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AccuSizer 780 AD 多功能自动计数粒度仪


  • Single Particle Optical Sizing

    The AccuSizer 780 uses the method of single-particle optical sizing   (SPOS) to quickly count and size a large number of particles, one at a   time, thus constructing the true particle size distribution (PSD).   This approach is in sharp contrast to "ensemble" methods, such as   laser   diffraction and sedimentation, which must process information   produced simultaneously by many particles. These alternative   techniques require the use of complex mathematical algorithms to   invert the data and yield only rough approximations of the PSD, with   limited accuracy and very   poor resolution. The AccuSizer determines   PSDs with resolution and   accuracy comparable to those produced by the   classical resistive-pore, or electrozone, method. The 780 does not   miss the "details", which are often critically important in   determining the quality of many products. A wider size range, higher   count rate, compatibility with any liquid or gas, and relative   immunity to clogging make it an instrument in a class all its own.

    The   SPOS particle sizing method requires that concentrated suspensions be diluted, in order to eliminate particle coincidences in the sensing   photozone. Excessive dilution results in too low a count rate and poor statistical accuracy of the PSD, while overly concentrated suspensions     produce distortions in the distribution. The AccuSizer 780 uses   AutodilutionPat, which quickly and automatically dilutes the starting     sample to the optimum concentration, resulting in efficient and accurate     analysis. Trial-and-error manual dilution is eliminated, paving the   way   for single-keystroke operation; a complete analysis and flush   cycle can   be completed in less than 3 minutes.

    The   780*s single particle sensitivity detects the important features in   the size distribution which other techniques usually miss. Single   particle optical sensing makes the measurement accurate, while   AutodilutionPat and leading-edge electronics make it fast and easy to   use. Trading off accuracy and resolution for speed and ease of use no   longer have to be   made with the AccuSizer 780.

    The   AccuSizer 780 delivers reliable size and count data for even the   largest particles.A few outliers can spell the difference between   product success and failure; however traditional laser diffraction   particle size analyzers cannot detect large particle outliers in a sea   of smaller particles.The AccuSizer 780 reveals particle size   differences that previously went unnoticed.The 780 is a stable,   sensitive instrument that uses Single Particle Optical   Sizing (SPOS)   to count and size particles one at a time, eliminating   missed   particles while allowing:

    • Particle sensitivity of 10 PPT

    • Particle size accuracy of 2%

    • Particle count accuracy of 10%

    Recently,an independent study proved that SPOS analyzers were 1,500 to 25,000     times more sensitive in detecting outliers than light scattering and accoustical sizing instruments.

    The   AccuSizer 780 can also resolve fine particle distributions that are   directly related to the materials' properties. It is a proven and   valuable tool that laboratories around the world are   already using to   reformulate their product lines from R&D to production.

    A modular solution to meet your most challenging applications

    The   AccuSizer 780 AD Autodiluter is the cornerstone of the modular family   of instruments. The AccuSizer 780 AD incorporates a series of wide dynamic range sensors with a single stage exponential diluter to provide   a flexible high resolution, accurate, sensitive particle sizer. It     provides particle size information with unprecedented resolution and accuracy. It is especially suited to providing information on particle size distributions (PSDs) that are on scale but is not limited in the statistical information that it can provide on tails of mostly   submicron distributions. This patented module eliminates the need for   manual dilution of concentrated samples. Autodilution makes particle   size  analysis quick and easy, with no training required. Results are   highly reproducible.

    AccuSizer 780/APS Automatic Particle Sizer

    APS.jpg

     

    The   APS has been called the bolder detector by many of our customers     because of its ability to detect low levels of aggregates several     standard deviations away from the mean of the distribution. Often these     aggregates are the difference between a good and bad sample. One     independent study showed the APS was 1,500 to 25,000 times more     sensitive in seeing outliers in the CMP slurry than commonly used laser     light scattering and acoustical sizing instruments. The same   sensitivity   will apply to other applications such as inks, pigments,   drug emulsions   where a few large particles spell the difference   between success and   disaster.

    AccuSizer FX Focused Extinction

    AccuSizer FX- right angle (2).jpg

    The   AccuSizer FX is a new breed of particle size monitoring system   designed to go from the R&D lab to the process line with minimum   system   reconfiguration. The FX utilizes a patented focused beam   technology that   allows the sensor to focus on a specific area of the   flow channel to count and size individual particles at concentration   levels that are   hundreds of times higher than traditional sensors.   Although this type of   approach has been tried by other techniques it   has been plagued by low   resolution and accuracy. The new FX sensor   technology utilizes a   patented electro-optical configuration that   maintains the same levels of   resolution and accuracy found in   traditional SPOS sensors.

    The AccuSizer 780/LVS Large Volume Sizer

    6371304098666175116681927.png

    The   AccuSizer 780/LVS Large Volume Sizer is specifically designed to     analyze large volumes of liquid with particles as large as 2000   microns.   Often it is imperative to pass large amounts of diluted   dispersion   through an SPOS sensor. The key to the AccuSizer LVS system   is its large   volume dilution chamber that combines the ease of use of   autodilution   with the speed of a quick flushing fluidics system.
             The   AccuSizer 780/LVS allows the user to introduce a spoon   full of material   into the large volume dilution chamber and   immediately start taking   data. Ease of use of a fully automated   dilution system is combined with   SPOS to provide fast, high   resolution, high sensitivity particle size   distributions.

    AccuSizer 780/SIS Syringe Injection Sampler

     

    780 SIS-2.jpg

    When   volumetric sampling is paramount,   the SIS sampler fits the bill. With   syringes ranging from 0.5 to 25 ml   and a precision stepper motor with   over 25000 steps per pull the SIS   sampler is a perfect addition to the   family of modular instruments. It   is specifically suited to applications   in the pharmaceutical industry   such as USP <788> small and large   volume injectables. Now   available for use with the AccuSizer 780/SIS is   21 CFR Part 11   compliant software, Calibration and Validation SOPs.


    AccuSizer 780/OL Online

    Our     patented Autodilution technology has allowed us to take our   laboratory   instrumentation known for high precision, accuracy,   resolution and   reproducibility,and carry it to the

    process     line. Simple customizable computer controlled fluid-sampling devices     are used to grab a precise aliquot of concentrated in-line dispersion     and automatically inject it into the Autodilution system. Then, just as     in our laboratory systems, the sample is diluted to the optimal     concentration for an SPOS measurement, without regard to its initial     concentration or particle size distribution (PSD). The resulting PSDs,     with unique single particle resolution are identical to those that     historically could only be obtained in the research laboratory. No     longer must correlation algorithms and complex statistical tools be     developed to compare laboratory findings with online results.

    The     Autodilution module is an integral part of both of our laboratory     instruments- the AccuSizer 780 Single Particle Optical Sizer and the     Nicomp 380 Submicron Particle Sizer. These laboratory instruments have     been modified to meet the rigors imposed by online process monitoring.     They have been redesigned utilizing ruggedized com-ponents and are     housed in different classes of NEMA enclosures, depending on the     application. These vary from dust and waterproof enclosures to     explosion-proof modules that can handle even the most aggressive     environments, including high pressures and sub-zero temperatures.

    Multi-port     systems are available with specialized software to monitor multiple     points in an online process. These reduce costs while maximizing     coverage to ensure that quality control requirements are met. Users have     a choice of using either an embedded mode Windows based controller or   a   Programmed Logic Controller (PLC) which are often found in process     control systems. In either case the resulting data can be displayed on     screen or passed to a Laboratory Information Management System (LIMS)   as   an ASCII file. It provides for limitless posbcapture data analysis   that   can easily be customized by the user with common programs found   on all   modern computer systems.

    The     AccuSizer 780/OL system is able to detect minute amounts of oversized     particles in the tail of the process dispersion. It has produced   results   where the difference between a good and bad sample is   determined by a   few hundredths percent in volume fraction above a   particular critical   particle diameter, several standard deviations   above the main peak of   the distribution. It is also able to detect   very small percentages of   “fines” in the presence of larger particles.   These fines often play an   important role in determining the   viscosity, flowability and other   characteristics of both the process   dispersion and the final product.


  • 工作原理

    目录结构:

    1.单颗粒光学传感技术简介 

    2.传统光阻法和光散法测量粒度的原理

    3.PSS的SPOS技术介绍

    4.自动稀释原理介绍


    1、单颗粒光学传感技术简介

          单颗粒光学传感技术(Single Particle Optical Sizing, SPOS)是一种用于测量溶剂中悬浮粒子的大小和数量浓度的激光粒度检测通用技术。在SPOS技术中液体悬浮液中的粒子流经传感器的样品池时,在激光光源的照射下,被阻挡或者被散射的光会转变成脉冲电压信号,脉冲信号的大小是由粒子的截面面积和物理判定规则即光散射或者光阻共同决定的。光阻也被称为不透光度或者光消减。而粒子间的相互阻挡和散射是和粒子的大小和浓度是有关系的,利用脉冲幅度分析器和校准曲线便可以得到悬浮粒子的数量浓度和粒度大小分布。传统光阻法可以测得1.5μm以上的粒子和并具有较高的分辨率。

          单颗粒传感技术(SPOS)填补了常见粒度仪检测技术在检测粒径分布中的重要不足—粒子数量的统计。自AccuSizer 780系列仪器诞生,以往以牺牲精确性和分辨率来换取检测速度和易用的历史一去不复返!

    粒粒皆清楚,不丢失任何细节。


    2.传统光阻法与光散射法原理

    图片6.png

    Figure 1 光阻法检测示意图

          图1为光阻法检测原理图,待测液体流过横截面很小的流通池,流通池两侧装有光学玻璃,激光器的光束通过透镜组准直,光束穿过流通池并被光电探测器所接收。若待测液体中没有颗粒,则光电探测器接收到的光信号稳定不变,输出的电压信号也恒定,将此恒定信号作为基准电压;若液体中有颗粒物质,颗粒通过流通池传感区域,将会遮挡激光,光电探测器接收到的光信号减小,产生一个负的脉冲电信号,如下图2所示。

    图片7.png

    Figure 2 光电二极管信号

          脉冲信号幅度与基准电压信号有如下关系:

                           图片11.png                (1)                        

          式(1)中:E为颗粒遮挡引起的脉冲幅度;a为颗粒的有效遮挡面积(等效为球形);A为光电探测器的有效面积;E0是没有颗粒时的光电探测器所产生的基准电压。因此,脉冲信号幅度对应颗粒的大小,脉冲信号个数对应颗粒的数量。


    图片8.png

    Figure 3 光散射法检测原理图


          图3为光散射法检测原理图,待测液体流过流通池,流通池两侧装有光学玻璃,激光器的光束通过透镜组准直,光束穿过流通池,照射在光陷进上。若待测液体中没有颗粒,则光电探测器就收不到光信号,若液体中有颗粒,颗粒通过流通池,与激光光束发生散射现象。某一个(或几个)角度下的散射光通过透镜收集汇聚到光电探测器上,产生正的电信号脉冲,脉冲信号的幅度和散射光强成正比。根据信号的幅度和个数可以对液体中的微小颗粒进行计数检测。

          当光束照射含有悬浮微粒的液体时光能减弱。根据文献, 此时悬浮液中微粒会对光产生散射和吸收等作用,因为这些作用导致的光强减弱与微粒的浓度存在线性关系。在文献中引用了如下公式,来描述当微粒浓度较小时,透射光强与入射光强之间的关系:

                                        1577260612(1).jpg

          它对应于因为散射和吸收而导致光的衰减总量。有米氏散射的理论,随着微粒的增大,光强大量集中于前向0度角附近,图1中我们也可以注意到这一点。(4)式中没有考虑到这样的事实:在光阻法检测中,前向0角度附近的散射光仍然能够被探测器接收,因此必须考虑对散射系数进行修正。实际中(4)式变为:

               1577260670(1).jpg                   

    3.PSS单颗粒光学传感技术简介

          经过光感区域的粒子由于大小不同,光强随之产生相应的变化。将探测器收集的光信号转换成电压信号,不同的电压信号对应不同的粒径大小,从而得到微粒的粒径。美国PSS粒度仪公司(Particle Sizing Systems)的单颗粒光学传感技术(Single Particle Optical Sizing,SPOS)是在传统光阻法(LE)大颗粒光学传感技术的基础上加入了激光散射模块(LS)。在两个模块(LE+LS)同时运行的情况下,检测下限由原来纯光阻的1.5μm下探至0.5μm。使得其在大颗粒检测领域的应用更加的广泛。

          SPOS技术对粒子的信号响应方式是信号与特定粒子相对应的。AccuSizer 780系列仪器中的传感器通过两种不同性质的物理作用:光消减(light extinction, LE)与光散射(light scattering, LS)对通过传感器的粒子进行测定。光消减技术检测通过流动池的光强变化,拥有检测粒子的粒径范围广且与粒子组份无关等优点。然而,它的灵敏度有限。另一方面,光散射技术具有相对窄的动态粒径范围 (取决于检测器/放大器的饱和值),但能检测到小粒径的粒子,使用大功率激光光源还能检测到粒径更小的粒子。通过合并光消减和光散射响应信号,传感器可同时拥有这两种方法的优点,因而在不损失单粒子分辨率巨大优势的前提下拥有相对较广的动态粒径范围。

    图片9.png


    4. 自动稀释原理介绍

          单颗粒光学传感技术(Single Particle Optical Sizing, SPOS)虽然具有独特的量化粒度分布的优点,但是相应的粒子间的重合效应会造成检测结果不准。PSS粒度仪使用自动稀释机制,可以将样品稀释到目标浓度,然后再采集数据,保证粒度可以以“single”状态通过传感器,从而实现高浓度样本的检测。

          系统可以根据稀释倍数自动计算给出原样品颗粒浓度,解决了高浓度样品的检测难题,适合测试其他技术手段无法检测高浓度样本,更加适合测量样品量稀少且珍贵的样品。

    图片2.png


    图5 自动稀释原理图




  • 分析方法及原理

    光阻法(基于单颗粒光学传感技术)

    光阻+光散法(基于单颗粒光学传感技术)

    测量范围(传感器可选)

    0.5-400μm

    1.5-400μm

    2.0-1000μm

    25.0-2500μm

    50.0-5000μm

    样品类型

    水相/有机相

    通道数量

    512

    自定义通道数

    32

    流速范围

    60-180ml/min

    进样量

    5μl-10ml

    取样方式

    手动

    自动稀释

    标配一步稀释

    样品最大浓度

    109个/ml

    符合标准

    CE

    Chamber

    30ml,60ml

    电动阀门驱动

    标配

    稀释剂

    标配:超纯水

    选配:有机溶剂

    搅拌器

    标准配置

    Windows系统

    Windows 7以上专业版操作软件

    分析操作软件

    标配:Windows兼容 研发软件

    电源选项

    220 – 240 VAC,50Hz 或100 – 120 VAC,60Hz

    外形尺寸

    主机1(计数器):20 cm *45 cm * 20 cm;

    主机2(自动稀释系统):25 cm * 45 cm * 56 cm;

    重量

    约30kg



  • 传感器

    LE400-05(0.5μm-400μm)

    LE400-1(1μm-400μm)

    LE1000-2(2μm-1000μm)

    LE2500-5(5μm-2500μm)

    LE5000-50(50μm-5000μm)

    提供了宽泛的测量范围,客户可以根据自己实际需要,选择适合自己样品的测量范围的传感器。

    阀门

    电子阀

    电控

    Chambe

    &转子r


    30ml,60ml

    1、由高净石英加工,并配合PFA上、下盖实现样品一步精确的静态稀释;

    2、并可视化跟踪样品的实时状态;

    3、光净的内表面实现高效率的快速清洗;

    4、标配PFA外衣的磁力搅拌子,实现静态稀释过程中样品的快速分散,稀释过程中被稀释样品的稳定均一;

    其他管路

    1/4

    1/8

    3/8

    不同规格的高纯PFA管路配合316不锈钢以及PTFE接头,满足稀释系统的各项严苛要求;

    计量泵


    30-120ml/min

    配备相位传感器由步进电机驱动陶瓷材质的柱塞式泵头,实现对稀释剂流量的精确控制以及超长的使用寿命;

    Cable

    10/14针

    Counter与Sensor、Sampler的连接采用航空级铝制插头,实现较长使用寿命及较高的通讯稳定性;

    过滤器

    Millipore定制0.2μm

    满足药典对稀释剂中不溶性微粒数量的要求,减少由于背景给测量结果带来的负面影响;

    清洗套件

    Mirco 90

    传感器Flow cell专用清洗套装,保证在长期使用之后可以恢复清洁状态;

    性能确认用标粒

    PQ:MML 0.8&2&5

    采用符合NIST的进口标准粒子对设备进行性能确认;

    校准用标粒

    Duke:0.5;0.7;0.8;1.0;1.7;2.0;5.0;10;15;25;50;100μm

    采用符合NIST的进口标准粒子对传感器进行校准;

    软件

    研发版 CW788

    研发软件可最大权限的协助非医药客户对未知样品的分析及检测;





  • 化学机械抛光液(CMP SLURRY)

    化学机械抛光是半导体制造加工过程中的重要步骤。化学机械抛光液是由腐蚀性的化学组分和磨料(通常是氧化铝、二氧化硅或氧化铈)两部分组成。抛光过程很大程度上取决于晶片表面构型。晶片的加工误差通常以埃计,对晶片质量至关重要。抛光液粒度越均匀、不聚集成胶则越有利于化学机械抛光加工过程的顺利进行。

    墨水

    随着打印机技术的不断发展,打印机用的墨水变得越来越重要。喷墨打印机墨水的粒度应当控制在一定的尺度以下,且分布均匀,大的颗粒易于堵塞打印头并影响打印质量。墨水是通过研磨方法制得的,可用粒度检测分析仪器设备监测其研磨加工过程,以保证墨水的颗粒粒度分布均匀,避免产生聚集的大颗粒。


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