CSPS_2015_submission_67
SCI编辑问：倾向性评分后，你验证了吗？
SCI编 辑 问 ： 倾 向 性 评 分 后 ， 你 验 证 了 吗 ？
缘起
精鼎48期SPSS统计软件实战训练营开班啦！
倾向性评分（PS）绝对可以算上近年统计分析领域的网红了，很多大牛期刊近年都有PS相 关的论文刊出。实现倾向性评分匹配目前常用软件有，SPSS、stata、R。本号也推过几期 PSM的推文。
然而权威杂志，对PS论文都有一个要求，就是你倾向性评分匹配后，你进行了匹配效果验证 了吗？
松哥统计说 倾向性评分是一种统计学上的不就方法，常用于观察性研究，但对实验性研究，但基线不均衡 时，也可以操作。
该方法的思想：就是在现有的个案中，选择一部分符合基线条件的个案进行后续分析。虽然增 加了可比性，但也损失了样本量。倾向性评分有4种处理方法，松哥新书里有详细说明. 匹配后数据均衡性检验，对于计量资料可以采用t检验，计数资料可以采用卡方检验。
算出后，进行画图即可。
【赠人玫瑰，手留余香】 【2055】SPSS25，作图优化啦，bayes也可统计了 【2054】SPSS太不靠谱，明明没有缺失值，非说有缺失值，难道是真的？ 【2053】Cox比例风险模型，等比例风险你验证了吗？ 【2052】SCI编辑让做控制协变量的生存曲线 【2051】趋势性检验集锦 【2050】析因设计方差分析 【2049】SCI作图又一技能-嵌入图
【2041】为什么SPSS读取Excel数据乱码或空值，真实案例 【2040】谁说SPSS不能画统计地图
> 10%; significant P-values) in baseline variables between propensity score-matched groups should not be overlooked .】 那么你会问，这这绝对标准差值如何算呢，请参考如下公式，分别针对计量与计数资料：
elastix_registration_method -回复
elastix_registration_method -回复什么是elastix_registration_method？elastix_registration_method是一种医学图像配准方法。
医学图像配准是将不同的医学图像（如CT扫描、MRI等）通过算法进行对齐和匹配的过程。
elastix_registration_method是开源软件elastix中的一种配准算法，可以实现二维和三维图像的配准。
配准是医学影像处理中重要的一环，它可以用于许多应用，包括病灶检测、手术导航和治疗规划等。
在许多医学图像中，由于不同的成像条件、位置和姿态变化，图像之间会存在一定的差异。
配准算法的目标就是通过对这些图像进行空间转换，使得它们在同一坐标系下对齐，便于后续的分析和处理。
elastix_registration_method使用弹性体变形模型将一个图像的像素点映射到另一个图像的对应位置。
通过对目标图像的每个像素点进行变形，使得目标图像和参考图像的特征点之间达到最佳的匹配。
这种变形模型可以通过最小化图像间的差异来优化，例如最小化目标图像和参考图像的灰度值差异或互信息。
elastix_registration_method具有以下几个步骤来实现图像配准：1. 数据准备：首先，需要准备待配准的图像数据。
这些图像数据可以来自同一个病例的不同时间点、不同成像设备或不同成像模态。
此外，还需要选择一个作为参考图像的基准图像。
2. 参数选择：elastix_registration_method具有许多可调节的参数，包括变形模型的类型、优化方法、正则化参数等。
根据具体的应用场景和数据特点，需要选择合适的参数。
3. 初始变形场估计：elastix_registration_method使用一个初始的变形场作为起点。
初始变形场可以是全局变形或局部变形，通过预处理方法获得。
当然，也可以根据应用场景的需要来选择是否需要初始变形场。
CS3012-ISZR,CS3011-ISZ,CS3011-ISZR,CDB30XX, 规格书,Datasheet 资料
2
DS597F6
芯天下--/
CS3011 CS3012
1. CHARACTERISTICS AND SPECIFICATIONS
ELECTRICAL CHARACTERISTICS
V+ = +5 V, V- = 0V, VCM = 2.5 V (Note 1) CS3011/CS3012 Parameter Input Offset Voltage Average Input Offset Drift Long Term Input Offset Voltage Stability Input Bias Current Input Offset Current Input Noise Voltage Density RS = 100 Ω, f0 = 1 Hz RS = 100 Ω, f0 = 1 kHz Input Noise Voltage Input Noise Current 0.1 to 10 Hz 0.1 to 10 Hz • (Note 4) (Note 5) • • • • Input Noise Current Density f0 = 1 Hz Input Common Mode Voltage Range Common Mode Rejection Ratio (dc) Power Supply Rejection Ratio Large Signal Voltage Gain RL = 2 kΩ to V+/2 Output Voltage Swing RL = 2 kΩ to V+/2 RL = 100 kΩ to V+/2 Slew Rate Overload Recovery Time Supply Current PWDN active (CS3011 Only) PWDN Threshold Start-up Time CS3011 CS3012 (Note 6) (Note 6) (Note 7) • • • • • RL = 2 k, 100 pF TA = 25º C TA = 25º C • • -0.1 115 120 200 +4.7 (Note 2) (Note 2) • • Min Typ ±0.01 (Note 3) ±50 ±100 12 12 250 100 1.9 120 136 300 +4.99 2 600 0.9 1.7 (V+)-1.25 1.4 2.4 15 12 ±1000 ±2000 pA pA
PDPS入门
1.整体界面介绍
安装软件完毕后，启动主程序Process Designer，经过登录和Logo画面，然后 就是图示项目选择画面，此列表新安装客户应当是空的，直接点击Cancel跳过
然后进入软件主界面，可以看到除了主菜单和主按钮栏，其他都是由各个小窗口构 成，这些窗口可以任意拖放，合并，隐藏（每个窗口右上角有隐藏和关闭按钮）。 这些窗口的布局称为Layout，程序内置多种方案供选择，图示是Standard方案，用 户可以根据自己操作习惯，任意修改，退出程序时，会有提示是否保存当前修改， 这里指的修改就是对界面布局的修改。
2.创建和整理结构
Process Designer是一个依赖数 据库的软件，他的所有数据分成 2部分： 一部分是3D数模，这部分数据是 放在sysroot下，这个文件夹的名 字可以随便取，只要在程序内 Options下告诉程序这个文件夹在 哪即可，所以不用担心A机器上 的成果到了B机器上看不了； 另一部分数据是3D数模的相互关 系，这部分数据是存储在Oracle 数据库中的，无法象3D数模这样 在Windows下查看，只能用程序 将这些关系以XML的形式导出和 存放。 所以，完整的PD成果必须包含该 模拟中所需要调用的数模和对应 的XML 本章将讲述如何新建项目然后导 出成果
8
Plant Simulation:
Process optimization
9
Reports:
Generation of process documentation
PS下模拟验证工艺与资源
10
© UGS Corp. 2008. All rights reserved.
工厂模拟后提出修改与 优化意见
正电子发射X射线计算机断层成像系统数字化技术专用注册审查指导原则
正电子发射/X射线计算机断层成像系统（数字化技术专用）注册审查指导原则本指导原则是对正电子发射/X射线计算机断层成像系统（Imaging system of positron emission and X-ray computed tomography，简称“PET/CT”）中所用的数字化技术的专用要求。
注册申请人应依据具体产品的特性对注册申报资料的内容进行充实和细化。
注册申请人还应依据具体产品的特性确定其中的内容是否适用，若不适用，需具体阐述其理由及相应的科学依据。
本指导原则是供注册申请人和技术审评人员使用的指导性文件，不包括注册审批所涉及的行政事项，不作为法规强制执行。
若有满足相关法规要求的其他方法，也可采用，并应提供详细的研究资料和验证资料。
本指导原则是在现行法规和标准体系以及当前认知水平下制定的，应在遵循相关法规的前提下使用。
随着法规和标准的不断完善，以及科学技术的不断发展，本指导原则相关内容也将进行适时的调整。
本指导原则作为《正电子发射/X射线计算机断层成像系统注册技术审查指导原则》（简称“PET/CT指导原则”）的补充，是对PET/CT数字化技术的专用要求。
申报资料除符合本指导原则的要求外，还应符合“PET/CT指导原则”的要求。
一、适用范围本指导原则适用于PET/CT产品数字化技术相关的要求，该产品按照《医疗器械分类目录》，产品属于目录06医用成像器械，一级产品类别为17组合功能融合成像器械，二级产品类别为02正电子发射/X射线计算机断层成像系统，按第三类医疗器械管理。
正电子发射断层成像系统（简称PET）单独申报或正电子发射磁共振成像系统（简称PET/MR）设备中PET数字化技术相关要求可参照本指导原则。
二、技术分类（一）PET信号数字化技术路线数字化是指将连续模拟量通过采样、量化、编码及必要的辅助运算方式转换为离散数字量的过程。
PET数字化技术是以数字化的信号处理硬件为手段，以实现入射光子的准确测量为目的，而发展的一系列技术。
CSPS 2015 中文征稿v1
2015 The 4th International Conference on Communications,Signal Processing, and Systems(CSPS2015)第四届通信、信号处理和系统国际会议将于2015年10月23日-24日在四川成都举行。
会议旨在为世界各地的研究人员、工程师和学者提供一个交流通信与信息技术领域最新研究成果的平台。
论文将在由Springer出版的Lecture Notes in Electrical Engineering中发表，并被EI和ISTP检索。
另外，优秀论文将在SCI期刊中发表。
前三届CSPS会议分别于2012、2013和2014年在北京、天津和呼和浩特举行，所发表的会议论文全部已被EI检索，并有共计100多篇优秀论文（扩充后）发表在：∙EURASIP Journal on Wireless Communications and Networking∙Wiley Security and Communication Networks (SCN) Journal∙International Journal of Sensor Networks∙EURASIP Journal on Advances in Signal Processing∙(Elsevier) Physical Communications共5篇SCI源期刊中。
CSPS 2015会务组希望在今年的会议中出现更多的优秀论文，让科研工作者可以分享和交流自己的成果。
重要日期：◆论文提交日期（全英文）:2015年8月15日◆录用通知日期：2015年9月25日◆最终稿提交时间：2015年10月10日◆会议时间：2015年10月23-24日征文主题（不局限于）：∙Wireless communications∙Wireless networks∙Optical communications and networks∙Internet of Things∙Wireless sensor networks∙Wireless mesh networks∙Ad hoc networks∙Underwater sensor networks∙Network security∙Testbed of communications and networks∙Information theory and coding∙Multimedia communications∙Smart grid∙Radar signal processing∙Audio and acoustic signal processing∙Bio imaging and signal processing∙Design and implementation of signal processing systems∙Image, video and multidimensional signal processing∙Industry technology tracks∙Information forensics and security∙Machine learning for signal processing∙Multimedia signal processing∙Multisensor data fusion∙Sensor array and multichannel signal processing∙Signal processing education∙Signal processing for communications and networking∙Signal processing theory and methods∙Speech processing∙Spoken language processing∙Analog Signal Processing∙Genomics Signal Processing∙Biomedical and Life-Science Circuits, Systems and Applications ∙Circuits and Systems for Communications∙Computer-Aided Network Design∙Digital Signal Processing∙Education in Circuits and Systems∙Live Demonstrations of Circuits and Systems∙Multimedia Systems and Applications∙Nanoelectronics and Gigascale Systems∙Neural Networks and Systems∙Fuzzy Logic Systems∙Nonlinear Circuits and Systems∙Power and Energy Circuits and Systems∙Sensory Systems∙Radar Systems∙Chaos Systems∙Visual Signal Processing and Communications∙VLSI Systems and Applications文章要求全英文PDF格式投稿，投稿链接：https:///conferences/?conf=csps2015更多信息请查看会议网站：如果对会议或投稿有任何问题，请发送邮件至：Jiasong Mu <mujiasong@>Wei Wang <weiwangvip@>。
低频活动漂浮潜水船声探测系统（LFATS）说明书
LOW-FREQUENCY ACTIVE TOWED SONAR (LFATS)LFATS is a full-feature, long-range,low-frequency variable depth sonarDeveloped for active sonar operation against modern dieselelectric submarines, LFATS has demonstrated consistent detection performance in shallow and deep water. LFATS also provides a passive mode and includes a full set of passive tools and features.COMPACT SIZELFATS is a small, lightweight, air-transportable, ruggedized system designed specifically for easy installation on small vessels. CONFIGURABLELFATS can operate in a stand-alone configuration or be easily integrated into the ship’s combat system.TACTICAL BISTATIC AND MULTISTATIC CAPABILITYA robust infrastructure permits interoperability with the HELRAS helicopter dipping sonar and all key sonobuoys.HIGHLY MANEUVERABLEOwn-ship noise reduction processing algorithms, coupled with compact twin line receivers, enable short-scope towing for efficient maneuvering, fast deployment and unencumbered operation in shallow water.COMPACT WINCH AND HANDLING SYSTEMAn ultrastable structure assures safe, reliable operation in heavy seas and permits manual or console-controlled deployment, retrieval and depth-keeping. FULL 360° COVERAGEA dual parallel array configuration and advanced signal processing achieve instantaneous, unambiguous left/right target discrimination.SPACE-SAVING TRANSMITTERTOW-BODY CONFIGURATIONInnovative technology achievesomnidirectional, large aperture acousticperformance in a compact, sleek tow-body assembly.REVERBERATION SUPRESSIONThe unique transmitter design enablesforward, aft, port and starboarddirectional transmission. This capabilitydiverts energy concentration away fromshorelines and landmasses, minimizingreverb and optimizing target detection.SONAR PERFORMANCE PREDICTIONA key ingredient to mission planning,LFATS computes and displays systemdetection capability based on modeled ormeasured environmental data.Key Features>Wide-area search>Target detection, localization andclassification>T racking and attack>Embedded trainingSonar Processing>Active processing: State-of-the-art signal processing offers acomprehensive range of single- andmulti-pulse, FM and CW processingfor detection and tracking. Targetdetection, localization andclassification>P assive processing: LFATS featuresfull 100-to-2,000 Hz continuouswideband coverage. Broadband,DEMON and narrowband analyzers,torpedo alert and extendedtracking functions constitute asuite of passive tools to track andanalyze targets.>Playback mode: Playback isseamlessly integrated intopassive and active operation,enabling postanalysis of pre-recorded mission data and is a keycomponent to operator training.>Built-in test: Power-up, continuousbackground and operator-initiatedtest modes combine to boostsystem availability and accelerateoperational readiness.UNIQUE EXTENSION/RETRACTIONMECHANISM TRANSFORMS COMPACTTOW-BODY CONFIGURATION TO ALARGE-APERTURE MULTIDIRECTIONALTRANSMITTERDISPLAYS AND OPERATOR INTERFACES>State-of-the-art workstation-based operator machineinterface: Trackball, point-and-click control, pull-down menu function and parameter selection allows easy access to key information. >Displays: A strategic balance of multifunction displays,built on a modern OpenGL framework, offer flexible search, classification and geographic formats. Ground-stabilized, high-resolution color monitors capture details in the real-time processed sonar data. > B uilt-in operator aids: To simplify operation, LFATS provides recommended mode/parameter settings, automated range-of-day estimation and data history recall. >COTS hardware: LFATS incorporates a modular, expandable open architecture to accommodate future technology.L3Harrissellsht_LFATS© 2022 L3Harris Technologies, Inc. | 09/2022NON-EXPORT CONTROLLED - These item(s)/data have been reviewed in accordance with the InternationalTraffic in Arms Regulations (ITAR), 22 CFR part 120.33, and the Export Administration Regulations (EAR), 15 CFR 734(3)(b)(3), and may be released without export restrictions.L3Harris Technologies is an agile global aerospace and defense technology innovator, delivering end-to-endsolutions that meet customers’ mission-critical needs. The company provides advanced defense and commercial technologies across air, land, sea, space and cyber domains.t 818 367 0111 | f 818 364 2491 *******************WINCH AND HANDLINGSYSTEMSHIP ELECTRONICSTOWED SUBSYSTEMSONAR OPERATORCONSOLETRANSMIT POWERAMPLIFIER 1025 W. NASA Boulevard Melbourne, FL 32919SPECIFICATIONSOperating Modes Active, passive, test, playback, multi-staticSource Level 219 dB Omnidirectional, 222 dB Sector Steered Projector Elements 16 in 4 stavesTransmission Omnidirectional or by sector Operating Depth 15-to-300 m Survival Speed 30 knotsSize Winch & Handling Subsystem:180 in. x 138 in. x 84 in.(4.5 m x 3.5 m x 2.2 m)Sonar Operator Console:60 in. x 26 in. x 68 in.(1.52 m x 0.66 m x 1.73 m)Transmit Power Amplifier:42 in. x 28 in. x 68 in.(1.07 m x 0.71 m x 1.73 m)Weight Winch & Handling: 3,954 kg (8,717 lb.)Towed Subsystem: 678 kg (1,495 lb.)Ship Electronics: 928 kg (2,045 lb.)Platforms Frigates, corvettes, small patrol boats Receive ArrayConfiguration: Twin-lineNumber of channels: 48 per lineLength: 26.5 m (86.9 ft.)Array directivity: >18 dB @ 1,380 HzLFATS PROCESSINGActiveActive Band 1,200-to-1,00 HzProcessing CW, FM, wavetrain, multi-pulse matched filtering Pulse Lengths Range-dependent, .039 to 10 sec. max.FM Bandwidth 50, 100 and 300 HzTracking 20 auto and operator-initiated Displays PPI, bearing range, Doppler range, FM A-scan, geographic overlayRange Scale5, 10, 20, 40, and 80 kyd PassivePassive Band Continuous 100-to-2,000 HzProcessing Broadband, narrowband, ALI, DEMON and tracking Displays BTR, BFI, NALI, DEMON and LOFAR Tracking 20 auto and operator-initiatedCommonOwn-ship noise reduction, doppler nullification, directional audio。
cs和ncs临床试验判定标准
cs和ncs临床试验判定标准随着生物医学科学的发展和临床研究的不断深入，CS和NCS临床试验的判定标准也日益完善。
CS试验代表了对某种药物或治疗方法的疗效进行评价，而NCS试验则主要评估不同治疗方法之间的差异。
本文将简要介绍CS和NCS临床试验的判定标准，并探讨其重要性和发展趋势。
CS临床试验是疗效判定的主要手段之一。
其主要目的是通过比较患者在接受治疗前后的病情变化，来评估治疗是否有效。
在进行CS临床试验时，通常需要确定一些评估指标，如病情缓解率、生存期延长和病情恶化时间等。
同时，还需要选择合适的对照组，以便进行比较。
在CS试验中，通常使用的判定标准有严格的标准化指南，如RECIST （疾病评价标准），用于判断疗效的大小。
此外，还需要考虑一些其他因素，如样本量、随机分组和盲法等。
与CS临床试验相比，NCS临床试验的判定标准更加复杂。
NCS试验通常将患者分为不同的治疗组，以评估不同治疗方法之间的差异。
对于NCS试验，判定疗效的指标也会相应改变。
常用的判定标准包括治疗效果分级、生存期和生活质量等。
此外，还需要考虑其他因素，如样本量、随机分组和盲法等。
CS和NCS临床试验的判定标准在临床研究中具有重要意义。
准确的判定标准可以使研究结果更加客观和科学，从而为患者提供更好的治疗方案。
然而，随着药物和治疗方法的不断创新，现有的判定标准也需要不断更新和完善。
因此，建立统一的判定标准和指南也变得尤为重要。
为了解决这个问题，许多国际组织和政府机构开始制定和发布相关的指南和标准。
例如，美国FDA（食品和药物管理局）制定了一系列评估新药疗效和安全性的指南，以指导临床试验的进行。
此外，世界卫生组织（WHO）也发布了一些关于临床试验判定标准的指南，以协助全球范围内的临床研究。
在未来，随着技术和医学的不断发展，CS和NCS临床试验的判定标准也将不断更新和改进。
例如，随着分子生物学和基因组学的进步，可能会引入更多的生物学指标来评估疗效。
MIDI类型表
aif audio/x-aiff
aifc audio/x-aiff
aiff audio/x-aiff
als audio/X-Alpha5
amc application/x-mpeg
ani application/octet-stream
movie video/x-sgi-movie
mp2 audio/x-mpeg
mp3 audio/x-mpeg
mp4 video/mp4
mpc application/vnd.mpohun.certificate
mpe video/mpeg
application/vnd.lotus-1-2-3
3gp video/3gpp
aab application/x-authoware-bin
aam application/x-authoware-map
aas application/x-authoware-seg
mdb application/x-msaccess
mdz audio/x-mod
me application/x-troff-me
mel text/x-vmel
mi application/x-mif
mid audio/midi
midi audio/midi
au audio/basic
avb application/octet-stream
avi video/x-msvideo
awb audio/amr-wb
bcpio application/x-bcpio
bin application/octet-stream
CSCO2015：JCO审稿流程与论文写作
CSCO2015：JCO审稿流程与论文写作来源：MedSci整理自CSCO 2015年会报告The Journal of Clinical Oncology（JCO,临床肿瘤学杂志）为读者提供可信，权威而重大的临床肿瘤学研究资讯，有印刷版和电子版两种。
在本届CSCO年会论文撰写与国际期刊投稿专场上，来自香港中文大学威尔斯医院，JCO副主编莫树锦教授详细阐述了JCO如何审稿及论文写作方面的知识。
以下为演讲PPT整理，供参考借鉴。
为何会被拒稿？投稿JCO的论文有87%会被拒，原因通常是论文思想不好，缺乏创新；研究设计很差，研究方法不充分。
另外，还有写作水平太差，缺乏必要的逻辑论证。
而莫教授的拒稿原因一般是：研究没有提供新的信息（也就是没有创新）、研究结果对肿瘤学实践无益、研究缺乏科学实力、研究方法不充分、缺乏充分的证据等。
有统计学问题的稿件也可能被拒：•多种对照小样本•没有预先假设、没有有说服力的计算或统计校正•缺乏独立验证组•倾向分数匹配没有考虑到所有相关的协方差•时间偏倚；奈曼分布发生偏差；信息审查；确认偏倚JCO如何评估稿件？稿件投递到JCO办公室后会分配给副主编，未被拒的论文会被送审，由副主编决定是否接收。
审稿流程中会将论文分别发送给四位审稿人，由他们给出各自建议。
审稿人的选择标准也很严苛，要考虑到是否专业、全球不同地区、利益冲突、友好还是不友好等。
四位审稿人会分别给出四种建议：接收、小修、大修、拒绝。
最终决定论文能否被接收了取决于是否有好的想法，你的想法是否新颖，是否可以潜在改变临床实践。
如果你的想法很好，审稿人又给出不错的建议（机会好），那么论文就能最终被接收。
审查研究方法•前瞻性还是回顾性•生物标志物可信赖：如果是回顾性研究，则生物标志物要明确有力•主要终点是什么•样本量，样本量，样本量（重要的话说三遍）•统计学数据分析•坚持主要终点事件，即使它是阴性的•评估次要终点的价值•探索性分析仅是脑力游戏写作计划首先，论文由谁来写？由PI来决定作者名单，第一作者和资深作者对提高写作计划负责，负责撰写文章的重要部分。
technical_guide_for_the_elaboration_of_monographs_7th_edition_2015
Technical guide for the ELABORATION OF MONOGRAPHSEuropean Pharmacopoeia7th Edition2015European Directorate for the Quality of Medicines & HealthCareEnglish version2015 Making copies of this file for commercial purposes or posting it on a websitefor which access is charged is strictly prohibited. Re-use of the file, in whole or in part, requires that the sourcebe clearly cited and the EDQM(@edqm.eu)be informed.European Directorate for the Qualityof Medicines & HealthCare (EDQM)Council of Europe7, allée KastnerCS 30026F-67081 STRASBOURGFRANCE Cover image: © EDQM - Council of Europe Director of the Publication: Dr S. KeitelPage layout: EDQMwww.edqm.eu© Council of Europe, 2015TECHNICAL GUIDE FOR THE ELABORATION OF MONOGRAPHS7th Edition – 2015TABLE OF CONTENTSI.INTRODUCTION (1)I.1.PURPOSE OF THE GUIDE (1)I.2.TEST PROCEDURES (1)I.3.EQUIPMENT (2)I.4.QUANTITIES (2)I.5.REAGENTS (4)MERCIAL NAMES (4)I.7.REFERENCE STANDARDS (4)II.MONOGRAPH ON A SUBSTANCE FOR PHARMACEUTICAL U SE (5)II.1.TITLE (5)II.2.DEFINITION (6)binations (7)II.2.2.Content (7)II.3.CHARACTERS (8)II.3.1.Appearance (8)II.3.2.Taste (9)II.3.3.Odour (9)II.3.4.Solubility (9)II.3.5.Stability factors (10)II.3.6.Hygroscopicity (10)II.3.7.Solid-state properties (10)II.3.8.Other characteristics (10)II.3.9.Behaviour in solution (11)II.4.IDENTIFICATION (11)II.4.1.General (11)II.4.2.Second Identification series (12)II.4.3.Infrared absorption spectrophotometry (13)II.4.4.Ultraviolet and visible absorption spectrophotometry (13)II.4.5.Melting point, freezing point and boiling point (14)II.4.6.Specific optical rotation (15)II.4.7.Thin-layer chromatography (15)II.4.8.Gas chromatography and liquid chromatography (16)II.4.9.Chemical reactions (16)II.5.TESTS (16)II.5.1.General (16)II.5.2.Title of tests (17)II.5.3.Solution S (18)II.5.4.Appearance of solution (19)II.5.4.1. Clarity and degree of opalescence (2.2.1.) (19)II.5.4.2. Degree of coloration (2.2.2.) (19)II.5.5.pH and Acidity or alkalinity (20)II.5.6.Optical rotation (2.2.7.) (21)II.5.7.Absorption spectrophotometry (ultraviolet and visible) (2.2.25.) (22)II.5.8.Related substances (23)II.5.8.1. Thin-layer chromatography (TLC) (2.2.27.) (27)II.5.8.2. Liquid chromatography (LC) (2.2.29.) (28)II.5.8.3. Gas-liquid chromatography (GC) (2.2.28.) (33)II.5.8.4. Capillary electrophoresis (CE) (2.2.31.) (33)II.5.9.Readily carbonisable substances (34)II.5.10.Foreign anions and/or cations (35)II.5.11.Heavy metals – Elemental Impurities (35)II.5.12.Loss on drying (2.2.32.) (36)II.5.13.Thermogravimetry (2.2.34.) (36)II.5.14.Semi-micro determination of water (2.5.12.) – (volumetric Karl Fischer) (37)II.5.15.Micro determination of water (2.5.32.) – (coulometric Karl Fischer) (37)II.5.16.Gas chromatographic determination of water (37)II.5.17.Determination of water by distillation (2.2.13.) (38)II.5.18.Sulfated ash (2.4.14.) (38)II.5.19.Residue on evaporation (38)II.5.20.Residual solvents (2.4.24.) (38)II.5.21.Bacterial endotoxins (38)II.6.ASSAY (39)II.6.1.Ultraviolet and visible spectrophotometry (2.2.25.) (40)II.6.1.1. Direct measurement (40)II.6.1.2. Measurement after a colour reaction (40)II.6.2.Volumetric analysis (40)II.6.3.Chromatography (41)II.6.4.Determination of nitrogen by sulfuric acid digestion (2.5.9.) (41)II.7.STORAGE (41)BELLING (42)II.9.IMPURITIES (42)II.10.FUNCTIONALITY-RELATED CHARACTERISTICS (43)III.ANALYTICAL VALIDATION (44)III.1.DEFINITIONS AND TERMINOLOGY (44)III.1.1.Introduction (44)III.1.2.Types of analytical procedures to be validated (44)III.1.3.Validation characteristics and requirements (45)III.1.4.Glossary (46)III.2.METHODOLOGY (47)III.2.1.Introduction (47)III.2.2.Specificity (48)III.2.2.1. Identification (48)III.2.2.2. Assays and impurity tests (49)III.2.3.Linearity (49)III.2.4.Range (50)III.2.5.Accuracy (51)III.2.5.1. Assay (51)III.2.5.2. Impurities (quantification) (51)III.2.5.3. Recommended data (51)III.2.6.Precision (51)III.2.6.1. Repeatability (52)III.2.6.2. Intermediate precision (52)III.2.6.3. Reproducibility (52)III.2.6.4. Recommended data (52)III.2.7.Detection limit (52)III.2.7.1. Based on visual evaluation (52)III.2.7.2. Based on signal-to-noise ratio (52)III.2.7.3. Based on the standard deviation of the response and the slope (53)III.2.7.4. Recommended data (53)III.2.8.Quantitation limit (53)III.2.8.1. Based on visual evaluation (53)III.2.8.2. Based on signal-to-noise ratio (53)III.2.8.3. Based on the standard deviation of the response and the slope (54)III.2.8.4. Recommended data (54)III.2.9.Robustness (54)III.2.10.System suitability testing (55)III.3.SPECIFIC APPLICATION TO METHODS USED IN THE PH. EUR. (55)III.3.1.Optical rotation (2.2.7.) (55)III.3.1.1. Introduction (55)III.3.1.2. Identification (55)III.3.1.3. Tests (55)III.3.2.Ultraviolet spectrophotometry (2.2.25.) (56)III.3.2.1. Identification (56)III.3.2.2. Limit test (56)III.3.2.3. Assay (56)III.3.3.Non-instrumental limit tests (57)III.3.3.1. Appearance of solution (2.2.1. and 2.2.2.) (57)III.3.3.2. Acidity or alkalinity (57)III.3.3.3. Limit tests for anions/cations (2.4.) (57)III.3.4.Atomic absorption spectrometry (2.2.23.) (58)III.3.4.1. Specificity (58)III.3.4.2. Calibration (58)III.3.4.3. Matrix effects (59)III.3.4.4. Detection and quantification limit (based on the standard deviation of the blank) (59)III.3.5.Separation techniques (59)III.3.5.1. Thin-layer chromatography (2.2.27.) (59)III.3.5.2. Liquid chromatography (2.2.29.) (60)III.3.5.3. Gas chromatography (2.2.28.) (62)III.3.6.Semi-micro determination of water (2.5.12.) (63)III.3.7.Volumetric titrations (2.5.11. - 2.2.19. - 2.2.20.) (64)III.3.8.Peptide identification by nuclear magnetic resonance spectrometry (2.2.64.) (66)I.INTRODUCTIONI.1.PURPOSE OF THE GUIDEThis document is a guide for the authors of monographs and also a means of communicating the principles for the elaboration of monographs to the users of the European Pharmacopoeia (Ph. Eur.), especially industry, licensing authorities and official medicines control laboratories. Since the principles applied and guidance given for the elaboration of monographs should be the same as those applied by licensing authorities, the Technical Guide may also serve as a guideline in the elaboration of specifications intended for inclusion in licensing applications.It is necessary to bear in mind that a monograph will be a mandatory standard and must be applicable in licensing procedures in all Member States of the Convention on the Elaboration of a European Pharmacopoeia.I.2.TEST PROCEDURESThe methods chosen for the identification tests, purity tests and assay(s) constituting the bulk of a pharmacopoeial monograph are preferably those already described and utilised in the Ph. Eur.. In this context, the author of a monograph is referred not only to the General Methods of the Ph. Eur.. but also to published monographs on similar materials. The above considerations aim at ensuring a reasonable degree of harmonisation within the Ph. Eur. and they only apply in cases where the methods are found to be adequate for the specific purposes. However, due attention is also to be paid to the development of new methods that offer significant improvements in terms of sensitivity, precision, accuracy or discriminating power (selectivity).Methods included in monographs must be validated as described in the chapter on analytical validation and other relevant specific chapters of this guide. Validation reports are provided to the EDQM but are not published or otherwise provided to users.The test procedures included in a monograph should be verified in 2 or more laboratories and the laboratory reports on this verification should be provided to the EDQM to ensure future traceability.The instructions describing any method of analysis cover all factors that can influence the results and that are deemed essential to enable an experienced analyst working according to acknowledged laboratory practices, yet without necessarily having any prior knowledge of the investigation in question, to perform the analysis. Variations in the description of similar methods are to be avoided.If an analytical procedure is expected to be used generally or if it requires a lengthy description and is used more than once, it may be proposed for inclusion in the general chapters of the Ph. Eur., to be referred to in the individual monographs. The methods are prescribed on the scale conventionally applied in the Ph. Eur. except in cases where for reasons of availability of the material to be analysed, or because of its toxicity or its cost, work on a small scale would be advantageous.I.3.EQUIPMENTIf the equipment utilised for a method of analysis is not generally available in the States party to the European Pharmacopoeia Convention, it must be possible to have it constructed according to its description in the Ph. Eur.I.4.QUANTITIESIn prescribing the quantities, i.e. masses and volumes, of substances, reagents, and solvents to be taken for identifications, tests and assays, it is the practice of the Ph. Eur. to indicate the accuracy with which they are to be measured (see General Notices). It is therefore necessary to take this aspect into consideration when drafting pharmacopoeial texts.As guidance to minimise errors in the preparation of analytical solutions, Table 1, giving estimations of the relative uncertainty, is to be consulted.In order to avoid either the use of extremely low amounts or an unnecessarily large expenditure of solvents, a dilution series will often have to be prescribed for the preparation of dilute solutions used particularly for spectrophotometric measurement. In this context not all combinations of (usually 2 or 3) dilution steps will contribute equally to the random error of the dilution procedure. If critical for the purpose, the optimal dilution is prescribed in consideration of the relative errors (capacity tolerance divided by nominal volume) associated with the various sizes of volumetric pipettes and volumetric flasks commonly used for these operations (taking the usual formula: square root of the sum of the squares of individual relative errors, to estimate the relative dilution error).Tables giving the optimal number and nature of dilution steps needed to achieve a given dilution ratio, based upon given specifications for the capacity tolerances of volumetric glassware, are available in the literature. For guidance see Table 2 (it is to be noted that these factors do not include reading errors).Table 1 – Relative uncertainties in the preparation of analytical solutionsConcentration to be prepared Preparation of solution Percentage relative uncertainty Mass Volume Total10 g/1000 mL 10 g/1000 mL1 g/100 mL0.5 g/50 mL0.25 g/25 mL0.1 g/10 mL< 0.010.020.040.080.020.050.120.170.230.500.050.120.170.240.541g/1000 mL1 g/1000 mL0.5 g/500 mL0.25 g/25 mL100 mg/100 mL50 mg/50 mL10 mg/10 mL0.020.040.080.20.42.00.050.070.230.120.170.500.050.080.240.230.432.060.1 g/1000 mL 100 mg/1000 mL50 mg/500 mL25 mg/250 mL10 mg/100 mL5 mg/50 mL1 mg/10 mL0.20.40.82.04.020.00.050.070.080.120.170.500.210.410.802.04.020.00.01 g/1000 mL 10 mg/1000 mL5 mg/500 mL1 mg/100 mL2.04.020.00.050.070.122.04.020.0An uncertainty of 0.2 mg for the weighing procedure has been assumed for the calculations of the percentage relative uncertainties.Table 2 – Relative errors for dilution with analytical glassware (pipettes P/flasks F)Concentration ratio No. of steps Step 1 Step 2 Relative errorP F P F1/2 1 25 50 0.161/2.5 1 20 50 0.181/5 1 20 100 0.171/10 1 25 250 0.131/12.5 1 20 250 0.161/30 1 15 500 0.201/50 1 20 1000 0.151/100 1 25 250 25 250 0.181/125 2 20 250 25 250 0.201/160 2 25 1000 25 100 0.191/200 2 25 500 25 100 0.181/250 2 20 250 25 500 0.201/400 2 25 250 25 1000 0.181/500 2 20 500 25 500 0.201/1000 2 20 1000 25 500 0.20Adapted from R.B. Lam and T.L. Isenhour, Minimizing relative error in preparation of standard solutions by judicious choice of volumetric glassware, Analytical Chemistry, 1980, 53, 1158-1161.I.5.REAGENTSWhen the quality of a reagent substance in one or more respects is critical for its intended use, it must be carefully defined, when necessary by prescribing appropriate tests to demonstrate its suitability. Normally, analytical grade reagents are employed in which case it is sufficient to give the name of the reagent, the CAS number and its formula.Whenever possible, the reagent substances, reagent solutions, volumetric solutions and standard solutions for limit tests already described in the chapter 4.Reagents of the Ph. Eur. are to be employed. Simple solutions of reagent substances or solutions that are prepared for use on a single occasion are to be described in the monograph itself.The use of reagents that are acknowledged to be extremely toxic or otherwise hazardous (e.g. carcinogenic), is to be avoided, especially in circumstances where their dangerous properties are difficult to control, e.g. when handled as fine powders or in spray reagents. The use of those substances that are prohibited or restricted in one or more of the States party to the European Pharmacopoeia Convention is also to be avoided (e.g. mercury containing reagents, REACH regulation annex XIV).MERCIAL NAMESCommercial names are given systematically as footnotes in draft monographs for chromatography columns/plates and based on usefulness for the analysts in other cases (e.g. test kits, reagents that are available from a single supplier, etc.). Commercial names are not included in the text published in the Ph. Eur. but are transferred to the EDQM Knowledge Database after adoption of the monograph.I.7.REFERENCE STANDARDSThe policy and procedures regarding reference standards are described for information in general chapter 5.12.Reference standards. Procurement, establishment, storage and monitoring of reference standards are the responsibility of the EDQM. Many reference standards, notably impurity standards, are available only in limited quantities, and the amount prescribed for preparation of solutions must be kept to a minimum. Before publication of a monograph in Pharmeuropa, the required quantities of reference standards should be supplied to the EDQM, who will advise on the best strategy for optimising the use of substances that are available in limited quantities (for example, preparation of a spiked substance rather than supply of the single impurity). The aim of the EDQM is to present the reference standards for adoption at the same time as the monograph or, failing that, by the time of publication at the very latest.For IR identification, preference is given to chemical reference substances over reference spectra, except in special cases, for example where provision of a reference substance entails practical difficulties.II.MONOGRAPH ON A SUBSTANCE FOR PHARMACEUTICAL USE Monographs are based on the specifications for substances used in medicinal products approved in Member States. When a monograph is added to the work programme, enquiries are made by the EDQM to identify manufacturers of such substances and all data received is taken into account for preparation of the monograph. Interested parties should be invited to participate in the elaboration of the monograph before publication in Pharmeuropa, since the 3-month public period will often be too short for all interested parties to check the draft monograph.Prior to the preparation of any monograph, it is essential to gather as much information as possible on the substance in question.In particular it is necessary to ascertain:•whether the substance is of natural, synthetic or semi-synthetic origin;•whether the substance is a mixture or a single entity;•the method(s) of preparation in detail;•whether there are different crystalline forms, since the properties of the substance may vary in accordance with this parameter;•whether both an enantiomer as well as the racemate or other mixtures of enantiomers are available;•whether different hydrates are available;•whether different entities (acid, base, salt, etc) are available.The Ph. Eur. and other relevant documents on the state of work must be consulted to see if monographs on similar substances exist or are being elaborated. If this is the case, it is important to ensure that similar monographs follow the same approach unless there are good reasons to deviate, e.g. developments in analytical techniques.When a substance exists both in a water-free form and in the form of (a) hydrate(s) with different water contents, and if all these forms are used, they are normally treated as individual substances requiring separate monographs. The same rule applies for other solvates.Substances that are to be described in a monograph may be members of a group of very similar substances (family). This holds true especially for excipients such as macrogols. A master monograph (family monograph) is to be drafted clearly stating the attributes common to all members of the family and that can be used to identify single members of the family.All active substances and excipients described in the Ph. Eur. are subject to the provisions of the general monograph Substances for pharmaceutical use (2034).II.1.TITLEThe International Nonproprietary Name (INN) established by the World Health Organization should be used wherever it is available; it is supplemented as appropriate by the name of the anion or cation and by the degree of hydration. Anions and cations are indicated as “mono-, di-, tri-, etc.”, as appropriate.The following rules apply for the degree of hydration.•In the case of a well-defined hydrate, “mono-, di-, tri-, etc…hydrate” is added to the title whereas if the monograph covers more than one degree of hydration, the general term “hydrate” is used. In the latter case, a sentence is added to the DEFINTION section (see chapter II.2). For monographs published prior to the 9th edition of the Ph. Eur., retrospective introduction of the degree of hydration in titles would only be made after careful consideration.•As of the 9th edition of the Ph. Eur, monographs referring to “anhydrous” substances will no longer specify this in their title with the exception of a few monographs where the information has a recognised added value and/or is used in common scientific language(e.g. Ethanol, anhydrous).•For monographs covering substances that can be either water-free or with, a defined or variable, degree of hydration, no mention will be added to the title. This information will be supplemented in the DEFINITION section of the monographs (see part II.2.).Where a substance is used in approved medicinal products for veterinary use only in Member States, “for veterinary use” is included in the title.II.2.DEFINITIONThe chemical structure must be ascertained with the greatest possible care in order to establish the exact:•graphic formula;•empirical formula and relative molecular mass. The latter is calculated as follows: first, the relative atomic masses, or multiples thereof, are added together using all thefigures of the International Table of Relative Atomic Masses; the total is then roundedoff to 4 significant figures if the initial digit is 1, 2, 3, 4 or 5, or to 3 significant figures ifthe initial digit is 6, 7, 8 or 9; the last figure is increased by 1 when the part rejectedexceeds one half-unit. When the part rejected is equal to or less than one half-unit, thelast figure taken is not modified;•chemical name. This involves investigating in particular:o the possible existence of isomers so as to be able to specify which isomer is used or, otherwise, to state that the product is a mixture of isomers;o in the case of an optical isomer, it is insufficient to take into account only the direction of the optical rotation. The absolute configuration is given by the R/Ssystem at the asymmetrical centre(s) or any other appropriate system (e.g., forcarbohydrates and amino acids);o ascertaining the state of hydration so as to distinguish clearly between the well-defined hydrates (mono-, di-, tri-, etc… hydrate) and the products that containvariable quantities of water. In the latter case, the term “x-hydrate” is introduced inthe chemical name.If the substance contains a variable quantity of water, or refers to both water-free and hydrate form, a sentence is added to the DEFINITION section to explain the exact scope of the monograph.Some chemical substances, particularly those obtained from raw materials of natural origin and substances produced by fermentation may not be easily separated from certain related substances (for instance, quinine salts). These may be treated as:• a chemical product when obtained in a very pure state and when they can be assayed by a physico-chemical method;• a substance accompanied by a certain proportion of related substances, giving an exact definition of the main component only (e.g. neomycin);• a mixture of several components, sometimes difficult to define, where an overall description may suffice (e.g. nystatin).Where applicable, the origin of the substance must be specified (name and strain of the organism from which the substance is derived). Where applicable, the monograph indicates that the substance is semi-synthetic and derived from a fermentation product [to clarify application of the general monograph Substances for pharmaceutical use (2034)].binationsIn therapeutics, more or less well-defined chemical combinations (for instance, theophylline- ethylenediamine) or even mixtures are sometimes used. In such cases, it is necessary to specify precisely each component of the combination or mixture, with its chemical structure and the proportion in which it is present.II.2.2.ContentThe substance described by a monograph is never a wholly pure substance but contains a limited proportion of impurities. The content is therefore an important part of the definition. Assay limits are specified between which the content must fall.In setting these limits for the active substance content, account is taken of:•the method of preparation, which determines the degree of purity that may be reasonably required;•the reproducibility and accuracy of the analytical method;•current batch data of about 10 production batches at release;•the evaluation of batch stability data;• a sufficient number of experimental results obtained on several batches (at least 3), if possible, of different origins and ages.For a non-specific assay by titrimetry the limits are set according to the table provided in part III.3.7 i.e. usually 99.0-101.0 %. Some monographs still include an assay by UV-Vis spectrophotometry usually bearing wider limits.For a specific assay using a separation technique (for example, liquid or gas chromatography), the upper assay limit is normally 102.0 %; the lower assay limit will take any necessary account of the impurities present based on the available batch data and approved specifications. It may therefore be lower than 98.0 %.assay, or when it contains only a very low proportion of impurities interfering with the assay, the results of the assay can be used directly. It will then be stated that: “[the substance] contains not less than x per cent and not more than the equivalent of y per cent (at least 100.5 %, but often a little more) of [chemical definition of the pure product]”. The content of the substance is usually expressed with reference to the anhydrous or dried substance. According to the general monograph Substances for pharmaceutical use (2034) the content of residual solvent is taken into account for calculation of the assay content of the substance, therefore no reference in the DEFINITION section of the individual monograph is made.In cases where the water content is high (e.g. in the case of disodium phosphate dodecahydrate), limits of content may be expressed with reference to the hydrate form of the substance, taking into account the molecular mass of the hydrate form (only for well-defined hydrates) or with reference to the substance on the anhydrous/dried basis in combination with determination of water content/loss on drying.When the substance to be examined contains a relatively large proportion (a few %) of impurities, which are determined at the same time as the active ingredient, an appropriate wording is to be used (for instance, in the case of quinine salts: “x per cent of total alkaloid salts, expressed as quinine salts”).Exceptionally reference is made to only a part of the molecule or to an element (for example assay of magnesium oxide in light magnesium carbonate or assay of magnesium in magnesium stearate).In the case of antibiotics determined by microbiological assays, the active ingredient content is expressed in International Units, where these exist, and only a minimum value is given.See also under part II.6.II.3.CHARACTERSAs defined in the General Notices, statements under the heading CHARACTERS are not to be interpreted in a strict sense and are not regarded as analytical requirements. The principal items that may be referred to under this heading are the following.II.3.1.AppearanceThis description will normally embrace colour and physical form. The term “white” is not used without qualification since, if viewed against a standard white material, very few pharmaceutical materials will appear truly white. It is, of course, not intended that such a comparison be made but experience shows that certain users of the Ph. Eur. may insist on doing so as part of a purchasing contract. The term “white or almost white” is used instead. Where positive colours are to be described, this is done in terms of primary colours or combinations of primary colours.Colour: the following descriptive terms are used: black, orange, blue, pink, brown, red, colourless, violet, green, white/almost white, grey, yellowCompound terms may be used:English Frenchgreenish-blue bleu-vertbluish-green vert-bleuviolet-red rouge-violetreddish-violet violet-rougebrownish-red rouge-brunreddish-brown brun-rougeIt can be noted that in English, the dominant is placed second, whereas in French, it is placed first. Expressions such as lemon-yellow, buff, salmon-pink are to be avoided; standard dictionaries give equivalents for such terms as spectral colours with suitable qualifiers (for example, buff is described as “dull yellow”). The following adjectives are also used; light, slight, fluorescent, intense, pale, dull, deep, dark.It is to be noted that the allowed colours and colour combinations also apply to the description of the colour changes of indicators when used in acid/alkalinity tests or in titrimetric assay procedures.II.3.2.TasteThe taste is not to be taken into consideration.II.3.3.OdourIn general, no reference is made to odour. In particular no reference to odour is made for those materials that would constitute a hazard if inhaled. Mention of odour in other cases must be justified.II.3.4.SolubilityA method recommended for the estimation of solubility is given in general chapter5.11.Characters section in monographs. All solubilities are quoted in the general terms defined in the General Notices. Solvents quoted are normally confined to water, an alcohol and a lipophilic solvent (e.g. water, ethanol, heptane). Solubilities in chloroform and ether are not mentioned and the use of hexane is discouraged. In special cases the solubility of different samples of a material may vary rather considerably even though their composition is still within the limits set by the monograph. The solubilities in the solvents thereby affected are then given to cover more than one solubility class, e.g. “sparingly soluble to soluble in...”. The solubilities or miscibilities in other solvents with which the material is often combined in practice such as fatty oils, etc., may also be mentioned. In some cases it may be useful to specify solubility in alkalis or acids and, particularly in cases of materials that are very insoluble in the above-mentioned solvents, a special solvent may be indicated, e.g. dimethylformamide or dimethyl sulfoxide. It is not necessary to specify the solubility in every solvent that is used in performing the tests of the。
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Nanosized CaCO3 as Hard Template for Creation of Intracrystal Pores within Silicalite-1 Crystal
Nanosized CaCO3as Hard Template for Creation of IntracrystalPores within Silicalite-1Crystal†Haibo Zhu,‡Zhicheng Liu,§Yangdong Wang,§Dejin Kong,§Xiaohong Yuan,§andZaiku Xie*,‡,§School of Chemistry and Chemical Technology,Shanghai Jiao Tong Uni V ersity,800Dongchuan Road, Shanghai200240,China,and SINOPEC Shanghai Research Institute of Petrochemical Technology,1658Pudong Beilu,Shanghai201208,ChinaRecei V ed May22,2007.Re V ised Manuscript Recei V ed July31,2007The silicalite-1crystal with intracrystal pores in the range of50–100nm was synthesized by using the nanosized CaCO3as a hard template.The nanosized CaCO3can be trapped into the silicalite-1crystal during the crystallization process.By means of acid dissolution,the encapsulated nanoparticles were removed,giving rise to the intracrystal pores within the zeolite crystal.Characterization techniques including XRD,TEM,SEM,and N2adsorption provided the detailed information on this hierarchical pore structure.The hydroxyl groups on the surface of CaCO3are essential to taking the hard template effect.The secondary pores within zeolite correspond well to the morphology of the nanosized CaCO3, which confirms the template effect of nanosized CaCO3.These results suggest that using CaCO3as a hard template may be a useful approach for the synthesis of hierarchical porous materials.IntroductionZeolites are the crystalline porous materials with uniform pores in the molecular dimension,as well as a high internal surface,flexible framework,and controllable chemistry, making them widely application in catalysis,purification, adsorption,separation,and other industrialfields.1But the small channels and cavities in the zeolite framework,usually in the range of0.5-1.5nm,not only reduce the diffusion of reagents and reaction products through the pore network but also limit the bulk molecules involved the reaction.The finding of mesoporous materials with pore sizes of2–50nm, such as MCM-41,MCM-48,and SBA-15,may afford an opportunity to overcome this problem.2,3However,the weak acidity and low hydrothermal stability resulting from the amorphous nature of the mesoporous walls dramatically prevent them from being used in practical applications in industrialfields.In an attempt to circumvent such difficulty,the construc-tion of mesopore-modified zeolites with the advantages of microporous and mesoporous materials may show satisfac-tory activity toward some catalytic reactions.4The template-directed method has been exploited to synthesize mesoporous pared to conventional steaming and chemical leaching approaches,this technique provides a route for the formation of mesopores in zeolites in a controllable manner.Carbon-based porous materials,such as carbon black,5 multiwall carbon nanotube,6and carbon nanofiber,7are effective templates for the synthesis of mesoporous zeolites. Jacobsen et al.have investigated the synthesis of mesoporous zeolites including ZSM-5,ZSM-11,TS-1,TS-2,and sili-calite-2with a pore size distribution of10–100nm by using carbon black and multiwall carbon nanotubes as mesopore-forming templates.8,9Tao et al.have reported the preparation of zeolite ZSM-5and Y monolith with a bimodal pore structure of uniform mesopores by the templating method using a carbon aerogel of uniform mesopores.10–14An ordered mesoporous aluminosilicate with completely crystal-line ZSM-5wall structure has been successfully synthesized, upon the recrystallization of SBA-15using in situ formed CMK-5as the hard template.15The ZSM-5zeolite with unique supermicropores has been obtained by synthesizing the zeolite using well-ordered mesoporous carbon(CMK-3) as the solid template,and the texture properties of the resulting ZSM-5can be tailored by changing the nature of the(CMK-3)template.16†Part of the“Templated Materials Special Issue”.*To whom correspondence should be addressed.E-mail:xzk@. Fax:862168462283.‡Shanghai Jiao Tong University.§Shanghai Research Institute of Petrochemical Technology.(1)Corma,A.Chem.Re V.1995,95,559.(2)Kresge,C.T.;Leonowicz,M.E.;Roth,W.J.;Vartuli,J.C.;Beck,J.S.Nature1991,352,710.(3)Zhao,D.;Feng,J.;Huo,Q.;Melosh,N.;Fredrickson,G.H.;Chmelka,B.F.;Stucky,G.D.Science1998,279,548.(4)Hartmann,M.Angew.Chem.,Int.Ed.2004,43,5880.(5)Jacobsen,C.J.H.;Madsen,C.;Houzvicka,J.;Schmidt,I.;Carlsson,A.J.Am.Chem.Soc.2000,122,7116.(6)Schmidt,I.;Boisen,A.;Gustavsson,E.;Stahl,K.;Pehrson,S.;Dahl,S.;Carlsson,A.;Jacobsen,C.J.H.Chem.Mater.2001,13,4416.(7)Janssen,A.H.;Schmidt,I.;Jacobsen,C.J.H.;Koster,A.J.;de Jong,K.P.Micorporous Mesoporous Mater.2003,65,59.(8)Kustova,M.Y.;Hasselriis,P.;Christensen,C.H.Catal.Lett.2004,96,205.(9)Schmidt,I.;Krogh,A.;Wienberg,K.;Carlsson,A.;Brorson,M.;Jacobsen,mun.2000,2157.(10)Tao,Y.;Kanoh,H.;Kaneko,K.J.Am.Chem.Soc.2003,125,6044.(11)Tao,Y.;Kanoh,H.;Hanzawa,Y.;Kaneko,K.Colloids Surf.,A2004,241,75.(12)Tao,Y.;Kanoh,H.;Kaneko,K.J.Phys.Chem.B2003,107,10974.(13)Li,W.C.;Lu,A.H.;Schüth,F.Chem.Mater.2005,17,3620.(14)Tao,Y.;Hattori,Y.;Matumoto,A.;Kanoh,H.;Kaneko,K.J.Phys.Chem.B2005,109,194.(15)Fang,Y.M.;Hu,H.Q.J.Am.Chem.Soc.2006,128,10636.(16)Yang,Z.;Xia,Y.;Mokaya,R.Ad V.Mater.2004,16,727.1134Chem.Mater.2008,20,1134–113910.1021/cm071385o CCC:$40.75 2008American Chemical SocietyPublished on Web12/01/2007Recently,the mesoscale polymer template route has been developed to fabricate hierarchical mesoporous zeolites.The silane functionalized polyethylenimine has shown promise in the synthesis of MFI and FAU zeolites with small intracrystal mesopores and narrow pore size distribution.17 Xiao et al.have demonstrated a facile,controllable,and universal route for the synthesis of hierarchal mesoporous zeolites templated from a mixture of small organic am-monium salt and mesoscale cationic polymer.18Meanwhile, the organosilane-modified surfactant designed by Choi and colleagues has been found to be effective in synthesizing polycrystalline zeolite assemblies with relatively uniform mesopores that lead to superior performance in the catalytic reactions involving large organic molecules.19–21 Herein,we describe a new method by using a hard template to synthesize silicalite-1with intracrystal pores.The nanosized CaCO3,which is cheap and easily available,is used as the hard template to create the intracrystal pores within zeolite crystal.Experimental SectionMaterials.Hydrophilic and hydrophobic nanosized CaCO3used as a hard template were obtained from Shanghai Yaohua nanotech Corporation(China).The particle size distribution of CaCO3is in the range of50–100nm,and the surface of the hydrophobic CaCO3 is modified by fatty acid.Aerosil-200(99%,degussa),NaOH(99%), and tetrapropyl ammonium hydroxide(25%,denoted as TPAOH)were commercial available and used in the synthesis without further purification.Synthesis of Silicalite-1with Intracrystal Pores.In a typical synthesis of hierarchical porous silicalite-1,6g of the nanosized CaCO3was added to a clear solution of tetrapropylammonium hydroxide,water,and NaOH.The suspension was under strong stirring in order to produce a paste in which the nanosized CaCO3 is highly dispersed.Four grams of Aerosil-200was then slowly added into this suspension.The resulting mixture underwent ultrasonic agitation for10min in order to give the homogeneous dispersion of CaCO3particle into silica gel.Afterward,the homogeneous mixture was vigorously stirred for2h.The resulting mixture of silica gel(0.4TPAOH:0.03Na2O:1SiO2:20H2O)and the nanosized CaCO3was introduced to a Teflon-lined steel autoclave for further hydrothermal treatment.The hydrothermal crystallization was carried out at140°C for7days.After the completion of the hydrothermal synthesis,the composite was acid-treated to dissolve the nanosized CaCO3,which released the secondary pores within the crystal.The HCl solution was added to the composite dropwise until the pH value was below6.0and no gas came out from the product.The as-synthesized zeolite was isolated byfiltration, washed with water,and dried at100°C for2h.The organic structure-directing agent trapped in the pores was thoroughly removed by calcination at550°C for6h.For comparison,the synthesis procedure without the addition of the nanosized CaCO3was also performed in the same condition. Steam Treatment.The hydrothermal stability test was carried out byflowing water through the sample hold on a microreactor at 600°C for6h,and the waterflow was generated by a pump. Finally,the obtained samples were taken out and dried for XRD characterization.Characterization Methods.X-ray powder diffraction(XRD) patterns were measured on a Bruker diffractometer equipped with a rotating anode and Cu KR radiation.The microstructure charac-terizations were carried out using a JSM-7401F scanning electron microscopy(SEM)operating at5kV.Transmission electron microscopy(TEM)studies were carried out on a Tecnai20S-TWIN instrument using an electron beam generated by a CeB6filament and an acceleration voltage of120kV.Samples for TEM studies were prepared by dipping a carbon-coated copper grid into a suspension of samples in ethanol that was presonicated.Infrared spectra(IR)data was recorded on a Nicolet5700Fourier Transform Infrared Spectrophotometer;the samples were ground with KBr and pressed into thin wafers.The nitrogen adsorption/desorption isotherms were measured at-196°C on a Micromertitics ASAP 2020M instrument.Before measurement,samples were evacuated overnight at250°C.The BET surface area was calculated from the linear part of the BET plot according to IUPAC recommenda-tions.The mesopore size distribution was analyzed from the nitrogen desorption branch using the BJH model.Results and DiscussionThe X-ray powder diffraction patterns of CaCO3and the silicalite-1/CaCO3composite are shown in Figure1.Dif-fraction peaks located at2θ)23.1,29.4,35.9,39.4, 43.1,47.6,and48.5°clearly reveal that CaCO3belongs to the calcite phase.22The composite of silicalite-1/CaCO3 exhibits two groups of diffraction peaks.The peaks with(17)Wang,H.;Pinnavaia,T.J.Angew.Chem.,Int.Ed.2006,45,7603.(18)Xiao,F.X.;Wang,L.F.;Yin,C.Y.;Lin,K.F.;Di,Y.;Li,J.X.;Xu,R.R.;Su,D.S.;Schlögl,R.;Yokoi,T.;Tatsumi,T.Angew.Chem., Int.Ed2006,45,3090.(19)Choi,M.;Cho,S.H.;Srivastava,R.;Venkatesan,C.;Choi,D.H.;Ryoo,R.Nat.Mater.2006,5,718.(20)Choi,M.;Srivastava,R.;Ryoo,mun.2006,4380.(21)Srivastava,R.;Choi,M.;Ryoo,mun.2006,4489.(22)Wang,C.Y.;Sheng,Y.;Zhao,X.;Zhao,J.Z.;Ma,X.K.;Wang,Z.C.Mater.Sci.Eng.,C2007,27,42.Figure1.XRD patterns of(a)silicalite-1/CaCO3,and(b)nanosized CaCO3.1135Chem.Mater.,Vol.20,No.3,2008Intracrystal Pores within Silicalite-1Crystalhigher intensity are ascribed to the diffraction of calcite,suggesting that CaCO 3is stable enough to resist the hydro-thermal synthesis in alkaline media.In addition,the char-acteristic peaks of silicalite-1emerging at 2θ)7.9,8.8,23.1,24.0,and 24.5°are also detectable in the composite of silicalite-1/CaCO 3.23The comparison of X-ray powder diffraction patterns of the material obtained by the removal of CaCO 3from the silicalite-1/CaCO 3composite and the conventional silicalite-1are shown in Figure 2.After the removal of CaCO 3,the peaks indexed to the crystalline calcite disappear completely.Determined from an EDS mounted on the SEM,the residual content of CaCO 3occluded in zeolite is only about 0.1%,which is negligible.CaCO 3is easily soluble in an acidic medium,even though the weak organic acid such as acetic acid can remove CaCO 3trapped into zeolite.For the reasons stated above,the acid treatment can dissolve the nanosized CaCO 3encapsulated in the crystal,releasing the correspond-ing intracrystal pores within crystal.On the other hand,the characteristic diffraction peaks of silicalite-1become evident in the new material.This new material shows a high level of crystallinity comparable to that of the conventional silicalite-1,which is synthesized in the same conditions without the addition of nanosized CaCO 3.The comparison of X-ray powder diffraction means that the crystallinity of the last product is not remarkably influenced by the nanosized CaCO 3.The nanosized particles play a decisive role in generating the intracrystal pores within silicalite-1,so the morphology of CaCO 3is important to evaluate the hard template effect.The SEM images in Figure 3give details on its morphology.The low magnification image shows that the particles are uniform.The SEM image taken at a magnification of 40000times reveals that the particles exhibit nearly cubic shape and the particle size is in the range of 50–100nm.The results of scanning electron microscopy (SEM)for the hard-template-directed silicalite-1are shown in Figure 4,and the sample appears to be highly crystalline.Estimated from the SEM overview,the average crystal size of sili-calite-1is in the range of 400–800nm.Interestingly,some mesopores and macropores caused by the acid dissolution of CaCO 3that are opening at the external surface of the silicalite-1can be directly observed in the high-magnification image of the SEM.Such intracrystal pores leading to the surface may promote the diffusion of bulk guest molecules into the internal surface of zeolite.A TEM image is a projection of the mass density encountered by electrons passing through the sample;pores show up as bright areas.Therefore,it is a powerful technique for direct observation of secondary pores in zeolite.24The representative TEM images of the intracrystal-pore-modified zeolite are shown in Figure 5.The zeolite particles display regular shape in the TEM images.Hence,they should be considered as the single crystals.The TEM images under the high magnification show that the noncrystallographic pores created by the hard template are clearly visible in the images.The intracrystal pores are different from the regular mesopore structure in typical mesoporous materials and are randomly distributed in a whole crystal.It also can be observed that some noncrystallographic pores are intercon-nected to each other in a single crystal;accordingly,such pore system can be beneficial for efficient mass transport in zeolite crystal.Besides,the shape of the intracrystal pores is consistent with the morphology of cubic-shaped CaCO 3,suggesting that the secondary pore structure imprints the morphology of the nanosized CaCO 3.The TEM images prove that the nanosized inorganic material takes a significant template effect on creating secondary pores within zeolite crystal.The N 2adsorption isotherm of the silicalite-1with intrac-rystal pores is shown in Figure 6,and the corresponding pore size distribution is given in the inset of Figure 6.The N 2adsorption isotherm exhibits a steep increase at relatively low pressure (P /P 0)<0.02.This adsorption is interpreted as micropores filling and capillary condensation.Besides,the N 2isotherm shows a hysteresis loop from P /P 0)0.8to P /P 0)1.This hysteresis loop is relative to the existence of the intracrystal pores.25Relative to conventional ordered mesoporous materials,the pore size distribution of the mesopores in the silicalite-1sample is relatively wide.The pore size distribution is calculated from the desorption branch of the isotherms on the basis of the Barrett–Joyner–Halenda (BJH)model,and the result shows that the pore width is widely distributed in the range of 50–100nm.This result is not only in good agreement with the particle diameter of(23)Van Koningsveld,H.;Jansen,J.C.;van Bekkum,H.Zeolite 1990,10,235.(24)Boisen,A.;Schmidt,I.;Carlsson,A.;Dahl,S.;Brorson,M.;Jacobsen,mun.2003,958.(25)Groen,J. C.;Peffer,L.;A, A.;Pérez-Ramírez,J.MicoporousMesoporous Mater.2003,60,1.Figure 2.XRD patterns of (a)silicalite-1with intracrystal pores,and (b)conventional silicalite-1.1136Chem.Mater.,Vol.20,No.3,2008Zhu et al.the nanosized CaCO 3but also consistent with the pore size directly observed from the TEM image.It is important to note that the pronounced peak at 4nm in the BJH desorption pore size distribution does not suggest real pore,which is due to the tensile strength effect (TSE)of the adsorbed phase.26Quantitatively,the BET total surface area of the sample is 445m 2/g,with micropore and mesopore areas of 215and 230m 2/g,respectively.The total pore volume is 0.40cm 3/g,consisting of micropore volume of 0.10cm 3/g (calculated by the t -plot method of Lipens and de Boer 27)and mesopore volume of 0.30cm 3/g.The micropore volume of this new material is almost same as that of the conven-tional silicalite-1zeolite.28The N 2adsorption isotherm as well as the TEM image result suggest that the intracrystal pores within silicalite-1are caused by the nanosized CaCO 3trapped into the crystal during the zeolization.It is well-known that the drawback of mesoporous and macroporous materials is the low stability and hydrothermal stability,resulting from the amorphous wall.Many methods have been developed to enhance the ability to resist the hydrothermal condition,but most of them are far fromindustrial requirements.29–31To evaluate the hydrothermal stability of this material,we put the sample under steam destruction at 600°C for 6h.The comparison of XRD patterns of the parent sample and the sample treated by steam (see the Supporting Information),indicates that the sample retains the crystallinity at a high level even after steam treatment for a long time.Meanwhile,the intracrystal pores can be also observed in the TEM image.It can thus be concluded that steam treatment at high temperature does not cause significant destruction on its structure.Although the intracrystal pores are introduced into the crystal through CaCO 3template,the atom distribution in zeolite still retains a short-range order.The hydrothermal stability can be attributed to the highly ordered crystalline structure.The creation of hierarchal pores in silicalite-1is attributed to the use of nanosized CaCO 3as a hard template.The efficiency of the hard template effect largely depends on the surface property of nanosized CaCO 3.Hydrophilic and hydrophobic CaCO 3have been used to conduct the synthesis in the same condition.These two types of nanosized CaCO 3are the same in morphology but different in surface proper-ties.The hydrophobic CaCO 3is produced upon the modi-(26)Groen,J.C.;Pérez-Ramírez,J.Appl.Catal.,A 2004,268,121.(27)Lipens,B.C.;de Boer,J.H.J.Catal.1965,4,319.(28)Li,W.C.;Lu,A.H.;Palkovits,R.;Schmidt,W.;Spliethoff,B.;Schüth,F.J.Am.Chem.Soc.2005,127,12595.(29)Selvaraj,M.;Kawi,S.Chem.Mater.2007,19,509.(30)Kato,M.;Shigeno,T.;Kimura,T.;Kuroda,K.Chem.Mater.2005,17,6416.(31)Kruk,M.;Celer,E.B.;Jaroniec,M.Chem.Mater.2004,16,698.Figure 3.Low-and high-magnification SEM image of nanosized CaCO 3.Figure 4.Low-and high-magnification SEM image of silicalite-1with intracrystal pores.1137Chem.Mater.,Vol.20,No.3,2008Intracrystal Pores within Silicalite-1Crystalfication of the surface of hydrophilic CaCO 3by fatty acid.In addition to the vibration modes assigned to calcite structure absorption,the absorption occurring around 2927and 2865cm -1are detected in the IR of hydrophobic CaCO 3(see the Supporting Information).They are due to the characteristic absorption of H -C -H asymmetric and sym-metric stretching vibrations,respectively,which result from the alkyl groups in the fatty acid.The IR data prove that the organic moieties are bound onto the surface of hydrophobic CaCO 3.Because of the difference in surface properties,only the hydrophilic nanosized CaCO 3can work well to yield the intracrystal pores in silicalite-1crystal.In the case of the synthesis using hydrophobic CaCO 3as a template,the last product is the conventional zeolite without the hierarchical pore.The hard template effect of the nanosized CaCO 3may be related to its hydrophilic property.This effect is different from the synthesis of mesoporous zeolite templated by carbon-based porous materials in the previous reports.5,6Because of the pores in carbon materials,the zeolite crystal growth proceeds within the void;subsequently,large zeolite single crystal grows and encapsulates the whole carbon particles.On the contrary,CaCO 3is a solid rather than porous material.However,there is a large number of hydroxyl groups on the surface of the hydrophilic nanosized CaCO 3.These highly active hydroxyl groups can give rise to strong interaction between SiO 2and CaCO 3.Because of this interaction,the nanosized CaCO 3dispersed in the silica gel is encapsulated into the crystal during the crystallization process.Because of the attachment of fatty acid to thesurfaceFigure 5.TEM images of silicalite-1synthesized in the presence of the nanosized CaCO 3.Figure 6.N 2adsorption/desorption isotherm of silicalite-1samples with intracrystal pores,and mesopore size distributions calculated from the adsorption branch by the BJH method.1138Chem.Mater.,Vol.20,No.3,2008Zhu et al.of hydrophilic CaCO3,the active hydroxyl groups may be protected.Therefore,it hinders the interaction between SiO2 and CaCO3.This phenomenon proves that the hydrophilic property of the nanosized CaCO3is essential to taking the template effect.ConclusionsIn conclusion,the preparation of silicalite-1single crystal with intracrystal pores in the range of50–100nm by using the nanosized CaCO3as a hard template is reported for the first time.The nanosized CaCO3can be trapped in the silicalite-1crystal during the crystallization process.By means of acid dissolution,the encapsulated nanoparticles are removed and give rise to the intracrystal pores within the zeolite crystal.The hydroxyl groups on the surface of CaCO3 are essential to taking the hard template effect.The combined use of X-ray diffraction,TEM,SEM image analysis,and N2adsorption/desorption proves that the synthesized material exhibits two levels of hierarchy in pore organization.The intracrystal pores correspond well to the morphology of the nanosized CaCO3,which confirms the effectiveness of nanosized CaCO3as a hard template in the creation of secondary pores within zeolite.Hierarchical zeolites combining an intrinsic micropore with an intracrystal mesopore and macropore system has shown unique properties in catalysis and otherfields.32–34Detailed studies of the synthesis,characterization,and catalytic reactivity of such porous zeolites are currently underway. Acknowledgment.We gratefully acknowledgefinancial support from the Major State Basic Research Development Program of the People’s Republic of China(2003CB615802).Supporting Information Available:XRD patterns and IR spectra(PDF).This material is available free of charge via the Internet at .CM071385O(32)Christensen,C.H.;Schmidt,I.;Carlsson,A.;Johannsen,K.;Herbst,K.J.Am.Chem.Soc.2005,127,8098.(33)Christensen,C.H.;Johannsen,K.;Schmidt,I.;Christensen,C.H.J.Am.Chem.Soc.2003,125,13370.(34)Schmidt,I.;Krogh,A.;Wienberg,K.;Carlsson,A.;Brorson,M.;Jacobsen,mun.2000,2157.1139Chem.Mater.,Vol.20,No.3,2008Intracrystal Pores within Silicalite-1Crystal。
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一般性描述 主要组件
TS15 共同术语，描述全站仪 Leica Viva Series。 组件 TS15 仪器 描述 • • • • 一款可进行测量，计算以及采集数据的全站仪。 包含多种不同精度级别的仪器。 集成 GNSSGNSS 系统，可构成 SmartStation。 结合多功能的 CS10/CS15 外业手簿实现遥控测量。
本手册中的符号含义： 类型 描述 表示一个可能遇到的危险情形，如果不加以避免，将导致严重伤害 甚至死亡事故。 表示潜在的或操作不当所致的危险情况，如果不加以避免，将造成 伤亡或严重损害。 表示潜在的或操作不当所致的危险情况，如果不加以避免，将造成 伤亡或严重损害 表示潜在的或操作不当所导致的危害，如果不加以避免，将导致轻 微的人身伤害或明显的设备、经济损失和环境的损害。 表示在实际使用中必须注意的重要章节，以便能够正确、有效地使 用该仪器。
临床试验cs评价报告
临床试验cs评价报告临床试验CS评价报告本次临床试验针对某特定疾病的治疗效果进行评价。
试验的目的是评估该疾病的治疗方案在临床应用中的有效性和安全性。
以下为该试验的详细内容及结果分析：1. 试验设计：本次试验采用随机对照实验设计。
参与者被随机分为实验组和对照组，实验组接受新的治疗方案，对照组接受传统治疗方案。
两组参与者的基线特征相似。
试验期为12个月，期间对参与者的相关数据进行收集和分析。
2. 参与者招募与筛选：参与者来自不同医疗机构。
招募标准包括与特定疾病的确诊、特定症状的存在等。
筛选过程严格按照入选标准进行，确保参与者的代表性和可比性。
3. 治疗方案介绍：实验组接受的治疗方案是基于前期临床研究的结果，具有一定理论依据和临床应用经验的新方案。
对照组接受的是当前社会上广泛应用的传统治疗方案。
两组方案都进行了详细的说明和操作流程。
4. 数据收集与分析：试验期间，对两组参与者进行定期随访，收集相关数据，包括疾病指标、生活质量评估、不良事件记录等。
收集到的数据经过统计学分析，运用适当的方法进行数据描述和比较。
同时，对不良事件进行分类和反应性评估。
5. 结果分析：根据收集到的数据和统计结果，对疾病指标、生活质量评估等进行比较分析。
通过统计学方法判断两组间的差异是否具有显著性，并计算相关的效应量。
同时，对不良事件发生率和严重程度进行统计描述。
6. 结论：根据结果分析，得出了对于治疗方案有效性和安全性的结论。
对实验组和对照组的疾病治疗效果进行综合评价。
此外，试验还可以提出对进一步研究的建议，包括样本量的增加、随访时间的延长、不同亚组的分析等。
总结：本次临床试验对某特定疾病的治疗方案进行了评价。
试验设计严谨，数据收集和分析方法合理。
通过对结果的分析和比较，可以为该特定疾病的临床治疗提供科学依据和参考。
该研究的结果对该特定疾病的治疗方案选择和优化具有重要的临床意义。
ISO 9000-2015基础与术语(E,20150915)
© ISO 2015Quality management systems — Fundamentals and vocabularySystèmes de management de la qualité — Principes essentiels et vocabulaireINTERNATIONAL STANDARDISO 9000Fourth edition 2015-09-15Reference number ISO 9000:2015(E)ISO 9000:2015(E)ii© ISO 2015 – All rights reservedCOPYRIGHT PROTECTED DOCUMENT© ISO 2015, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of the requester.ISO copyright officeCh. de Blandonnet 8 • CP 401CH-1214 Vernier, Geneva, Switzerland Tel. +41 22 749 01 11Fax +41 22 749 09 47copyright@ --`,,,``,`````,,``,,,``,`,,,-`-`,,`,,`,`,,`---ISO 9000:2015(E)Contents Page Foreword (iv)Introduction (v)1 Scope (1)2 Fundamental concepts and quality management principles (1)2.1 General (1)2.2 Fundamental concepts (2)2.2.1 Quality (2)2.2.2 Quality management system (2)2.2.3 Context of an organization (2)2.2.4 Interested parties (2)2.2.5 Support (2)2.3 Quality management principles (3)2.3.1 Customer focus (3)2.3.2 Leadership (4)2.3.3 Engagement of people (5)2.3.4 Process approach (6)2.3.5 Improvement (6)2.3.6 Evidence-based decision making (7)2.3.7 Relationship management (8)2.4 Developing the QMS using fundamental concepts and principles (9)2.4.1 QMS model (9)2.4.2 Development of a QMS (9)2.4.3 QMS standards, other management systems and excellence models (10)3 Terms and definitions (10)3.1 Terms related to person or people (10)3.2 Terms related to organization (11)3.3 Terms related to activity (13)3.4 Terms related to process (15)3.5 Terms related to system (16)3.6 Terms related to requirement (18)3.7 Terms related to result (20)3.8 Terms related to data, information and document (23)3.9 Terms related to customer (25)3.10 Terms related to characteristic (26)3.11 Terms related to determination (27)3.12 Terms related to action (29)3.13 Terms related to audit (30)Annex A (informative) Concept relationships and their graphical representation (33)Bibliography (47)Alphabetical index of terms (49)© ISO 2015 – All rights reserved iiiISO 9000:2015(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see /directives). Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see /patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISO’s adherence to World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: /iso/foreword.html. The committee responsible for this document is Technical Committee ISO/TC 176, Quality management and quality assurance, Subcommittee SC 1, Concepts and terminology.This fourth edition cancels and replaces the third edition (ISO 9000:2005), which has been technically revised.iv© ISO 2015 – All rights reservedISO 9000:2015(E)IntroductionThis International Standard provides the fundamental concepts, principles and vocabulary for quality management systems (QMS) and provides the foundation for other QMS standards. This International Standard is intended to help the user to understand the fundamental concepts, principles and vocabulary of quality management, in order to be able to effectively and efficiently implement a QMS and realize value from other QMS standards.This International Standard proposes a well-defined QMS, based on a framework that integrates established fundamental concepts, principles, processes and resources related to quality, in order to help organizations realize their objectives. It is applicable to all organizations, regardless of size, complexity or business model. Its aim is to increase an organization’s awareness of its duties and commitment in fulfilling the needs and expectations of its customers and interested parties, and in achieving satisfaction with its products and services.This International Standard contains seven quality management principles supporting the fundamental concepts described in 2.2. In 2.3, for each quality management principle, there is a “statement” describing each principle, a “rationale” explaining why the organization would address the principle, “key benefits” that are attributed to the principles, and “possible actions” that an organization can take in applying the principle.This International Standard contains the terms and definitions that apply to all quality management and QMS standards developed by ISO/TC 176, and other sector-specific QMS standards based on those standards, at the time of publication. The terms and definitions are arranged in conceptual order, with an alphabetical index provided at the end of the document. Annex A includes a set of diagrams of the concept systems that form the concept ordering.NOTE Guidance on some additional frequently-used words in the QMS standards developed by ISO/TC 176, and which have an identified dictionary meaning, is provided in a glossary available at: http://www.iso. org/iso/03_terminology_used_in_iso_9000_family.pdf--`,,,``,`````,,``,,,``,`,,,-`-`,,`,,`,`,,`---© ISO 2015 – All rights reserved v--`,,,``,`````,,``,,,``,`,,,-`-`,,`,,`,`,,`---Quality management systems — Fundamentals and vocabulary1 ScopeThis International Standard describes the fundamental concepts and principles of quality management which are universally applicable to the following:— organizations seeking sustained success through the implementation of a quality management system;— customers seeking confidence in an organization’s ability to consistently provide products andservices conforming to their requirements;— organizations seeking confidence in their supply chain that product and service requirements willbe met;— organizations and interested parties seeking to improve communication through a commonunderstanding of the vocabulary used in quality management;— organizations performing conformity assessments against the requirements of ISO 9001;— providers of training, assessment or advice in quality management;— developers of related standards.This International Standard specifies the terms and definitions that apply to all quality management and quality management system standards developed by ISO/TC 176.2 Fundamental concepts and quality management principles2.1 GeneralThe quality management concepts and principles described in this International Standard give the organization the capacity to meet challenges presented by an environment that is profoundly different from recent decades. The context in which an organization works today is characterized by accelerated change, globalization of markets and the emergence of knowledge as a principal resource. The impact of quality extends beyond customer satisfaction: it can also have a direct impact on the organization’s reputation.Society has become better educated and more demanding, making interested parties increasingly more influential. By providing fundamental concepts and principles to be used in the development of a quality management system (QMS), this International Standard provides a way of thinking about the organization more broadly.All concepts, principles and their interrelationships should be seen as a whole and not in isolation of each other. No individual concept or principle is more important than another. At any one time, finding the right balance in application is critical.INTERNATIONAL STANDARD ISO 9000:2015(E)© ISO 2015 – All rights reserved1N o r e p r o d u c t i o n o r n e t w o r k i n g p e r m i t t e d w i t h o u t l i c e n s e f r o m I H SISO 9000:2015(E)2.2 Fundamental concepts2.2.1 QualityAn organization focused on quality promotes a culture that results in the behaviour, attitudes, activities and processes that deliver value through fulfilling the needs and expectations of customers and other relevant interested parties.The quality of an organization’s products and services is determined by the ability to satisfy customers and the intended and unintended impact on relevant interested parties.The quality of products and services includes not only their intended function and performance, but also their perceived value and benefit to the customer.2.2.2 Quality management systemA QMS comprises activities by which the organization identifies its objectives and determines the processes and resources required to achieve desired results.The QMS manages the interacting processes and resources required to provide value and realize results for relevant interested parties.The QMS enables top management to optimize the use of resources considering the long and short term consequences of their decision.A QMS provides the means to identify actions to address intended and unintended consequences in providing products and services.2.2.3 Context of an organizationUnderstanding the context of the organization is a process. This process determines factors which influence the organization’s purpose, objectives and sustainability. It considers internal factors such as values, culture, knowledge and performance of the organization. It also considers external factors such as legal, technological, competitive, market, cultural, social and economic environments. Examples of the ways in which an organization’s purpose can be expressed include its vision, mission, policies and objectives.2.2.4 Interested partiesThe concept of interested parties extends beyond a focus solely on the customer. It is important to consider all relevant interested parties.Part of the process for understanding the context of the organization is to identify its interested parties. The relevant interested parties are those that provide significant risk to organizational sustainability if their needs and expectations are not met. Organizations define what results are necessary to deliver to those relevant interested parties to reduce that risk. Organizations attract, capture and retain the support of the relevant interested parties they depend upon for their success.2.2.5 Support2.2.5.1 GeneralTop management support of the QMS and engagement of people enables:— provision of adequate human and other resources;— monitoring processes and results;2 © ISO 2015 – All rights reservedISO 9000:2015(E)— determining and evaluating of risks and opportunities;— implementing appropriate actions.Responsible acquisition, deployment, maintenance, enhancement and disposal of resources support the organization in achieving its objectives.2.2.5.2 PeoplePeople are essential resources within the organization. The performance of the organization is dependent upon how people behave within the system in which they work.--`,,,``,`````,,``,,,``,`,,,-`-`,,`,,`,`,,`---Within an organization, people become engaged and aligned through a common understanding of the quality policy and the organization’s desired results.2.2.5.3 CompetenceA QMS is most effective when all employees understand and apply the skills, training, education and experience needed to perform their roles and responsibilities. It is the responsibility of top management to provide opportunities for people to develop these necessary competencies.2.2.5.4 AwarenessAwareness is attained when people understand their responsibilities and how their actions contribute to the achievement of the organization’s objectives.2.2.5.5 CommunicationPlanned and effective internal (i.e. throughout the organization) and external (i.e. with relevant interested parties) communication enhances people’s engagement and increased understanding of:— the context of the organization;— the needs and expectations of customers and other relevant interested parties;— the QMS.2.3 Quality management principles2.3.1 Customer focus2.3.1.1 StatementThe primary focus of quality management is to meet customer requirements and to strive to exceed customer expectations.2.3.1.2 RationaleSustained success is achieved when an organization attracts and retains the confidence of customers and other relevant interested parties. Every aspect of customer interaction provides an opportunity to create more value for the customer. Understanding current and future needs of customers and other interested parties contributes to the sustained success of the organization.2.3.1.3 Key benefitsSome potential key benefits are:— increased customer value;© ISO 2015 – All rights reserved 3ISO 9000:2015(E)— increased customer satisfaction;— improved customer loyalty;— enhanced repeat business;— enhanced reputation of the organization;— expanded customer base;— increased revenue and market share.2.3.1.4 Possible actionsPossible actions include:— recognize direct and indirect customers as those who receive value from the organization;— understand customers’ current and future needs and expectations;— link the organization’s objectives to customer needs and expectations;— communicate customer needs and expectations throughout the organization;— plan, design, develop, produce, deliver and support products and services to meet customer needs and expectations;— measure and monitor customer satisfaction and take appropriate actions;— determine and take action on relevant interested parties’ needs and appropriate expectations that can affect customer satisfaction;— actively manage relationships with customers to achieve sustained success.2.3.2 Leadership2.3.2.1 StatementLeaders at all levels establish unity of purpose and direction and create conditions in which people are engaged in achieving the organization’s quality objectives.2.3.2.2 RationaleCreation of unity of purpose and the direction and engagement of people enable an organization to align its strategies, policies, processes and resources to achieve its objectives.2.3.2.3 Key benefitsSome potential key benefits are:— increased effectiveness and efficiency in meeting the organization’s quality objectives;— better coordination of the organization’s processes;— improved communication between levels and functions of the organization;— development and improvement of the capability of the organization and its people to deliver desired results.--`,,,``,`````,,``,,,``,`,,,-`-`,,`,,`,4 © ISO 2015 – All rights reserved2.3.2.4 Possible actionsPossible actions include:— communicate the organization’s mission, vision, strategy, policies and processes throughout the organization;— create and sustain shared values, fairness and ethical models for behaviour at all levels of the organization;— establish a culture of trust and integrity;— encourage an organization-wide commitment to quality;— ensure that leaders at all levels are positive examples to people in the organization;— provide people with the required resources, training and authority to act with accountability;— inspire, encourage and recognize the contribution of people.2.3.3 Engagement of people2.3.3.1 StatementCompetent, empowered and engaged people at all levels throughout the organization are essential to enhance the organization’s capability to create and deliver value.2.3.3.2 RationaleIn order to manage an organization effectively and efficiently, it is important to respect and involve all people at all levels. Recognition, empowerment and enhancement of competence facilitate the engagement of people in achieving the organization’s quality objectives.2.3.3.3 Key benefitsSome potential key benefits are:— improved understanding of the organization’s quality objectives by people in the organization and increased motivation to achieve them;— enhanced involvement of people in improvement activities;— enhanced personal development, initiatives and creativity;— enhanced people satisfaction;— enhanced trust and collaboration throughout the organization;— increased attention to shared values and culture throughout the organization.2.3.3.4 Possible actionsPossible actions include:— communicate with people to promote understanding of the importance of their individual contribution;— promote collaboration throughout the organization;— facilitate open discussion and sharing of knowledge and experience;— empower people to determine constraints to performance and to take initiatives without fear;© ISO 2015 – All rights reserved 5— recognize and acknowledge people’s contribution, learning and improvement;— enable self-evaluation of performance against personal objectives;— conduct surveys to assess people’s satisfaction, communicate the results and take appropriate actions.2.3.4 Process approach2.3.4.1 StatementConsistent and predictable results are achieved more effectively and efficiently when activities are understood and managed as interrelated processes that function as a coherent system.2.3.4.2 RationaleThe QMS consists of interrelated processes. Understanding how results are produced by this system enables an organization to optimize the system and its performance.2.3.4.3 Key benefitsSome potential key benefits are:— enhanced ability to focus effort on key processes and opportunities for improvement;— consistent and predictable outcomes through a system of aligned processes;— optimized performance through effective process management, efficient use of resources and reduced cross-functional barriers;— enabling the organization to provide confidence to interested parties related to its consistency, effectiveness and efficiency.2.3.4.4 Possible actionsPossible actions include:— define objectives of the system and processes necessary to achieve them;— establish authority, responsibility and accountability for managing processes;— understand the organization’s capabilities and determine resource constraints prior to action;— determine process interdependencies and analyse the effect of modifications to individual processes on the system as a whole;— manage processes and their interrelations as a system to achieve the organization’s quality objectives effectively and efficiently;— ensure the necessary information is available to operate and improve the processes and to monitor, analyse and evaluate the performance of the overall system;— manage risks which can affect outputs of the processes and overall outcomes of the QMS.2.3.5 Improvement2.3.5.1 StatementSuccessful organizations have an ongoing focus on improvement.6 © ISO 2015 – All rights reserved N o r e p r o d u c t i o n o r n e t w o r k i n g p e r m i t t e d w i t h o u t l i c e n s e f r o m I H S2.3.5.2 RationaleImprovement is essential for an organization to maintain current levels of performance, to react to changes in its internal and external conditions and to create new opportunities.2.3.5.3 Key benefitsSome potential key benefits are:— improved process performance, organizational capability and customer satisfaction;— enhanced focus on root cause investigation and determination, followed by prevention and corrective actions;— enhanced ability to anticipate and react to internal and external risks and opportunities;— enhanced consideration of both incremental and breakthrough improvement;— improved use of learning for improvement;— enhanced drive for innovation.2.3.5.4 Possible actionsPossible actions include:— promote establishment of improvement objectives at all levels of the organization;— educate and train people at all levels on how to apply basic tools and methodologies to achieve improvement objectives;— ensure people are competent to successfully promote and complete improvement projects; --`,,,``,`````,,``,,,``,`,,,-`-`,,`,,`,`,,`---— develop and deploy processes to implement improvement projects throughout the organization;— track, review and audit the planning, implementation, completion and results of improvement projects;— integrate improvement consideration into development of new or modified products and services and processes;— recognize and acknowledge improvement.2.3.6 Evidence-based decision making2.3.6.1 StatementDecisions based on the analysis and evaluation of data and information are more likely to produce desired results.2.3.6.2 RationaleDecision-making can be a complex process and it always involves some uncertainty. It often involves multiple types and sources of inputs, as well as their interpretation, which can be subjective. It is important to understand cause and effect relationships and potential unintended consequences. Facts, evidence and data analysis lead to greater objectivity and confidence in decision making.2.3.6.3 Key benefitsSome potential key benefits are:— improved decision making processes;© ISO 2015 – All rights reserved 7— improved assessment of process performance and ability to achieve objectives;— improved operational effectiveness and efficiency;— increased ability to review, challenge and change opinions and decisions;— increased ability to demonstrate the effectiveness of past decisions.2.3.6.4 Possible actionsPossible actions include:— determine, measure and monitor key indicators to demonstrate the organization’s performance;— make all data needed available to the relevant people;— ensure that data and information are sufficiently accurate, reliable and secure;— analyse and evaluate data and information using suitable methods;— ensure people are competent to analyse and evaluate data as needed;— make decisions and take actions based on evidence, balanced with experience and intuition.2.3.7 Relationship management2.3.7.1 StatementFor sustained success, organizations manage their relationships with relevant interested parties, such as providers.2.3.7.2 RationaleRelevant interested parties influence the performance of an organization. Sustained success is more likely to be achieved when the organization manages relationships with all of its interested parties to optimize their impact on its performance. Relationship management with its provider and partner networks is of particular importance.2.3.7.3 Key benefitsSome potential key benefits are:— enhanced performance of the organization and its relevant interested parties through responding to the opportunities and constraints related to each interested party;— common understanding of objectives and values among interested parties;— increased capability to create value for interested parties by sharing resources and competence and managing quality related risks;--`,,,``,`````,,``,,,``,`,,,-`-`,,`,,`,`,,`---— a well-managed supply chain that provides a stable flow of products and services.2.3.7.4 Possible actionsPossible actions include:— determine relevant interested parties (such as providers, partners, customers, investors, employees or society as a whole) and their relationship with the organization;— determine and prioritize interested party relationships that need to be managed;8 © ISO 2015 – All rights reserved— establish relationships that balance short-term gains with long-term considerations;— gather and share information, expertise and resources with relevant interested parties;— measure performance and provide performance feedback to interested parties, as appropriate, to enhance improvement initiatives;— establish collaborative development and improvement activities with providers, partners and other interested parties;— encourage and recognize improvements and achievements by providers and partners.2.4 Developing the QMS using fundamental concepts and principles2.4.1 QMS model2.4.1.1 GeneralOrganizations share many characteristics with humans as a living and learning social organism. Both are adaptive and comprise interacting systems, processes and activities. In order to adapt to their varying context, each needs the ability to change. Organizations often innovate to achieve breakthrough improvements. An organization’s QMS model recognizes that not all systems, processes and activities can be predetermined; therefore it needs to be flexible and adaptable within the complexities of the organizational context.2.4.1.2 SystemOrganizations seek to understand the internal and external context to identify the needs and expectations of relevant interested parties. This information is used in the development of the QMS to achieve organizational sustainability. The outputs from one process can be the inputs into other processes and are interlinked into the overall network. Although often appearing to be comprised of similar processes, each organization and its QMS is unique.2.4.1.3 ProcessesThe organization has processes that can be defined, measured and improved. These processes interact to deliver results consistent with the organization’s objectives and cross functional boundaries. Some processes can be critical while others are not. Processes have interrelated activities with inputs to deliver outputs.2.4.1.4 ActivityPeople collaborate within a process to carry out their daily activities. Some activities are prescribed and depend on an understanding of the objectives of the organization, while others are not and react to external stimuli to determine their nature and execution.2.4.2 Development of a QMSA QMS is a dynamic system that evolves over time through periods of improvement. Every organization has quality management activities, whether they have been formally planned or not. This International Standard provides guidance on how to develop a formal system to manage these activities. It is necessary to determine activities which already exist in the organization and their suitability regarding the context of the organization. This International Standard, along with ISO 9004 and ISO 9001, can then be used to assist the organization to develop a cohesive QMS.A formal QMS provides a framework for planning, executing, monitoring and improving the performance of quality management activities. The QMS does not need to be complicated; rather it needs to accurately© ISO 2015 – All rights reserved 9。
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2 Enhanced Cell Reselection Mechanism for Heterogeneous Wireless System 2.1 Cell Reselection Mechanism in 3GPP TS 36.304
We first present cell reselection process defined in the latest technical specification (TS) [1] in 3GPP protocol in a mathematical manner. This protocol is essentially designed for 3GPP cellular wireless system. To provide more theoretical insight, we model the system in a general manner. Consider 4G LTE system and its evolution
Title Suppressed Due to Excessive Length
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scenario, where adjacent macro evolved node Bs(MeNBs) form wide-area coverage for UEs in each corresponding cell (macro cell), and low power nodes (LPNs) within each cell form hot-spot coverage. The criterion for UE to perform cell reselection is the value of reference signal power denoted by Pk , where k denotes the index of different types of nodes and cells. In real application scenarios, all overlapping RAT cells in the heterogeneous wireless system have the rank of priority, according to which UE will perform cell reselection to the specific cell when Pk meets certain thresholds requirements. Priority rank parameters are broadcasted to all UE by system information or dedicated signallings [1]. For UE that has camped on others cells adjacent to cell k, if Pk is large enough, the UE will try to reselect to cells k for better access service. Define Tkin as the threshold for Pk when UE tries to camp on cell k, above which UE will try to perform cell reselection to cell k. For UE already camped on cell k, if Pk is too small, it will try to reselect to other cells. Define Tkout as the threshold for Pk when UE tries to camp on other cells, below which UE will try to perform cell reselection to other cells. Assume UE currently camps on cell k, and try to perform cell reselection to other cells with different priority ranks. Let the cell with index h represent the cell with higher priority, and let the cell with index l represent the cell with lower priority. The algorithm for cell reselection is summarized as follows: • If Ph > Thin holds for a consecutive time treselection , UE shall perform cell reselection from cell k to cell h. • If Pl > Tlin and Pk < Tkout hold for a consecutive time treselection , UE shall perform cell reselection from cell k to cell l . If more than one cell meet the above requirements, UE shall perform cell reselection to the cell with highest priority.
Analysis for the Enhanced Cell Reselection Mechanism in Heterogeneous Wireless System
Xinran Zhang, Songlin Sun
Abstract This work proposes an enhanced algorithm for cell reselection mechanism in heterogeneous wireless system. A Markov model based analytical method is proposed to describe system behavior and derive performance metric. The optimal QoS control parameter for the algorithm is derived based on system model and analysed in numerical results. It is shown the network performance can be improved by utilizing the proposed algorithm, and the optimal value of QoS control parameter varies according to system traffic condition, which provides insight for network deployment and radio resource ll reselection process of user equipment (UE) is an important physical-layer process of cellular wireless communication system. It is defined and described in third generation partner project (3GPP) physical layer specifications [1, 2], and essentially specifies UE’s behavior to choose other access cells when the power or quality of the received signal varies. In tradition simple scenarios of cellular system like Global System for Mobile Communication (GSM) system or third generation (3G) Wideband Code Division Multiple Access (WCDMA) system, the radio access network (RAN) is constituted by the so-called macro cells, where the base station (BS) or node B (NB) serves as the access point for UEs in a wide coverage area. In that case the cell reselection behavior happens when UE moves through the edge of different cells and requires handoff to the cell with best access quality. This sXinran Zhang Beijing Univ. of Posts and Telecomm., No.10 Xitucheng Road, Beijing e-mail: zhangxr.wspn@ Songlin Sun Beijing Univ. of Posts and Telecomm., No.10 Xitucheng Road, Beijing e-mail: slsun@
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Xinran Zhang, Songlin Sun
cenario can be construed as homogeneous wireless system. With the emergence of fourth generation (4G)long term evolution (LTE) standard and its rapid deployment around the world, more complex network scenarios unlike traditional homogeneous wireless system are introduced and referred as the heterogeneous wireless systems. The concept of heterogeneity and its related theories have become heated research topics in the past decade. In the family of 3GPP cellular systems, the typical scenario of heterogeneous wireless system consists of GSM system, Enhanced Data Rate for GSM Evolution (EDGE) system, WCDMA system, LTE system, and even in the future, fifth generation (5G) system. Within theses systems, different nodes are involved such as pico nodes and femto nodes, along with macro nodes deployed in a overlapping manner. To make the scenario more complicated, the wireless local area network (WLAN) system are also considered in heterogeneous wireless system, since the convergence of different radio access technologies (RATs) is a fundamental aspect for 3GPP cellular system and an inevitable trend of future wireless communication system. These conditions provide a much more complicated scenario for UE mobility management problem, in which the cell reselection problem has already become an important technique applied in current cellular wireless systems as well as an interesting theoretical research point. In the field of mobility management and radio resource management (RRM) research, the Markov-related model is extensively studied and discussed in existing literatures [3] - [7] due to its accuracy, simplicity and validity, and is considered to be an ideal research methodology to model the cell reselection mechanism in heterogeneous wireless system. In this work we first present the proposed mechanism for cell reselection in heterogeneous wireless system defined in 3GPP specifications, then derived a Markov model based analytical method for the system to obtain system performance metric, then provide detailed analysis for optimal parameter in the algorithm. The paper is organized as follows: in Section 2 the cell reselection mechanism in [1] and the proposed algorithm is described. Then in Section 3 we present the mathematical model for the system, and derived the optimal parameter solutions to the model. Section 4 presents the main results for the optimal quality of service (QoS) parameter analysis. Section 5 concludes the paper.