GPC와 역상 HPLC에 의한 에폭시 봉지제 중 고분자 물질 분석

윤상영; 오명숙; 박내정

Polymer(Korea), Vol.22, No.6, 1007-1013, November, 1998

Export Citation

GPC와 역상 HPLC에 의한 에폭시 봉지제 중 고분자 물질 분석

Analysis of Polymer Materials in Epoxy Molding Compounds by GPC and Reversed Phase HPLC

윤상영, 오명숙, 박내정

초록

상용 EMC 중의 고분자 성분을 분석하기 위해 시료를 적당한 유기용매로 추출하고, 분리, 확인하기 위하여 GPC와 역상 HPLC, 분취 HPLC 등을 이용한 분석방법을 연구하였다. B-stage 상태의 EMC를 여러 가지 극성이 다른 용매를 사용하여 추출한 결과 휘발성이 가장 높은 acetone이 가장 적합한 추출용매 이었다. EMC제조공정 중 kneading 후에도 약 60%의 물질이 추출가능한 상태로 남아 있어 사용 고분자 성분의 추적이 가능하였다. 추출조작에서 시료량과 추출 용매의 양의 비는 1:10이 가장 적합하였다. GPC에 의해서는 에폭시 수지, 페놀 경화제, 브롬화 에폭시 난연제 성분의 분리가 이루어지지 않았으나 역상 HPLC상에서는 분리가 매우 양호하여 각 성분의 분취가 가능하였다. 분취 HPLC를 이용하여 각 성분을 분취하여 GPC로 확인한 결과 각 성분을 정확하게 동정할 수 있었다.

An analytical method for polymer materials; in epoxy molding compounds (EMC) was investigated via extraction, and GPC and reversed phase HPLC of the extract. Acetone was one of the best solvents to extract the polymer materials from B-stage EMC. About 60% of polymer materials were extracted with 1:10 sample to solvent ratio. GPC was not successful to separate the epoxy resin, phenol novolac hardener, and brominated epoxy flame retardant. On the other hand, reversed phase HPLC was very effective for the separation of polymer materials in EMC. Preparative HPLC was used to collect the separated polymer fractions. GPC analyses of these fractions confirmed the presence of each component.

Keywords:EMC;GPC;HPLC;extraction;polymers

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[2] Soane DS, Martynenko Z, "Encapsulations and Packaging of Integrated Circuits," in "Polymers in Microelectronics, Fundamentals and Applications," p. 213, Elsevier, N.Y. (1989)

[3] Licari JJ, Hugues LA, "Handbook of Polymer Coatings for Electronics," p. 14, Noyes Publications, Park Ridge, N.Y. (1990)

[4] Hadad DW, SAMPE J., 14, 4 (1978)

[5] Dark WA, Conrad EC, Crossman LW, J. Chromatogr., 91, 247 (1974)

[6] Shiono S, Karino I, Ishimura A, Enomoto J, J. Chromatogr., 193, 243 (1980)

[7] Martin JR, Johnson JF, Cooper AR, J. Macromol. Sci.-Rev. Macromol. Chem. Phys., C8(1), 57 (1972)

[8] Brown RP, "Handbook of Plastics Test Methods," 2nd ed., Godwin/PRI, London (1981)

[9] Van Krevelen DW, "Properties of Polymers: Correlation with Chemical Structure," p. 17, Elsevier, Amsterdam (1972)

[10] Podzimek S, Hroch L, J. Appl. Polym. Sci., 47, 2005 (1993)

[11] McCrary TJ, Am. Lab., 86, Jan. (1985)

[12] Hagnauer GL, Setton I, J. Liq. Chromatogr., 1, 55 (1978)

[13] Zucconi TD, Humphrey JS, Polym. Eng. Sci., 16, 11 (1976)

[14] Batzer H, Zahir SA, J. Appl. Polym. Sci., 21, 1843 (1977)

[15] Antal I, Fuzes L, Samay G, Csillag L, J. Appl. Polym. Sci., 26, 2783 (1981)

[16] Hangauer GL, Ind. Res. Dev., Apr., 128 (1981)

[17] Hangauer GL, Dunn DA, J. Appl. Polym. Sci., 26, 1837 (1981)