摘要
采用扫描电镜(SEM)、X射线衍射(XRD)和傅里叶红外光谱(FTIR)研究了凝胶体系中尿抑制剂酒石酸钠(Na2tart)的浓度和结晶温度对草酸钙(CaOxa)晶体生长的影响。当Na2tart浓度为0·01mol·L-1时,体系中主要生成棱角尖锐的蔷薇花状一水草酸钙(COM)聚集体,二水草酸钙(COD)含量小于5%,此时XRD图谱上主要为归属于COM的(101),(020)和(202)晶面的衍射峰,FTIR光谱中COM晶体的羧基不对称伸缩振动νas(COO-)和对称伸缩振动νs(COO-)分别为1618和1317cm-1。当Na2tart浓度增加到0·10和0·50mol·L-1时,COD百分含量分别增加至10%和50%,COM晶体的比表面积减小。COD含量增加后,XRD图谱上归属于COD的(200),(211),(411)和(213)晶面的衍射峰增强。环境温度的影响比浓度的影响更为显著。高温(>47℃)有利于COM生成,而低温(<27℃)有利于Na2tart诱导COD。FTIR光谱中COD的νas(COO-)和νs(COO-)分别为1647·6和1327·7cm-1。
Crystallization of calcium oxalate （CaOxa） was investigated in the presence of sodium tartrate （Na2tart） of different concentration in a gel system by scanning electron microscopy （SEM）, X-ray diffraction （XRD） and Fourier transform infrared （FTIR） spectroscopy. It was found that in the presence of a low concentration of Na2tart （0. 01 mol· L^-1）, calcium oxalate monohydrate （COM） is the dominant crystal phase. The percentage of calcium oxalate dihydrate （COD） is less than 5%. In the XRD pattern the main diffraction peaks are （101）, （020）, and （-↑202） planes of COM crystals. In the FTIR spectrum, the main asymmetric carbonyl stretching band vas（COO^-） and the metal-carboxylate stretch vs（COO-） of COM occur at 1 618 and 1 317 cm^-1, respectively. With the concentration of Na2tart increasing to 0.10 and 0. 50 mol · L^-1, the percentage of COD crystals increases to 10% and 50%, respectively, and the surface area of COM crystals decreases. The diffraction peaks that assigned to the （200）, （211）, （411）, and （213） planes of COD crystals become stronger and stronger. The temperature can influence the modulation of Na2tart in terms of the phase composition and morphology of CaOxa crystals. As the temperature decreases, the percentage of COD increases. At a higher temperature beyond 47℃, COM is the dominant phase; but COM is dominant when the temperature is lower than 27℃. The vas （COO^-） and vs （COO^-） of COD crystals occur at 1 647. 6 and 1 327. 7 cm^-1, respectively.
出处
《光谱学与光谱分析》
SCIE
EI
CAS
CSCD
北大核心
2006年第5期874-878,共5页
Spectroscopy and Spectral Analysis
基金
国家自然科学基金(20471024)
国家自然科学基金重点项目(20031010)
广东省"千百十工程"优秀人才培养基金(Q02060)
南京大学配位化学国家重点实验室开放基金项目资助
