分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2015年
9期
1422-1428
,共7页
李晴%黄晓兰%林晓珊%吴惠勤
李晴%黃曉蘭%林曉珊%吳惠勤
리청%황효란%림효산%오혜근
电化学腐蚀%不锈钢丝%固相微萃取%地沟油%特征杂质成分%气相色谱-质谱
電化學腐蝕%不鏽鋼絲%固相微萃取%地溝油%特徵雜質成分%氣相色譜-質譜
전화학부식%불수강사%고상미췌취%지구유%특정잡질성분%기상색보-질보
Electrochemical corrosion%Stainless steel%Solid phase microextraction%Gutter oil%Characteristic impurities%Gas chromatography-mass spectrometry
通过电化学腐蚀的方法制得多孔不锈钢针/丝作为基体,涂渍特异性吸附地沟油杂质的涂层材料(NACC-2),成功制备了固相微萃取(SPME)萃取头,并应用于地沟油样品分析。研究表明,所用的不锈钢针电化学腐蚀最佳条件为:30 mA 电流强度下,2 mol/L HCl中腐蚀1 min,超声3 min,重复5次;涂渍的条件为5%的涂层溶液,涂渍35次。萃取头用于地沟油样品微量特征杂质成分的萃取富集,选择性好、耐用、稳定性好,成本低。测得某典型地沟油样品中的特征杂质成分含量为乙酸42.7 mg/kg,3-丁烯腈21.6 mg/kg,二硫化碳71.8 mg/kg,烯丙基异硫氰酸酯2.8 mg/kg。
通過電化學腐蝕的方法製得多孔不鏽鋼針/絲作為基體,塗漬特異性吸附地溝油雜質的塗層材料(NACC-2),成功製備瞭固相微萃取(SPME)萃取頭,併應用于地溝油樣品分析。研究錶明,所用的不鏽鋼針電化學腐蝕最佳條件為:30 mA 電流彊度下,2 mol/L HCl中腐蝕1 min,超聲3 min,重複5次;塗漬的條件為5%的塗層溶液,塗漬35次。萃取頭用于地溝油樣品微量特徵雜質成分的萃取富集,選擇性好、耐用、穩定性好,成本低。測得某典型地溝油樣品中的特徵雜質成分含量為乙痠42.7 mg/kg,3-丁烯腈21.6 mg/kg,二硫化碳71.8 mg/kg,烯丙基異硫氰痠酯2.8 mg/kg。
통과전화학부식적방법제득다공불수강침/사작위기체,도지특이성흡부지구유잡질적도층재료(NACC-2),성공제비료고상미췌취(SPME)췌취두,병응용우지구유양품분석。연구표명,소용적불수강침전화학부식최가조건위:30 mA 전류강도하,2 mol/L HCl중부식1 min,초성3 min,중복5차;도지적조건위5%적도층용액,도지35차。췌취두용우지구유양품미량특정잡질성분적췌취부집,선택성호、내용、은정성호,성본저。측득모전형지구유양품중적특정잡질성분함량위을산42.7 mg/kg,3-정희정21.6 mg/kg,이류화탄71.8 mg/kg,희병기이류청산지2.8 mg/kg。
A special solid phase micro extraction ( SPME ) fibre was successfully attained by coating with a special adsorptive material on a porous stainless steel support. And the porous stainless steel support was prepared by electrochemical corrosion for the first time. The optimized erosion condition in this research was as follows: the current intensity of 30 mA, the stainless steel was etched in 2 mol/L hydrochloride solution for 1 min, then sonicated for 3 min; these procedures repeated 5 times. Meanwhile, the treated fiber coated 35 times in the sorbent solution with concentration of 5% ( m/V) in dichloromethane. The SPME fibre was applied to the analysis of gutter oil samples, and the performance of the SPME fibre for the headspace solid phase micro extraction of the exogenous impurities in gutter oil was specific, durable, stable and low-cost. The four detected trace level characteristic impurities in certain gutter oil were given as follows:42 . 7 mg/kg for acetic acid, 21. 6 mg/kg 3-butenenitrile, 71. 8 mg/kg carbon disulfide and 2. 8 mg/kg allylisothiocyanate.