ASTM E439-23

Standard Test Methods for Chemical Analysis of Beryllium

SIGNIFICANCE AND USE
4.1 These test methods for the chemical analysis of beryllium metal are primarily intended as referee methods to test such materials for compliance with compositional specifications. It is assumed that all who use these test methods 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.
SCOPE
1.1 These test methods cover the chemical analysis of beryllium having chemical compositions within the following limits:    
Element  
Range, %  
Aluminum  
0.05 to 0.30  
Beryllium  
97.5 to 100    
Beryllium Oxide  
0.3 to 3    
Carbon  
0.05 to 0.30  
Copper  
0.005 to 0.10  
Chromium  
0.005 to 0.10  
Iron  
0.05 to 0.30  
Magnesium  
0.02 to 0.15  
Nickel  
0.005 to 0.10  
Silicon  
0.02 to 0.15  
1.2 The test methods in this standard are contained in the sections as follows.    
Sections  
Chromium by the Diphenylcarbazide Spectrophotometric Test Method
[0.004 % to 0.04 %]  
10 – 19  
Iron by the 1,10-Phenanthroline Spectrophotometric Test Method
[0.05 % to 0.25 %]  
20 – 29  
Manganese by the Periodate Spectrophotometric Test Method
[0.008 % to 0.04 %]  
30 – 39  
Nickel by the Dimethylglyoxime Spectrophotometric Test Method
[0.001 % to 0.04 %]  
40 – 49  
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 appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

General Information

• Status: Published
• Publication Date: 30-Jun-2023
• ICS: 77.040.30 - Chemical analysis of metals
• ICS: 77.120.99 - Other non-ferrous metals and their alloys
• Technical Committee: E01 - Analytical Chemistry for Metals, Ores, and Related Materials
• Drafting Committee: E01.05 - Cu, Pb, Zn, Cd, Sn, Be, Precious Metals, their Alloys, and Related Metals

Relations

• Refers: ASTM E135-20 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 01-Jan-2020
• Refers: ASTM E1601-19 - Standard Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method
• Effective Date: 01-Nov-2019
• Refers: ASTM E135-19 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-May-2019
• Refers: ASTM E88-11(2017) - Standard Practice for Sampling Nonferrous Metals and Alloys in Cast Form for Determination of Chemical Composition
• Effective Date: 01-Sep-2017
• Refers: ASTM E50-17 - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
• Effective Date: 01-Sep-2017
• Refers: ASTM E50-11(2016) - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
• Effective Date: 01-Aug-2016
• Refers: ASTM E135-16 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-May-2016
• Refers: ASTM E135-15a - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 01-Jul-2015
• Refers: ASTM E135-15 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-May-2015
• Refers: ASTM E135-14b - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-Aug-2014
• Refers: ASTM E135-14a - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 01-Apr-2014
• Refers: ASTM E135-14 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-Feb-2014
• Refers: ASTM E135-13a - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 01-Dec-2013
• Refers: ASTM E1601-12 - Standard Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method
• Effective Date: 15-Dec-2012
• Refers: ASTM E50-11 - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
• Effective Date: 15-Oct-2011

Overview

ASTM E439-23: Standard Test Methods for Chemical Analysis of Beryllium provides a set of referee test methods specifically designed for the accurate chemical analysis of beryllium metal. These methods are essential for testing beryllium and its alloys to ensure compliance with strict compositional specifications in industrial quality assurance and laboratory settings. Developed by ASTM Committee E01, the standard supports both routine and high-precision chemical analysis, promoting safety, reliability, and consistency in measuring key elements present in beryllium.

Test methods outlined in ASTM E439-23 address chemical compositions for major and trace elements within the following limits:

• Beryllium: 97.5%-100%
• Beryllium oxide, aluminum, carbon, copper, chromium, iron, magnesium, nickel, silicon: trace to minor percentages

Key Topics

ASTM E439-23 details spectrophotometric methods for analyzing specific elements in beryllium, including:

• Chromium (0.004% to 0.04%)
  Determined by the Diphenylcarbazide Spectrophotometric Test Method.

• Iron (0.05% to 0.25%)
  Measured using the 1,10-Phenanthroline Spectrophotometric Test Method.

• Manganese (0.008% to 0.04%)
  Analyzed by the Periodate Spectrophotometric Test Method.

• Nickel (0.001% to 0.04%)
  Quantified using the Dimethylglyoxime Spectrophotometric Test Method.

Other elements (Al, BeO, C, Cu, Mg, Si) are considered within the scope of the standard’s application, with maximum allowable mass fractions specified to avoid interference with analytic results. All values are reported in SI units as standard.

Safety Considerations:
ASTM E439-23 requires all laboratory work to be conducted by trained analysts in properly equipped laboratories, emphasizing the importance of following appropriate safety, health, and environmental practices. Handling beryllium compounds requires particular care due to toxicity and the potential for serious lung disorders stemming from inhalation exposure.

Applications

The methods provided in ASTM E439-23 are widely applicable in:

• Material Specification Compliance:
  Used by manufacturers and quality control laboratories to verify that beryllium and its alloys meet stringent compositional requirements.

• Industrial and Research Laboratories:
  Essential for metals analysts and technicians performing routine or referee chemical analysis of beryllium in sectors such as aerospace, nuclear, electronics, and specialty material production.

• Interlaboratory Studies:
  The standard’s methodologies are suitable for participation in interlaboratory studies and proficiency testing, ensuring consistency and comparability of analytical data across institutions.

• Product Certification:
  Supports certification and traceability for beryllium products in regulated industries where chemical composition is critical for safety and performance.

Related Standards

ASTM E439-23 is supported and referenced by several related standards on chemical analysis and laboratory practices, including:

• ASTM D1193 – Specification for Reagent Water
• ASTM E29 – Practice for Using Significant Digits in Test Data
• ASTM E50 – Practices for Apparatus, Reagents, and Safety Considerations
• ASTM E60 – Practice for Analysis of Metals by Spectrophotometry
• ASTM E55 – Performance for Sampling Wrought Nonferrous Metals
• ASTM E88 – Practice for Sampling Nonferrous Metals in Cast Form
• ASTM E1601 – Practice for Interlaboratory Study Performance

These documents provide guidance on sample collection, reagent standards, apparatus suitability, laboratory safety, and quality control, ensuring the reliable implementation of ASTM E439-23 in chemical analysis of beryllium and its alloys.

---

Keywords: chemical analysis of beryllium, ASTM E439-23, spectrophotometric test methods, beryllium alloy testing, laboratory chemical analysis standard, beryllium safety, quality control in beryllium production, material specification compliance.

Standards Content (Sample)

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.
Designation: E439 − 23
Standard Test Methods for
Chemical Analysis of Beryllium
This standard is issued under the fixed designation E439; 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 2. Referenced Documents
1.1 These test methods cover the chemical analysis of 2.1 ASTM Standards:
beryllium having chemical compositions within the following D1193 Specification for Reagent Water
limits: E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
Element Range, %
Aluminum 0.05 to 0.30
E50 Practices for Apparatus, Reagents, and Safety Consid-
Beryllium 97.5 to 100
erations for Chemical Analysis of Metals, Ores, and
Beryllium Oxide 0.3 to 3
Related Materials
Carbon 0.05 to 0.30
Copper 0.005 to 0.10
E55 Practice for Sampling Wrought Nonferrous Metals and
Chromium 0.005 to 0.10
Alloys for Determination of Chemical Composition
Iron 0.05 to 0.30
E60 Practice for Analysis of Metals, Ores, and Related
Magnesium 0.02 to 0.15
Nickel 0.005 to 0.10
Materials by Spectrophotometry
Silicon 0.02 to 0.15
E88 Practice for Sampling Nonferrous Metals and Alloys in
1.2 The test methods in this standard are contained in the
Cast Form for Determination of Chemical Composition
sections as follows.
E135 Terminology Relating to Analytical Chemistry for
Sections Metals, Ores, and Related Materials
Chromium by the Diphenylcarbazide Spectrophotometric Test
E173 Practice for Conducting Interlaboratory Studies of
Method
Methods for Chemical Analysis of Metals (Withdrawn
[0.004 % to 0.04 %] 10 – 19
Iron by the 1,10-Phenanthroline Spectrophotometric Test Method
1997)
[0.05 % to 0.25 %] 20 – 29
E1601 Practice for Conducting an Interlaboratory Study to
Manganese by the Periodate Spectrophotometric Test Method
Evaluate the Performance of an Analytical Method
[0.008 % to 0.04 %] 30 – 39
Nickel by the Dimethylglyoxime Spectrophotometric Test Method
3. Terminology
[0.001 % to 0.04 %] 40 – 49
1.3 The values stated in SI units are to be regarded as
3.1 For definitions of terms used in this test method, refer to
standard. No other units of measurement are included in this
Terminology E135.
standard.
4. Significance and Use
1.4 This standard does not purport to address all of the
4.1 These test methods for the chemical analysis of beryl-
safety concerns, if any, associated with its use. It is the
lium metal are primarily intended as referee methods to test
responsibility of the user of this standard to establish appro-
such materials for compliance with compositional specifica-
priate safety, health, and environmental practices and deter-
tions. It is assumed that all who use these test methods will be
mine the applicability of regulatory limitations prior to use.
trained analysts capable of performing common laboratory
1.5 This international standard was developed in accor-
procedures skillfully and safely. It is expected that work will be
dance with internationally recognized principles on standard-
performed in a properly equipped laboratory.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
5. Apparatus, Reagents, and Spectrophotometric Practice
mendations issued by the World Trade Organization Technical
5.1 Apparatus and reagents required for each determination
Barriers to Trade (TBT) Committee.
are listed in separate sections preceding the procedure unless
These test methods are under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct For referenced ASTM standards, visit the ASTM website, www.astm.org, or
responsibility of Subcommittee E01.05 on Cu, Pb, Zn, Cd, Sn, Be, Precious Metals, contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
their Alloys, and Related Metals. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved July 1, 2023. Published July 2023. Originally published the ASTM website.
in 1971. Last previous edition approved in 2017 as E439 – 17. DOI: 10.1520/ The last approved version of this historical standard is referenced on
E0439-23. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E439 − 23
otherwise specified. The apparatus and standard solutions shall 11. Summary of Test Method
conform to the requirements prescribed in Practices E50.
11.1 Chromium is oxidized by peroxydisulfate in the pres-
Spectrophotometers shall conform to the requirements pre-
ence of silver nitrate, and the chromium diphenylcarbazide
scribed in Practice E60.
complex is then developed. Spectrophotometric measurement
5.2 Spectrophotometric practice prescribed in these test is made at 540 nm.
methods shall conform to Practice E60.
12. Chromium Concentration Range
5.3 Purity of Reagents—Reagent grade chemicals shall be
12.1 The recommended concentration range is from
used in all tests. Unless otherwise indicated, all reagents shall
0.02 mg to 0.10 mg of chromium per 250 mL of solution, using
conform to the specifications of the Committee on Analytical
a 2-cm cell.
Reagents of the American Chemical Society where such
specifications are available. Other grades may be used, pro-
NOTE 1—This test method has been written for cells having a 2-cm light
path. Cells having other dimensions may be used, provided suitable
vided it is first ascertained that the reagent is of sufficiently
adjustments can be made in the amounts of sample and reagents used.
high purity to permit its use without lessening the accuracy of
the determination.
13. Stability of Color
13.1 The color of the chromium complex develops almost
6. Hazards
immediately but starts to fade after about 10 min. Spectropho-
6.1 For precautions to be observed in these test methods,
tometric measurements should be made within 5 min after
refer to Practices E50.
developing the color.
6.2 Processing beryllium and beryllium-containing materi-
14. Interferences
als poses a health risk if safe-handling practices are not
followed. Inhalation of airborne beryllium may cause a serious
14.1 The elements ordinarily present do not interfere if their
lung disorder in some individuals. Occupational safety and
mass fractions are under the maximum limits shown in 1.1.
health regulatory agencies have set mandatory limits on
15. Reagents
occupational respiratory exposures. Read and follow the guid-
ance in the SDS before working with these materials.
15.1 Acetone (CH COCH ).
3 3
15.2 Ammonium Peroxydisulfate Solution (100 g ⁄L)—
7. Sampling
Dissolve 10 g of ammonium peroxydisulfate ((NH ) S O ) in
4 2 2 8
7.1 Wrought products shall be sampled in accordance with
water and dilute to 100 mL. Do not use a solution that has
Practice E55. Cast products shall be sampled in accordance
stood more than 12 h.
with Practice E88. However, these practices do not supersede
15.3 Chromium, Standard Solution (1 mL = 0.005 mg Cr)—
any sampling requirements specified in a specific ASTM
Dissolve 0.2830 g of potassium dichromate (K Cr O ) in water
2 2 7
material specification.
in a 1-L volumetric flask, dilute to volume, and mix. Using a
pipet, transfer 5 mL to a 100-mL volumetric flask, dilute to
8. Rounding Calculated Values
volume, and mix.
8.1 Rounding of test results obtained using this test method
15.4 Diphenylcarbazide Solution (5 g ⁄L)—Dissolve 0.50 g
shall be performed as directed in Practice E29, Rounding
of diphenylcarbazide (1,5-diphenylcarbohydrazide) in 100 mL
Method, unless an alternative rounding method is specified by
of acetone. Do not use a solution that has stood for more than
the customer or applicable material specification.
1 h.
9. Interlaboratory Studies
15.5 Potassium Pyrosulfate (K S O ).
2 2 7
9.1 These test methods have been evaluated in accordance
15.6 Silver Nitrate Solution (2.5 g ⁄L)—Dissolve 0.25 g of
with Practice E173, unless otherwise noted in the precision
silver nitrate (AgNO ) in water and dilute to 100 mL.
section.
15.7 Sodium Hydroxide Solution (500 g/L)—Dissolve 50 g
of NaOH in water and dilute to 100 mL.
CHROMIUM BY THE DIPHENYLCARBAZIDE
SPECTROPHOTOMETRIC TEST METHOD
15.8 Purity of Water—Unless otherwise indicated, refer-
ences to water shall mean reagent water conforming to Type I
10. Scope
or Type II of Specification D1193. Type III or Type IV may be
used if they effect no measurable change in the blank or
10.1 This test method covers the determination of chro-
sample.
mium from 0.004 % to 0.04 %.
16. Preparation of Calibration Curve
16.1 Calibration Solutions:
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
Standard-Grade Reference Materials, American Chemical Society, Washington,
16.1.1 Using a pipet, transfer (5, 10, 15, and 20) mL of
DC. For suggestions on the testing of reagents not listed by the American Chemical
chromium standard solution (1 mL = 0.005 mg Cr) to 400-mL
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
beakers. Add 1 mL of H PO (1 + 1) and dilute to 250 mL
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma- 3 4
copeial Convention, Inc. (USPC), Rockville, MD. with water.
E439 − 23
16.1.2 Adjust the pH to 0.95 6 0.05 with NaOH solution or 18. Calculation
H SO (1 + 1). Add 10 mL of AgNO solution, 10 mL of
2 4 3
18.1 Convert the net spectrophotometric absorbance reading
(NH ) S O solution, and a few glass beads. Cover the beaker
4 2 2 8
of the test solution to milligrams of chromium by means of the
with a ribbed cover glass, and boil for at least 25 min. During
calibration curve. Calculate the percentage of chromium as
this period, add water as required to maintain a volume not less
follows:
than 150 mL. Cool, and transfer to a 250-mL volumetric flask.
Chromium, % 5 A/ B × 10 (1)
~ !
Proceed as directed in 16.3.
where:
16.2 Reference Solution—Add 1 mL of H PO (1 + 1) to
3 4
A = chromium found in 250 mL of the final test solution,
250 mL of water in a 400-mL beaker. Proceed as directed in
mg, and
16.1.2.
B = sample represented in 250 mL of the final test solution,
16.3 Color Development—Add 2.0 mL of diphenylcarbaz-
g.
ide solution. Dilute to volume, and mix.
16.3.1 Prepare only that number of solutions which can be
19. Precision and Bias
measured 5 min after color development.
19.1 Precision—Eight analysts from seven laboratories co-
16.4 Spectrophotometry: operated in testing this test method and obtained the data
summarized in Table 1.
16.4.1 Multiple-Cell Spectrophotometer—Measure the cell
correction, using absorption cells with a 2-cm light path and a
19.2 Bias—No certified reference materials suitable for
light band centered at 540 nm. Using the test cell, take the
testing this test method were available when this interlabora-
spectrophotometric absorbance readings of the calibration
tory testing program was conducted. The user of this standard
solutions.
is encouraged to employ accepted reference materials, if
16.4.2 Single-Cell Spectrophotometer—Transfer a suitable available, to determine the bias of this test method as applied
portion of the reference solution to an absorption cell with a
in a specific laboratory.
2-cm light path and adjust the spectrophotometer to the initial
19.3 Practice E173 has been replaced by Practice E1601.
setting using a light band centered at 540 nm. While maintain-
The Reproducibility Index R of Practice E173 corresponds to
ing this adjustment, take the spectrophotometric absorbance
the Reproducibility Index R of Practice E1601. The Repeat-
readings of the calibration solutions.
ability Index R of Practice E173 corresponds to the Repeat-
ability Index r of Practice E1601.
16.5 Calibration Curve—Plot the net spectrophotometric
absorbance readings of the calibration solutions against milli-
IRON BY THE 1,10-PHENANTHROLINE
grams of chromium per 250 mL of solution.
SPECTROPHOTOMETRIC TEST METHOD
17. Procedure
20. Scope
17.1 Test Solution:
20.1 This test method covers the determination of iron from
17.1.1 Transfer a 0.50-g sample, weighed to the nearest
0.05 % to 0.25 %.
0.1 mg, to a 250-mL beaker. Add 100 mL of water and, in small
increments, add 15 mL of H SO (1 + 1). When reaction has
2 4 21. Summary of Test Method
ceased, warm until all action stops. If the chromium content of
21.1 The iron is reduced with hydroxylamine hydrochloride
the sample is between 0.02 % and 0.04 %, use a 0.25-g sample.
and converted to the 1,10-phenanthroline complex. Spectro-
17.1.2 Filter through an 11-cm fine filter paper into a
photometric measurement is made at 515 nm.
400-mL beaker. Wash the paper five times or six times with hot
water. Reserve the filtrate. Transfer the paper to a platinum
22. Iron Concentration Range
crucible, dry, and ignite at 700 °C.
22.1 The recommended concentration range is from
17.1.3 Treat the residue with one drop of H SO (1 + 1),
2 4
0.05 mg to 0.250 mg of iron per 100 mL of solution using a
three drops or four drops of HNO , and 3 mL or 4 mL of HF.
2-cm cell.
Evaporate to complete dryness and ignite for 3 min to 4 min at
900 °C. Fuse the residue with about 1 g of potassium pyro- NOTE 2—This test method has been written for cells having a 2-cm light
path. Cells having other dimensions may be used, provided suitable
sulfate (K S O ). Cool, leach in 25 mL of water, add this
2 2 7
adjustments can be made in the amounts of sample and reagents used.
solution to the reserved filtrate (17.1.2), and dilute to 250 mL.
Proceed as directed in 16.1.2.
17.2 Reference Solution—Carry a reagent blank through the
TABLE 1 Statistical Information
entire procedure, using the same amounts of all reagents with
the sample omitted. Repeatability Reproducibility
Chromium
Test Material (R , Practice (R , Practice
1 2
Found, %
17.3 Color Development—Proceed as directed in 16.3. E173) E173)
1 0.007 less than 0.001 0.001
17.4 Spectophotometry—Take the spectrophotometric ab-
2 0.020 0.002 0.003
sorbance reading of the test solution as directed in 16.4.
E439 − 23
23. Stability of Color setting, using a light band centered at 515 nm. While main-
taining this adjustment, take the spectrophotometric absor-
23.1 The color develops within 10 min and is stable for at
bance readings of the calibration solutions.
least 2 h.
26.5 Calibration Curve—Plot the net spectrophotometric
24. Interferences
absorbance readings of the calibration solutions against milli-
grams of iron per 100 mL of solution.
24.1 Nickel forms a complex with and consumes 1,10-
phenanthroline. However, an amount of nickel equivalent to
27. Procedure
four times the amount of iron does not affect the iron
27.1 Test Solution:
determination. Other elements ordinarily present in beryllium
27.1.1 Transfer a 1.0-g sample, weighed to the nearest 1 mg
do not interfere if their mass fractions are under the maximum
to a 250-mL beaker. Add 100 mL of water and, in small
limits shown in 1.1.
increments, add 25 mL of H SO (1 + 1). When the reaction
2 4
25. Reagents
has ceased, warm until all action stops.
27.1.2 Filter using an 11-cm fine paper into a 500-mL
25.1 Ammonium Acetate Solution (230 g ⁄L)—Dissolve
volumetric flask. Wash the paper five times or six times with
115 g of ammonium acetate in water and dilute to 500 mL.
hot water. Transfer the paper to a platinum crucible and ignite
25.2 Hydroxylamine Hydrochloride Solution (100 g ⁄L)—
at 700 °C. Reserve the filtrate.
Dissolve 5.0 g of hydroxylamine hydrochloride (NH OH·HCl)
27.1.3 Treat the residue with one drop of H SO (1 + 1),
2 4
in 50 mL of water. Prepare fresh as needed.
three drops or four drops of HNO , and 3 mL to 4 mL of HF.
25.3 Iron, Standard Solution (1 mL = 0.01 mg Fe)— Evaporate to complete dryness and ignite for 3 min to 4 min at
900 °C. Fuse the residue with 1 g of potassium pyrosulfate
Dissolve 0.7020 g of ferrous ammonium sulfate
(Fe(NH ) (SO ) ·6H O) in 10 mL of water, and add 1 mL of (K S O ). Cool, leach in 25 mL of water, and add this solution
4 2 4 2 2 2 2 7
to the reserved filtrate (27.1.2). Dilute to volume and mix.
H SO (1 + 1). Transfer to a 100-mL volumetric flask, dilute
2 4
to volume, and mix. Using a pipet, transfer 50.0 mL to a 100-mL volumetric flask.
27.2 Reference Solution—Carry a reagent blank through the
25.4 1,10-Phenanthroline Solution (1 g ⁄L)—Dissolve 0.1 g
of 1,10-phenanthroline monohydrate in 100 mL of water. entire procedure, using the same amounts of all reagents with
the sample omitted.
25.5 Potassium Pyrosulfate (K S O ).
2 2 7
27.3 Color Development—Proceed as directed in 26.3.
25.6 Purity of Water—Unless otherwise indicated, refer-
ences to water shall mean reagent water conforming to Type I 27.4 Spectrophotometry—Take the spectrophotometric ab-
or Type II of Specification D1193. Type III or Type IV may be sorbance reading of the test solution as directed in 26.4.
used if they effect no measurable change in the blank or
28. Calculation
sample.
28.1 Convert the net spectrophotometric absorbance reading
26. Preparation of Calibration Curve
of the test solution to milligrams of iron by means of the
calibration curve. Calculate the percentage of iron as follows:
26.1 Calibration Solutions—Using a pipet, transfer (5, 10,
15, 20, and 25) mL of iron standard solution (1 mL = 0.01 mg
Iron, % 5 A/~B × 10! (2)
Fe) to 100-mL volumetric flasks. Add 1 mL of H SO (1 + 1)
2 4
where:
and dilute to 50 mL. Proceed as directed in 26.3.
A = iron found in 100 mL of final test solution, mg, and
26.2 Reference Solution—Transfer 50 mL of water and
B = sample represented in 100 mL of final test solution, g.
1 mL of H SO (1 + 1) to a 100-mL volumetric flask. Proceed
2 4
as directed in 26.3.
29. Precision and Bias
26.3 Color Development—Add 3 mL of NH OH·HCl
solution, and 20 mL of ammonium acetate solution, and mix.
29.1 Precision—Eight laboratories cooperated in testing this
Add 10 mL of 1,10-phenanthroline solution, and mix. Check
test method and obtained the data summarized in Table 2.
the pH of the solution with indicator paper and,
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: E439 − 17 E439 − 23
Standard Test Methods for
Chemical Analysis of Beryllium
This standard is issued under the fixed designation E439; 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 These test methods cover the chemical analysis of beryllium having chemical compositions within the following limits:
Element Range, %
Aluminum 0.05 to 0.30
Beryllium 97.5 to 100
Beryllium 97.5 to 100
Beryllium Oxide 0.3 to 3
Carbon 0.05 to 0.30
Copper 0.005 to 0.10
Chromium 0.005 to 0.10
Iron 0.05 to 0.30
Magnesium 0.02 to 0.15
Nickel 0.005 to 0.10
Silicon 0.02 to 0.15
1.2 The test methods in this standard are contained in the sections indicated below.as follows.
Sections
Chromium by the Diphenylcarbazide Spectrophotometric Test
Method
[0.004 % to 0.04 %] 10 – 19
Iron by the 1,10-Phenanthroline Spectrophotometric Test Method
[0.05 % to 0.25 %] 20 – 29
Manganese by the Periodate Spectrophotometric Test Method
[0.008 % to 0.04 %] 30 – 39
Nickel by the Dimethylglyoxime Spectrophotometric Test Method
[0.001 % to 0.04 %] 40 – 49
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 problems,concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appropriate safety and healthsafety, health, and environmental practices and
determine the applicability of regulatory limitations prior to use.
1.5 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.
These test methods are under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and are the direct responsibility
of Subcommittee E01.05 on Cu, Pb, Zn, Cd, Sn, Be, Precious Metals, their Alloys, and Related Metals.
Current edition approved May 1, 2017July 1, 2023. Published July 2017July 2023. Originally published in 1971. Last previous edition approved in 20102017 as
E439 – 10.E439 – 17. DOI: 10.1520/E0439-17.10.1520/E0439-23.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E439 − 23
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E50 Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
E55 Practice for Sampling Wrought Nonferrous Metals and Alloys for Determination of Chemical Composition
E60 Practice for Analysis of Metals, Ores, and Related Materials by Spectrophotometry
E88 Practice for Sampling Nonferrous Metals and Alloys in Cast Form for Determination of Chemical Composition
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E173 Practice for Conducting Interlaboratory Studies of Methods for Chemical Analysis of Metals (Withdrawn 1997)
E1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method
3. Terminology
3.1 For definitions of terms used in this test method, refer to Terminology E135.
4. Significance and Use
4.1 These test methods for the chemical analysis of beryllium metal are primarily intended as referee methods to test such
materials for compliance with compositional specifications. It is assumed that all who use these test methods 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.
5. Apparatus, Reagents, and Spectrophotometric Practice
5.1 Apparatus and reagents required for each determination are listed in separate sections preceding the procedure unless
otherwise specified. The apparatus, standard solutions, and reagents apparatus and standard solutions shall conform to the
requirements prescribed in Practices E50. Spectrophotometers shall conform to the requirements prescribed in Practice E60.
5.2 Spectrophotometric practice prescribed in these test methods shall conform to Practice E60.
5.3 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, all reagents shall conform
to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such specifications are
available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use
without lessening the accuracy of the determination.
6. Hazards
6.1 For precautions to be observed in these test methods, reference is made refer to Practices E50. Both beryllium metal and its
compounds may be toxic. Exercise care to prevent contact of beryllium-containing materials with the skin. The inhalation of any
beryllium-containing substance, either as a volatile compound or as finely divided powder, should be especially avoided.
Beryllium-containing residues (especially ignited oxide) should be carefully disposed of.
6.2 Processing beryllium and beryllium-containing materials poses a health risk if safe-handling practices are not followed.
Inhalation of airborne beryllium may cause a serious lung disorder in some individuals. Occupational safety and health regulatory
agencies have set mandatory limits on occupational respiratory exposures. Read and follow the guidance in the SDS before
working with these materials.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
ACS Reagent Chemicals, Specifications and Procedures for Reagents and Standard-Grade Reference Materials, American Chemical Society, Washington, DC. For
suggestions on the testing of reagents not listed by the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and
the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
E439 − 23
7. Sampling
7.1 Wrought products shall be sampled in accordance with Practice E55. Cast products shall be sampled in accordance with
Practice E88. However, these test methods practices do not supersede any sampling requirements specified in a specific ASTM
material specification.
8. Rounding Calculated Values
8.1 Rounding of test results obtained using this test method shall be performed as directed in Practice E29, Rounding Method,
unless an alternative rounding method is specified by the customer or applicable material specification.
9. Interlaboratory Studies
9.1 These test methods have been evaluated in accordance with Practice E173, unless otherwise noted underin the precision
section.
CHROMIUM BY THE DIPHENYLCARBAZIDE
(SPECTROPHOTOMETRIC)SPECTROPHOTOMETRIC TEST METHOD
10. Scope
10.1 This test method covers the determination of chromium from 0.004 % to 0.04 %.
10.2 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.
10. Scope
10.1 This test method covers the determination of chromium from 0.004 % to 0.04 %.
11. Summary of Test Method
11.1 Chromium is oxidized by peroxydisulfate in the presence of silver nitrate, and the chromium diphenylcarbazide complex is
then developed. Spectrophotometric measurement is made at 540 nm.
12. Chromium Concentration Range
12.1 The recommended concentration range is from 0.02 mg to 0.10 mg of chromium per 250 mL of solution, using a 2-cm cell.
NOTE 1—This test method has been written for cells having a 2-cm light path. Cells having other dimensions may be used, provided suitable adjustments
can be made in the amounts of sample and reagents used.
13. Stability of Color
13.1 The color of the chromium complex develops almost immediately but starts to fade after about 10 min. Spectrophotometric
measurements should be made within 5 min after developing the color.
14. Interferences
14.1 The elements ordinarily present do not interfere if their mass fractions are under the maximum limits shown in 1.1.
15. Reagents
15.1 Acetone (CH COCH ).
3 3
E439 − 23
15.2 Ammonium Peroxydisulfate Solution (100 g ⁄L)—Dissolve 10 g of ammonium peroxydisulfate ((NH ) S O ) in water and
4 2 2 8
dilute to 100 mL. Do not use a solution that has stood more than 12 h.
15.3 Chromium, Standard Solution (1 mL = 0.005 mg Cr)—Dissolve 0.2830 g of potassium dichromate (K Cr O ) in water in a
2 2 7
1-L volumetric flask, dilute to volume, and mix. Using a pipet, transfer 5 mL to a 100-mL volumetric flask, dilute to volume, and
mix.
15.4 Diphenylcarbazide Solution (5 g ⁄L)—Dissolve 0.50 g of diphenylcarbazide (1,5-diphenylcarbohydrazide) in 100 mL of
acetone. Do not use a solution that has stood for more than 1 h.
15.5 Potassium Pyrosulfate (K S O ).
2 2 7
15.6 Silver Nitrate Solution (2.5 g ⁄L)—Dissolve 0.25 g of silver nitrate (AgNO ) in water and dilute to 100 mL.
15.7 Sulfuric Acid Sodium Hydroxide Solution (1 + 1)—Mix carefully and with stirring one volume of concentrated H(500
g/L)—Dissolve 50 g of NaOH in SO (sp gr 1.84) into one volume of water. water and dilute to 100 mL.
2 4
15.8 Purity of Water—Unless otherwise indicated, referencereferences to water shall be understood to mean reagent water as
defined by Type conforming to Type I or Type II of Specification D1193. Type III or Type IV may be used if they effect no
measurable change in the blank or sample.
16. Preparation of Calibration Curve
16.1 Calibration Solutions:
16.1.1 Using a pipet, transfer (5, 10, 15, and 20) mL of chromium standard solution (1 mL = 0.005 mg Cr) to 400-mL beakers.
Add 1 mL of H PO (1 + 1) and dilute to 250 mL with water.
3 4
16.1.2 Adjust the pH to 0.95 6 0.05 with NaOH solution or H SO (1 + 1). Add 10 mL of AgNO solution, 10 mL of (NH ) S O
2 4 3 4 2 2 8
solution, and a few glass beads. Cover the beaker with a ribbed cover glass, and boil for at least 25 min. During this period, add
water as required to maintain a volume not less than 150 mL. Cool, and transfer to a 250-mL volumetric flask. Proceed as directed
in 16.3.
16.2 Reference Solution—Add 1 mL of H PO (1 + 1) to 250 mL of water in a 400-mL beaker. Proceed as directed in 16.1.2.
3 4
16.3 Color Development—Add 2.0 mL of diphenylcarbazide solution. Dilute to volume, and mix.
16.3.1 Prepare only that number of solutions which can be measured 5 min after color development.
16.4 Spectrophotometry:
16.4.1 Multiple-Cell Spectrophotometer—Measure the cell correction, using absorption cells with a 2-cm light path and a light
band centered at 540 nm. Using the test cell, take the spectrophotometric absorbance readings of the calibration solutions.
16.4.2 Single-Cell Spectrophotometer—Transfer a suitable portion of the reference solution to an absorption cell with a 2-cm light
path and adjust the spectrophotometer to the initial setting using a light band centered at 540 nm. While maintaining this
adjustment, take the spectrophotometric absorbance readings of the calibration solutions.
16.5 Calibration Curve—Plot the net spectrophotometric absorbance readings of the calibration solutions against milligrams of
chromium per 250 mL of solution.
17. Procedure
17.1 Test Solution:
E439 − 23
17.1.1 Transfer a 0.50-g sample, weighed to the nearest 0.1 mg, 0.1 mg, to a 250-mL beaker. Add 100 mL of water and, in small
increments, add 15 mL of H SO (1 + 1). When reaction has ceased, warm until all action stops. If the chromium content of the
2 4
sample is between 0.02 % and 0.04 %, use a 0.25-g sample.
17.1.2 Filter through an 11-cm fine filter paper into a 400-mL beaker. Wash the paper five times or six times with hot water.
Reserve the filtrate. Transfer the paper to a platinum crucible, dry, and ignite at 700 °C.
17.1.3 Treat the residue with one drop of H SO (1 + 1), three drops or four drops of HNO , and 3 mL or 4 mL of HF. Evaporate
2 4 3
to complete dryness,dryness and ignite for 3 min to 4 min at 900 °C. Fuse the residue with about 1 g of potassium pyrosulfate
(K S O ). Cool, leach in 25 mL of water, add this solution to the reserved filtrate (17.1.2), and dilute to 250 mL. Proceed as
2 2 7
directed in 16.1.2.
17.2 Reference Solution—Carry a reagent blank through the entire procedure, using the same amounts of all reagents with the
sample omitted.
17.3 Color Development—Proceed as directed in 16.3.
17.4 Spectophotometry—Take the spectrophotometric absorbance reading of the test solution as directed in 16.4.
18. Calculation
18.1 Convert the net spectrophotometric absorbance reading of the test solution to milligrams of chromium by means of the
calibration curve. Calculate the percentage of chromium as follows:
Chromium,%5 A/ B ×10 (1)
~ !
where:
A = chromium found in 250 mL of the final test solution, mg, and
B = sample represented in 250 mL of the final test solution, g.
19. Precision and Bias
19.1 Precision—Eight analysts from seven laboratories cooperated in testing this test method and obtained the data summarized
in Table 1.
19.2 Bias—No certified reference materials suitable for testing this test method were available when this interlaboratory testing
program was conducted. The user of this standard is encouraged to employ accepted reference materials, if available, to determine
the bias of this test method as applied in a specific laboratory.
19.3 Practice E173 has been replaced by Practice E1601. The Reproducibility Index R of Practice E173 corresponds to the
Reproducibility Index R of Practice E1601. The Repeatability Index R of Practice E173 corresponds to the Repeatability Index
r of Practice E1601.
IRON BY THE 1,10-PHENANTHROLINE
SPECTROPHOTOMETRIC TEST METHOD
TABLE 1 Statistical Information
Repeatability Reproducibility
Chromium
Test Material (R , Practice (R , Practice
1 2
Found, %
E173) E173)
1 0.007 less than 0.001 0.001
2 0.020 0.002 0.003
E439 − 23
20. Scope
20.1 This test method covers the determination of iron from 0.05 % to 0.25 %.
20.2 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.
20. Scope
20.1 This test method covers the determination of iron from 0.05 % to 0.25 %.
21. Summary of Test Method
21.1 The iron is reduced with hydroxylamine hydrochloride and converted to the 1,10-phenanthroline complex. Spectrophoto-
metric measurement is made at 515 nm.
22. Iron Concentration Range
22.1 The recommended concentration range is from 0.05 mg to 0.250 mg of iron per 100 mL of solution using a 2-cm cell.
NOTE 2—This test method has been written for cells having a 2-cm light path. Cells having other dimensions may be used, provided suitable adjustments
can be made in the amounts of sample and reagents used.
23. Stability of Color
23.1 The color develops within 10 min and is stable for at least 2 h.
24. Interferences
24.1 Nickel forms a complex with and consumes 1,10-phenanthroline. However, an amount of nickel equivalent to four times the
amount of iron does not affect the iron determination. Other elements ordinarily present in beryllium do not interfere if their
percentages mass fractions are under the maximum limits shown in 1.1.
25. Reagents
25.1 Ammonium Acetate Solution (230 g ⁄L)—Dissolve 115 g of ammonium acetate in water and dilute to 500 mL.
25.2 Hydroxylamine Hydrochloride Solution (100 g ⁄L)—Dissolve 5.0 g of hydroxylamine hydrochloride (NH OH·HCl) in 50 mL
of water. Prepare fresh as needed.
25.3 Iron, Standard Solution (1 mL = 0.01 mg Fe)—Dissolve 0.7020 g of ferrous ammonium sulfate (Fe(NH ) (SO ) · 6H·6H O)
4 2 4 2 2
in 10 mL of water, and add 1 mL of H SO (1 + 1). Transfer to a 100-mL volumetric flask, dilute to volume, and mix.
2 4
25.4 1,10-Phenanthroline Solution (1 g ⁄L)—Dissolve 0.1 g of 1,10-phenanthroline monohydrate in 100 mL of water.
25.5 Potassium Pyrosulfate (K S O ).
2 2 7
25.6 Purity of Water—Unless otherwise indicated, referencereferences to water shall be understood to mean reagent water as
defined by Type conforming to Type I or Type II of Specification D1193. Type III or Type IV may be used if they effect no
measurable change in the blank or sample.
26. Preparation of Calibration Curve
26.1 Calibration Solutions—Using a pipet, transfer (5, 10, 15, 20, and 25) mL of iron standard solution (1 mL = 0.01 mg Fe) to
100-mL volumetric flasks. Add 1 mL of H SO (1 + 1) and dilute to 50 mL. Proceed as directed in 26.3.
2 4
E439 − 23
26.2 Reference Solution—Transfer 50 mL of water and 1 mL of H SO (1 + 1) to a 100-mL volumetric flask. Proceed as directed
2 4
in 26.3.
26.3 Color Development—Add 3 mL of NH OH·HCl solution, and 20 mL of ammonium acetate solution, and mix. Add 10 mL
of 1,10-phenanthroline solution, and mix. Check the pH of the solution with indicator paper and, if required, add ammonium
acetate solution to adjust the pH to between 4.0 and 4.5. Dilute to volume, and mix.
26.4 Spectrophotometry:
26.4.1 Multiple-Cell Spectrophotometer—Determine the cell correction using absorption cells with a 2-cm light path and a light
band centered at 515 nm. Using the test cell, take the spectrophotometric absorbance readings of the calibration solutions.
26.4.2 Single-Cell Spectrophotometer—Transfer a suitable portion of the reference solution to an absorption cell with a 2-cm light
path and adjust the spectrophotometer to the initial setting, using a light band centered at 515 nm. While maintaining this
adjustment, take the spectrophotometric absorbance readings of the calibration solutions.
26.5 Calibration Curve—Plot the net spectrophotometric absorbance readings of the calibration solutions against milligrams of
iron per 100 mL of solution.
27. Procedure
27.1 Test Solution:
27.1.1 Transfer a 1.0-g sample, weighed to the nearest 1 mg to a 250-mL beaker. Add 100 mL of water and, in small increments,
add 25 mL of H SO (1 + 1). When the apparent reaction has ceased, warm until all action stops.
2 4
27.1.2 Filter using an 11-cm fine paper into a 500-mL volumetric flask. Wash the paper five times or six times with hot water.
Transfer the paper to a platinum crucible and ignite at 700 °C. Reserve the filtrate.
27.1.3 Treat the residue with one drop of H SO (1 + 1), three drops or four drops of HNO , and 3 mL to 4 mL of HF. Evaporate
2 4 3
to complete dryness and ignite for 3 min to 4 min at 900 °C. Fuse the residue with 1 g of potassium pyrosulfate (K S O ). Cool,
2 2 7
leach in 25 mL of water, and add this solution to the reserved filtrate (27.1.2). Dilute
...