1.1 本指南介绍了用有机分析物或成分“加标”水性样品的一般技术。它适用于水性介质中的各种有机材料。尽管没有描述所有类型化合物所需的具体细节和处理程序，但提供这种通用方法是为了指导分析员准确制备加标样品，以便进行后续分析或比较。还提供了指导，以帮助分析员计算回收率和解释结果。分析员有责任确定此处引用的方法和材料是否与感兴趣的分析物兼容。 1.2 本指南中的程序侧重于“基质尖峰”的准备、分析、结果和解释。这些程序适用于通过加标制备校准标准品、校准检查标准品、实验室控制标准品、参考材料和其他质量控制材料是偶然的。 样品（基质）用感兴趣的分析物强化（加标），用于各种分析和质量控制目的。虽然讨论了多个样品测试部分的加标，但未涵盖标准添加的方法。 1.3 本指南旨在与提供分析物或感兴趣成分程序的单独分析测试方法结合使用。该测试方法用于确定分析物或成分的背景水平，并在加标后再次确定其现在的升高水平。每种测试方法通常不仅为样品提供程序，还为校准标准品或分析控制溶液或两者提供程序。这些程序包括准备、处理、储存、保存和分析技术。这些程序适用于加标解决方案，并根据具体情况使用分析师的判断进行扩展，本指南中不重复这些程序。 另请参阅实践 E200 用于准备和存储信息。 1.4 这些程序仅适用于以刺突加任何背景材料的浓度可溶于水的分析物，或可溶于本身是水溶性的溶剂的分析物。在后一种情况下使用的系统必须产生分析物和样品的均匀溶液。如果无法获得样品中感兴趣的分析物的水溶液或均匀悬浮液，则无法获得有意义的回收数据。 1.5 基质加标可以在现场或实验室进行，具体取决于要测试分析过程的哪一部分。现场加标测试整个过程的回收率，包括样品的保存和运输。实验室加标仅测试实验室过程。加标样品提取物、浓缩物或稀释液将仅测试加标后过程的这一部分。 1.6 以国际单位制表示的数值应视为标准。本标准不包括其他计量单位。 1.7 本标准并不旨在解决与其使用相关的所有安全问题（如有）。本标准的使用者有责任在使用前制定适当的安全、健康和环境实践，并确定监管限制的适用性。 1.8 本国际标准是根据世界贸易组织技术性贸易壁垒委员会发布的《关于制定国际标准、指南和建议的原则的决定》中确立的国际公认的标准化原则制定的。 ====意义和用途====== 5.1 样品的基质加标通常用于确定特定分析条件下的偏差，或通过确定在这些条件下从样品基质中回收添加的加标的程度来确定测试方法对特定样品基质的适用性。 分析物或感兴趣的组分与样品基质的反应或相互作用可能对回收产生显著的积极或消极影响，并可能使所选择的分析或监测过程对该样品基质无效。 5.2 作为常规质量保证计划的一部分，样品的基质加标也可用于监测实验室、单个仪器或分析员的性能。随着时间的推移，来自相同或相似基质的尖峰回收率的变化可能表明分析和分析结果的质量存在变化。 5.3 根据要测试的分析过程的哪一部分，可以在现场或实验室进行样品加标。现场加标测试整个过程的回收率，包括样品的保存和运输，可以被视为基质中分析物稳定性的衡量标准。 实验室加标仅测试实验室过程。样品提取物、浓缩物或稀释液的加标将仅反映加标后过程的那一部分。 5.4 当非人工人员在现场进行扣球时，应遵守特殊预防措施。建议由经验丰富的分析员在实验室中进行所有加标准备工作，以便现场操作仅包括向样品基质中添加准备好的加标溶液。有必要对现场人员进行培训并验证其加标技术，以确保准确且可重复地添加加标。可使用重复现场尖峰的一致且可接受的回收率来记录采样和尖峰技术的再现性。当使用对环境不稳定的化合物作为刺突剂时，应通过适当的方式保护刺突剂溶液直到使用时，如冷却、防止阳光和氧气照射或化学保存。 注1: 任何现场加标样品，如果实验室已知，应在最终结果报告中标记为现场加标。此外，只要可能，应避免现场添加挥发性化合物。 5.5 通常默认从样品中回收分析物组分的程度与从加标样品中回收相同分析物的尖峰的程度大致相同。这种假设可能不正确的一个原因是，刺突可能不会像天然存在的分析物结合在样品中那样结合在样品（例如，与悬浮物质）中。因此，可以不同于分析物的背景水平从样品中回收尖峰。由于这个原因，以及偏差校正会增加可变性的事实，使用峰值回收率校正分析数据不是一个好的做法。但是，峰值恢复信息应与相关样本分析结果一起报告。 5.6 本指南也适用于通过标准添加方法进行定量的尖峰的制备和使用，以及替代品和内标的添加。

1.1 This guide covers the general technique of “spiking” aqueous samples with organic analytes or components. It is intended to be applicable to a broad range of organic materials in aqueous media. Although the specific details and handling procedures required for all types of compounds are not described, this general approach is given to serve as a guideline to the analyst in accurately preparing spiked samples for subsequent analysis or comparison. Guidance is also provided to aid the analyst in calculating recoveries and interpreting results. It is the responsibility of the analyst to determine whether the methods and materials cited here are compatible with the analytes of interest. 1.2 The procedures in this guide are focused on “matrix spike” preparation, analysis, results, and interpretation. The applicability of these procedures to the preparation of calibration standards, calibration check standards, laboratory control standards, reference materials, and other quality control materials by spiking is incidental. A sample (the matrix) is fortified (spiked) with the analyte of interest for a variety of analytical and quality control purposes. While the spiking of multiple sample test portions is discussed, the method of standard additions is not covered. 1.3 This guide is intended for use in conjunction with the individual analytical test method that provides procedures for analysis of the analyte or component of interest. The test method is used to determine an analyte or component's background level and, again after spiking, its now elevated level. Each test method typically provides procedures not only for samples, but also for calibration standards or analytical control solutions, or both. These procedures include preparation, handling, storage, preservation, and analysis techniques. These procedures are applicable by extension, using the analyst's judgement on a case-by-case basis, to spiking solutions, and are not reiterated in this guide. See also Practice E200 for preparation and storage information. 1.4 These procedures apply only to analytes that are soluble in water at the concentration of the spike plus any background material, or to analytes soluble in a solvent that is itself water-soluble. The system used in the later case must result in a homogeneous solution of analyte and sample. Meaningful recovery data cannot be obtained if an aqueous solution or homogeneous suspension of the analyte of interest in the sample cannot be attained. 1.5 Matrix spiking may be performed in the field or in the laboratory, depending on which part of the analytical process is to be tested. Field spiking tests the recovery of the overall process, including preservation and shipping of the sample. Laboratory spiking tests the laboratory process only. Spiking of sample extracts, concentrates, or dilutions will test only that portion of the process subsequent to the addition of the spike. 1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. 1.8 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee. ====== Significance And Use ====== 5.1 Matrix spiking of samples is commonly used to determine the bias under specific analytical conditions, or the applicability of a test method to a particular sample matrix, by determining the extent to which the added spike is recovered from the sample matrix under these conditions. Reactions or interactions of the analyte or component of interest with the sample matrix may cause a significant positive or negative effect on recovery and may render the chosen analytical, or monitoring, process ineffectual for that sample matrix. 5.2 Matrix spiking of samples can also be used to monitor the performance of a laboratory, individual instrument, or analyst as part of a regular quality assurance program. Changes in spike recoveries from the same or similar matrices over time may indicate variations in the quality of analyses and analytical results. 5.3 Spiking of samples may be performed in the field or in the laboratory, depending on what part of the analytical process is to be tested. Field spiking tests the recovery of the overall process, including preservation and shipping of the sample and may be considered a measure of the stability of the analytes in the matrix. Laboratory spiking tests the laboratory process only. Spiking of sample extracts, concentrates, or dilutions will be reflective of only that portion of the process subsequent to the addition of the spike. 5.4 Special precautions shall be observed when nonlaboratory personnel perform spiking in the field. It is recommended that all spike preparation work be performed in a laboratory by experienced analysts so that the field operation consists solely of adding a prepared spiking solution to the sample matrix. Training of field personnel and validation of their spiking techniques are necessary to ensure that spikes are added accurately and reproducibly. Consistent and acceptable recoveries from duplicate field spikes can be used to document the reproducibility of sampling and the spiking technique. When environmentally labile compounds are used as spikes, the spiking solution shall be protected up to the time of use by appropriate means such as chilling, protection from sunlight and oxygen, or chemical preservation. Note 1: Any field spiked sample, if known to the laboratory, should be labeled as a field spike in the final results report. Also, whenever possible, field spiking of volatile compounds should be avoided. 5.5 It is often tacitly assumed that the analyte component is recovered from the sample to approximately the same extent that a spike of the same analyte is recovered from a spiked sample. One reason that this assumption may be incorrect is that the spike may not be bound up in the sample (for example, with suspended matter) in the same way that the naturally occurring analyte is bound in the sample. The spike may therefore be recovered from the sample differently than the background level of the analyte. For this reason, as well as the fact that bias corrections can add variability, it is not good practice to correct analytical data using spike recoveries. Spike recovery information should, however, be reported along with the related sample analysis results. 5.6 This guide is also applicable to the preparation and use of spikes for quantification by the method of standard additions and to the addition of surrogates and internal standards.