摘要
电解锰试样用盐酸和过氧化氢溶解,以砷作载体,氯化铜为催化剂,加次磷酸钙还原硒,用苯萃取沉淀与锰和杂质分离。加溴酸钾将砷硒沉淀溶于水相中,除去过量氧化剂后,3·3′-二氨基联苯胺溶液与二氧化硒生成有色配合物,用甲笨萃取,于分光光度计420 nm波长处测量其吸光度。本法准确稳定,测定范围为0.005%—0.05%。
A new sensitive method for spectrophotometic determination of trace of Se in electrolytic manganese with 3·3′-diaminobenzidine has been developed. The sample is dissolved with hydrocloric acid and hydrogen peroxide solution. Using copper chloride as a catalyst, calcium hypopheosphite as a reducer, Se is coprecipited with arsenous acid as a carrier in the form of selenious acid. Then potassium bromate as an oxide the selenious acid is extracted with benzene, and hydrochloride acid solution extracts selenic chloride back to aqueous solution, as a result Se react with 3·3-diaminobenzidine to form yellow complex. Being extracted by toluene, Se content in the organic phase is determined by photometric method at 420 nm wave length. The method has been used in the determination of trace Se in the range of 0.005 % to 0.05 %.
出处
《稀有金属材料与工程》
SCIE
EI
CAS
CSCD
1992年第5期59-63,共5页
Rare Metal Materials and Engineering
关键词
电解锰
硒
分光光度法
测定
Spectrophotometic Selenium Electrdytic manganese 3·3' -Diaminobenzidine