光纤耦合微通道反应系统原位监测海水氨氮和亚硝酸盐的研究

姜双城; 杜虹; 郑惠东; 汤新华; 潘文涛; 高俊; 范丹阳; 林琪; 吕海霞; 林旭聪

doi:10.12284/hyxb2023006

光纤耦合微通道反应系统原位监测海水氨氮和亚硝酸盐的研究

doi: 10.12284/hyxb2023006

姜双城^{1, 2,},
杜虹²,
郑惠东¹,
汤新华^{3, 4},
潘文涛¹,
高俊⁴,
范丹阳⁴,
林琪^1, ,,
吕海霞⁴,
林旭聪^{4, 5, ,}

1.
福建省水产研究所，福建厦门 361013
2.
汕头大学理学院，广东汕头 515063
3.
厦门斯坦道科学仪器股份有限公司，福建厦门 361013
4.
福建省产品质量与食品安全检测试剂和仪器工程技术研究中心，福建福州 350108
5.
福州大学化学学院，福建福州 350108

基金项目: 福建省海洋与渔业结构调整专项(2020HYJG05，2021HYJG09)；福建省海洋发展补助资金专项(ZHHY−2019−4，FJHJF−L−2020−8，FJHJF−L−2021−9)；福建省高校产学合作项目（2020Y4004）；科技部重点专项（SQ2020YFF0426577）。

详细信息

作者简介:
姜双城（1980-），男，山东省济宁市人，助理研究员，主要从事海洋环境监测与保护研究。 E-mail: 2001082011@163.com

通讯作者:
林琪，男，研究员，主要从事水产养殖科研工作。E-mail: xmqlin@sina.com

林旭聪，男，教授，主要从事环境分析与食品安全研究，E-mail: xulin@fzu.edu.cn

中图分类号: O657.3
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出版历程
- 收稿日期: 2022-04-02
- 修回日期: 2022-06-27
- 网络出版日期: 2022-07-13
- 刊出日期: 2023-01-09

In-situ monitoring of ammonia nitrogen and nitrite in seawater by fiber-coupled micro-channel reaction system

Jiang Shuangcheng^{1, 2
,},
Du Hong²,
Zheng Huidong¹,
Tang Xinhua^{3, 4},
Pan Wentao¹,
Gao Jun⁴,
Fan Danyang⁴,
Lin Qi^{1
, ,},
Lü Haixia⁴,
Lin Xucong^{4, 5
, ,}

1.
Fisheries Research Institute of Fujian, Xiamen 361013, China
2.
College of Science, Shantou University, Shantou 515063, China
3.
Xiamen Standards Scientific Instrument Co. Ltd., Xiamen 361013, China
4.
Engineering Technology Research Center on Reagent and Instrument for Rapid Detection of Product Quality and Food Safety, Fuzhou 350108, China
5.
Chemistry College, Fuzhou University, Fuzhou 350108, China

摘要

摘要: 原位监测海水中氨氮（NH₃-N）和亚硝酸盐（${\rm{NO}}_2^- $）对于水体富营养化评价十分重要。针对现有的氨氮、亚硝酸盐原位监测仪器难以在同一检测模块中分别实现荧光和分光光度分析，仪器高效集成及利用受到限制等问题，本文基于光纤耦合微通道反应系统，通过光波长切割、光纤波导和微通道反应 Z 型检测池等技术集成和条件优化，提出了在同一光纤偶联微反应系统中实现氨氮荧光分析和亚硝酸盐分光光度分析的原位测定技术。结果表明，该技术实现了荧光和可见光光度法的模式切换并可分别测定NH₃-N和${\rm{NO}}_2^- $；在恒温条件下，NH₃-N测定荧光信号漂移小于−2.0%，${\rm{NO}}_2^- $测定吸光度稳定；不同的盐度对氨氮和亚硝酸盐测定影响较小；不同浊度下氨氮测定误差为−6.6%～2.5%，浊度补偿校正后${\rm{NO}}_2^-$测定误差小于0.1%。将该仪器应用于养殖海水中开展氨氮和亚硝酸盐的原位分析，仪器原位监测值与实验室方法测定值相符合。本文所提出的技术在同一模块中分别实现了氨氮和亚硝酸盐的荧光和分光光度两种模式的原位监测，为海水营养盐原位监测仪器的集成化设计提供了新的思路。
- 原位监测 /
- 光纤耦合 /
- 微通道反应系统 /
- 氨氮 /
- 亚硝酸盐
Abstract: In-situ monitoring of ammonia nitrogen (NH₃-N) and nitrite (${\rm{NO}}_2^- $) in seawater is important for evaluating water eutrophication. To date, it is difficult to achieve fluorescence and spectrophotometric analysis of ammonia nitrogen and nitrite in a single detection module, and the efficient integration and utilization of instruments are limited. Herein, in view of this problem, a fiber-coupled micro-channel reaction system was proposed based on technologies such as optical wavelength cutting, optical fiber waveguide and micro-channel reaction Z-cell detection, and realized the fluorescence detection of ammonia nitrogen and the in-situ determination of nitrite by spectrophotometry in the same detection system. The results showed that the mode switching of fluorescence and visible photometry could be realized and NH₃-N and ${\rm{NO}}_2^- $ was accomplished by this technique, respectively. Under the constant temperature condition, the drift value of fluorescence signal in NH₃-N measurement was less than −2.0%, and the absorbance intensity of ${\rm{NO}}_2^- $ measurement was stable. Little effect on the determination of ammonia nitrogen and nitrite was provided by different salinity. The acceptable measurement error of ammonia nitrogen under different turbidity ranged in −6.6% to 2.5%, and the measurement error of ${\rm{NO}}_2^- $ after turbidity compensation correction was less than 0.1%. The instrument was applied to the in-situ analysis of ammonia nitrogen and nitrite in aquaculture seawater, and the detection value achieve by this method was consistent with the standard method. This method realized in-situ automatic detection of ammonia nitrogen and nitrite in a same module, and provided a new idea for the better integration of in-situ monitoring instruments for real-time monitoring of NH₃-N and ${\rm{NO}}_2^- $ in seawater.
- in-situ monitoring /
- fiber-coupled /
- micro-channel reaction system /
- ammonia nitrogen /
- nitrite

HTML全文

图 1 光纤耦合微通道反应系统原位检测装置示意图

Fig. 1 Schematic of the fiber-coupled micro-channel reaction system for in-situ detection

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图 2 不同浓度氨氮的荧光光谱（a）和亚硝酸盐的吸收光谱（b）

Fig. 2 Fluorescence spectra (a) and absorption spectra (b) of ammonia nitrogen and nitrite with different concentrations, respectively

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图 3 温度对氨氮检测荧光强度（a）和亚硝酸盐吸光度（b）的影响

Fig. 3 Effect of temperature on fluorescence intensity of ammonia nitrogen detection (a) and absorbance of nitrite (b)

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图 4 pH对反应荧光强度和吸光度的影响

Fig. 4 Effects of pH on fluorescence intensity and absorbance of the reaction

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图 5 盐度对氨氮测定荧光强度的影响

Fig. 5 Effects of salinity on fluorescence intensity for ammonia nitrogen detection

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图 6 盐度−浊度−亚硝酸盐浓度变化量的曲面图

Fig. 6 Surface plot of salinity-turbidity-nitrite concentration variation

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图 7 不同盐度下亚硝酸盐预测值及盐度补偿结果

Fig. 7 Predicted values of nitrite and salinity compensation results under different salinities

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图 8 不同浊度下亚硝酸盐溶液预测值及补偿结果

Fig. 8 Predicted value and compensation result of nitrite under different turbidity

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表 1 浊度对氨氮测定的影响

Tab. 1 Effects of turbidity on the determination of ammonia nitrogen

序号	浊度/ NTU	直接检测氨氮浓度/（μg·L⁻¹）	0.45 μm过滤氨氮浓度/（μg·L⁻¹）	过滤前后相对误差/%
1	50	110.0	111.6	−1.4
2	60	107.4	107.6	−0.2
3	70	114.9	112.0	2.5
4	80	113.4	121.4	−6.6
5	90	109.4	110.2	−0.7
6	50	120.0	120.2	−0.2
7	60	118.4	122.0	−3.0
8	70	118.4	122.0	−3.0
9	80	118.2	121.6	−2.8
10	90	124.8	123.8	0.8

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表 2 实验室内氨氮检测结果对比

Tab. 2 Comparison of test results of ammonia nitrogen in laboratory

编号	海水水样	国标法检测浓度/ (μg·L⁻¹)	原位仪器法检测浓度/ (μg·L⁻¹)	相对误差/%
1	晋江海水1	100.2	104.8	4.6
2	晋江海水2	88.0	84.3	−4.1
3	晋江海水3	51.0	53.9	5.7
4	长乐海水1	62.4	64.6	3.6
5	长乐海水2	58.9	55.2	−6.3
6	长乐海水3	96.0	93.3	−2.8
7	长乐海水4	115.8	110.6	−4.5
8	长乐海水5	82.5	80.4	−2.5
9	长乐海水6	69.1	73.7	6.6

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表 3 实验室内亚硝酸盐检测结果对比

Tab. 3 Comparison of test results of nitrite in laboratory

编号	海水水样	国标法检测浓度/ (μg·L⁻¹)	原位仪器法检测浓度/ (μg·L⁻¹)	相对误差/%
1	晋江海水1	68.4	65.6	−4.1
2	晋江海水2	58.7	60.1	2.4
3	晋江海水3	70.1	67.8	−3.3
4	长乐海水1	83.6	85.1	1.7
5	长乐海水2	51.6	53.5	3.5
6	长乐海水3	43.8	46.0	4.9
7	长乐海水4	79.9	76.6	−4.1
8	长乐海水5	64.4	67.2	4.4
9	长乐海水6	88.0	84.6	−3.8

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表 4 现场水样氨氮原位监测结果对比

Tab. 4 Comparison of in-situ monitoring results of ammonia nitrogen in field water samples

监测批次（n−m）	实验室方法检测浓度/ （μg·L⁻¹）	原位仪器法检测浓度/ （μg·L⁻¹）	相对误差/%
1−1	38.1	34.0	−10.8
1−2	29.3	34.1	16.3
1−3	32.3	36.7	13.6
2−1	50.7	45.0	−11.2
2−2	54.0	47.0	−13.0
2−3	46.2	50.0	8.2
3−1	61.8	66.4	7.5
3−2	58.4	50.9	−12.9
3−3	51.0	42.4	−16.9
4−1	64.2	62.0	−3.4
4−2	66.1	57.5	−13.0
4−3	57.5	49.8	−13.4
5−1	83.5	77.0	−7.8
5−2	72.1	78.0	8.2
5−3	75.1	81.2	8.1
6−1	67.9	64.0	−5.7
6−2	64.0	55.9	−12.6
6−3	65.1	67.0	2.9
7−1	61.0	54.0	−11.5
7−2	61.3	68.2	11.3
7−3	61.1	62.1	1.7
8−1	64.5	62.5	−3.1
8−2	61.9	68.1	10.0
8−3	52.5	52.3	−0.3
9−1	58.8	69.9	18.8
9−2	58.6	61.2	4.5
9−3	63.9	68.2	6.8
10−1	53.7	45.2	−15.9
10−2	39.2	46.2	17.9
10−3	42.6	36.8	−13.6
11−1	21.3	21.8	2.4
12−1	20.8	24.2	16.4
12−3	16.4	15.8	−3.6
13−1	8.6	<10.0	/
13−2	6.0	<10.0	/
13−3	7.5	<10.0	/
14−1	69.0	57.7	−16.4
14−2	49.3	46.1	−6.4
14−3	36.1	40.1	11.2
注：n−m代表第n天第m批次，其中m为1～3时代表同一天内分别在3个时间段分别采样3次；/代表由于检测浓度低于仪器检测限，故而未进行计算。

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表 5 亚硝酸盐原位检测结果对比

Tab. 5 Comparison of in situ detection results of nitrite in field water samples

监测批次（n−m）	实验室方法检测浓度/ （μg·L⁻¹）	原位仪器法检测浓度/ （μg·L⁻¹）	相对误差/%
1−1	6.6	7.0	6.1
1−2	7.1	7.0	−1.4
1−3	7.8	7.0	−10.3
2−1	4.8	<5.0	/
2−2	5.3	5.0	−5.7
2−3	7.1	7.1	−0.7
3−1	6.1	5.0	−18.0
3−2	6.3	5.3	−16.6
3−3	4.8	<5.0	/
4−1	5.6	6.0	7.1
4−2	7.8	6.8	−13.1
4−3	7.8	6.6	−15.1
5−1	4.1	<5.0	/
5−2	5.3	6.0	13.2
5−3	3.6	<5.0	/
6−1	2.6	<5.0	/
6−2	2.6	<5.0	/
6−3	2.8	<5.0	/
7−1	4.1	<5.0	/
7−2	4.3	<5.0	/
7−3	4.6	<5.0	/
8−1	5.6	6.0	7.1
8−2	5.3	5.0	−5.7
8−3	5.8	6.4	10.7
9−1	7.8	6.8	−13.1
9−2	7.1	7.0	−1.4
9−3	6.6	6.0	−9.1
10−1	5.3	5.0	−5.7
10−2	4.8	5.0	4.2
10−3	5.6	6.4	15.0
11−1	2.1	<5.0	/
12−1	2.3	<5.0	/
12−3	2.6	<5.0	/
13−1	2.1	<5.0	/
13−2	3.1	<5.0	/
13−3	2.8	<5.0	/
14−1	0.8	<5.0	/
14−2	1.1	<5.0	/
14−3	1.6	<5.0	/
注：n−m代表第n天第m批次，其中m为1～3时代表同一天内分别在3个时间段分别采样3次；/代表由于检测浓度低于仪器检测限，故而未进行计算。

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光纤耦合微通道反应系统原位监测海水氨氮和亚硝酸盐的研究

doi: 10.12284/hyxb2023006

作者简介:
姜双城（1980-），男，山东省济宁市人，助理研究员，主要从事海洋环境监测与保护研究。 E-mail: 2001082011@163.com

通讯作者:
林琪，男，研究员，主要从事水产养殖科研工作。E-mail: xmqlin@sina.com

林旭聪，男，教授，主要从事环境分析与食品安全研究，E-mail: xulin@fzu.edu.cn

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In-situ monitoring of ammonia nitrogen and nitrite in seawater by fiber-coupled micro-channel reaction system

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光纤耦合微通道反应系统原位监测海水氨氮和亚硝酸盐的研究

doi: 10.12284/hyxb2023006

作者简介: 姜双城（1980-），男，山东省济宁市人，助理研究员，主要从事海洋环境监测与保护研究。 E-mail: 2001082011@163.com

通讯作者: 林琪，男，研究员，主要从事水产养殖科研工作。E-mail: xmqlin@sina.com 林旭聪，男，教授，主要从事环境分析与食品安全研究，E-mail: xulin@fzu.edu.cn

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In-situ monitoring of ammonia nitrogen and nitrite in seawater by fiber-coupled micro-channel reaction system

计量

出版历程

目录

作者简介:
姜双城（1980-），男，山东省济宁市人，助理研究员，主要从事海洋环境监测与保护研究。 E-mail: 2001082011@163.com

通讯作者:
林琪，男，研究员，主要从事水产养殖科研工作。E-mail: xmqlin@sina.com

林旭聪，男，教授，主要从事环境分析与食品安全研究，E-mail: xulin@fzu.edu.cn