一种测定油田含油污水中二氧化硅含量的方法

公开号:CN101368902公开日:2009.02.18申请人:辽河石油勘探局摘要本发明涉及油田化工样品分析的方法,尤其是一种测定油田含油污水中二氧化硅含量的方法。该方法基于钼酸盐与硅酸盐反应显色原理,在屏蔽油田含油污水中溶解的有机杂质对测定的干扰后,应用分光光度计比色分析油田污水中二氧化硅的含量:首先,以标准物质建立标准曲线,然后取适量的含油污水于比色管中加入盐酸、草酸溶液,用蒸馏水稀释即成空白溶液,测试时取污水样加入钼酸铵溶液,草酸溶液,以空白试验溶液作参比,测定吸光度,最后利用标准曲线和测定吸光度计算污水中二氧化硅含量值。该方法快捷、简单能有效屏蔽含油污水中有机杂质对测定的干扰,解决了含油污水测定的问题,为抽油锅炉合理使用污水提供了可靠保证。一种测定油田含油污水中二氧化硅含量的方法     

痕量苯胺的单扫描极谱法测定

１引言环境水样中痕量苯胺的测定多采用偶氮化色法，利用苯胺偶氮盐与羟基化合物偶合生成的偶氮化合物的吸附波间接测定苯胺的方法已有报道。作者观察到，在氨水－氯化铵介质中，８－羟基喹啉与苯胺重氮盐偶合生成的偶氮化合物在滴汞电极上于－０．７４Ｖ（ｖｓ．ＳＣＥ）处产生－灵敏的导数极谱波，苯胺浓度在０．００８～１．４０ｍｇ／Ｌ范围内与波高呈良好的线性关系，可用于痕量苯胺的测定，方法用于污水中痕量苯胺的测定，结果令人满意。２实验部分２．１仪器与试剂ＪＰ－２型示波极谱仪；三电极体系导数档；苯胺标准溶液：１００与１…     

多波长线性回归紫外吸光光度法同时测定炼油厂污水苯？…

提出用多波长线性回归紫外吸光光度法同时测定炼油厂污水中的苯酚和苯胺。方法省去了萃取，蒸馏，显色等步骤，操作简单，对合成水样进行测定，相对标准偏差≤４．５７％，相对误差≤±２．３％。对炼油厂水样进行测定并进行加标回收试验，苯酚和苯胺的回收率分别为９９．４％－１０３．０％和９７．２％－１０４．）％，结果良好，苯酚和苯胺的最低检出限分别为０．０１０和０．０４８μｇ．ｍｌ＾－１。     

卡尔曼滤波伏安法同时测定炼油废水中苯酚和苯胺的研究

炼油废水中主要含有石油类、苯酚和苯胺等物质。由于石油类、苯酚和苯胺等毒性极大，排放含这些物质的废水将对环境造成极大的污染，严重影响社会的可持续发展，故需测定炼油废水中这些物质的含量以便于处理控制。目前常用的测定石油类和苯酚的方法有石油醚萃取紫外分光光度法，CC14萃取红外光谱法和蒸馏4－AAP比色法。这些方法的主要缺点是水样预处理步骤繁琐，工作效率低，测定成本高，并且因使用有机溶剂而造成二次污染，危害测试人员的健康。此外，对于苯酚和苯胺含量较低的水样，由于萃取和蒸馏效率的制约，难以准确测量。我们用自制的蒙脱石－石墨－聚氯乙烯复合电极和卡尔曼滤波伏安法对模拟炼油废水中苯酚和苯胺进行了同时测定，取得了满意的效果，该法简单、准确、快速，具有较大的推广应用价值。     

水中油荧光在线测量系统研究

针对污水中石油类污染物的荧光特性和石油类污染物浓度之间关系,采用在线荧光光谱技术构建一个自动萃取式水中油荧光测量系统,实现对污水中石油类污染物含量的检测。测试结果表明:本系统可实现对污水中石油类污染物的自动检测;与传统的检测方式相比,本系统省去了取样和人工萃取等环节,可实现污水中石油类污染物的在线测量;针对该系统的测量误差,测试结果表明其满量程平均误差为1.8%,满足测量要求;针对系统的稳定性,测试结果表明其相对误差为1.8%。该测量系统可用于石油开采、石油炼制以及冶金等行业含油污水的在线检测。     

吸光光度法测定水中微量苯胺

苯胺类物质是制药、染料和纺织等工业的重要化工原料。这类物质毒性大，有明显的致癌作用。因其对环境和人体健康的影响极大，而被优先列人我国十四类环境污染物黑名单。因此，对苯胺类物质的测定是环境监测中一项十分重要的内容。简便的苯胺测定方法是偶氮比色法，常用的显色剂     

一种使荧光法与其它方法测得水中油含量有可比性的方法

使荧光法与其它方法测得水中油含量有可比性的方法，涉及工业废水的环境监测技术．具体是：对取样分组用荧光图谱测定的方法扫描图谱，同时采用通常的其它检测方法测量；对不同浓度的样品从低向高逐个测定，确定荧光值对含油浓度关系曲线；对照含油浓度曲线，在相同的条件下用荧光法直接测定无溶剂萃取水样的含油量。本发明使得用荧光法经萃取或不经萃取直接测得的水中石油类含量与重量法、红外法、紫外法、GC—MS等的测定结果之间具有可比性，从而使测定更经济、环保、高效、灵敏的荧光法在更大范围内得到推广应用，解决了在线监测水中石油类含量的关键性技术障碍。     

反萃取紫外分光法测定水中总酚和总苯胺

用现有的分析方法测定水中酚类和苯胺类,都有一定困难。我们建立了反萃取紫外分光法,其操作简便、测定迅速、灵敏度高,并能有效地排除干扰,适用于各种水质分析。 (一)方法原理苯酚和苯胺易溶于有机溶剂而难溶于水,因此我们可以用有机溶剂将苯酚类和苯胺类化合物从水中萃取出来;同时苯酚盐和苯胺盐易溶于水而不溶于有机溶剂, 又可用NaOH水溶液将苯酚类和用盐酸将苯胺类化合物从有机溶剂中反萃取出来。萃取前,将水样pH调至9.0,使其中所含苯甲酸、苯磺酸和醋酸生成盐以消除其干扰。萃取和反萃取,不仅有效地排除了干扰,起到浓缩作用,而且使酚类和苯     

阻抑动力学光度法测定痕量苯胺类化合物

研究发现，在醋酸介质中痕量苯胺能灵敏地阻抑H2O2和KBrO3氧化二甲苯兰FF褪色的指示反应。通过研究该反应的最佳实验条件及动力学参数，建立了一种测定痕量苯胺类化合物（以苯胺计）的新方法。本方法的测定范围为0．0～48．0μg/L苯胺，检测限低至3.62×10(-6)g／L苯胺，用于废水中苯胺类物质的测定，结果满意。     

加盐蒸馏同时富集分析污水中苯酚和苯胺

根据盐效应原理 ,研究了在pH =7 0± 0 5的中性介质中、大量氯化钠存在条件下加盐蒸馏 ,同时分离、富集水中微量苯酚和苯胺的实验方法。结果表明 ,2 50ml水样加入 1 50gNaCl,只须接取最初 50ml(水样体积的 1 5)馏出液 ,就可获得 93%左右的苯酚和 91 %以上的苯胺回收率。若同时辅之以紫外 4阶导数光谱法进行测定 ,经回收率校正后 ,可准确测定水中微量苯酚和苯胺。此方法可应用于各类污水中酚、胺的同时分离测定。     

自动电位滴定法测定炼油工业污水中的氯离子

介绍自动电位滴定法测定炼油工业污水中氯离子含量。炼油工业污水样品经加热煮沸、双氧水氧化等预处理后,通过调节使其pH=2～6,以硝酸银标准溶液为滴定剂,在自动电位滴定仪上进行电位滴定。试验表明,本方法可以用来测定带色度的炼油工业污水样品,且对样品的酸碱度无苛刻要求,过量的双氧水不影响测定结果,不同浓度的标准样品其测定结果与其标称浓度无显著性差异。     

Preconcentration and Quantitative Determination of Esomeprazole Magnesium Present in Water

A simple, accurate, and sensitive preconcentration method for determination of esomeprazole magnesium in treated sewage water was developed based on HPLC. A preconcentration method was developed for aqueous solution containing pure drug using solid phase extraction. Macroporous beads of polystyrene divinyl benzene (PSDVB) polymer were used for preconcentration followed by chromatographic determination. Experimental parameters were optimized. This optimized method can detect esomeprazole magnesium concentration up to 0.003 mg L^?1 after preconcentration. This method was used for determination of esomeprazole magnesium in water collected from a sewage treatment facility. Esomeprazole magnesium could not be detected in the treated sewage water sample collected for the study.     

Gas chromatographic analysis of phenylurea herbicides following catalytic hydrolysis on silica gel

Summary A method is described for the rapid catalytic hydrolysis of phenylurea herbicides on silica gel at elevated temperatures. After derivatisation of the anilines produced with heptafluorobutyric acid anhydride final analysis is done on a gas chromatograph equipped with an electroncapture detector. Detection limits are in the 1–5 picogram range. The method has successfully been applied to residue analysis of water samples at the 1 ppb level. The determination of free anilines present in water samples and the potential of various techniques to be used to discriminate between free anilines and parent herbicides are also discussed.     

ICP-MS multielement determination in fly ash after microwave-assisted digestion of samples

A microwave assisted digestion procedure has been developed for dissolution of fly ash samples prior to the inductively coupled plasma-mass spectrometric determination of their elemental composition. The developed methodology was validated by carrying out the analysis of two high-silicate containing reference materials (CRM 134R sewage amended soil and NIES JR 1 rock) and by means of the comparison between results found by microwave-assisted digestion and ICP-MS of fly ash samples with those found by neutron activation analysis (NAA) for Sb, Cs, Cr, Co, Fe, U and Zn determination. The method developed can be recommended for routine multielement analysis of fly ash.     

连续流动法同时测定污水中氨氮和总磷

采用连续流动分析法测定污水中氨氮、总磷的含量。比较了污水样品不同的稀释倍数对测定结果的影响。实验结果表明:氨氮和总磷的质量浓度在0.1~8 mg/L范围内线性良好,线性相关系数均为0.99997;测量结果的相对标准偏差分别为2.01%,0.84%(n=7);方法检出限分别为0.012,0.009 mg/L;质控样测量值均在标示值范围内;样品加标回收率为93.4%~101.1%。污水的洁净程度对测定结果影响较大。洁净度高的污水,直接测定与稀释后测定,测定值无显著性差异;而洁净度低的污水,直接测定与稀释后测定结果差异比较大。该法采用全谱直读CCD检测方式,灵敏度高,稳定性好,无光谱干扰,且支持氨氮和总磷同时测定,方便快捷,适合污水中氨氮和总磷的测定。     

催化柴油中氮化物分布的气相色谱-原子发射光谱分析方法的研究

建立了催化柴油馏分中各种氮化物类型分布的气相色谱-原子发射光谱(GC-AED)分析方法,考察了色谱条件和不同的试剂气压力对各种氮化物分离和检测灵敏度的影响,定性(或归类)了某典型催化柴油中的73个氮化物,计算了程升条件下各种氮化物的保留指数,为不同实验室的定性比较提供了依据。以峰面积对质量浓度作图,氮化物在2.0~600 mg/L浓度范围内,AED检测器对不同氮化物有良好的线性响应,线性相关系数达0.998。几种氮化物(吲哚、1-甲基吲哚、C2-吲哚、咔唑、1-甲基咔唑、1,8-二甲基咔唑)峰面积的相对标     

Determination of aromatic amines in water samples by capillary electrophoresis with electrochemical and fluorescence detection

Two capillary electrophoresis methods have been compared for the determination of aniline derivatives in environmental water samples. With the first method the anilines were separated as cations by free zone electrophoresis at low pH, and detected by amperometry. For this, the separation capillary was connected through a palladium field decoupler to an electrochemical detection cell which had been modified to match the volume scale of the separation. Most anilines tested, except chlorinated compounds, could be detected with full sensitivity at a detection potential of +0.7 V. Detection limits with this detection scheme were on a low microg/l level. The alternative method involved the derivatization of the anilines with fluorescamine, the separation of the derivatives formed by micellar electrokinetic chromatography, and fluorescence detection. For detection a lamp-based, fibre optics instrument was used. Detection limits with fluorimetry were comparable with those obtained with amperometric detection (in the order of 1 microg/l). Still, this method was preferred since it gave a higher separation efficiency and shorter analysis times (approximately 4 min). The most important argument, however, was its higher reliability and ease-of-handling. Preliminary experiments with water samples collected in areas where pollution with anilines may be expected showed that the method is highly specific, with few interferences showing up in the electropherograms.     

Simultaneous derivatization and extraction of anilines in waste water with dispersive liquid-liquid microextraction followed by gas chromatography-mass spectrometric detection

The one-step derivatization and extraction technique for the determination of anilines in river water by dispersive liquid-liquid microextraction (DLLME) is presented. In this method the anilines are extracted by DLLME and derivatized with pentafluorobenzaldehyde (PFBAY) in aqueous solution simultaneously. In this derivatization/extraction method, 0.5 ml acetone (disperser solvent) containing 10 microl chlorobenzene (extraction solvent) and 30 g/l pentafluorobenzaldehyde (PFBAY) dissolved in methanol was rapidly injected by syringe into 5 ml aqueous sample (pH 4.6). Within 20 min the analytes extracted and derivatized were almost finished. After centrifugation, 2 microl sedimented phase containing enriched analytes was determined by GC-MS. The effects of extraction and disperser solvent type and their volume, pH value of sample solution, derivatization and extraction time, derivatization and extraction temperature were investigated. Linearity in this developed method was ranging from 0.25 to 70 microg/l, and the correlation coefficients (R2) were between 0.9955 and 0.9989, and reasonable reproducibility ranging from 5.8 to 11.8% (n=5). Method detection limits (MDLs) ranged from 0.04 to 0.09 microg/l (n=5).     

Ag2SO4-CuSO4 催化-微波消解快速测定炼油污水中化学需氧量

以Ａｇ２ＳＯ４－ＣｕＳＯ４为催化剂,探讨了微波消解测定炼油污水中化学需氧量（Ｃｈｅｍｉｃａｌ Ｏｘｙｇｅｎ Ｄｅｍａｎｄ,ＣＯＤｃｒ）的方法。确定了微波消解测定炼油污水ＣＯＤｃｒ的最佳条件;消解功率、消解时间、混酸介质Ｈ３ＰＯ４－Ｈ２ＳＯ４用量、催化剂配比等。用该方法测定炼油水各处理装置出水 的ＣＯＤｃｒ,与经典的ＣＯＤｃｒ回流法所得结果一致。方法适用于临控生产过程。     

油田污水中聚丙烯酰胺(HPAM)的降解机理研究

随着聚合物驱油技术在我国油田的大面积推广,含聚丙烯酰胺污水的产量在逐年增加 .聚丙烯酰胺在为油田生产提高原油采收率的同时,也大幅度增加了混合液的粘度和乳化性 ,使油水分离难度加大,造成采出水含油量严重超标.含聚丙烯酰胺污水具有粘度高、油水分离难度大、可生化性差等特点,对环境的负面影响也越来越明显.因此,亟待解决的问题便是部分水解聚丙烯酰胺的降解.本文综述了聚丙烯酰胺化学、生物降解机理,总结了降解聚丙烯酰胺的典型的微生物种群,阐述了生物方法的优势,为油田含聚丙烯酰胺污水的处理研究提供参考.