Determination of Total Nitrogen in Plant Fruits by Graphite Digestion Apparatus and Automatic Azotometer
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摘要: 通过测定植物果实中的氮元素含量，能够掌握植物生长状况，为提高优质果实的产量提供重要信息。目前分析测试植物果实中全氮的方法为传统凯氏定氮法，主要步骤为消解、蒸馏和滴定，消解时间约90min，蒸馏滴定时间约10~20min，分析测定过程较为繁琐，容易产生人为误差，不适于大批量植物果实样品的分析检测。为了缩短植物果实样品全氮的分析测定时间、提高工作效率，避免人为误差以及解决消解过程中样品飞溅和白烟逸出的问题，本文使用石墨消解仪对样品进行消解，加入浓硫酸和催化剂并加盖回流塞，使用全自动定氮仪进行分析测定，消解过程中样品不发生损失，白烟不逸出，消解时间约50min，蒸馏时间约3min，试剂消耗量小，相对误差和相对标准偏差均小于5%。本文建立的方法能够满足实验室快速、准确检测大批量植物样品中全氮的分析需求，已在中国地质调查局地调招标项目和河北省农用地土壤污染状况详查项目中得到了应用。Abstract:
BACKGROUNDBy measuring the nitrogen content in plant fruits, the growth status of plants can be grasped and important information for improving the yield of high-quality fruits can be provided. At present, the traditional Kjeldahl method is used to determine nitrogen in plant fruits. The main steps are digestion, distillation and titration. The digestion time of traditional method is 90 minutes, and the titration and distillation time is 10-20 minutes. The determination process is complicated and produces errors, which is not suitable for the analysis of large amounts of plant fruits. OBJECTIVESTo shorten the analysis and determination time of total nitrogen in plant fruit samples, improve work efficiency, avoid artificial errors, and solve the problems of sample splashing and white smoke escaping during digestion. METHODSA graphite digestion instrument was used for digestion. Concentrated sulfuric acid and a catalyst were added, the reflux plug was capped, and an automatic nitrogen determination instrument was used for analysis. RESULTSThe sample did not splash and the white smoke did not escape. The digestion time was 50 minutes and the distillation time was 3 minutes. The reagent consumption was reduced by 2mL. The relative error and relative standard deviation were less than 5%. CONCLUSIONSThe established method meets the needs of the laboratory to quickly and accurately detect total nitrogen in large amounts of plant samples. It has been applied in the detailed survey project of the China geological survey bidding project and the detailed investigation of the soil pollution status of agricultural land in Hebei Province. -
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表 1 石墨消解仪不同温度下全氮的测试结果
Table 1. Analytical results of total nitrogen digested by graphite digestion apparatus at different temperatures
样品 全氮含量测定值(mg/kg) 全氮含量认定值(mg/kg) 320℃ 350℃ 400℃ 450℃ GBW10019 2739 2840 3098 2842 3100 GBW10020 20630 22400 24747 22681 24700 GBW10014 22043 25860 28002 25896 28000 GBW10016 38074 47210 50046 47063 51000 样品A 1517 1704 1852 1712 - 样品B 762 998 1092 991 - 样品C 1411 1658 1802 1703 - 
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表 2 准确度和精密度实验
Table 2. Accuracy and precision tests of the method
标准物质编号 全氮含量(mg/kg) 相对误差
(%)RSD
(%)认定值 12次测定值 平均值 GBW10019 3100 3043 3050 3028 3115
3070 3099 3052 3070
3058 3098 3059 30893069 -1.00 0.8 GBW10020 24700 24110 24005 24747 24608
24284 24162 24114 24152
24692 24851 24845 2439824414 -1.16 1.3 GBW10014 28000 27838 27785 27461 28208
28796 27900 28796 27873
27567 28708 27658 2800228049 0.18 1.7 GBW10016 51000 50926 51195 50264 50538
50541 50523 50541 50650
50046 50770 50782 5035650594 -0.80 0.6
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