CN115993414A - Method for determining amine substances of automobile nonmetallic material - Google Patents
Method for determining amine substances of automobile nonmetallic material Download PDFInfo
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- CN115993414A CN115993414A CN202310061961.2A CN202310061961A CN115993414A CN 115993414 A CN115993414 A CN 115993414A CN 202310061961 A CN202310061961 A CN 202310061961A CN 115993414 A CN115993414 A CN 115993414A
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Abstract
The invention relates to a method for determining amine substances of an automobile nonmetallic material, which comprises GCMS and LCMS. The invention establishes a complete and comprehensive test method for the amine substances of the automobile nonmetallic materials, provides a specific test method for each type of substances, solves the problems of incomplete test types and single test method of the existing test standard and literature amine substances, and provides a comprehensive solution for the detection of the amine substances of the automobile nonmetallic materials.
Description
Technical Field
The invention belongs to the field of automobile material detection, and particularly relates to a method for measuring amine substances of an automobile nonmetallic material.
Background
Amine-containing materials in the nonmetallic materials of the automobile are widely used, for example, catalyst triethylene diamine and N-ethylmorpholine of polyurethane materials; the anti-aging agents of the rubber material comprise aldamines, diphenylamines and the like. Applications of these materials in the automotive field include automotive seating, dashboards, weatherstrips, steering wheels, door panels, foam, interior trim panels, and the like.
The odor threshold of the amine substances is low, the special odor can be emitted at extremely low concentration, the odor environment in the vehicle is influenced and deteriorated, most of the amine substances have toxicity, people can be poisoned by long-term contact and inhalation, and some aromatic amines such as beta-naphthylamine, benzidine and the like have cancerogenic action and are harmful to the sense organs and bodies of consumers.
At present, the coverage of the test standard of the amine substances in the air is narrower, and only part of the aliphatic and aromatic amine substances have the test standard. The testing method is limited, and mainly comprises gas chromatography, liquid chromatography mass spectrometry, spectrophotometry and the like. The prior literature mainly researches aromatic amine substances such as aniline, nitroaniline and the like which have great harm to human bodies, and researches odorous and harmful substances such as low-carbon aliphatic amines, alcohol amines, polyamines and the like. Therefore, no systematic and perfect testing method exists for the amine substances emitted by the nonmetallic materials of the automobile.
Disclosure of Invention
The invention aims to provide a method for measuring amine substances of an automobile nonmetallic material. A complete and comprehensive test method is established for the amine substances (55 types) of the automobile nonmetallic materials, a specific test method is provided for each type of substances, the problems that the existing test standard and the existing test method for the amine substances are not comprehensive and the test method is single can be solved, and a comprehensive solution is provided for the detection of the amine substances of the automobile nonmetallic materials.
The invention provides a method for determining amine substances of an automobile nonmetallic material, which comprises the following steps:
determination of tertiary amine species using GCMS:
dissolving tertiary amine substances with acetonitrile and fixing the volume to prepare 300 mg/L mixed standard stock solution; diluting with acetonitrile to a concentration of 3.0mg/L during analysis, and performing GCMS test;
determination of primary and secondary amines by LCMS:
dissolving primary and secondary amine substances with acetonitrile and fixing the volume to prepare 3000 mg/L mixed standard stock solution; then adding m-methylbenzoyl chloride derivatization reagent and sodium hydroxide solution for derivatization, and using acetonitrile to fix the volume; the assay was diluted with acetonitrile to a concentration of 3.0. 3.0mg/L and tested by LCMS.
The test conditions of the GCMS are as follows: gas phase conditions: the temperature of the sample inlet is 250 ℃, the flow rate of carrier gas is 2mL/min, the temperature is raised at 40 ℃ for 3min, the temperature is raised to 100 ℃ for 2min at 10 ℃/min, the temperature is raised to 200 ℃ at 15 ℃/min, the temperature is raised to 30 ℃ at 20 ℃/min, the sample injection volume is 1 mu L, and the split ratio is 20:1; mass spectrometry conditions: the ion source temperature is 230 ℃, the quaternary rod temperature is 150 ℃, the solvent excision time is 1min, the scanning frequency is 3.1 times/second, and the electron bombardment energy is 70Ev.
The volume concentration of the m-methylbenzoyl chloride derivatization reagent is 0.5%; the volume ratio of the m-methylbenzoyl chloride derivatization reagent to the mixed standard stock solution is 1:20.
The mass concentration of the sodium hydroxide solution is 40%; the volume ratio of the sodium hydroxide solution to the mixed standard stock solution is 1:100.
The LCMS test conditions were: gas phase conditions: column temperature 40 ℃, flow rate 0.3mL/min, sample injection volume 5 μl, mobile phase 0.1% formic acid water solution, acetonitrile; mass spectrometry conditions: sheath air temperature 300 ℃, sheath air flow rate 11 mL/min, dryer temperature 300 ℃, dryer flow rate 7mL/min, atomizer pressure 30psi, capillary voltage 4000V, nozzle voltage 1500V.
The derivatization method specifically comprises the following steps: adding 5-mL m-methylbenzoyl chloride derivatization reagent into a 100mL volumetric flask, adding 1mL sodium hydroxide solution, adding 100 mu L of standard solution into a light shaking flask body, screwing a cover, placing on an oscillator for oscillating for 1h, and standing for 0.5-1h; after the upper organic phase is dried in a nitrogen blowing instrument, acetonitrile is used for dissolving a nitrogen blowing pipe and 1mL of acetonitrile is used for fixing the volume; the standard solution concentration was 0.3 mg/L.
TABLE 1 list of amines as nonmetallic materials for automobiles
TABLE 2 method for testing amines of nonmetallic materials of automobiles (test of selected part of representative materials)
Advantageous effects
The invention establishes a complete and comprehensive test method for the amine substances (55 types) of the automobile nonmetallic materials, provides a specific test method for each type of substances, solves the problems of incomplete test types and single test method of the existing test standard and literature amine substances, and provides a comprehensive solution for the detection of the amine substances of the automobile nonmetallic materials.
Drawings
FIG. 1 is a GCMS chromatogram of a tertiary amine standard.
Fig. 2 is a primary secondary amine standard LCMS chromatogram.
FIG. 3 is a GCMS chromatogram of a tertiary amine sample.
Fig. 4 is a LCMS chromatogram of a primary amine sample.
Description of the embodiments
The invention will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
Example 1
Determination of tertiary amine species using GCMS:
(1) Main instrument and reagent standard
Instrument: gas Chromatography Mass Spectrometer (GCMS) Agilent GC7890B MS 5977B.
Reagent standard: acetonitrile HPLC/UPLC grade
And (5) marking: the concentration of the amine substance standard solution is 300 mg/L.
Actual sample: automobile cushion foam sample bag method test (100L).
(2) The testing method comprises the following steps:
and (5) marking: dissolving a tertiary amine substance sample with acetonitrile and fixing the volume to prepare 300 mg/L mixed standard stock solution; acetonitrile was diluted to a concentration of 3.0. 3.0mg/L for analysis and tested by GCMS. FIG. 1 is a GCMS chromatogram of the standard.
Sample: sampling foam 20×10×10cm (length×width×thickness), placing in 100L Tedlar sampling bag
(polyvinyl fluoride (PVF)) and 8L of gas is collected by a silica gel sampling tube at a flow rate of 500mL/min after being placed at a high temperature of 65 ℃ for 2 hours, and is eluted into a 5mL test tube by acetonitrile after collection, and then the test is carried out by GCMS. FIG. 3 sample GCMS chromatogram.
(3) Gas chromatograph mass spectrometer test conditions
Table 3 analysis conditions of gas chromatograph mass spectrometer
(4) Sample test results
TABLE 4 GCMS test results for foam samples
Examples
Determination of the primary and secondary species by LCMS:
(1) Main instruments and reagent standards.
Instrument: liquid Chromatography Mass Spectrometer (LCMS) Agilent LCMS 6465B, ultra-pure water device (Milli-Q ultra-pure water device Q-POD in America, nitrogen blowing device Shanghai Annotation model DC-12, constant temperature water bath oscillator (model WE-2) of European instruments and meters Limited in Tianjin city.
Reagent standard: acetonitrile HPLC/UPLC grade, formic acid UPLC/LC-MS grade, purity of m-methylbenzoyl chloride purity >98%, purity of sodium hydroxide purity >97%, and purity of amine substance standard solution.
And (5) marking: the concentration of the amine substance standard solution is 3000 mg/L.
Actual sample: automobile cushion foam sample bag method test (100L).
(2) Test method.
And (5) marking: standard stock solutions were diluted with acetonitrile to a mixed concentration series at a concentration of 3.0mg/L, derivatized with m-methylbenzoyl chloride, and subjected to LCMS for testing analysis. FIG. 2 standard LCMS chromatogram.
Sample: the foam sample is taken to be 20 multiplied by 10cm (length multiplied by width multiplied by thickness), placed in a 100L Tedlar sampling bag (made of polyvinyl fluoride (PVF)), and after being placed at a high temperature of 65 ℃ for 2 hours, 12L of gas is collected by a silica gel sampling tube at a flow rate of 1L/min, after the collection, acetonitrile is used for eluting into a 5mL test tube, 100 mu L of solution is taken for derivatization reaction, and the reaction is completely tested by LCMS. Figure 4 LCMS chromatogram of standard sample.
(3) Liquid chromatograph mass spectrometer test conditions.
Table 5 analysis conditions of liquid chromatograph mass spectrometer
(4) Sample test results.
Table 6 LCMS test results for foam samples
Claims (6)
1. A method for determining amine substances of an automobile nonmetallic material comprises the following steps:
determination of tertiary amine species using GCMS:
dissolving tertiary amine substances with acetonitrile and fixing the volume to prepare 300 mg/L mixed standard stock solution; diluting with acetonitrile to a concentration of 3.0mg/L during analysis, and performing GCMS test;
determination of primary and secondary amines by LCMS:
dissolving primary and secondary amine substances with acetonitrile and fixing the volume to prepare 3000 mg/L mixed standard stock solution; then adding m-methylbenzoyl chloride derivatization reagent and sodium hydroxide solution for derivatization, and using acetonitrile to fix the volume; the assay was diluted with acetonitrile to a concentration of 3.0. 3.0mg/L and tested by LCMS.
2. The method according to claim 1, characterized in that: the test conditions of the GCMS are as follows: gas phase conditions: the temperature of the sample inlet is 250 ℃, the flow rate of carrier gas is 2mL/min, the temperature is raised at 40 ℃ for 3min, the temperature is raised to 100 ℃ for 2min at 10 ℃/min, the temperature is raised to 200 ℃ at 15 ℃/min, the temperature is raised to 30 ℃ at 20 ℃/min, the sample injection volume is 1 μl, and the split ratio is 20:1; mass spectrometry conditions: the ion source temperature is 230 ℃, the quaternary rod temperature is 150 ℃, the solvent excision time is 1min, the scanning frequency is 3.1 times/second, and the electron bombardment energy is 70Ev.
3. The method according to claim 1, characterized in that: the volume concentration of the m-methylbenzoyl chloride derivatization reagent is 0.5%; the volume ratio of the m-methylbenzoyl chloride derivatization reagent to the mixed standard stock solution is 1:20.
4. The method according to claim 1, characterized in that: the mass concentration of the sodium hydroxide solution is 40%; the volume ratio of the sodium hydroxide solution to the mixed standard stock solution is 1:100.
5. The method according to claim 1, characterized in that: the LCMS test conditions were: gas phase conditions: column temperature 40 ℃, flow rate 0.3mL/min, sample injection volume 5 μl, mobile phase 0.1% formic acid water solution, acetonitrile; mass spectrometry conditions: sheath air temperature 300 ℃, sheath air flow rate 11 mL/min, dryer temperature 300 ℃, dryer flow rate 7mL/min, atomizer pressure 30psi, capillary voltage 4000V, nozzle voltage 1500V.
6. The method according to claim 1, characterized in that: the derivatization method specifically comprises the following steps: adding 5-mL m-methylbenzoyl chloride derivatization reagent into a 100mL volumetric flask, adding 1mL sodium hydroxide solution, adding 100 mu L of standard solution into a light shaking flask body, screwing a cover, placing on an oscillator for oscillating for 1h, and standing for 0.5-1h; after the upper organic phase is dried in a nitrogen blowing instrument, acetonitrile is used for dissolving a nitrogen blowing pipe and 1mL of acetonitrile is used for fixing the volume; the standard solution concentration was 0.3 mg/L.
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