摘要
以四苯基卟啉(TPP)和硫酸为原料,微波法合成了四对磺酸苯基卟啉(TPPS4),产率高达94.7%,通过紫外可见吸收光谱(UV)、红外光谱(IR)、核磁共振(1HNMR)验证了其结构。在pH 6.5的HAc-NaAc的缓冲溶液中和Hg2+存在下,于沸水浴中TPPS4和铜、铬、镍反应15 min可实现柱前衍生。以四乙基溴化铵(TEABr)作离子对试剂,在C18柱上采用甲醇-水(体积比为40∶60)体系作流动相,在420 nm处检测,实现了高效液相色谱法分离和测定铜、铬、镍。络合物和反应试剂在15 min内出峰完毕。铜、铬、镍的检测限分别为0.01μg/L,0.50μg/L,0.10μg/L。此法可用于集中处理后的电镀废液中铜、铬、镍的测定。
Tetra-（p-sulfonato phenyl） porphyrin （TPPS4） was synthesized by microwave irradiation from tetraphenyl porphyrin （TPP） and sulfuric acid, whose yield was 94.7%. The structure of the product was validated by UV, IR and ^1HNMR. In HAc-NaAc buffer solution at pH 6.5, the pre-column derivation could be achieved by the reaction of TPPS4 with copper, chromium and nickel for 15 min in the presence of Hg^2＋. With tetraethylammonium bromide （TEABr） as ion-pair reagent and methanol-water （40 60 of volume ratio） as mobile phase in C18 column, the separation and determination of copper, chromium and nickel by high-performance liquid chromatography were realized at 420 nm. The peaking of complexes and reagents were finished within 15 min. The detection limits for copper, chromium and nickel were 0.01 μg/L, 0.50 μg/L and 0. 10 μ g/L, respectively. This method can be applied to the determination of these three metal ions in electroplating wastewater after treatment.
出处
《冶金分析》
CAS
CSCD
北大核心
2009年第5期16-19,共4页
Metallurgical Analysis
基金
湖南省环境科学学科建设项目(2006180)
关键词
四对磺酸苯基卟啉
微波合成
高效液相色谱
铜
铬
镍
tetra-（p-sulfonato phenyl） porphyrin
microwave synthesis
high-performance liquid chromagraphy
copper
chromium
nickel
