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利用自动电位滴定仪和DP5光度电极研究了原位自动光度滴定法在全铁测量中的应用。以HNO3、HCl和HF溶液为溶剂,采用密封微波消解系统分解试样。用NaOH溶液调节溶液酸度至pH 1.5,在原消解罐中以乙二胺四乙酸二钠盐(磺基水杨酸为指示剂)滴定铁。主要对滴定温度、试样的分解条件以及杂质对测定的干扰情况进行了研究。研究结果表明,称样量为0.05 g,溶剂为60%王水10 mL加1 mL HF(1+99),温度为210℃,消解时间为20 min时溶样效果最好,50～60℃条件下,pH 1.5时进行滴定,结果准确可靠,能有效消除干扰。
The use of automatic potentiometric titration and DP5 photodetector has been investigated for the application of in situ photometric titration in full iron measurement. With HNO3, HCl and HF solution as a solvent, sealed microwave digestion system decomposition samples. The solution acidity was adjusted to pH 1.5 with NaOH solution and iron was titrated with disodium ethylenediaminetetraacetate (sulfosalicylic acid as an indicator) in the original digestion tank. Mainly on the titration temperature, the sample decomposition conditions and impurities on the determination of the interference situation were studied. The results showed that the sample was weighed at 0.05 g, the solvent was 60% aqua regia 10 mL plus 1 mL HF (1 + 99), the temperature was 210 ℃ and the digestion time was 20 min, Conditions, pH 1.5 when titration, the result is accurate and reliable, can effectively eliminate interference.