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1.
对于通用型酚醛树脂和专用型酚醛树脂,其游离酚的分析方法通常采用容量法。但对碳素材料专用酚醛树脂,由于在生产时添加氯化苄对酚醛树脂进行改性,使树脂能浸润碳素材料的中心。这种树脂的生产过程控制和产品质量检验时,涉及游离酚、氯化苄和苄醇的分析测定,如果采用分别测定,其操作相当繁琐,准确性也不高。在常规方法蒸馏苯酚的过程中,氯化苄和苄醇也会被蒸馏出来,蒸馏出来的氯化苄和苄醇对苯酚的容量分析有干扰。在此基础之上,对氯化苄、苄醇和苯酚的蒸馏进行回收率测定,结果表明回收率满足要求。因此,本文建立了气相色谱法同时测定碳素材料专用树脂中的氯化苄、苄醇和苯酚的分析方法。即采用与容量分析方法一样的样品前期处理(酒精溶解样品、水浴蒸馏),使游离酚、氯化苄和苄醇同时与树脂分离后,采用气相色谱法测定。本方法使测定步骤简化,可用于氯化苄改性的专用酚醛树脂的科研和生产控制。  相似文献   

2.
建立气相色谱外标标准曲线法测定酚醛树脂中游离苯酚的含量。采用DB–5(30 m×0.25 mm, 0.25μm)色谱柱,程序升温,气化室温度为250℃,以火焰离子化检测器(FID)检测,检测器温度为280℃,以标准曲线外标法计算游离苯酚含量。苯酚的质量浓度在0.05~10.0 mg/mL范围内与色谱峰面积呈良好的线性关系,线性相关系数(r)为1,方法检出限为0.003 7 mg/mL。样品加标回收率为98.0%~102.0%,测定结果的相对标准偏差为1.07%~1.26%(n=6)。该方法简单、快速,测定结果准确、可靠,可用于酚醛树脂中游离苯酚含量的检测。  相似文献   

3.
王娟  赵彤 《高分子学报》2012,(2):103-110
酚醛树脂分子量及分布的表征方法有很多,如蒸气压渗透法(VPO)、气相色谱、高压液相色谱和凝胶渗透色谱等,但由于酚醛树脂存在众多异构体,这些方法均有一定限制性.场解吸质谱(FD-MS)方法的特点是只给出样品固有组分的分子峰,不产生碎片离子峰,用于酚醛树脂的表征,可以直接得出树脂所有固有组分的分子离子峰值,及树脂不同缩合度组分的相对含量,非常适用于组份繁多的酚醛树脂的的分子量及分布表征研究.以苯酚、甲酚及甲醛等原料分别制备了Resole型苯酚-甲醛树脂、Novolac型苯酚-甲醛树脂、Novolac型甲酚树脂及混酚-甲醛树脂,利用FD-MS对制备的几种不同类型酚醛树脂的分子量及分布进行了研究.结果表明,通过FD-MS谱图分析还可以得到树脂缩聚程度、原料种类、树脂特性等信息,对于鉴别及剖析各种类型酚醛树脂方便有效.  相似文献   

4.
酚醛树脂因其材料成本低、工艺简单、原料易得等优点,在工业上得到了广泛应用。但由于其耐热性不足以及游离酚含量较高等因素,限制了其应用范围。本文利用硼酸对酚醛树脂进行改性,利用红外和质谱对其结构进行表征,改性后酚醛树脂的耐热性能、游离酚等指标得到明显改善。当失重20%时酚醛树脂改性前后耐热性能提高了56℃,可能是由于硼酚醛树脂中含有硼的三维交联网状结构,提高了树脂的交联密度;游离酚含量从改性前的4.12%降低到了2.21%,说明硼元素的引入改变了苯酚的活性,提高了树脂聚合度。  相似文献   

5.
探讨生物质液化制备酚醛树脂的液化条件、树脂化条件及其性能,分析了生物质的液化率、残渣率,生物质酚醛树脂的红外谱图、粘度、残余酚含量、复合材料拉伸性能等实验数据。研究结果表明,不同生物质对液化条件的要求各不相同,其中竹粉的最佳液化条件是以苯酚重量5%的硫酸为催化剂,反应时间为60 min;同样液化条件下,生物质液化物合成酚醛树脂的树脂化条件相近,每10 g生物质液化物盐酸催化剂添加量为0.6 mL,反应时间为30 min;在最佳实验条件下,竹粉酚醛树脂的各项综合指标最佳,相对粘度最大、液化率最高、残渣率最低、残余酚含量低,其与玻璃纤维布复合的拉伸弹性模量经向和纬向分别是1 508.56 MPa和1 161.40 MPa,大大提高了基底材料性能,使材料刚度更好;通过红外谱图研究发现,不同生物质液化物制备的酚醛树脂结构相同,说明生物质液化物可替代苯酚作为原料与甲醛进行树脂化反应,大大降低了生产成本,减少了苯酚对环境的污染。  相似文献   

6.
直接进样-气相色谱法分析发酵液中的脂肪酸   总被引:5,自引:0,他引:5  
齐凤兰  韩英素  赵金海 《色谱》1987,5(6):382-384
在酒醅中加入己酸发酵液进行混合发酵是提高白酒风味的有效措施之一。其加入量需根据发酵液中己酸含量而定。这就需要准确地测定发酵液中各酸的含量。 测定脂肪酸的方法很多,一般有比色法,柱色谱法,纸色谱法及目前常用的气相色谱法。比色法只能测单个酸,不能测定混合酸。柱色谱法和纸色谱法分离时间长,试剂用量大,准确度低,重现性差。气相色谱法分析脂肪酸一般采用衍生化法,其中包括甲酯化法、乙酯化法、丁酯化法和苄酯化法,对于己酸发酵  相似文献   

7.
本文报道树脂法从混合物中分离纯化邻硝基苯甲醛的方法。研究说明,通过伯胺树脂与醛的反应对邻硝基苯甲醛进行化学吸附,可以将邻硝基苯甲醛从含有邻硝基甲苯、邻硝基苯甲醛、邻硝基溴苄、邻硝基-α,α─二溴苄、以及邻硝基苄醇的混合物中有效地分离出来。  相似文献   

8.
气相色谱法快速测定白酒与发酵液中的低沸点有机酸   总被引:2,自引:1,他引:2  
胡家元  李家明 《色谱》1993,11(2):87-88
测定白酒和发酵液中有机酸含量,对指导酿酒生产具有重要意义。气相色谱法测定上述试样的低沸点有机酸,常用的有直接进样法和苄酯化等法。直接进样法仍需对样品进行一定处理,而且不能测定响应信号极小的甲酸以及对酒的风味与发酵过程有着重要影响的乳酸含量。苄酯衍生化法因使用毒性催泪试剂苄基溴而未能广泛应用。本文采用四甲基氢氧化铵中和上述试样中的各酸使之生成相应酸的四甲基铵盐,蒸发除去水与其它成分后,在偶极  相似文献   

9.
气相色谱法测定酚醛树脂中的氯化苄   总被引:1,自引:1,他引:0  
氯化苄在有机工业中得到广泛应用,是生产碳素材料专用酚醛树脂的原料之一,酚醛树脂产品中氯化苄的含量必须通过测定加以控制。通常氯化苄的测定方法主要有重量法和气相色谱法等。由于树脂大分子和氯化苄分子较难分离,直接采用气相色谱法测定其中的氯化苄困难较大。本文用酒精溶解碳素材料专用酚醛树脂,加一定量的水作为混溶剂,然后用氯仿萃取其中的氯化苄,萃取分离后的氯化苄等物质,再用气相色谱法分离,测定结果满意。  相似文献   

10.
应用库仑滴定法测定了新洁尔灭溶液中溴化苄烷铵的含量。用0.09mol·L-1硝酸溶液和0.5%(w)明胶溶液以体积比10比1混合的混合溶液作电解液,银棒作阳极进行恒电流电解,电解电流为10mA。电解过程中,从银电极释放出的Ag+与试液中溴化苄烷铵的Br-反应生成沉淀。Br-被完全沉淀时,电流上升,滴定到达终点,根据法拉第定律计算溴化苄烷铵的含量。溴化苄烷铵的质量浓度在0.422 8~1.480g·L-1范围内与所消耗的电量之间呈线性关系。对同一样品的分析,本方法的测定结果与四苯硼钠滴定法的测定结果相符,本方法测定结果的相对标准偏差(n=6)为0.9%。用标准加入法进行回收试验,测得回收率在99.6%~102%之间。  相似文献   

11.
国内光催化研究进展简述   总被引:4,自引:0,他引:4  
郑云  潘志明  王心晨 《催化学报》2013,34(3):524-535
分1975~1985, 1985~1995和1995~2012三个时期简要介绍了国内光催化研究进展, 主要侧重于光催化材料及其改性、应用和反应机理方面的研究进展, 并指出了当前光催化领域存在的一些重要问题和未来的发展趋势, 涉及到光解水、CO2还原、环境净化和选择性有机合成等方面.  相似文献   

12.
青蒿素研究进展   总被引:20,自引:0,他引:20  
青蒿素是目前治疗疟疾的特效药。本文对自青蒿素发现以来的最新研究进展进行了比较详尽的综述。内容包括: 青蒿素的发现及历史, 青蒿素的来源, 青蒿素的全合成,青蒿素的生物合成, 青蒿素衍生物以及植物组织培养生产青蒿素。  相似文献   

13.
The toxicity of inorganic trivalent arsenic for living organisms is reduced by in vivo methylation of the element. In man, this biotransformation leads to the synthesis of monomethylarsonic (MMA) and dimethylarsinic (DMA) acids, which are efficiently eliminated in urine along with the unchanged form (Asi). In order to document the methylation process in humans, the kinetics of Asi, MMA and DMA elimination were studied in volunteers given a single dose of one of these three arsenicals or repeated doses of Asi. The arsenic methylation efficiency was also assessed in subjects acutely intoxicated with arsenic trioxide (As2O3) and in patients with liver diseases. Several observations in humans can be explained by the properties of the enzymic systems involved in the methylation process which we have characterized in vitro and in vivo in rats as follows: (1) production of Asi metabolites is catalyzed by an enzymic system whose activity is highest in liver cytosol; (2) different enzymic activities, using the same methyl group donor (S-adenosylmethionine), lead to the production of mono- and di-methylated derivatives which are excreted in urine as MMA and DMA; (3) dimethylating activity is highly sensitive to inhibition by excess of inorganic arsenic; (4) reduced glutathione concentration in liver moderates the arsenic methylation process through several mechanisms, e.g. stimulation of the first methylation reaction leading to MMA, facilitation of Asi uptake by hepatocytes, stimulation of the biliary excretion of the element, reduction of pentavalent forms before methylation, and protection of a reducing environment in the cells necessary to maintain the activity of the enzymic systems.  相似文献   

14.
Electrochemistry is one of the most advanced techniques for monitoring neurochemical activities in the living brain because electrochemical approaches bear the advantageous features of high spatial and temporal resolutions, which facilitate its tremendous potential in investigating the highly spatially heterogeneous brain system and the fast dynamics of neurochemical activities. On the other hand, since brain is the most complicated organ in the sense of its numerous kinds of neurochemical species, high selectivity is always required for any analytical methods that approach the brain. In this review, we will discuss various electrochemical methodologies to achieve selective detection of neurochemicals in mammalian brain and the strategies developed mainly by our group towards selective monitoring of both electrochemically active and inactive neurochemicals. At the end, we will discuss possible solutions towards brain mapping of neurochemical species and combination of neurochemical detection strategy with electrophysiology as the direction of future development of electroanalysis in living brain.  相似文献   

15.
Neutron activation analysis (NAA) is a very sensitive and accurate multielement analytical method that is widely applied to the investigation of environmental and archaeological problems. The first part of this paper is a review of pollution studies of toxic trace elements in sediments, seawater and marine organisms of Saronikos Gulf, Greece by NAA. The second part of this paper is a review of provenance studies based on minor and trace element research in ancient ceramics, obsidian, flint, limestone, marble and lead by Instrumental NAA, performed at the NCSR Demokritos.  相似文献   

16.
17.
Contento NM  Branagan SP  Bohn PW 《Lab on a chip》2011,11(21):3634-3641
In situ generation of reactive species within confined geometries, such as nanopores or nanochannels is of significant interest in overcoming mass transport limitations in chemical reactivity. Solvent electrolysis is a simple process that can readily be coupled to nanochannels for the electrochemical generation of reactive species, such as H(2). Here the production of hydrogen-rich liquid volumes within nanofluidic structures, without bubble nucleation or nanochannel occlusion, is explored both experimentally and by modeling. Devices comprised of multiple horizontal nanochannels intersecting planar working and quasi-reference electrodes were constructed and used to study the effects of confinement and reduced working volume on the electrochemical reduction of H(2)O to H(2) and OH(-). H(2) production in the nanochannel-embedded electrode reactor output was monitored by fluorescence emission of fluorescein, which exhibits a pH-dependent emission intensity. Initially, the fluorescein solution was buffered to pH 6.0 prior to stepping the potential cathodic of E(0)' for the generation of OH(-) and H(2). Because the electrochemical products are obtained in a 2:1 stoichiometry, local measurements of pH during and after the cathodic potential steps can be converted into H(2) production rates. Independent experimental estimates of the local H(2) concentration were then obtained from the spatiotemporal fluorescence behavior and current measurements, and these were compared with finite element simulations accounting for electrolysis and subsequent convection and diffusion within the confined geometry. Local dissolved H(2) concentrations were correlated to partial pressures through Henry's Law and values as large as 8.3 atm were obtained at the most negative potential steps. The downstream availability of electrolytically produced H(2) in nanochannels is evaluated in terms of its possible use as a downstream reducing reagent. The results obtained here indicate that H(2) can easily reach saturation concentrations at modest overpotentials.  相似文献   

18.
李菊仁  何兴涛 《合成化学》1993,1(4):296-303
报导了近几十年来国内外关于乙基香兰素的研究进展与动态,并简单介绍了本文作者在该方面所取得的研究成果,参考文献33篇。  相似文献   

19.
Reactions in droplets in microfluidic channels   总被引:5,自引:0,他引:5  
Fundamental and applied research in chemistry and biology benefits from opportunities provided by droplet-based microfluidic systems. These systems enable the miniaturization of reactions by compartmentalizing reactions in droplets of femoliter to microliter volumes. Compartmentalization in droplets provides rapid mixing of reagents, control of the timing of reactions on timescales from milliseconds to months, control of interfacial properties, and the ability to synthesize and transport solid reagents and products. Droplet-based microfluidics can help to enhance and accelerate chemical and biochemical screening, protein crystallization, enzymatic kinetics, and assays. Moreover, the control provided by droplets in microfluidic devices can lead to new scientific methods and insights.  相似文献   

20.
Russian Chemical Bulletin -  相似文献   

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