新试剂5-(2'-氨基-4'-羟基苯偶氮)邻苯二甲酰肼(AHPP)的合成及其光度法测定钴  

Synthesis of 5-(2＇-Amino-4＇-hydroxyphenylazo)-2,3-dihydro-1,4-phthalazinedione and Its Use in Photometric Determination of Cobalt

作　　者：马会民[1] 黄月仙[1] 梁树权[1] 

机构地区：[1]中国科学院化学研究所,北京100080

出　　处：《化学学报》1994年第12期1199-1202,共4页Acta Chimica Sinica

基　　金：国家自然科学基金;所长基金资助的项目.

摘　　要：本文报道新试剂5-(2′-氨基-4′-羟基苯偶氮)邻苯二甲酰肼的合成,并研究了该试剂用于光度法测定钴的反应条件.钴与试剂在 pH7.7～9.0(0.06mol·L^(-1)Na_2B_4O_7-HCl缓冲介质)时形成稳定配合物,最大吸收位于542nm处,摩尔吸光率为5.7×10~3L·mol^(-1)·cm^(-1),配合物的组成为 1:2的 Co:AHPP,钴浓度在0～1.02×10^(-4)mol·L^(-1)范围内符合Beer′s law.试验了共存离子的影响,发现除Cu(Ⅱ),Ni(Ⅱ)略有干扰(可掩蔽)外,其它常见离子均允许大量存在,该法已直接用于不锈钢和维生素B_(12)中钴的测定.A new reagent, 5-(2'-amino-4'-hydroxyphenylazo)-2,3-dihydro-l,4-phthalazinedione (AHPP), has been synthesized by diazotizing luminol and then coupling the diazotized product with m-aminophenol in weak acidic media (pH5~ 7). The structure of AHPP has been confirmed with IR, elemental analysis and other physical methods. AHPP and its Co-complex exhibit max. absorption at 456 and 542nm respectively in pH7.7 buffered solution (Na2B4O7-HC1). Various parameters such as optimum acidity, amount of AHPP, and effects of surfactants and diverse ions, for cobalt photometric determination are studied. In the complex, the ratio of Co to AHPP is found to be 1:2 with both Job's continuous variation and molar ratio methods. The proposed method has been applied to the determinations of cobalt in stainless steel and vitamin B12 with satisfactory results.

关 键 词：邻苯二甲酰肼 合成 光度法 钴 

分 类 号：O614.812[理学—无机化学]