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1.
重油催化裂化汽油中酚类化合物的分离分析   总被引:1,自引:0,他引:1  
利用100g/L NaOH作萃取剂,二氯甲烷为反萃取剂,油剂比为5:1(体积比)时浓缩分离石家庄炼油厂和燕山石油化工公司的重油催化裂化(RFCC)稳定汽油和预碱洗后汽油中的酚类化合物;多面手利用色谱-质谱联用法对浓缩分离出的酚类化合物进行了检测,结果发现RFCC汽油中的酚类化合物主要是C0-C3苯酚,还有少量C4苯酚;所用稳定汽油和预碱洗后汽油的酚类组成相似,但碱洗后苯酚含量减少。  相似文献   

2.
李延红  姜元博  孙策  邹滢 《分析测试学报》2013,32(11):1316-1321
采用酸液萃取的方法从煤液化油中提取碱性氮化物,气相色谱-质谱联用(GC-MS)和氮化学发光检测器(GC/NCD)进行定性定量。从分析结果可见,碱性氮化物可以通过酸液萃取与油样达到较完全的分离。用GC-MS定性出全馏程煤液化油中含有38种碱性氮化物,主要为吡啶类、苯胺类以及喹啉类氮化物。用GC/NCD对18种全馏程煤液化油中的碱性氮化物定量分析,结果显示其占碱性氮化物总量的88.9%,其中吡啶类占碱性氮化物总量的24.48%,苯胺类占37.98%,喹啉类占26.48%。  相似文献   

3.
利用溶剂萃取和柱色谱等技术浓缩分离新疆宝明页岩油柴油馏分中的碱性氮化物。以宝明页岩柴油为原料,经糠醛溶剂精制,初步得到富集碱性氮化物的抽出油。以抽出油为深度富集碱性氮化物的原料,采用柱色谱等分离方法,从抽出油中分离得到碱性氮化物。利用傅立叶变换红外光谱仪(FT-IR)和气相色谱-质谱联用仪(GC-MS)分别对富集的碱性氮化物进行官能团检测和定性、定量分析。结果表明:新疆宝明页岩油柴油馏分中的碱性氮化物经溶剂精制和柱色谱等分离方法梯度富集后,碱性氮化物的质量分数由抽出油的12.08%提高到最终产物的69.48%,并在富集分离的产物中鉴定出60种碱性氮化物,其中主要为苯胺类、喹啉类和吡啶类化合物,各占25.85%,23.56%和16.52%。  相似文献   

4.
利用盐析辅助液液萃取(SALLE)/高效液相色谱-串联质谱(HPLC-MS/MS)建立了测定渔业水体中环丙沙星等7种喹诺酮类抗生素的分析方法。水样用乙腈提取,硫酸镁盐析分层,提取液经氮吹浓缩后,采用Waters Atlantis C18 色谱柱 (150 mm × 2.1 mm,3.0 μm)以0.1%(体积分数)甲酸水溶液-甲醇为流动相进行梯度洗脱,采用电喷雾正离子模式检测,外标法定量。实验考察了水样pH值、萃取剂、盐析剂以及涡旋混合时间对萃取效率的影响。在最优的实验条件下,7种喹诺酮类抗生素在各自的质量浓度范围内线性良好,相关系数(r2)均大于0.995,检出限(LOD)和定量下限(LOQ)分别为3~10 ng/L和10~25 ng/L。对空白水样进行3个水平的加标回收实验,回收率为77.8%~104%,相对标准偏差(RSD)为3.1%~10%。该方法简单、灵敏、高效,可应用于渔业水体中喹诺酮类抗生素的检测。  相似文献   

5.
吸附法脱除烷基化用汽油中的碱性氮化物   总被引:2,自引:0,他引:2  
考察了磺酸树脂NKC-9、CT-175、D005-Ⅱ和LSI-600以及13X分子筛对催化裂化汽油(FCC 汽油)中碱性氮化物的脱除能力,以及对汽油中的烯烃和噻吩类硫化物的吸附影响.结果表明,以LSI-600为吸附剂时,对FCC汽油中碱性氮化物的吸附选择性最佳.在室温25℃左右、常压,剂油质量比1:35,碱性氮的脱除率达到100%所需要的吸附时间为15min,经溶剂再生,可重复使用.对这5种吸附剂,增大孔径和比表面积均有利于碱性氮化物的吸附,但当孔径足够大时,孔径和比表面积对碱性氮吸附的影响程度减弱.  相似文献   

6.
重油催化裂化汽油中含硫化合物的分析   总被引:7,自引:0,他引:7  
梁咏梅  刘文惠  刘耀芳 《色谱》2002,20(3):283-285
 采用气相法 ,分别利用火焰光度检测器 (FPD)和原子发射检测器 (AED)对中国石化北京燕山石油化工公司 (简称燕化 )炼油厂和石家庄炼油厂生产的重油催化裂化 (RFCC)汽油中的硫化物进行了分析。燕化炼油厂RFCC汽油中总硫只有 2 9 5mg/L ,采用FPD无法检测 ;石家庄炼油厂的RFCC汽油中总硫为 72 0 1mg/L。用标样和气相 质谱法 (GC MS)定性 ,FPD分离检测出 19种硫化物 ,主要是硫醇、噻吩类硫化物 ,硫醚类硫化物和二硫化物均未检出。用AED鉴定出燕化炼油厂RFCC汽油中的硫化物 12种 ,主要是噻吩和四氢噻吩类、低碳硫醇和二硫化物。  相似文献   

7.
多烷基支链仲胺从碱性氰化液中萃取金   总被引:6,自引:0,他引:6  
余建民  李奇伟  陈景 《应用化学》2001,18(4):276-280
研究了多烷基支链促胺从碱性氰化液中萃取金,考察了平衡时间、水相初始pH值、金浓度、离子强度、温度、萃取剂浓度、稀释剂、相比等因素对金萃取率的影响,绘制了萃取等温线,测定了金的饱和容量,考察了萃取体系对银(Ⅰ)、铁(Ⅱ)、铜(Ⅰ)、镍(Ⅱ)、锌(Ⅱ)的萃取性能,计算出了金与这些杂质元素的分离系数,研究了负载有机相中金的反萃,结果表明,该萃取体系在pH5-11范围内对Au(CN)2^-有较高的萃取率和选择性,pH1/2=11.7,可用于碱性氰化液中金的萃取分离。  相似文献   

8.
该文建立了同时检测血液、尿液样本中2C-H、2C-D、2C-P、2C-T-2、2C-T-4、2C-T-7、25D-NBOMe、25C-NBOMe、25B-NBOMe和25I-NBOMe 10种2C系列苯乙胺类衍生物含量的超高效液相色谱-串联质谱(UPLC-MS/MS)法。通过比较沉淀蛋白(PPT)、液-液萃取(LLE)和固相萃取(SPE)3种前处理方法,选用甲醇沉淀蛋白法对血液和尿液样品进行提取。通过对色谱柱和流动相的优化,选用甲醇-水(0.1%甲酸)作为流动相,ACQUITY UPLC?BEH C18(100 mm × 2.1 mm,1.7 μm)色谱柱进行分离。串联质谱的离子源为电喷雾电离源(ESI+),采用多反应监测模式(MRM)进行检测。10种目标物在0.005 ~ 50 ng/mL范围内线性关系良好,相关系数(r2)为0.995 8 ~ 0.999 9。血液和尿液中的检出限分别为0.01 ~ 2 ng/mL和0.002 ~ 5 ng/mL,3个不同加标浓度(1、5、20 ng/mL)下,血液、尿液中的基质效应为71.9%~112%,提取回收率为78.8% ~ 99.3%,日内、日间相对标准偏差(RSD,n = 3)均不高于15%。该方法分离效果好,提取回收率高,基质效应低,且操作简便,检材用量少,适用于血液和尿液中2C系列苯乙胺类衍生物的快速检测。  相似文献   

9.
用Florsil小柱固相萃取分离纯化、气相色谱定性定量同时测定卷烟中5种氨基甲酸酯类农药(西维因、叶蝉散、速灭威、呋喃丹、灭多威)在卷烟烟气中的捕集转移率(CSE)。用OV-101毛细管色谱柱为分离柱,FID(火焰离子检测器)检测。5种农药在12min内得到很好分离。线性范围1-25mg/L,检出限11-16ng。CSE分别为4.3%-10%。  相似文献   

10.
TritonX-100-盐-水液-固萃取体系分离Co,Cd,Zn   总被引:5,自引:0,他引:5  
在含有一定浓度硫酸铵的条件下,TritonX-100水溶液能形成盐水相与聚合物固相。本实验研究了Co(Ⅱ)、Cd(Ⅱ)、Zn(Ⅱ)、Cu(Ⅱ)、Fe(Ⅲ)与4-(2-吡啶偶氮)间苯二酚(PAR)形成的配合物在TritonX-100盐水萃取体系液固两相中的分配行为。主要探讨萃取酸度,萃取剂用量和硫酸铵浓度等条件对金属离子萃取率的影响。用控制酸度的方法实现了Co(Ⅱ)与Cd(Ⅱ),Co(Ⅱ)与Zn(Ⅱ)的定量分离。每组金属离子浓度在1∶1000倍情况下分离互不干扰,结果满意。该法可用于样品的提纯与分离。  相似文献   

11.
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.  相似文献   

12.
KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.  相似文献   

13.
The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.  相似文献   

14.
Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.  相似文献   

15.
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.  相似文献   

16.
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.  相似文献   

17.
The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion.  相似文献   

18.
19.
An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions.  相似文献   

20.
Quercetin, the polyphenolic compound, which has the highest daily intake, is well known for its protective effects against aging diseases and has received a lot of attention for this reason. Both quercetin 3-O-β-d-glucuronide and quercetin 3′-O-β-d-glucuronide are human metabolites, which, together with their regioisomers, are required for biological as well as physical chemistry studies. We present here a novel synthetic route based on the sequential and selective protections of the hydroxyl functions of quercetin allowing selective glycosylation, followed by TEMPO-mediated oxidation to the glucuronide. This methodology enabled us to synthesize the five O-β-d-glucosides and four O-β-d-glucuronides of quercetin, including the major human metabolite, quercetin 3-O-β-d-glucuronide.  相似文献   

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