当前位置: 其他 > 其他 > 方案详情

高分辨纳米粒度仪分析中前处理检测方案(激光粒度仪)

检测样品 其他

检测项目 其他

关联设备 共2种 下载方案

方案详情

采用美国MASS公司CHDF系列高分辨率纳米粒度分析仪进行样品的粒径分布测试前,样品应进行一系列的处理,文章对CHDF测试前的样品准备要求进行了讲解。

智能文字提取功能测试中

21 22 if the operator chooses to have the sample fractogram deconvoluted into its primary components (See SoftwareSection). Data Analysis The CHDF4000 determines the concentration of particles exiting the fractionation cartridge as a function oftransit time from injection. This data is compared to a calibration curve generated by measuring the transittimes of monodisperse polystyrene latex size standards. The raw data can be mathematically deconvoluted intocomponent peaks. From the deconvolution and the absolute calibration using the known size standards, theparticle size and size distribution are automatically determined. The user may also choose to not have the datadeconvolved. The CHDF4000 Operating Software automatically calculates and displays the weight average, area average,volume average, and number average particle size. In addition, the area, weight and number relative andcumulative particle size distributions along with the standard deviation, half height width, and the 25% and75% percentiles are available on hard copy in either tabular or graphical form. The raw data, which is theabsolute detector output,is available as well. It should be noted that both the theoretical foundation for CHDF and the calibration curve are for sphericalparticles. If your particles are rod shaped or platelets, then the size measured by CHDF will be an approximatespherical diameter. Distributions in size will still be absolutely determined, but no specific information will begiven on the aspect ratio of the particles. Sample Preparation The CHDF4000 requires 1 milliliter of sample at 0.1-5 volume %(actual injected volume is 100-200 pl). Theinjection valve sample loop volume is 25 pl for Capillary Columns and 5 pl for Packed Columns. The samplemust beaqueous based (non-aqueous applications may be possible in the future). The sample can be preparedin either of two ways; dilution of a concentrate or the addition of the disperse phase to the eluent. It isrecommended that the GR-500 be used for dilutions or making dispersions. The concentration of the dispersephase should be high enough to obtain good resolution and a favorable signal to noise ratio. This is particularlyimportant when trying to identify very small sub-populations. On the other hand, it should be kept low enoughto avoid particle aggregation or injection valve clogging problems. Do not run samples above 5 volume %orthis may clog the injection valve or damage the fractionation cartridge. The CHDF4000 can determine the complete particle size distribution over the entire specified size range.Polydisperse samples do not need special pretreatment. The standard size range is 5 nm to 1100 nm particlediameter. Other size ranges will be available in the future. The actual state of dispersion and the stability of the sample are important considerations for any particlecharacterization technique. The CHDF4000 measures the effective hydrodynamic particle size. An aggregatewill behave as a larger particle and will not be resolved into the smaller primary particle size. For somesamples this may cause discrepancies between CHDF and transmission electron microscopy (TEM). The standard CHDF4000 GR-500 eluent is designed for anionic dispersions. When diluting a concentrate, usethe GR-500 fluid as the diluent. This will help ensure a stable, well dispersed system. Most systems will beanionic when dispersed in GR-500. For specific systems, this can be checked using microelectrophoresis orelectro-acoustic ESA analysis. Problems may occur when diluting systems stabilized with cationic surfactants.For specific information regarding specific sample systems, please contact Mass Applied Science directly. Most samples will need to be sonicated before analysis. For many samples prepared by the dilution of aconcentrate, placing the sample container in an ultrasonic bath will be sufficient. For dispersing powders intoMass Applied Science liquids or when dealing with materials which may have a strong tendency to form aggregates, it will benecessary to use an ultrasonic probe immersed in the sample itself. In both cases, the objective is to prepare auniform dispersion in which the particles exist in the actual state of dispersion that you wish to characterize. The CHDF4000 requires that the sample be injected by syringe through an injection valve, or the sample maybe injected using an autosampler. In many cases it is necessary to filter the sample before injection to removecoagulum or outsize particles. Five-micron filters which attach directly to the end of the syringe arerecommended. These filters are available from Mass Applied Science. The standard eluent supplied for use with the CHDF4000 is designated GR-500 and is for anionic systems.Most materials will be anionic when dispersed in GR-500. The eluent consists of surface active agents in de-ionized water. GR-500 is supplied in the form of a concentrate which must be diluted 10:1 for use, e.g., 950 mlde-ionized water to 50 ml GR500 concentrate. GR-500 should be diluted with de-ionized. Care should alwaysbe taken when handling the GR-500 to avoid contamination. The eluent should be used within 3 days ofpreparation. The GR-500 concentrate should be used within six months of receipt. It should be keptrefrigerated. Matec supplies three types ofGR-500 eluent: 1X-GR500,2X-GR500, and LA-GR500. The appropriateconductivity ranges (uSiemens/cm) of final eluent solutions are 7-10 for 1X-GR500, 14-19 for LA-GR500, and22-27 for 2X-GR500. Each of these eluents can be used with any of the three types of cartridges available. Mostcommonly,2X-GR500 is used in conjunction with a C-202 cartridge. Both 2X-eluents produce the same resolution and use the same calibration curves. The 2X-GR500 contains 10milligrams/l sodium azide biocide; the 2X-GR500-LA eluent contains only 0.5 milligram/l sodium azide. As aresult, the 2X-GR500-LA eluent degrades faster due to bacterial growth. The shelf-life for these eluents is threedays for the 2X-GR500-LA, and one week for the 2X-GR500. The 2X-GR500 cannot be used at 200 nm UV-detection because of the high UV-absorption by sodium azide. . The 1X-GR500 provides higher particle resolution efficiency than the 2X-formulas. The upper particle sizelimit is lower with 1X-GR500. The 1X-GR500 contains 0.5 milligrams/l sodium azide. Its shelf life is threedays. NOTE: The CHDF4000 and the fractionation cartridge have been specifically calibrated for use with GR-500 eluentThe use of any other eluent will give erroneous results. Hudson St., Northborough,MA USA Mass Applied ScienceHudson St., Northborough,MA USAPh: email: colloid@matec.com; web: massappliedscience.com      测试前,CHDF4000高分辨率纳米粒度仪需要1毫升体积分数为0.1-5%的样品(实际注入体积为100-200µl)。毛细管柱的进样阀样品回路体积为25µl,填充柱的进样阀样品回路体积为5µl。样品必须是水性的(将来可能会有非水性应用)。样品的制备有两种方法:浓缩液稀释或向洗脱液中添加分散相。建议将GR-500用于稀释或分散。分散相的浓度应足够高,以获得良好的分辨率和良好的信噪比。在试图识别非常小的亚群体时,这一点尤为重要。另一方面,应将其保持在足够低的水平,以避免颗粒聚集或注射阀堵塞问题。不要让样品的体积分数超过5%,否则可能会堵塞进样阀或损坏分馏筒。     CHDF4000高分辨率纳米粒度仪可以确定整个指定粒度范围内的完整粒度分布。多分散样品无需特殊预处理。标准粒径范围为5 nm至1100 nm粒径。其他尺寸范围将在未来提供。  对于任何粒子表征技术来说,分散的实际状态和样品的稳定性都是重要的考虑因素。CHDF4000高分辨率纳米粒度仪测量有效流体动力颗粒尺寸。聚集体将表现为较大的颗粒,不会分解为较小的主要颗粒尺寸。对于一些样品,这可能会导致CHDF和透射电子显微镜(TEM)表现出的测试结果之间存在差异。  标准CHDF4000 GR-500洗脱液用于阴离子分散。稀释浓缩液时,使用GR-500液体作为稀释剂。这将有助于确保一个稳定、分散的系统。当分散在GR-500中时,大多数体系都是阴离子的。对于特定系统,可使用微电泳或电声ESA分析方法进行检查。稀释用阳离子表面活性剂稳定的系统时可能会出现问题。有关特定样品系统的具体信息,请直接联系MASS公司。  大多数样品在分析前需要进行超声波处理。对于通过稀释浓缩液制备的许多样品,将样品容器放置在超声波浴中就足够了。为了将粉末分散到液体中,或在处理可能具有强烈倾向形成聚集体的材料时,有必要使用浸入样品中的超声波探头。在这两种情况下,目标都是制备均匀的分散体,其中粒子以您希望表征的实际分散状态存在。  CHDF4000高分辨率纳米粒度仪要求通过注射器通过注射阀注射样品,或者使用自动取样器注射样品。在许多情况下,有必要在注射前过滤样品,以去除凝结物或超大颗粒。建议使用直接连接到注射器末端的五微米过滤器。这些过滤器可从Mass Applied Science获得。仪器介绍CHDF4000型号高分辨率纳米粒度仪通过毛细管流体分离技术,可对包含不同尺寸颗粒的混合乳液进行粒径分布分析及组分分析。其技术优势为:1、通过毛细管分馏,得到样品真实的PSD数据,无需对粒径分布的形状进行假设;2、在测试范围内提供完整、真实、详细的PSD数据;3、自动采样器自动分析,PSD测试结果与密度无关,适用于不均匀成分样品;4、样品测试体积小于1毫升,四个紫外波长同时检测,可分辨样品中的不同粒子。

关闭
  • 1/2
  • 2/2

产品配置单

上海胤煌科技有限公司为您提供《高分辨纳米粒度仪分析中前处理检测方案(激光粒度仪)》,该方案主要用于其他中其他检测,参考标准《暂无》,《高分辨纳米粒度仪分析中前处理检测方案(激光粒度仪)》用到的仪器有分馏法原液高分辨纳米粒度仪、CHDF4000高分辨率纳米粒度仪。

我要纠错

推荐专场

相关方案