流动注射技术结合光谱分析技术测定水体痕量总磷
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摘要
为解决目前水质监测系统存在的量程过大、检出限过高、测定精度低、废液排量高和测定周期长的问题,利用钼酸铵分光光度法结合光谱分析法,在流动注射平台下实现了水体痕量总磷(TP)的测定。测定范围涵盖GB 3838-2002和GB 18918-2002规定的总磷标准限值。对影响测定结果的因素进行分析并提出解决方案,在优化监测系统工作条件下,总磷测定的量程为0.0～1.2μg/mL,校正决定系数为0.996 3,残差平方和为0.002 3,最低检出限为0.01μg/mL;重复性测定的相对标准偏差(RSD)为0.49%～3.67%;加标回收率为99.291 67%～101.941 70%,一次完整测定的废液排量约30.15mL,测定周期约25.50min。
Considering the large range, high detection limit and low measuring accuracy, high effluent displacement and long determination period of the existing water quality monitoring system, the total trace phosphorus in water was measured by making use of ammonium molybdate spectrophotometry and spectroscopic analysis under a flow injection platform. The measurement range covers the specified limits for total phosphorus content of surface waters stipulated in GB 3838-2002 and GB 18918-2002. Analyzing the factors which influencing the measurement result was carried out and solutions to it were proposed to show that, through optimizing the working condition of the monitoring system, the measurement range of total phosphorus stays at 0.0 to 1.2μg/mL along with the correction coefficient of 0.996 3 and the residual squared sum of 0.002 3 and the minimum detection limit of 0.01μg/mL; the RSD of repeatability ranges from 0.49% to 3.67% and the recovery rate from 99.291 67% to 101.941 70%. As for waste liquid displacement of about 30.15 mL completely measured, the required period of determination is about 25.50 min.
Considering the large range, high detection limit and low measuring accuracy, high effluent displacement and long determination period of the existing water quality monitoring system, the total trace phosphorus in water was measured by making use of ammonium molybdate spectrophotometry and spectroscopic analysis under a flow injection platform. The measurement range covers the specified limits for total phosphorus content of surface waters stipulated in GB 3838-2002 and GB 18918-2002. Analyzing the factors which influencing the measurement result was carried out and solutions to it were proposed to show that, through optimizing the working condition of the monitoring system, the measurement range of total phosphorus stays at 0.0 to 1.2μg/mL along with the correction coefficient of 0.996 3 and the residual squared sum of 0.002 3 and the minimum detection limit of 0.01μg/mL; the RSD of repeatability ranges from 0.49% to 3.67% and the recovery rate from 99.291 67% to 101.941 70%. As for waste liquid displacement of about 30.15 mL completely measured, the required period of determination is about 25.50 min.
引文
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[2] 毛艳贞,刘耀敏,宋军,等.分光光度法测定饲料级磷酸盐中总磷含量[J].饲料研究,2012,(3):72～74.
[3] 黄城,周燕,曾淦宁,等.抗坏血酸—钼蓝分光光度法测定海藻中磷的研究探讨[J].海洋环境科学,2009,28(z1):76～78.
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[5] 袁石林,马天云,宋韬,等.土壤中总氮与总磷含量的近红外光谱实时检测方法[J].农业机械学报,2009,40(z1):150～153.
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[7] 蔡秀萍.分光光度法测定水中总磷的若干影响因素[J].江苏农业科学,2011,39(4):436～438.
[8] 所汝丽,周可立.分光光度法测定总磷含量的探讨[J].工业水处理,2008,28(8):68～69.
[9] 刘建利,张沛,宋蓓,等.连续流动分析法测定水中总磷、总氮比对研究[J].化学研究与应用,2016,28(7):936～941.
[10] 张景飞,牛晓君,马宏瑞,等.流动注射分光光度法测定水体总磷[J].分析化学,2002,30(7):839～842.
[11] 王庆霞,苏苓,黄晓菊.流动注射氯化亚锡还原光度法测定水中总磷[J].环境监测管理与技术,2006,18(3):21～22.
[12] 陈艳玲,黎艳葵.氯化亚锡还原光度法测定总磷的方法改进[J].环境科学与技术,2004,27(z1):43～44.
[13] 王海峰,李春燕,刘新侠.钼酸铵分光光度法测定水中总磷的改进消解方法[J].中国给水排水,2009,25(16):81～83.
[14] 丁明军,杨慧中.水中总磷和总氮含量的离子色谱测定法[J].分析化学,2012,40(3):381～385.
[15] 翁艳.吸光光度法测定水中总磷的改进[J].理化检验(化学分册),2002,38(11):593～594.
[16] GB 3838-2002,地表水环境质量标准[S].北京:中国标准出版社,2002.
[17] GB 18918-2002,城镇污水处理厂污染物排放标准[S].北京:中国标准出版社,2002.
[18] GB/T 11893-1989,水质总磷的测定钼酸铵分光光度法[S].北京:中国标准出版社,1990.
[2] 毛艳贞,刘耀敏,宋军,等.分光光度法测定饲料级磷酸盐中总磷含量[J].饲料研究,2012,(3):72～74.
[3] 黄城,周燕,曾淦宁,等.抗坏血酸—钼蓝分光光度法测定海藻中磷的研究探讨[J].海洋环境科学,2009,28(z1):76～78.
[4] 杨广杏,陈桂枝,钟远清.蔬菜中总磷、总氮联合消解方法的研究[J].农业环境保护,1998,(6):24～26.
[5] 袁石林,马天云,宋韬,等.土壤中总氮与总磷含量的近红外光谱实时检测方法[J].农业机械学报,2009,40(z1):150～153.
[6] 邱慎初,丁堂堂.探讨城市污水生物处理出水的总磷达标问题[J].中国给水排水,2002,18(9):23～25.
[7] 蔡秀萍.分光光度法测定水中总磷的若干影响因素[J].江苏农业科学,2011,39(4):436～438.
[8] 所汝丽,周可立.分光光度法测定总磷含量的探讨[J].工业水处理,2008,28(8):68～69.
[9] 刘建利,张沛,宋蓓,等.连续流动分析法测定水中总磷、总氮比对研究[J].化学研究与应用,2016,28(7):936～941.
[10] 张景飞,牛晓君,马宏瑞,等.流动注射分光光度法测定水体总磷[J].分析化学,2002,30(7):839～842.
[11] 王庆霞,苏苓,黄晓菊.流动注射氯化亚锡还原光度法测定水中总磷[J].环境监测管理与技术,2006,18(3):21～22.
[12] 陈艳玲,黎艳葵.氯化亚锡还原光度法测定总磷的方法改进[J].环境科学与技术,2004,27(z1):43～44.
[13] 王海峰,李春燕,刘新侠.钼酸铵分光光度法测定水中总磷的改进消解方法[J].中国给水排水,2009,25(16):81～83.
[14] 丁明军,杨慧中.水中总磷和总氮含量的离子色谱测定法[J].分析化学,2012,40(3):381～385.
[15] 翁艳.吸光光度法测定水中总磷的改进[J].理化检验(化学分册),2002,38(11):593～594.
[16] GB 3838-2002,地表水环境质量标准[S].北京:中国标准出版社,2002.
[17] GB 18918-2002,城镇污水处理厂污染物排放标准[S].北京:中国标准出版社,2002.
[18] GB/T 11893-1989,水质总磷的测定钼酸铵分光光度法[S].北京:中国标准出版社,1990.