光谱学与光谱分析
光譜學與光譜分析
광보학여광보분석
SPECTROSCOPY AND SPECTRAL ANALYSIS
2015年
1期
193-197
,共5页
尹晓航%施文健%沈昕%马骏涛%李亮
尹曉航%施文健%瀋昕%馬駿濤%李亮
윤효항%시문건%침흔%마준도%리량
芳香族氨基化合物%J酸(2-氨基-5-萘酚-7-磺酸)%重氮偶合%分光光度法
芳香族氨基化閤物%J痠(2-氨基-5-萘酚-7-磺痠)%重氮偶閤%分光光度法
방향족안기화합물%J산(2-안기-5-내분-7-광산)%중담우합%분광광도법
Aromatic amino compound%J-Acid(2-amino-5-naphthol-7-sulfonic acid)%Diazotion-coupling%Spectrophotometry
综合考虑显色反应选择性、反应速度、灵敏度和偶氮化合物的水溶性等问题,通过对偶合组分分子结构的理论设计和实验筛选,研究了显色反应方法和条件,提出利用J酸(2-氨基-5-萘酚-7-磺酸)作为偶合试剂分光光度法测定水中芳香族氨基化合物。溴化钾催化,室温下,亚硝酸盐与芳香族氨基化合物在稀盐酸水溶液中发生重氮化反应,在碳酸钠水溶液中重氮盐与 J酸偶合生成有色偶氮化合物,最大吸收波长480 nm。所测苯胺、4-氨基苯磺酸和1-萘胺的表观摩尔吸光系数分别为3.95×104,3.24×104和3.91×104 L?mol-1?cm -1。水中共存离子影响研究结果表明:地表水中常见离子对测定结果不产生影响。采用J酸分光光度法测定了上海市复兴岛运河水样,同时,用标准加入法做回收实验,实验结果:苯胺回收率为98.5%~102.1%,相对标准偏差2.08%。J酸是一种常见有机试剂,易溶于水,挥发性低,其毒性大大低于盐酸萘乙二胺。J酸分光光度法测定芳香族氨基化合物具有灵敏度高、选择性好、操作简单快速、测定结果准确等优点,可用于环境水体中痕量芳香族氨基化合物的测定。
綜閤攷慮顯色反應選擇性、反應速度、靈敏度和偶氮化閤物的水溶性等問題,通過對偶閤組分分子結構的理論設計和實驗篩選,研究瞭顯色反應方法和條件,提齣利用J痠(2-氨基-5-萘酚-7-磺痠)作為偶閤試劑分光光度法測定水中芳香族氨基化閤物。溴化鉀催化,室溫下,亞硝痠鹽與芳香族氨基化閤物在稀鹽痠水溶液中髮生重氮化反應,在碳痠鈉水溶液中重氮鹽與 J痠偶閤生成有色偶氮化閤物,最大吸收波長480 nm。所測苯胺、4-氨基苯磺痠和1-萘胺的錶觀摩爾吸光繫數分彆為3.95×104,3.24×104和3.91×104 L?mol-1?cm -1。水中共存離子影響研究結果錶明:地錶水中常見離子對測定結果不產生影響。採用J痠分光光度法測定瞭上海市複興島運河水樣,同時,用標準加入法做迴收實驗,實驗結果:苯胺迴收率為98.5%~102.1%,相對標準偏差2.08%。J痠是一種常見有機試劑,易溶于水,揮髮性低,其毒性大大低于鹽痠萘乙二胺。J痠分光光度法測定芳香族氨基化閤物具有靈敏度高、選擇性好、操作簡單快速、測定結果準確等優點,可用于環境水體中痕量芳香族氨基化閤物的測定。
종합고필현색반응선택성、반응속도、령민도화우담화합물적수용성등문제,통과대우합조분분자결구적이론설계화실험사선,연구료현색반응방법화조건,제출이용J산(2-안기-5-내분-7-광산)작위우합시제분광광도법측정수중방향족안기화합물。추화갑최화,실온하,아초산염여방향족안기화합물재희염산수용액중발생중담화반응,재탄산납수용액중중담염여 J산우합생성유색우담화합물,최대흡수파장480 nm。소측분알、4-안기분광산화1-내알적표관마이흡광계수분별위3.95×104,3.24×104화3.91×104 L?mol-1?cm -1。수중공존리자영향연구결과표명:지표수중상견리자대측정결과불산생영향。채용J산분광광도법측정료상해시복흥도운하수양,동시,용표준가입법주회수실험,실험결과:분알회수솔위98.5%~102.1%,상대표준편차2.08%。J산시일충상견유궤시제,역용우수,휘발성저,기독성대대저우염산내을이알。J산분광광도법측정방향족안기화합물구유령민도고、선택성호、조작간단쾌속、측정결과준학등우점,가용우배경수체중흔량방향족안기화합물적측정。
The problems such as chromogenic reaction selectivity ,reaction rate ,sensitivity and water-solubility of azo com-pounds were considered .The molecular structures of coupling components were theoretically designed and screened in the pres-ent research .The reaction conditions and methods of chromogenic reaction were investigated .J-Acid (2-amino-5-naphthol-7-sul-fonic acid) as a coupling reagent to determine aromatic amino compounds was established .In the presence of potassium bromide , at room temperature ,nitrite reacted with aromatic amino compounds in the medium of thin hydrochloric acid .Then diazonium salt reacted with J-Acid in the aqueous solution of sodium carbonate ,forming coloured azo dye ,which had a maximum adsorption at 480 nm .The molar adsorption coeffcients of aniline ,4-aminobenzene sulfonic acid and 1-naphthylamine were 3.95 × 104 ,3.24 × 104 and 3.91 × 104 L?mol-1 ?cm-1 ,respectively .Experimental results showed that common coexisting ions on the surface water did not affect the results of determination .J-Acid of spectrophotometry was used to determine the samples of Shanghai Fu Xing Dao canal .Meanwhile ,recovery experiments by standard addition method were done .Experiment results showed that the recoveries of aniline were in the range of 98.5% ~102.1% ,and RSD was 2.08% .J-Acid is a common organic reagent .It is sol-uble in water and low volatile ,and its toxicity is much lower than N-ethylenediamine .spectrophotometric determination of aro-matic amino compounds by J-Acid has the advantage of high sensitivity ,good selectivity ,simple rapid operation and accurate re-sults ,and thus it can be used for the determination of trace aromatic amino compounds in the environmental water .