A Note on Fractionation of Polymers by Thin Layer Chromatography

Inagaki, Hiroshi; Kamiyama, Fumio; Yagi, Toshiharu

doi:10.1021/ma60019a028

Cited by 29 publications

(8 citation statements)

References 1 publication

Supporting

Mentioning

Contrasting

Order By: Relevance

“…3 To confirm the result further we have applied another separation mechanism, i.e., the solubilitycontrolled phase-separation mechanism, 3 which leads to fractionation largely by molecular weight. A gradient development on silica gel thin-layer was performed at ca.…”

Section: Component Species Separated From Kraton 1101mentioning

confidence: 91%

“…2 The above two findings were attained using a separation mechanism in TLC, which involves adsorption-desorption processes. 3 Since this mechanism has been known to lead to polymer separation without appreciable interference from the molecular weight, 3 we thought it feasible with TLC to identify the chain architecture of given block-copolymer samples independent of their molecular weight. This paper deals with such identification problems for styrenebutadiene (SB) copolymers which are now of * Present address:…”

mentioning

confidence: 99%

See 1 more Smart Citation

Thin-Layer Chromatographic Identification of Chain Architectures of Styrene—Butadiene Copolymers

Donkai

Miyamoto

Inagaki

1975

Polym J

View full text Add to dashboard Cite

ABSTRACT:The feasibilities of thin-layer chromatography as a tool to identify the chain architecture of given copolymer samples have been investigated. To this end, styrene-butadiene (SB) block copolymers with known chain architecture were prepared and used as reference samples. Preliminary TLC experiments on these samples indicated that the random, tapered, diblock and triblock SB-samples could be chromatographically distinguished from one another under suitable development conditions. By applying the procedures thus established, the chain architecture of various commercial SB-products could be identified without appreciable interference from the molecular weight and composition.

show abstract

Section: Component Species Separated From Kraton 1101mentioning

confidence: 91%

mentioning

confidence: 99%

Thin-Layer Chromatographic Identification of Chain Architectures of Styrene—Butadiene Copolymers

Donkai

Miyamoto

Inagaki

1975

Polym J

View full text Add to dashboard Cite

show abstract

“…In the first region (-80% CHC13), samples of different molecular weight show no difference in R{. The sec- ond region (~70% CH3OH), where precipitation is imminent, shows a strong dependence of Rt on molecular weight (14).…”

Section: Polymer Behavior In Tlcmentioning

confidence: 95%

“…Recently efforts in three separate laboratories have been successful in determining the molecular weight distribution of a polymer sample by TLC techniques (9)(10)(11)(12). An explana tion of the facility and high resolving power observed has been sought through a number of continuing experiments (11)(12)(13)(14)(15)(16). The purpose of this report is to review the results of these studies and to comment on the fractionation mechanisms postulated.…”

Section: Thin-layer Chromatography (Tlc) Is a Common Laboratory Technmentioning

confidence: 98%

Thin-Layer Methods for Determining Molecular Weight Distribution

Otocka¹

1973

Polymer Molecular Weight Methods

View full text Add to dashboard Cite

Thin-layer chromatography (TLC) is a common laboratory technique for separating complex mixtures of solutes, usually by an adsorbtion mechanism. Several laboratories have applied the technique to the separation of polymer fractions and characterization of polymer molecular weight distribu tions. This work reviews the experimental results and theoretical approaches to the fractionation mechanisms.^phin-layer chromatography (TLC) is a well-known technique for the separation of mixed solutes by adsorption. Compared with related techniques in column chromatography, TLC offers several advantages. The use of adsorbents having large surface area ( particle size ~10 μ vs. 50 μ) results in excellent resolution. Separation and analysis time are reduced because many samples can be run simultaneously and material need not be eluted for quantitation. Several references provide a com prehensive background on TLC ( 1-3 ).TLC has been a widely accepted technique in biochemistry and or ganic chemistry for a number of years. With modern quantitation TLC is being used today in such diverse applications as air pollution analysis and clinical medicine.The initial applications of TLC to problems in polymer chemistry were directed to the separation of polymer blends, stereoisomers, and a variety of copolymers ( 4-8 ). From these investigations occasional molec ular weight effects were noted (8). Recently efforts in three separate laboratories have been successful in determining the molecular weight distribution of a polymer sample by TLC techniques (9-12). An explana tion of the facility and high resolving power observed has been sought through a number of continuing experiments (11)(12)(13)(14)(15)(16). The purpose of this report is to review the results of these studies and to comment on the fractionation mechanisms postulated. 55Downloaded by UCSF LIB CKM RSCS MGMT on December 2, 2014 |

show abstract

“…The results for 20/80 (v/v) nitromethane-methanol mixture by VP-TLC are also plotted in the figure using the triangle. From Figure 9 we obtain Rr,w=3.78-0.275 Ne (wt%) silica gel at 25°C (6) 11.5~Ne (wt%)~12.7 and Rr,w=2.59-0.184 Ne (wt%) kieselghur at 25°C (7) 1 l.5~Ne (wt%)~12.7 Equation 6 should be compared with eq 4; eq 7 corresponds to eq 5. In the case of VP-TLC with acetone-methanol-chloroform (silica gel), the Rr,w value of the fraction S 19-5 deviates slightly from the value expected from eq 6.…”

mentioning

confidence: 99%

Characterization of Cellulose Nitrate by Thin-Layer Chromatography

Kamide

Okada

Terakawa

et al. 1978

Polym J

View full text Add to dashboard Cite

ABSTRACT:The intent of this work is to establish a method for evaluating the chemical compositional distribution (CCD, in this case, nitrogen content (Ne)) and the molecular weight distribution (MWD) of cellulose nitrate (CN) using open and vapor-programed (VP) thin-layer chromatography (TLC). CCD could be determined with a nitromethane-methanol mixture in open TLC and with acetone-methanoi----{;hioroform in VP-TLC. With mainly the former, the change in the rate of flow Rt was based on the adsorption-desorption mechanism and with the latter, the separation of polymer according to Ne was interpreted by the phase separation mechanism. Both methods gave similar CCD for given CN samples. The most effective method for evaluating the weight-average molecular weight was achieved with 1,4-dioxane-methanol-isopropanol mixture in VP-TLC, for which the phase separation mechanism was operative.KEY WORDS Cellulose Nitrate / Thin-Layer Chromatography / Compositional Distribution / Molecular Weight Distribution/ AdsorptionDesorption Mechanism / Phase Separation Mechanism / Since its first appearance in 183 I, cellulose nitrate (hereafter designated as CN) has occupied, in spite of rapid growth of the production of synthetic polymers, invariably an important position in industry owing to its numerous favorable features. As is well-known, CN is commercially utilized by changing it's average molecular weight and the average degree of esterification (i.e., the nitrogen content by wt% as expressed by Ne). A number of attempts have been made to separate whole CN polymer with respect to molecular weight or Ne. But, unfortunately no effective method of compositional fractionation has yet been proposed for CN. In 1973 Kamide, et al., 1 succeeded, by using thin-layer chromatography (TLC), to evaluate molecular weight distribution (MWD) and chemical compositional distribution (CCD) of cellulose acetate. Quite recently, Kamiyama and Inagaki2 studied by TLC the compositional heterogeneity of some commercial CN samples by a concentration-gradient development using a binary acetone-ethylacetate (20/3, v/v) and another binary chloroformethylacetate (1/2, v/v) as initial and second solvents, respectively. However, they have not established a method for estimating MWD or CCD of CN by TLC technique. This work intends to fractionate CN on the basis of Ne or its molecular weight by TLC.Polymer J., Vol. 10, No. 5, 1978 EXPERIMENTAL Preparation of Polymer SamplesEleven whole samples have been used in this work. These samples were ptepared by nitrating purified cotton linter with a mixture of nitric acid and sulfuric acid, followed by a conventional thermal degradation at elevated temperatures in water. The sample W 119 was fractionated, by successive solutional fractionation (SSF) technique, into five fractions at 25°C from a 0.8-wt % solution in acetone using hexane as a precipitant. 547

show abstract

A Note on Fractionation of Polymers by Thin Layer Chromatography

Cited by 29 publications

References 1 publication

Thin-Layer Chromatographic Identification of Chain Architectures of Styrene—Butadiene Copolymers

Thin-Layer Chromatographic Identification of Chain Architectures of Styrene—Butadiene Copolymers

Thin-Layer Methods for Determining Molecular Weight Distribution

Characterization of Cellulose Nitrate by Thin-Layer Chromatography

Contact Info

Product

Resources

About