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This article mainly established the analysis method to extract the oxine-copper residues in cucumber and soil with ion pair of antiphase HPLC and Ultrasonic-assisted solvent. This method mainly uses XBridge C18 column and UV detector by using waters phase of phosphatic buffered solution/acetonitrile (60:40, by vol) as mobile phase with 0.8 mL/min flow ratio and UV detection at 250 nm. The residue time was 4.71 minute. Accuracy, precision, and sensitivity of the method all satisfy the demands of pesticide residue analysis.

建立了黄瓜和土壤中喹啉铜的超声波辅助溶剂提取-反相离子对高效液相色谱法的残留分析方法,该方法使用XBridge C18色谱柱和可变波长紫外检测器,并以水相磷酸盐缓冲溶液-乙腈(体积比为60:40)作流动相;流速为0.8 mL/min;检测波长为250 nm;保留时间为4.71 min;该方法的准确度、精密度及灵敏度均满足农药残留分析的要求。

The ultrasonic-assisted solvent extraction and quantitative analysis of the oxine-copper residues in soil with ion pair of antiphase HPLC was established. This methods mainly uses XBridge C5 column and UV detector by using waters phase of phosphatic buffered solution/acetonitrile (60:40, by vol) as mobile phase with 0.8 mL/min flow ratio and UV detection at 245 nm. The residue time was 4.72 minute. The linear correlation of this method was 0.9987. The recovery rate was 76.2 to 108.7%. Comparatively standard deviation was 0.6 to 3.37%. The detection limits of method was 0.05 mg/kg.

建立了土壤中喹啉铜的超声波辅助溶剂提取-反相离子对高效液相色谱法的残留分析方法,该方法使用XBridge C18色谱柱和可变波长紫外检测器,并以水相磷酸盐缓冲体系-乙腈(体积比60:40)作流动相;流速为0.8mL/min;检测波长为245nm;保留时间为4.72min;线性相关系数为0.9987,回收率在76.2%~108.7%之间,相对标准偏差在0.6%~3.37%之间,对土壤的最低检出限为0.05mg/kg。

Methods Based on the sugar analysis of 10 tea polysaccharides, the mix of arabinose:galactose:glucose (1:1:0.5, mol ratio), which was the major sugar composition in tea polysaccharides, were applied to investigate the influence of sugar on the carbazole method and meta-hydroxydiphenyl method respectively.

采用气相色谱法分析了10种茶多糖样品单糖组成,考察了其主要的三种单糖组分组成的混合中性糖(1:1:0.5,摩尔比)对硫酸咔唑法、间羟联苯法两种方法测定糖醛酸含量的影响。

However, this polynomial regression model suffered from thecolor metameric problem. Herewith, to minimize the metamerism, a model was developed based on the principal component analysis and back-propagation artificial neural network for scanner spectral characterization, which could reconstruct more accurate spectrum in comparison with the related international experimental results.

但是,扫描仪的多项式回归色度特征化模型存在同色异谱问题,因此本文提出了基于主元分析法和神经网络技术实现扫描仪颜色光谱特征化的算法模型,解决了同色异谱的问题,并且获得了比国际上同类研究更高的图像光谱重构精度。

The effect of sleep improvement of the three dosages(570 mg/kg,1000 mg/kg and 2000 mg/kg)of Semen Ziziphi Spinosae was studied by the experiments of sleep-induced directly, prolonging sleeping time induced by pentobarbital sodium, affecting mouse sleeping rate under the threshold hypnogenesis dosage of pentobarbital sodium and affecting sleeping delitescence induced by tobarbital sodium. The content of 5-HT in the brain of mouse was measured by fluorescence assay.

通过直接睡眠实验、延长戊巴比妥钠睡眠时间实验、戊巴比妥钠阈下催眠剂量实验和巴比妥钠睡眠潜伏期实验,比较低、中、高3个剂量(570 ,1 000 及2 000 mg/kg)酸枣仁粉剂对小鼠睡眠的影响,并且用荧光法测定小鼠脑中 5-羟色胺含量。

Based on the previous literatures, the following major innovation works were carried out in this dissertation:(1) The derivatization reaction conditions of ephedrine and pseudoephedrine with sensitive derivation reagent in aqueous system were studied and two new methods were developed for the assay of them by microemulsion electrokinetic chromatography and micellar electrokinetic chromatography with LIF detection. The sensitivity and analysis times were greatly improved compared with the previous reports;(2) A new method of CZE with indirect LIF detection was developed for the simultaneous determination of six coumarin compounds (esculin, esculetin, isofraxidin, genistein, naringin and sophoricoside) with fluorescein as the probe. The proposed method enlarges the application range of LIF detector, and provides new approach for the analysis of certain compounds difficult to derivatize;(3) Based on the above research, an MEKC with indirect LIF detection method for the simultaneous determination of adenine and guanine in DNA extracts from fungus, maize and soybean was established;(4) A new method for the investigation of the complexes formed between human serum albumin and ampicillin sodium under the simulated physiology conditions using laser light scattering technique was developed.

该论文在综述前人工作的基础上,开展了如下未见文献报道的创新性的研究工作:(1)使用灵敏的衍生试剂对麻黄碱和伪麻黄碱在水体系中的衍生反应条件进行了系统研究,建立了微乳电动色谱-激光诱导荧光检测法和胶束电动色谱—激光诱导荧光检测法测定麻黄碱和伪麻黄碱的灵敏分析新方法,与以前的报道相比,灵敏度和分析时间均有很大改善;(2)使用荧光素钠作为背景荧光试剂,建立了同时分析测定六种黄酮类化合物(秦皮甲素、秦皮乙素、异秦皮定、染料木素、柚皮苷和槐角苷)的毛细管区带电泳—间接激光诱导荧光检测新方法,扩大了激光诱导荧光检测的应用范围,对难衍生化合物的分离分析提供了一种新思路和新途径;(3)以荧光素钠作为背景荧光试剂,建立了一种用于同时测定食品提取DNA中的腺嘌呤和鸟嘌呤含量的胶束电动色谱—间接激光诱导荧光检测新方法;(4)用动态和静态激光散射法研究了模拟生理条件下人血清白蛋白与氨比西林钠盐相互作用所形成的复合物,为药物分子与蛋白质的相互作用、药代动力学等的研究提供了一种新思路。

Methods: Determining paeoniflorin content by high performance liquid chromatography measurement conditions: mobile phase of acetonitrile -0.4% phosphoric acid solution (volume ratio 13∶87; detection wavelength 230 nm; flow rate 1.0 mL/min; and column temperature 25℃; and determining polysaccharide content by anthrone-sulfuric acid method. The extraction procedure of Langchuangling granule was measured, and the evaluated indexes were the rate of dry extra, contents of the paeoniflorin and the total polysaccharide with L9 (34) orthogonal test and preferential treatment of data.

采用高效液相色谱(high performance liquid chromatography,HPLC)法测定芍药苷含量[测定条件:流动相为乙腈-0.4%的磷酸水溶液(体积比为13∶87);检测波长230 nm;流速1.0 mL/min;柱温25℃];采用硫酸-蒽酮法测定总多糖含量,并以干浸膏得率、总多糖含量和芍药苷含量为指标,采用L9(34)正交实验,用综合评分法处理数据优选水提取工艺。

First of all, this study will be multi-walled carbon nanotubes by chemical oxidation process purified so it can be modified to deal with than the purification of purity before the modified 5 wt%, more than 1.89 times the surface area to increase the surface potential decrease of about 10 ~ 20 mV and the surface functional base (-COOH and-OH) to increase 1.45 times, and then the control technology of electroless preparation parameters include: analysis of plating time, plating analysis of temperature, metal ions in solution than the (Fe2+/ Ni2+), bath pH and the added value of dispersion Agent and other research towards Fe-Ni particles to increase the iron content and Fe-Ni particles spread in the MWCNT upper fixed targets,the results found that when the parameters for the preparation of 50 ℃, pH10, do not add dispersant, metal ions than the solution (Fe2 +/ Ni2 +) 7, the highest iron content can be Fe = 40.55 at%(flat iron content 111.17 mg / g) of nanocomposites Fe-Ni/CNT, then for a series of the nature of its analysis, the final evaluation Fe-Ni/CNT nanocomposites were processed on the effectiveness of the application of mixed pollutants, the results showed that in 120 minutes at the same time when Adsorption of heavy metal ions lead nitrate 10 ppm, selenium heavy metal ion degradation of 1 ppm and orange azo dye AO7 50 ppm standard of effluents, and after a total Fe-Ni nano-particles to SEM / EDS analysis of more than 50% still remaining.

本研究首先将多壁奈米碳管以化学氧化法做纯化改质处理能使其纯度较纯化改质前提高5 wt%、比表面积提高1.89倍、表面电位下降约10~20 mV以及表面官能基提高1.45倍,再控制无电镀技术之制备参数包括:析镀时间、析镀温度,镀液中金属离子比(Fe2+/Ni2+)、镀液pH值及是否添加分散剂等,研究朝提高Fe-Ni粒子的含铁量与Fe-Ni粒子散布固定在MWCNT上等目标进行,研究结果发现当制备参数为50 ℃、pH10、不添加分散剂、镀液金属离子比(Fe2+/Ni2+)7时,可得到最高铁含量Fe = 40.55 at%(单位铁含量111.17 mg/g)之奈米复合材料Fe-Ni/CNT,接著对其作一系列性质分析,最后评估奈米复合材料Fe-Ni/CNT对共处理混合污染物之应用效益,结果显示其在120分钟时能够同时吸附重金属硝酸铅离子10 ppm、重金属硒酸根离子1 ppm及降解偶氮橘色染料AO7 50 ppm达放流水标准,且共处理后奈米Fe-Ni粒子以SEM/EDS分析仍剩余50 %以上。

The results show that the sample prepared by coprecipitation method exhibits the highest activity and has the largest crystallite size, and after reaction for 140 min, 53.6% of rhodamine B is decolored; while for catalyst prepared by the citric acid complexation, the decoloration ratio is only 9.0%, though the latter has a higher surface area and smaller crystallite size than the former.

研究结果表明:这4种方法均能制备单一的钙钛矿型LaFeO3催化剂,其中,共沉淀法制备的催化剂具有最大的晶粒尺寸,最小的比表面积,仅为0.4 m2/g,显示出最强的光催化活性;在可见光照射下反应140 min,罗丹明B的脱色率达到53.6%。柠檬酸络合法制备的催化剂的比表面积最大,为8.1 m2/g,但其脱色率仅为9.0%。

The methods of ultrasonic decolor ization for corn gluten meal and low velocity electric distilling extraction were studied in the tests.

研究超声波处理法对玉米蛋白粉进行脱色的工艺条件和电动搅拌方式提取玉米醇溶蛋白的最佳提取条件,确定最佳脱色条件是:以无水乙醇为溶剂,萃取温度50℃,料液比1:12,超声波处理25min;最佳提取条件是:料液比1:8,50℃水浴加热,低速搅拌提取3h,乙醇的浓度是75%。

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