Mkukuma L D, Skakle J M S, Gibson I R, Imrie C T, Aspden R M, Hukins D W L
Department of Orthopaedic Surgery, University of Aberdeen, Foresterhill, Aberdeen AB25 2ZD, UK.
Calcif Tissue Int. 2004 Oct;75(4):321-8. doi: 10.1007/s00223-004-0199-5. Epub 2004 Jul 13.
Thermogravimetric analysis linked to mass spectrometry (TGA-MS) shows changes in mass and identifies gases evolved when a material is heated. Heating to 600 degrees C enabled samples of bone to be classified as having a high (cod clythrum, deer antler, and whale periotic fin bone) or a low (porpoise ear bone, whale tympanic bulla, and whale ear bone) proportion of organic material. At higher temperatures, the mineral phase of the bone decomposed. High temperature X-ray diffraction (HTXRD) showed that the main solids produced by decomposition of mineral (in air or argon at 800 degrees C to 1000 degrees C) were beta-tricalcium phosphate (TCP) and hydroxyapatite (HAP), in deer antler, and CaO and HAP, in whale tympanic bulla. In carbon dioxide, the decomposition was retarded, indicating that the changes observed in air and argon were a result of the loss of carbonate ions from the mineral. Fourier transform infrared (FTIR) spectroscopy of bones heated to different temperatures, showed that loss of carbon dioxide (as a result of decomposition of carbonate ions) was accompanied by the appearance of hydroxide ions. These results can be explained if the structure of bone mineral is represented by [Formula: see text] where V(Ca) and V(OH) correspond to vacancies on the calcium and hydroxide sites, respectively, and 2-x-y = 0.4. This general formula is consistent in describing both mature bone mineral (i.e., whale bone), with a high Ca/P molar ratio, lower HPO4(2-) content, and higher CO3(2-) content, and immature bone mineral (i.e., deer antler), with a low Ca/P ratio, higher HPO4(2-), and lower CO3(2-) content.
热重分析与质谱联用(TGA-MS)显示了材料加热时质量的变化并识别出逸出的气体。加热到600摄氏度能够将骨样品分类为含有高比例(鳕鱼肩胛骨、鹿茸和鲸耳周围鳍骨)或低比例(鼠海豚耳骨、鲸鼓泡和鲸耳骨)有机物质的样品。在更高温度下,骨的矿物相分解。高温X射线衍射(HTXRD)表明,矿物分解(在800摄氏度至1000摄氏度的空气或氩气中)产生的主要固体在鹿茸中是β-磷酸三钙(TCP)和羟基磷灰石(HAP),在鲸鼓泡中是CaO和HAP。在二氧化碳中,分解受到抑制,这表明在空气和氩气中观察到的变化是矿物中碳酸根离子损失的结果。对加热到不同温度的骨进行傅里叶变换红外(FTIR)光谱分析表明,二氧化碳的损失(由于碳酸根离子分解)伴随着氢氧根离子的出现。如果骨矿物的结构由[公式:见原文]表示,其中V(Ca)和V(OH)分别对应钙和氢氧根位点上的空位,且2 - x - y = 0.4,那么这些结果就可以得到解释。这个通式在描述成熟骨矿物(即鲸骨)时是一致的,成熟骨矿物具有高Ca/P摩尔比、较低的HPO4(2-)含量和较高的CO3(2-)含量,以及未成熟骨矿物(即鹿茸),未成熟骨矿物具有低Ca/P比、较高的HPO4(2-)和较低的CO3(2-)含量。