摘要
随着水土资源环境日益恶化,监测氨氮量对水土的污染程度也备受关注。为了准确测定铝灰渣浸出液中的氨氮量,建立了纳氏试剂分光光度法测定铝灰渣浸出液中的氨氮含量的方法。通过对振荡方法、振荡时间、固液比、试液过滤方式、纳氏试剂加入量以及测定干扰因素的研究,确定了以翻转振荡为前处理方式,最佳振荡时间为14 h,固液比为1∶10,最佳纳氏试剂加入量为1.0 mL,通过改善过滤方式降低空白值的方法。由实验结果可知,F-对氨氮量的测定不产生干扰;对于浸出液中Cl-、Al^(3+)和Ca^(2+)浓度高的样品,可通过移取稀释液2.00 mL,加入1.0 mL酒石酸钾钠溶液(500 g/L),即可消除其干扰。运用纳氏试剂分光光度法测定铝灰渣浸出液中的氨氮量,得到氨氮标准曲线线性相关系数为0.9998,方法检出限为0.39 mg/L,相对标准偏差(RSD,n=6)<5%,加标回收率在94.7%~105%。方法简单快速,精密度高,且具有较低的检出限,适用于大批量铝灰、铝渣等固体废物浸出液中氨氮量的测定。
With the deteriorating environment of water and soil resources,the monitoring of the pollution degree of ammonia nitrogen in water and soil has also attracted much attention.To accurately determine the amount of ammonia nitrogen in the leaching solution of aluminum ash slag,the oscillation method,the oscillation time,solid-liquid ratio,test solution filtration method,the amount of Nessler reagent added,and the determination of interfering factors were studied.It was determined that the pretreatment method was inversion oscillation,the optimal oscillation time was 14 h,the solid-liquid ratio was 1∶10,and the optimal addition amount of Nessler reagent was 1.0 mL and reduced blank values by improving filtering.It can be seen from the experimental results:F-does not interfere with the determination of ammonia nitrogen;for samples with high concentrations of Cl-,Al^(3+)and Ca^(2+)in the leaching solution,its interference can be eliminated by pipetting 2.00 mL of the diluent and adding 1.0 mL of potassium sodium tartrate solution(500 g/L).The content of ammonia nitrogen in the leaching solution of aluminum ash slag was determined by Nessler′s reagent spectrophotometry,the linear correlation coefficient of the nitrogen standard curve was 0.9998,the detection limit of the method was 0.39 mg/L,RSD(n=6)<5%,and the recoveries were between 94.7%and 105%.The method is simple,rapid,has high precision,has a low detection limit,and is suitable for the determination of ammonia nitrogen in the leaching solution of large quantities of aluminum ash and aluminum slag,and other solid wastes.
作者
吕长宽
曾志平
施意华
唐碧玉
张征莲
LYU Changkuan;ZENG Zhiping;SHI Yihua;TANG Biyu;ZHANG Zhenglian(China Nonferrous Metal(Guilin)Geology and Mining Co.,Ltd.,Guilin,Guangxi 541004,China)
出处
《中国无机分析化学》
CAS
北大核心
2022年第6期82-88,共7页
Chinese Journal of Inorganic Analytical Chemistry
基金
广西科学研究与技术开发计划项目(桂科AD20325011)。
关键词
固体废物
翻转振荡
纳氏试剂
铝灰渣
氨氮量
solid waste
inversion oscillation
nessler reagent
aluminium ash slag
ammonia nitrogen amount
