• Title/Summary/Keyword: Average molecular weight (MW)

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Effect of Analytical Parameters of Gel Permeation Chromatography on Molecular Weight Measurements of Urea-Formaldehyde Resins

  • Jeong, Bora;Park, Byung-Dae
    • Journal of the Korean Wood Science and Technology
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    • v.45 no.4
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    • pp.471-481
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    • 2017
  • As the molecular weight (MW) of urea-formaldehyde (UF) resins had a great impact on their properties, this work was conducted to study effect of analytical parameters of gel permeation chromatography (GPC) on the MW measurement of UF resins. GPC parameters such as flow rate, column, detector temperature, and sample injection temperature were selected to compare number-average molecular weight (Mn), weight-average molecular weight (Mw), molecular weight distribution (MWD) and polydispersity index (PDI) of two UF resins with different viscosities. As expected, UF resin with higher viscosity resulted in greater Mn and Mw than those of low viscosity UF resin. When the flow rate increased, both Mn and Mw of UF resins decreased and MWD became narrower. By contrast, both Mn and Mw increased and MWD became wide when the column, detector, and sample injection temperature increased. The column, detector, and sample injection temperature of $50^{\circ}C$ at a flow rate of $0.5m{\ell}/min$ resulted in the highest MW and broadest MWD for the GPC analysis. These results suggest that the apparent molecular size or a hydrodynamic radius of UF resin molecules dissolved in the mobile phase affect to Mn, Mw and MWD.

Effects of Hydrolysis pH on Distribution of Molecular Weights of Alginates of Sea Tangle Laminaria japonica (다시마 (Laminaria japonica) 알긴산의 분자량 분포에 미치는 가수분해 pH의 영향)

  • Lim, Yeong-Seon;You, Byeong-Jin
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.39 no.4
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    • pp.313-317
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    • 2006
  • To prepare oligouronic acids from high-molecular-weight alginates, sea tangle (Laminaria japonica) alginates were hydrolyzed at various pHs for 1 hr at 80$^{\circ}C$. The effects of hydrolysis pH (HpH) on the average molecular weight (AMW) and MW distribution ratios (DRs) in the hydrolyzed alginates were investigated. As HpH decreased, the DRs of the alginates with MW>500 kDa and MW=300-500 kDa decreased exponentially, while it increased exponentially for MW<50 kDa. For MW=100-300 kDa, DR increased exponentially as HpH fell from 5.0 to 3.5, and then decreased exponentially. Similarly, for MW=50-100 kDa, DR increased exponentially as HpH increased to 1.0 from 5.0, and then decreased exponentially. As HpH decreased, the MW cutoff size and AMW of alginates fraction with the highest DR were decreased. For HpH 4.5 and 5.0, the MW cutoff size with the highest DRs was MW=300-500 kDa; the DRs were 28.9 and 32.6%, respectively; and the AMW of both was about 400 kDa, for HpH 3.5 and 4.0, the cutoff size was MW=100-300 kDa; the DRs were about 28%: and the AMWs were both about 200 kDa. For HpH 3.0, the cutoff size was MW=50-100; the DR was 29.0%; and the AMW was 73 kDa. For HpH values below 2.0, the MW cutoff size with the highest DRs was MW<50 kDa, and all of the AMWs were below 28 kDa.

Effects of Hydrolysis Temperature on the Distribution of the Molecular Weights of Alginates Prepared from Sea Tangle, Laminaria japonica (다시마 Laminaria iaponicus 알긴산의 분자량 분포에 미치는 가수분해 온도의 영향)

  • Lim, Yeong-Seon;You, Byeong-Jin
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.40 no.4
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    • pp.187-192
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    • 2007
  • To prepare oligouronic acids from high-molecular-weight alginates prepared from sea tangle (Laminaria japonica), the alginates were hydrolyzed at various temperatures for 1 hr at pH 5.0. The effects of hydrolysis temperature $(H_{Temp})$ on the average molecular weight (AMW) and distribution ratio of MW (DR) in the hydrolyzed alginates were investigated. As $(H_{Temp})$ increased, the AMW of the alginates decreased exponentially; in addition the DR of the alginates with MW>500 kDa decreased exponentially, while the DR of those with MW=50-100 and MW<50 kDa increased exponentially. For the alginates with MW=300-500 and MW=100-300 kDa the DR increased exponentially until $H_{Temp}$ reached $80^{\circ}C$, and then decreased exponentially at above $80^{\circ}C$. AS $H_{Temp}$ increased, the MW cutoff size and AMW Of the alginates fraction With the highest DR both decreased. For $H_{Temp}<60^{\circ}C$, the MW cutoff size with the highest DR was MW>500 kDa; the DR was 39-67% and the AMW 1,000-1,300 kDa. For $H_{Temp}$ $80^{\circ}C$, the MW cutoff size with the highest DR was MW=300-500 kDa and the DR was about 33% and the AMW about 400 kDa. For $H_{Temp}\;100-121^{\circ}C$, the MW cutoff size with the highest DRs was MW=50-100 kDa, with a DR of 39-44% and an AMW of 70-80 kDa.

Effects of Synthesis Method, Melamine Content and GPC Parameter on the Molecular Weight of Melamine-Urea-Formaldehyde Resins

  • KIM, Minjeong;PARK, Byung-Dae
    • Journal of the Korean Wood Science and Technology
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    • v.49 no.1
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    • pp.1-13
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    • 2021
  • This study was conducted to investigate the effects of the synthesis method, melamine content, and GPC parameters (such as flow rate, column-detector temperature, and sample injection temperature) on the molecular weight of melamine-urea-formaldehyde (MUF) resins. Two different synthesis methods were employed. In the first method, MUF-A resins were synthesized by simultaneously reacting urea, formaldehyde, and melamine (5%, 10%, and 20%) using the reaction of alkaline-acid-alkaline steps under controlled temperature and viscosity. In the second method, MUF-B resins were synthesized by first reacting melamine at the same levels with formaldehyde and then by adding urea. The highest weight average molecular weight (Mw) of MUF-A resins was found at 10% melamine content when the flow rate was 0.3 and 0.8 ml/min; Mw decreased slightly at 20% melamine content. The results showed that Mw increased with an increase in the melamine content when the flow rate was 0.5 and 1.0 ml/min. In addition, Mw was the highest when the flow rate, column-detector temperature, and injection temperature were 0.3 ml/min, 50℃, and 25℃, respectively. On the contrary, MUF-B resins had greater Mw and number average molecular weight (Mn) than MUF-A resins. Overall, Mw and Mn increased as the melamine content increased. The optimal GPC parameter for MUF resins was determined as follows: a flow rate of 0.5 ml/min, a column-detector temperature of 50℃, and a sample injection temperature of 50℃.

Measurement of Molecular Weights of Melamine-Urea-Formaldehyde Resins and Their Influences to Properties of Medium Density Fiberboards

  • Jeong, Bora;Park, Byung-Dae
    • Journal of the Korean Wood Science and Technology
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    • v.44 no.6
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    • pp.913-922
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    • 2016
  • This study attempted to measure molecular weight (MW) of melamine-urea-formaldehyde (MUF) resins prepared by two different synthesis methods: the one-step MUF resins were synthesized in one batch procedure, while the two-step MUF resins were prepared by a physical mixing of urea-formaldehyde (UF) resin with melamine-formaldehyde (MF) resin that had been synthesized in a separate procedure. The properties of medium density fiberboard (MDF) panels bonded with two types of MUF resins were also investigated. MWs of these MUF resins were measured using gel permeation chromatography (GPC). In addition, this study measured the MWs of one-step MUF resin during its synthesis procedure. The performance of two types of MUF resins was evaluated by determining properties of MDF panels prepared in laboratory. As the synthesis procedure progressed, both number average MW ($M_n$) and weight average MW ($M_w$) of one-step MUF resin gradually increased, while the polydispersity index (PDI) decreased. And low Mw species of the resin predominantly decreased as the synthesis step progressed. The one-step MUF resin showed greater $M_n$ and $M_w$ than those of the two-step ones even though the PDI values of both resins were very similar each other. As expected, the one-step MUF resin resulted in better properties of MDF panels than those of two-step resins. In particular, the one-step MUF resin provided better internal bond (IB) strength and thickness swelling (TS) with MDF panels than those of two-step ones, indicating better water resistance of the one-step resin. These results suggest that the preparation method of MUF resins have a great impact on the MW and final panel properties.

Evaluation of Granular Activated Carbon Process Focusing on Molar mass and size distribution of DOM (DOM의 분자량과 크기분포에 따른 입상활성탄 공정의 평가)

  • Chae, Seon H.;Lee, Kyung H .
    • Journal of Korean Society of Water and Wastewater
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    • v.22 no.1
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    • pp.31-38
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    • 2008
  • The primary objective of this study was to evaluate the variation of the molecular size distribution by granular activated carbon (GAC) adsorption. GAC adsorption was assessed by using the rapid small-scale column test (RSSCT) and high-performance size-exclusion chromatography (HPSEC) was used to analyze the molecular size distribution (MSD) in the effluent of GAC column. RSSCT study suggested that GAC adsorption exhibited excellent interrelationship between dissolved organic carbon (DOC) breakthrough and MSD as function of bed volumes passed. After GAC treatment, the nonadsorbable fraction which was about 25percents of influent DOC corresponded to the hydrophilic (HPI) natural organic carbon (NOM) of NOM fractions and was composed entirely of <300 molecular weight (MW) in the HPSEC at the initial stage of the RSSCT operation. The dominant MW fraction in the source water was 1,000~5,000daltons. At the bed volumes 2,500, MW <500 of GAC treated water was risen rather than it of source water. After the bed volumes 7,300 of operation, the MW 1,000~3,000 fraction was closed to about 80percents of DOC found in the GAC influent. The Number-average molecular weight (Mn) value determined using HPSEC for the effluent of GAC column was gently increased as DOC breakthrough progress. The quotient p(Mw/Mn) can be used to estimate the degree of polydispersity was shown greatest value for the GAC effluent at the initial stage of the RSSCT operation.

A Study on the Molecular Weight Distribution of Starch (전분의 분자량 분포도에 관한 연구)

  • Kim Kyeong-Yee
    • Food Science and Preservation
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    • v.11 no.4
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    • pp.496-502
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    • 2004
  • Purified acorn starch was obtained from alkali precipitation method. Acorn amylose and acorn amylopectin were fractionated from purified acorn starch by butanol improvement method. Gel permeation chromatography (GPC) was used to measure molecular weight distribution of acorn starch, acorn amylose, acorn amylopectin and corn starch, corn amylose, corn amylopectin. GPC measurement diagrams were obtained by each retention time. And then, we used DMSO and DMF as solvent, pullulan as standard material. We calculated the Number-average molar mass (Mn), Weight-average molar mass (Mw) and polydispersity from molecular weight distribution of each sample. As a result of estimating molecular weight using GPC, Mw of amylose has small value than Mw of amylopectin. From this fact, the molecular structural aspects of amylose and amylopectin were predicted and it was in good agrement with the tendency of polydispersity by GPC. The polydispersity of starch had big value than amylose and amylopectin, from this result, it might be known that the range of molecular weight appeared broad by heterogeneous properties of two components. The viscosity of purified acorn starch, amylose, amylopectin seperated from acorn starch, was decreased by increasing the shear rate and raising the temperature exponentially. Acorn starch solutions exhibited pseudoplastic power law fluid behavior.

Pure-Separation of Calcium chloride-treated Silk Fibroin Hydrolysate by Gel Filtration Chromatography and Effect of It's Enzymatic Hydrolysis (Calcium chloride 피브로인 용해물의 Gel Filtration Chromatography에 의한 순수분리 및 효소 가수분해 효과)

  • 여주홍;이광길;이용우
    • Journal of Sericultural and Entomological Science
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    • v.41 no.3
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    • pp.211-215
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    • 1999
  • The pure-separation of calcium chloride-treated fibroin hydrolysates could be carried out using gel filtration chromatography. Also, the effect of its enzymatic hydrolysis was investigated in order to find out the enhancement of their functionality. The average molecular weight(Mw), solubility and free amino acid compositions of three hydrolysates samples (calcium chloride, calcium chloride-flavourzyme and calcium chloride-thermoase)were measured to compare their characteristics. The molecular weight of calcium chloride hydrolysate was about Mw 46,800 and it can be reduced to Mw 12,500 and 1,070 upon the enzymatic hydrolysis by flavourzyme and thermoase, repectively. A solubility of calcium chloride-treated samples shows about 60% while calcium chloride/enzyme-treated samples are perfectly soluble (100% solubility). The total amino acid composition of calcium chloride enzymatic hydrolysates are much higher than that of calcium chloride hydrolysate.

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Thermal-and Bio-degradation of Starch-Polyethylene Films Containing High Molecular Weight Oxidized-Polyethylene

  • Kim, Mee-Ra;Pometto, Anthony-L.
    • Preventive Nutrition and Food Science
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    • v.3 no.1
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    • pp.27-35
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    • 1998
  • Starch-polyethylene films containing high molecular weight(NW) oxidized-polyethylene and prooxidant were prepared , and thermal -and bio-degradability of the films were determined. Increased levels of starch resulted in a corresponding reduction in mechanical strength of the films. However, the addition of high MW oxidized-polyethylene did not significantly reduce the percent elongation of the films. Thefilms containing high MW oxidized-polyethylene andproosicant were degreaded faster than those containing no aadditive during the heat treatment. The films lost their measureable mechanical properties when their weight-average MW(Mw) fell below 50,000. Biodegradability of the films was determined by a pure culture assay with either Streptomyces badius 252.S. setonii 75Vi2 or S. viridosporous T7A, and by an extracellulr enzyme assay using S. setonii 75vi2. The results from pure culture assay indicated that biomass accumulation on the film surface inhibited chemical and biological degradation of the films. The extracellular enzyme assay demonstrated decrease of percent elongation and increase of carbonyl index of the films. Therefore, extracellular enzyme assay could be used as a good method to evaluate biodegradability of the films.

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Changes of Silk Protein Compositions by Solubility Condition (용해조건에 따른 견 단백질의 조성 변화)

  • Yeo, Joo-Hong;Lee, Kwang-Gill;Lee, Yong-Woo;Nam, Jin;Kim, Sun-Yeou
    • Analytical Science and Technology
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    • v.12 no.4
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    • pp.306-311
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    • 1999
  • Changes of silk protein compositions of average molecular weight (Mw) and free amino acid composition to different solubility conditions were studied by SDS-polyacrylamide electropholesis, gel permeation chromatography (GPC), and free amino acid analysis method. We can not detected average molecular weight distribution of different hydrochloric acid (HCl) conditions as SDS-polyacrylamide method, but as using GPC method, molecular weight distribution of 2N-HCl, 1N-HCl and 0.5N-HCl (3 hrs at $110^{\circ}C$ treated) are confirmed Mw 800, 1,500 and 3,700, respectively. The average molecular weight of calcium chroride and calcium chloride-enzyme treated samples are shown Mw 46,800 and 12,500, respectively. The degree of hydrolysis and the composition of the free amino acid in the fibroin hydrolysates effected significantly composition of free amino acids of the fibroin powder. The increase of the degree of hydrolysis and ratio of free amino acids and oligopeptides were found to be directly related to the concentration of hydrochloric acid and treatment of enzyme, resulting in the increase of water solubility.

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