炽灼残渣操作-final.doc

炽灼残渣操作指南 Operation Guidelines for the Determination of Residue on Ignition 目的 PURPOSE The operation guidelines are intended to guide the operation of residue on ignition (ROI) experiment. 范围 SCOPE 本规程适用于。 责任 RESPONSIBILITY 部负责执行本规程。 规程PROCEDURE 参照USP34281 Residue on Ignition Reference: USP34281 Residue on Ignition 取干净、合适材质的坩埚（如二氧化硅、铂金、石英或者瓷质）置马弗炉内，经640 ℃炽灼（一般炽灼过夜）；取出坩埚置于干燥器（硅胶或其他合适干燥剂）中冷却约1.5小时；精密称定坩埚的重量W1。 Ignite a suitable crucible (for example, silica, platinum, quartz, or porcelain) at 640 ℃ (typically overnight) in a muffle furnace, cool for about 1.5 hours in a desiccator (silica gel or other suitable desiccant), weigh it accurately as W1. 注：如供试品分子中含有碱金属或氟元素，则应使用铂坩埚，含磷或含硅化合物建议采用其他方法。 Note: A platinum crucible should be used for testing of alkali metals or fluorine substances. Determination of ROI of phosphorus or silicon compounds should be advised to use other methods. 精密称取1.0~2.0 g样品W2，或个别文献特定说明质量的样品，放在之前冷却后的坩埚中。 Weigh accurately 1.0 to 2.0 g of the substance as W2, or the amount specified in the individual monograph, in the crucible. 注：在称取样品时，应将样品置于称量纸上称量；如果样品引湿性较强，应以初次稳定的读数为准。 Note: weigh the substance on the weight paper, which is hygroscopic, should register the initial, steady value. 用少量（通常1mL）硫酸润湿样品，然后在尽量低的温度下慢慢加热(加热样品至有微量烟冒出，恒定温度直至不冒烟, 随后，逐渐旋至高档位，缓慢加热至不再有白烟生成；避免供试品受热骤然膨胀或燃烧而溢出)，直至样品完全炭化；冷却；然后, 除了个别文献另有说明外，再加入少量（通常1mL）硫酸润湿样品，缓慢加热至不再有白烟生成。 Moisten the sample with a small amount (usually 1mL) of sulfuric acid, then heat gently at a temperature as low as practicable(adjust electric cooker knob to heat gently until smoke generated slightly, keep the temperature constant until there is no smoke. Then adjust electric cooker knob to high temperature gently until white fumes are no longer evolved; avoid the sample overflow because of expanding suddenly or burning.) until the sample is thoroughly charred, cool, then, unless otherwise directed in the individual monograph, moisten the residue with a small amount (usually 1mL) of sulfuric acid, heat gently un