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Triethanol amine 鹽酸鹽의 結晶學的 硏究

Triethanol amine 鹽酸鹽의 結晶學的 硏究
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대학원 화학과
Triethanol amine염산염결정학
이화여자대학교 대학원
One mole each aqueous solution of triethanol amine and hydrochloric acid were reacted by mole ratio of 1 : 1, and single crystals of triethanol amine HC1 salt were grown according to the openair evaporation method. Oscillation, equator and lst. layer Weissenberg photographs of the a, b and c axes were taken by using characteristic X-ray (Cu-K_(α), λ= 1.5418 Å), and it was found out that this triethanol amino HCl crystal belongs to monoclinic system ai the results of analysis and calculation of these photographs. Also it was measured that the length of three axes of unit cell from the layer distance of oscillation photographs, and β angle value between a and c axes from the b-axis Weissenberg photograph, and density of this single crystal in accordance with floatation method. Then chemical formula unit, Z, in a unit cell was calculated and the following values of cell dimension were obtained. a = 8.97 Å b = 8.19 Å c = 12.70 Å β = 83° Z = 4 Assignment of Miller indices and intensity measurement for each spot on the Weissenberg photograph were conducted and intensity adjustment were made by using Lorentz-Polarization factor and it was found out that possible space group is C^6_(2h) or C^4_s according to the extinction law. To determine final space group for this crystal, calculations were made by the Wilson's intensity statistical method and the result was indicating this crystal has the space group of C^4_s. For the support of this result, the final conclusion of the space group was reached as C^4_s for this crystal after the analysis and combined review of symmetry of triethanol amine HCl molecule, correlation between symmetry elements of C^(6)_(2h) and C⁴_s, and. evaluated Z value of 4 for this crystal. Consequently, the coordinates of equivalent position which is indicating molecular symmetry relationships are as follows : (0, 0, 0 ; ½, ½, ½) + (x, y, z ; x, y­, ½+z). To determine the coordinate of chlorine atom which is most heaviest atom within the triethanol amine HCl molecule, the Patterson-function syntheses indicating inter-atomic vector projections on the planes of a and b axes were made based on the following mathematical equations. ◁수식 삽입▷(원문을 참조하세요) By the selection of Cl-Cl vectors from the projection reap of Patterson-function, it was able to obtain the coordinate of chlorine atoms within the unit cell. The coordinate of chlorine atom seems to be reasonable as the Cl-Cl distance value lies between 6.07 - 8.79 Å.
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