为了准确地检测出粉煤灰中残留的氨含量,分析了纳氏分光光度法、中和滴定法和氨气敏电极法检测粉煤灰中残留氨含量的主要影响因素,探讨了这3种检测方法的主要影响因素的最佳值选取,研究了3种方法结果的相关性。结果表明:影响纳氏分光光度法的主要因素为浸提剂、浸提固液比和浸提时间,最佳值选取分别为0.05 mol/L H2SO4、1∶10和30 min;影响中和滴定法的主要因素为吸收溶液、氢氧化钠加入量和蒸馏时间,最佳值选取分别为0.05 mol/L H2SO4、0.2 g和30 min;影响氨气敏电极法的主要因素为提取液和搅拌时间,最佳值选取分别为去离子水和[10,25] min。同时,这3种方法检测结果的相关性较好。研究成果探究了适用于有效定量检测粉煤灰中残留氨的方法,为控制和限定粉煤灰中残留氨提供检测基础。
Abstract
The residual ammonia in fly ash was measured by Nessler’s reagent spectrophotometry method, neutralization titration method, and ammonia-sensitive electrode method respectively in this paper. The main influence factors and their values were determined and the correlation among results of these three methods were investigated in detail. Results showed that the main influence factors of Nessler’s reagent spectrophotometry method were extraction solvent (best as 0.05 mol/L H2SO4), liquid ratio (optimum as 1∶10), and extraction time (optimum as 30 min); the main influence factors of neutralization titration method were absorption solution(best as 0.05mol/L H2SO4), sodium hydroxide content (optimum as 0.2 g) and distillation time (optimum as 30 min); the main influence factors of ammonia-sensitive electrode method were extracting solution (best as deionized water) and stirring time (optimum as [10, 25] min). In addition, the results of the three methods are of good correlation.
关键词
粉煤灰 /
残留氨 /
检测方法 /
影响因素 /
纳氏分光光度法 /
中和滴定法 /
氨气敏电极法 /
相关性
Key words
fly ash /
residual ammonia /
measuring method /
influence factor /
Nessler’s reagent spectrophotometry /
neutralization titration method /
ammonia-sensitive electrode method /
correlation
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参考文献
[1] BITTNER J, GASIOROWSKI S, HRACH F. Removing Ammonia from Fly Ash[C] ∥International Ash Utilization Symposium, Center for Applied Energy Research. Kentucky, USA,October 22-24,2001.
[2] 张 宇,王 智,孙化强,等. 脱硝后粉煤灰中氨氮物质的性质探讨[J] .粉煤灰,2015,27(5):5-6.
[3] 张 宇,王 智,王子仪,等. 燃煤电厂脱硝工艺对其粉煤灰性质的影响[J] . 非金属矿,2015(4):9-12.
[4] MINKARA R Y. Control of Ammonia Emission from Ammonia-laden Fly Ash in Concrete: US, US6790264[P] . 2004.
[5] 黄洪财. 粉煤灰氨味问题成因的调查研究[J] . 新型建筑材料,2013,40(12):23-25.
[6] 吴丹虹. 问题粉煤灰引起混凝土异常现象的原因分析[J] . 粉煤灰,2009, 21(3):42-48.
[7] 罗 斌. 新拌混凝土的氨味分析及对强度的影响[J] . 湖南交通科技,2015,41(3):33-36.
[8] KWAN J, CHO S D, DONG H, et al. Effect of Ammonia Concentration on the Utilization of ACFA (Ammonia Contaminated Fly Ash) as an Additive in Mortar and Concrete Mixture[J] . Journal of Industrial & Engineering Chemistry, 2007, 13(6): 932-938.
[9] 钟智坤,路 璐,吴华成,等. 电极法检测灰中氨的样品处理研究[J] . 华北电力技术,2014(12):52-54.
[10] 徐陆妹,陈荣乐. 生活饮用水中氨氮检测方法的研究[J] . 中国卫生检验杂志,2010,20(3):673-674.
[11] HJ 535—2009,水质 氨氮的测定 纳氏试剂分光光度法[S] .北京:中国环境出版社,2019.
基金
中央级公益性科研项目(CKSF2017032/GC,CKSF2017034/GC)