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氟-羟磷灰石的~1H NMR谱学研究
作者:刘羽 STOPPAF TONUCCIL 彭明生 
单位:武汉化工学院材料系 d’A大学 d’A大学 中山大学地球与环境科学学院 武汉 430073 中山大学地球与环境科学学院 广州 510275  意大利 Chieti市意大利G  意大利 Chieti市意大利G  广州 510275 
关键词:羟磷灰石  核磁共振谱  氢键  氟含量 
分类号:O657.2
出版年,卷(期):页码:2002,30(S1):42-44
DOI:
摘要:
羟磷灰石(HAP)是重要的生物陶瓷材料,F的进入会影响其性质。通过对合成氟-羟磷灰石1H的NMR实验研究,发现HAP中结构羟基的1H化学位移与吸附水中的1H化学位移不同。在纯HAP中的1H的δ=-0.04×10-6,而随着F含量的增加,该谱峰不但变弱并消失,而且向低场区位移。在F相对含量为75%的F—HAP中,δ=0.44×10-6。随着F的替换,NMR谱中出现一个位于0.90×10-6~1.61×10-6的新谱蜂,其强度与F含量正相关,其位置也随着F的增加向低场区位移。这说明F的进入形成了氟氢键,从而产生了新的谱峰。由于这两个谱峰的位置和相对强度比均与F含量呈正相关,因此可以根据NMR谱中1H核的化学位移值及谱峰的相对强度来区分结晶态HAP与非晶态的磷酸盐,并对氟羟二元磷灰石的氟-羟基相对含量进行估算。
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The effect of 1H NMR spectroscopic characteristics of OH on F ions in the apatite structure was investigated. The samples include hydrothermal synthesized hydroxyapatite (HAP, sample code FO) and fluoridated hydroxyapatite (F- HAP) with F/F+ OH mole ratio from 5 % to 95 %. The following figures are found : (1) There is difference in the 1H NMR chemical shift for hydrox-yl in apatite structure (d= -0.04X 10-6-1.61 x 10-6) and absorbed water(8 = -0.04X 10-6-1.61 x 1(T6). (2) The chemical shift of 'H due to H-O bond (A) shifts to lower field region as F content increase in apatite. (3) As F enter the structure, a new NMR resonance occurs near 0.90 X 10-6-1.61 X 10-6, whose intensity increases with F, This phenomena indicates that a F-H bond is formed in apatite structural channel. As the position and intensity of these NMR peaks correlated positively with the F content, it is possible to use the chemical shift of 'H and the relative intensity of the spectral peaks to distinguish the crystalline HAP and non-crystalline phosphate, and to estimate the F and/or OH content in binary fluor- hydroxyapatite.
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基金项目:
武汉化工学院与意大利G,d’A大学校际合作项目。
作者简介:
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参考文献:
[1] REGNIER P, LASAGA AC, BERNER RA, et al. Mechanism of CO32-substitution in carbonate-fluorapatite: evidence from FTIR spectroscopy, 13C NMR, and quantum mechanical calcula-tions[J]. Am Mineral, 1994, 79:908-818. [2] BURCHILL P, HOWARTH O W, RICHARDS D G, et al. Solid-state nuclear magnetic resonance studies of phosphorus and boron in coals and combustion residues[J]. Fuel, 1990, 69: 421-428. [3] ALI A F, MUSTARELLI P, MAGISTRIS A. Optimal synthesis of ogano-phosphate precursors for sol-gel preparations[J]. Miner Res Bull, 1998, 33:697-710. [4] TURNER G L, SMITH K A, KIRKPATRICK RJ, et al. Structure and cation effects on phosphorous-31 NMR chemical shifts and chemical-shift anisotropies of orthophosphates[J]. J Magn Resonance, 1986, 70: 408-415. [5] PRAHAKAR S, RAO K J, RAO. C N R. A magic-angle spinning 31 PNMR investigation of crystalline and glassy inorganic phosphates[J]. Chem Phys Letts, 1987, 139, 96-101. [6] BESHEN K, REY C, GLIMCHER MJ, et al. Solid state carbon-13 and proton NMR studies of carbonate-containing calcium phosphates and enamel[J]. J Solid State Chem, 1990, 84:71-81. [7] BRAUN M, HARTMAN P. 19F and 31P NMR spectroscopy of calcium apatites [J]. J Mater Sci: Mater Medicine, 1995, 6: 150-154.
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