SIMULTANEOUS DETERMINATION OF VOLATILE PHENOL AND CYANIDE IN GROUNDWATER BY CONTINUOUS FLOW INJECTION METHOD
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摘要:
采用SEAL AA3连续流动分析仪同时测定地下水中挥发酚和氰化物, 在最佳实验条件下, 挥发酚和氰化物的标准曲线相关系数全部在99.5%以上, 检出限分别为0.221 μg/L(以-OH计)、0.868 μg/L(以-CN计), 精密度和准确度较好, 相对标准偏差均小于1.5%. 挥发酚和氰化物的样品回收率分别为94.76%~102.5%和92.8%~103.01%, 采用双指标同时测试与单指标分别测试方法无显著差异. 采用连续流动分析法同时测定地下水中挥发酚和氰化物, 测试周期短, 自动化程度高, 适合大批量样品同时检测.
Abstract:The volatile phenol and cyanide in groundwater are determined simultaneously by SEAL AA3 continuous flow analyzer. Under the optimal experimental conditions, the standard curve correlation coefficients of volatile phenol and cyanide are all above 99.5%, with the detection limits of 0.221 μg/L(measured by -OH) and 0.868 μg/L (measured by -CN), respectively, and good precision and accuracy, the relative standard deviations of both less than 1.5%. The sample recovery rates of volatile phenol and cyanide are 94.76%-102.5% and 92.8%-103.01%, respectively. There is no significant difference between the duel-index simultaneous test and single-index separate test. The continuous flow analysis for simultaneous determination of volatile phenol and cyanide in groundwater is characterized by short test period and high degree of automation, which is suitable for simultaneous testing of large quantities of samples.
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Key words:
- continuous flow injection /
- groundwater /
- volatile phenol /
- cyanide
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表 1 酚氰标准曲线
Table 1. Parameters for standard curve of volatile phenol and cyanide
标准系列 挥发酚 氰化物 浓度/（mg/L） 相对峰高AU 浓度/（mg/L） 相对峰高AU 1 0 0 0 0 2 0.001 0.22 0.001 1.19 3 0.002 0.49 0.002 2.3 4 0.005 1.23 0.005 5.64 5 0.01 2.55 0.01 11.08 6 0.02 5.29 0.02 22.39 7 0.05 13.2 0.05 54.96 8 0.1 26.19 0.1 110.05 相关系数 1.00 1.00 线性方程 y=262.67x-0.0266 y=1099.3x+0.1188 
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表 2 方法检出限计算
Table 2. Calculation results of method detection limits
测定项目 测定值/（mg/L） 平均值 标准偏差 检出限 1 2 3 4 5 6 7 挥发酚 0.0015 0.0015 0.0015 0.0015 0.0014 0.0014 0.0014 0.001457 5.35E-05 0.000221 氰化物 0.0017 0.0014 0.0012 0.0011 0.001 0.0017 0.0014 0.001357 0.000276 0.000868
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表 3 方法检出限计算t值取值表
Table 3. Table of t values in the calculation of method detection limits
平行测定次数（n） 自由度（n-1） t（n－1，0.99） 7 6 3.143 8 7 2.998 9 8 2.896 10 9 2.821
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表 4 精密度和准确度测定结果表
Table 4. Test results of precision and accuracy
测定项目 测定值/（mg/L） 平均值 相对标准偏差/% 相对误差/% 1 2 3 4 5 6 挥发酚 0.0103 0.0103 0.0105 0.0103 0.0102 0.01006 0.010277 1.41% 2.77% 氰化物 0.0099 0.0098 0.0099 0.0096 0.0097 0.00975 0.009775 1.20% -2.25%
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表 5 加标回收率测定
Table 5. Determination of spiked recovery rate
样品 挥发酚/（mg/L） 加标回收率/% 氰化物/（mg/L） 加标回收率/% 本底值 测定值 本底值 测定值 水样1 0.005 0.025 102.5 0.005 0.0251 103.01 水样2 0.01 0.0286 95.86 0.01 0.028 92.80 水样3 0.05 0.0676 94.76 0.05 0.0682 97.82
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表 6 分析方法比较
Table 6. Comparison of analysis methods
样品 挥发酚/（mg/L） 氰化物/（mg/L） 单指标测定 双指标测定 相对偏差/% 单指标测定 双指标测定 相对偏差/% 水样1 0.0014 0.0015 6.89 0.0011 0.0012 8.69 水样2 0.0013 0.0014 7.41 0.0008 0.00085 6.06 水样3 0.0021 0.0020 -4.88 0.0007 0.0007 0
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[1] 邸志强, 苗英, 贾伟光, 等. 东北地区水资源现状及可持续利用对策[J]. 地质与资源, 2004, 13(2): 112-115. http://www.dzyzy.cn/article/id/9641
Di Z Q, Miao Y, Jia W G, et al. The present situation and measures of sustainable utilization for water resources in northeast China[J]. Geology and Resources, 2004, 13(2): 112-115. http://www.dzyzy.cn/article/id/9641
[2] 黎华, 李方林, 鲍征宇. 巴东北部地区地表水的环境化学特征及水质评价[J]. 地质与资源, 2002, 11(3): 168-172. http://www.dzyzy.cn/article/id/9741
Li H, Li F L, Bao Z Y. The environmental chemistry and quality evaluation of the surface water in the north of Badong region[J]. Geology and Resources, 2002, 11(3): 168-172. http://www.dzyzy.cn/article/id/9741
[3] 孟瑞芳, 杨会峰, 包锡麟, 等. 京津冀平原非常规水资源利用前景分析及其生态环境效应[J]. 中国地质, 2024, 51(1): 221-233.
Meng R F, Yang H F, Bao X L, et al. Prospect analysis of unconventional water resources utilization and eco-environmental effects in Beijing-Tianjin-Hebei Plain[J]. Geology in China, 2024, 51(1): 221-233.
[4] 于慧明, 郭晓东, 王晓光, 等. 松辽流域地下水资源评价区划分研究[J]. 中国地质, 2023, 50(4): 1016-1031.
Yu H M, Guo X D, Wang X G, et al. A division study of the groundwater resources evaluation area in the Songliao River Basin[J]. Geology in China, 2023, 50(4): 1016-1031.
[5] 中华人民共和国国土资源部. DZ/T 0290-2015地下水水质标准[S]. 北京: 中国标准出版社, 2016.
Ministry of Land and Resources of the People's Republic of China. DZ/T 0290-2015 Standard for groundwater quality[S]. Beijing: Standards Press of China, 2016.
[6] 田芹, 江林, 王丽平. 水体中挥发酚测定中的流动注射分光光度法研究进展[J]. 岩矿测试, 2010, 29(2): 161-168.
Tian Q, Jiang L, Wang L P. Progresses and application of flow injection analysis-spectrophotometric determination of volatile phenols in water[J]. Rock and Mineral Analysis, 2010, 29(2): 161-168.
[7] 中国环境优先监测研究课题组. 环境优先污染物[M]. 北京: 中国环境科学出版社, 1989: 15.
China Environmental Priority Monitoring Research Group. Environmental priority pollutants[M]. Beijing: China Environmental Science Press, 1989: 15. (in Chinese)
[8] 康春莉, 王英, 杜尧国, 等. 水体中挥发酚测定方法的改进[J]. 分析化学, 2000, 28(7): 872-875. doi: 10.3321/j.issn:0253-3820.2000.07.019
Kang C L, Wang Y, Du Y G, et al. Improvement on the determination of volatile phenols in water[J]. Chinese Journal of Analytical Chemistry, 2000, 28(7): 872-875. doi: 10.3321/j.issn:0253-3820.2000.07.019
[9] 国家环境保护总局《水和废水监测分析方法》编委会, 魏复盛. 水和废水监测分析方法[M]. 4版. 北京: 中国环境科学出版社, 2002: 460-462.
Editorial Committee of the Monitoring and Analysis Methods for Water and Wastewater of the State Environmental Protection Administration, Wei F S. Water and wastewater monitoring and analysis methods[M]. 4th ed. Beijing: China Environmental Science Press, 2002: 460-462. (in Chinese)
[10] 环境保护部. HJ 503-2009水质: 挥发酚的测定4-氨基安替比林分光光度法[S]. 北京: 中国环境科学出版社, 2009.
Ministry of Environmental Protection. HJ 503-2009 Water quality: Determination of volatile phenolic compounds: 4-AAP spectrophotometric method[S]. Beijing: China Environmental Science Press, 2009.
[11] 邸玉敏, 朱军, 常靖, 等. 氰化物检测方法研究进展[J]. 理化检验: 化学分册, 2011, 47(12): 1491-1494.
Di Y M, Zhu J, Chang J, et al. Recent advance of detection method of cyanide[J]. Physical Testing and Chemical Analysis Part B: Chemical Analysis, 2011, 47(12): 1491-1494.
[12] 中华人民共和国自然资源部. DZ/T 0064.2-2021地下水质分析方法第2部分: 水样的采集和保存[S]. 北京: 地质出版社, 2021.
Ministry of Natural Resources of the People's Republic of China. DZ/T 0064.2-2021 Methods for analysis of groundwater quality, Part 2: Collection and preservation of water samples[S]. Beijing: Geological Publishing House, 2021.
[13] 李苗, 王敏. 环境水体样品中挥发酚的稳定性探究[J]. 云南化工, 2022, 49(8): 95-96, 122.
Li M, Wang M. Study on stability of volatile phenol in environmental water samples[J]. Yunnan Chemical Technology, 2022, 49(8): 95-96, 122.
[14] 中华人民共和国自然资源部. DZ/T 0064.85-2021地下水质分析方法第85部分: 挥发性酚的测定流动注射在线蒸馏法[S]. 北京: 地质出版社, 2021.
Ministry of Natural Resources of the People's Republic of China. DZ/T 0064.85-2021 Methods for analysis of groundwater quality, Part 85: Determination of volatile phenol compounds: Flow injection online distillation[S]. Beijing: Geological Publishing House, 2021.
[15] 中华人民共和国自然资源部. DZ/T 0064.86-2021地下水质分析方法第86部分: 氰化物的测定流动注射在线蒸馏法[S]. 北京: 地质出版社, 2021.
Ministry of Natural Resources of the People's Republic of China. DZ/T0064.85-2021 Methods for analysis of groundwater quality, Part 86: Determination of cyanide: Flow injection online distillation[S]. Beijing: Geological Publishing House, 2021.
[16] 罗淞元. SAN++连续流动分析仪同时测定水体中挥发酚和总磷的方法探究[J]. 广西水利水电, 2023(1)142-145.
Luo S Y. Study of method for simultaneous determination of volatile phenol and total phosphorus in water with SAN++continuous flow analyzer[J]. Guangxi Water Resources & Hydropower Engineering, 2023(1)142-145.
[17] 王琬. Seal-AA3流动注射测定饮用水中阴离子合成洗涤剂[J]. 中国卫生检验杂志, 2014, 24(14): 1994-1995, 1999.
Wang W. Determination of anion synthetic detergent in drinking water by Seal-AA3 flow injection analysis[J]. Chinese Journal of Health Laboratory Technology, 2014, 24(14): 1994-1995, 1999.
[18] 俞佳铭, 沙贤亮, 朱炳祺, 等. 连续流动注射分光光度法测定杏仁中氰化物和挥发酚的含量[J]. 理化检验-化学分册, 2023, 59(6): 678-682.
Yu J M, Sha X L, Zhu B Q, et al. Determination of cyanide and volatile phenol in almond by continuous flow injection spectrophotometry[J]. Physical Testing and Chemical Analysis (Part B: Chemical Analysis), 2023, 59(6): 678-682.
[19] 张敏, 甘瑛琳, 吴恩宁, 等. 连续流动注射分析法同时测定水中挥发酚、氰化物及阴离子合成洗涤剂[J]. 医学动物防制, 2020, 36(4): 404-407.
Zhang M, Gan Y L, Wu E N, et al. Simultaneous determination of volatile phenol, cyanide and anion synthetic detergents in water by continuous flow injection analysis[J]. Journal of Medical Pest Control, 2020, 36(4): 404-407.
[20] 中华人民共和国国土资源部. DZ/T 0130-2006地质矿产实验室测试质量管理规范[S]. 北京: 中国标准出版社, 2006.
Ministry of Land and Resources of the People's Republic of China. DZ/T 0130-2006 The specification of testing quality management for geological laboratories[S]. Beijing: Standards Press of China, 2006.
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