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比较了直接在石英蒸馏瓶中不加CaO进行灰化,然后直接以磷酸溶解进行甲醇蒸馏分离硼,以美黄素比色法测定石墨中硼的方法和在铂坩埚中加CaO灰化,以磷酸溶解后移入聚乙烯蒸馏瓶中进行蒸馏分离硼,以姜黄素比色法测定石墨中硼的方法。得出:当以石英蒸馏瓶不加CaO直接进行灰化,流出气体以NaOH溶液吸收,再以此溶液来接受甲醇馏出液时,所得结果能与加CaO灰化的结果相符合;但由于石英瓶经长时间使用后会被磷酸所腐蚀,使结果重现性不佳。因此,拟定了在铂坩埚中加CaO灰化,以磷酸溶解后以聚乙烯瓶进行蒸馏分离硼,以姜黄素法比色测定石墨中硼的方法。所得结果表明,当含量在3×10~(-5)%左右时,结果的相对标准偏差为11%。当取2克样品时,方法的测定下限为2×10~(-6)%(误差不大于50%)。回收率在95%以上。
Compared directly to the quartz distillation flask without CaO ashing, and then dissolved directly to phosphoric acid methanol distillation separation of boron, with photometric method for the determination of boron in graphite and platinum crucible with CaO ashing, with Phosphoric acid dissolved into the polyethylene distillation flask distillation separation boron, with curcumin colorimetric method for the determination of boron in graphite. It can be concluded that when the ashing is carried out directly without ashing in CaO, the effluent gas is absorbed in NaOH solution and the solution is used to receive the methanol distillate. The result is consistent with the result of CaO ashing. However, Quartz bottles will be corroded by phosphoric acid after prolonged use, resulting in poor reproducibility of results. Therefore, the preparation of calcium in the platinum crucible ashing, phosphoric acid dissolved in polyethylene bottles after distillation separation boron, curcumin colorimetric determination of boron in graphite method. The results showed that when the content is about 3 × 10 ~ (-5)%, the relative standard deviation of the results is 11%. When taking 2 grams of sample, the method has a lower limit of detection of 2 × 10 -6% (error no greater than 50%). Recovery rate of 95% or more.