炽灼残渣操作

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炽灼残渣操作指南

OperationGuidelinesfortheDeterminationofResidueon

Ignition

1.目的PURPOSE

1.1.本规程旨在指导炽灼残渣操作。

Theoperationguidelinesareintendedtoguidetheoperationofresidueonignition(ROI)experiment.

2.范围SCOPE

2.1.本规程适用于检查有机药物中混入的非挥发性无机杂质。

TheguidelinesapplytoallROIanalysisconductedatAnalyticalDepartment.

3.责任RESPONSIBILITY

3.1.分析部负责执行本规程。

Analyticalstaff:followtheproceduresdefinedintheguidelinesManagement:ensuresthattheguidelinesarefollowed

4.规程PROCEDURE

4.1.参照USP34ResidueonIgnition

Reference:USP34ResidueonIgnition

4.1.1.取清白、适合材质的坩埚（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）；取出坩埚置于枯燥器（硅胶或其他适合枯燥剂）中冷却约1.5小时；缜密称定坩埚的重量W1。

Igniteasuitablecrucible(forexample,silica,platinum,quartz,orporcelain)at640℃(typicallyovernight)inamufflefurnace,coolforabout1.5hoursinadesiccator(silicagelorothersuitabledesiccant),weighitaccuratelyasW1.

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:Aplatinumcrucibleshouldbeusedfortestingofalkalimetalsorfluorinesubstances.DeterminationofROIofphosphorusorsiliconcompoundsshouldbeadvisedtouseothermethods.

4.1.2.缜密称取1.0~2.0g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。

Weighaccurately1.0to2.0gofthesubstanceasW2,ortheamountspecifiedintheindividualmonograph,inthecrucible.

注：在称取样品时，应将样品置于称量纸上称量；假使样品引湿性较强，应以初次稳定的读数为准。

Note:weighthesubstanceontheweightpaper,whichishygroscopic,shouldregister

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theinitial,steadyvalue.

4.1.3.用少量（寻常1mL）硫酸润湿样品，然后在尽量低的温度下渐渐加热(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；避免供试品受热猛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，再参与少量（寻常1mL）硫酸润湿样品，缓慢加热至不再有白烟生成。

Moistenthesamplewithasmallamount(usually1mL)ofsulfuricacid,thenheatgentlyatatemperatureaslowaspracticable(adjustelectriccookerknobtoheatgentlyuntilsmokegeneratedslightly,keepthetemperatureconstantuntilthereisnosmoke.Thenadjustelectriccookerknobtohightemperaturegentlyuntilwhitefumesarenolongerevolved;avoidthesampleoverflowbecauseofexpandingsuddenlyorburning.)untilthesampleisthoroughlycharred,cool,then,unlessotherwisedirectedintheindividualmonograph,moistentheresiduewithasmallamount(usually1mL)ofsulfuricacid,heatgentlyuntilwhitefumesarenolongerevolved.

4.1.4.将上述坩埚置马弗炉内，坩埚盖斜盖于坩埚上，除非个别文献另有说明，在640℃

炽灼(一般炽灼过夜)，直至样品完全灰化；取出坩埚置于枯燥器（硅胶或其他适合枯燥剂）中冷却约1.5小时；缜密称定坩埚及残渣的重量W3。

Ignitethesampleat640℃（typicallyovernight）andthecruciblemaybelooselycoveredwithasuitablelidduringtheigniting，unlessanothertemperatureisspecifiedintheindividualmonograph,untiltheresidueiscompletelyincinerated,coolthecrucibleforabout1.5hoursinadesiccator(silicagelorothersuitabledesiccant),weighitaccuratelyasW3.

4.1.5.按公式计算其炽灼残渣：ROI%=(W3-W1)/W2*100。

Calculatethepercentageofresidueasfollows:ROI%=(W3-W1)/W2*100.

4.1.6.假使算得的数值明显超过特定文献的限度，则需重复以上硫酸润湿、加热、炽灼

的过程，直至连续两次测得的残渣的质量相差小于0.5mg，或者算得的炽灼残渣在特定的文献限度内。

Iftheamountoftheresiduesoobtainedexceedsthelimitspecifiedintheindividualmonograph,repeatthemoisteningwithsulfuricacid,heatingandignitingasbefore,untiltwoconsecutiveweightingsoftheresiduedonotdifferbymorethan0.5mgoruntilthepercentageofresiduecomplieswiththelimitintheindividualmonograph.

4.2.参照Ch.P2023ⅧN炽灼残渣检查法

Reference:Ch.P2023ⅧNResidueonIgnition

4.2.1取清白的坩埚（如供试品分子中含有碱金属或氟元素，则应使用铂坩埚）置马弗

炉内，将坩埚盖斜盖于坩埚上，经700℃炽灼(一般炽灼过夜)；取出坩埚置于枯燥器（硅胶或其他适合枯燥剂）中，盖好坩埚盖，放冷至室温（约1.5h）；缜密称定坩埚(去

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盖)的重量。再以同样条件重复操作，直至恒重W1(连续两次质量相差小于0.3mg)，备用。炽灼至恒重的其次次称重应在继续炽灼30min后进行。

Igniteasuitablecrucible(aplatinumcrucibleshouldbeusedfortestingofalkalimetalsorfluorinesubstances)at700℃inamufflefurnace（typicallyovernight）andthecruciblemaybelooselycoveredwithasuitablelidduringtheigniting,coolthecruciblecoveredwiththelidinadesiccators(silicagelorothersuitabledesiccant)about1.5hours,weighthecrucible(withoutlid)accurately.Repeattheprocedure,untilthecruciblereachtheconstantweightW1（twoconsecutiveweightingsofthecrucibledonotdifferbymorethan0.3mg）.Thesecondweighingafterreachtheconstantweightshouldbeconductedin30minutesofcontinuousignition.注：含磷或含硅化合物建议采用其他方法。

Note:DeterminationofROIofphosphorusorsiliconcompoundsshouldbeadvisedtouseothermethods.

4.2.2取供试品1.0~2.0g或各品种项下规定的重量，置已炽灼至恒重的坩埚内，缜密

称定其重量为W2。

Weighaccurately1.0to2.0gofthesubstanceasW2,ortheamountspecifiedintheindividualmonograph,inthecrucible.

4.2.3将盛有供试品的坩埚置电炉上缓缓灼烧（应避免供试品受热猛然膨胀或燃烧而溢

出），直至供试品全部炭化，并不再冒烟；放冷至室温；除另有规定外，滴加硫酸0.5~1.0mL，使其全部润湿，浸润约10分钟后继续在电炉上缓慢加热至硫酸蒸气除尽。

Heatthecruciblewiththesamplegentlyatatemperatureaslowaspracticable(avoidthesampleoverflowbecauseofexpandingsuddenlyorburning)untilthesampleisthoroughlycharredandwhitefumesarenolongerevolved,cool,then,unlessotherwisedirectedintheindividualmonograph,moistentheresiduewith0.5~1.0mLsulfuricacidforabout10min,thenheatgentlyuntilfumesarenolongerevolved.

4.2.4将上述坩埚置马弗炉内，并且坩埚盖斜盖于坩埚上，在700℃）炽灼(一般炽灼过

夜)，直至供试品完全灰化；取出坩埚置于枯燥器（硅胶或其他适合枯燥剂）中，盖好坩埚盖，放冷至室温（约1.5h）；缜密称定坩埚及残渣的重量。再以同样条件重复操作，直至恒重W3。

Ignitethesampleat700℃inthemufflefurnace（typicallyovernight）andthecruciblemaybelooselycoveredwithasuitablelidduringtheigniting,untiltheresidueiscompletelyincinerated,coolthecruciblecoveredwiththelidinadesiccator(silicagelorothersuitabledesiccant)forabout1.5hours,weighitaccurately.Repeattheprocedure,untilthecrucibleandresiduereachtheconstantweightW3.

4.2.5按公式计算其炽灼残渣：ROI%=(W3-W1)/W2*100。

Calculatethepercentageofresidueasfollows:ROI%=(W3-W1)/W2*100.

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5.附录Appendix

无。None

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