Determination of Total Nitrogen in Plant Fruits by Graphite Digestion Apparatus and Automatic Azotometer
-
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. -
-
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 - 
下载: 导出CSV
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
下载: 导出CSV
-
[1] 赵平, 孙谷畴, 彭少麟.植物氮素营养的生理生态学研究[J].生态科学, 1998(2):39-44. http://www.cnki.com.cn/Article/CJFDTotal-STKX802.006.htm
Zhao P, Sun G C, Peng S L.Ecophysiological research on nitrogen nutrition of plant[J].Ecologic Science, 1998(2):39-44. http://www.cnki.com.cn/Article/CJFDTotal-STKX802.006.htm
[2] 张敬敏, 桑茂鹏, 朱哲, 等.植物对氨基酸的吸收研究进展[J].氨基酸和生物资源, 2013, 35(2):19-22. http://d.old.wanfangdata.com.cn/Periodical/ajshswzy201302006
Zhang J M, Sang M P, Zhu Z, et al.Progress on the amino acid absorption of plant[J].Amino Acids and Biotic Resources, 2013, 35(2):19-22. http://d.old.wanfangdata.com.cn/Periodical/ajshswzy201302006
[3] 杨成, 贺华中, 罗绪强, 等.大气污染影响下凯里植物氮、硫含量分析[J].环境监测管理与技术, 2012, 24(3):52-55. doi: 10.3969/j.issn.1006-2009.2012.03.011
Yang C, He H Z, Luo X Q, et al.Analysis on nitrogen and sulphur contents in plant leaves under air pollution in Kaili, Guizhou[J].The Administration and Technique of Environmental Monitoring, 2012, 24(3):52-55. doi: 10.3969/j.issn.1006-2009.2012.03.011
[4] 周显骥.巨峰葡萄施氮技术研究[J].湖南农业大学学报, 1999(3):188-190. http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=hunannydx199903005
Zhou X J.Studies on application of nitrogen to Jufeng grape[J].Journal of Hunan Agricultural University, 1999(3):188-190. http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=hunannydx199903005
[5] 蒋万峰, 崔永峰, 张卫东, 等.无核白葡萄叶内矿质元素含量年生长季内的变化[J].西北农林科技大学学报(自然科学版), 2005(8):91-95. doi: 10.3321/j.issn:1671-9387.2005.08.019
Jiang W F, Cui Y F, Zhang W D, et al.Annual changes of mineral elements in foliar of thompsons seedless[J]. Journal of Northwest Agriculture and Forest University (Natural Science Edition), 2005(8):91-95. doi: 10.3321/j.issn:1671-9387.2005.08.019
[6] 武丽艳, 郑翼腾, 吴勇, 等.凯氏定氮装置的改进[J].化学通报, 2008, 71(2):158-160. http://d.old.wanfangdata.com.cn/Periodical/hxtb2200802014
Wu L Y, Zheng Y T, Wu Y, et al.Improvements on the equipment of Kjeldahl method[J]. Chemistry Bulletin, 2008, 71(2):158-160. http://d.old.wanfangdata.com.cn/Periodical/hxtb2200802014
[7] 王雅.蛋白质测定实验的研究[J].实验室研究与探索, 2005(4):58-59. doi: 10.3969/j.issn.1006-7167.2005.04.021
Wang Y.Study on protein determination experiment[J].Research and Exploration in Laboratory, 2005(4):58-59. doi: 10.3969/j.issn.1006-7167.2005.04.021
[8] 郭颖娜, 孙卫.蛋白质含量测定方法的比较[J].河北化工, 2008(4):36-37. doi: 10.3969/j.issn.1003-5059.2008.04.015
Guo Y N, Sun W.Comparison of methods for determination of protein content[J].Hebei Chemical Industry, 2008(4):36-37. doi: 10.3969/j.issn.1003-5059.2008.04.015
[9] 罗小芬.浅谈凯氏定氮法测定蛋白质准确度的操作技巧及关键点[J].现代食品, 2017(19):99-100. http://d.old.wanfangdata.com.cn/Periodical/lsltjs201719031
Luo X F.Talking about the operation skills and key points of determining protein accuracy by Kjeldahl method[J].Modern Food, 2017(19):99-100. http://d.old.wanfangdata.com.cn/Periodical/lsltjs201719031
[10] Jung S, Rickert D A, Deak N A, et al.Comparison of Kjeldahl and Dumas methods for determining protein contents of soybean products[J].Journal of the American Oil Chemists' Society, 2003, 80(12):1169-1173. doi: 10.1007/s11746-003-0837-3
[11] 张泽泉, 罗翠婷, 李孔寿, 等.凯氏定氮法蛋白质测定的改进探讨[J].海峡预防医学杂志, 2017, 23(1):64-66. http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=hxyfyxzz201701030
Zhang Z Q, Luo C T, Li K S, et al.Modification of protein determination by Kjeldahl method[J].Strait Journal of Preventive Medicine, 2017, 23(1):64-66. http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=hxyfyxzz201701030
[12] 刘正, 刘亚兵, 张进, 等.乳及乳制品中蛋白质含量的测定[J].农业科技与信息, 2014(7):24-25. doi: 10.3969/j.issn.1003-6997.2014.07.020
Liu Z, Liu Y B, Zhang J, et al.Determination of protein content in dairy products and dairy products[J].Agricultural Science-Technology and Information, 2014(7):24-25. doi: 10.3969/j.issn.1003-6997.2014.07.020
[13] 曾庆庭.半微量凯氏定氮法测定地球化学样品中全氮时的影响因素及消除方法[J].广东化工, 2018, 45(12):225-226. doi: 10.3969/j.issn.1007-1865.2018.12.100
Zeng Q T.The influence factors and elimination methods of the determination of nitrogen in geochemical samples by semi-micro Kjeldahl method[J].Guangdong Chemical Industry, 2018, 45(12):225-226. doi: 10.3969/j.issn.1007-1865.2018.12.100
[14] Daun J K, Declercq D R.Comparison of combustion and Kjeldahl methods for determination of nitrogen in oilseeds[J].Journal of the American Oil Chemists' Society, 1994, 71(10):1069-1072. doi: 10.1007/BF02675898
[15] 白金峰, 胡外英, 张勤, 等.半微量凯氏法测定土壤全氮量的不确定度评定[J].岩矿测试, 2007, 26(1):40-44. doi: 10.3969/j.issn.0254-5357.2007.01.011 http://www.ykcs.ac.cn/article/id/ykcs_20070118
Bai J F, Hu W Y, Zhang Q, et al. Uncertainty evaluation of measurement results for the determination of total nitrogen in soil samples by semimicro Kjeldahl method[J].Rock and Mineral Analysis, 2007, 26(1):40-44. doi: 10.3969/j.issn.0254-5357.2007.01.011 http://www.ykcs.ac.cn/article/id/ykcs_20070118
[16] 胡子峰.凯氏定氮仪原理和校准的方法[J].上海计量测试, 2011, 38(3):49-50. doi: 10.3969/j.issn.1673-2235.2011.03.015
Hu Z F.Principle and calibration method of Kjeldahl nitrogen determiner[J].Shanghai Measurement and Testing, 2011, 38(3):49-50. doi: 10.3969/j.issn.1673-2235.2011.03.015
[17] 李宇庆, 陈玲, 赵建夫.土壤全氮测定方法的比较[J].广州环境科学, 2006, 21(3):28-29. http://d.old.wanfangdata.com.cn/Periodical/scgyxyxb201403020
Li Y Q, Chen L, Zhao J F.Comparison of methods for determining total nitrogen in soil[J].Guangzhou Environmental Sciences, 2006, 21(3):28-29. http://d.old.wanfangdata.com.cn/Periodical/scgyxyxb201403020
[18] 刘广东, 田翠芳, 王雅菁.石墨消解仪在测定土壤中铬的应用研究[J].广州化工, 2018, 46(13):64-65. doi: 10.3969/j.issn.1001-9677.2018.13.022
Liu G D, Tian C F, Wang Y J, et al.Study on application of graphite dissociator in measurement of chromium in soil[J].Guangzhou Chemical Industry, 2018, 46(13):64-65. doi: 10.3969/j.issn.1001-9677.2018.13.022
[19] 谢小玲, 李海锋, 李雪莹, 等.土壤全氮半微量定氮法与自动定氮仪定氮法的比较分析[J].生态环境学报, 2012, 21(6):1071-1074. http://d.old.wanfangdata.com.cn/Periodical/tryhj201206013
Xie X L, Li H F, Li X Y, et al.Comparison and analysis of semi-micro nitrogen determination method and automatic nitrogen determination method for soil total nitrogen[J].Ecology and Environment Sciences, 2012, 21(6):1071-1074. http://d.old.wanfangdata.com.cn/Periodical/tryhj201206013
[20] 郑贤光, 辛若竹.全自动凯氏定氮仪测定化肥中的含氮量[J].化学分析计量, 2014, 23(5):41-43. doi: 10.3969/j.issn.1008-6145.2014.05.014
Zheng X G, Xin R Z.Determination of nitrogen content of fertilizer by automatic Kjeldahl apparatus[J].Chemical Analysis and Meterage, 2014, 23(5):41-43. doi: 10.3969/j.issn.1008-6145.2014.05.014
[21] 徐新娟, 黄中文, 王伟.全自动凯氏定氮仪测定大豆蛋白质方法的研究[J].黑龙江农业科学, 2016(2):108-110. http://d.old.wanfangdata.com.cn/Periodical/hljnykx201602029
Xu X J, Huang Z W, Wang W.Study on the processing conditions of soybean protein sample with automatic Kjeldahl nitrogen determination apparatus[J].Heilongjiang Agricultural Sciences, 2016(2):108-110. http://d.old.wanfangdata.com.cn/Periodical/hljnykx201602029
[22] 于兆水, 胡外英, 张勤.多目标地球化学调查土壤样品中氮和碳的快速测定[J].岩矿测试, 2007, 26(3):235-237. doi: 10.3969/j.issn.0254-5357.2007.03.015 http://www.ykcs.ac.cn/article/id/ykcs_20070381
Yu Z S, Hu W Y, Zhang Q.Rapid determination of nitrogen and carbon in soil samples for the multi-purpose geochemical survey[J].Rock and Mineral Analysis, 2007, 26(3):235-237. doi: 10.3969/j.issn.0254-5357.2007.03.015 http://www.ykcs.ac.cn/article/id/ykcs_20070381
[23] 栾慧, 刘红, 高一娜, 等.土壤速效氮测定方法的改进[J].湖南农业科学, 2017(3):88-89. http://d.old.wanfangdata.com.cn/Periodical/hunannykx201703025
Luan H, Liu H, Gao Y N, et al.Study on the determination method of soil alkali hydrolysis nitrogen[J].Hunan Agricultural Sciences, 2017(3):88-89. http://d.old.wanfangdata.com.cn/Periodical/hunannykx201703025
[24] 杨娜, 董迈青, 谢海东, 等.应用响应曲面法优化凯氏定氮法的消解条件[J].岩矿测试, 2014, 33(1):40-43. doi: 10.3969/j.issn.0254-5357.2014.01.008 http://www.ykcs.ac.cn/article/id/4820adaa-2b6b-4bd5-8e26-bbc5296b229e
Yang N, Dong M Q, Xie H D, et al.Optimization of digestion conditions in the Kjeldahl method for nitrogen analysis using response surface methodology[J].Rock and Mineral Analysis, 2014, 33(1):40-43. doi: 10.3969/j.issn.0254-5357.2014.01.008 http://www.ykcs.ac.cn/article/id/4820adaa-2b6b-4bd5-8e26-bbc5296b229e
[25] 袁静宇.凯氏定氮法测定玉米淀粉蛋白质含量最佳消化温度的摸索[J].粮食与饲料工业, 2013(11):25-27. http://d.old.wanfangdata.com.cn/Periodical/lsyslgy201311007
Yuan J Y.Optimum digestion temperature for determina-tion of protein content by Kjeldahl method[J].Cereal and Feed Industry, 2013(11):25-27. http://d.old.wanfangdata.com.cn/Periodical/lsyslgy201311007
[26] 陈春霏, 付洁, 梁鹏, 等.土壤中全氮分析方法的研究进展[J].中国环境监测, 2018, 34(1):112-119. http://d.old.wanfangdata.com.cn/Periodical/zghjjc201801015
Chen C F, Fu J, Liang P, et al.Research progress on analytical methods for total nitrogen in soil[J].Environmental Monitoring in China, 2018, 34(1):112-119. http://d.old.wanfangdata.com.cn/Periodical/zghjjc201801015
[27] 李玉华, 刘红, 陈燕芹, 等.自动电位滴定法测定煤中氮[J].贵州工程应用技术学院学报, 2015, 33(6):149-151. doi: 10.3969/j.issn.1673-7059.2015.06.026
Li Y H, Liu H, Chen Y Q, et al.Automatic potentiometric titration method for the determination of nitrogen element in coal[J].Journal of Guizhou University of Engineering Science, 2015, 33(6):149-151. doi: 10.3969/j.issn.1673-7059.2015.06.026
[28] 李杉杉.凯氏定氮法测定蛋白质的方法分析[J].现代食品, 2018(21):140-142. http://d.old.wanfangdata.com.cn/Periodical/lsltjs201821045
Li S S.Analysis the methods of protein determination by Kjeldahl method[J].Modern Food, 2018(21):140-142. http://d.old.wanfangdata.com.cn/Periodical/lsltjs201821045
[29] 李海锋, 李雪莹, 袁红梅.用全自动凯氏定氮仪测定肥料中总氮含量方法探讨[J].广州化工, 2018, 46(10):87-89. doi: 10.3969/j.issn.1001-9677.2018.10.029
Li H F, Li X Y, Yuan H M.Determination of total nitrogen content in fertilizer by full automatic Kjeldahl nitrogen meter[J].Guangzhou Chemical Industry, 2018, 46(10):87-89. doi: 10.3969/j.issn.1001-9677.2018.10.029
[30] 马怡飞, 张尼, 魏增, 等.振荡交换-抽滤淋洗结合凯氏定氮法快速测定土壤中的阳离子交换量[J].岩矿测试, 2019, 38(1):129-135. http://www.ykcs.ac.cn/article/doi/10.15898/j.cnki.11-2131/td.201712110191
Ma Y F, Zhang N, Wei Z, et al.Rapid determination of soil cation exchange capacity by automatic Kjeldahl analyzer after oscillating exchange and suction filtration[J].Rock and Mineral Analysis, 2019, 38(1):129-135. http://www.ykcs.ac.cn/article/doi/10.15898/j.cnki.11-2131/td.201712110191
[31] 谌国莲, 徐小艳.一种新型半微量凯氏定氮仪在本科实验教学中的开发应用[J].实验室科学, 2018, 21(6):171-174. doi: 10.3969/j.issn.1672-4305.2018.06.046
Chen G L, Xu X Y.Development and application of a new semi-micro Kjeldahl nitrogen-fixation instrument in undergraduate experimental teaching[J].Laboratory Science, 2018, 21(6):171-174. doi: 10.3969/j.issn.1672-4305.2018.06.046
-
图(2)
表(2)
计量
- 文章访问数: 1498
- PDF下载数: 96
- 施引文献: 0