岩矿测试
巖礦測試
암광측시
ROCK AND MINERAL ANALYSIS
2014年
3期
433-438
,共6页
油气化探样品%稠环芳烃%前处理%振荡萃取法
油氣化探樣品%稠環芳烴%前處理%振盪萃取法
유기화탐양품%주배방경%전처리%진탕췌취법
oil and gas exploration samples%poly-nuclear aromatic hydrocarbons%pre-treatment%oscillation extraction
在油气化探工作中,稠环芳烃含量对区域油气异常有着重要的指示作用。对于稠环芳烃的测定,诸多前处理条件对稠环芳烃的提取效率有显著的影响。本文研究了油气化探样品振荡提取法的多种前处理条件(提取溶剂、样品粒径、振荡时间和静置时间、提取温度)对荧光强度测定结果的影响。实验结果表明,提取溶剂不同,测定结果存在较大差异,各提取溶剂的提取效率大小依次为:二氯甲烷﹥正己烷﹥乙酸乙酯﹥石油醚。综合考虑溶剂背景值对测定结果的影响,选择以正己烷为提取溶剂进行条件实验。在研究的粒径范围内,荧光强度随样品粒径的减小而增大,但粒径过小荧光强度反而降低,粒径在0.125~0.090 mm之间的样品荧光强度最高;荧光强度随着振荡时间和静置时间的增加而增强,其中静置时间的影响较大,静置9h后荧光强度提高不显著;振荡时间的影响相对较小,振荡20 min后提取效率提高不显著;提取温度对荧光强度的影响最为显著,在相同条件下,提取温度越高荧光强度越大,且提取温度是影响稠环芳烃测定结果重现性的关键因素。油气化探样品前处理的最优化条件为:采用粒径在0.090~0.177 mm之间的样品,以色谱纯正己烷为溶剂,提取温度25℃,振荡时间20 min,静置时间12 h。
在油氣化探工作中,稠環芳烴含量對區域油氣異常有著重要的指示作用。對于稠環芳烴的測定,諸多前處理條件對稠環芳烴的提取效率有顯著的影響。本文研究瞭油氣化探樣品振盪提取法的多種前處理條件(提取溶劑、樣品粒徑、振盪時間和靜置時間、提取溫度)對熒光彊度測定結果的影響。實驗結果錶明,提取溶劑不同,測定結果存在較大差異,各提取溶劑的提取效率大小依次為:二氯甲烷﹥正己烷﹥乙痠乙酯﹥石油醚。綜閤攷慮溶劑揹景值對測定結果的影響,選擇以正己烷為提取溶劑進行條件實驗。在研究的粒徑範圍內,熒光彊度隨樣品粒徑的減小而增大,但粒徑過小熒光彊度反而降低,粒徑在0.125~0.090 mm之間的樣品熒光彊度最高;熒光彊度隨著振盪時間和靜置時間的增加而增彊,其中靜置時間的影響較大,靜置9h後熒光彊度提高不顯著;振盪時間的影響相對較小,振盪20 min後提取效率提高不顯著;提取溫度對熒光彊度的影響最為顯著,在相同條件下,提取溫度越高熒光彊度越大,且提取溫度是影響稠環芳烴測定結果重現性的關鍵因素。油氣化探樣品前處理的最優化條件為:採用粒徑在0.090~0.177 mm之間的樣品,以色譜純正己烷為溶劑,提取溫度25℃,振盪時間20 min,靜置時間12 h。
재유기화탐공작중,주배방경함량대구역유기이상유착중요적지시작용。대우주배방경적측정,제다전처리조건대주배방경적제취효솔유현저적영향。본문연구료유기화탐양품진탕제취법적다충전처리조건(제취용제、양품립경、진탕시간화정치시간、제취온도)대형광강도측정결과적영향。실험결과표명,제취용제불동,측정결과존재교대차이,각제취용제적제취효솔대소의차위:이록갑완﹥정기완﹥을산을지﹥석유미。종합고필용제배경치대측정결과적영향,선택이정기완위제취용제진행조건실험。재연구적립경범위내,형광강도수양품립경적감소이증대,단립경과소형광강도반이강저,립경재0.125~0.090 mm지간적양품형광강도최고;형광강도수착진탕시간화정치시간적증가이증강,기중정치시간적영향교대,정치9h후형광강도제고불현저;진탕시간적영향상대교소,진탕20 min후제취효솔제고불현저;제취온도대형광강도적영향최위현저,재상동조건하,제취온도월고형광강도월대,차제취온도시영향주배방경측정결과중현성적관건인소。유기화탐양품전처리적최우화조건위:채용립경재0.090~0.177 mm지간적양품,이색보순정기완위용제,제취온도25℃,진탕시간20 min,정치시간12 h。
The content of poly-nuclear aromatic hydrocarbons is a very important index to trace abnormalities in regional oil and gas for geochemical exploration samples. The extraction efficiency of the target compounds is influenced by many pre-treatment conditions such as extraction solvents,grain size,shaking time,standing time and extraction temperature. The above-mentioned conditions were studied systematically in this research with oscillation extraction for oil and gas geochemical exploration samples. Based on research results,the solvent plays an important role in preparation. The extraction efficiency of solvents in turn from high to low are dichloromethane, n-hexane,ethyl acetate and petroleum ether. Considering the background effect of different solvents to measured results,the n-hexane was selected to study the experimental conditions. The fluorescence intensity was reduced when grain size was below 0. 090 mm. Satisfactory data can be obtained when sample grain size is between 0. 125-0. 090 mm. The fluorescence intensity was increased simultaneously with increasing oscillation time and hold time. When the hold time extended to 9 h,the extraction efficiency was improved insignificantly. The oscillation time has a minor effect on extraction efficiency while more than 20 min oscillation time does not improve the extraction efficiency. The extraction temperature plays an important role for extraction efficiency. Under the same conditions, the fluorescence intensity was increased when the temperature was raised. The temperature is the most important factor for the repeatability test. The experimental conditions were optimized with grain size of 0. 090-0. 177 mm, solvent of dichloromethane,extraction temperature of 25℃,20 min shaking time,and 12 h hold time.