다중텅그스텐산 아민염의 분자량 측정

Cryoscopy of Amine-Polytungstates

  • 변종홍 (한국과학기술연구소) ;
  • 연손수 (한국과학기술연구원 무기화학연구실)
  • 발행 : 1974.04.30

초록

비수용성 긴고리 지방족 아민인$(n-C_8H_{17})_3N$$(n-C_8H_{17})_3NCH_3Cl$을 사용하여 산도가 틀린 텅그스텐산수용액(pH=2, 4, 6)으로 부터 용매추출법에 의하여 유기용매에 녹는 다중텅그스텐산아민염을 제조하는데 성공하였다. 제조된 텅그스텐산 아민염의 분자량을 벤젠용매에서 더미스트를 이용한 감도 1/$4000^{\circ}C$의 훼트스톤 브리지를 사용하여 측정할 수 있었다. 분자량 측정결과와 화학분석 및 적외선 스펙트럼으로 부터 pH=2, 4에서 생긴 아민염은 메타텅그스텐산염, pH=6에서 생긴 아민염은 파라텅그스텐산염이 아니고 미지의 새로운 다중텅고스텐산염임을 알 수 있었다.

Trioctylamine-and tricaprylylmethylammonium chloride-tungstate salts have been prepared by solvent extraction from the sodium tungstate solution of various acidities(pH = 2, 4, 6). The molecular weights of the amine-tungstate salts thus obtained could be cryoscopically measured in benzene by means of a home-built Wheatstone bridge utilizing thermistor with sensitivity of 1/$4000^{\circ}C$. The cryoscopic data along with the results of chemical analysis and infrared spectra of the salts indicate that the amine-tungstates prepared at pH = 2 and 4 are all metatungstate whereas the salt obtained at pH = 6 is an unknown form quite different from the expected paratungstate.R = 0.14. By hydrogen bonding a guanidyl nitrogen of a sulfaguanidine molecule is linked to the sulfonyl oxygens of the other molecules indirectly through two different water molecules. The role of water molecule is both a .nor and an acceptor in hydrogen-bonding formation and these hydrogen bonds are tetrahedrally o?ented. The hydrogen-bonding networks form infinite molecular layers parallel to (001) plane.

키워드

참고문헌

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