提出了一种利用已知过量的亚硝酸盐与氨基磺酸反应,对氨基磺酸进行分光光度测定的方法.未反应的亚硝酸根采用其与对硝基苯胺及N-(1-萘基)乙二胺二盐酸盐(NEDA)之间的重氮偶合反应来测定.所生成的偶氮染料的最大吸收波长为545 nm,实测摩尔吸光度为6.1×100 L/(mol·cm).该方法可用于测量总体积为25 mL的样品中0～25 μg的氨基磺酸.当样本数为10时,测定15μg氨基磺酸的相对标准偏差为2%.将该方法用于测定镍、铅、铁、钌、锢等金属的氨基磺酸盐电镀液废水中氨基磺酸的含量,其结果采用加标回收率方法进行了验证.
A proposed spectrophotometric method for the determination of sulfamic acid involves reaction of sulfamic acid with known excess of nitrite. The unreacted nitrite is determined by diazo coupling reaction involving p-nitroaniline and N-(1-naphthyi)ethylenediamine dihydrochloride [NEDA]. The absorption maximum (λmax) for the formed azo dye is at 545 nm and the calculated molar absorptivity is sulfamic acid in the range of 0-25 lag in an overall volume of 25 mL, and the relative standard deviation is 2% for n = 10at 15 μg level of sulfamic acid. The developed method was applied to the determination of sulfamic acid in the effluents of nickel, lead, iron, ruthenium and indium sulfamate electroplating baths. The results obtained were validated by recovery studies of added sulfamic acid.
参考文献
| [1] | Kirk-Othmer Encyclopedia of Chemical Technology[M].New York:John Wiley and Sons,Inc,1997:23,120. |
| [2] | LOWENHEIM F A.Modem Electroplating[M].New York:John Wiley and Sons,Inc,1974:249. |
| [3] | Metal Finishing 53rd Guidebook and Directory[M].Hackensack:Metals and Plastics Publications Inc,1985:177,256,258,335. |
| [4] | POHAN1SH R P;GREENE S A.Hazardous Chemical Safety Guide for the Plastic Industry[M].New York:mcgraw-hill Book Company,inc,2000 |
| [5] | BAUMGARTEN P;KRUMMACHER A-H .(U)bet die umsetzung von schwefeltrioxyd mit ammoniak in w(a)βriger znsammensetzung der sog.,,schwefeltrioxyd-nebel"[J].Berichte der dentschen chemischen Gesellschaft,1934,67(07):1257-1260. |
| [6] | MEUWESEN A;MERKEL H .Gasvolumetrische bestimmung der amidosulfons(a)ure,H2NSO3H[J].Zeitschrift Fur Anorganische Und Allgemeine Chemie,1940,244(01):89-93. |
| [7] | CARSON W N .Gasometric determination of nitrite and sulfamate[J].Analytical Chemistry,1951,23(07):1016-1019. |
| [8] | BOWLER W W;ARNOLD E A .Comparison of methods for determination of sulfamates[J].Analytical Chemistry,1947,19(05):336-337. |
| [9] | DEEPA B;NAGARAJA K S;BALASUBRAMANIAN N .Speetrophotometric determination of sulfamie acid in metal sulfamate bath effluents[J].Plating and Surface Finishing,2005,92(04):54-57. |
| [10] | PANDURANGAPPA M;BALASUBRAMANIAN N .Extractive speetrophotometric determination of trace amounts of nitrogen dioxide,nitrite,and nitrate[J].Mikroehimiea Acta,1996,124(1/2):137-146. |
| [11] | VOGEL A I;BASSETT J;DENNY R C;JEFFERY C H.Vogel's Textbook of Quantitative Inorganic Analysis[M].London:ELBS,1989:515. |
| [12] | SITTIG M.Electroplating and Related Metal Finishing:Pollutant and Toxic Materials Control[M].Park Ridge:Noyes Data Corporation,1978:150. |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%