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本文提出了石墨中微量氯的分光光度测定法,即将石墨样品在氧气流量为400—450毫升/分,温度已为830—880℃的条件下燃烧,氯化物经高温水解后被10%H_2O_2吸收,然后于H_2O_2吸收液中加入NaOH,蒸发除去H_2O_2之后,以Hg(SCN)_2和Fe(NO_3)_3比色测定氯。本法简便,不需分离,影响因素少。对于1克试作,方法的测定下限为1×10~(-4)%。含量为1.9×10~(-4)%时,6次测定结果的相对标准偏差为±14%。加入试验的回收率在85%以上。
In this paper, a spectrophotometric method for the determination of trace chlorine in graphite is proposed. The graphite sample is burned under the conditions of an oxygen flow rate of 400-450 ml / min and a temperature of 830-880 ° C. The chloride is absorbed by 10% H 2 O 2 after being hydrolyzed at high temperature Then, NaOH was added into the H 2 O 2 absorbing solution, and H 2 (SCN) 2 and Fe (NO 3) 3 colorimetric determination of chlorine was carried out after the H 2 O 2 was removed by evaporation. This law is simple, without separation, less influencing factors. For a 1 gram trial, the method of determination of the lower limit of 1 × 10 ~ (-4)%. When the content was 1.9 × 10 ~ (-4)%, the relative standard deviation of the 6 determinations was ± 14%. The test recovery rate of 85% or more.