本文介绍了核纯石墨中微量硫的分光光度测定。试样以通氧气燃烧法处理,燃烧温度为900—1300℃,氧气流量为100毫升/分钟,燃烧时间为20分钟。逸出气体用3%过氧化氢溶液吸收,这时硫形成硫酸盐。以碘氢酸、甲酸、次亚磷酸的混合还原液将硫还原成硫化物,用次甲基蓝比色法进行硫的测定。试样分析结果的重现性较好,加入标准回收率在90%以上,本方法的测定下限为5×10~(-4)%,相对标准偏差为12%。 This article describes the determination of trace sulfur in nuclear pure graphite spectrophotometry. The sample was treated with oxygen combustion at a temperature of 900-1300 ° C with an oxygen flow rate of 100 ml / min and a burn time of 20 minutes. The escaping gas is absorbed by 3% hydrogen peroxide solution, when sulfur forms sulphate. Sulfur was reduced to sulfide by a mixed reduction solution of iodohydric acid, formic acid and hypophosphorous acid, and sulfur was determined by methine blue colorimetry. The reproducibility of the sample analysis was good. The standard recovery was above 90%. The lower limit of this method was 5 × 10 ~ (-4)% and the relative standard deviation was 12%.