Nickel speciation of spent electroless nickel plating effluent along the typical sequential treatment scheme

The electroless nickel (EN) industry has suffered from the reduction in Ni concentration to lower than 0.1 mg/L. Hence, Ni speciation along a typical sequential treatment scheme has important implications to optimize the design of advanced treatment. For the first time, we revealed the Ni speciation in segmented EN outfall effluents by virtue of multiple analytical methods. After ensuring all the Ni-bearing complexes were completely dissolved by size-fractioned ultrafiltration trials, customized mass spectra analysis was conducted. In a series of ICP-MS assays, the potential polyatomic interfering species was primarily excluded. The chromatography hyphenated IC-ICP-MS and SEC-ICP-MS results demonstrated that the dominant Ni species in the EN effluents was similar to EDTA-Ni but with a smaller size. The LC-MS experiment further distinguished several typical Ni-bearing complexes. Although Ni concentration declined continuously along the treatment scheme, the number of detected Ni-bearing complexes gradually increased but with lower molecular weights. Most of the detected mononuclear complexes had higher indexes of hydrogen deficiency (IHD) than EDTA-Ni, whereas it was believed that the similar stereo ring shape was widespread in the EN effluent. Considering the efficient Ni decrease after the Fenton unit, further post-treatment approaches featuring higher active radical yields were suggested.