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1.
探讨用溴甲酚绿碱性分相滴定法测定石油磺酸盐的质量浓度。该法采用了碱性乙醇—水系溶剂,以溴甲酚绿作指示剂,用磷酸缓冲溶液来调节pH,并用阳离子表面活性剂溶液进行滴定,从而测定出石油磺酸盐的质量浓度。实验测得值与样品参考值误差较小,此方法用来测定石油磺酸盐的质量浓度是可行的。此外,本实验研究了指示剂的用量、有机相溶剂的选择及用量、缓冲溶液用量、无机盐、醇、碱、聚合物、多重综合因素对测定结果的影响,并研究了此方法的测定范围以及可靠性验证。 相似文献
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采用柱层析法将石油磺酸盐产品分离成未磺化油、油溶性组分、中间性组分和亲水性组分,考察柱层析的进样量和温度对各组分含量测定值的影响。用红外光谱分析各组分的结构信息,并用测定Krafft点的方法判断石油磺酸盐产品中各组分的水溶性。实验结果表明:石油磺酸盐产品是由不同极性组分组成的复杂表面活性物。柱层析进样量为1.0~1.7 g时,各组分的质量分数重现性好;柱层析的适宜温度为50℃,此时回收率较高。用电导法测定各组分的Krafft点,水溶性石油磺酸盐的Krafft点最低。 相似文献
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研究建立了同时测定三磷酸胞苷二钠中乙醇、丙酮、氯甲醚、甲苯、苯乙烯5种有机溶剂残留量的毛细管气相色谱法。样品以乙腈为溶剂,经DB-FFAP(30 m×0.32 mm×0.25μm)毛细管柱分离,氢火焰离子化检测器检测,这5种有机溶剂呈良好的线性响应,平均回收率在98.3%~99.5%,精密度RSD在0.21%~1.92%,最低检出限可达5.0~7.5 mg/kg。本方法简单、灵敏、准确,完全能满足药品中所述有机溶剂残留量的测定要求。 相似文献
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石油磺酸盐原料是影响磺酸盐产品质量的重要因素。原料中可磺化组分含量决定了磺酸盐产品的活性物含量,而原料组成又决定了产品的稳定性能,因此,选择一种适合生产石油磺酸盐的原料,对于石油磺酸盐在油田大规模应用推广具有重要意义。本文通过调整润滑油系统的工艺控制条件,提高馏分油的可磺化组分,同时对润滑油馏分油及其副产物进行组成分析,优化出适合磺化生产磺酸盐的原料。 相似文献
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建立了阳极电泳涂料中有机溶剂含量的顶空毛细管气相色谱分析方法。选用大口径HP-快速GC残留溶剂柱为分离柱,FID为检测器,内标法进行定量,并讨论了顶空平衡温度、平衡时间对测定的影响。分析结果表明:该方法对有机溶剂达到了完全分离,溶剂和内标乙二醇乙醚的不同质量比与其相应特征峰的峰面积之比有较好的线性关系,相关系数为0.9993~0.9997,测定结果的RSD为1.12%~2.65%,样品的回收率为98.87%~100.35%。 相似文献
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为缩短叠氮硝胺吸收药组分定量分析时间,采用压延烘干法制备了样品,并与过筛烘干法制备的样品进行了比较。用液相色谱法、卡尔·费休法分别检测了两种样品的组分含量和水分含量。结果表明,压延烘干法制备样品共需要1.2h,明显少于过筛烘干法的4.5h。压延烘干法制得的样品均匀性更好,使得取样量可以由过筛烘干法的2g减少到0.2g,配制试样溶液时所需的溶剂体积减少了90%。压延烘干后的样品含水质量分数为0.06%~0.12%,低于过筛烘干法制备的样品。表明用压延烘干法制备样品,可以减少样品组分定量分析的总时间,并且可以减少废溶剂量。 相似文献
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报道了在没有有机溶剂加氯仿的条件下,烷基苯磺酸盐和烷基磺酸盐(AS)测定方法的进展情况。烷基苯磺酸盐和AS与钙盐经沉淀,然后经过过滤分离。通过这个过程,它们和体系中的无机含硫化合物分离。被分离物中的硫含量通过电感耦合等离子体原子发射光谱(ICP-AES)测定。这样可以测定总的阴离子表面活性剂的含量。AS通过高压水解,未水解的烷基苯磺酸盐用同样的方法测定。烷基苯磺酸盐、AS、磷酸盐、硅酸盐、硫酸盐和 相似文献
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Akihiko Kawauchi 《Journal of the American Oil Chemists' Society》1997,74(7):787-792
This paper reports the development of a method for measuring alkylbenzene sulfonates and alkyl sulfates (AS) without requiring
the use of chlorinated organic solvents, such as chloroform. Alkylbenzene sulfonates and AS are precipitated with calcium
and then isolated by filtration. Through this filtration process, they are separated from inorganic sulfur compounds. After
the precipitate is prepared, the level of sulfur is measured by inductively coupled plasma atomic emission spectrometry (ICP-AES)
to determine the total anionic surfactant level. Separately, AS are hydrolyzed in an autoclave, and the level of alkylbenzene
sulfonates is then measured in the same manner. By using the autoclave, a safe and rapid hydrolysis step has been achieved.
In addition to alkylbenzene sulfonates and AS, phosphate, silicate, sulfate, and zeolite can be determined with this sample
preparation. This sample preparation procedure was investigated by ICP-AES and was confirmed applicable for simultaneous measurements
of alkylbenzene sulfonates, AS, phosphate, silicate, sulfate, and zeolite without using organic solvents. Relative standard
deviation for the analysis is less than 1.7%, recovery is more than 99.0%, and the calibration curve gives a correlation coefficient
of R=1.000. The detection limit of this method for alkylbenzene sulfonates and AS is 0.6%, for zeolite, 0.04%, for phosphate,
0.4%, for silicate, 0.1%, and for sulfate, 0.2%, by weight in product. This method is applicable to various laundry detergent
products that contain the materials mentioned above and is 10 times faster than the six wet chemical methods normally used
to analyze these compounds. 相似文献
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Akihiko Kawauchi 《Journal of surfactants and detergents》1999,2(1):79-83
This paper reports the development of a method for measuring alkyl-benzene sulfonates, alkyl sulfates, and other inorganic
ingredients in laundry detergent products without requiring the use of chlorinated organic solvents such as chloroform. Zeolite
is first filtered as a residue on filter paper from an aqueous detergent solution. A calcium solution is then added to the
filtrate. Alkyl-benzene sulfonates, alkyl sulfates, and phosphate are precipitated as calcium salts and recovered as residues
via filtration. The filters are then subjected to X-ray fluorescence spectrometry (XRF) for measuring the levels of zeolite,
phosphate, and total anionic surfactant. The remaining filtrate is also subjected to XRF by using the microdroplet preparation
for measuring levels of sulfate and silicate. Separately, the level of alkyl-benzene sulfonates is measured following the
same XRF procedure after alkyl sulfates are hydrolyzed using an autoclave. This sample preparation procedure was investigated
using XRF and was confirmed to be applicable for simultaneous measurements of alkyl-benzene sulfonates, alkyl sulfates, zeolite,
phosphate, silicate, and sulfate without using any organic solvents. In the method described in this paper, interelement effects
between anionic surfactants and phosphate are not negligible. Fluorescent X-rays of sulfur or phosphorus are absorbed by calcium
complexes of phosphate or anionic surfactants. The slope of calibration curves varies with the levels of coexistent elements;
external calibration methods cannot be employed for unknown sample matrices. However, for quality assurance purposes, this
method is ideal in terms of turnaround time and laboratory hygiene. 相似文献
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利用有机溶剂提取微藻油脂的方法探究 总被引:1,自引:0,他引:1
在传统化石能源日益枯竭的趋势下,微藻生物柴油作为第三代绿色可再生的替代型能源越来越受到人们的重视.在微藻生物柴油的产业链上,油脂的提取是影响其推广应用的一个关键环节.本文实验利用有机溶剂提取微藻油脂,探究在不同的条件下微藻油脂的提取效果,并特别研究了先后使用甲醇和石油醚两种有机溶剂对微藻油脂提取率的影响.研究结果表明:温度、液料比、浸提时间对提取效率都有一定的影响,并且使用甲醇和石油醚两种溶剂分步提取时会使微藻油脂提取率明显提高;在液料比为15mL/g、提取温度为45℃、提取时间为5h时,使用石油醚作为提取剂的提取率为58.71%;使用甲醇溶剂提取后再使用石油醚提取时,在液料比和提取时间相同的条件下,温度为35℃时提取率即可达87.90% 相似文献
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褐藻糖胶的萃取和反萃 总被引:5,自引:1,他引:4
研究了无机盐种类和浓度对N263萃取褐藻糖胶的影响. 结果表明,无机盐浓度是影响褐藻糖胶萃取的最主要因素, 褐藻糖胶的萃取率随盐浓度的增加而迅速降低,在无机盐存在下,增加萃取剂浓度并不能增加对褐藻糖胶的萃取. 用盐水溶液反萃不同条件下萃取的褐藻糖胶,结果表明,反萃率随盐浓度的增加而增加,在相同的氯离子浓度下,钠盐的反萃效率优于钙盐,随有机相中褐藻糖胶浓度的增加, 盐的反萃效率降低. 比较了不同溶剂作为稀释剂对用盐溶液反萃褐藻糖胶的影响,表明CCl4作为稀释剂时盐的反萃效率最低. 相似文献
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以发烟硫酸作为磺化剂,选用C9催化重整烷基化重质产物为原料,在不同反应条件下合成一种石油三采用的表面活性剂重质烷基苯磺酸盐,确定了磺化反应的最佳条件。对产品进行红外谱图分析,结果表明磺酸根存在;通过石油醚萃取法测定未磺化油含量,从而计算磺化率;测定乙醇不溶物含量确定无机盐含量。通过中和滴定测定磺酸的中和值,从而得出反应产生的废酸量与磺化剂用量有关。此外,配制一系列浓度重质烷基苯磺酸盐溶液,测量了其表面张力,得到表面张力与产品溶液浓度之间的关系,并且得出其临界胶束浓度、饱和吸附量以及极限分子面积;采用两相滴定法测定重质烷基苯磺酸盐的平均相对分子质量,并确定其活性物含量。 相似文献
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溶剂萃取法从褐藻浸提液中分离提取褐藻糖胶 总被引:4,自引:0,他引:4
用溶剂萃取法分离提取了实际海藻浸提液中的褐藻糖胶. 考察了接触时间、溶剂加入量及萃取剂浓度等对萃取的影响,并与从多糖配制液中的萃取情况进行比较. 考察了无机盐水溶液反萃褐藻糖胶的性能及在溶剂中加入TOA(三正辛胺)对萃取和反萃的影响,结果表明,季铵盐从实际鼠尾藻浸提液中萃取褐藻糖胶受溶剂加入量的影响很大,溶剂加入量越大,萃取率越低;而萃取时间对萃取的影响不大. 海带浸提液的萃取优于鼠尾藻浸提液,而超声破碎法有利于萃取. TOA的加入既有利于褐藻糖胶的萃取也有利于无机盐水溶液反萃褐藻糖胶. 采用溶剂萃取法制备的固体褐藻糖胶的纯度优于乙醇分步沉淀法制备的固体褐藻糖胶的纯度. 相似文献
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Analysis of Petroleum Sulfonates The application of column chromatography using silica gel and ion-exchange resins has been studied for the separation of components of petroleum sulfonates present in technical products. The customary standard procedures based on extraction have been replaced by column chromatography, since the latter is more reliable and rapid. The various petroleum sulfonates and other products of sulfonation are differentiated by spectroscopic methods. 相似文献