土壤腐殖酸慢热解表征实验影响因素研究
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摘要
以土壤提取的腐殖酸为研究对象,进行了差式量热扫描(DSC)和热重分析(TGA)的可重复性实验、样品质量对比实验和预处理对比实验。综合分析了影响慢热解特征温度参数的因素和效应,并根据作用原理将其总结为热滞后效应和反应平衡滞后效应。结果表明,高级热分析技术用于土壤慢热解表征可重复性良好,差式量热扫描与热重分析结果可比性强,然而热分析曲线和热特征参数对实验条件的响应灵敏,其中样品质量和升温速率的影响尤其显著。研究结果表明,慢热解技术用于土壤有机质分析具有良好的准确性和重现性,提出了保障土壤腐殖酸慢热解质量控制的最佳样品量[DSC为(10±0.1)mg]、最佳气体氛围(He)和最佳升温速率(10℃/min)、精确压实程度等实验条件。
Take soil humic acid as the research object, the repeatability experiments, quality comparison experiments and pretreatment comparison experiments were carried out by differential scanning calorimetry(DSC) and thermogravimetric analysis(TGA). The factors and effects that affect the temperature parameters of slow pyrolysis were analyzed, and the two principles of heat lag effect and reaction equilibrium lag effect were summarized. The results showed that the advanced thermal technique used for soil slow pyrolysis characterization had good repeatability, and the results of DSC and TGA results were highly comparable. The thermal analysis curves and thermal characteristic parameters sensitively responded to the purge gas, crucible property and other factors, while the influence of sample quality and heating rate was particularly significant. The research results are important for promoting the application of thermal analysis technology in soil monitoring and evaluation.
Take soil humic acid as the research object, the repeatability experiments, quality comparison experiments and pretreatment comparison experiments were carried out by differential scanning calorimetry(DSC) and thermogravimetric analysis(TGA). The factors and effects that affect the temperature parameters of slow pyrolysis were analyzed, and the two principles of heat lag effect and reaction equilibrium lag effect were summarized. The results showed that the advanced thermal technique used for soil slow pyrolysis characterization had good repeatability, and the results of DSC and TGA results were highly comparable. The thermal analysis curves and thermal characteristic parameters sensitively responded to the purge gas, crucible property and other factors, while the influence of sample quality and heating rate was particularly significant. The research results are important for promoting the application of thermal analysis technology in soil monitoring and evaluation.
引文
[1] 王业耀,赵晓军,何立环. 我国土壤环境质量监测技术路线研究[J].中国环境监测,2012,28(3):116-120.WANG Yeyao,ZHAO Xiaojun,HE Lihuan,et al.The Research of Technique Route for National Soil Environment Monitoring[J].Environmental Monitoring in China,2012,28(3):116-120.
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[3] OUDGHIRI F,GARCíA-MORALES J L,RODRíGUEZ-BARROSO M R. Novel use of TGA-FTIR Technique to Predict the Pollution Degree in Marine Sediments[J].Infrared Physics & Technology,2015,72:52-57.
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[8] WU F,XU L,SUN Y,et al.Exploring the Relationship Between Polycyclic Aromatic Hydrocarbons and Sedimentary Organic Carbon in Three Chinese Lakes[J].J Soils Sediments,2012,12(5):774-783.
[9] WU F,XU L,LIAO H,et al.Relationship Between Mercury and Organic Carbon in Sediment Cores from Lakes Qinghai and Chenghai,China[J].J Soils Sediments,2013,13(6):1 084-1 092.
[10] BAI Y,WU F,XING B,et al.Isolation and Characterization of Chinese Standard Fulvic Acid Sub-Fractions Separated from Forest Soil by Stepwise Elution with Pyrophosphate Buffer[J].Scientific Reports,2015,5:8 723.
[11] 王业耀,孟凡生,陈锋.阴极pH控制对污染土壤电动修复效率的影响[J].环境科学研究,2007,20(2):36-40.WANG Yeyao,MENG Fansheng,CHEN Feng.Effect of pH Control at the Cat Hode for the Electrokinetic Remediation Efficiency[J].Research of Environmental Sciences,2007,20(2):36-40.
[12] 杨冬雪.土壤监测几种质量控制指标及评价方法探讨[J].中国环境监测,2010,26(4):78-82.YANG Dongxue.Research on Quality Control Index System and Evaluation Method of Soil Monitoring[J].Environmental Monitoring in China,2010,26(4):78-82.
[13] 邹志勇,张志朋,彭靖恺,等.桂林蔬菜基地土壤监测的质量控制与质量保证[J].环境科学与技术,2014,(S2):396-400.ZOU Zhiyong,ZHANG Zhipeng,PENG Jingkai,et al.The Quality Control and Quality Assurance of Soil Environmental Quality Monitoring in Vegetable-Soils of Guilin City[J].Environmental Science & Technology,2014,(S2):396-400.
[14] CEBULAK S,LANGIER-KUZNIAROWA A.Application of Oxyreactive Thermal Analysis to the Examination of Organic Matter Associated with Rocks[J].J Therm Anal,1997,50(1/2):175-190.
[15] FERNáNDEZ J M,PLANTE A F,LEIFELD J,et al.Methodological Considerations for Using Thermal Analysis in the Characterization of Soil Organic Matter[J].J Therm Anal Calorim,2011,104(1):389-398.
[16] 王镛先,朱华仁,白冰冰.热分析测定条件对结果的影响[J].矿物岩石,1983,(2):87-93.WANG Yongxian,XIAN Huaren,BAI Bingbing.The Influence of the Thermal Analytic Measuring Conditions on the Results[J].Journal of Mineralogy and Petrology,1983,(2):87-93.
[17] SCHAWE J E K.Modulated Temperature DSC Measurements:The Influence of the Experimental Conditions[J].Thermochim Acta,1996,271(95):127-140.
[18] 张建策.热分析实验条件选择对实验结果的影响[J].化工技术与开发,2010,39(12):44-45.ZHANG Jiance.Effect of Experimental Conditions Choice on Thermal Analysis Experiment Results[J].Technology & Development of Chemical Industry,2010,39(12):44-45.
[19] GUO F,MU Y,CHEN C,et al.Thermal and Spectral Characterization of Anaerobic Thermal Behavior Patterns in a Lacustrine Sediment Core[J].Environmental Science & Pollution Research,2016,23(19):19 949-19 957.
[20] GUO F,WU F,MU Y,et al.Characterization of Organic Matter of Plants from Lakes by Thermal Analysis in a N2 Atmosphere[J].Scientific Reports,2016,(6):22 877.
[21] BONANNO A,BERNOLD L E.Exploratory Review of Sintered Lunar Soil Based on the Results of the Thermal Analysis of a Lunar Soil Simulant[J].Journal of Aerospace Engineering,2014,28(4):04014114.
[22] 邹华红,胡坤,桂柳成,等.一水草酸钙热重-差热综合热分析的最优化表征方法[J].广西科学院学报,2011,27(1):17-21.ZOU Huahong,HU Kun,GUI Liucheng,et al.Research on Optimal Characterization Method of CaC2O4·H2O by Thermogravimetry-Differential Thermal Analyzer[J].Journal of Guangxi Academy of Sciences,2011,27(1):17-21.
[23] FATHOLLAHI M,POURMORTAZAVI S M,HOSSEINI S G.Particle Size Effects on Thermal Decomposition of Energetic Material[J].J Energ Mater,2007,26(1):52-69.
[24] 丁恩勇,梁学海.不同实验条件对DSC峰形的影响以及相变温度的确定[J].分析测试学报,1993(5):50-54.DING Enyong,LIANG Xuenai.The Influenees of Experimental Conditions on the Shape of DSC Curve and the Determination of Phase-Change Temperature[J].分析测试学报,1993(5):50-54.
[25] WARNE S S J.Thermal Analysis of Minerals:Dumitru N.Todor.Abacus Press,Tunbridge Wells,Kent,England[J].Geoderma,1978,21(3):245-246.
[26] PLANTE A F,FERNáNDEZ J M,HADDIX M L,et al.Biological,Chemical and Thermal Indices of Soil Organic Matter Stability in Four Grassland Soils[J].Soil Biology and Biochemistry,2011,43(5):1 051-1 058.
[27] VITOORI A L,DELL′ABATE M T,BUSCAROLI A,et al.Role of Soil Organic Matter Characteristics in a Pedological Survey:“Bosco Frattona” Natural Reserve(Site of Community Importance,Italy) Case Study[J].Geoderma,156(3/4):302-315.
[28] MIAO S J,QIAO Y F,YOU M,et al.Thermal Stability of Soil Organic Matter Was Affected by 23-yr Maize and Soybean Continuous Cultivation in Northeast of China[J].J Therm Anal Calorim,2016,123(3):2 045-2 051.
[2] 陆泗进,王业耀,何立环. 中国土壤环境调查、评价与监测[J].中国环境监测,2014,30(6):19-26.LU Sijin,WANG Yeyao,HE Lihuan. Soil Environmental Quality Survey and Monitoring in China[J].Environmental Monitoring in China,2014,30(6):19-26.
[3] OUDGHIRI F,GARCíA-MORALES J L,RODRíGUEZ-BARROSO M R. Novel use of TGA-FTIR Technique to Predict the Pollution Degree in Marine Sediments[J].Infrared Physics & Technology,2015,72:52-57.
[4] OUTRIDGE P,SANEI H,STERN G,et al.Evidence for Control of Mercury Accumulation Rates in Canadian High Arctic Lake Sediments by Variations of Aquatic Primary Productivity[J].Environ Sci Technol,2007,41(15):5 259-5 265.
[5] KWON E,CASTALDI M J. Fundamental Understanding of the Thermal Degradation Mechanisms of Waste Tires and Their Air Pollutant Generation in a N2 Atmosphere[J].Environ Sci Technol,2009,43(15):5 996-6 002.
[6] LORENZ K,LAL R. The Depth Distribution of Soil Organic Carbon in Relation to Land use and Management and the Potential of Carbon Sequestration in Subsoil Horizons[J].Adv Agron,2005,88:35-66.
[7] 崔婷婷,窦森,杨轶囡,等.秸秆深还对土壤腐殖质组成和胡敏酸结构特征的影响[J].土壤学报,2014,(4):718-725.CUI Tingting,DOU Sen,YANG Yinan,et al.Effect of Deep Applied Corn Stalks on Composition of Soil Humus and Structure of Humic Acid[J].Acta Pedologica Sinica,2014,(4):718-725.
[8] WU F,XU L,SUN Y,et al.Exploring the Relationship Between Polycyclic Aromatic Hydrocarbons and Sedimentary Organic Carbon in Three Chinese Lakes[J].J Soils Sediments,2012,12(5):774-783.
[9] WU F,XU L,LIAO H,et al.Relationship Between Mercury and Organic Carbon in Sediment Cores from Lakes Qinghai and Chenghai,China[J].J Soils Sediments,2013,13(6):1 084-1 092.
[10] BAI Y,WU F,XING B,et al.Isolation and Characterization of Chinese Standard Fulvic Acid Sub-Fractions Separated from Forest Soil by Stepwise Elution with Pyrophosphate Buffer[J].Scientific Reports,2015,5:8 723.
[11] 王业耀,孟凡生,陈锋.阴极pH控制对污染土壤电动修复效率的影响[J].环境科学研究,2007,20(2):36-40.WANG Yeyao,MENG Fansheng,CHEN Feng.Effect of pH Control at the Cat Hode for the Electrokinetic Remediation Efficiency[J].Research of Environmental Sciences,2007,20(2):36-40.
[12] 杨冬雪.土壤监测几种质量控制指标及评价方法探讨[J].中国环境监测,2010,26(4):78-82.YANG Dongxue.Research on Quality Control Index System and Evaluation Method of Soil Monitoring[J].Environmental Monitoring in China,2010,26(4):78-82.
[13] 邹志勇,张志朋,彭靖恺,等.桂林蔬菜基地土壤监测的质量控制与质量保证[J].环境科学与技术,2014,(S2):396-400.ZOU Zhiyong,ZHANG Zhipeng,PENG Jingkai,et al.The Quality Control and Quality Assurance of Soil Environmental Quality Monitoring in Vegetable-Soils of Guilin City[J].Environmental Science & Technology,2014,(S2):396-400.
[14] CEBULAK S,LANGIER-KUZNIAROWA A.Application of Oxyreactive Thermal Analysis to the Examination of Organic Matter Associated with Rocks[J].J Therm Anal,1997,50(1/2):175-190.
[15] FERNáNDEZ J M,PLANTE A F,LEIFELD J,et al.Methodological Considerations for Using Thermal Analysis in the Characterization of Soil Organic Matter[J].J Therm Anal Calorim,2011,104(1):389-398.
[16] 王镛先,朱华仁,白冰冰.热分析测定条件对结果的影响[J].矿物岩石,1983,(2):87-93.WANG Yongxian,XIAN Huaren,BAI Bingbing.The Influence of the Thermal Analytic Measuring Conditions on the Results[J].Journal of Mineralogy and Petrology,1983,(2):87-93.
[17] SCHAWE J E K.Modulated Temperature DSC Measurements:The Influence of the Experimental Conditions[J].Thermochim Acta,1996,271(95):127-140.
[18] 张建策.热分析实验条件选择对实验结果的影响[J].化工技术与开发,2010,39(12):44-45.ZHANG Jiance.Effect of Experimental Conditions Choice on Thermal Analysis Experiment Results[J].Technology & Development of Chemical Industry,2010,39(12):44-45.
[19] GUO F,MU Y,CHEN C,et al.Thermal and Spectral Characterization of Anaerobic Thermal Behavior Patterns in a Lacustrine Sediment Core[J].Environmental Science & Pollution Research,2016,23(19):19 949-19 957.
[20] GUO F,WU F,MU Y,et al.Characterization of Organic Matter of Plants from Lakes by Thermal Analysis in a N2 Atmosphere[J].Scientific Reports,2016,(6):22 877.
[21] BONANNO A,BERNOLD L E.Exploratory Review of Sintered Lunar Soil Based on the Results of the Thermal Analysis of a Lunar Soil Simulant[J].Journal of Aerospace Engineering,2014,28(4):04014114.
[22] 邹华红,胡坤,桂柳成,等.一水草酸钙热重-差热综合热分析的最优化表征方法[J].广西科学院学报,2011,27(1):17-21.ZOU Huahong,HU Kun,GUI Liucheng,et al.Research on Optimal Characterization Method of CaC2O4·H2O by Thermogravimetry-Differential Thermal Analyzer[J].Journal of Guangxi Academy of Sciences,2011,27(1):17-21.
[23] FATHOLLAHI M,POURMORTAZAVI S M,HOSSEINI S G.Particle Size Effects on Thermal Decomposition of Energetic Material[J].J Energ Mater,2007,26(1):52-69.
[24] 丁恩勇,梁学海.不同实验条件对DSC峰形的影响以及相变温度的确定[J].分析测试学报,1993(5):50-54.DING Enyong,LIANG Xuenai.The Influenees of Experimental Conditions on the Shape of DSC Curve and the Determination of Phase-Change Temperature[J].分析测试学报,1993(5):50-54.
[25] WARNE S S J.Thermal Analysis of Minerals:Dumitru N.Todor.Abacus Press,Tunbridge Wells,Kent,England[J].Geoderma,1978,21(3):245-246.
[26] PLANTE A F,FERNáNDEZ J M,HADDIX M L,et al.Biological,Chemical and Thermal Indices of Soil Organic Matter Stability in Four Grassland Soils[J].Soil Biology and Biochemistry,2011,43(5):1 051-1 058.
[27] VITOORI A L,DELL′ABATE M T,BUSCAROLI A,et al.Role of Soil Organic Matter Characteristics in a Pedological Survey:“Bosco Frattona” Natural Reserve(Site of Community Importance,Italy) Case Study[J].Geoderma,156(3/4):302-315.
[28] MIAO S J,QIAO Y F,YOU M,et al.Thermal Stability of Soil Organic Matter Was Affected by 23-yr Maize and Soybean Continuous Cultivation in Northeast of China[J].J Therm Anal Calorim,2016,123(3):2 045-2 051.
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