CN113176354A - Method for detecting volatile odor of high-temperature thermally-modified wood - Google Patents
Method for detecting volatile odor of high-temperature thermally-modified wood Download PDFInfo
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Abstract
The invention provides a method for detecting volatile odor of high-temperature thermally-modified wood, which comprises the following steps: (1) pretreatment of wood samples: taking wood subjected to thermal modification treatment at different temperatures, grinding, weighing in a sample bottle, and sealing; (2) headspace solid phase microextraction: incubating the thermally modified wood powder in a hot water bath, and collecting volatile gas from the thermally modified wood powder through headspace solid phase microextraction; (3) gas chromatography-mass spectrometry: adopting a VF-WAXms chromatographic column as a solid phase, wherein the programmed temperature rise condition of the column temperature is as follows: the initial temperature is 50-55 ℃, the temperature is increased to 150 ℃ at 3-4 ℃/min, the temperature is increased to 210 ℃ at 2-3 ℃/min, the temperature is kept for 1-2 min, and mass spectrometry is carried out; the detection method disclosed by the invention is simple to operate, can realize better detection rate of volatile odor components of the high-temperature thermal modified wood, and has the characteristics of high sensitivity and high detection rate.
Description
Technical Field
The invention relates to the technical field of wood gas detection, in particular to a method for detecting volatile smell of high-temperature thermally modified wood.
Background
With the rapid development of economy, the quality of life of people is continuously improved, the consumption demand of wood and products thereof is greatly increased, and the wood serving as a renewable green material is widely applied to the aspects of furniture manufacture and interior decoration due to the unique mechanical and decorative properties of the wood.
The rubber wood has beautiful texture and good processing performance, but the content of starch and free sugar is higher than that of other tree species, and the rubber wood is generally subjected to antiseptic modification treatment and heat treatment modification, so that the decay resistance and the mildew resistance of the rubber wood can be improved, the problems of decay, worm damage and the like of the rubber wood are effectively solved, the dimensional stability of the rubber wood is obviously improved, and the equilibrium water content is reduced. The heat treatment technology is a process for performing heat treatment on the wood under the action of high temperature so as to improve the dimensional stability, corrosion resistance and weather resistance of the wood. Although no toxic chemicals are added in the heat treatment process, the wood thermal modification process usually comprises high-temperature drying, carbonization treatment, temperature and humidity reduction, cooling and kiln discharge, the process is actually equivalent to the drying and pre-carbonization stages of wood pyrolysis, the main components of the wood, namely hemicellulose and cellulose, are degraded to different degrees, and a large amount of mixed gas of organic volatile compounds (VOC) is necessarily generated. The odor generated by these gases gives an unpleasant feeling and may have a certain effect on their use. According to market research, the percentage of custom furniture businesses that have recently been subject to customer complaints for furniture odor problems is as high as 1%.
As the high-temperature thermal modification technology of wood enters the industrial production stage, most of researches on the high-temperature thermal modification technology are focused on the improvement of the heat treatment process conditions and the change of the physical and chemical properties of the heat treatment material, and the composition characteristics of organic volatile matters released by the heat modification material are less researched. The method is characterized in that the composition of volatile organic compounds released in the thermal modification process of the European fir is analyzed and researched by adopting a gas chromatography-mass spectrometry technology by the foreign Niv Graf, and the main components of the volatile organic compounds are acetic acid, furfural, toluene, terpene substances (mainly alpha-pinene) and the like. Xuezui adopts dynamic headspace sweeping method to collect volatile organic compounds released by poplar heat treatment material, and uses GC-MS technology to analyze components of different volatile matters, and researches show that poplar can generate a plurality of volatile components such as alkane, aromatic compounds, aldehydes, terpenes and the like in the heat treatment process.
At present, a great blank exists for a retrieval technology of volatile smell of high-temperature thermal modified wood, and effective detection of the smell of the thermal modified wood has important significance for realizing monitoring of safety quality of the thermal modified wood and widely serving as furniture production materials and other applications.
Disclosure of Invention
Therefore, the method for detecting the odor of the thermal modified wood has the advantages of simple operation, high sensitivity and high detection rate, improves the extraction efficiency and yield by adopting the solid-phase microextraction method and hot water bath incubation, realizes better detection rate of volatile odor components of the high-temperature thermal modified wood by combining gas chromatography-mass spectrometry, and is simple and convenient to operate and high in accuracy.
The technical scheme of the invention is realized as follows:
a method for detecting volatile odor of high-temperature thermally modified wood comprises the following steps:
(1) pretreatment of wood samples: taking the wood subjected to thermal modification treatment at different temperatures, grinding the wood into thermal modified wood powder with the particle size of 30-120 meshes, weighing the thermal modified wood powder in a sample bottle, and sealing;
(2) headspace solid phase microextraction: incubating the thermally modified wood powder obtained in the step 1 in a hot water bath, and collecting volatile gas from the thermally modified wood powder through headspace solid phase microextraction;
(3) gas chromatography-mass spectrometry: a VF-WAXms polar chromatographic column is adopted as a solid phase, and the programmed temperature rise condition of the column temperature is as follows: the initial temperature is 50-55 ℃, the temperature is increased to 150 ℃ at 3-4 ℃/min, the temperature is increased to 210 ℃ at 2-3 ℃/min, the temperature is kept for 1-2 min, and mass spectrometry is carried out.
Further, a sample injection needle of the solid phase microextraction technology is 50/30 μm DVB/Car/PDMS, the sample injection needle is activated at 220-240 ℃ to a peak shape without a compound in a chromatogram before each sampling, and the activated sample injection needle is inserted into a sample bottle and placed above a sample for extraction and adsorption.
Further, the extraction time of the solid phase micro-extraction is 5-10 min.
Further, the thermal modified wood powder is incubated in a hot water bath at 95-98 ℃ for 20-30 min.
Further, the carrier gas for gas chromatography-mass spectrometry is helium, the flow rate is 0.6-0.8 mL/min, and the temperature of a sample inlet is 225-235 ℃.
Further, the mass spectrometry conditions of the gas chromatography-mass spectrometry are as follows: the mass scanning range is 35-500 m/z, the ion voltage is 70eV, the ion current is 150 muA, the ion source temperature is 230 ℃, and the quadrupole rod temperature is 150 ℃.
Further, the temperature of the wood thermal modification is 150-220 ℃.
Further, the thermally modified wood includes any one of rubber wood, acacia wood, and eucalyptus wood.
Compared with the prior art, the invention has the beneficial effects that: the method is used for detecting the volatile smell of the high-temperature thermal modification material based on a headspace solid-phase microextraction sampling technology and a gas chromatography-mass spectrometry combined analysis technology, and effectively determines effective detection of various main components and relative contents of the smell of the thermal modification material. Wherein, the hot water bath incubation and the headspace solid phase micro-extraction are combined, which is more beneficial to improving the efficiency and the yield of the extraction of the aldehyde and ester components in the thermal modified wood, meanwhile, a VF-WAXms polar chromatographic column is adopted as a stationary phase and combined with effective temperature programming treatment, the column loss is low, the separation effect can be fully improved, more comprehensive components consisting of the odor of the thermal modification material can be effectively separated, the effective separation and detection of more than 8 types of substance components such as aldehydes, esters, ketones, acids, alcohols, phenols, alkanes, aromatics and the like in the synchronous thermal modification wood can be realized, the detection rate of the volatile odor components of the high-temperature thermal modification wood can be obviously improved, the detection sensitivity is high, the operation is simple and convenient, the implementation is easy, the theoretical basis is provided for the use of the high-temperature thermal modification material, the method has important guiding significance for analyzing the odor of the thermal modification material and determining the application range of the thermal modification material with different temperatures.
Drawings
FIG. 1 is a total ion flow chromatogram for detecting volatile odor components of 190 ℃ thermally modified rubber wood in example 3 of the present invention;
FIG. 2 is a total ion flow chromatogram for detecting volatile odor components of 210 ℃ thermally modified rubber wood in example 4 of the present invention;
FIG. 3 is a total ion flow chromatogram for detecting volatile odor components of 210 ℃ thermally modified rubber wood of comparative example 1 of the present invention.
Detailed Description
In order to better understand the technical content of the invention, specific examples are provided below to further illustrate the invention.
The experimental methods used in the examples of the present invention are all conventional methods unless otherwise specified.
The materials, reagents and the like used in the examples of the present invention can be obtained commercially without specific description.
Example 1
Detecting the volatile odor of high-temperature thermally modified eucalyptus wood, comprising the following steps:
the method comprises the following steps: taking a rubber wood sample treated by a thermal modification process at 150 ℃, grinding the rubber wood sample into wood powder with the particle size of 30 meshes, weighing 1.5g of the wood powder sample in a 15mL sample bottle, screwing a bottle cap, and sealing;
step two: incubating the thermally modified wood powder in the first step in a hot water bath, wherein the incubation temperature is 95 ℃, and the incubation time is 20 min; collecting volatile gas from the thermally modified wood powder by adopting headspace solid-phase microextraction, wherein a sample injection needle of the solid-phase microextraction technology is 50/30 mu m DVB/Car/PDMS, the sample injection needle is activated at 220 ℃ before each sampling till the peak shape of a compound does not appear in a chromatogram, the activated sample injection needle is inserted into a sample bottle and is placed above a sample for extraction and adsorption, and the extraction time is 5min to obtain an extracted sample;
step three: performing gas chromatography-mass spectrometry on the extracted sample, and adopting a 30m multiplied by 0.25mm multiplied by 0.25 mu m VF-WAXms chromatographic column as a solid phase, wherein the temperature programming condition of the column temperature is as follows: the initial temperature is 50 ℃, the temperature is increased to 150 ℃ at the rate of 3 ℃/min, the temperature is increased to 210 ℃ at the rate of 2 ℃/min, the temperature is maintained for 1min, and mass spectrometry is carried out, wherein the carrier gas is high-purity helium, the flow rate is 0.6mL/min, and the injection port temperature is 225 ℃;
the mass spectrum conditions are as follows: the mass scanning range is 35-500 m/z, the ion voltage is 70eV, the ion current is 150 muA, the ion source temperature is 230 ℃, the quadrupole temperature is 150 ℃, and mass spectrometry is carried out.
Example 2
The method for detecting the volatile smell of the high-temperature thermally modified acacia wood comprises the following steps:
the method comprises the following steps: taking a rubber wood sample treated by a 220 ℃ thermal modification process, grinding the rubber wood sample into wood powder with the particle size of 120 meshes, weighing 1.5g of the wood powder sample in a 15mL sample bottle, screwing a bottle cap, and sealing;
step two: incubating the thermally modified wood powder in the first step in a hot water bath, wherein the incubation temperature is 98 ℃, and the incubation time is 30 min; collecting volatile gas from the thermally modified wood powder by adopting headspace solid-phase microextraction, wherein a sample injection needle of the solid-phase microextraction technology is 50/30 mu m DVB/Car/PDMS, the sample injection needle is activated at 240 ℃ before each sampling till the peak shape of a compound does not appear in a chromatogram, the activated sample injection needle is inserted into a sample bottle and is placed above a sample for extraction and adsorption, and the extraction time is 10min to obtain an extracted sample;
step three: performing gas chromatography-mass spectrometry on the extracted sample, and adopting a 30m multiplied by 0.25mm multiplied by 0.25 mu m VF-WAXms chromatographic column as a solid phase, wherein the temperature programming condition of the column temperature is as follows: the initial temperature is 55 ℃, the temperature is increased to 150 ℃ at 4 ℃/min, the temperature is increased to 210 ℃ at 3 ℃/min, the temperature is kept for 2min, and mass spectrometry is carried out, wherein the carrier gas is high-purity helium, the flow rate is 0.8mL/min, and the temperature of a sample inlet is 235 ℃;
the mass spectrum conditions are as follows: the mass scanning range is 35-500 m/z, the ion voltage is 70eV, the ion current is 150 muA, the ion source temperature is 230 ℃, the quadrupole temperature is 150 ℃, and mass spectrometry is carried out.
Example 3
The method for detecting the volatile smell of the high-temperature thermal modified rubber wood comprises the following steps:
the method comprises the following steps: taking a rubber wood sample treated by a thermal modification process at 190 ℃, grinding the rubber wood sample into wood powder with the particle size of 30 meshes, weighing 1.5g of the wood powder sample in a 15mL sample bottle, screwing a bottle cap, and sealing;
step two: incubating the thermally modified wood powder in the first step in a hot water bath, wherein the incubation temperature is 95 ℃, and the incubation time is 20 min; collecting volatile gas from the thermally modified wood powder by adopting headspace solid-phase microextraction, wherein a sample injection needle of the solid-phase microextraction technology is 50/30 mu m DVB/Car/PDMS, the sample injection needle is activated at 230 ℃ before each sampling till the peak shape of a compound does not appear in a chromatogram, the activated sample injection needle is inserted into a sample bottle and is placed above a sample for extraction and adsorption, and the extraction time is 10min to obtain an extracted sample;
step three: performing gas chromatography-mass spectrometry on the extracted sample, and adopting a 30m multiplied by 0.25mm multiplied by 0.25 mu m VF-WAXms chromatographic column as a solid phase, wherein the temperature programming condition of the column temperature is as follows: the initial temperature is 50 ℃, the temperature is increased to 150 ℃ at 4 ℃/min, the temperature is increased to 210 ℃ at 3 ℃/min, the temperature is maintained for 1min, and mass spectrometry is carried out, wherein the carrier gas is high-purity helium, the flow rate is 0.8mL/min, and the injection port temperature is 230 ℃;
the mass spectrum conditions are as follows: the mass scanning range is 35-500 m/z, the ion voltage is 70eV, the ion current is 150 muA, the ion source temperature is 230 ℃, the quadrupole temperature is 150 ℃, mass spectrometry is carried out, and the total ion current chromatogram is shown in figure 1.
Example 4
The method for detecting the volatile smell of the high-temperature thermal modified rubber wood comprises the following steps:
the method comprises the following steps: taking a rubber wood sample treated by a 210 ℃ thermal modification process, grinding the rubber wood sample into wood powder with the particle size of 50 meshes, weighing 1.0g of the wood powder sample in a 15mL sample bottle, screwing a bottle cap, and sealing;
step two: incubating the thermally modified wood powder in the first step in a hot water bath, wherein the incubation temperature is 96 ℃, and the incubation time is 30 min; collecting volatile gas from the thermally modified wood powder by adopting headspace solid-phase microextraction, wherein a sample injection needle of the solid-phase microextraction technology is 50/30 mu m DVB/Car/PDMS, the sample injection needle is activated at 230 ℃ before each sampling till the peak shape of a compound does not appear in a chromatogram, the activated sample injection needle is inserted into a sample bottle and is placed above a sample for extraction and adsorption, and the extraction time is 5min to obtain an extracted sample;
step three: performing gas chromatography-mass spectrometry on the extracted sample, and adopting a 30m multiplied by 0.25mm multiplied by 0.25 mu m VF-WAXms chromatographic column as a solid phase, wherein the temperature programming condition of the column temperature is as follows: the initial temperature is 50 ℃, the temperature is increased to 150 ℃ at 4 ℃/min, the temperature is increased to 210 ℃ at 3 ℃/min, the temperature is maintained for 1min, and mass spectrometry is carried out, wherein the carrier gas is high-purity helium, the flow rate is 0.8mL/min, and the injection port temperature is 230 ℃;
the mass spectrum conditions are as follows: the mass scanning range is 35-500 m/z, the ion voltage is 70eV, the ion current is 150 muA, the ion source temperature is 230 ℃, the quadrupole temperature is 150 ℃, mass spectrometry is carried out, the total ion current chromatogram is shown in figure 2, the spectrum separation effect is better, the peak shapes are symmetrical and have no overlap, the substance types for detecting the volatile odor of the thermally modified rubber wood by the method comprise aldehydes, esters, ketones, acids, alcohols, phenols, alkanes, aromatics and other substances, and the analysis and detection results are shown in the following table, which indicates that the method can realize effective separation and detection of more than 8 substance components in the thermally modified wood, the detection rate of an extraction sample reaches 93.14%, the detection rate of the volatile odor components of the high-temperature thermally modified wood is better, and the operation is simple.
Table 1210 deg.c compound composition and relative content of volatile smell components of thermally modified rubber wood
Comparative example 1
The comparative example differs from example 4 in that: step three: the HP-5 nonpolar chromatographic column with the temperature of 30m multiplied by 0.25mm multiplied by 0.25 mu m is used as a solid phase, the temperature programming condition and the mass spectrum condition of the column temperature are the same as those of the embodiment 4, the total ion current chromatogram is shown in figure 3, the HP-5 nonpolar chromatographic column is used for detecting a sample, the chromatographic separation effect is poor, the peak shape is trailing, the detected substances are obviously reduced through analysis and detection, and the detection rate of the extracted sample is 72.25 percent, which indicates that the VF-WAXms chromatographic column selected by the invention is more suitable for detecting the volatile odor substances of the high-temperature thermal modified wood, and has high detection sensitivity, good separation effect and high result accuracy.
Comparative example 2
The comparative example differs from example 4 in that: step three: the DB-VAX polar chromatographic column with the temperature of 30m multiplied by 0.25mm multiplied by 0.25 mu m is used as a solid phase, the temperature programming condition and the mass spectrum condition of the column temperature are the same as those of the embodiment 4, and the result shows that the DB-VAX polar chromatographic column is used for detecting the sample, the chromatographic peak shape is easy to trail, the column loss condition is generated, and the detection rate of the extracted sample is reduced, so that the VF-WAXms chromatographic column is more suitable for detecting the volatile odor substances of the high-temperature thermal modified wood, and the detection sensitivity is high, the separation effect is good, and the result accuracy is high.
Comparative example 3
This comparative example differs from example 4 in that: step three: the programmed temperature conditions of the column temperature are as follows: the initial temperature is 60 ℃, the temperature is increased to 150 ℃ at the rate of 5 ℃/min, the temperature is increased to 210 ℃ at the rate of 5 ℃/min, the temperature is maintained for 1min, the rest conditions are the same as those in the embodiment 4, and the detection result of analysis shows that the detection rate of the extraction sample is 88.06 percent, which shows that the control of a certain temperature programming condition of the stationary phase is beneficial to improving the detection rate of the volatile odor components of the high-temperature thermal modified wood.
Comparative example 4
This comparative example differs from example 4 in that: step two: the thermal modified wood powder is incubated in a hot water bath, volatile gas is directly collected from the thermal modified wood powder through headspace solid-phase microextraction, the rest conditions are the same as those in the embodiment 4, the detection result of analysis shows that the detection rate of an extraction sample is 81.06%, the relative content of aldehyde and ester in the thermal modified wood is obviously reduced, and the combination of the incubation in the hot water bath and the headspace solid-phase microextraction is favorable for improving the efficiency and yield of the extraction of the aldehyde and ester in the thermal modified wood.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A method for detecting volatile odor of high-temperature thermally modified wood is characterized by comprising the following steps: the method comprises the following steps:
(1) pretreatment of wood samples: taking the wood subjected to thermal modification treatment at different temperatures, grinding the wood into thermal modified wood powder with the particle size of 30-120 meshes, weighing the thermal modified wood powder in a sample bottle, and sealing;
(2) headspace solid phase microextraction: incubating the thermally modified wood powder obtained in the step 1 in a hot water bath, and collecting volatile gas from the thermally modified wood powder through headspace solid phase microextraction;
(3) gas chromatography-mass spectrometry: a VF-WAXms polar chromatographic column is adopted as a solid phase, and the programmed temperature rise condition of the column temperature is as follows: the initial temperature is 50-55 ℃, the temperature is increased to 150 ℃ at 3-4 ℃/min, the temperature is increased to 210 ℃ at 2-3 ℃/min, the temperature is kept for 1-2 min, and mass spectrometry is carried out.
2. The method for detecting volatile odor of high temperature thermally modified wood according to claim 1, wherein: the sample injection needle of the solid phase microextraction technology is 50/30 mu m DVB/Car/PDMS, the sample injection needle is activated at 220-240 ℃ before each sampling until the peak shape of a compound does not appear in a chromatogram, and the activated sample injection needle is inserted into a sample bottle and placed above a sample for extraction and adsorption.
3. The method for detecting volatile odor of high temperature thermally modified wood according to claim 2, wherein: the extraction time of the solid-phase micro-extraction is 5-10 min.
4. The method for detecting volatile odor of high temperature thermally modified wood according to claim 1, wherein: and incubating the thermally modified wood powder in a hot water bath at the temperature of 95-98 ℃ for 20-30 min.
5. The method for detecting volatile odor of high temperature thermally modified wood according to claim 1, wherein: the carrier gas for gas chromatography-mass spectrometry is helium, the flow rate is 0.6-0.8 mL/min, and the temperature of a sample inlet is 225-235 ℃.
6. The method for detecting volatile odor of high temperature thermally modified wood according to claim 1, wherein: the mass spectrum conditions of the gas chromatography-mass spectrometry are as follows: the mass scanning range is 35-500 m/z, the ion voltage is 70eV, the ion current is 150 muA, the ion source temperature is 230 ℃, and the quadrupole rod temperature is 150 ℃.
7. The method for detecting volatile odor of high temperature thermally modified wood according to claim 1, wherein: the temperature of the wood thermal modification is 150-220 ℃.
8. The method for detecting volatile odor of high temperature thermally modified wood according to claim 1, wherein: the thermally modified wood comprises any one of rubber wood, acacia wood and eucalyptus wood.
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| EP4345451A1 (en) * | 2022-09-28 | 2024-04-03 | Sumitomo Rubber Industries, Ltd. | Analyzer, analysis method, and analysis program for rubber composition |
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