汽油机油基础油和汽油清净剂高温模拟蒸馏特征分析

利用NB/SH/T 0829《沸程范围174～700℃石油馏分沸程分布的测定气相色谱法》测定了矿物油、天然气合成油(GTL)、PAO、Ⅲ类基础油、汽油清净剂的模拟蒸馏数据,探讨了润滑油基础油和3种汽油清净剂的模拟蒸馏曲线特征。矿物油由于含有较多的正构烷烃,模拟蒸馏曲线显示正构烷烃特征; GTL和Ⅲ类基础油正构烷烃含量低,模拟蒸馏曲线呈现光滑特征; PAO和汽油清净剂是聚合产品,对于低聚合度产品模拟蒸馏出现沸程非连续性特征。利用该方法可以区分汽油机油基础油和汽油清净剂组分的某些特征。     

质谱技术研究加氢裂化尾油链烷烃结构组成

利用气相色谱-质谱（GC-MS）联用技术,在瓦斯油中饱和烃馏分的烃类测定方法（SH/T 0659）的基础上,建立了测定加氢裂化尾油中正、异构链烷烃总含量及正构链烷烃碳数分布的分析方法,再根据气相色谱-场电离高分辨飞行时间质谱（GC-FI TOFMS）得到样品的链烷烃碳数分布,进而得到异构链烷烃的碳数分布。该技术与现有的烃类组成测定方法相比,能够提供更详细的链烷烃分子组成信息。利用所建方法对转化深度不同的3种加氢裂化尾油进行了分析,研究了转化深度对其链烷烃结构的影响,结果表明：随转化程度的加深,加氢裂化尾油中正、异构链烷烃含量均升高,总链烷烃含量增加,正构链烷烃占总链烷烃的比例下降;3种加氢裂化尾油的正构烷烃、异构烷烃以及总链烷烃的碳数均呈正态分布,高转化率时加氢裂化尾油含低碳数正、异构链烷烃较多,而中低转化率时加氢裂化尾油含高碳数正、异构链烷烃较多。     

异构烷烃分析及在石油地质研究中的应用

简要介绍了展构烷烃分析技术。利用热解气相色谱分析方法,依据担体物理性质和被测物化学结构特点,优选出最佳担体,保证了异构烷烃分析精度,从而使异构烷烃分析能够直接从烃源岩、储集岩、饮和烃等样品难过热蒸发分离进行检测。降低分流比,增加进样量,提高灵敏度,使常量分析提高到痕量分析。对异构烷烃化合物在石油地质方面的应用进行了初步探讨。     

原料性质对正构烷烃加氢异构化选择性影响的研究

对不同烃类在分子筛催化剂上的加氢异构化反应进行研究,考察正构烷烃链长变化对其加氢异构化选择性的影响、长链正构烷烃与短链正构烷烃之间的影响、正构烷烃与异构烷烃之间的影响。结果表明：正构烷烃的碳链越长其降凝越困难;混合原料中长链烷正构烷烃与短链正构烷烃相互影响、正构烷烃与异构烷烃相互影响,长链烷烃存在时会影响短链烷烃的反应活性,而异构烷烃的存在对正构烷烃反应活性无影响,但对正构烷烃的异构产物分布有影响;在转化率相当的条件下,混合原料的异构产物分布比单纯正构烷烃的异构烷烃分布更加有利于降低凝点。     

氧化氮化学电离质谱法测定减压馏分油中链烷烃

用5%NO/95%N2的混合气体作为反应气,用氧化氮化学电离质谱法分析得到了大庆减压馏分油中链烷烃的碳数分布及正构烷烃与异构烷烃的分布。探讨了影响分子离子峰强度的各种因素,选择了最佳的工作条件。在确定的工作条件下,不需加入标准化合物,即可对不同碳数的链烷烃进行定性分析,准确得到相对分子质量信息,同时,结合总离子流色谱图,通过抽提离子的方法可以得到链烷烃中正构烷烃和异构烷烃的定量结果。     

加氢异构化催化剂的研究——-加氢功能的影响

以ZSM 22分子筛为酸性组分,制备了不同分子筛含量、不同金属负载量以及不同金属种类的加氢异构催化剂。采用XRD、氢氧滴定、N2吸附、吡啶吸附和SEM等表征工具对所用分子筛以及制备的催化剂进行了详细的表征。以正癸烷为模型化合物,考察了制备的催化剂的烷烃异构转化活性和选择性,并将获得的反应结果与表征数据相关联。结果表明,对于长链烷烃加氢异构反应,当加氢功能不足时,长链烷烃加氢/脱氢反应为控制步骤;为了制备双功能平衡的加氢异构催化剂,Pd负载量要高于Pt,但当双功能平衡后2种催化剂的异构反应行为一致。对于长链烷烃加氢异构反应,加氢中心与酸性中心之间的距离不是影响催化剂异构选择性的关键因素。     

烃源岩中支链烷烃化合物的检出及意义

以板桥地区烃源岩为例，对烃源岩中的坛链烷烃化合物进行了详细的研究。烃源岩中的支链烷烃主要包括异构、反异构、单甲基中间支链烷烃和类异戊二烯烷烃。在板桥地区烃源岩中，共检测到各类支链烷烃６１种，对它们的结构进行了鉴定；对其分布特征及生源意义作了初步探讨。推测这类化合物大多反映烃源岩中细菌微生物生源输入的贡献。     

多维气相色谱法测定石脑油族组成

建立了一种采用具有多阀、多柱和吸附阱的多维气相色谱测定石脑油族组成的分析方法。通过5个阀对7根选择性不同的色谱柱进行准确切换控制,使样品分别进入不同的色谱柱中,分离出正构、异构烷烃,正构、异构烯烃,环烷烃,环烯烃和芳烃,然后利用程序升温,使各族组分再按碳数分离后进行定量分析。对标样的测定结果表明,组分质量分数可精确至0.01%,加标回收率为99.7%～108.6%,相对标准偏差为0.24%～1.40%。     

5A分子筛吸附正构烷烃试验研究

用5A分子筛进行重整抽余油吸附试验,脱除重整抽余油中的正构烷烃,得到异构烷烃吸余油作为高辛烷值汽油的调和组分。试验了不同厂家、不同温度、不同分子筛用量、不同吸附时间对吸附效果的影响,得到优化的工艺条件。     

柱头进样气相色谱法测定石蜡、微晶蜡的组成

采用柱头进样的高温气相色谱技术，建立了测定石蜡和微晶蜡中正、异构烷烃含量及相应的碳数分布的方法。首先采用当前基线积分得到正、异构烷烃的总量，再从中扣除由谷谷积分所得正构烷烃部分而得到异构烷烃含量的方法进行各碳数正、异构烷烃含量的计算。石蜡组成测定的相对标准偏差在±３％以内，微晶蜡测定的相对标准偏差±６％以内。并与分子筛吸附法的测定结果进行了对比，两者有很好的一致性。本方法适用范围广，信息量大，同时具有分析速度快，准确度、精密度高等特点，有实用价值。     

T702添加剂中石油磺酸钠分析方法的优化

分析了化学法和红外光谱法测定T702添加剂中石油磺酸钠的优势和不足,将这两种分析方法的优势结合起来,优化了T702添加剂中石油磺酸钠的分析方法,提高了分析效率。     

议水化学氯离子分析中的指示剂用量

对于各种分析方法(包括部颁标准),如存在某些不够严谨之处,都会给分析工作带来不顺利,甚至造成过失。本文针对"水中氯离子的分析"这一方法,就指示剂的加入量,从理论和实践两方面进行讨论。      

Determination of melamine in feed: Validation of a gas chromatography–mass spectrometry method according to 2004/882/CE regulation

Pet food, animal feed and other protein-based food commodities were recently found to contain melamine, an industrial chemical used in the manufacturing of plastics, flame retardants, and other products. The US Food and Drug Administration do not approve it for use in food or animal feed. Then there is a need for analytical methods to determine melamine that may be present in dry animal feed. Cause the validation is required for the analytical methods used in the official control of feed, we validated a Gas chromatography–mass spectroscopy method according to 2004/882/CE regulation.     

Review on the qualitative and quantitative analysis of the mycotoxin citrinin

Citrinin is a toxic metabolite produced by several filamentous fungi of the genera Penicillium, Aspergillus and Monascus, which has been encountered as a natural contaminant in grains, foods, feedstuffs, as well as biological fluids. This mycotoxin is hepato-nephrotoxic and implicated in disease outbreaks in animals and humans. Some analytical systems have been developed for its detection and quantification. The purpose of this paper is to review physicochemical properties, qualitative and quantitative analytical methods of citrinin, evaluate advantages and disadvantages of various analytical techniques, and bring forward some constructive suggestions on establishment of international criteria for quality control of products contaminated with citrinin by comparing chromatographic properties, sample pre-treatment, recovery rate and detection limit of citrinin among various analytical methods. This paper concentrates the most important achievements on the analytical methods of citrinin published from 1980 to early 2004.     

苯酚钾的合成及应用

重点讨论了苯酚钾的合成方法,简要介绍了苯酚钾的分析方法,初步介绍了苯酚钾在有机合成中的应用。     

Detection of addition of apple juice in purple grape juice

Due to increasing grape juice consumption, quality control is a reality in all countries which produce and consume this product. The most common form of adulteration is by substituting grape juice with apple juice. The adulterated samples can be identified by specific analysis, since apple juice has some compounds that grape has not. There are many studies about the phlorizin and sorbitol content in wines, but in grape juice they are scarce. Therefore, analytical methods to identify the composition of grape juices and determine their authenticity are needed to ensure quality control. The present study aimed to the validation and application of analytical methods for the determination of phlorizin and sorbitol, to detect the addition of apple juice in purple grape juice, by high-performance liquid chromatography. Initially, the methods were validated and tests were conducted by additions of percentages of apple juices in grape juices. Finally, experimental and commercial grape and apple juices were analyzed. Our study found that both methods are effective in detecting the addition of apple juice in grape juice. Four of the 39 commercial grape juices analyzed showed adulteration by the addition of apple juice in grape juice.     

高浓度组份的色谱定量方法研究(Ⅱ)

给出了一种测定高浓度组份含量的解析法。此法是根据色谱峰曲线的Gauss方程推导而得。由于 Gauss 方程仅是一种近似描述色谱峰曲线的数学模型,本文严格地讨论了解析法本身的定量精度,并给出了相应的误差估计公式,确定了方法的适用范围。最后,从理论上和实际定量结果与其它方法进行了比较。     

土壤挥发性有机物分析方法现状与进展

为了建立石化行业土壤中挥发性有机物（VOCs）的分析方法,研究了国内外土壤中VOCs的分析标准,综述了土壤中VOCs的前处理技术和检测方法,并对建立石化行业土壤中VOCs分析方法提出建议。我国目前已有7项土壤中VOCs的分析标准,但涵盖的VOCs种类偏少,分析对象主要为卤代烃和芳烃。土壤中VOCs的前处理技术主要有溶剂萃取、顶空、吹扫捕集和固相微萃取等,检测方法有GC-FID,GC-MS,GC-PID。由于石化行业土壤中VOCs污染物种类不仅包括卤代烃和芳烃,还可能会有酮类、醛类、烷烃、环烷烃、烯烃等,因此需要根据不同的污染物种类建立对应的分析标准,并探索适合石化行业的土壤中VOCs前处理技术和检测方法。     

INVESTIGATION AND EVALUATION OF PETROLEUM ASPHALT AGING PROPERTY ON OXYGEN ABSORPTION BY INVERSE GAS LIQUID CHROMATOGRAPHY

The aging mechanisms and performances on oxygen absorption of ten petroleum asphalts were studied and evaluated by the inverse gas liquid chromatography with the Aging Comprehensive Index, the Aging Subtraction Number, the Aging Total Area and the Aging Character Factor methods based on the changes of the retention coefficients of analytical compounds in the petroleum asphalt chromatographic column during continuous aging caused by oxygen absorption under an oxygen flow rate of 15∼30 ml/min at 140°C, after the inert support was evenly coated with toluene-dissolved petroleum asphalt and packed into the chromatographic column. The relative polarity of petroleum asphalt and the retention coefficients of analytical compounds increase after absorbing oxygen and the changes of the retention coefficients of the oxygen-containing analytical compounds, especially phenol are evidently greater than those of the nitrogen and sulfur-containing and aromatic analytical compounds. There are obvious differences between the retention coefficients of analytical compounds in the petroleum asphalt columns from different sources and between their changes with the aging on oxygen absorption. The repeated determinations of these evaluation methods show that the standard deviations are less than 1.63 and the variable coefficients under 0.2. The test data are found.to be reliable by Grubhs examination at 95% confidence level. Of the four evaluation methods the Aging Subtraction Number method is the most simple and convenient in operation and takes least time in evaluation.     

利用地质方法研究小断块油藏剩余油分布

针对八面河油田北区小断块油藏断裂系统复杂,剩余油分布认识难度大的特点,提出利用断层分析法、构造形态分析法、测井二次解释法等地质方法研究剩余油分布。实际应用效果表明,在油田开发中后期,地质研究方法是剩余油分布研究的重要方法。