XU Chengyi,WANG Wenchang,CHEN Zhidong*.Determination of Chloride Ion in Acidic Copper Plating Bath by Pulse Voltammetry[J].Plating & Finishing,2020,(1):41-46.[doi:10.3969/j.issn.1001-3849.2020.01.009]
脉冲伏安法测定酸性镀铜液中氯离子
- Title:
- Determination of Chloride Ion in Acidic Copper Plating Bath by Pulse Voltammetry
- 文献标志码:
- A
- 摘要:
- 本文以三电极体系为基础，采用脉冲伏安法测定酸性镀铜液中Cl-的含量，考察了富集电位，富集时间，电解液中CuSO4·5H2O浓度、H2SO4浓度和Cl-浓度对溶出峰电流密度的影响。实验结果表明，在酸性光亮镀铜液中，富集电位为0.30 V、富集时间为30 s时，Cl-的脉冲伏安法曲线峰形好，峰电流密度高，检测灵敏度高，Cl-检测限线性范围为0.1~20 mg/L，线性方程的方差为R2=0.9965，检测限为0.047 mg/L。本文所采用的脉冲伏安法测定酸性光亮镀铜液中Cl-含量灵敏度高、稳定性好并且抗干扰性强。利用此方法在实际生产过程中无需样品前处理即可对Cl-含量进行即时测定。
- Abstract:
- The work aims to provide a no-pretreatment method for fast and accurate determination of chloride in copper plating baths. Based on the three-electrode system, the content of Cl－ in acid copper plating solution was determined by the pulse voltammetry. The effects of enrichment potential, enrichment time, copper sulfate concentration, sulfuric acid concentration and chloride ion concentration on the pulse voltammetry curve were investigated. The experimental results indicated that the peak of Cl－ in the pulse voltammetry curve exhibited a good shape when the enrichment potential was 0.30 V and the enrichment time was 30 s. Moreover, the current intensity showed a good correlation to the concentration of Cl－ in the range of 0.1-20 mg/L and the variance of the linear equation is R2=0.9965,with a detection limit of 0.047 mg/L. The pulse voltammetry method developed in this research for detecting Cl－ content in acid bright copper plating solution possesses a high sensitivity, good stability and strong anti-interference. With this method, the Cl－ content can be measured immediately in the actual production process.
参考文献/References:
[1] Reid J D, David A P. Impedance behavior of a sulfuric acid‐cupric sulfate/copper cathode interface[J]. Journal of the Electrochemical Society, 1987, 134(6): 1389-1394.
[2] Farmer J C. Underpotential deposition of copper on gold and the effects of thiourea studied by AC impedance[J]. Journal of the Electrochemical Society, 1985, 132(11): 2640-2648.
[3] 刘烈炜, 吴曲勇, 卢波兰, 等. 氯离子对酸性镀铜电沉积的影响[J]. 电镀与环保, 2004, 24(5): 7-9.
[4] Mirkova L. Anodic behaviour of copper during electrorefining using a rotating ring-disc electrode[J]. Journal of Applied Electrochemistry, 1994, 24(5): 420-425.
[5] 李立清, 安文娟, 王义. MPS 和氯离子在电镀铜盲孔填充工艺中的作用机理[J]. 表面技术, 2018, 47(5): 122-129.
[6] 步华, 杭东良. 氯离子在酸性光亮铜镀液中的作用及其浓度控制[J]. 材料保护, 2003, 36(11): 72-72.
[7] 黄业, 谢静静, 唐春保. 酸性光亮镀铜溶液降低氯离子浓度的处理方法[J]. 广东化工, 2017, 44(7): 149-149.
[8] 张雨青. 电位法测定循环水中的氯离子[J]. 光谱实验室, 2012, 29(3): 1659-1662.
[9] 佟琦, 高丽华. 莫尔法与自动电位滴定法测定水中氯离子含量的比较[J]. 工业水处理, 2008, 28(11): 69-71.
[10] 周游, 叶蔓莉. 离子色谱法测定水中氟和氯[J]. 广东化工, 2018, 45(18): 176,167.
[11] Guarda A, Aramendía M, Andrés I, et al. Determination of chlorine via the CaCl molecule by high-resolution continuum source graphite furnace molecular absorption spectrometry and direct solid sample analysis[J]. Talanta, 2017, 162: 354-361.
[12] Bujes-Garrido J, Arcos-Martínez M J. Development of a wearable electrochemical sensor for voltammetric determination of chloride ions[J]. Sensors and Actuators B: Chemical, 2017, 240: 224-228.
[13] Chen X, Chu B, Xi H, et al. Determination of chlorine ions in raw milk by pulsed amperometric detection in a flow injection system[J]. Journal of Dairy Science, 2018, 101(11): 9647-9658.
[14] 李成虹. 镀铜溶液中硫酸铜, 铁离子及氯离子测定方法的改进[J]. 电镀与精饰, 2005, 27(1): 41-42.
[15] 胡荣宗, 吕建平. 离子色谱法测量酸性镀铜液中微量的氯离子[J]. 厦门大学学报: 自然科学版, 2000, 39(6): 798-802.
[16] Sanz L, Palma J, García-Quismondo E, et al. The effect of chloride ion complexation on reversibility and redox potential of the Cu (II)/Cu (I) couple for use in redox flow batteries[J]. Journal of Power Sources, 2013, 224: 278-284.
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备注/Memo
收稿日期： 2019-08-11；修回日期： 2019-09-19
通信作者： 陈智栋， email： zdchen@cczu.edu.cn