CN114441650B - Genuine leather smell tracing analysis and control method - Google Patents
Genuine leather smell tracing analysis and control method Download PDFInfo
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- CN114441650B CN114441650B CN202011192249.9A CN202011192249A CN114441650B CN 114441650 B CN114441650 B CN 114441650B CN 202011192249 A CN202011192249 A CN 202011192249A CN 114441650 B CN114441650 B CN 114441650B
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Abstract
The invention discloses a dermis smell tracing analysis and control method, which belongs to the technical field of dermis smell tracing analysis and comprises the following steps: sampling the leather finished product, sampling a certain amount of strip leather sample, directly placing the strip leather sample into a glass material sampling tube, plugging quartz cotton at two ends of the glass material sampling tube, placing a thermal desorption instrument sample tray in a specified direction, and starting gas chromatography mass spectrometry sniffing detection analysis of smell substances; according to the invention, the gas chromatography mass spectrometry analysis means is combined with automatic sniffing for the leather finished product and related raw materials, so that smell substances sniffing and corresponding analysis of a chromatography mass spectrometry spectrogram are carried out, and the heavy smell contribution substances are traced to the leather materials added in the production process. After the important odor contribution substances are found, the odor of the leather products can be improved and controlled by adjusting the formula and the production process, including controlling the odor type, the odor direction and the intensity of the leather products, so that the problem of improving the leather odor is really solved.
Description
Technical Field
The invention belongs to the technical field of dermis smell tracing analysis, and particularly relates to a dermis smell tracing analysis and control method.
Background
In the leather production process, nearly hundred leather chemical products (liquid, powder and collectively called as leather materials) are used, wherein more than 10 basic chemical material components used in the working procedure before tanning are relatively single, but organic synthetic substances, polymers or mixed substances are used in the retanning dyeing and fatliquoring and finishing working procedures, the components are complex and unclear, the leather chemical products are absorbed or filled in the leather fibers or adhered to the surfaces after being added in the production working procedure, interactions exist among the substances in the process, the substances contained in raw materials (white wet leather and blue wet leather) are also very abundant, so that the substances contained in the leather finished products are too many to be cleared, and the situation is extremely complex.
The dermis volatilizes a smelly smell at normal or high temperature, and the corresponding components are very complex, so that the mixed smell of all substances emitted from hundreds or thousands of substances at that temperature point is the smell substance balance formed by the emission of the specific temperature point of the specific environment. The smell of human being cannot be recognized at all, what is contained or not contained in the mixed smell, and what is particularly contributed by the substances cannot be confirmed, so that the conventional means are used for analyzing and improving the dermal smell, and the method is difficult and has little effect, so that a method for analyzing and controlling the trace source of the dermal smell is needed.
Disclosure of Invention
The invention aims at: in order to solve the problem that the dermis volatilizes smelly smell at normal temperature or high temperature, the corresponding components are very complex, so that the mixed smell of all substances emitted by hundreds or thousands of substances at that temperature point is the smell substance balance formed by the emission of specific temperature points of specific environments. The smell of human being can not be recognized at all what is contained or not contained in the mixed smell, and what kind of components the smell is particularly contributed by the substances can not be confirmed, and the problems of difficulty, heaviness and very little effect are solved by analyzing and improving the dermal smell by the traditional means, so that the method for analyzing and controlling the trace source of the dermal smell is provided.
In order to achieve the above purpose, the present invention adopts the following technical scheme: the dermis smell tracing analysis and control method comprises the following steps:
s1, sampling a leather finished product, sampling a certain amount of strip leather samples, directly putting the strip leather samples into a glass material sampling tube, and plugging quartz wool at two ends of the glass material sampling tube;
s2, sealing one end of the sample tube with the notch by using a passivated semi-permeable sealing piece, and placing the other end of the sample tube with the notch into a sample tray of a thermal desorption instrument according to a specified direction after the sealing is confirmed by using a common stainless steel semi-permeable sealing piece;
s3, weighing a certain amount of liquid skinning material, placing the skinning material in a glassware with enough dead weight, putting the glassware in a Tedlar bag with a certain capacity, sealing the glassware with a pressing strip, and cleaning the glassware with high-purity nitrogen with a certain purity, and inflating a certain amount each time for cleaning for several times;
s4, filling a certain amount of high-purity nitrogen after cleaning is finished, placing the mixture in a walk-in oven, keeping the mixture in a certain temperature environment for a period of time, extracting a certain amount of gas by using a Tenax tube according to a flow rate, taking parallel samples from each sample, and storing the Tenax sample tube at a low temperature for later use;
s5, weighing a certain amount of powdery dermatoplastic materials, placing the powdery dermatoplastic materials into glassware with enough dead weight, pouring about 30 g of water, stirring uniformly, placing the glassware in a Tedlar bag with a certain capacity, sealing the glassware with a pressing strip, cleaning the glassware with high-purity nitrogen with a certain degree of purity or above, and inflating a certain amount each time, and cleaning the glassware for several times;
s6, repeating the step S4;
s7, drying a white wet skin tanned and cured by the pelt or a sample of the blue wet skin at a certain temperature, and controlling the water content within a certain range;
s8, cutting a certain amount of strip skin sample, directly placing the strip skin sample into a glass material sampling tube, plugging quartz wool at two ends of the glass material sampling tube, sealing one end of the sample tube with a notch by using a passivated semi-permeable sealing piece, and placing the other end of the sample tube with the notch into a thermal desorption instrument sample tray according to the direction after confirming the sealing;
s9, starting a thermal desorption instrument, a GC-MS and a sniffing instrument, setting desorption temperature, desorption time and GC gas phase heating program by thermal desorption, heating to a certain temperature at a certain rate for a period of time at an initial temperature, heating to a certain value at a certain rate, and keeping for a certain time;
s10, after relevant software is selected and set parameters are introduced, detection analysis is started, substances flowing out of a thermal desorption instrument are separated through a gas-phase capillary column and are split by a three-way splitter, one path of substances flows to a Mass Spectrometer (MS) for analysis, the other path of substances flows to a sniffing instrument for sniffing, a human nose faces to a horn mouth of the sniffing instrument, when the human nose can sniff a certain smell, the type of the smelled smell and the peak outlet time on 5977B mass spectrometry equipment are recorded, meanwhile, the number keys 1-6 representing the intensity of the smell are selected to be pressed on an analysis operation interface of the Sniffer9100 instrument (the numbers 1-6 represent the smell with different concentration grades, the larger numbers represent the stronger grades), and the sniffing operation is continued until the peak outlet is finished;
s11, searching a compound corresponding to a peak spectrogram at the time point of manually sniffing the odor through qualitative analysis software, determining the name of a substance, the type of the odor and the intensity of the odor, namely the contribution degree of the odor to the dermis odor, finding out the offensive odor substances in the sample, selecting 10-20 substances with the largest contribution of the bad odor from the sniffing result, and tracing the odor.
As a further description of the above technical solution:
in S1, a sample of approximately 10-20 mg of the strip is taken.
As a further description of the above technical solution:
in the step S3, about 50-52mg of liquid skinning material is weighed, put into a 10L Tedlar bag, and cleaned by high-purity nitrogen with the purity of 99.999% or more, and inflated 3L each time for 3 times.
As a further description of the above technical solution:
in the step S4, 5L of high-purity nitrogen is filled after the cleaning is finished, the mixture is placed in a walk-in oven to be kept at 90 ℃ for 0.5 hour, 1L of gas is extracted by a Tenax tube according to the flow rate of 200ml/min, 2 parallel samples are taken from each sample, and the Tenax sample tube is stored at a low temperature for standby.
As a further description of the above technical solution:
in the step S5, about 48-50mg of powdery dermatoplastic material is weighed, put into a 10L Tedlar bag, and cleaned by high-purity nitrogen with the purity of 99.999 percent or more, and inflated 3L each time for 3 times.
As a further description of the above technical solution:
in S7, a sample of white or blue wet skin tanned and cured from pelts is dried at 50 ℃ with a moisture content of 15% ± 3%.
As a further description of the above technical solution:
in S8, about 19-20mg of the strip of the skin sample is cut.
As a further description of the above technical solution:
in S9, the desorption temperature is set at 90 ℃ for 30min, the desorption time is set by a GC gas phase temperature rise program, the initial temperature is set at 40 ℃ for 3min, the temperature is raised to 92 ℃ at the speed of 3 ℃/min, the temperature is raised to 160 ℃ at the speed of 5 ℃/min, the temperature is raised to 310 ℃ at the speed of 10 ℃/min, and the temperature is kept for 20min.
The invention also provides a dermis smell tracing control method, which comprises the following steps:
s1, performing odor substance sniffing spectrogram correspondence analysis on a leather finished product and a related raw material, namely a leather material and wet white (blue) leather;
s2, screening a bill of materials with the odor type and the peak time basically coincident according to the odor distinguishing spectrogram of the leather finished product and the related raw materials, and repeatedly testing and analyzing for a plurality of times, wherein analysis data with consistent results are used as effective data;
s3, removing substances or skin materials which contribute obviously to the confirmed smell from the actual production formula, selecting skin materials without obvious smell influencing substances and re-formulating a sample process formula by using wet white (blue) skin;
s4, comparing the finished product with the odor substances of the related raw materials, and screening the raw materials (the skinned materials/the wet white (blue) skin) repeatedly in the forward direction or the reverse direction for a plurality of times;
s5, adjusting a process formula, producing a sample, tracing by sniffing analysis, improving the process formula, producing the sample, improving by sniffing analysis, and finally controlling the odor type, direction and odor intensity of the leather product.
As a further description of the above technical solution:
in the step S2, the analysis is repeated for 3 times, and the analysis data with the consistent result is taken as effective data.
In summary, due to the adoption of the technical scheme, the beneficial effects of the invention are as follows:
the invention uses the leather products and the related raw materials: the method comprises the steps of carrying out odor substance sniffing spectrogram correspondence analysis on the skinned material and the wet skin, effectively screening a bill of substances with basically coincident odor types and peak time, taking the analysis data with consistent results as effective data, removing substances with obvious odor contribution from the actual production formula or the skinned material as (GG), selecting the skinned material without obvious odor influencing substances and the wet skin to reform a sample process formula, carrying out odor substance comparison on the finished product and related raw materials again after the finished product is produced, screening the raw materials (the skinned material/the wet skin) repeatedly forward or backward, adjusting the process formula, carrying out sample production, tracing the odor analysis, improving the process formula, carrying out sample production, carrying out odor sniffing analysis improvement again, finally effectively controlling the odor types, the odor directions and the intensity of the dermis products, solving the problem of odor improvement, adopting a gas chromatography-mass spectrometry analysis method to combine with automatic odor quality analysis, fixing a specific test method, carrying out full analysis on the odor problem of the dermis products and tracing the large odor contribution substances to the skinned material added in the production process, and carrying out odor improvement and control on the dermis products.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The invention provides a technical scheme that: the dermis smell tracing analysis and control method comprises the following steps of;
s1, sampling a leather finished product, sampling 15.2g of long leather sample, directly putting the long leather sample into a glass sampling tube, and plugging quartz cotton at two ends of the glass sampling tube;
s2, sealing one end of the sample tube with the notch by using a passivated semi-permeable sealing piece, and placing the other end of the sample tube with the notch into a sample tray of a thermal desorption instrument according to a specified direction after the sealing is confirmed by using a common stainless steel semi-permeable sealing piece;
s3, weighing about 50mg of liquid skinning material, placing the skinning material in a glassware with enough dead weight, putting the glassware into a 10L Tedlar bag horizontally, cleaning the glassware with high-purity nitrogen with the purity of 99.999% or more, and inflating the glassware for 3L for 3 times;
s4, filling 5L of high-purity nitrogen after cleaning is finished, placing the mixture in a walk-in oven to keep the environment at 90 ℃ for 0.5 hour, extracting 1L of gas by using a Tenax tube according to the flow rate of 200ml/min, taking 2 parallel samples from each sample, and storing the Tenax sample tube at a low temperature for later use;
s5, weighing about 50mg of powdery dermatoplastic material, placing the powdery dermatoplastic material in a glassware with enough dead weight, pouring about 30 g of water, uniformly stirring, placing the mixture in a 10L Tedlar bag, cleaning the mixture by using high-purity nitrogen with the purity of 99.999% or more, and inflating the mixture 3L each time for 3 times;
s6, repeating the step S4;
s7, drying a sample of white wet skin or blue wet skin tanned and cured by the pelt at 50 ℃, wherein the water content is controlled to be 15+/-3%;
s8, cutting a strip skin sample of about 19.2mg, directly placing the strip skin sample into a glass material sampling tube, plugging quartz wool at two ends of the glass material sampling tube, sealing one end of the sample tube with a notch by using a passivated semi-permeable sealing piece, and placing the other end of the sample tube with the notch into a thermal desorption instrument sample tray according to the direction after confirming the sealing;
s9, starting a thermal desorption instrument, a GC-MS and a sniffing instrument, setting desorption temperature of thermal desorption at 90 ℃ for 30min, setting GC gas phase temperature rise program, setting initial temperature at 40 ℃ for 3min, heating to 92 ℃ at the rate of 3 ℃/min, heating to 160 ℃ at the rate of 5 ℃/min, heating to 310 ℃ at the rate of 10 ℃/min, and keeping for 20min;
s10, after relevant software is selected and set parameters are introduced, detection analysis is started, substances flowing out of a thermal desorption instrument are separated through a gas-phase capillary column and are split by a three-way splitter, one path of substances flows to a Mass Spectrometer (MS) for analysis, the other path of substances flows to a sniffing instrument for sniffing, a human nose faces to a horn mouth of the sniffing instrument, when the human nose can sniff a certain smell, the type of the smelled smell and the peak outlet time on 5977B mass spectrometry equipment are recorded, meanwhile, the number keys 1-6 representing the intensity of the smell are selected to be pressed on an analysis operation interface of the Sniffer9100 instrument (the numbers 1-6 represent the smell with different concentration grades, the larger numbers represent the stronger grades), and the sniffing operation is continued until the peak outlet is finished;
s11, searching a compound corresponding to a peak spectrogram at the time point of manually sniffing the odor through qualitative analysis software, determining the name of a substance, the type of the odor and the intensity of the odor, namely the contribution degree to the dermis odor of all odorous monomer compounds, finding out unpleasant odor substances in the sample, selecting 10-20 substances with the largest contribution of the bad odor from the sniffing result, and tracing the odor;
the invention also provides a dermis smell tracing control method, which comprises the following steps:
s1, performing odor substance sniffing spectrogram correspondence analysis on a leather finished product and a related raw material, namely a leather material and wet white (blue) leather;
s2, screening a bill of materials with basically coincident gas types and peak time, and repeatedly testing and analyzing for 3 times, wherein analysis data with consistent results are used as effective data;
s3, removing substances or skin materials which contribute obviously to the confirmed smell from the actual production formula, selecting skin materials without obvious smell influencing substances and re-formulating a sample process formula by using wet white (blue) skin;
s4, comparing the finished product with the odor substances of the related raw materials, and screening the raw materials (the skinned materials/the wet white (blue) skin) repeatedly in the forward direction or the reverse direction for a plurality of times;
s5, adjusting a process formula, producing a sample, tracing by sniffing analysis, improving the process formula, producing the sample, improving by sniffing analysis, and finally controlling the odor type, direction and odor intensity of the leather product.
Example 2
The invention provides a technical scheme that: the dermis smell tracing analysis and control method comprises the following steps of;
s1, sampling a leather finished product, sampling 17g of strip leather samples, directly placing the strip leather samples into a glass sampling tube, and plugging quartz wool at two ends of the glass sampling tube;
s2, sealing one end of the sample tube with the notch by using a passivated semi-permeable sealing piece, and placing the other end of the sample tube with the notch into a sample tray of a thermal desorption instrument according to a specified direction after the sealing is confirmed by using a common stainless steel semi-permeable sealing piece;
s3, weighing about 50mg of liquid skinning material, placing the skinning material in a glassware with enough dead weight, putting the glassware into a 10L Tedlar bag horizontally, cleaning the glassware with high-purity nitrogen with the purity of 99.999% or more, and inflating the glassware for 3L for 3 times;
s4, filling 5L of high-purity nitrogen after cleaning is finished, placing the mixture in a walk-in oven to keep the environment at 90 ℃ for 0.5 hour, extracting 1L of gas by using a Tenax tube according to the flow rate of 200ml/min, taking 2 parallel samples from each sample, and storing the Tenax sample tube at a low temperature for later use;
s5, weighing about 48.7mg of powdery dermatoplastic material, placing the powdery dermatoplastic material in a glassware with enough dead weight, pouring about 30 g of water, stirring uniformly, placing the glassware in a 10L Tedlar bag horizontally, cleaning the glassware with high-purity nitrogen with the purity of 99.999% or more, and inflating 3L each time for 3 times;
s6, repeating the step S4;
s7, drying a sample of white wet skin or blue wet skin tanned and cured by the pelt at 50 ℃, wherein the water content is controlled to be 15+/-3%;
s8, cutting a strip skin sample of about 19.2mg, directly placing the strip skin sample into a glass material sampling tube, plugging quartz wool at two ends of the glass material sampling tube, sealing one end of the sample tube with a notch by using a passivated semi-permeable sealing piece, and placing the other end of the sample tube with the notch into a thermal desorption instrument sample tray according to the direction after confirming the sealing;
s9, starting a thermal desorption instrument, a GC-MS and a sniffing instrument, setting desorption temperature of thermal desorption at 90 ℃ for 30min, setting GC gas phase temperature rise program, setting initial temperature at 40 ℃ for 3min, heating to 92 ℃ at the rate of 3 ℃/min, heating to 160 ℃ at the rate of 5 ℃/min, heating to 310 ℃ at the rate of 10 ℃/min, and keeping for 20min;
s10, after relevant software is selected and set parameters are introduced, detection analysis is started, substances flowing out of a thermal desorption instrument are separated through a gas-phase capillary column and are split by a three-way splitter, one path of substances flows to a Mass Spectrometer (MS) for analysis, the other path of substances flows to a sniffing instrument for sniffing, a human nose faces to a horn mouth of the sniffing instrument, when the human nose can sniff a certain smell, the type of the smelled smell and the peak outlet time on 5977B mass spectrometry equipment are recorded, meanwhile, the number keys 1-6 representing the intensity of the smell are selected to be pressed on an analysis operation interface of the Sniffer9100 instrument (the numbers 1-6 represent the smell with different concentration grades, the larger numbers represent the stronger grades), and the sniffing operation is continued until the peak outlet is finished;
s11, searching a compound corresponding to a peak spectrogram at the time point of manually sniffing the odor through qualitative analysis software, determining the name of a substance, the type of the odor and the intensity of the odor, namely the contribution degree to the dermis odor of all odorous monomer compounds, finding out unpleasant odor substances in the sample, selecting 10-20 substances with the largest contribution of the bad odor from the sniffing result, and tracing the odor;
the invention also provides a dermis smell tracing control method, which comprises the following steps:
s1, performing odor substance sniffing spectrogram correspondence analysis on a leather finished product and a related raw material, namely a leather material and wet white (blue) leather;
s2, screening a bill of materials with basically coincident gas types and peak time, and repeatedly testing and analyzing for 3 times, wherein analysis data with consistent results are used as effective data;
s3, removing substances or skin materials which contribute obviously to the confirmed smell from the actual production formula, selecting skin materials without obvious smell influencing substances and re-formulating a sample process formula by using wet white (blue) skin;
s4, comparing the finished product with the odor substances of the related raw materials, and screening the raw materials (the skinned materials/the wet white (blue) skin) repeatedly in the forward direction or the reverse direction for a plurality of times;
s5, adjusting a process formula, producing a sample, tracing by sniffing analysis, improving the process formula, producing the sample, improving by sniffing analysis, and finally controlling the odor type, direction and odor intensity of the leather product.
Example 3
The invention provides a technical scheme that: the dermis smell tracing analysis and control method comprises the following steps of;
s1, sampling a leather finished product, sampling 20g of strip leather samples, directly placing the strip leather samples into a glass sampling tube, and plugging quartz wool at two ends of the glass sampling tube;
s2, sealing one end of the sample tube with the notch by using a passivated semi-permeable sealing piece, and placing the other end of the sample tube with the notch into a sample tray of a thermal desorption instrument according to a specified direction after the sealing is confirmed by using a common stainless steel semi-permeable sealing piece;
s3, weighing about 52mg of liquid skinning material, placing the skinning material in a glassware with enough dead weight, putting the glassware into a 10L Tedlar bag horizontally, cleaning the glassware with high-purity nitrogen with the purity of 99.999% or more, and inflating the glassware for 3L for 3 times;
s4, filling 5L of high-purity nitrogen after cleaning is finished, placing the mixture in a walk-in oven to keep the environment at 90 ℃ for 0.5 hour, extracting 1L of gas by using a Tenax tube according to the flow rate of 200ml/min, taking 2 parallel samples from each sample, and storing the Tenax sample tube at a low temperature for later use;
s5, weighing about 50mg of powdery dermatoplastic material, placing the powdery dermatoplastic material in a glassware with enough dead weight, pouring about 30 g of water, uniformly stirring, placing the mixture in a 10L Tedlar bag, cleaning the mixture by using high-purity nitrogen with the purity of 99.999% or more, and inflating the mixture 3L each time for 3 times;
s6, repeating the step S4;
s7, drying a sample of white wet skin or blue wet skin tanned and cured by the pelt at 50 ℃, wherein the water content is controlled to be 15+/-3%;
s8, cutting about 20mg of strip skin sample, directly placing the strip skin sample into a glass material sampling tube, plugging quartz wool at two ends of the glass material sampling tube, sealing one end of the sample tube with a notch by using a passivated semi-permeable sealing piece, and placing the other end of the sample tube with the notch into a thermal desorption instrument sample tray according to the direction after confirming the sealing;
s9, starting a thermal desorption instrument, a GC-MS and a sniffing instrument, setting desorption temperature of thermal desorption at 90 ℃ for 30min, setting GC gas phase temperature rise program, setting initial temperature at 40 ℃ for 3min, heating to 92 ℃ at the rate of 3 ℃/min, heating to 160 ℃ at the rate of 5 ℃/min, heating to 310 ℃ at the rate of 10 ℃/min, and keeping for 20min;
s10, after relevant software is selected and set parameters are introduced, detection analysis is started, substances flowing out of a thermal desorption instrument are separated through a gas-phase capillary column and are split by a three-way splitter, one path of substances flows to a Mass Spectrometer (MS) for analysis, the other path of substances flows to a sniffing instrument for sniffing, a human nose faces to a horn mouth of the sniffing instrument, when the human nose can sniff a certain smell, the type of the smelled smell and the peak outlet time on 5977B mass spectrometry equipment are recorded, meanwhile, the number keys 1-6 representing the intensity of the smell are selected to be pressed on an analysis operation interface of the Sniffer9100 instrument (the numbers 1-6 represent the smell with different concentration grades, the larger numbers represent the stronger grades), and the sniffing operation is continued until the peak outlet is finished;
s11, searching a compound corresponding to a peak spectrogram at the time point of manually sniffing the odor through qualitative analysis software, determining the name of a substance, the type of the odor and the intensity of the odor, namely the contribution degree to the dermis odor of all odorous monomer compounds, finding out unpleasant odor substances in the sample, selecting 10-20 substances with the largest contribution of the bad odor from the sniffing result, and tracing the odor;
the invention also provides a dermis smell tracing control method, which comprises the following steps:
s1, performing odor substance sniffing spectrogram correspondence analysis on a leather finished product and a related raw material, namely a leather material and wet white (blue) leather;
s2, screening a bill of materials with basically coincident gas types and peak time, and repeatedly testing and analyzing for 3 times, wherein analysis data with consistent results are used as effective data;
s3, removing substances or skin materials which contribute obviously to the confirmed smell from the actual production formula, selecting skin materials without obvious smell influencing substances and re-formulating a sample process formula by using wet white (blue) skin;
s4, comparing the finished product with the odor substances of the related raw materials, and screening the raw materials (the skinned materials/the wet white (blue) skin) repeatedly in the forward direction or the reverse direction for a plurality of times;
s5, adjusting a process formula, producing a sample, tracing by sniffing analysis, improving the process formula, producing the sample, improving by sniffing analysis, and finally controlling the odor type, direction and odor intensity of the leather product.
Examples 1 to 3 are described as follows: since the heating temperature of the sample specified in the odor detection standard of most automobile companies is 80 degrees or lower, after the study is based on a series of experimental study analysis at three heating temperature points of 80 degrees, 85 degrees and 90 degrees, the heating temperature with 90 degrees as the real leather odor smell recognition and odor source analysis is determined, namely, the heating temperature is slightly higher than the odor test temperature specified by customers, so that the analysis result can be completely corresponding to and suitable for the relevant odor standard of automobile factories.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (10)
1. The dermis smell tracing analysis method comprises the following steps:
s1, sampling a leather finished product, sampling a certain amount of strip leather samples, directly putting the strip leather samples into a glass material sampling tube, and plugging quartz wool at two ends of the glass material sampling tube;
s2, sealing one end of the sample tube with the notch by using a passivated semi-permeable sealing piece, and placing the other end of the sample tube with the notch into a sample tray of a thermal desorption instrument according to a specified direction after the sealing is confirmed by using a common stainless steel semi-permeable sealing piece;
s3, weighing a certain amount of liquid skinning material, placing the skinning material in a glassware with enough dead weight, putting the glassware in a Tedlar bag with a certain capacity, sealing the glassware with a pressing strip, and cleaning the glassware with high-purity nitrogen with a certain purity, and inflating a certain amount each time for cleaning for several times;
s4, filling a certain amount of high-purity nitrogen after cleaning is finished, placing the mixture in a walk-in oven, keeping the mixture in a certain temperature environment for a period of time, extracting a certain amount of gas by using a Tenax tube according to a flow rate, taking parallel samples from each sample, and storing the Tenax sample tube at a low temperature for later use;
s5, weighing a certain amount of powdery dermatoplastic materials, placing the powdery dermatoplastic materials into glassware with enough dead weight, pouring about 30 g of water, stirring uniformly, placing the glassware in a Tedlar bag with a certain capacity, sealing the glassware with a pressing strip, cleaning the glassware with high-purity nitrogen with a certain purity, and inflating a certain amount each time, and cleaning the glassware for several times;
s6, repeating the step S4;
s7, drying a white wet skin tanned and cured by the pelt or a sample of the blue wet skin at a certain temperature, and controlling the water content within a certain range;
s8, cutting a certain amount of strip skin sample, directly placing the strip skin sample into a glass material sampling tube, plugging quartz wool at two ends of the glass material sampling tube, sealing one end of the sample tube with a notch by using a passivated semi-permeable sealing piece, and placing the other end of the sample tube with the notch into a thermal desorption instrument sample tray according to the direction after confirming the sealing;
s9, starting a thermal desorption instrument, a GC-MS and a sniffing instrument, setting desorption temperature, desorption time and GC gas phase temperature rise program by thermal desorption, keeping for a period of time at an initial temperature, respectively raising the temperature to a set temperature at a certain rate in three stages, and keeping for a certain time;
s10, after relevant software is selected and set parameters are introduced, detection analysis is started, substances flowing out of a thermal desorption instrument are separated through a gas-phase capillary column and are split by a three-way splitter, one path of substances flows to a mass spectrometer MS for analysis, the other path of substances flows to a sniffing instrument for sniffing, a human nose faces to a horn mouth of the sniffing instrument, when the human nose can sniff a certain smell, the type of the smelled smell and the peak outlet time on 5977B mass spectrometry equipment are recorded, meanwhile, the numerical keys 1-6 representing the intensity of the smell are selected to be pressed on an analysis operation interface of the Sniffer9100 instrument, the numbers 1-6 represent the smell with different concentration levels, the larger the numbers represent the stronger the levels, and the sniffing operation is continued until the peak outlet is finished;
s11, searching substances corresponding to a peak spectrogram at the time point of manually distinguishing the smell by qualitative analysis software, determining the names of all the smelly monomer substances, the types of the smells, the intensity of the smells, namely the contribution degree to the dermis smell, finding out the offensive odor substances in the sample, selecting 10-20 substances with the largest contribution of the bad smell from the smell distinguishing result, and tracing the smell.
2. The method according to claim 1, wherein the sampling amount in S1 is 10-20 mg of the strip-like skin.
3. The method for analyzing the natural skin smell according to claim 1, wherein in the step S3, 50-52mg of the liquid skin material is weighed, the liquid skin material is put into a 10L Tedlar bag, and the liquid skin material is cleaned with high-purity nitrogen gas with the purity of 99.999% or more, and the liquid skin material is inflated 3L each time for 3 times.
4. The method for analyzing the natural leather odor according to claim 1, wherein in the step S4, 5L of high-purity nitrogen is filled after the cleaning is finished, the mixture is placed in a walk-in oven to keep the environment at 90 ℃ for 0.5 hours, 1L of gas is extracted by a Tenax tube at the flow rate of 200ml/min, 2 parallel samples are taken for each sample, and the Tenax sample tube is stored at a low temperature for later use.
5. The method for analyzing the natural skin smell according to claim 1, wherein in the step S5, 48-50mg of powdery dermatome material is weighed, put into a 10L Tedlar bag, and cleaned with high-purity nitrogen gas having a purity of 99.999% or more, and inflated 3L each time for 3 times.
6. The method according to claim 1, wherein in S7, the sample of white wet skin or blue wet skin tanned and cured from the pelt is dried at 50 ℃ with a moisture content of 15% ± 3%.
7. The method according to claim 1, wherein 19-20mg of the strip of skin sample is excised in S8.
8. The method according to claim 1, wherein in S9, the thermal desorption is performed at a desorption temperature of 90 ℃ for 30min, the gc gas phase temperature increasing program is performed at an initial temperature of 40 ℃ for 3min, the temperature is increased to 92 ℃ at a rate of 3 ℃/min, the temperature is increased to 160 ℃ at a rate of 5 ℃/min, the temperature is increased to 310 ℃ at a rate of 10 ℃/min, and the temperature is maintained for 20min.
9. The dermis smell tracing control method is characterized by comprising the following steps of:
a1, performing an odor substance analysis on the dermis final product and raw material according to the method of any of claims 1-8;
a2, screening a bill of materials with basically coincident odor types and peak time according to the sniffing spectrograms of the leather finished product and the related raw materials, and repeatedly testing and analyzing for a plurality of times, wherein analysis data with good result consistency are used as effective data;
a3, removing substances or skin materials which contribute obviously to the confirmed smell from the actual production formula, selecting skin materials without obvious smell influencing substances and re-formulating a sample process formula by using white wet skin or blue wet skin;
a4, carrying out odor substance sniffing analysis on the finished product and the related raw materials according to the method of any one of claims 1-8, and screening the raw materials repeatedly in the forward direction or the reverse direction, wherein the raw materials comprise skinned materials and white wet skin or blue wet skin;
a5, adjusting a process formula, producing a sample, tracing by sniffing analysis, improving the process formula, producing the sample, improving by sniffing analysis, and finally controlling the odor type, direction and odor intensity of the leather product.
10. The dermis smell trace source control method according to claim 9, wherein in A2, the trial and error analysis is performed 3 times, and the analysis data with good consistency is used as the effective data.
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| CA2210766A1 (en) * | 1996-07-19 | 1998-01-19 | The University Of Nottingham | Apparatus and methods for the analysis of trace constituents in gases |
| CN109521127A (en) * | 2018-12-25 | 2019-03-26 | 广州广电计量检测股份有限公司 | A kind of qualitative and quantitative analysis method carrying out Odor Evaluations to single odoring substance |
| CN111812239A (en) * | 2020-07-10 | 2020-10-23 | 广电计量检测（天津）有限公司 | Method for determining key odor substances in shoes |
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| CA2210766A1 (en) * | 1996-07-19 | 1998-01-19 | The University Of Nottingham | Apparatus and methods for the analysis of trace constituents in gases |
| CN109521127A (en) * | 2018-12-25 | 2019-03-26 | 广州广电计量检测股份有限公司 | A kind of qualitative and quantitative analysis method carrying out Odor Evaluations to single odoring substance |
| CN111812239A (en) * | 2020-07-10 | 2020-10-23 | 广电计量检测（天津）有限公司 | Method for determining key odor substances in shoes |
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| 气相色谱-质谱/嗅辨法同步分析地表水中特征异味物质初探;陈贝;刘劲松;叶伟红;王成;李沐霏;张胜军;冯元群;;环境化学(09);全文 * |
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