ASTM E2626 - 08e1

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Designation: E2626 −08
´1
Standard Guide for
Spectrometric Analysis of Reactive and Refractory Metals
1
This standard is issued under the ﬁxed designation E2626; 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
NOTE—Editorial corrections were made throughout in October 2009.
1. Scope
1.1 This guide covers a variety of analytical techniques that
have proven to be acceptable for the analysis of the reactive
and refractory metals titanium, zirconium, niobium, hafnium,
tantalum, molybdenum, tungsten, and vanadium.
1.2 The principles and techniques in this guide can be used
by ISO 17025 compliant laboratories that need to implement
other performance-based test methods or need to document and
validate extensions of standard test methods, or non-standard
test methods.
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
standard.
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 and health practices and determine the applica-
bility of regulatory limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
2
D1193 Speciﬁcation for Reagent Water
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
E539 Test Method for Analysis of Titanium Alloys by X-Ray
Fluorescence Spectrometry
E882 Guide for Accountability and Quality Control in the
Chemical Analysis Laboratory
E1097 Guide for Determination of Various Elements by
Direct Current Plasma Atomic Emission Spectrometry
E1184 Practice for Determination of Elements by Graphite
Furnace Atomic Absorption Spectrometry
E1479 Practice for Describing and Specifying Inductively-
Coupled Plasma Atomic Emission Spectrometers
E1552 Test Method for Determining Hafnium in Zirconium
and Zirconium Alloys By Direct Current Plasma—Atomic
Emission Spectrometry
E1601 Practice for Conducting an Interlaboratory Study to
Evaluate the Performance of an Analytical Method
E1621 Guide for X-Ray Emission Spectrometric Analysis
E1770 Practice for Optimization of Electrothermal Atomic
Absorption Spectrometric Equipment
E2371 Test Method for Analysis of Titanium and Titanium
Alloys by Atomic Emission Plasma Spectrometry
E2437 Practice for Designing and Validating Performance-
Based Test Methods for the Analysis of Metals, Ores, and
Related Materials
E2438 Practice for Implementing Standard Performance
Based Test Methods for the Analysis of Metals, Ores, and
Related Materials
2.2 ISO Standards:
3
ISO 17025 General Requirements for the Competence of
Testing and Calibration Laboratories
ISO Guide 32 Calibration in Analytical Chemistry and Use
of Certiﬁed Reference Materials
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 reactive metal, n—a metal, such as titanium or
zirconium, that readily reacts with the environment. It has a
strong affinity for oxygen and nitrogen and forms very stable
compounds that passivate in thin layers. When the reactive
coating is damaged, it self heals by reaction with the atmo-
sphere.
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 E01.06 on Ti, Zr, W, Mo, Ta, Nb, Hf, Re.
Current edition approved June 15, 2008. Published July 2008. DOI: 10.1520/
E2626-08E01.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
3
Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
 

3.2.2 refractory metal, n—a metal, such as hafnium,

molybdenum, niobium, tantalum, vanadium, or tungsten, char-

acterized by very high melting points, above about 1900 °C,

that oxidizes at temperatures far below its melting point.

4. Signiﬁcance and Use

4.1 Test methods for chemical analysis of reactive and

refractory metals are primarily intended to test such materials

for compliance with compositional speciﬁcations. It is assumed

that all who use this guide will be trained analysts capable of

performing common laboratory procedures skillfully and

safely. It is expected that work will be performed in a properly

equipped laboratory under appropriate quality control practices

such as those described in Guide E882 and Practice E2437,as

well as in ISO 17025 and ISO Guide 32.

4.2 This guide is intended to aid analytical chemistry

laboratories in the analysis of reactive and refractory metals

and their alloys when no speciﬁc standard test methods are

available. The principles incorporated in this practice can also

be applied in laboratories that wish to validate and document

non-standard test methods.

4.3 The analysis of reactive and refractory materials is

typically performed by only a small number of laboratories.

Few of these laboratories have analytical instrumentation in

common for use in interlaboratory proﬁciency testing pro-

grams. This requires the use of within-laboratory developed

test methods that vary between laboratories. It is intended that

this practice will give general guidance to experienced person-

nel that will assist them in the development of a procedure that

will meet their analytical objectives.

4.4 Practice E2438 provides guidance for the development

and documentation of an In-House Standard Operating Proce-

dure (SOP).

5. Hazards

5.1 The dissolution of these metals usually requires the use

of hydroﬂuoric acid. Read and follow label precautions and

mandatory safety data sheet (MSDS) information, and refer to

Practices E50.

5.2 Fine turnings, chips, or powder require more water to

moderate the reaction rate. If the metal is solid chunks rather

than ﬁnely divided, the dissolution will be much slower and

require less water. It will also require additional acid to

complete the dissolution. See Speciﬁcation D1193 for reagent

water speciﬁcations.

5.3 Fine turnings or powder of hafnium, titanium, and

zirconium are pyrophoric. Observe the proper precautions.

6. Test Methods

6.1 Atomic Absorption Spectrometry (AAS)—This technique

is applicable to elements that can be dissolved and placed in the

vapor state (ﬂame or ﬂameless) as ground state atoms. Radia-

tion from a hollow cathode light source emits the spectrum of

the element to be analyzed, which is then passed through vapor

containing the element to be analyzed, and into a monochro-

mator set for radiation characteristic of the element. The degree

of absorption is measured, and is proportional to the amount of

the particular element present. Analysis is made by comparison

to reference materials. Lists of elements that can be

determined, sensitivities, wavelengths, and operating param-

eters are provided by the instrument manufacturers. Due to the

requirements of the materials speciﬁcations, the AAS detection

limits for many elements will not be low enough for the use of

this technique. AAS has been utilized for the analysis of iron,

chromium, nickel, and tin in zirconium alloys and for the

determination of iron and zirconium in hafnium. Practices

E1184 and E1770 provide further details.

6.2 Atomic Emission Spectrometry (AES)—This technique

has historically been the main means of analysis for these

metals. Analysis by the techniques described in this section is

based upon the fact that each vaporized element, when suitably

excited by an arc, spark, plasma, or other means, is made to

emit its characteristic spectrum. The radiation thus emitted

passes into a spectrometer where it is resolved into its

component wavelengths and recorded by various means as a

deﬁnite pattern. The position of the spectral information

indicates QUALITATIVELY which elements are present. The

intensity determines QUANTITATIVELY the amount of each

element in the sample when compared to intensities obtained

by using calibration materials. Calibration materials can be

reference materials or industry acceptable analyzed specimens.

6.2.1 Arc/Spark Spectrometry (AS-AES)—Instruments uti-

lizing photographic ﬁlm or plates were the mainstay for many

years until parts and supplies became very difficult, if not

impossible, to obtain. Electronic read-out arc/spark instruments

are still used by a number of laboratories. The primary problem

with arc/spark is the unavailability of solid reference materials

for calibration. Metallurgical history and surface grain size

effects can become an issue. However, if proper calibration

materials were available, the majority of the necessary ele-

ments in a typical material speciﬁcation could be analyzed.

6.2.2 Direct Current Plasma Atomic Emission Spectrometry

(DCP-AES)—Since DCP-AES analysis, like atomic

absorption, Inductively Coupled Plasma Atomic Emission

Spectrometry (ICP-AES) (see 6.2.3), and Inductively Coupled

Plasma-Mass Spectrometry (ICP-MS) (see 6.2.4), relies on

sample dissolution, the major difficulties with reference mate-

rials for calibration with can be overcome by the techniques

discussed in 9.4. One of the main positive attributes of this

technique is the high resolution available due to the Echelle

grating. The highly complex spectra of reactive and refractory

metals require an instrument with good spectral resolving

power in order to ﬁnd interference-free wavelengths. The

DCP-AES has a rugged sample introduction system that lends

itself well to the analysis of materials that have been dissolved

in acids such as hydroﬂuoric, nitric, and hydrochloric acids. In

most cases, due to the nature of the source design, the

DCP-AES does not achieve the detection limits or the precision

of an Inductively Coupled Plasma (ICP) source. In some cases,

however, its signiﬁcantly superior resolving power may allow

it to out-perform an ICP that utilizes a conventional ruled

grating. The corrosion resistant nature of the sample introduc-

tion system and jet materials on DCP-AES has allowed it to be

very capable for the analysis of silicon in a hydroﬂuoric acid

E2626 − 08

´1

solution. DCP-AES is unable to achieve the necessary detec-
tion limits for elements such as boron and cadmium in a
zirconium sample at the levels required by most speciﬁcations.
Test Method E1552 gives details for the analysis of hafnium in
zirconium and zirconium alloys using the DCP-AES technique
and Test Method E2371 describes the analysis of titanium and
titanium alloys. Guide E1097 discusses the technique in more
general terms.
6.2.3 Inductively Coupled Plasma Atomic Emission Spec-
trometry (ICP-AES)—Practice E1479 describes the compo-
nents of an ICP-AES that are basic to its operation and to the
quality of its performance. ICP-AES and ICP-MS represent the
instruments most commonly used for the analysis of reactive
and refractory metals. These solution-based techniques
complement each other to provide a reliable means of analysis
of reactive and refractory metals. Care must always be taken to
avoid serious spectral interferences due to the line-rich nature
of reactive and refractory metals. The advent of solid-state
detectors has provided much ﬂexibility in the selection of
wavelengths. Section 8.3 gives guidance in wavelength selec-
tion. Test Method E2371 gives details for the analysis of
titanium and titanium alloys, while Practice E1479 discusses
the techniques in more general terms.
6.2.4 Inductively Coupled Plasma-Mass Spectrometry (ICP-
MS)—This technique is distinguished from ICP-AES by the
detection system used to analyze the species excited by a
plasma. A mass spectrometer is utilized in this case. Much of
the information in Practice E1479 is applicable to ICP-MS.
This technique is capable of analyzing the majority of the metal
elements necessary to satisfy the material speciﬁcations for
reactive and refractory metals. The high sensitivity of ICP-MS
may require signiﬁcant dilution of the sample solution in order
to analyze elements at concentrations above 0.1 %, by mass.
6.3 Glow Discharge Spectrometry—The issue mentioned
above in securing solid reference materials is a concern that
must be addressed with this technique. Glow Discharge instru-
mentation is normally divided into two types of instrumenta-
tion.
6.3.1 Glow Discharge-Mass Spectrometry (GD-MS)—In
this technique, the surface of a solid sample is sputtered with
argon gas. Ionized species are then subjected to high-resolution
mass spectrometric analysis. This results in the high sensitivity
analysis of all elements in the periodic table, except hydrogen
at the trace level. GD-MS has been used for the multi-element
survey analysis for these metals included in the scope of this
guide. Care must be taken in the interpretation of the results,
however, due to the non-homogeneity of the sample surface.
Reactive and refractory metals typically exhibit a relatively
large grain size compared to the small area sampled by the
conventional “pin” sample used by the GD-MS. It is also
possible to sample a ﬂat surface, which may help alleviate the
grain size problem. One should keep in mind that only a few
hundred micrograms of material are sampled, which under-
scores the importance of homogeneity. Due to the high cost and
complexity of the instrumentation, GD-MS is found in very
few captive laboratories. Commercial analysis is available
through a limited number of laboratories.
6.3.2 Glow Discharge Atomic Emission Spectrometry (GD-
AES)—The glow discharge excitation source is a device that
produces luminous plasma. Solid samples are sputtered using
the low-pressure argon plasma. The argon ions etch atoms and
small atomic clusters from the sample surface making them
available for dissociation and excitation in the plasma. Metal-
lurgical history is reduced because sampling and excitation
take place in separate locations. Calibration requires the use of
reference materials and where available it is possible to
determine the alloying and minor constituents simultaneously.
6.4 X-ray Emission Spectrometry (XRF)—See Guide E1621
for details of the instrumentation. Again, the requirement for a
set of homogeneous, solid reference materials limits the use of
this technique. The low detection limit requirements for many
of the required elements in these materials will not be achieved
by this technique. The analysis of iron, chromium, nickel, and
tin in zirconium alloys and zirconium in hafnium have been
demonstrated to work well by X-ray. Test Method E539 and
Guide E1621 give valuable guidance.
7. Calibration
7.1 Set up the instrument for calibration as recommended by
the manufacturer. The publications listed in Section 2, as well
as in texts, the analytical literature, and other standards
organizations, will also provide valuable guidance.
8. Interferences
8.1 Guide E1097, Practice E1184, Practice E1479, Guide
E1621, and Practice E1770 describe some of the interferences
encountered during analysis. The user is responsible for
ensuring the absence of, or compensating for interferences that
may bias test results obtained using their standard operating
procedures.
8.2 The physical interferences resulting from variations in
sample and calibration solution aerosol transport rates may be
compensated for by the use of an internal standard in some
techniques.
8.3 Table 1 lists wavelengths that have been used to analyze
the listed elements in the given metals and are suggested for the
user of atomic emission spectrometers. Due to the resolution of
individual instruments, conﬁrmation of these suggestions will
be required. Depending on the speciﬁc spectrometer, other
wavelengths will be found to be applicable.
9. Reference Materials
9.1 Standard Reference Material (SRM) Zircaloy-4, SRM
360b, is available from National Institute of Standards and
Technology
4
and other commercial suppliers. Three zirconium
materials known as Zr 20, Zr 30, and Zr 40 are available from
several commercial suppliers. Due to non-homogeneity, they
are recommended for X-ray ﬂuorescence use only. BCR-098 is
a Zircaloy-4 alloy that is certiﬁed for chromium, hafnium, iron,
and tin.
4
Available from National Institute of Standards and Technology (NIST), 100
Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http://www.nist.gov.
E2626 − 08
´1
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摘要：

ASTM E2626 - 08e1 是一项关于不锈钢及其他特殊合金在高温或腐蚀性环境下抗敏化性能评估的标准指南，主要适用于奥氏体不锈钢、铁素体不锈钢及双相不锈钢等材料。该标准旨在通过弯曲试验法快速判断材料在焊接或热处理过程中是否发生敏化，从而评估其在极端环境下的耐晶间腐蚀能力。对于从事材料工程、压力容器制造或石油化工行业的专业人员而言，遵循 ASTM E2626 可帮助优化材料选择与工艺控制，降低因敏化导致的腐蚀失效风险。指南中详细规定了试验样品的制备、试剂配制及结果评判方法，确保不同实验室之间

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