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

Abstract

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

CLC Number:

TQ443.1

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.

Figures/Tables 11

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References 25

[1]	SOUMARE A， SARR D， DIÉDHIOU A G.Potassium sources，microorganisms and plant nutrition：Challenges and future research directions［J］.Pedosphere，2023，33（1）：105-115.
[2]	伊跃军，张秀峰，张利珍，等.中国钾盐资源开发利用现状及建议［J］.无机盐工业，2024，56（10）：12-19.
	YI Yuejun， ZHANG Xiufeng， ZHANG Lizhen，et al.Present situation and suggestions on exploitation and utilization of potassium salt resources in China［J］.Inorganic Chemicals Industry，2024，56（10）：12-19.
[3]	AI Zhong， LI Shoujiang， ZHAO Yunliang，et al.Atomic insights into flotation separation of KCl and NaCl from a new viewpoint of hydration layer：A molecular dynamic study［J］.Colloids and Surfaces A：Physicochemical and Engineering Aspects，2020，602：125071.
[4]	SUN Kangkang， NGUYEN C V， NGUYEN N N，et al.Flotation surface chemistry of water-soluble salt minerals：From experimental results to new perspectives［J］.Advances in Colloid and Interface Science，2022，309：102775.
[5]	HUANG Zhiqiang， CHENG Chen， ZHONG Hong，et al.Flotation of sylvite from potash ore by using the Gemini surfactant as a novel flotation collector［J］.Minerals Engineering，2019，132：22-26.
[6]	靳莹皓，王思远，于雪峰，等.氯化钾浮选阴阳离子混合型捕收剂的复配与应用［J］.无机盐工业，2023，55（10）：93-99.
	JIN Yinghao， WANG Siyuan， YU Xuefeng，et al.Recombination and application on mixed amine collector（cationic/anionic） for KCl flotation［J］.Inorganic Chemicals Industry，2023，55（10）：93-99.
[7]	WANG Linjian， XU Yanxia， CHEN Hang，et al.New insights into octadecylamine-monoacid selective adsorption on KCl/NaCl surface：Experimental and molecular dynamic simulation［J］.Applied Surface Science，2021，554：149613.
[8]	SUN Kangkang， NGUYEN N N， NGUYEN A V.Unique selective activating effect of lead ions on the flotation of NaCl crystals against KCl crystals with fatty acid collector colloids［J］.Minerals Engineering，2024，216：108908.
[9]	SUN Kangkang， NGUYEN C V， NGUYEN N N，et al.Crucial roles of ion-specific effects in the flotation of water-soluble KCl and NaCl crystals with fatty acid salts［J］.Journal of Colloid and Interface Science，2023，636：413-424.
[10]	LU Miao， MA Liang， YE Xiushen，et al.Novel method for rapid determination of octadecylamine using UV spectrophotometry［J］.Journal of Applied Spectroscopy，2023，90（5）：1101-1106.
[11]	HUANG Xiaofen， ZHANG Qin， LI Xianbo，et al.An HPLC method for the determination of amines in flotation pulp based on derivatization［J］.Chromatographia，2021，84（5）：463-471.
[12]	YANG Keli， ZHANG Yaoling， DONG Yaping，et al.Characterization of dissolved organic matter in solar ponds by elemental analysis，infrared spectroscopy，nuclear magnetic resonance and pyrolysis-GC-MS［J］.International Journal of Environmental Research and Public Health，2022，19（15）：9067.
[13]	PAULO VIEIRA C， PEREIRA DA COSTA M， SILVA V L M，et al.Development and validation of RP-HPLC-DAD method for biogenic amines determination in probiotic yogurts［J］.Arabian Journal of Chemistry，2020，13（1）：1582-1597.
[14]	BOSCO ACKERMAN B， MARTÍN S， ESPINOSA M，et al.Development and validation of a liquid chromatography-mass spectrometry method for quantification of octadecylamine in the secondary circuit of a nuclear power plant in the presence of other amines［J］.Separation Science Plus，2024，7（8）：e202400099.
[15]	宋忠梅，路淼，张慧芳，等.萃取分光光度法测定氯化钾体系中的十八胺［J］.光谱学与光谱分析，2024，44（8）：2240-2249.
	SONG Zhongmei， LU Miao， ZHANG Huifang，et al.Extraction spectrophotometric determination of octadecylamine in potassium chloride［J］.Spectroscopy and Spectral Analysis，2024，44（8）：2240-2249.
[16]	JAHANGARD S， JAHANGARD S， SARAJI M.Combination of headspace single-drop microextraction with smartphone-based on-drop colorimetric detection for determination of ammonia and total nitrogen in environmental and food samples［J］.Microchemical Journal，2024，199：109965.
[17]	DU Peixuan， MA Yubo， WANG Ning，et al.A new method for the determination of carbohydrate content in starch samples by alkaline potassium persulfate digestion［J］.Journal of Food Composition and Analysis，2024，135：106645.
[18]	LIU Dongmei， XIONG Yu， ZENG Hui，et al.Deep UV-LED induced nitrate-to-nitrite conversion for total dissolved nitrogen determination in water samples through persulfate digestion and capillary electrophoresis［J］.Analytica Chimica Acta，2023，1278：341743.
[19]	SUN Xiaofang， CHEN Huixuan， LIU Zhengyu，et al.Investigations on ozone-based and UV/US-assisted synergistic digestion methods for the determination of total dissolved nitrogen in wa- ters［J］.Processes，2020，8（4）：490.
[20]	LIU Xiaohui， LIU Ying， LU Shaoyong，et al.Degradation difference of ofloxacin and levofloxacin by UV/H₂O₂ and UV/PS（persulfate）：Efficiency，factors and mechanism［J］.Chemical Engineering Journal，2020，385：123987.
[21]	GENTLE B S， ELLIS P S， GRACE M R，et al.Flow analysis methods for the direct ultra-violet spectrophotometric measurement of nitrate and total nitrogen in freshwaters［J］.Analytica Chimica Acta，2011，704（1/2）：116-122.
[22]	刘振超，李志雄，陆迁树，等.碱性过硫酸钾-紫外分光光度法测定水质总氮方法的改进［J］.岩矿测试，2024，43（1）：114-123.
	LIU Zhenchao， LI Zhixiong， LU Qianshu，et al.Improvement of the method for determining total nitrogen in water quality using alkaline potassium persulfate ultraviolet spectrophotometry［J］.Rock and Mineral Analysis，2024，43（1）：114-123.
[23]	TONG Angxin， TANG Xiaojun， ZHANG Feng，et al.Study on the shift of ultraviolet spectra in aqueous solution with variations of the solution concentration［J］.Spectrochimica Acta Part A：Molecular and Biomolecular Spectroscopy，2020，234：118259.
[24]	张慧芳，刘海宁，郭敏，等.紫外分光光度法快速测定溶液中微量碘离子［J］.分析科学学报，2011，27（2）：238-240.
	ZHANG Huifang， LIU Haining， GUO Min，et al.Rapid determination of trace iodide in solutions by UV spectrophotometry［J］.Journal of Analytical Science，2011，27（2）：238-240.
[25]	中华人民共和国生态环境部.环境监测分析方法标准制订技术导则：HJ 168—2020［S］.北京：中国环境科学出版社， 2020.

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

National Inorganic Salts Information Center

Inorganic Acid-Base-Salt Committee of CIESC

Optimization of determination for octadecylamine content in brine based on potassium persulfate digestion method

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