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AA型自动分析仪检测总挥发碱的改进

Improvement on Determining Total Volatile Bases in Tobacco Leaves by AA Ⅱ Automatic Analyzer

  • 摘要: 用AA Ⅱ型自动分析仪测定烟叶中的总挥发碱存在3种缺陷:①测定结果不准确;②基线不稳定;③分析管路腐蚀严重。为了使AA Ⅱ型自动分析仪能够快速准确地测定烟叶中的总挥发碱,参考烟草行业标准YC/T 35-1996《烟草及烟草制品总挥发碱的测定》的测试原理,对AA Ⅱ型自动分析仪挥发碱检测模块进行了4种改进:①增设了蒸馏装置,使挥发碱的测定结果符合行业标准规定的要求;②用pH=8磷酸钾缓冲溶液替代NaOH溶液作蒸馏介质,克服了NaOH溶液腐蚀AA Ⅱ型自动分析仪分析管路的缺陷;③用水循环法代替气体冷却法,确保了基线稳定,使得标准溶液的工作曲线线性良好;④在碘酸钾-碘化钾反应平衡体系中加入一定量的稀磷酸(0.075mL 85%磷酸+1 000mL水)和在磷酸钾缓冲液中加入一定量的甘油(250mL甘油+1 000mL水)使基线更加稳定。确定了改进后的AA Ⅱ型自动分析仪检测挥发碱的最佳参数。这些参数为:进样速率:30个样品/h;进样与清洗时间比:1:1;比色计增益参数:35;蒸馏介质:磷酸钾缓冲液(pH=8);蒸馏温度:140℃;反应体系:碘化钾(KI)-碘酸钾(KIO3);滤光片波长:420nm。测定了标准溶液的工作曲线,在0~65mg/L (以氨计算)检测范围内为线性方程,其相关系数为r=0.999 6。检测烟叶总挥发碱的变异系数<2.0%,回收率为98.0%~99.6%,与YC/T 35-1996规定方法的相对平均偏差在0.08%~5%范围内,符合YC/T 35-1996规定的"两平行测定结果相对平均偏差不大于6.0%"的要求。满足了企业快速检测烟叶和卷烟产品总挥发碱的需要,并为企业节省了大量人力物力。改进得到了德国BRAN+LUEBBE公司及国内同行的认可,以改进技术开发的AA Ⅲ型自动分析仪已在国内烟草行业推广应用。

     

    Abstract: There were three disadvantages in determining the total volatile bases in tobacco leaves with AA Ⅱ automatic analyzer-inaccuracy of result, unsteadiness of baseline and heavy erosion of analytic tube.Modifications were made based on the principle of the industrial standard YC/T 35-1996, including:1) adding a volatile base distiller;2) using a buffer solution of potassium phosphate replacing the aqueous solution of hydroxide sodium as distilling medium to prevent the analytic tube from erosion;3) using circulated water cooling in place of the air cooling to stabilize the baseline;4) adding a fixed amount of dilute phosphorous acid (0.075 mL 85% phosphorous acid + 1 000 mL water) and glycerin (250 mL glycerin +1 000 mL water) to the reaction system of potassium iodidepotassium iodate and the buffer solution of potassium phosphate respectively, to further the baseline steady.The quency:30 samples per hour;ratio of injection time to purging time:1:1;gain factor of colorimeter:35;distilling medium:pH=8 buffer solution of potassium phosphate;distilling temperature:140℃;reaction system:potassium iodide-potassium iodate;and wavelength of light filter:420nm.The calibration curve of the standard solution was a linear equation in the range of 0 to 65mg/L (as NH3) and its correlation coefficient was 0.999 6.The coefficient of variation was below 2.0%and the recoveries of the volatile bases were in the range of 98.0% to 99.6%.The relative mean deviation of test results between the improved analyzer and the standard method was within 0.08% to 5%, and was in conformity with the requirement of YC/T 35-1996.These improvements were adopted by German BRAN +LUEBBE Company and some domestic tobacco enterprises.The AA Ⅲ automatic analyzer developed on the basis of the improvements was broadly applied in Chinese tobacco industry.

     

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