JP2014016273A - Deterioration test method for specimen - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a versatile method of performing a deterioration test on a specimen.SOLUTION: The method of performing a deterioration test on a specimen comprises: a measurement process (Step S201) for measuring a chemical change of a marker in a specimen containing the marker which chemically reacts with deterioration or of a component derived from the marker; and an estimation process (Step S201, S203) for estimating a deterioration state of the specimen on the basis of the result measured through the measurement process. For example, material imparting prescribed performance to the specimen (such as light stabilizer) can be used as the marker.

Description

  The present invention relates to a specimen deterioration test method for measuring a deterioration state of a specimen.

  An organic compound may partially change to another substance or change its characteristics over time. A chemical change that occurs with the passage of time is used as an index for measuring the deterioration state of the organic compound, and the deterioration state of the organic compound is measured.

  For example, Patent Document 1 describes a deterioration test method in which a sealing material is dissolved with a solvent and the deterioration of the sealing material is measured based on the elution amount of the urethane component of the sealing material.

JP 2004-137383 A

  However, the chemical change is different for each specimen to be measured for deterioration. For this reason, the conventional deterioration test method has low versatility because it is necessary to grasp a chemical change for each specimen and to perform measurement according to the chemical reaction of the specimen. For this reason, a highly versatile degradation test method is desired.

  Therefore, the present invention solves such problems of the prior art, and an object of the present invention is to provide a highly versatile test method for a test object.

  In order to solve the above problems, the test method for deterioration of a test object according to the present invention measures a chemical change in a marker of a test object including a marker that chemically reacts due to deterioration, or a marker-derived component of the marker. And a estimating step for estimating the deterioration state of the test object based on the result measured in the measuring step.

  In this invention, the chemical change of the marker contained in a test object or a marker-derived component is measured. Based on the measured result, the deterioration state of the test object is estimated. Thus, the deterioration state of a test object can be estimated by measuring the chemical change about a marker or a marker-derived component. That is, since it is only necessary to measure a chemical change with respect to the marker or the marker-derived component regardless of the type of the test object, this is a highly versatile test method for test object deterioration.

  The marker is preferably a substance that imparts a predetermined performance to the test object. In this case, the marker can serve both as a function of giving a predetermined performance to the test object and a function of measuring deterioration of the test object. Thus, it is not necessary to add a substance only for measuring the deterioration state to the test object, and the efficiency is high.

  The marker is preferably at least one of an antioxidant, a light stabilizer, an ultraviolet absorber, and a plasticizer. The deterioration state of the test object can be measured based on these substances that impart predetermined performance to the test object or the components derived from these substances, and the efficiency is high.

  The test object is preferably an organic compound. Thereby, the deterioration state of an organic compound can be measured.

  The organic compound is preferably a building material used for building construction. Thereby, the deterioration state of a building material can be measured.

  The building material is preferably at least one of a sealing material, an adhesive, a paint, and a waterproof sheet. Thereby, the deterioration state of these materials can be measured and it can become a standard of maintenance work etc.

  In the measurement step, it is preferable to measure the chemical change of the marker or the marker-derived component using a pyrolysis gas chromatography method or pyrolysis gas chromatography mass spectrometry. Thereby, the chemical change of a marker or a marker-derived component can be accurately measured using these methods.

  In the measurement step, it is preferable to measure a chemical change of a marker or a marker-derived component using a solvent extraction method. Thereby, the chemical change of a marker or a marker-derived component can be accurately measured using this method.

  In the measurement step, it is preferable to further measure the chemical change of the marker or the marker-derived component using a gas chromatography method or a gas chromatography mass spectrometry method. Thereby, the chemical change of a marker or a marker-derived component can be measured with higher accuracy using these methods.

  In the measurement step, it is further preferable to measure a chemical change of the marker or the marker-derived component using a nuclear magnetic resonance method. Thereby, the chemical change of a marker or a marker-derived component can be measured with higher accuracy using these methods.

  ADVANTAGE OF THE INVENTION According to this invention, the deterioration test method of the test object with high versatility can be provided.

It is process drawing which shows the preparatory process of the deterioration test method of a to-be-tested object. It is a figure which shows schematic structure of a pyrolysis gas chromatography mass spectrometer. It is a figure which shows the chromatogram which shows the peak of a light stabilizer. It is a figure which shows the peak area ratio of the light stabilizer for every accelerated deterioration time. It is a graph which shows the relationship between a peak area ratio and accelerated deterioration time. It is process drawing which shows the test process of the deterioration test method of a to-be-tested object.

  Hereinafter, embodiments of a test method for deterioration of a test object according to the present invention will be described in detail with reference to the drawings.

  The inventors of the present invention, when a marker that reacts chemically due to deterioration (substance other than the specimen itself) is contained in the specimen, the marker contained in the specimen, not the specimen itself It was also found that the deterioration state of the test object can be estimated by measuring the chemical change of the marker-derived component. This is based on the fact that the marker changes as the test object deteriorates. Here, the marker-derived component refers to a substance in which the marker has changed due to deterioration, a substance generated by the deterioration of the marker, or the like.

  In this embodiment, a deterioration test method for measuring a deterioration state of a sealing material mainly composed of polyether-based polyurethane as a test object will be described. In addition, it is assumed that the sealing material contains a light stabilizer (hindered amine compound: HALS) as a marker. The light stabilizer has a function of improving light resistance and weather resistance with respect to the sealing agent.

<Preparation process>
First, a preparation process is performed before performing a deterioration test of a sealing material as a test object. As shown in FIG. 1, a sealing material used in the preparation process is created (step S101). Here, a plurality of sealing materials, which are the same as the test object to be subjected to the deterioration test, are made of a polyether-based polyurethane, added with a light stabilizer, and formed into a sheet shape.

  Next, an accelerated deterioration test is performed on the plurality of sealing materials to obtain a plurality of sealing materials having different accelerated deterioration test times (step S102). Here, as an example, the accelerated degradation test conditions are a temperature of 80 ° C. and a humidity of 5% RH, and the accelerated degradation test times are 2000 hours, 4000 hours, and 6000 hours.

  Next, the chemical change of the light stabilizer is measured for the sealing material not subjected to the accelerated deterioration test and the sealing material after the accelerated deterioration test (step S103). Here, the light stabilizer decreases as the sealing material, which is the test object, deteriorates. For this reason, the content of the light stabilizer decreases as the sealing material has a longer accelerated deterioration test time.

  In the present embodiment, the content of the light stabilizer is analyzed by pyrolysis gas chromatography mass spectrometry (PyGC / MS method). Here, the pyrolysis gas chromatography mass spectrometer will be described. As shown in FIG. 2, the pyrolysis gas chromatography mass spectrometer 10 includes a sample injection section 2, a pyrolysis apparatus 3, a column 4, a splitter 5, a detector 6, an interface 7, and a mass spectrometer 8. Composed. A sealing material X to be analyzed is introduced into the sample injection unit 2. The thermal decomposition apparatus 3 rapidly heats and decomposes the sealing material X introduced from the sample injection unit 2.

  Gas generated by heating and decomposition of the sealing material X is introduced into the column 4 from the thermal decomposition apparatus 3 by the carrier gas 1. When performing gas chromatographic analysis, gas is introduced into the detector 6 through the splitter 5, and analysis is performed in the detector 6. Further, gas is introduced into the interface 7 through the splitter 5 and then introduced into the mass spectrometer 8, and mass analysis is performed in the mass spectrometer 8.

  As an example, as shown in the chromatogram shown in FIG. 3, a peak indicating a light stabilizer is detected among peaks of a plurality of substances. The content of the light stabilizer can be represented by the area of the peak derived from the light stabilizer. Therefore, the peak of the sealing material that has not been subjected to the accelerated deterioration test, the sealing material that has been subjected to the accelerated deterioration test for 2000 hours, the sealing material that has been subjected to the accelerated deterioration test for 4000 hours, and the sealing material that has been subjected to the accelerated deterioration test for 6000 hours are listed in order. The area becomes smaller.

  Next, using the detection results of the pyrolysis gas chromatography mass spectrometer performed for each sealing material, the peak area of the light stabilizer in the sealing material not subjected to the accelerated deterioration test and the light in the other sealing materials A ratio with the area of the peak derived from the stabilizer is obtained (step S104). Here, as shown in FIG. 4, when the area of the peak derived from the light stabilizer in the sealing material not subjected to the accelerated deterioration test is “1”, the light stabilizer of the sealing material subjected to the accelerated deterioration test for 2000 hours. The ratio of the area of the peak derived from “0.57”, the ratio of the area of the peak derived from the light stabilizer of the sealing material subjected to the accelerated deterioration test for 4000 hours was “0.28”, and the accelerated deterioration test was performed for 6000 hours. It is assumed that the ratio of the peak area derived from the light stabilizer of the sealing material was “0.038”.

  Next, the graph shown in FIG. 5 is obtained by associating the obtained peak area ratio with the accelerated deterioration time (step S105). In the graph shown in FIG. 5, the horizontal axis represents the accelerated deterioration time, and the vertical axis represents the peak area ratio. And the straight line L which shows the relationship between accelerated deterioration time and a peak area ratio is calculated | required so that it may complement between each accelerated deterioration time for which the peak area ratio was calculated.

  Here, the deterioration state of the substance after the accelerated deterioration test is correlated with the deterioration state with the passage of actual time. Therefore, based on the straight line L shown in FIG. 5, the accelerated deterioration time can be obtained from the numerical value of the peak area ratio of the light stabilizer of the sealing material. And the deterioration state of the sealing material accompanying the progress of actual time can be estimated from this accelerated deterioration time.

  The service life limit of the sealing material is arbitrarily set by the user or designer. Generally, it is often set by physical indicators such as repeated fatigue and maximum strength. Therefore, the accelerated deterioration time to reach the arbitrarily set service life is grasped in advance.

<Test process>
Next, the deterioration test of the sealing material which is a test object is performed. Here, as an example, the deterioration state of the sealing material collected from the building is estimated. As shown in FIG. 6, first, the chemical change of the light stabilizer contained in the sealing material that is the test object is measured (step S201: measurement process). In the present embodiment, the content of the light stabilizer is analyzed by pyrolysis gas chromatography mass spectrometry as described above.

  Next, using the detection results of the pyrolysis gas chromatography mass spectrometer, the area of the peak derived from the light stabilizer in the sealing material that has not been subjected to the accelerated deterioration test described above, and the light stability in the sealing material that is the test object A ratio with the area of the peak derived from the agent is obtained (step S202: estimation step).

  Next, the deterioration state of the sealing material that is the test object is estimated using the calculated area ratio of the peak derived from the light stabilizer (step S203: estimation step). As an example, based on the calculated area ratio of the peak derived from the light stabilizer and the graph corresponding to the ratio of the peak area and the accelerated deterioration time shown in FIG. 5, the ratio of the accelerated deterioration time and the actual elapsed time of the test object Therefore, the acceleration magnification can be obtained. The service life can be obtained by the product of an accelerated deterioration time and an acceleration magnification that reach an arbitrarily set service life limit. In addition, the lifetime up to the service life can be obtained from the difference between the service life and the actual elapsed time.

  The present embodiment is configured as described above, and it is possible to estimate the deterioration state of the sealing material that is the test object by measuring the chemical change of the light stabilizer included in the sealing material that is the test object. it can. That is, since it is only necessary to measure a chemical change with respect to the light stabilizer regardless of the type of the test object, this is a highly versatile test method for test object deterioration.

  The light stabilizer is for preventing the sealing material from being deteriorated by light. As described above, the light stabilizer has both a function of imparting a predetermined performance to the test object and a function of measuring deterioration of the test object. Therefore, it is not necessary to add a substance only for measuring the deterioration state to the test object, and the efficiency is high.

  Since the deterioration state of the sealing material used for building construction can be measured, it is easy to repair and design the building.

  By using pyrolysis gas chromatography mass spectrometry, the chemical change of the light stabilizer can be accurately measured.

  Although one embodiment of the present invention has been described above, the present invention is not limited to the above embodiment. For example, as a chemical change of the marker, the content of the light stabilizer (marker) that changes chemically due to deterioration is measured, but in addition to this, a chemical change of the marker-derived component is measured. May be.

  Moreover, although the light stabilizer was demonstrated to the example as a marker added to a test object, it is not limited to this, What is necessary is just to change chemically by deterioration. For example, the marker may be an antioxidant, an ultraviolet absorber, or a plasticizer. Furthermore, as markers, flame retardants, colorants, nucleating agents, clearing agents, heavy metal deactivators, antistatic agents, lubricants, design imparting agents, coupling agents, fillers, adhesion imparting agents, storage stability Improving agent, catalyst, cross-linking agent, cross-linking aid, vulcanizing agent, vulcanization accelerator, softener, reinforcing agent, preservative, anti-fungal agent, anti-algae agent, tackifier, foaming agent, processing aid, release agent You may use a shape agent, a latex compounding agent, or a solvent.

  Moreover, although the sealing material was demonstrated to the example as a test object, things other than sealing may be used. The test object may be, for example, an organic compound or a building material made of an organic compound. Moreover, as a building material, an adhesive agent, a coating material, a waterproof sheet, etc. can be used, for example.

  Moreover, when measuring the chemical change of the marker, pyrolysis gas chromatography mass spectrometry was used, but pyrolysis gas chromatography or solvent extraction may be used. Moreover, when measuring the chemical change of the marker, in addition to the solvent extraction method, a gas chromatography method or a gas chromatography mass spectrometry method may be used. Moreover, when measuring the chemical change of the marker, in addition to the solvent extraction method, a nuclear magnetic resonance method may be used. Even if these measurement methods are used, the chemical change of the marker can be accurately measured.

  DESCRIPTION OF SYMBOLS 1 ... Carrier gas, 2 ... Sample injection part, 3 ... Thermal decomposition apparatus, 4 ... Column, 5 ... Splitter, 6 ... Detector, 7 ... Interface, 8 ... Mass spectrometer, 10 ... Thermal decomposition gas chromatography mass spectrometry apparatus , X ... Sealing material.

Claims (10)

A measurement step of measuring a chemical change in the marker of the test object including a marker that chemically reacts due to deterioration, or a marker-derived component of the marker;
Based on the result measured in the measurement step, an estimation step for estimating the deterioration state of the test object,
Deterioration test method for specimens including   The test object deterioration test method according to claim 1, wherein the marker is a substance that imparts a predetermined performance to the test object.   The test method for deterioration of a test object according to claim 2, wherein the marker is at least one of an antioxidant, a light stabilizer, an ultraviolet absorber, and a plasticizer.   The deterioration test method for a test object according to any one of claims 1 to 3, wherein the test object is an organic compound.   The test method for deterioration of a test object according to claim 4, wherein the organic compound is a building material used for building a building.   The test method for deterioration of a test object according to claim 5, wherein the building material is at least one of a sealing material, an adhesive, a paint, and a waterproof sheet.   The said measurement process measures the chemical change of the said marker or the said marker-derived component using a pyrolysis gas chromatography method or a pyrolysis gas chromatography mass spectrometry. The deterioration test method for a test object according to any one of the above.   In the said measurement process, the deterioration test method of the test object as described in any one of Claims 1-6 which measures the chemical change of the said marker or the said marker origin component using a solvent extraction method. .   The test according to claim 8, wherein in the measurement step, a chemical change of the marker or the marker-derived component is further measured using gas chromatography or gas chromatography mass spectrometry. Deterioration test method for objects.   The test method according to claim 8, wherein in the measurement step, a chemical change of the marker or the marker-derived component is further measured using a nuclear magnetic resonance method.

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