一般財団法人材料科学技術振興財団　MST List of Products and Services

The temperature-programmed desorption gas analysis method (TDS) is a mass spectrometry technique that directly heats a sample by irradiating it with infrared light and monitors the gases generated at each temperature. When analyzing samples that cannot absorb infrared light, such as glass substrates, it is possible to conduct the analysis by changing the sample stage from transparent to black. The black stage absorbs infrared light, raising its temperature, which in turn increases the temperature of the sample through thermal conduction, generating gases.

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TOF-SIMS allows for simultaneous elemental analysis and molecular information analysis of organic and inorganic substances through mass spectra obtained by locally analyzing specific areas, making it effective for evaluating foreign substances and micro-regions. This document summarizes examples of analysis in sub-micron order micro-regions. Samples that were sputter-processed with FIB on layered structures were measured using TOF-SIMS. Evaluation of sub-micron order micro-regions has been achieved.

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To investigate the causes of solder delamination, it is effective to conduct component analysis of the solder and the substrate interface. TOF-SIMS is a suitable method for evaluating delaminated areas because it can simultaneously analyze elemental composition and molecular information of organic and inorganic substances, as well as perform imaging analysis. This document presents a case study analyzing the cross-section of a delaminated solder area, confirming the distribution of substrate components, resin components, and organic components other than resin.

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Epoxy resin is excellent in heat resistance, chemical resistance, and insulation properties, and also has high mechanical strength, making it suitable for various applications such as insulation materials for electronic devices, adhesives, paints, and construction materials. However, due to the lack of solvent solubility, the analytical methods for structural determination are limited. This case presents an example of thermal decomposition GC/MS measurement of epoxy resin used as a sealing material for LEDs. The thermal decomposition products reflecting the structures of the main agent and curing agent were obtained, and this resin was estimated to be a bisphenol A/anhydride type epoxy resin.

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The HfZrOx film, which is attracting attention as a high-k material and ferroelectric, has its physical properties such as dielectric constant significantly affected by its crystal structure. Therefore, identifying the crystal structure and calculating the proportion of each crystal structure are important evaluation criteria. While these can typically be assessed using XRD and XAFS, combining these two methods can provide more detailed information, even in cases where detailed analysis is difficult with just one method. In this instance, we present a case of identifying the crystal structure of HfZrOx films and calculating the proportions of each crystal structure through combined analysis of XRD and XAFS.

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TOF-SIMS is an effective method for evaluating distribution, as it can simultaneously analyze elemental composition and molecular information of organic and inorganic substances, as well as perform imaging analysis. This document presents a case study analyzing the inner wall of a nozzle. The distribution of the nozzle surface and inner wall was confirmed, and the presence or absence of peaks at various locations was verified. Measurement method: TOF-SIMS Product field: Manufacturing equipment, parts, daily goods Analysis purpose: Composition distribution evaluation For more details, please download the document or contact us.

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UV-Vis is a method that measures the absorbance and transmittance of a sample by irradiating the sample with light divided by wavelength and measuring the intensity of the light that has passed through the sample. By measuring absorbance, it is possible to perform qualitative and quantitative analysis of the target components in the sample, as well as evaluate the wavelength characteristics of the sample. Additionally, transmittance measurements can assess the specific transmittance characteristics of components within the sample. - It is possible to obtain absorption and transmission spectra in the ultraviolet to visible to near-infrared regions (wavelength range approximately 190 nm to approximately 3000 nm).

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TOF-SIMS is an effective method for analyzing the distribution and penetration of target components in samples, as it can simultaneously perform elemental analysis and molecular information analysis of organic and inorganic substances, as well as image analysis. This document presents the results of image analysis of the "cross-section and surface" of hair and the "surface" of hair using siloxane-based hair care agents. It was confirmed that there are differences in the distribution of components between the cuticles of the tip and the root of the hair. Measurement method: TOF-SIMS Product field: Pharmaceuticals and cosmetics Analysis purpose: Composition evaluation, identification, composition distribution evaluation For more details, please download the document or contact us.

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When describing cleaning methods in brochures for medical devices, it is necessary to confirm the validity of those cleaning methods. In this case, as a verification experiment for the wiping method of medical devices, we applied bovine serum albumin (BSA), a blood model drug, to sheets of acetyl cellulose (TAC), SUS-made scalpels, and glass, and evaluated the residual components before and after wiping using TOF-SIMS. As a result, it was found that ethanol is more suitable than water for wiping BSA, and that the wiping effectiveness varies depending on the substrate. Measurement method: TOF-SIMS Product field: Medical devices and pharmaceuticals Analysis purpose: Composition evaluation, identification, composition distribution evaluation, failure analysis, defect analysis For more details, please download the materials or contact us.

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Silicon oxide films are widely used as gate dielectrics in MOS devices and as anode materials in lithium-ion secondary batteries, but it is known that the presence of intermediate oxides and the bonding states at the interface have a significant impact on device characteristics. XAFS measurements using synchrotron radiation can detect information from a depth of several tens of nanometers from the sample surface, allowing for non-destructive analysis of the structure and bonding states in both bulk and at the interface. This document presents a case study investigating the presence of intermediate oxides in silicon oxide films using XAFS.

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Biological samples and foods contain multiple triglycerides with different fatty acid compositions. In the analysis of total fatty acids, triglycerides are broken down into glycerol and fatty acids for measurement, but information about the combination of fatty acids in the triglyceride state is lost. Here, we present a case study that analyzes the fatty acid composition of triglycerides in food by directly analyzing them using GC/MS.

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One method to obtain the temperature profile of gases generated during sample heating is the EGA-MS method. However, this method introduces the generated gases into the mass spectrometer as a mixture without passing through a GC column, making it difficult to identify the compounds. In such cases, by trapping the gases once and performing GC/MS measurements using the heart-cut EGA method, it becomes possible to separate and identify the compounds. This example presents a case where polyvinyl acetate was measured using the heart-cut EGA method, revealing differences in the decomposition mechanisms depending on the heating temperature.

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Gallium oxide (Ga2O3) has a wider bandgap than SiC and GaN, and possesses excellent physical properties, making it a material of interest for high-efficiency, low-cost power devices. Controlling the impurity concentration, which affects the characteristics, is crucial in wafer development. This document presents a case study of quantitative analysis of metal elements in the vicinity of Ga2O3 films. TOF-SIMS allows for highly sensitive evaluation even in very shallow regions.

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TOF-SIMS allows mass imaging analysis of samples ranging from micrometers to centimeters in size. We conducted mass imaging analysis using TOF-SIMS on the cross-section of a capsule-type drug. We performed cross-section processing and present imaging examples focusing on the entire drug (approximately 7mm x 20mm) and a single granule inside it (approximately 500μm in diameter).

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Resveratrol is a type of polyphenol found in red wine and the skins of peanuts, and it is believed to have antioxidant and anti-inflammatory effects. It is known that resveratrol is absorbed in the stomach after ingestion and is rapidly metabolized. During the metabolic process, it becomes glucuronide and sulfate conjugates, but by converting those metabolites back to resveratrol for quantification, the amount of resveratrol absorbed can be calculated.

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In the field of semiconductors and their manufacturing processes, it is considered important to control inorganic and organic substances present in the environment. At MST, it is possible to collect components from the indoor atmosphere using the impinger collection method and analyze the types and quantities of corrosive components in the atmosphere. This time, we will introduce a case analyzed using the impinger collection-ion chromatography method.

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Products containing liquid in smartphone cases are being sold, but there have been incidents of skin injuries such as chemical burns due to leaks of this liquid, as well as cases of people experiencing health issues due to unpleasant odors. In response, the National Consumer Affairs Center issued a warning in April 2016, and in some cases, liquids with modified ingredients have been used. Here, we conducted non-target analysis using GC/MS on the liquid inside cases that were sold before the warning was issued to investigate what components are present.

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In the fabrication of Si-based semiconductor devices, various processes such as ion implantation and annealing are performed. It is considered important to confirm the degree of irradiation defects and the extent of crystallinity recovery before and after these processes in order to control the manufacturing process. Photoluminescence (PL) measurements at low temperatures are one effective means of investigating these aspects. An example of PL measurements of samples that underwent ion implantation on a Si substrate followed by annealing treatment is presented.

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TOF-SIMS is a highly effective method for investigating the causes of foreign substances, contamination, and discoloration in various processes, as it allows for localized analysis of specific areas and simultaneous analysis of elemental composition and molecular information of organic and inorganic substances through the obtained mass spectrum. Additionally, it enables image analysis, making the visualization of molecular information of organic substances possible. This document summarizes the analysis results of discoloration in clean suits, which are textile products. From the qualitative results obtained by TOF-SIMS, it was inferred that the discolored areas may be due to sebum.

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Hydrogen water is said to be able to remove active oxygen in the body, and attention is being drawn to its antioxidant effects. However, the amount of hydrogen that dissolves in water is minimal, and when left in the air, hydrogen gradually escapes. Additionally, because hydrogen is a very small molecule, it is known that some storage containers cannot maintain it for long periods. Therefore, the choice of storage container and method is considered important. This case presents the results of a GC (TCD) analysis showing how much hydrogen has escaped from hydrogen water transferred to a paper cup compared to a pouch-type storage container.

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Polyimide resin is excellent in heat resistance, chemical resistance, and toughness, and also has high insulation properties, making it used in various applications, including insulation materials for electronic devices. However, due to its almost non-existent solvent solubility, the analytical methods for structural determination are limited. This case introduces an example of thermal decomposition GC/MS measurement of commercially available polyimide resin. Multiple thermal decomposition products reflecting the polymer structure were observed in high-boiling components with long retention times, demonstrating that this method is a powerful means for structural determination.

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When conducting structural analysis of condensation-type polymers such as polyester, the conventional thermal decomposition GC/MS method may result in complex decomposition products that do not allow for structural estimation. In such cases, the reactive thermal decomposition GC/MS method, which involves the coexistence of derivatization reagents during thermal decomposition, is effective. This example introduces the thermal decomposition of polyethylene terephthalate (PET) in the presence of tetramethylammonium hydroxide. While numerous peaks were observed with the conventional thermal decomposition method, the reactive thermal decomposition method detected simpler decomposition products that reflected the monomer structure.

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TOF-SIMS identifies components based on the mass of molecular ions, eliminating the need for labels such as fluorescent substances, allowing for imaging evaluations without their influence. Additionally, by performing cross-sectional imaging, it is possible to assess distribution in the depth direction. In this study, a gel formulation of indomethacin was applied to rat skin for 2 hours, and the distribution of the permeated active ingredient was visualized. As a result, indomethacin was found to be highly concentrated at approximately 5μm on the stratum corneum surface, and the depth profile analysis showed that it was gradually permeating.

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When evaluating organic foreign substances present in resin, it may be difficult to assess them in their original state depending on the sample and analysis conditions. Therefore, we will introduce a case where evaluation became possible by cross-sectioning the resin to expose the foreign substances at the surface. After exposing foreign substances measuring several tens of micrometers that were mixed into epoxy resin through cross-sectioning, we evaluated them using TOF-SIMS. We were able to identify the components of the foreign substances and confirm their distribution.

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We conducted LC/MS analysis to compare how the components in commercially available tablet-type headache medications change before and after harsh testing. The LC/MS total ion chromatogram (TIC) revealed the presence of characteristic components that were not found in the new product after the harsh testing, and the precise mass was identified through the MS spectrum. Furthermore, by performing LC/MS/MS analysis, we were able to estimate the structure based on the information from fragment ions. The combination of LC/MS and LC/MS/MS allows for the structural estimation of unknown components.

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In this document, we prepared cross-sectional slices of mouse brain, heart, liver, kidneys, and teeth, and performed imaging using TOF-SIMS. The imaging area can range from approximately 10 μm to several centimeters, allowing for high-resolution analysis tailored to the focus of interest. Slices can be prepared according to the various organs of the organism, enabling imaging of their components. Additionally, this method is effective for visualizing the distribution of administered components within biological materials in pharmacokinetic studies and pharmaceutical research and development. Measurement method: TOF-SIMS Product field: Biotechnology, Pharmaceuticals Analysis purpose: Composition distribution evaluation For more details, please download the document or contact us.

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To evaluate the component distribution in mouse tibia, we prepared tibial sections and conducted imaging analysis using TOF-SIMS. The distribution of components derived from mice, such as K, Ca, calcium phosphate, and phospholipids, was confirmed. Since TOF-SIMS identifies components based on the mass of molecular ions, it does not require labeling substances like fluorescent materials, allowing for distribution evaluation without the influence of labeling agents. This technique can be applied to drug dynamics analysis and research on Drug Delivery Systems (DDS), enabling imaging of drug distribution within organs.

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To evaluate the components contained in commercially available tablet-type headache medications and their distribution, mass imaging analysis of the tablet cross-section was performed using TOF-SIMS. It was found that Al and Mg, derived from antacids, and the active ingredient acetylsalicylic acid were separated into two distinct regions. Additionally, as a harsh test, the tablets were placed in an environment of 50°C and 75% humidity for four weeks to assess changes in the components. This is effective for visualizing formulation research and stability evaluation. Measurement method: TOF-SIMS Product field: Biotechnology and Pharmaceuticals Analysis purpose: Composition evaluation, identification, and composition distribution evaluation For more details, please download the materials or contact us.

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If you want to qualitatively evaluate metallic foreign substances, analyzing only the very surface may result in information about the oxide film present on the surface of the foreign substance, and you may not obtain information about the foreign substance itself. By performing depth analysis using TOF-SIMS, it is possible to evaluate the composition and state of the foreign substance located deeper than the oxide film. This document presents case studies evaluating the state of three locations that are believed to contain aluminum-based foreign substances.

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In the quantitative and compositional evaluation of impurities in the semiconductor material SiGe using SIMS, the following considerations must be taken into account during analysis: ● If appropriate quantification corrections are not made according to the Ge concentration, the impurity quantification values may differ by more than 50% from the actual values. Standard samples corresponding to each composition are necessary for quantitative evaluation. ● It is known that the sputtering rates differ between Si and SiGe. In samples where the composition varies with depth, the sputtering rate changes with depth as well. At MST, high-precision compositional analysis is possible through the preparation of standard samples. Additionally, by using calibration curves, impurity analysis and sputtering rate corrections for each composition of SiGe can be performed.

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Gallium oxide (Ga2O3) has a higher band gap and superior physical properties compared to SiC and GaN, making it a material of interest for power devices that can be expected to be high-efficiency and low-cost. Controlling the impurity concentration, which affects the characteristics, is crucial in wafer development. This document presents a case study of impurity concentration analysis in Ga2O3 films. It is found that B and C are below the background level, while Si is present. MST offers a range of Ga2O3 standard samples and can quantify over 30 types of impurities.

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In the development of ultra-high voltage, low-loss SiC power devices that can be used in substations, controlling low carrier concentration is necessary, and SIMS analysis is effective for evaluating extremely low concentrations of impurities. In SIMS analysis, it is possible to evaluate extremely low concentrations by limiting the impurities to one element without simultaneously acquiring multiple elements. This document presents analysis examples that evaluate the extremely low concentration range of impurities in SiC with ultra-high sensitivity, which has been difficult to assess conventionally.

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When analyzing samples containing nitrogen compounds using GC, simultaneous measurement with MS (mass spectrometer) and NPD (nitrogen-phosphorus detector) allows for the detection of components that do not appear as peaks in the MS, enabling the acquisition of MS spectra from their retention times for qualitative analysis. In this case, a sample containing trace amounts of the nitrogen-containing compound trimethylamine was measured using GC/MS/NPD. A peak that was buried in the baseline in the MS was confirmed by the NPD, allowing for the qualitative identification of trimethylamine from the mass spectrum at the same retention time.

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The sample concentration needle is a device that concentrates volatile components by sucking them from vials or sampling bags and adsorbing the volatile components passing through the needle onto an adsorbent medium, which is then introduced into GC/MS. There are different adsorbent media available, such as "for organic solvents," "for fatty acids," and "for amines," which are used depending on the target components. In the headspace method used for the analysis of volatile components, it is common to heat the sample to obtain sensitivity; however, in analyses using the sample concentration needle, heating is not necessary, allowing only the volatile components to be supplied for GC/MS analysis at room temperature.

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In the process of confirming metal contamination adhered to the wafer surface after the formation of the SiO2 film, a method has traditionally been used where the SiO2 film is dissolved in acid as a pre-treatment for analysis, followed by the analysis of the solution. This method results in analysis that combines metal contamination on the very surface with that within the SiO2 film, making it unsuitable for analyzing only the metal contamination on the very surface. In MST, it is possible to evaluate the metal contamination elements on the wafer's very surface by dissolving only the metal elements adhered to the very surface without dissolving the SiO2 film during the pre-treatment.

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Color printers use ink to print on the surface of paper. The ink contains dyes and pigments, which have characteristic molecular information based on their colors. By visualizing this molecular information, it becomes possible to obtain information about the distribution of ink components on the paper surface and how deeply the ink components penetrate into the paper cross-section. Below, I will summarize the "imaging results of the paper surface" visualized by TOF-SIMS. TOF-SIMS can perform image analysis of molecular information ranging from 10 μm to 3 cm square.

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Organic EL (OLED) is used in various applications such as high-definition display panels and lighting, and the demand for layer structure analysis and degradation analysis is increasing. However, since it is formed by combining various organic materials, elemental analysis alone can only capture a portion of the phenomena. This document presents a case study where depth direction analysis data of OLED was obtained using TOF-SIMS, and insights into the degradation of the sample were gained through MSDM (Mass Spectra Depth Mapping).

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In depth profiling analysis using TOF-SIMS, if the positional information on the plane (x, y) is ignored, mass spectra exist at each depth (z), resulting in three-dimensional data of depth, mass, and spectral intensity. The visualization of this three-dimensional data as a single image is called MSDM (Mass Spectra Depth Mapping) representation.

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Solid polymer electrolyte fuel cells (PEFC) are attracting attention for their high output at room temperature, making them suitable for automotive applications, home cogeneration, and mobile use. In this study, we simulated the degradation of solid polymer electrolyte membranes using Fenton's reagent (a solution of hydrogen peroxide and iron ions) and investigated the degradation byproducts in the solution. Composition information of the degradation byproducts was obtained using LC/MS, while information on the eluted ions was acquired using IC.

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Organic EL (OLED) is used in various applications such as high-definition display panels and lighting, and the demand for layer structure analysis and degradation analysis is increasing. However, since it is formed by combining various organic materials, elemental analysis alone can only capture some phenomena. This document presents a case study where depth direction analysis data of OLED was obtained using TOF-SIMS and analyzed through MSDM (Mass Spectra Depth Mapping).

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GaN-based high electron mobility transistors, known as GaN HEMTs (High Electron Mobility Transistors), achieve a two-dimensional electron gas layer through an AlGaN/GaN heterostructure, resulting in high electron mobility. This document presents a case study of the disassembly and evaluation of commercially available GaN HEMT devices. Using HAADF-STEM, we confirmed the crystallographic integrity near the AlGaN/GaN interface. Additionally, we assessed the compositional distribution using EELS. Measurement methods: TEM, EELS. Product field: Power devices. Analysis purpose: Structural evaluation, film thickness evaluation. For more details, please download the document or contact us.

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GaN, which is being utilized as a power device and optical device, has a hexagonal wurtzite structure and exhibits crystallographic asymmetry (Ga polarity and N polarity) in the c-axis direction. The growth processes of epitaxial films differ between Ga polarity and N polarity, and the surface physical properties and chemical reactivity of the crystal also vary. In this document, the polarity of GaN was evaluated through annular bright field (ABF)-STEM observation. As a result, the positions of the Ga sites and N sites were identified, allowing for a visual clarification of the characteristics of Ga polarity and N polarity. Measurement method: TEM Product fields: Power devices, optical devices Analysis objectives: Shape evaluation, structural evaluation, thickness evaluation For more details, please download the document or contact us.

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In the analysis of foreign substances, it is important to appropriately select the analytical methods based on the size of the foreign substance, the expected materials, and the condition of the substrate. By combining techniques such as optical microscopy, elemental analysis (XRF), and bonding state analysis (XRD, FT-IR), it is possible to gain insights into the multiple components contained in the powder. This document presents examples of qualitative analysis of powder foreign substances using the aforementioned methods.

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When analyzing additives used in polymer materials such as resin products, it is necessary to separate the polymer materials from the additives. We will introduce a case where a sample pre-treated using the "dissolution-reprecipitation method," which involves dissolving commercially available resin products in a solvent and then precipitating the polymer components to extract the additive components, was analyzed. The results of the LC/MS analysis indicated that a component with a high abundance (m/z=548.50) was estimated to be a type of phenolic antioxidant through LC/MS/MS analysis.

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Many additives, including plasticizers, are used in polymer materials such as resin products. We present a case study on the qualitative analysis of additives contained in commercially available PVC resin. The components eluted by immersion in an organic solvent were qualitatively analyzed using LC/MS. As a result, components estimated to be DEHP (DOP) as a plasticizer and epoxy fat (plasticizer/stabilizer) were detected. By using standard samples, it is also possible to quantify each detected additive component.

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