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Determination of Hexafluorophosphate in Waste Water Using Ion Chromatography
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摘要: 建立了离子色谱-抑制电导测定废水中六氟磷酸根的分析方法. 采用IonPac AG23+IonPac AS23阴离子交换柱分离，流速1 mL/min，KOH等度淋洗，抑制型电导检测. 采集的样品经过0.22 μm滤膜、C18柱、On-Guard Na柱处理后进样分析. 以信噪比S/N=3计算检出限，六氟磷酸根的检出限为0.02 mg/L. 方法线性相关系数r为0.999 7，试验结果峰面积的相对标准偏差为1.85%，实际样品的加标回收率在94.0%~103.3%之间. 方法简便、结果准确，可以用于实际样品检测.Abstract: An analytical method was developed for the determination of hexafluorophosphate in waste water using ion exclusion chromatography with suppressed conductivity. The separation was performed on an IonPac AG23+IonPac AS23 separate ion exchange column with a flow rate of 1 mL/min, KOH isocratic drenching and inhibited conductivity detection. The collected samples were processed on a 0.22 μm filter membrane, a C18 column, an On-Guard Na column, and then injected into the sample for analysis. The detection limit (S/N=3) of hexafluorophosphate was 0.02 mg/L. The linear coefficient was 0.999 7. The relative standard deviation of the peak area was 1.85%, and the spiked recoveries of waste water ranged from 94.0% to 103.3%. The method is simple and accurate, and can be used for the detection of actual samples.
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Key words:
- ion chromatography /
- suppressor conductivity /
- waste water /
- hexafluorophosphate
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表 1 1号样品的回收率测定结果（n=6）
Table 1. Recoveries of sample 1 (n=6)
样品原质量
分数/（mg/L）加入标样质量
分数/（mg/L）加标后测定质量
分数/（mg/L）回收
率/%n.d. 0.06 0.062 103.3 0.10 0.094 94.0 0.15 0.147 98.0 0.20 0.202 101.0 
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[1] 李玉芳, 伍小明. 我国六氟磷酸锂合成技术研究进展[J]. 精细与专用化学品,2022,30(5):8-10, 18LI Yufang, WU Xiaoming. Synthesis technology progress of lithium hexafluorophosphate in China[J]. Fine and Specialty Chemicals,2022,30 (5):8-10, 18. [2] 刘丹丹, 吴清山. 锂离子电池用电解质六氟磷酸锂的研究现状[J]. 化工管理,2021(16):74-75, 98LIU Dandan, WU Qingshan. The status analysis of lithium hexafluorophosphate liquid electrolytes in lithium ion batteries[J]. Chemical Enterprise Management,2021 (16):74-75, 98. [3] 李佳, 田雷雷, 赵封林, 等. 六氟磷酸锂产业化关键技术[J]. 应用化工,2011,40(3):524-527, 534LI Jia, TIAN Leilei, ZHAO Fenglin, et al. Key technology on lithium hexafluophosphate industrialization[J]. Applied Chemical Industry,2011,40 (3):524-527, 534. [4] 杨灵, 于泓, 李偲文. 六氟磷酸根的离子色谱-直接电导检测法分析[J]. 分析测试学报,2009,28(9):1077-1080 doi: 10.3969/j.issn.1004-4957.2009.09.020YANG Ling, YU Hong, LI Siwen. Determination of hexafluorophosphate by ion chromatography with direct conductivity detection[J]. Journal of Instrumental Analysis,2009,28 (9):1077-1080. doi: 10.3969/j.issn.1004-4957.2009.09.020 [5] Zhu Z Y, Xu J G, Zhong N F, et al. Fast determination of hexafluorophosphate, fluorid, chloride, nitrate and sulfate inorganic anions by ion chromatography with valve switching[J]. Chinese Journal of Analytical Chemistry (Chinese Version),2012,39 (11):1738-1742. doi: 10.3724/SP.J.1096.2011.01738 [6] 刘玉珍, 于泓, 张仁庆. 反相离子对色谱-直接电导检测法分析六氟磷酸根离子液体阴离子[J]. 分析测试学报,2012,31(5):530-534 doi: 10.3969/j.issn.1004-4957.2012.05.004LIU Yuzhen, YU Hong, ZHANG Renqing. Determination of hexafluorophosphate ionic liquid anion by reversed-phase ion-pair chromatography coupled with direct conductivity detection[J]. Journal of Instrumental Analysis,2012,31 (5):530-534. doi: 10.3969/j.issn.1004-4957.2012.05.004 [7] 堀尾博英. 一种基于离子色谱技术六氟磷酸锂纯度的测定方法: CN113899822A[P]. 2022-01-07. [8] 钟乃飞, 曾雪灵, 叶明立, 等. 离子色谱法测定碘鎓盐中的六氟磷酸根[J]. 中国无机分析化学,2012,2(S1):51-52. [9] 宋作忠, 蒋玉湘, 马培华. 氯化四苯砷用于电流滴定法测定六氟磷酸根离子[J]. 盐湖研究,1999,7(3):30-35 doi: 10.3969/j.issn.1008-858X.1999.03.005SONG Zuozhong, JIANG Yuxiang, MA Peihua. The application of tetraphenylarsonium chloride in the determination of hexafluorophsphate ion by amperometric titration[J]. Journal of Salt Lake Research,1999,7 (3):30-35. doi: 10.3969/j.issn.1008-858X.1999.03.005 [10] Gidi L, Honores J, Ibarra J, et al. Electrodetermination of Gallic acid using multi-walled carbon nanotube paste electrodes and N-octylpyridinium hexafluorophosphate[J]. Electroanalysis,2022,34 (7):1163-1173. doi: 10.1002/elan.202100476 [11] 王海, 曾有胜, 范伟贞, 等. 一种紫外分光光度计测定锂离子电池电解液中六氟磷酸锂含量的方法: CN106248609B[P]. 2019-03-19. [12] Fu L, Xie H L, Huang J H, et al. Determination of metal impurity elements in lithium hexafluorophosphate using inductively coupled plasma tandem mass spectrometry based on reaction gas mixtures[J]. Spectrochimica Acta Part B:Atomic Spectroscopy,2021,181 :106217. doi: 10.1016/j.sab.2021.106217 [13] Kohlmeyer C, Schäfer A, Huy P H, et al. Formamide-catalyzed nucleophilic substitutions: mechanistic insight and rationalization of catalytic activity[J]. ACS Catalysis,2020,10 (19):11567-11577. doi: 10.1021/acscatal.0c03348 [14] 肖跃龙, 戴璇, 张翼, 等. 红外光谱法对六氟磷酸锂的快速定量分析[J]. 分析科学学报,2012,28(3):357-360XIAO Yuelong, DAI Xuan, ZHANG Yi, et al. Rapid quantitative analysis of lithium hexafluorophosphate by infrared spectroscopy[J]. Journal of Analytical Science,2012,28 (3):357-360. [15] 管利娜, 闫晓宾, 吕秀夯, 等. 一种使用ICP测试锂离子功能电解液中六氟磷酸锂浓度含量的方法: CN111474165A[P]. 2020-07-31. [16] Fliri L, Partl G, Winkler D, et al. Ionic and neutral fluorosurfactants containing ferrocene moieties as chromophoric constituents[J]. Journal of Fluorine Chemistry,2021,241 :109674. doi: 10.1016/j.jfluchem.2020.109674 -
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