2024年4月7日发(作者：惠普电脑怎样进入bios界面)

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ELEMENTAL IMPURITIES—PROCEDURES

元素杂质

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程序

INTRODUCTION

介绍

This chapter describes two analytical procedures (Procedures 1 and 2) for the evaluation of the

levels of the elemental impurities. The chapter also describes criteria for acceptable alternative

procedures. By means of validation studies, analysts will confirm that the analytical procedures

described herein are suitable for use on specified material.

本章描述了评价元素杂质水平的两种分析方法(程序1和程序2)。本章还描述了可接受的

替代程序的标准。通过验证研究，分析人员将确认本文描述的分析方法适用于特定的物料。

Use of Alternative Procedures

使用替代程序

The chapter also describes criteria for acceptable alternative procedures. Alternative procedures

that meet the validation requirements herein may be used in accordance with General Notices,

6.30 Alternative and Harmonized Methods and Procedures. Information on the Requirements for

Alternate Procedure Validation is provided later in this chapter.

本章还描述了可接受的替代程序。可根据通则6.30替代和协调的方法和程序使用满足本

文验证要求的替代方法和程序。关于备用工艺验证要求的信息将在本章后面提供。

Speciation

形态

The determination of the oxidation state, organic complex, or combination is termed speciation.

Analytical procedures for speciation are not included in this chapter, but examples may be found

elsewhere in USP–NF and in the literature.

氧化态、有机络合物或组合的测定称为形态。本章不包括物种形成的分析方法，但可以

在USP-NF中其他地方和文献中找到例子。

PROCEDURES

程序

•Compendial Procedures 1 and 2

程序

1

和

2

System standardization and suitability evaluation using applicable reference materials should

be performed on the day of analysis.

使用标准物质进行系统标化和适用性评估应在分析当天进行。

Procedure and detection technique: Procedure 1 can be used for elemental impurities generally

amenable to detection by inductively coupled plasma–atomic (optical) emission spectroscopy

(ICP–AES or ICP–OES). Procedure 2 can be used for elemental impurities generally amenable to

detection by ICP–MS. Before initial use, the analyst should verify that the procedure is

appropriate for the instrument and sample used (procedural verification) by meeting the alternative

procedure validation requirements below.

程序和检测技术：

程序1可用于一般适用于电感耦合等离子体原子(光学)发射光谱(ICP-AES

或ICP-OES)检测的元素杂质。程序2可用于一般适用于ICP-MS检测的元素杂质。在首次

使用前，检验员应通过满足以下替代程序验证（程序确认）要求来验证程序适用于所使用的

仪器和样品。

Sample preparation: Forms of sample preparation include Neat, Direct aqueous solution, Direct

organic solution, and Indirect solution. The selection of the appropriate sample preparation

depends on the material under test and is the responsibility of the analyst. When a sample

preparation is not indicated in the monograph, an analyst may use any of the following

appropriately validated preparation procedures. In cases where spiking of a material under test is

necessary to provide an acceptable signal intensity, the blank should be spiked with the same

Target elements, and where possible, using the same spiking solution. Standard solutions may

contain multiple Target elements. [Note—All liquid samples should be weighed.]

样品制备：

样品制备形式包括净溶液、直接水溶液、直接有机溶液和间接溶液。选择合适的

样品制剂取决于被测材料，这是分析员的责任。当各论中未指明样品制备时，检验员可使用

下列任何经适当验证的制备程序。如果为了提供可接受的信号强度，有必要对被测材料进行

加钉，则空白材料应使用相同的目标元素，并在可能的情况下，使用相同的加钉溶液。标准

溶液可能包含多个目标素。【注:所有液体样品均需称重】

Neat: Used for liquids or alternative procedures that allow the examination of unsolvated samples.

净溶液：

用于液体或允许检查未溶解样品的替代程序

Direct aqueous solution: Used when the sample is soluble in an aqueous solvent.

直接水溶液：

当样品可溶于水溶剂时使用。

Direct organic solution: Used where the sample is soluble in an organic solvent.

直接有机溶液：

适用于样品可以溶解在有机溶剂的情况。

Indirect solution: Used when a material is not directly soluble in aqueous or organic solvents.

Total metal extraction is the preferred sample preparation approach to obtain an Indirect solution.

Digest the sample using the Closed vessel digestion procedure provided below or one similar to it.

The sample preparation scheme should yield sufficient sample to allow quantification of each

element at the limit specified in the corresponding monograph or chapter.

间接溶液：

当一种材料不能直接溶于水或有机溶剂时使用。全金属萃取是获得间接溶液的首

选样品制备方法。使用下面提供的封闭容器消化程序或类似的程序消化样品。样品制备方案

应提供足够的样品，以允许在相应的专论或章节规定的限度内定量每个元素。

Closed vessel digestion: This sample preparation procedure is designed for samples that must be

digested in a Concentrated acid using a closed vessel digestion apparatus. Closed vessel

digestion minimizes the loss of volatile impurities. The choice of a Concentrated acid depends on

the sample matrix. The use of any of the Concentrated acids may be appropriate, but each

introduces inherent safety risks. Therefore, appropriate safety precautions should be used at all

times. [Note—Weights and volumes provided may be adjusted to meet the requirements of the

digestion apparatus used.]

封闭的消化容器：

此样品制备程序是为必须在浓酸中使用密闭容器消化装置消化的样品设计

的。密闭容器消化将挥发性杂质的损失降至最低。浓酸的选择取决于样品基质。任何一种浓

酸的使用都可能是合适的，但每一种都会带来固有的安全风险。因此，任何时候都应该采取

适当的安全措施。【注:所提供的重量和体积可调整以满足所使用的消化设备的要求】

An example procedure that has been shown to have broad applicability is the following.

Dehydrate and predigest 0.5 g of primary sample in 5 mL of freshly prepared Concentrated acid.

Allow to sit loosely covered for 30 min in a fume hood. Add an additional 10 mL of Concentrated

acid, and digest, using a closed vessel technique, until digestion or extraction is complete. Repeat,

if necessary, by adding an additional 5 mL of Concentrated acid. [Note—Where closed vessel

digestion is necessary, follow the manufacturer’s recommended procedures to ensure safe use.]

下面是一个已被证明具有广泛适用性的示例过程。将0.5 g样品脱水并放入5ml新鲜配制

的浓酸中预消化。在通风柜中放置30分钟。再加入10毫升浓酸，用密闭容器技术消化，直

到消化或提取完成。如有必要，再加5ml浓酸。【注：如果需要密闭容器消化，请遵循制

造商推荐的程序，以确保安全使用】