ASTM E1097 - 25 通过直流等离子体原子发射光谱法测定各种元素的标准指南

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Designation: E1097 −25
Standard Guide for
Determination of Various Elements by Direct Current
Plasma Atomic Emission Spectrometry
1
This standard is issued under the ﬁxed designation E1097; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This guide covers procedures for using a Direct Current
Plasma Atomic Emission Spectrometer (DCP-AES) to deter-
mine the concentration of elements in solution. Recommenda-
tions are provided for preparing and calibrating the instrument,
assessing instrument performance, diagnosing, and correcting
for interferences, measuring test solutions, and calculating
results. A method to correct for instrument drift is included.
1.2 This guide does not specify all the operating conditions
for a DCP-AES because of the differences between models of
these instruments. Users should follow instructions provided
by the manufacturer of the particular instrument.
1.3 This guide does not attempt to specify in detail all of the
hardware components and computer software of the instru-
ment. It is assumed that the instrument, whether commercially
available, modiﬁed, or custom built, will be capable of per-
forming the analyses for which it is intended, and that the user
has veriﬁed this before performing the analysis.
1.4 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 appro-
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
Speciﬁc precautionary statements are given in Section 7.
1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
2
E29 Practice for Using Signiﬁcant Digits in Test Data to
Determine Conformance with Speciﬁcations
E50 Practices for Apparatus, Reagents, and Safety Consid-
erations for Chemical Analysis of Metals, Ores, and
Related Materials
E135 Terminology Relating to Analytical Chemistry for
Metals, Ores, and Related Materials
E882 Guide for Accountability and Quality Control in the
Chemical Analysis Laboratory
E1601 Practice for Conducting an Interlaboratory Study to
Evaluate the Performance of an Analytical Method
3. Terminology
3.1 Deﬁnitions: For deﬁnitions of terms used in this guide,
refer to Terminology E135.
3.2 Deﬁnitions of Terms Speciﬁc to This Standard:
3.2.1 background equivalent concentration (BEC), n—in
DCP-AES, the analyte concentration whose signal is equivalent
to the signal generated by the plasma and matrix at the analyte
line when the actual analyte concentration is zero.
3.2.2 detection limit (DL), n—in addition to the DL deﬁned
in Terminology E135, the following detection limits are
described and used in this guide:
3.2.2.1 instrumental detection limit (IDL), n—in DCP-AES,
the analyte concentration corresponding to three times the
standard deviation of the background noise beneath the analyte
line on a set of nine consecutive 10-s measurements of the
background intensity of the blank.
3.2.2.2 method detection limit (MDL), n— in DCP-AES, the
detection limit measured on the matrix blank.
1
This guide is under the jurisdiction of ASTM Committee E01 on Analytical
Chemistry for Metals, Ores, and Related Materials and is the direct responsibility of
Subcommittee E01.20 on Fundamental Practices.
Current edition approved April 1, 2025. Published April 2025. Originally
approved in 1986. Last previous edition approved in 2017 as E1097 – 12 (2017).
DOI: 10.1520/E1097-25.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at www.astm.org/contact. For Annual Book of
ASTM Standards volume information, refer to the standard’s Document Summary
page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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.
1

3.2.3 equivalent analyte concentration, n—the apparent

concentration of an interfering element on an analyte.

3.2.4 linear dynamic range, n—the concentration range

from the limit of quantiﬁcation to the highest concentration that

remains within 610 % of linearity based on lower concentra-

tions.

3.2.5 limit of quantiﬁcation (LOQ), n—the lowest concen-

tration at which the instrument can measure reliably with a

deﬁned error and conﬁdence level.

3.2.6 sensitivity, n—the slope of the calibration curve, which

is the ratio of the change in emission intensity to the change in

concentration.

4. Summary of Guide

4.1 DCP-AES’s, either simultaneous or sequential, measure

the concentration of elements in solution. Solutions are nebu-

lized and the aerosol is transported to the direct current plasma

jet where excitation occurs and characteristic emission spectra

are produced. The spectra are dispersed by an echelle grating

and cross-dispersed by a prism or grating. The spectra then

impinge on photomultiplier tubes, whose outputs are inter-

preted by a computer as emission intensities. Background

correction can be used to compensate for some interferences.

The computer generates calibration curves and calculates

analyte concentration.

5. Signiﬁcance and Use

5.1 Analyses using DCP-AES require proper preparation of

test solutions, accurate calibration, and control of analytical

procedures. E01 test methods that refer to this guide shall

provide speciﬁcs on test solutions, calibration, and procedures.

5.2 DCP-AES analysis is primarily concerned with testing

materials for compliance with speciﬁcations, but may range

from qualitative estimations to umpire analysis. These may

involve measuring major and minor constituents or trace

impurities, or both. This guide suggests some approaches to

these different analytical needs.

5.3 This guide assists users in developing new methods.

5.4 It is assumed that the users of this guide will be trained

analysts capable of performing common laboratory procedures

skillfully and safely. It is expected that the work will be

performed in a properly equipped laboratory.

5.5 This guide does not purport to deﬁne all of the quality

assurance parameters necessary for DCP-AES analysis. Users

should ensure that proper quality assurance procedures are

followed, especially those deﬁned by the test method. Refer to

Guide E882.

6. Preparation of Solutions

6.1 Solutions are prepared for different purposes. Not all

may be necessary for every test. Prepare only those directed by

the method or required to meet speciﬁc experimental objec-

tives.

6.2 Rinse Solution—Prepare a rinse solution to contain the

acids or bases present in the test solution at the same

concentration. Prepare a quantity sufficient to clean the end of

the sample uptake tubing and to ﬂush the sample introduction

system between each determination of calibration solutions and

test solutions. Occasionally, an analyte requires a conditioning

time in the aspiration/nebulization system of the instrument.

For this, use the test solution as a rinse and allow a sufficient

residence time before taking a reading.

6.3 Reagent Blank Solution—This solution consists of all

reagents and other additions at the same concentration used in

preparing the test solution. Carry this solution through the

entire sample preparation procedure.

6.4 Matrix Blank Solution—Prepare this solution to be as

close in composition to the test solution as possible (including

dissolution reagents and matrix elements), but omitting the

elements to be determined. The matrix elements should be of

high purity.

6.5 Control—Select a reference material or other material of

known composition and prepare it as directed in the test

method. Analyze the control regularly as a blind sample and

use the results for quality control as directed in Guide E882.

6.6 Calibration Solutions—The number and type of these

solutions will depend on the method, and on the type of

DCP-AES instrument and its computer. Generally, prepare two

instrument calibration solutions, one high concentration, and

one low concentration or a blank, that bracket the expected

concentration range of the sample test solutions. More may be

prepared if the computer can utilize them, especially if the

analyte composition of the test solutions is expected to cover a

wide range or if the calibration curve is non-linear. Prepare the

calibration solutions by adding aliquots from stock solutions to

solutions that are similar to the matrix of the test sample.

6.6.1 Match the matrix of the calibration solutions as

closely as possible to that of the test solution in acidity, total

solids, reagents, and matrix elements, especially if easily

ionized elements are present. Some matrix elements may be

eliminated if it can be shown by spike addition or standard

additions that the effect on the test solution analytes is

insigniﬁcant. Use stock solutions or pure elements prepared by

a method similar to that used to prepare the test solutions. If the

composition of the test solution is unknown to the extent that

matrix-matched solutions cannot be prepared, or if a suffi-

ciently pure matrix material is not available, refer to the

method of standard additions described in 6.7 and 10.6.

6.6.1.1 If the instrument is designed to use a blank as the

low concentration calibration solution, prepare it the same way

as the high concentration calibration solution, omitting the

elements to be determined. Where matrix-matched calibration

solutions are employed, this will be the matrix blank solution.

6.6.2 Optimum Calibration Solution Concentration

Range—For calibration in the linear range, the highest concen-

tration should be no more than 85 % of the upper limit of the

calibration curve linearity. For an instrument that accepts a low

concentration calibration solution, its concentration should be

at least four times the MDL and above the LOQ.

6.7 Standard Additions Solutions—Prepare as directed in

either 6.7.1 or 6.7.2 as follows:

6.7.1 Prepare four separate test solutions of the sample. To

all but one, add known amounts of the analyte equal to (0.5,

E1097 − 25

1.0, and 1.5) times or (1.0, 2.0, and 3.0) times the expected
concentration of the analyte(s) in the test solution. The original
analyte concentration should be at or above its LOQ. The ﬁnal
analyte concentration in the highest spike should not be greater
than the linear range of the emission line used. Dilute all
solutions to the mark and mix. Prepare an equal volume of the
reagent blank solution when using 10.6.2.
6.7.2 Transfer four equal volumes of a test solution to four
volumetric ﬂasks of the same size. To all but one, add known
amounts of the analyte equal to (0.5, 1.0, and 1.5) times, or
(1.0, 2.0, and 3.0) times the expected concentration of the
analyte(s) in the test solution. The ﬁnal analyte concentration
in the test solution should be at or above the LOQ. The ﬁnal
analyte concentration in the highest spike should not exceed
the linear dynamic range of the emission line used. Dilute all
solutions to the mark and mix. Prepare an equal volume of the
reagent blank solution if using 10.6.2. Multiply the ﬁnal value
by a factor to compensate for dilution.
6.8 Calibration Veriﬁcation Solution—To verify the
calibration, prepare one or more solutions whose concentra-
tions are between the highest concentration calibration solution
and the LOQ.
6.9 Spike Recovery Sample—Prepare a test solution as
directed in the method. Add a spike of the analyte(s) equal to
at least 5 times each analyte’s LOQ.
6.10 LOQ Solution—Prepare a solution containing amounts
of analyte three times to six times the method detection limit or
10 % to 20 % of the BEC and matched as closely to the matrix
as possible.
7. Hazards
7.1 Protect eyes from the intense ultraviolet radiation of the
plasma.
7.2 Follow the manufacturer’s recommended operating
practices for initiating the plasma and operating the instrument.
7.3 Ensure that HF-resistant materials are used when ana-
lyzing solutions containing HF. Avoid strongly caustic solu-
tions that may cause the ceramic sleeves of the electrodes to
fuse.
7.4 For other safety precautions, refer to Practice E50.
8. Characterization of Analytical Wavelengths
8.1 Overview:
8.1.1 When researching a new method, use the recommen-
dations in this section to select a wavelength and evaluate the
possible interferences. Measure the approximate linear range,
BEC, sensitivity and LOQ experimentally, and ascertain that
they are adequate for the analysis. Once these have been
established for a speciﬁc instrument, periodic conﬁrmation is
recommended and especially whenever a change is made in the
hardware (for example, transport or detection devices) or
optics. Conﬁrm by analysis of controls, including LOQ mea-
surements when required, that the daily performance of the
instrument meets the criteria of the method.
8.1.2 When adapting a documented test method for the ﬁrst
time, conﬁrm that freedom from interferences, linearity, DL,
LOQ and sensitivity meet the criteria of the method.
8.1.3 For lists of wavelengths and information on their
characteristics, refer to Harrison (1)
3
, Meggers (2), Phelps (3),
Reader (4), or Winge (5).
8.1.3.1 In the laddered array of spectra from the DCP’s
echelle grating, some wavelengths appear in two adjacent
orders. These wavelengths usually have similar intensities.
Occasionally, one may prove more useful for a speciﬁc
application.
8.2 Interferences—Several types of interferences may affect
measurements. This is especially true for test solutions con-
taining high concentrations of solids or acids or containing
elements having intense emission, a large number of atomic
emission lines, or high concentrations of easily ionized ele-
ments. The presence of interferences should be considered
when selecting calibration solutions and the method of analy-
sis. See 8.2.3 for suggestions on how to compensate for
interferences.
8.2.1 Types of Interference:
8.2.1.1 Chemical Interferences—Effects from excitation,
molecular compound formation, and solvent vaporization.
8.2.1.2 Physical Interferences—Factors that change the rate
of sample delivery such as viscosity, surface tension, and
reaction with parts of the sample delivery system.
8.2.1.3 Spectral Interferences—Spectral line or molecular
band overlap from the matrix or solvents, background resulting
from continuum radiation, or stray light.
8.2.2 Diagnosis of Interferences—Use the following proce-
dures for each new sample matrix:
8.2.2.1 Comparison with Alternative Method(s) of
Analysis—Use established methods to compare analytical re-
sults where possible.
8.2.2.2 Wavelength Scanning—If possible, scan the wave-
length region near the analyte emission to detect spectral
interferences and high background in calibration solutions, test
solutions, and solutions containing suspected interfering ele-
ments.
8.2.2.3 Spike Recovery—Add a known quantity or spike of
the analyte equal to at least ﬁve times the LOQ. It should be
recovered to within 62σof 100 %, where σis the standard
deviation of at least three replicate measurements. If not, a
matrix effect or other interference may be present.
8.2.2.4 Serial Dilution—If the analyte concentration is suf-
ﬁciently high, analysis of a ten-fold dilution should agree with
the expected concentration to within 5 %. If not, a chemical or
physical interference may be present.
8.2.2.5 Equivalent Analyte Concentration—To obtain a
quantitative measurement of the amount of interference from
individual elements, measure the equivalent analyte concentra-
tion by testing 1 g ⁄L solutions of these elements without using
background correction.
8.2.3 Correction for Interference Effects—If interference
effects are indicated, use one or more of the following
techniques:
3
The boldface numbers in parentheses refer to a list of references at the end of
this standard.
E1097 − 25
3

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标签： #离子体 #发射光谱法 #测定

摘要：

本指南详细介绍了ASTM E1097-25标准，即通过直流等离子体原子发射光谱法（DCP-AES）测定各类样品中多种元素的分析方法与操作规范。该标准适用于金属、合金、矿石及其他无机材料中主要、次要及痕量元素的定量分析，涵盖样品准备、仪器校准、光谱干扰校正及质量控制等关键步骤。遵循此指南可以确保实验室在材料检测、环境监测及工业品控中获得的元素分析结果具有高准确度与可重复性，是相关领域技术人员进行规范化测试的重要参考依据。

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ASTM E1097 - 25 通过直流等离子体原子发射光谱法测定各种元素的标准指南

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