Frontier Laboratories Ltd.

Kōriyama, Japan

Frontier Laboratories Ltd.

Kōriyama, Japan
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PubMed | KOTITI Testing & Research Institute, Korea University, Hallym University, University of Suwon and 3 more.
Type: | Journal: Journal of chromatography. A | Year: 2016

For the quantitative analysis of phthalates in polymers, a thermal desorption (TD)-GC-MS method was compared with solvent extraction (SE)-GC-MS methods which require the long pretreatment procedures using large amount of harmful organic solvents. Calibration curves of TD-GC-MS showed good linearity (r(2)>0.9997) and low method detection limit (<30mg/kg with 9.0% RSD). Quantification results for three kinds of test phthalate polymer samples (test PTPSs) showed an RSD below 7.4% and acceptable recoveries (78.3-117.4%) as in the standard method of International Electrotechnical Commission. Even in a sample with a high concentration of phthalates (PTPS #3), the method also showed good recovery with low RSD values. The TD-GC-MS results were comparable with those results by SE-GC-MS methods, indicating that TD-GC-MS method also can be used for the quantification of phthalates in polymers. The average recovery (92-103%) and RSD (<20%) values obtained from international inter-laboratory study for TD-GC-MS performed in six laboratories also indicated that TD-GC-MS can be used as an international standard method for the quantification of phthalates in polymers.


Hosaka A.,Frontier Laboratories Ltd. | Watanabe C.,Frontier Laboratories Ltd. | Teramae N.,Frontier Laboratories Ltd. | Teramae N.,Tohoku University | Ohtani H.,Nagoya Institute of Technology
Journal of Analytical and Applied Pyrolysis | Year: 2014

A new micro reaction sampler is developed to facilitate the thermally assisted hydrolysis and methylation (THM) reaction of intractable condensation polymers, at an elevated temperature in a sealed glass capsule under high pressure. The sampler is integrated with a glass capsule and a crushing metal rod, and it is air-tightly mounted inside a vertical micro-furnace pyrolyzer of a pyrolysis (Py)-GC/MS system. The developed sampler is firstly applied for THM-GC/MS measurements of polycarbonate (PC) whose structural characterization using tetramethylammonium hydroxide (TMAH) as a reagent has been reported in detail previously, to confirm the applicability of the developed sampler. Two peaks are clearly observed in the pyrogram and they are assigned to methyl derivatives of a main chain unit (bisphenol A) and a terminal group (tert-butyl phenol) which are the THM reaction products of PC. The area ratio of these two peaks is almost the same as that obtained by the conventional THM-GC/MS, suggesting the effectiveness of the developed reaction sampler. Further, the developed sampler is applied for THM of nylon 6.6 which has been hardly analyzed by conventional THM-GC/MS using TMAH as a reagent in the open system where samples are exposed to the ambient gas in a pyrolyzer. Using the developed method, measured pyrogram clearly shows several peaks with fairly high yields that are assigned to methyl derivatives of monomer units of nylon 6.6, that is, adipic acid and hexamethylenediamine, and a hybrid dimer of each monomer. Therefore, it can be said that the developed sampler based on the closed system, sealed glass capsule, is quite useful for the pyrolysis analysis of intractable condensation polymers such as nylon 6.6, compared to the conventional THM-GC/MS using the open system. © 2014 Elsevier B.V.


Watanabe C.,Frontier Laboratories Ltd. | Ramus T.,Diablo Analytical | Meijboom R.,University of Johannesburg | Freeman B.,Frontier Laboratories United States
Environmental Progress and Sustainable Energy | Year: 2014

The design of a tandem micro-reactor is discussed. A tandem micro-reactor, consists of two reactors (upper and lower), which are individually temperature-controlled. The upper reactor (1st reactor) is used to preheat a gas, vaporize a liquid, or thermally decompose (i.e., pyrolyze) organic solids in order to form a vapor phase sample. The catalyst reaction tube is packed with a catalyst and placed in the lower reactor (2nd reactor). Vapors from the 1st reactor flow into the reaction tube in the lower reactor, where they react with the catalyst. A mass flow controller allows selection of one to three reactant gases that can be introduced to the sample vapors exiting the upper reactor prior to entering the lower reactor containing the catalyst bed. The reaction products exiting the lower reactor flow directly into the gas chromatograph for analysis. The catalyst is evaluated by noting what compounds are formed and their relative distribution using mass spectrometer detection. The transformation of cellulose, glycerol, and Jatropha "press cake" illustrate the value and convenience of using the tandem micro reactor to rapidly characterize a catalyst or a series of catalysts. © 2014 American Institute of Chemical Engineers.


Kim Y.-M.,University of Seoul | Kim Y.-M.,Frontier Laboratories Ltd. | Lee H.W.,University of Seoul | Kim S.,Hallym University | And 2 more authors.
Bioenergy Research | Year: 2015

In this study, the non-isothermal pyrolysis of citrus unshui (C. unshiu) peel was studied by thermogravimetric analysis (TGA) and evolved gas analysis/pyrolyzer-gas chromatography/mass spectrometry (EGA/Py-GC/MS). Two types of analytical pyrolysis-GC/MS experiments, EGA-MS and multi-shot GC/MS, were conducted to determine the thermal profiles of the pyrolysis products, as well as the detailed pyrolysis product distribution of each thermal zone. The pyrolysis of pectin, hemicellulose, cellulose, and lignin was also carried out to interpret the pyrolysis behavior of C. unshiu peel. TGA and EGA-MS of C. unshiu peel revealed five main weight loss stages, such as water and limonene vaporization, pyrolysis of pectin, hemicellulose, cellulose, lignin, and char stabilization. Multi-shot GC/MS revealed the specific pyrolysis products of each component of C. unshiu peel. Limonene was vaporized with water below 140 °C. Large amounts of methanol, acetic acid, 5-hydroxymethylfurfural, 3,5-dihydroxy-6-methyl-2,3-dihydro-4H-pyran-one, and p-vinylguaiacol were produced between 140 and 280 °C, at which temperature range pectin and hemicellulose decomposed. The specific pyrolyzates of cellulose formed between 211 and 360 °C, and a small amount of lignin pyrolyzates were also detected over a wide temperature range (141–360 °C). At temperatures higher than 360 °C, small amounts of aromatics were produced as the by-products of char stabilization. © 2014, Springer Science+Business Media New York.


Yuzawa T.,Frontier Laboratories Ltd. | Watanabe C.,Frontier Laboratories Ltd. | Nemoto N.,Nihon University | Ohtani H.,Nagoya Institute of Technology
Polymer Degradation and Stability | Year: 2013

Photo, thermal and oxidative degradation behaviors of high impact polystyrene (HIPS) containing butadiene rubber (BR) were evaluated by online ultraviolet irradiation-pyrolysis (UV/Py)-GC/MS system with a micro-UV irradiator. Volatile degradation products evolved during UV irradiation at 60°C in air were identified and quantified through online GC/MS measurements. Formation of some typical volatiles from the HIPS sample during 1 h irradiation, such as benzaldehyde, acetophenone and benzoic acid originating from PS and 2-propenal from BR, clearly indicates the contribution of oxidative reactions in the polymer chains. Moreover, the residual HIPS samples after irradiation up to 12 h were characterized by evolved gas analysis-mass spectrometry (EGA-MS). The observed EGA thermograms clearly showed not only lower temperature shifts of onset and peak top of gas evolution, but also peak broadening compared with that of the original HIPS sample, reflecting some structural changes in HIPS polymer chains during the irradiation. Furthermore, the degradation behavior of HIPS by the micro-irradiator was compared with that obtained by the conventional accelerated degradation test using a Xe weather meter. The observed EGA profile of HIPS irradiated by the Xe weather meter for 300 h showed the equivalent temperature shift and broadening to that for the residual HIPS after 1 h irradiation by the micro-UV irradiator. This result suggests that the micro-UV irradiator in UV/Py-GC/MS system might achieve the comparable degradation processes of polymeric materials much more rapidly compared with the conventional accelerated degradation test methods. © 2012 Elsevier Ltd. All rights reserved.


Yuzawa T.,Frontier Laboratories Ltd. | Watanabe C.,Frontier Laboratories Ltd. | Tsuge S.,Nagoya University | Shimane N.,Asahi Kasei Corporation | Imai H.,Asahi Kasei Corporation
Polymer Degradation and Stability | Year: 2011

A pyrolysis-GC/MS system incorporating with micro-UV irradiator (Xe-Hg lamp) was applied to the evaluation of the weatherability of the acrylic coating paints for house exterior walls. The deterioration of the materials during UV irradiation under thermal, and oxidative atmosphere was evaluated within a relatively short period of time with evolved gas analysis-mass spectrometry (EGA-MS) using a sub-milligram polymer sample. The EGA-MS thermograms indicated that both micro-UV irradiator with Xe-Hg lamp and weather meter with metal halide lamp caused similar photo, thermal, and oxidative degradation to the coating paint samples. Strong correlations between the results obtained by the UV/Py-GC/MS and that obtained by conventional weathering test using metal halide lamp was observed. It was suggested that UV/Py-GC/MS method could be used for compensating the conventional method by reducing the test period. © 2010 Elsevier Ltd. All rights reserved.


PubMed | Frontier Laboratories United States, Nagoya Institute of Technology and Frontier Laboratories Ltd.
Type: Journal Article | Journal: Analytical chemistry | Year: 2016

Pyrolysis-gas chromatography/mass spectrometry of polymer samples is studied focusing on the effect of hydrogen (H2) carrier gas on chromatographic and spectral data. The pyrograms and the related mass spectra of high density polyethylene (HDPE), low density polyethylene, and polystyrene (PS) serve to illustrate the differences between the species formed in H2 and the helium environment. Differences in the pyrograms and the spectra are generally thought to be a result of the hydrogenation reaction of the pyrolyzates. From the peak intensity changes in the pyrograms of HDPE and PS, hydrogenation of unsaturated pyrolyzates is concluded to occur when the pyrolysis is done in H2. Moreover, additional hydrogenation of the pyrolyzates occurs in the electron ionization source of a MS detector when H2 is used as a carrier gas. Finally, the applicability of mass spectral libraries to characterize pyrograms obtained in H2 is illustrated using 24 polymers. The effect of the hydrogenation reaction on the library search results is found to be negligible for most polymer samples with polar and nonpolar monomer units.


Patent
Frontier Laboratories Ltd. | Date: 2015-09-30

There is provided a gas phase component analyzer which obtains excellent separation performance, when a gas phase component mixture generated by catalysis is analyzed on-line. A gas phase component analyzer 1 includes heating apparatuses 2 and 3 which generate a first gas phase component mixture, a catalyst 14, a carrier gas introduction apparatus 9, first pressure control apparatuses 17 and 20 which bring the first gas phase component mixture into contact with the catalyst 14 under a predetermined pressure, to generate a second gas phase component mixture, a gas conduit 16, a column 26, a detector 29, second pressure control apparatuses 21 and 24 which control the second gas phase component mixture to pressure at which passing the column 26 is possible and an analysis is possible.


Patent
Frontier Laboratories Ltd. | Date: 2013-12-17

There is provided a capillary column comprising a flat cross section and a desired theoretical plate number and having both high resolution and high sample load capacity. The capillary column 1 comprising a stationary phase on an inactivated inner surface, which is used in gas chromatography, comprises a narrow part 3 formed in a central part of a cross section of internal space and a bulge part 4 formed on each of both sides of the narrow part 3.


Patent
Frontier Laboratories Ltd. | Date: 2014-12-15

There is provided a gas phase component analyzer which obtains excellent separation performance, when a gas phase component mixture generated by catalysis is analyzed on-line. A gas phase component analyzer 1 includes heating apparatuses 2 and 3 which generate a first gas phase component mixture, a catalyst 14, a carrier gas introduction apparatus 9, first pressure control apparatuses 17 and 20 which bring the first gas phase component mixture into contact with the catalyst 14 under a predetermined pressure, to generate a second gas phase component mixture, a gas conduit 16, a column 26, a detector 29, second pressure control apparatuses 21 and 24 which control the second gas phase component mixture to pressure at which passing the column 26 is possible and an analysis is possible.

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