ASTM F3139-15(2023)
(Test Method)Standard Test Method for Analysis of Tin-Based Solder Alloys for Minor and Trace Elements Using Inductively Coupled Plasma Atomic Emission Spectrometry
Standard Test Method for Analysis of Tin-Based Solder Alloys for Minor and Trace Elements Using Inductively Coupled Plasma Atomic Emission Spectrometry
SIGNIFICANCE AND USE
4.1 Tin-based solder alloys are commonly used to manufacture electrical and electronic goods. The elements lead, cadmium, mercury, antimony and bismuth are often declarable substances in solder materials. This test method provides a means of determining the listed declarable substances, as well as other minor and trace constituents, in tin-based solder alloys.
4.2 Two methods of dissolving tin-based solder alloys are given in this standard. The first method uses open-vessel hydrofluoric and nitric acid room temperature digestions; the second method employs closed-vessel nitric and hydrofluoric acid microwave digestions, both for use only with ICP-AES instruments equipped with a hydrofluoric acid resistant sample introduction system.
4.3 The method of preparing calibration solutions uses 1000 mg/kg single element reference material solutions, and uses matching concentrated acids for both the calibration solutions and the sample solutions.
4.4 This test method is intended for use by laboratories experienced with the set-up, calibration and analysis of samples using ICP-AES.
SCOPE
1.1 This test method covers procedures for the analysis of tin-based solder alloys for minor and trace elements using inductively-coupled plasma atomic emission spectrometry (ICP-AES) instrumentation.
1.2 These test procedures were validated for the analytes and mass fractions listed below.
Element
Validated Mass Fraction
Range, mg/kg
Lead
115 to 965
Cadmium
25 to 60
Mercury
5 to 530
Antimony
85 to 1330
Bismuth
80 to 210
Arsenic
95 to 360
Silver
4000 to 42100
Cobalt
0.5 to 60
Iron
15 to 115
Chromium
0.5 to 1.5
Copper
3000 to 30600
Indium
25 to 115
Nickel
5 to 150
Phosphorus
10 to 110
Selenium
1 to 30
Zinc
2 to 160
Aluminum
1 to 3
1.3 The procedures appear in the following order:
Procedure
Section
Internal Standardization
8
Calibration Solution Preparations
9
Preparation of Sample and Validation Solutions
10
Calibration
11
Analysis Procedure
12
1.4 The values stated in SI units are to be regarded as the standard. Any other values are for information only.
1.5 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.
1.6 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
Relations
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: F3139 − 15 (Reapproved 2023)
Standard Test Method for
Analysis of Tin-Based Solder Alloys for Minor and Trace
Elements Using Inductively Coupled Plasma Atomic
Emission Spectrometry
This standard is issued under the fixed designation F3139; 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 priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.1 This test method covers procedures for the analysis of
1.6 This international standard was developed in accor-
tin-based solder alloys for minor and trace elements using
dance with internationally recognized principles on standard-
inductively-coupled plasma atomic emission spectrometry
ization established in the Decision on Principles for the
(ICP-AES) instrumentation.
Development of International Standards, Guides and Recom-
1.2 These test procedures were validated for the analytes
mendations issued by the World Trade Organization Technical
and mass fractions listed below.
Barriers to Trade (TBT) Committee.
Element Validated Mass Fraction
Range, mg/kg
2. Referenced Documents
Lead 115 to 965
2.1 ASTM Standards:
Cadmium 25 to 60
D1129 Terminology Relating to Water
Mercury 5 to 530
Antimony 85 to 1330 E177 Practice for Use of the Terms Precision and Bias in
Bismuth 80 to 210
ASTM Test Methods
Arsenic 95 to 360
E416 Practice for Planning and Safe Operation of a Spec-
Silver 4000 to 42100
Cobalt 0.5 to 60 trochemical Laboratory (Withdrawn 2005)
Iron 15 to 115
E691 Practice for Conducting an Interlaboratory Study to
Chromium 0.5 to 1.5
Determine the Precision of a Test Method
Copper 3000 to 30600
Indium 25 to 115
E1479 Practice for Describing and Specifying Inductively
Nickel 5 to 150
Coupled Plasma Atomic Emission Spectrometers
Phosphorus 10 to 110
Selenium 1 to 30
Zinc 2 to 160
3. Terminology
Aluminum 1 to 3
3.1 Definitions—For definitions of other terms used in this
1.3 The procedures appear in the following order:
test method, refer to Terminology D1129.
Procedure Section
3.2 Acronyms:
Internal Standardization 8
Calibration Solution Preparations 9
3.2.1 ACS, n—American Chemical Society
Preparation of Sample and Validation Solutions 10
Calibration 11 3.2.2 ICP-AES, n—inductively-coupled plasma atomic
Analysis Procedure 12
emission spectrometry
1.4 The values stated in SI units are to be regarded as the
3.2.3 PE, n—polyethylene
standard. Any other values are for information only.
3.2.4 SI, n—Le Système International d’Unités, Interna-
1.5 This standard does not purport to address all of the
tional System of Units
safety concerns, if any, associated with its use. It is the
3.3 Definitions of Terms Specific to This Standard:
responsibility of the user of this standard to establish appro-
1 2
This test method is under the jurisdiction of ASTM Committee F40 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Declarable Substances in Materials and is the direct responsibility of Subcommittee contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
F40.01 on Test Methods. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Oct. 1, 2023. Published November 2023. Originally the ASTM website.
approved in 2015. Last previous edition approved in 2015 as F3139 – 15. DOI: The last approved version of this historical standard is referenced on
10.1520/F3139-15R23. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F3139 − 15 (2023)
3.3.1 calibration blank, n—a volume of water containing where such specifications are available. Other grades equiva-
the same acid matrix as found in the calibration standards. lent or better than the ACS grade reagents may also be used.
5.2 Purity of Water—Unless otherwise indicated, references
3.3.2 calibration standards, n—a series of known standard
to water shall be understood to mean high purity water, that
solutions used to calibrate an instrument.
-1
when produced, measures at minimum 18 Megohm cm
3.3.3 check standard, n—standard used to verify proper
resistivity.
instrument calibration.
5.3 Concentrated Acids—When acids are specified by name
3.3.4 instrument linear range, n—range where instrument
or chemical formula only, it should be understood that concen-
response and accuracy remain within typically 5 to 10 % of
trated reagents of the following mass fractions are intended:
known values.
Nominal Mass
Concentrated Acid
Fraction
3.3.5 internal standard, n—pure element(s) added in known
amount(s) to a solution to be used to improve instrument
Hydrofluoric acid, HF 48 %
accuracy. Nitric acid, HNO 69 %
5.4 Single Element Reference Material Solutions—All
3.3.6 reference material solution, n—solution standard with
single element solutions used in this method must have
known certified mass fraction(s), typically commercially avail-
assigned mass fraction values in mg/kg units as opposed to
able.
mg/L units. It is possible to derive mg/kg values from mg/L
3.3.7 sample introduction system, n—plasma torch, mixing
assigned values through determination of standard solution
chamber and nebulizer used to deliver solutions to the plasma
density and subsequent calculation of mg/kg unit values.
for analysis.
5.4.1 The method of preparing calibration solutions uses
1000 mg/kg single element reference material solutions of Pb,
3.3.8 validation sample, n—a solder alloy sample that has
Cd, Hg, Sb, Bi, As, Ag, Co, Fe, Cr, Cu, In, Ni, P, Se, Zn, Al,
been certified or well characterized for mass fractions of
Ge, and Tl. A single element reference material solution of Sc
analytes present, and can be used to validate the method.
at 1000 mg/kg is required for use as an internal standard.
5.4.2 It is not important that the assigned value of the
4. Significance and Use
reference material solutions be exactly 1000 mg/kg; for
4.1 Tin-based solder alloys are commonly used to manufac-
example, the assigned value may be 1001 mg/kg or 997 mg/kg.
ture electrical and electronic goods. The elements lead,
6. Equipment
cadmium, mercury, antimony and bismuth are often declarable
substances in solder materials. This test method provides a
6.1 Inductively Coupled Plasma-Atomic Emission Spec-
means of determining the listed declarable substances, as well
trometry System (ICP-AES)—Many makes and models of
as other minor and trace constituents, in tin-based solder alloys.
ICP-AES instruments are available on the market. See Practice
E1479 for a general description of ICP-AES instrumentation.
4.2 Two methods of dissolving tin-based solder alloys are
The specific instrumentation used is not as important as its
given in this standard. The first method uses open-vessel
performance with regard to precision and sensitivity. However,
hydrofluoric and nitric acid room temperature digestions; the
a few important considerations for successful method perfor-
second method employs closed-vessel nitric and hydrofluoric
mance are given below:
acid microwave digestions, both for use only with ICP-AES
6.1.1 Sample Introduction System—Measurement of
instruments equipped with a hydrofluoric acid resistant sample
samples prepared using hydrofluoric acid (HF) requires that the
introduction system.
sample introduction system must be designed specifically to
4.3 The method of preparing calibration solutions uses 1000
come in contact with HF. Glass sample introduction systems
mg/kg single element reference material solutions, and uses
are not compatible with HF, as glass is dissolved (etched) by
matching concentrated acids for both the calibration solutions the acid. HF contact causes excessive wear of glass parts and
and the sample solutions.
contamination of samples, thus having a negative impact on the
equipment as well as results. Consult with the instrument
4.4 This test method is intended for use by laboratories
manufacturer before using solutions containing HF.
experienced with the set-up, calibration and analysis of
6.1.2 Nebulizer—Analysis of samples prepared using HF
samples using ICP-AES.
requires that the nebulizer, as part of the sample introduction
5. Reagents
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
5.1 Purity of Reagents—Reagent grade chemicals, at a
listed by the American Chemical Society, see Analar Standards for Laboratory
minimum, shall be used in all tests. Unless otherwise indicated,
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
all reagents shall conform to the specifications of the Commit-
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
tee on Analytical Reagents of the American Chemical Society, MD.
F3139 − 15 (2023)
system, must be compatible with HF. In addition, this method 8.2 Internal Standard Solution—Weigh approximately 5 g
requires analysis of solutions with relatively high solids (to the nearest 10 mg) of 1000 mg/kg Sc reference material
content on the order of 0.5 % by mass (5000 mg/kg). The solution into a 100 mL polyethylene bottle and dilute to 100 g
nebulizer should be chosen to accommodate free flow of with 5 % v/v HNO . Prepare fresh at least monthly. The same
high-solids solutions such that the nebulizer does not clog batch of internal standard solution should be used for all
during the procedure, thus allowing consistent sample intro- blanks, calibrations standards, validation samples, and un-
duction. known samples within an analysis.
6.1.3 Facility Design—A general description of design con-
siderations for a spectrochemical laboratory can be found in
9. Calibration Solution Preparations
Practice E416. Temperature control within the laboratory
9.1 Preparation of Calibration Solutions—Sample Prepara-
housing the ICP-AES system, and consistent power supply to
tion Method 1, Section 10.1:
the instrument are two of the most important considerations.
9.1.1 Calibration Blank—Prepare a calibration blank by
ICP-AES equipment tends to produce a significant amount of
making a 10 % v/v HNO /10 % v/v HF solution, and adding
heat while in operation and variation in room temperature can
2.0 g 6 20 mg (weighed to the nearest 10 mg) of 50 mg/kg Sc
have a significant impact on the stability of instrument mea-
internal standard solution per 100 g final weight of blank
surements. Sufficient equipment warm-up period and subse-
solution. The Sc internal standard will be at the same mass
quent stabilization of room temperature may be necessary to
fraction as in the calibration standards and samples (1.0 mg/kg
produce consistent measurements. Variations in power sup-
Sc).
plied to the instrument can likewise have an impact on the
9.1.2 Calibration Standards—2 mg/kg and 10 mg/kg—
stability of instrument measurements, so stabilization of the
Weigh 0.2 g 6 2 mg and 1 g 6 10 mg (to the nearest 1 mg),
power input may also be necessary to produce consistent
respectively, of each of the single element 1000 mg/kg refer-
measurements.
ence material solutions into 100 mL polyethylene bottles.
6.2 Analytical Balance—A balance with minimum readabil-
Dilute each with approximately 50 g of 10 % v/v HNO /10 %
ity of 0.0001 g for loads up to 150 g is required for successful
v/v HF, and add 2.0 6 0.2 g (weighed to the nearest 10 mg) of
performance of this method.
50 mg/kg Sc internal standard solution. Dilute to final weight
of 100 g 6 1.0 g (weighed to the nearest 100 mg) with 10 %
6.3 Microwave Digestion Equipment—Modern laboratory
v/vHNO /10 % v/v HF.
microwave equipment, including pressure vessels, provide heat
9.1.3 Check Standards—Prepare at least one instrument
and pressure to digest difficult samples without potential loss of
check standard in the same manner as the calibration standards,
analytes common to open hotplate digestions. Closed-vessel
such that the element mass fractions in the check standards are
microwave digestion can help prevent possible loss of volatile
similar to the element mass fractions in the test samples.
elements, such as mercury, during sample preparation. Use
9.1.4 Verify that the internal standard element is stable in
only microwave equipment designed specifically for laboratory
solution by visually examining for cloudiness or precipitate.
use.
9.2 Preparation of Calibration Solutions—Sample Prepara-
7. Hazards
tion Method 2, Section 10.2:
7.1 Hydrofluoric acid and hydrofluoric acid fumes can pose
9.2.1 Prepare calibration standards as directed in 9.1, using
significant risk to the operator. Proper handling should be
a 7 % v/v HNO /7 % v/v HF acid mixture, instead of the 10 %
observed at all times, including the use of laboratory fume
v/v HNO /10 % v/v HF solution.
hoods, and laboratory coats, polymer gloves and protective
eyewear. Carefully handle all solutions. Be sure to let micro-
10. Preparation of Sample and Validation Solutions
wave vessels cool for a sufficient amount of time before
10.1 Method 1–Open Vessel Digestion—For each sample
opening. Be sure to use only HF resistant sample introduction
and validation sample, weigh out 0.5 g 6 10 mg (to the nearest
components so as not to cause damage to glass parts. Always
1 mg) and place into 60 mL polyethylene bottles. This sample
maintain the capability to flush skin with water for at least 5
weight is defined as SW . To digest, add 5 mL H O, followed
1 2
min in case of skin contact with HF; keep calcium gluconate or
by the slow addition of 5 mL concentrated HF. Add 5 mL
equivalent in the laboratory to neutralize contact with HF. Seek
concentrated HNO in 0.2 mL increments to reduce volatility
appropriate emergency medical help after contact with HF or
of the reaction. Most samples will dissolve immediately or
HF fumes for unknown or extended periods of time.
within 5 to 10 min. Add approximately 20 g H O to sample and
mix. Add 1.0 g 6 10 mg (weighed to the nearest 10 mg) of 50
8. Internal Standardization
mg/kg Sc internal standard solution (prepared from 1000
8.1 The internal standard procedure requires that every test
mg/kg Sc reference material solution), and dilute sample to
solution have the same mass fraction of an internal standard
final weight of 50 6 0.5 g (weighed to the nearest 10 mg) with
element that is n
...
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