The gas chromatography detection conditions are set as follows:

[0148] Detector: Flame Ionization (FID) detector;

[0149] Chromatographic column: HP-5, 30m × 320μm × 0.25μm;

[0150] Column temperature: 230℃ for 10 min, then increase to 280℃ at a rate of 20℃ / min and hold for 8 min;

[0151] Inlet temperature: 300℃;

[0152] Detector temperature: 310℃;

[0153] Carrier gas: High-purity nitrogen (99.99% purity), flow rate 1 mL / min;

[0154] Flow split ratio: 120:1;

[0155] Injection volume: 1.0 μL.

[0156] (2) Preparation of the sample solution to be tested:

[0157] Same as Example 1.

[0158] By comparing the test conditions of the experimental process in Comparative Example 2, it was found that if the split ratio is increased, the low-boiling point and high-boiling point impurities in the sample solution will be below the detection limit and cannot be detected.

[0159] Comparative Example 3

[0160] In Comparative Example 3, the gas chromatographic conditions for the gas chromatography detection of 3-amino-4'-nitrodiphenyl ether were the same as in Example 1, except that the injection port temperature was increased (310°C) in Comparative Example 3. The specific process is as follows:

[0161] (1) The gas chromatography detection conditions are set as follows:

[0162] Detector: Flame Ionization (FID) detector;

[0163] Chromatographic column: HP-5, 30m × 320μm × 0.25μm;

[0164] Column temperature: 230℃ for 10 min, then increase to 280℃ at a rate of 20℃ / min and hold for 8 min;

[0165] Inlet temperature: 310℃;

[0166] Detector temperature: 310℃;

[0167] Carrier gas: High-purity nitrogen (99.99% purity), flow rate 1 mL / min;

[0168] Flow split ratio: 100:1;

[0169] Injection volume: 1.0 μL.

[0170] (2) Preparation of the sample solution to be tested:

[0171] Same as Example 1.

[0172] By comparing the test conditions of the experimental process in Comparative Example 3, it was found that if the injection port temperature is too high, the elution times of the solvent acetonitrile and 3-amino-4'-nitrodiphenyl ether will be too close, which is not conducive to the separation of solvent acetonitrile, 3-amino-4'-nitrodiphenyl ether and low-boiling-point impurities.

[0173] Comparative Example 4

[0174] In Comparative Example 4, the gas chromatographic conditions for the gas chromatography detection of 3-amino-4'-nitrodiphenyl ether were the same as in Example 1, except that the injection port temperature was lowered (260°C). The specific process is as follows:

[0175] (1) The gas chromatography detection conditions are set as follows:

[0176] Detector: Flame Ionization (FID) detector;

[0177] Chromatographic column: HP-5, 30m × 320μm × 0.25μm;

[0178] Column temperature: 230℃ for 10 min, then increase to 280℃ at a rate of 20℃ / min and hold for 8 min;

[0179] Inlet temperature: 260℃;

[0180] Detector temperature: 310℃;

[0181] Carrier gas: High-purity nitrogen (99.99% purity), flow rate 1 mL / min;

[0182] Flow split ratio: 100:1;

[0183] Injection volume: 1.0 μL.

[0184] (2) Preparation of the sample solution to be tested:

[0185] Same as Example 1.

[0186] By comparing the test conditions of the experimental process in Comparative Example 3, it was found that if the injection port temperature is too low, 3-amino-4'-nitrodiphenyl ether will not be completely vaporized, affecting the accuracy of the test results.

[0187] Comparative Example 5

[0188] In Comparative Example 5, the gas chromatographic conditions for the detection of 3-amino-4'-nitrodiphenyl ether were the same as in Example 1, except that the column temperature in Comparative Example 5 was not programmed. The specific process is as follows:

[0189] (1) The gas chromatography detection conditions are set as follows:

[0190] Detector: Flame Ionization (FID) detector;

[0191] Chromatographic column: HP-5, 30m × 320μm × 0.25μm;

[0192] Column temperature: Increase to 280℃ at a rate of 20℃ / min and maintain for 8min;

[0193] Inlet temperature: 300℃;

[0194] Detector temperature: 310℃;

[0195] Carrier gas: High-purity nitrogen (99.99% purity), flow rate 1 mL / min;

[0196] Flow split ratio: 100:1;

[0197] Injection volume: 1.0 μL.

[0198] (2) Preparation of the sample solution to be tested:

[0199] Same as Example 1.

[0200] The comparison of the test conditions in Comparative Example 5 shows that if the column temperature is not programmed, the separation effect between the solvent peak and the 3-amino-4'-nitrodiphenyl ether product peak will be poor, ultimately affecting the detection accuracy of the 3-amino-4'-nitrodiphenyl ether product.

[0201] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are exhaustively listed. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0202] For those skilled in the art, various modifications and improvements can be made without departing from the concept of the present invention, and these modifications and improvements are all within the scope of protection of the present invention. The scope of protection of the present invention is defined by the appended claims.

Claims

1. A method for the gas phase detection of 3-amino-4'-nitrodiphenyl ether, characterized in that, The detection method is: S1, preparation of standard solution and sample solution: Preparation of standard solution: take 3-amino-4'-nitro diphenyl ether standard, and prepare a series of standard solutions with different concentrations by using acetonitrile; Preparation of sample solution: take 3-amino-4'-nitro diphenyl ether sample, and prepare sample solution by using solvent acetonitrile; S2, standard solution and sample solution are detected by gas chromatography under the following conditions: Detector: hydrogen flame ionization detector; Chromatographic column: high temperature chromatographic column; Column temperature: programmed temperature; Injection port temperature: 280-300℃; Detector temperature: 300-310℃; Split ratio: (80-100): 1; The column temperature condition of programmed temperature is: 210-240℃ for 8-12min, then heated to 260-300℃ at a rate of 15-25℃ / min, and maintained for 6-10min.

2. The method of claim 1, wherein the 3-amino-4'-nitro diphenyl ether is detected by gas phase. The concentration of 3-amino-4'-nitro diphenyl ether in the sample solution is 4.5-5.5mg / mL.

3. The method of claim 1, wherein the 3-amino-4'-nitrodiphenyl ether is detected by gas chromatography. The chromatographic column is HP-5, and the size specification of the chromatographic column is 30m×320μm×0.25μm.

4. The method of claim 1, wherein the 3-amino-4'-nitro diphenyl ether is detected by gas phase. The column temperature condition of programmed temperature is: 230℃ for 8min, then heated to 280℃ at a rate of 20℃ / min, and maintained for 8min.

5. The method of claim 1, wherein the 3-amino-4'-nitro diphenyl ether is detected by gas phase chromatography. The carrier gas for gas chromatography detection is nitrogen, and the flow rate is 0.8-1.2mL / min.

6. The method of claim 1, wherein the 3-amino-4'-nitro diphenyl ether is detected by gas phase. The injection amount of the detection process is 0.8-1.2μL.

7. The method of claim 1, wherein the 3-amino-4'-nitro diphenyl ether is detected by gas phase chromatography. The injection port temperature is 300℃, and the detector temperature is 310℃.

8. The method of claim 1, wherein the 3-amino-4'-nitro diphenyl ether is detected by gas phase. The injection amount is 1.0μL, and the split ratio is 100:

1.

9. The gas phase detection method for 3-amino-4'-nitrodiphenyl ether according to claim 1, characterized in that, When preparing the standard solution, the concentrations of the series of standard solutions with different concentrations are 60±1mg / mL, 50±1mg / mL, 20±1mg / mL, 10±1mg / mL, 5±0.5mg / mL, 2±0.5mg / mL, and 1±0.5mg / mL.

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