冶金分析
冶金分析
야금분석
METALLURGICAL ANALYSIS
2010年
1期
61-64
,共4页
镍(Ⅱ)%4-硝基-4'-氟苯基重氮氨基偶氮苯%双波长分光光度法
鎳(Ⅱ)%4-硝基-4'-氟苯基重氮氨基偶氮苯%雙波長分光光度法
얼(Ⅱ)%4-초기-4'-불분기중담안기우담분%쌍파장분광광도법
nickel(Ⅱ)%4-nitro-4'-fluorophenyl diazo-amino-azobenzene%dual-wavelength spectrophotometry
报道了新含氟显色剂4-硝基-4'-氟苯基重氮氨基偶氮苯与镍(Ⅱ)的显色反应.试验表明,在pH 8.6 Na_2B_4O_7-HCl缓冲溶液、Tween-85存在下,试剂与镍(Ⅱ)形成4:1的稳定紫红色络合物.最大吸收正峰为504 nm,负峰为424 nm;且在25 mL显色液中镍(Ⅱ)的量在0~4 μg范围内符合比尔定律.在两最大正负吸收波长处分别进行单波长分光光度法测定,表观摩尔吸光系数分别为1.13×10~5 ,1.06×10~5 L·mol~(-1)·cm~(-1).再以424 nm为参比波长、504 nm为测量波长进行吸光度叠加的双波长光度法测定,表观摩尔吸光系数为2.17×10~5 L·mol~(-1)·cm~(-1).加入混合掩蔽剂NaF-硫脲,可消除常见共存离子的干扰.本法可用于测定多元素混合标准溶液和不锈钢中的镍(Ⅱ),回收率为96%~98%,混合标准溶液的测定值与认定值相一致.
報道瞭新含氟顯色劑4-硝基-4'-氟苯基重氮氨基偶氮苯與鎳(Ⅱ)的顯色反應.試驗錶明,在pH 8.6 Na_2B_4O_7-HCl緩遲溶液、Tween-85存在下,試劑與鎳(Ⅱ)形成4:1的穩定紫紅色絡閤物.最大吸收正峰為504 nm,負峰為424 nm;且在25 mL顯色液中鎳(Ⅱ)的量在0~4 μg範圍內符閤比爾定律.在兩最大正負吸收波長處分彆進行單波長分光光度法測定,錶觀摩爾吸光繫數分彆為1.13×10~5 ,1.06×10~5 L·mol~(-1)·cm~(-1).再以424 nm為參比波長、504 nm為測量波長進行吸光度疊加的雙波長光度法測定,錶觀摩爾吸光繫數為2.17×10~5 L·mol~(-1)·cm~(-1).加入混閤掩蔽劑NaF-硫脲,可消除常見共存離子的榦擾.本法可用于測定多元素混閤標準溶液和不鏽鋼中的鎳(Ⅱ),迴收率為96%~98%,混閤標準溶液的測定值與認定值相一緻.
보도료신함불현색제4-초기-4'-불분기중담안기우담분여얼(Ⅱ)적현색반응.시험표명,재pH 8.6 Na_2B_4O_7-HCl완충용액、Tween-85존재하,시제여얼(Ⅱ)형성4:1적은정자홍색락합물.최대흡수정봉위504 nm,부봉위424 nm;차재25 mL현색액중얼(Ⅱ)적량재0~4 μg범위내부합비이정률.재량최대정부흡수파장처분별진행단파장분광광도법측정,표관마이흡광계수분별위1.13×10~5 ,1.06×10~5 L·mol~(-1)·cm~(-1).재이424 nm위삼비파장、504 nm위측량파장진행흡광도첩가적쌍파장광도법측정,표관마이흡광계수위2.17×10~5 L·mol~(-1)·cm~(-1).가입혼합엄폐제NaF-류뇨,가소제상견공존리자적간우.본법가용우측정다원소혼합표준용액화불수강중적얼(Ⅱ),회수솔위96%~98%,혼합표준용액적측정치여인정치상일치.
The coloring reaction between a novel fluoride-bearing reagent
(4-nitro-4'-fluorophenyl diazo-amino-azobenzene) and nickel(Ⅱ) was studied. The results showed that, in presence of Tween-85, this reagent could form purple red complex with nickel (Ⅱ) in Na_2B_4O_7-HCl buffer solution at pH 8.6. The positive and negative maximum absorption peaks were at 504 nm and 424 nm,respectively.Beer's law was obeyed for nickel in the range of 0-4 μg/25 mL. The apparent molar absorptivity determined by single-wavelength spectrophotometry at positive and negative maximum absorption wavelengths were 1.13×10~5 and 1.06×10~5 L·mol~(-1)·cm~(-1), respectively. The dual-wavelength spectrophotometric determination was conducted with 424 nm as reference wavelength and 504 nm as measuring wavelength. The apparent molar absorptivity was 2.17×10~5 L·mol~(-1)·cm~(-1). The interference of common coexisting ions could be eliminated by adding mixed masking agent NaF-thiourea. This method could be applied to the determination of nickel(Ⅱ) in multi-element mixed standard solution and stainless steel. The recovery was 96 %-98 %, and the determination results of mixed standard solution were consistent with the certified values.