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实验定量研究了存在Ca2+、Mg2+和Fe3+时,应用高碘酸钾分光光度法测定Mn2+的准确性,旨在探讨应用该方法准确测定电解锰渣中Mn(Ⅱ)的可行性。结果发现Ca2+浓度超过320 mg/L时,测定过程中会产生大量絮状乳白色沉淀,对Mn2+的测定结果产生干扰。经过16 h的自然沉降,干扰被彻底消除。Mg2+在浓度为0~192 mg/L范围内对Mn2+浓度的测定不产生干扰。同时,Fe3+的存在对Mn2+浓度的测定产生灵敏的干扰,使用掩蔽剂氟化钾可以减少Fe3+的干扰,但却不能彻底消除Fe3+的干扰。提出了在电解锰行业中,没有彻底地消除Ca(Ⅱ)或Fe(Ⅲ)的干扰因素前,需要更为精确地测定Mn(Ⅱ)的浓度,不建议使用高碘酸钾分光光度法。
The experiment quantitatively studied the accuracy of potassium periodate spectrophotometric determination of Mn2 + in the presence of Ca2 +, Mg2 + and Fe3 + to explore the feasibility of using this method to accurately determine Mn (Ⅱ) in electrolytic manganese residue. The results showed that when the Ca2 + concentration exceeds 320 mg / L, a large amount of flocculent milky white precipitate will be produced during the measurement, which will interfere with the determination of Mn2 +. After 16 hours of natural settlement, interference was completely eliminated. The concentration of Mg2 + in the range of 0 ~ 192 mg / L did not interfere with the determination of Mn2 + concentration. At the same time, the presence of Fe3 + sensitive to the determination of Mn2 concentration, the use of masking agent potassium fluoride can reduce the interference of Fe3 +, but it can not completely eliminate the interference of Fe3 +. It is proposed that in the electrolytic manganese industry, the concentration of Mn (II) needs to be measured more accurately before the perturbation factor of Ca (II) or Fe (III) is completely eliminated. Potassium periodate spectrophotometry is not recommended.