基于过硫酸钾消解法的卤水中十八胺含量测定方法优化

doi:10.19964/j.issn.1006-4990.2024-0506

摘要/Abstract

摘要：

基于盐湖生产需求，研究优化检测卤水中十八胺（ODA）含量的方法。在碱性过硫酸钾消解紫外分光光度法的基础上，通过紫外灯照射和H₂O₂耦合（UV/H₂O₂）预处理，成功预消解ODA，有助于后续碱性过硫酸钾的充分氧化，提升检测的准确性和稳定性。优化后的检测条件为碱性过硫酸钾用量为5 mL、消解时间为10~20 min、消解温度为123~126 ℃、pH为5~7、MgCl₂质量浓度<2 g/L，无需额外掩蔽剂。测试方法适用于ODA质量浓度<10 mg/L的卤水溶液，其具有2.9%~4.2%的精密度和-1.5%~1.4%的准确度，加标回收率为98.18%~101.98%。研究有效解决ODA化学稳定性和卤水高盐特性带来的检测挑战，为盐湖生产中ODA浓度的准确检测和监控提供可靠的分析手段，有助于生产管理、工艺优化和产品质量提升。

关键词: 卤水, 十八胺, 碱性过硫酸钾, 紫外分光光度法, 消解

Abstract:

Based on the production needs of salt lake operations，a method for determining octadecylamine（ODA） content in brine was optimized.Building upon the alkaline potassium persulfate digestion-UV spectrophotometry method，a UV/H₂O₂ coupled pretreatment was introduced to successfully pre-digest ODA，facilitating subsequent complete oxidation by alkaline potassium persulfate and thereby improving the accuracy and stability of detection.The optimized parameters included that 5 mL of alkaline potassium persulfate，digestion time of 10~20 minutes，temperature maintained between 123~126 ℃，pH controlled within 5~7，MgCl₂ concentration below 2 g/L，with no additional masking agents required.The method was applicable to brine samples with ODA concentrations below 10 mg/L，demonstrating a precision of 2.9%~4.2%，an accuracy ranging from-1.5%~1.4%，and spike recovery rates between 98.18%~101.98%.This research effectively overcame the challenges posed by the chemical stability of ODA and the high-salinity matrix of brine，providing a reliable analytical approach for accurate detection and monitoring of ODA levels in salt lake production.It supported enhanced production management，process optimization，and product quality improvement.

Key words: brine, octadecylamine, alkaline persulfate, UV spectrophotometry, digestion

中图分类号:

TQ443.1

宋薇, 刘涛涛, 唐海英, 李兴海, 于雪峰, 张国玉, 赵宁, 王昌松. 基于过硫酸钾消解法的卤水中十八胺含量测定方法优化[J]. 无机盐工业, 2025, 57(11): 108-114.

SONG Wei, LIU Taotao, TANG Haiying, LI Xinghai, YU Xuefeng, ZHANG Guoyu, ZHAO Ning, WANG Changsong. Optimization of determination for octadecylamine content in brine based on potassium persulfate digestion method[J]. Inorganic Chemicals Industry, 2025, 57(11): 108-114.

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样品编号	未加标样品浓度/（mg·L^-1）	加标量/ （mg·L^-1）	加标后样品浓度/（mg·L^-1）	加标后吸光度	加标回收率/%
1	4.594	4.00	8.549	0.909	98.88
2	4.462	4.00	8.541	0.908	101.98
3	4.575	4.00	8.637	0.918	101.55
4	4.744	4.00	8.671	0.922	98.18
5	4.565	4.00	8.581	0.912	100.40
6	4.678	4.00	8.643	0.919	99.13

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