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

Organic contamination during the manufacturing process significantly affects product performance. In the analysis of organic substances in liquid samples, such as rinse solutions in the cleaning process, evaluations can be conducted using Total Organic Carbon (TOC) analyzers and Liquid Chromatography-Tandem Mass Spectrometry (LC/MS/MS). Here, we present an example of evaluation using TOC and LC/MS/MS for NPnEO (Nonylphenol Ethoxylate), one of the industrial surfactants.

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The electrolyte of lithium-ion secondary batteries is known to decompose and gasify due to repeated charging and discharging. By using GC-TCD and GC/MS, the decomposed gas components can be detected with high sensitivity. GC-TCD can analyze the composition ratios of eight components (H2, O2, N2, CO, CH4, CO2, C2H4, C2H6), while GC/MS can qualitatively analyze various decomposition products. We also support gas analysis in not only laminate-type cells but also coin-type and prismatic cells, as well as cells using ionic liquids.

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As exemplified by the separators used in lithium-ion secondary batteries, the microstructure of materials, such as porosity and shape, significantly influences the characteristics and functions of products. When materials have a low softening point, such as resins or polypropylene (PP), they may be damaged by electron beam irradiation during observation, leading to changes in their original structure. We will present a case where ultra-low acceleration SEM observation at an acceleration voltage of 0.1 kV was used to suppress alteration and evaluate the surface morphology of the sample in detail.

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Foods such as pork and eggs are rich in vitamin B1 (thiamine, HET) and vitamin B2 (riboflavin). These are often present as derivatives such as phosphate esters. The content of vitamin B1 and vitamin B2 can be quantified by performing enzymatic treatment as a pretreatment to convert them to their free forms, followed by analysis using HPLC with a fluorescence detector. Although vitamin B1 itself is not fluorescent, it is possible to detect fluorescence by reacting it with a red blood salt alkaline solution in a post-column method, converting it to the oxidized form of thiocrome.

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Water-soluble vitamins can be divided into about 10 types based on their functions in the body. For example, vitamin B1 consists of multiple components (thiamine, hydroxymethylthiazole, and its derivatives) that have the same function, and the total amount of these components determines the content. In this case, a multivitamin supplement was measured using LC/MS/MS, and qualitative analysis was conducted for each component of five types of water-soluble vitamins. By performing simultaneous analysis, it is possible to efficiently confirm the presence or absence of the target components. Analysis of other water-soluble vitamins is also possible, so please feel free to inquire.

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Geosmin and 2-methylisoborneol (2-MIB) are produced by cyanobacteria or actinomycetes and are considered substances that cause odor and taste disturbances in drinking water sourced from surface water such as dams, lakes, and rivers, as well as being known as substances that cause musty odors. This case presents the results of measuring geosmin and 2-MIB contained in water. Detection at ppt (ng/L) levels is possible using GC/MS.

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Linear alkylbenzene sulfonic acid and its salts (LAS) are considered substances of concern due to their potential impact on living organisms. Therefore, they have been added to the environmental standards related to the conservation of aquatic organisms within the environmental standards concerning the preservation of living environments affected by water pollution, and a standard value has been established (March 27, 2013). Since approximately 90% of the usage of LAS is for household detergents, measurements were conducted on existing household detergents and household wastewater, and a comparison of the distribution of LAS alkyl chain lengths (C10 to C14) was performed.

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Formaldehyde and volatile organic compounds (VOCs: Volatile Organic Compounds, such as toluene, xylene, and para-dichlorobenzene) emitted from building materials, adhesives, and preservatives are considered to be causes of sick house syndrome and sick school syndrome. This report introduces a case study analyzing the concentrations of formaldehyde and toluene in indoor air sampled using passive methods.

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Polycarbonate (PC) is a type of thermoplastic that has excellent transparency, impact resistance, and heat resistance, and is widely used as a material for solar panels, eyeglass lenses, CDs, automotive parts, and medical devices. In this study, TOF-SIMS analysis was conducted using GCIB (Ar cluster) with a sputter ion beam to evaluate the degradation layer on the surface of PC. *Note: GCIB stands for Gas Cluster Ion Beam.*

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In 2002, it was announced that acrylamide, which may have carcinogenic properties, is generated when foods high in carbohydrates are heated at temperatures above 120°C (Figure 1), attracting attention. According to the Ministry of Agriculture, Forestry and Fisheries (MAFF) website, acrylamide is found in many foods, including fried potato snacks, toast, and coffee. At MST, we participate in the proficiency testing FAPAS and confirm that the absolute value of the z-score is 2 or below (satisfactory), allowing us to accurately quantify acrylamide in food using LC/MS/MS.

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It has been announced that 4-t-octylphenol will be newly added as a monitoring item in the environmental standards related to the conservation of aquatic organisms, among the environmental standards concerning the preservation of living environments affected by water quality pollution (March 27, 2013). 4-t-octylphenol is considered to potentially hinder the habitat or growth of aquatic organisms through environmental pollution, and the guideline values are set between 0.0004 to 0.004 mg/L depending on the water area and type. MST provides a comprehensive service that includes the lending of specialized containers and measurement.

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Among the environmental standards related to the preservation of living environments concerning water quality pollution, 2,4-dichlorophenol has been newly added as a key monitoring item for the environmental standards related to the conservation of aquatic organisms (March 27, 2013). 2,4-dichlorophenol is considered to potentially hinder the habitat or growth of aquatic organisms through environmental pollution, with guideline values set between 0.003 and 0.03 mg/L depending on the water area and type. MST offers a comprehensive service that includes the lending of specialized containers and measurement.

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Organic acids such as citric acid and malic acid are widely used in various fields, including the semiconductor industry as additives in etching and plating solutions, as well as in food as sour agents and emulsifying stabilizers. In particular, the concentration of organic acids in plating solutions changes over time during use, and this balance affects the quality of the plating, making precise control important. Here, we will introduce a case study of organic acid analysis using IC (ion chromatography).

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The state of the water-repellent surface in water-repellent treatment differs based on whether fluorine-based compounds are distributed in an island-like manner or uniformly. Therefore, we conducted observations of the distribution of fluorine-based compounds using TOF-SIMS. As a result, it was found that they are distributed unevenly. Additionally, by performing qualitative analysis in a 1μm square area, it was determined that the fluorine-based film is Krytox. Measurement method: TOF-SIMS Product field: Electronic components and daily necessities Analysis purpose: Composition evaluation, identification, composition distribution evaluation For more details, please download the materials or contact us.

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Tetramethylammonium hydroxide (TMAH) is used as a developing solution and etching solution in semiconductors. When measuring the concentration of TMAH solution used in Si etching solutions, the large amount of dissolved Si can become an impurity and affect the measurement results. However, evaluation using the IC (ion chromatography) method allows for quantitative analysis of TMAH concentration without being influenced by Si.

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Incidents of foreign substances contaminating food have frequently caused public uproar, and in a Cabinet Office survey conducted in January 2014 regarding the promotion of consumer administration, the consumer issue that garnered the most attention was "food safety." To ensure food safety, MST conducts highly accurate analyses for cause investigation, making it possible to determine whether pesticide levels in food exceed the acceptable daily intake. An analysis of miso soup with a small amount of the herbicide glyphosate added revealed that the contaminant could be detected without overlooking any components.

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In controlling properties such as adhesion and wettability of polymer films, it is very important to quantitatively evaluate the polar functional groups (alcohol groups) present on the surface. XPS is optimal for quantitative evaluation; however, it is difficult to separate and quantify the adjacent oxidation state (C-O-C) and hydroxyl state (C-OH). In MST, after selectively reacting only the alcohol groups using a chemical modification method on polyvinyl alcohol (PVA), it is possible to quantify them using XPS. We present a case where the alcohol groups in PVA were chemically modified and evaluated using trifluoroacetic anhydride (TFAA). Measurement method: XPS, chemical modification Product fields: Electronic components, daily necessities Analysis purpose: Composition evaluation, identification, chemical bonding state evaluation For more details, please download the materials or contact us.

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Polycarbonate (PC) is a type of thermoplastic that has excellent transparency, impact resistance, and heat resistance. It has been reported that degradation occurs due to hydrolysis, leading to the generation of the raw material bisphenol A (BPA). Particularly in solar panels, it is important to understand how the surface of the material changes under UV (ultraviolet) irradiation. Below, we present a case study that evaluated the degree of degradation of the PC surface due to UV irradiation using TOF-SIMS.

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As electronic devices are increasingly used in various everyday locations, ensuring the reliability of products has become important. Since it is possible for the copper used in the wiring of printed circuit boards to migrate and cause defects in high temperature and high humidity environments, it is crucial to evaluate the components that promote migration. This case study introduces an example of quantitative analysis of cation components eluted from printed circuit boards using ion chromatography (IC). Thus, IC is an effective method for evaluating the corrosion components on the surface of solid samples.

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Nonylphenol ethoxylate (NPnEO) is known to produce nonylphenol (NP) as a degradation product. NP is considered an endocrine disruptor, and due to concerns about its impact on living organisms, it has been added to the environmental standards related to the conservation of aquatic organisms within the environmental standards concerning the preservation of living environments affected by water pollution, with a standard value established (August 22, 2012). To understand the trends of NP, for which a standard value has been set, it is necessary to also monitor the trends of its precursor, NPnEO, leading to an increased demand for analysis.

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Imaging SIMS is effective for obtaining spatial distribution information of hydrogen and impurities at ppm levels. By using a RAE (Resistive Anode Encoder) detector for projection-type imaging SIMS, it is possible to obtain distribution images with a larger diameter and deeper regions compared to the commonly used scanning methods in imaging analysis.

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1. Measure the spreading resistance (Ω) directly beneath the surface of the sample that has been polished at an angle by contacting two probes. 2. Create a calibration curve from the measurements of the standard sample and use it to convert the resistance to resistivity (Ω·cm). Additionally, perform distribution corrections as needed through volume correction. *) The calibration curve varies depending on the conductivity type (p-type/n-type) and the surface orientation. 3. Use the relationship between resistivity and carrier concentration*) to calculate the carrier concentration (/cm³).

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SR measurement involves diagonally polishing the sample and moving two probes in contact with the sample surface while measuring the electrical resistance directly beneath. The depth from the sample surface at a certain measurement point is determined by the product of the value of Sinθ (bevel angle) when the angle of diagonal polishing of the sample is θ and the distance from the bevel edge to that measurement point. The distance from the bevel edge is calculated as [X-step] × [number of measurement points].

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Acrylic resin has superior processability, transmittance, and safety compared to silicate glass, making it widely used as organic glass for windows in aircraft and automobiles, optical instruments such as lenses and prisms, medical materials, daily necessities, and crafts. Mass spectra of representative standard acrylic reagents were obtained using TOF-SIMS. In MST, by comparing the mass spectrum of the analyte with that of the standard reagent, it is possible to estimate the acrylic resin from the detected fragment ions.

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When conducting elemental analysis, it is possible to establish an efficient evaluation plan by first using XRF analysis to non-destructively examine the elements contained in the target before moving on to detailed analysis. In this case, we present data from XRF analysis conducted on blades for metal cutting. By performing surface analysis over a wide range on the order of millimeters, we roughly examined the distribution of metallic elements in the material and estimated the metal composition by calculating the elemental composition from the XRF point analysis results of characteristic areas. Measurement method: XRF Product field: Manufacturing equipment, parts, daily necessities 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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Ergothioneine is an amino acid homolog discovered in ergot, known for its strong antioxidant properties and anti-photoaging effects, and research and development are ongoing in the fields of medicine and beauty. Since humans cannot produce ergothioneine in their bodies, they obtain it from sources rich in it, such as certain mushrooms. An analysis of eight types of mushrooms using LC/MS/MS revealed that ergothioneine was detected in all of them. Quantitative analysis was conducted on three types of mushrooms from the Pleurotaceae family, which are said to have high ergothioneine content.

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In recent years, with the increase in health consciousness, various health foods have been attracting attention. One of these, Du Zhong tea, is suitable for individuals with high blood pressure and is designated as a Food for Specified Health Uses (Tokubetsu Hōshō). In this case study, Du Zhong tea was analyzed using LC/MS/MS, and five polyphenols were detected: geniposidic acid, chlorogenic acid, asperuloside, p-coumaric acid, and quercetin. Among these components, geniposidic acid, one of the glycosides from Du Zhong leaves, serves as a benchmark for the effective ingredient of Foods for Specified Health Uses.

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The vitamin C contained in food refers to the total amount of reduced L-ascorbic acid and oxidized dehydroascorbic acid. Its applications include not only nutritional enhancement but also use as an antioxidant. When measuring vitamin C using HPLC, it is common to convert the oxidized form after noting that dehydroascorbic acid has no UV absorption, and then derivatize it for measurement. By quantifying dehydroascorbic acid using LC/MS/MS, it becomes possible to simplify the pretreatment and analyze with high sensitivity.

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This document presents a case study of the quantitative analysis of free amino acids contained in alcoholic beverages using the OPA post-column method. It was found that sake, a brewed alcoholic beverage, contains a rich and well-balanced variety of free amino acids, including alanine and arginine. Furthermore, when comparing three sake products, differences were observed in both the content and balance of free amino acids. Although draft beer is also a brewed beverage like sake, it showed a lower content of free amino acids compared to sake. On the other hand, distilled spirits such as whiskey and awamori contained almost none.

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The OPA post-column method is a technique that reacts amino acids with the fluorescent reagent OPA after separation in a column and detects the fluorescence (Figures 1, 2). This method allows for high-sensitivity analysis compared to the ninhydrin method. The fluorescent reagent OPA selectively reacts with primary amines, making it less susceptible to interference from contaminants and enabling highly selective analysis. Proline is a secondary amino acid, but it can be converted into a primary amine by adding sodium hypochlorite to the reaction solution, allowing for measurement. This document presents a case study of simultaneous measurement of 17 amino acid components, including proline (Figure 3).

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By using a Cs-corrected TEM device that compensates for spherical aberration, it is possible to observe the cross-sectional structure of devices with high resolution. This case presents data from high-resolution (HR)-STEM observation and EDX elemental distribution analysis of the light-absorbing layer of CIGS thin-film solar cells. In CIGS, which has a polycrystalline structure composed of four elements, atomic resolution EDX analysis was performed, visually revealing the distribution of atoms.

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By using a Cs-corrected TEM device that compensates for spherical aberration, it is possible to observe the cross-sectional structure of devices with high resolution. This case presents data from high-resolution (HR)-TEM observation and EDX elemental distribution analysis of commercially available MPU transistor components. Even for fine multilayer structures like FinFETs, it is possible to clearly observe the structure and elemental distribution of the devices using a Cs-corrected TEM.

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By using a Cs-corrected TEM device that compensates for spherical aberration, it is possible to observe the cross-sectional structure of devices with high resolution. In this case, we present data from high-resolution (HR)-TEM observations of the MTJ: magnetic tunnel junction part, extracted from a commercially available hard disk. Thus, it is possible to clearly observe the structure even in multilayer structures of ultra-thin metal films.

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AES analysis is a method for obtaining compositional information from the surface to a depth of several nanometers. By performing AES measurements on the cross-section of a sample to obtain elemental distribution images, it is possible to clearly evaluate the layered structure. In addition to evaluating layered structures and conducting elemental analysis of the inner walls of trenches and holes, combining mechanical processing and ion beam processing allows for the assessment of thin alloy layers and phenomena such as diffusion and segregation of elements. In this case, we will present data evaluated using AES analysis for a thin film deposited on a silicon substrate.

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AES analysis is a method for obtaining compositional information from the surface down to a depth of several nanometers, and it is an effective analysis for investigating the composition of contaminants and foreign substances that occur on the surface during the manufacturing process. Since it rarely detects information about the substrate or base material, it allows for a simple examination of only the abnormal areas, such as foreign substances, without preprocessing. Additionally, by conducting surface analysis, it is possible to obtain elemental distribution images. In this case study, we will present data evaluated using AES analysis regarding foreign substances present on a Si wafer.

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In power semiconductor devices, crystal defects may be formed within the Si substrate for lifetime control. This presents a case study evaluating the carrier concentration distribution due to differences in thermal treatment conditions of hydrogen ions, one of the elements used to create the lifetime control region.

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Ion chromatography is a method for detecting ionic components in liquid samples. Additionally, these components that adhere to the surface of solids (materials) are measured by extracting them by immersing in pure water. MST enables qualitative and quantitative analysis of ions and organic acids contained in liquid samples, evaluation of the amount of ions eluted from material surfaces, and investigation of the causes of material corrosion.

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In XPS analysis, in addition to the photoelectron peaks used for evaluation, photoelectron peaks from other orbitals and Auger peaks from X-ray excitation are also detected. Depending on the combination of elements, these sub-peaks can overlap with the target peak and interfere with the evaluation. *Typically, a strong photoelectron peak emitted from an inner shell level close to the outer shell is used. In the quantitative calculations of XPS analysis, the removal of such interfering peaks is primarily performed using the following two methods: 1. Removal using sensitivity coefficient ratios 2. Removal using waveform separation

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By conducting EBSD analysis on thinned samples, higher spatial resolution can be achieved compared to conventional bulk samples.

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In semiconductors, it is possible to determine the ionization potential from the valence band maximum (VBM) and the rising position on the high binding energy side (Ek(min)). Measurements are conducted after Ar ion sputter cleaning to remove surface organic contamination. ■ Determination of the valence band maximum (VBM) The spectrum near the valence band edge is extrapolated linearly to find the intersection with the background. ■ Calculation of the ionization potential Ionization potential (I.P.) = hν - W hν: Energy of the incident ultraviolet light (He I line 21.22 eV) W: Energy width of the spectrum (Ek(min) - VBM)

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In recent years, as hybrid and electric vehicles have been becoming more widespread, there is a growing demand for larger and higher-performance lithium-ion secondary batteries for their power supply. To develop high-capacity positive electrode materials, it is crucial to identify the correlation between composition, structure, and electrochemical properties. By clarifying the electronic states of metal elements and their local structures in positive electrode materials through XAFS analysis using synchrotron radiation, it is possible to gain insights into the correlation between composition, structure, and electrochemical properties.

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Emulsions are dispersion systems in which water-soluble and fat-soluble components are mixed without separation due to the action of emulsifiers, and various emulsion technologies are widely used in processed foods. Mayonnaise is a representative processed food of the O/W type (oil-in-water emulsion). As a result of evaluation using cryo FIB-SEM observation, we were able to visualize the distribution of water, oil, emulsifiers, and other components. By conducting magnified observations, we can evaluate the fine structure, which is expected to be applied to sensory evaluations such as the smoothness and flavor of food.

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To observe the structure of liquid samples, it is necessary to conduct a series of analyses while maintaining the original structure of the sample. In cryo-SEM, the sample can be observed by rapidly freezing it to create a cross-section. Furthermore, by combining this with cross-section fabrication techniques using FIB processing, it is possible to obtain more detailed information about the internal structure.

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IGZO films are materials that are being researched and developed as TFT materials for displays. Since they are composed of multiple metal elements, it is important to understand how the composition, bonding state, and electronic state change depending on the process. We will introduce examples of evaluating the composition, bonding state, and electronic state of IGZO film surfaces using XPS and UPS.

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IGZO films are materials that are being researched and developed as TFT materials for displays. The presence or absence of crystalline structure in the thin film may affect the TFT characteristics and reliability, necessitating local crystalline evaluation within the device. We will introduce a case where the crystalline structure in IGZO films was continuously evaluated using electron diffraction measurements from TEM.

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