USP天平41及1251中英对照

1、USP36 天平（中英文）2013-12-11 17:36:56|分类： HYPERLINK /blog/ l m=0&t=1&c=fks_084070082083084068086081080095093094087074080081084068 o USP USP |标签： |举报 |字号大中小订阅 Change to read:This chapter states the requirements for balances used for materials that must be accurately weighed (see General Notices, 8.20). Un

2、less otherwise specified, when substances must be “accurately weighed”, the weighing shall be performed using a balance that is calibrated over the operating range and meets the requirements defined for repeatability and accuracy. For balances used for other applications, the balance repeatability a

3、nd accuracy should be commensurate with the requirements for its use.本章说明了用于必须“精密称定”（参见凡例8.20）的物料称量的天平的要求。除非另有说明，如果必须“精密称定”，则应采用在称量范围内经过校正，并且符合重复性和准确性要求的天平来称量。对于其它用途的天平，天平的重复性和准确度应根据其用途要求来确定。For discussion of the theoretical basis of these requirements, see general information chapter Weighing on an

4、 Analytical Balance 1251 , which may be a helpfulbut not mandatoryresource.关于这些要求的理论基础的讨论，参见凡例，可能会有帮助但不是必须。REPEATABILITY 重复性Repeatability is assessed by weighing one test weight NLT 10 times. NOTE The test weight must bewithin the balances operating range, but the weight need not be calibrated. Beca

5、use repeatability is virtually independent of sample mass within the balances capacity, use of a small test weight, which may be difficult to handle, is not required. 重复性采用对一个重量测试不少于10次来评估。【注用于测试的重量必须是在天平的称量范围内，但该砝码是不需要校正的。因为重复性实际上取决于天平称量能力内样品的重量，由于很小的砝码可能比较难操作，因此不一定必须使用很小的那个。】Repeatability is satis

6、factory if two times the standard deviation of the weighed value, divided by the nominal value of the weight used, does not exceed 0.10%. If the standard deviation obtained is less than 0.41d , where d is the scale interval, replace this standard deviation with 0.41d . In this case, repeatability is

7、 satisfactory if two times 0.41d , divided by the nominal value of the weight used, does not exceed 0.10%.如果各次所称得的重量值的标准偏差的2倍，除以所用砝码的名义重量值，不超过0.10%，则认为重复性满足要求。如果所得的标准偏差小于0.41d，这里d值是分度值，则采用0.41d替代该标准偏差。这种情况下，如果0.41d的2倍，除以所用砝码的名义重复值，不超过0.10%，则认为重复性满足要求。ACCURACY 准确度The accuracy of a balance is satisfac

8、tory if its weighing value, when tested with a suitable weight(s), is within 0.10% of the test weight value.如果采用一个适当的砝码，其称量值与标准值的差值在标准值的+/-0.10%以内，则认为天平的准确度满足要求。A test weight is suitable if it has a mass between 5% and 100% of the balances capacity. The test weights maximum permissible error (mpe),

9、or alternatively its calibration uncertainty, shall be NMT one-third of the applied test limit of the accuracy test. 适当的砝码是指其重量在天平的最大量程的5%-100%之间的重量。测试用砝码的最大允许偏差（mpe），或其校正不确定度，应不超过所使用的准确度测试的检测限的1/3。 NOTE Applicable standards are the following: ASTM E617 (available from HYPERLINK ) and OIML R 111 (av

10、ailable from HYPERLINK ). 【注适用标准引用ASTM E617】2S ( USP36 )Auxiliary Information Please check for your question in the FAQs before contacting USP.USP36NF31 Page 53USP36NF31 Supplement : No. 2 Page 6136USP37使用分析天平称量（中英文）2013-12-31 15:08:35|分类： HYPERLINK /blog/ l m=0&t=1&c=fks_084070082083084068086081080

11、095093094087074080081084068 o USP USP |标签： |举报 |字号大中小订阅 WEIGHING ON AN ANALYTICAL BALANCE使用分析天平称量（本文件来自USP37-NF32，目前尚未实施，信息仅供参考）INTRODUCTION 介绍Weighing is a frequent step in analytical procedures, and the balance is an essential piece of laboratory equipment. The general information described here a

12、pplies directly to electronic balances used in analytical procedures. Although many portions of the chapter are applicable to all balances, some are applicable only to analytical balances. This chapter should not be considered all-inclusive, and other sources of information (e.g., the US National In

13、stitute for Science and Technology and balance manufacturers) may be useful and applicable when analysts perform a weighing operation or implement a weighing procedurei National Physical Laboratory. Good practice guide No. 70, weighing in the pharmaceutical industry. 2004. http:/resource.npl.co.uk/d

14、ocs/science_technology/mass_force_pressure/clubs_groups/instmc_weighing_panel/pharmaweigh.pdf. Accessed 21 March 2012. NOTENomenclature in this chapter tends to follow this document, except where it conflicts with USP terms. iii American Society for Testing and Materials, E896 Standard test method o

15、f testing top-loading, direct-reading laboratory scales and balances. 2005 HYPERLINK /standards/E896.htm.%20Accessed%2021%20March%202012 /standards/E896.htm. Accessed 21 March 2012.ii. The information given in this chapter is applicable not only to balances used for materials that must be accurately

16、 weighed (see Balances 41 ) but also to balances used in all analytical procedures.称重在分析程序中是一个很频繁的操作，天平是化验室的基本设备。这里的一般信息适用于在分析过程中使用的电子天平。尽管本章节的一部分也适用于所有天平，一些仅适用于分析天平。本章不应作为包括所有的文件，一些其它来源的信息（例如，美国国家科学技术研究所和天平生产商）可能也很有用，适用于化验员进行称量操作，或实施称重程序。本章中给出的信息不仅适用于必须精密称定的物质（参见），同时也适用于所有分析过程中使用的天平。QUALIFICATION 确

17、认Users should consult Analytical Instrument Qualification 1058 , standard operating procedures, and recommendations from manufacturers when they devise qualification plans.用户在设计其确认计划时，应参考，标准操作规程，和生产商的推荐。Installation 安装 The balances performance depends on the conditions of the facility where it is in

18、stalled. Analysts should consult information provided by the manufacturer before they install a balance.天平的性能取决于其安装所处的环境。在安装天平前，化验员应参考供应商给出的信息。Support surface: The balance should be installed on a solid, level, nonmagnetic surface that minimizes the transmission of vibration (e.g., a floor-mounted,

19、granite weigh bench). If a metallic support surface is used, the surface should be grounded in order to prevent the buildup of static electricity.支持台面：天平应安装在坚固、水平、无磁场的平面，尽量减少震动传递（例如，安装在地板，花岗岩称重台）。如果采用了金属的支持台面，表面应接地，以避免静电聚积。Location: If possible, the balance should be located in a room that is temper

20、ature and humidity controlled. The location should have a clean, consistent electrical power supply. The location should be free of drafts and should not be near ovens, furnaces, air conditioner ducts, or cooling fans from equipment or computers.位置：如果可能，天平应安装在一个温湿度可控的房间。位置应清洁，具有持续的电力供应。位置应不会产生波动，不靠近

21、烘箱、马弗炉、空调送回风罩，或设备、空调的冷却风扇。The balance should be positioned away from outside windows so that direct sunlight does not strike the balance. The balance should not be installed near sources of electromagnetic radiation such as radiofrequency generators, electric motors, or hand-held communication devic

22、es (including cordless telephones, cellular telephones, and walkie-talkies). The balance should not be located near magnetic fields induced by laboratory instrumentation or other equipment.天平位置应远离窗户，以避免直接阳光照射。天平安装不应靠近电磁辐射源，如无线频率发向射源，电子马达，或手动通话设施（包括无绳电话、手机、手提无线电话机）。天平不应安装在化验室设备或其它设备产生的磁场区域附近。The perf

23、ormance of the balance should be assessed following installation and before use in order to demonstrate adequate performance. In some situations, it may not be possible to position the balance in an optimum environment. Examples of potential facility issues include the following:天平的性能在安装后使用前应进行评估，以证

24、明其性能符合要求。在某些情况下，可能无法将天平安装在一个理想的环境。潜在的设施问题包括以下：1. Air currents sometimes are present in the laboratory.化验室中有时会有气流2. Temperatures in the laboratory vary excessively (check the manufacturers literature about temperature sensitivity).化验室温度有时会快速波动（检查供应商关于温度敏感性的说明）3. Humidity is either very low or very hi

25、gh. Either condition may increase the rate at which the sample weight varies because of pickup or loss of water. Low humidity increases the buildup of static electricity.湿度可能会很低或很高。由于失水或吸水，太高或太低都会影响样品重量变动的速度。低湿度会增加静电积聚。4. Adjacent operations are causing vibration.邻近操作产生震动5. Corrosive materials are u

26、sed nearby or are routinely weighed.附近使用腐蚀性材料，或常规称量腐蚀性物料6. The balance is located within a fume hood because it is used to weigh corrosive or hazardous materials.由于天平用于称量腐蚀性或危险性物料，因此安装在排烟罩内7. The balance is adjacent to equipment that produces a magnetic field (e.g., a magnetic stirrer).天平邻近产生磁场的设备（例

27、如，电磁搅拌器）8. Direct sunlight strikes the balance.天平有直接太阳光照In situations when the balance is located near equipment or systems that induce vibration, drafts, electromagnetic radiation, magnetic fields, or changes in temperature or humidity, the assessment should be conducted with those systems operatin

28、g in order to duplicate a worst-case scenario.如果天平位置接近产生震动、摆动、电磁辐射、磁场或温湿度变化的设备，则需要对这些系统在操作状态下进行评估，以重复最差情况环境。Operational Qualification 运行确认An operational qualification should be performed either by the user or by a qualified third-party vendor after the equipment has been installed.在天平安装后，应由用户或第三方供应商

29、进行运行确认。As a minimum, the power should be turned on and the balance should be allowed to equilibrate according to the manufacturers instructions (124 h, depending on the type of balance) before use. Depending on the balance, analysts should include the following procedures in the operational qualific

30、ation:最低要求，要打开电源，根据生产商的要求，在使用前让天平平衡（1-24小时，根据型号不同而不同）。根据天平型号，化验员应在运行确认中包括以下程序：1. Mechanical mobility of all moveable parts所有可移动部件机械动态2. Control of stable indication稳定指示的控制3. Manually triggered or automatic adjustment by means of built-in weights内置砝码的手动或自动调节4. Operation of ancillary equipment辅助设备的操作5

31、. Tare function去皮功能6. Initial calibration初始校正Several types of electronic analytical balances use built-in weights for manually triggered or automatic adjustment. This adjustment usually is applied to reduce the drift of the balance over time and to compensate for drifts caused by variations in the a

32、mbient temperature.一些电子分析天平使用内置砝码，可以进行手动或自动调节。这种调节一般用于减少天平随时间的漂移，对由于周围产生震动引起的漂移进行补偿。Calibration normally is performed as part of the operational qualification, but it also can be performed periodically thereafter. Calibration should be performed at the location where the balance is used in normal op

33、eration.校正一般作为运行确认的一部分实施，但也可以在之后进行周期性校正。校正应在天平所正常操作的原位进行。Performance Qualification 性能确认Table 1 provides a list of the most important balance properties that should be assessed during performance qualification. Depending on the risk of the application and the required weighing process tolerance, some

34、 of these tests may be omitted. Tests also can be omitted if there is evidence that the property in question has only minimal effect on the weighing performance. Any procedures used should be consistent with in-house standard operating procedures, applicable for the specific balance, and adequately

35、justified. Performance qualification should be performed periodically as described in standard operating procedures, and the frequency of each of the individual tests can vary depending on the criticality of the property.表1提供了一个天平最重要属性的清单，在性能确认中应该进行评估。根据应用的风险不同，要求的称重允差不同，有时该类测试可以省略。如果有证据表明该属性仅对称量性能形

36、成很小的影响，则也可以省略对其进行的测试。任何所用的程序均应与公司内部，适用于该特定天平的标准操作规程一致，并应进行充分判定。性能确认应按标准操作规程的描述周期实施，各测试的实施频率可能根据属性的关键程度不同而不同。The weights that are used to perform the tests should be stored and handled in a manner that minimizes contamination. Before executing the tests, the analyst should place the weights in the vi

37、cinity of the balance for an appropriate time to reach sufficient thermal equilibrium. If possible, all tests should be carried out with a single test weight in order to minimize handling errors, but multiple test weights are permitted.用于测试的砝码存贮和使用过程应能尽量减少污染。在进行测试前，化验员应将砝码放置在天平附近一段时间，以使其温度达到与环境温度平衡。

38、如有可能，所有测试均应采用同一个砝码，以尽可能减少操作误差，但使用多个砝码也是允许的。The tests should be recorded in such a manner that the data can be used to easily track balance performance and to assist in laboratory investigations as needed. Meaningful acceptance criteria can be set depending on the required weighing tolerance, i.e., t

39、he maximum allowed deviation permitted by specifications, regulations, etc., of a quantity to be weighed from its target value. Procedures should be in place to address test results that are outside acceptable ranges and to provide assurance that balance cleanliness and environment have not affected

40、 the result. Also, a procedure should be in place for removing a balance from operation when observed results fall outside acceptable ranges.测试过程要进行记录，数据应能很容易地追踪到天平性能，帮助化验室进行必要的调查。根据要求的称重误差，即质量标准、法规等允许的与目标重量值的最大允差，可以设定实际的可接受标准。应有程序说明测试超出可接受范围的结果，并保证天平的清洁和环境不会对结果产生影响。应有程序说明如果观察到结果超出可接受标准，则天平则不能继续使用。T

41、able 1. Suggested Performance Tests and Acceptance Criteria表1. 推荐性能确认测试和可接受标准Property 属性Definition 定义Examples 举例Acceptance Criteria 可接受标准Sensitivity Change in weighing value divided by the change in load, usually measured between zero and the capacity of the balance.The test load at or sufficiently

42、close to the capacity of the balance. NMT 0.05% deviation where 41 is applicable. For other uses, respective tolerance requirement divided by 2. 灵敏度称量值变动值除以载重变动值，一般在零点和天平最大载荷间测量测试载重接近天平最大载荷如果适用，则0.05%偏差其它情况，以相应的要求允差除以2Linearity Ability of a balance to follow the linear relationship between a load an

43、d the indicated weighing value. Nonlinearity usually is expressed as the largest magnitude of any linearity deviation within the test interval. From 3 to 6 points over the range of the balance. NMT 0.05% deviation where 41 is applicable. For other uses, respective tolerance requirement divided by 2.

44、 线性天平在载重和指示的重量之间保持线性关系的能力。非线性一般表达为在测试间隔内的任何线性偏差的最大级别天平范围内从3-6点如果适用，则0.05%偏差其它情况，以相应的要求允差除以2Eccentricity Deviation in the measurement value caused by eccentric loadingin other words, the asymmetrical placement of the center of gravity of the load relative to the load receiver. Eccentricity usually is

45、 expressed as the largest magnitude of any of the deviations between an off-center reading and the center reading for a given test load. Performed in the center of gravity and the four quadrants (for rectangular platter shapes) or at analogous locations for other platter shapes. Test load usually sh

46、ould be 30% of the capacity of the balance or higher (refer to the manufacturers manual for any possible upper limit). NMT 0.05% deviation where 41 is applicable. For other uses, respective tolerance requirement divided by 2. 偏心率由于偏心载重引起的测量值的偏差，换句话说，载重盘中心荷载不均匀。偏心率一般表达为对一个给定的载重，非中心放置时读数与中心放置时的读数的偏差最大

47、级别。测量四角称量值（四边形称量盘）或其它形状称量盘类似的位置。测试用载重一般为天平最大载重量的30%，或更高（参见供应商手册中建议的可用最高限值）如果适用，则0.05%偏差其它情况，以相应的要求允差除以2Repeatability Ability of a weighing instrument to display identical measurement values for repeated weighings of the same objects under the same conditions, e.g., the same measurement procedure, sa

48、me operator, same measuring system, same operating conditions, and same location over a short period of time. Repeatability usually is expressed as the standard deviation of multiple weighings. 10 replicate weighings (using a test weight that is a few percent of the nominal capacity of the balance).

49、 Requirement from 41 where applicable. For other uses, user specified requirements will apply. 重复性在相同条件下，一个称重设备对同一物体的重复称重显示同一测量值的能力，例如，采用同样的称量很多种，同样操作者，同一测量系统，同一操作条件，同一位置在较短时间内。重复性一般表达为重复称量的标准偏差。10次重复称量（采用天平名义载重能力的百分之几的测试砝码）如果适用，则按照要求。其它情况，用户指定适用的要求Sensitivity, linearity, and eccentricity all accoun

50、t for systematic deviations; i.e., they limit the accuracy of the balance (based on the definition of accuracy in Validation of Compendial Procedures 1225 and ICH Q2). In the International Vocabulary of Metrology (VIM) and documents of the International Organization for Standardization, this concept

51、 is referred to as trueness. Because deviations are largely independent from each other, it is not likely that all deviations occur simultaneously and have the same algebraic sign. 灵敏度、线性和偏心率均为系统性误差，即它们会局限天平的精密度（基于精密度定义，和ICH Q2）。在国际计量词汇（VIM）中，和国际标准化组织文件中，本根据被引用为真实性。因为偏差很大程度上相互独立，因此不可能所有偏差同时产生，并具有同向性

52、（即同时正负）。Therefore the arithmetic addition of all individual deviations to assess the balance accuracy would constitute a rather conservative approach. A quadratic addition of the individual deviations is a more realistic approach. By allocating 50% of the weighing tolerance budget to the acceptance

53、criteria of the individual properties, e.g., sensitivity, linearity, and eccentricity, analysts ensure adherence to the required weighing tolerance. Therefore, the acceptance criteria for the individual properties that account for the systematic deviations are set to weighing tolerance divided by 2.

54、 These propertiesor a subset of them also can be taken to fulfill the accuracy requirement described in 41 . In this case the acceptance criteria thus allow a maximum deviation of 0.05% for sensitivity, linearity, and eccentricity. Repeatability preferably is tested with a test weight of a few perce

55、nt of the balance capacity. At the lower end of its measurement range, the performance of laboratory balances is limited by the finite repeatability, and limitations induced by systematic deviations normally can be neglected. Therefore, the whole weighing tolerance budget can be allocated to the acc

56、eptance criterion of the repeatability test.因此，采用所有单个误差的算术加和，来评估天平的准确度是一种较为保守的方法。采用单个偏差的二次加和是一种更现实的方法。将各单个属性的可接受标准置为称量允差的50%，如，灵敏度、线性和偏心率，化验员可以保证达到所需的称量允差。这样，单个属性的可接受标准作为系统误差设定为称量允差除以2。这些属性或属性的子集也可以认为是满足中描述的精密度要求。在这种情况下，可接受标准允许最大偏差为灵敏度、线性和偏心率的0.05%。重复性最好采用一个天平最大载重量百分之几重量的砝码测试。在测量范围的低值端，化验室天平的性能由有限次数

57、重复性所限度，由系统误差引入的限度一般可以忽略。因此，整个称量允差可以直接作为重复性测试的可接受标准。For the sensitivity and linearity tests as described above, the analyst should use certified weights with an appropriate weight class (e.g., according to International Organization of Legal Metrology R111 or American Society for Testing and Material

58、s E617, available from and HYPERLINK / , respectively). NOTEIf a differential method is used for the linearity test, certified weights may not be required.对于上述灵敏度和线性，化验员应使用具有适当重量分类（例如，根据国际法定计算组织R111或美国材料试验协会E617，可分别从上述网址获得）且认证过的砝码。【注如果使用了不同方法进行线性测试，认证过的砝码，可能不需要认证过的砝码】Depending on the acceptance crit

59、erion, it may be sufficient to consider only the nominal weight value of the test weights. If the nominal value of the test weight is considered, analysts should ensure that the maximum permissible error does not exceed one-third of the acceptance criterion. Alternatively, if the certified value of

60、the test weight is considered, its calibration uncertainty should not exceed one-third of the acceptance criterion. If more than one weight is used to perform the test, the calibration uncertainties of the weights must be summed and the sum should not exceed one-third of the acceptance criterion. Fo