ASTM E2330-19

Standard Test Method for Determination of Concentrations of Elements in Glass Samples Using Inductively Coupled Plasma Mass Spectrometry (ICP-MS) for Forensic Comparisons

SIGNIFICANCE AND USE
4.1 This technique is destructive, in that the glass fragments may need to be crushed, and digested in acid.  
4.2 Although the concentration ranges of the calibration curves shown in Appendix X1 are applicable to soda lime and borosilicate glass, this method is useful for the accurate measurement of element concentrations from a wide variety of glass samples.  
4.3 The determination of the element concentrations in glass yields data that can be used to compare fragments.  
4.4 It should be recognized that the method measures the bulk concentration of the target elements. Any extraneous material present on the glass that is not removed before digestion can result in inaccurate concentrations of the measured elements.  
4.5 The precision and accuracy of the method should be established in each laboratory that employs the method.
SCOPE
1.1 One objective of a forensic glass examination is to compare glass samples to determine if they can be discriminated using their physical, optical or chemical properties (for example, color, refractive index (RI), density, elemental composition). If the samples are distinguishable in any of these observed and measured properties, it may be concluded that they did not originate from the same source of broken glass. If the samples are indistinguishable in all of these observed and measured properties, the possibility that they originated from the same source of glass cannot be eliminated. The use of an elemental analysis method such as inductively coupled plasma mass spectrometry yields high discrimination among sources of glass. (1-16)2  
1.2 This test method covers a procedure for quantitative determination of the concentrations of magnesium (Mg), aluminum (Al), iron (Fe), titanium (Ti), manganese (Mn), rubidium (Rb), strontium (Sr), zirconium (Zr), barium (Ba), lanthanum (La), cerium (Ce), neodymium (Nd), samarium (Sm), and lead (Pb) in glass samples.  
1.3 This procedure is applicable to irregularly shaped samples as small as 200 micrograms, for the comparison of fragments of a known source to the recovered fragments from a questioned source. These elements are present in soda lime and borosilicate glass in μg/L to % levels.  
1.4 This procedure is applicable to other elements, other types of glass, and other concentration ranges with appropriate modifications of the digestion procedure (if needed for full recovery of the additional elements), calibration standards and the mass spectrometer conditions. Calcium and potassium, for example, could be added to the list of analytes in a modified analysis scheme. Alternative methods for the determination of concentrations of elements in glass are listed in the references.  
1.5 For any given glass, approximately 40 elements are likely to be present at detectable concentrations using this procedure with minor modifications. The element set stated here is an example of some of these elements that can be detected in glass and used for forensic comparisons.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.7 This standard cannot replace knowledge, skills, or abilities acquired through education, training, and experience and is to be used in conjunction with professional judgment by individuals with such discipline-specific knowledge, skills, and abilities.  
1.8 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.  
1.9 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 Organiz...

General Information

• Status: Published
• Publication Date: 30-Nov-2019
• ICS: 07.140 - Forensic science
• ICS: 71.040.40 - Chemical analysis
• ICS: 81.040.10 - Raw materials and raw glass
• Technical Committee: E30 - Forensic Sciences
• Drafting Committee: E30.01 - Criminalistics

Relations

• Refers: ASTM E177-14 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2014
• Refers: ASTM E177-13 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2013
• Refers: ASTM E177-10 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Oct-2010
• Refers: ASTM E177-08 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Oct-2008
• Refers: ASTM E177-06b - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 15-Nov-2006
• Refers: ASTM E177-06a - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2006
• Refers: ASTM E177-06 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2004
• Refers: ASTM E177-04 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2004
• Refers: ASTM E177-04e1 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2004
• Refers: ASTM E177-90a(2002) - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 10-Jan-2002

Overview

ASTM E2330-19 is the internationally recognized standard test method for the determination of elemental concentrations in glass samples using Inductively Coupled Plasma Mass Spectrometry (ICP-MS). This method is primarily applied in forensic science for glass comparisons, enabling the quantitative analysis of elements to distinguish between fragments. By providing highly discriminating chemical signatures, ICP-MS allows forensic laboratories to reliably associate or differentiate glass evidence from various sources, supporting criminal investigations, product tampering cases, and quality control scenarios.

Key Topics

• Scope and Application: The standard outlines procedures for analyzing the elemental composition of glass fragments, particularly those as small as 200 micrograms and of irregular shape.
• Elemental Analysis: ASTM E2330-19 focuses on quantifying elements such as magnesium, aluminum, iron, titanium, manganese, rubidium, strontium, zirconium, barium, lanthanum, cerium, neodymium, samarium, and lead. With appropriate modifications, it also applies to other detectable elements.
• Destructive Technique: The method requires crushing and acid digestion of glass samples, making it inherently destructive. It is essential to remove extraneous materials to ensure that measured concentrations represent the actual bulk composition of the glass.
• Laboratory Quality Control: Each laboratory must establish its own precision and accuracy for the method, using standard reference glasses and calibration protocols to ensure valid results.
• Sample Preparation: Glass samples are cleaned, crushed, weighed with high precision, digested in acid, and prepared for ICP-MS analysis following rigorous contamination control procedures.
• Data Interpretation: The method specifies statistical criteria for comparing elemental concentrations between known and questioned glass sources, helping determine whether two samples are distinguishable or could originate from the same source.
• Safety Considerations: Handling of hydrofluoric acid and operation of ICP-MS equipment require strict adherence to laboratory safety protocols.

Applications

• Forensic Investigations: ICP-MS glass comparison is widely used by forensic laboratories to link crime scene glass fragments to known sources, such as broken windows or containers, by matching their trace elemental profiles.
• Quality Assurance in Manufacturing: Glass manufacturers may use the method to ensure product consistency, monitor batch variations, or investigate product integrity in cases of contamination or tampering.
• Failure and Contamination Analysis: The procedure provides a means to analyze glass involved in product failures or suspected tampering incidents, allowing for precise identification of material origin and possible contaminants.
• Research and Development: The technique supports material scientists in characterizing the chemical properties of glass for new formulations, recycling processes, or modification of composition for specialized applications.

Related Standards

ASTM E2330-19 references and complements other important standards and practices relevant to forensic and analytical laboratories:

• ASTM E177: Practice for Use of the Terms Precision and Bias in ASTM Test Methods – fundamental for interpreting repeatability and reproducibility.
• NIST 1831 and NIST 612: Standard reference glasses commonly used for calibration and quality control in elemental glass analysis.
• Methods such as X-ray Fluorescence (XRF) or Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) are often considered alternate or complementary techniques for elemental analysis of glass.

Keywords: forensic science, elemental analysis, glass comparison, ICP-MS, trace elemental analysis, ASTM E2330-19, glass evidence, standard test method, forensic glass analysis, laboratory quality control.

This ASTM standard is critical for anyone involved in forensic, analytical, or manufacturing environments where accurate elemental determination in glass is required. Always consult the official document for complete procedural details and safety requirements.

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: E2330 − 19 An American National Standard
Standard Test Method for
Determination of Concentrations of Elements in Glass
Samples Using Inductively Coupled Plasma Mass
Spectrometry (ICP-MS) for Forensic Comparisons
This standard is issued under the fixed designation E2330; 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 1.5 For any given glass, approximately 40 elements are
likely to be present at detectable concentrations using this
1.1 One objective of a forensic glass examination is to
procedure with minor modifications. The element set stated
compare glass samples to determine if they can be discrimi-
here is an example of some of these elements that can be
nated using their physical, optical or chemical properties (for
detected in glass and used for forensic comparisons.
example, color, refractive index (RI), density, elemental com-
position). If the samples are distinguishable in any of these 1.6 The values stated in SI units are to be regarded as
observed and measured properties, it may be concluded that standard. No other units of measurement are included in this
they did not originate from the same source of broken glass. If standard.
the samples are indistinguishable in all of these observed and
1.7 This standard cannot replace knowledge, skills, or
measured properties, the possibility that they originated from
abilities acquired through education, training, and experience
the same source of glass cannot be eliminated. The use of an
and is to be used in conjunction with professional judgment by
elemental analysis method such as inductively coupled plasma
individuals with such discipline-specific knowledge, skills, and
mass spectrometry yields high discrimination among sources
abilities.
of glass. (1-16)
1.8 This standard does not purport to address all of the
1.2 This test method covers a procedure for quantitative
safety concerns, if any, associated with its use. It is the
determination of the concentrations of magnesium (Mg), alu-
responsibility of the user of this standard to establish appro-
minum (Al), iron (Fe), titanium (Ti), manganese (Mn), ru-
priate safety, health, and environmental practices and deter-
bidium (Rb), strontium (Sr), zirconium (Zr), barium (Ba),
mine the applicability of regulatory limitations prior to use.
lanthanum (La), cerium (Ce), neodymium (Nd), samarium
1.9 This international standard was developed in accor-
(Sm), and lead (Pb) in glass samples.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
1.3 This procedure is applicable to irregularly shaped
Development of International Standards, Guides and Recom-
samples as small as 200 micrograms, for the comparison of
mendations issued by the World Trade Organization Technical
fragments of a known source to the recovered fragments from
Barriers to Trade (TBT) Committee.
a questioned source. These elements are present in soda lime
and borosilicate glass in µg/L to % levels.
2. Referenced Documents
1.4 This procedure is applicable to other elements, other
2.1 ASTM Standards:
types of glass, and other concentration ranges with appropriate
E177 Practice for Use of the Terms Precision and Bias in
modifications of the digestion procedure (if needed for full
ASTM Test Methods
recovery of the additional elements), calibration standards and
the mass spectrometer conditions. Calcium and potassium, for
3. Summary of Test Method
example, could be added to the list of analytes in a modified
analysis scheme. Alternative methods for the determination of 3.1 The glass fragments are digested using a mixture of
concentrations of elements in glass are listed in the references. hydrofluoric, nitric and hydrochloric acids. Following acid
digestion,thesamplesaretakentodrynesstoeliminatemostof
the silicate matrix and the excess acids. Then an internal
ThistestmethodisunderthejurisdictionofASTMCommitteeE30onForensic
Sciences and is the direct responsibility of Subcommittee E30.01 on Criminalistics.
Current edition approved Dec. 1, 2019. Published January 2020. Originally
approved in 2004. Last previous edition approved in 2012 as E2330 – 12. DOI: For referenced ASTM standards, visit the ASTM website, www.astm.org, or
10.1520/E2330-19. contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
The boldface numbers in parentheses refer to a list of references at the end of Standards volume information, refer to the standard’s Document Summary page on
this standard. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2330 − 19
standard [rhodium (Rh)] is added as the samples are reconsti- 5.6 Laboratory Oven or Dry Bath Block.
tuted in nitric acid. Dilutions may be utilized to quantitate
5.7 Micropipettes.
those elements that are present in higher concentrations.
5.8 Fume Hood.
3.2 An inductively coupled plasma mass spectrometer is
used to measure the concentrations of the elemental suite listed 6. Hazards
in1.2.Theinstrumentisadjustedformaximumsensitivity,best
6.1 Hydrofluoric acid (HF) is corrosive to all body tissues
precision and to minimize oxides and doubly charged ion
and bone. Skin, eye or respiratory contact with HF presents a
interferences. The instrument is then calibrated per manufac-
significant health hazard that requires immediate first aid and
turer recommendations, using multi-elemental calibration stan-
possibly specialized medical care. Extreme care must be
dards with the same internal standards as that added to the
exercised in the presence of this acid. Calcium gluconate gel
samples.
should be kept in the immediate area of HF use in the event of
3.3 Reagent blanks are measured along with the samples a potential skin exposure. See the chemical manufacturer’s
because detection limits are usually limited by the background Safety Data Sheet for more information.
signals generated by the reagent blanks.The limits of detection
6.2 The argon plasma should not be observed directly
of the method are expected to be between 0.5 µg/Land 25 µg/L
without protective eyewear. Potentially hazardous UV light
for most elements.
may be emitted.
6.3 ICP-MS instruments generate high amounts of radio-
4. Significance and Use
frequency energy in their RF power supply and torch boxes
4.1 This technique is destructive, in that the glass fragments
that is potentially hazardous if allowed to escape. Safety
may need to be crushed, and digested in acid.
devices and safety interlocks should not be bypassed or
4.2 Although the concentration ranges of the calibration
disconnected.
curves shown in Appendix X1 are applicable to soda lime and
7. Sample Preparation
borosilicate glass, this method is useful for the accurate
measurement of element concentrations from a wide variety of
7.1 The sample set for analysis shall include all known
glass samples.
samples, questioned samples and at least two standard refer-
ence glasses. Prior to crushing the glass sample for the
4.3 Thedeterminationoftheelementconcentrationsinglass
digestion, soak samples in concentrated HNO , rinse 3 times
yields data that can be used to compare fragments.
with high purity water, and allow the samples to dry.
4.4 It should be recognized that the method measures the
7.2 Crush the samples between clean polymeric materials,
bulk concentration of the target elements. Any extraneous
such as polystyrene weighing boats or glassine sheets, taking
material present on the glass that is not removed before
care not to puncture the materials.
digestion can result in inaccurate concentrations of the mea-
sured elements.
7.3 Accurately weigh approximately 2 to 3 mg of each
sample using a microbalance (with a precision of 61µgor
4.5 The precision and accuracy of the method should be
better) and quantitatively transfer into a labeled non-glass tube
established in each laboratory that employs the method.
with a cap. At least three weighings per glass source shall be
made for a minimum of three analytical samples per glass
5. Apparatus
source for digestion. Prepare empty labeled non-glass tubes for
5.1 ICP-MS—An Inductively Coupled Plasma Mass Spec-
reagent blanks.
trometer (ICP-MS) instrument is employed. Since there are
7.4 All volumes are delivered using micropipets. Add con-
several manufacturers for ICP-MS instruments, the instrument
centrated hydrofluoric acid, concentrated hydrochloric acid,
maker, model, configuration, and major operational parameters
and concentrated nitric acid to each tube to makea2to1to1
should be noted within the analysis results.
mixture of the acids in the tubes.
5.2 Standard Reference Glasses—Aminimum of two differ-
7.5 Cap and vortex mix the tubes. The tubes may be placed
entstandardreferenceglassesofknownelementalcomposition
inanultrasonicbathtoassistinthedigestionforapproximately
should be used. Examples suitable for this analysis include
one hour. Uncap the tubes and place in a dry bath block or an
NIST 1831 and NIST 612 Reference Glasses.
oven, at 80°C or greater (but below the softening temperature
5.3 Non-Glass Laboratory Ware.
of the digestion tubes), until dry.
5.4 Micro-Balance—A microbalance with a precision of
7.6 Reconstitute the samples by adding 500 µL of 50 %
61 µg or better is necessary for the accurate weighing of the
HNO (8.0 mol/L). Recap the tubes and vortex mix.
glass samples.
7.7 Thetubesmaybeplacedinanultrasonicbathforatleast
5.5 High Purity Reagents—ICP-MS grade acids and re-
one hour or left to stand overnight.
agents shall be used for digestion and dilution.
7.8 Add 50 µL of a 10 mg/L Rh internal standard solution
and 4450 µL of ultrapure water to each tube and vortex mix
contents. Each tube will containa5mLsolution with 100 µg/L
Available from National Institute of Standards and Technology (NIST), 100
Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http://www.nist.gov. Rh internal standard in5%HNO .
E2330 − 19
8. Instrument Set-Up and Calibration measuring the concentrations of the elements of interest in
three procedure blanks on two non-consecutive days. The
8.1 Tune the instrument prior to the analysis using the
MDL is the standard deviation of the concentration of each
manufacturer’s recommendations covering the mass range of
element in the three procedure blanks times three. The LOQ is
the identified elements. The instrument shall be adjusted for
the standard deviation of the concentration of each element in
maximum sensitivity, best precision, and to minimize oxides
the three procedure blanks times ten. To calculate these limits
and doubly charged ion interferences.
of detection and quantitation, the average from the results for
8.2 Prepare calibration standards from pure element stan-
the two days is taken.
dards traceable to accepted metrological sources (NIST, etc.)
NOTE 1—Table X2.1 illustrates the values for MDL, LOQ, and range of
covering the expected range of concentrations of the glass
concentrations found in a set of 50 soda-lime glass samples all expressed
samples.
as ug/L of the elemental concentration in the final solution.
8.3 Prepare two calibration curves as well as two check
10.3 Accuracy of Standard Reference Material (SRM)—
standards. The first calibration curve shall consist of Mg,
SRMs with known concentrations of elements in glass are
27 47 57 55 88 90 138 206, 207, 208
Al, Ti, Fe, Mn, Sr, Zr, Ba, and Pb with
measured to assess the accuracy of the method. If one or more
a concentration range of 0.0, 1.0, 10.0, 50.0, 75.0, and 150.0
element concentrations fall outside of the acceptable ranges of
85 139
µg/L.The second calibration curve shall consist of Rb, La,
concentrations (as determined by each laboratory), the sample
140 146 148
Ce, Nd, Sm with a concentration range of 0.0, 0.1, 0.5,
analysiscanyieldinaccurateconcentrations.Correctiveactions
1.0,5.0,and50µg/L.Aninternalstandardof100µg/LRhshall
should be taken to address the source of the inaccuracy prior to
be used in each standard sample.
additional analysis.
8.4 The check standard (continuing calibration verification
11. Calculation and Interpretation of Results
or CCV) for the element standards calibration shall be 50.0
µg/L for the first group and 5.0 µg/L for the second group. 11.1 The procedure below shall be followed to conduct a
forensicglasscomparisonwhenusingtherecommendedmatch
8.5 Analyze the standard samples using the ICP-MS and
criteria (17-19).
calibration curves established for each group of elements.
11.1.1 For the Known source fragments, using a minimum
Analyzethecontinuingcalibrationverification(CCV)samples.
of 3 measurements, calculate the mean for each element.
The system should be recalibrated any time that the CCV falls
11.1.2 Calculate the standard deviation for each element.
outside the acceptable parameters established by the laboratory
This is the Measured SD.
or analyst for this procedure.
11.1.3 Calculate a value equal to3%ofthe mean for each
element. This
...

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: E2330 − 12 E2330 − 19
Standard Test Method for
Determination of Concentrations of Elements in Glass
Samples Using Inductively Coupled Plasma Mass
Spectrometry (ICP-MS) for Forensic Comparisons
This standard is issued under the fixed designation E2330; 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 One objective of a forensic glass examination is to compare glass samples to determine if they can be discriminated using
their physical, optical or chemical properties (for example, color, refractive index (RI), density, elemental composition). If the
samples are distinguishable in any of these observed and measured properties, it may be concluded that they did not originate from
the same source of broken glass. If the samples are indistinguishable in all of these observed and measured properties, the
possibility that they originated from the same source of glass cannot be eliminated. The use of an elemental analysis method such
as inductively coupled plasma mass spectrometry yields high discrimination among sources of glass. (1-16)
1.2 This test method covers a procedure for quantitative determination of the concentrations of magnesium (Mg), aluminum
(Al), iron (Fe), titanium (Ti), manganese (Mn), rubidium (Rb), strontium (Sr), zirconium (Zr), barium (Ba), lanthanum (La), cerium
(Ce), neodymium (Nd), samarium (Sm), and lead (Pb) in glass samples.
1.3 This procedure is applicable to irregularly shaped samples as small as 200 micrograms, for the comparison of fragments of
a known source to the recovered fragments from a questioned source. These elements are present in soda lime and borosilicate
glass in ppbμg/L to % levelslevels.
1.4 This procedure is applicable to other elements, other types of glass, and other concentration ranges with appropriate
modifications of the digestion procedure (if needed for full recovery of the additional elements), calibration standards and the mass
spectrometer conditions. Calcium and potassium, for example, could be added to the list of analytes in a modified analysis scheme.
Alternative methods for the determination of concentrations of elements in glass are listed in the references.
1.5 For any given glass, approximately 40 elements are likely to be present at detectable concentrations using this procedure
with minor modifications. The element set stated here is an example of some of these elements that can be detected in glass and
used for forensic comparisons.
1.6 This guide cannot replace knowledge, skill, or ability acquired through appropriate education, training, and experience and
should be used in conjunction with sound professional judgment.
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.7 This standard cannot replace knowledge, skills, or abilities acquired through education, training, and experience and is to
be used in conjunction with professional judgment by individuals with such discipline-specific knowledge, skills, and abilities.
1.8 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.9 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.
This test method is under the jurisdiction of ASTM Committee E30 on Forensic Sciences and is the direct responsibility of Subcommittee E30.01 on Criminalistics.
Current edition approved June 15, 2012Dec. 1, 2019. Published July 2012January 2020. Originally approved in 2004. Last previous edition approved in 20042012 as E2330
– 04.12. DOI: 10.1520/E2330-12.10.1520/E2330-19.
The boldface numbers in parentheses refer to a list of references at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2330 − 19
2. Referenced Documents
2.1 ASTM Standards:
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
3. Summary of Test Method
3.1 The glass fragments are digested using a mixture of hydrofluoric, nitric and hydrochloric acids. Following acid digestion,
the samples are taken to dryness to eliminate most of the silicate matrix and the excess acids. Then an internal standard [rhodium
(Rh)] is added as the samples are reconstituted in nitric acid. Dilutions may be utilized to quantitate those elements that are present
in higher concentrations.
3.2 An inductively coupled plasma mass spectrometer is used to measure the concentrations of the identified elements
(elemental suite listed in 1.11.2). The instrument should be is adjusted for maximum sensitivity, best precision and to minimize
oxides and doubly charged ion interferences. The instrument is then calibrated per manufacturer recommendations, using
multi-elemental calibration standards with the same internal standards as that added to the samples.
3.3 Reagent blanks are measured along with the samples because detection limits are usually limited by the background signals
generated by the reagent blanks. The limits of detection of the method are expected to be between 0.5 ppbμg/L and 25 ppb in
solution μg/L for most elements.
4. Significance and Use
4.1 This technique is destructive, in that the glass fragments may need to be crushed, and must be digested in acid.
4.2 Although the concentration ranges of the calibration curves shown in Appendix X1 are applicable to soda lime and
borosilicate glass, this method is useful for the accurate measurement of element concentrations from a wide variety of glass
samples.
4.3 The determination of the element concentrations in glass yields data that can be used to compare fragments.
4.4 It should be recognized that the method measures the bulk concentration of the target elements. Any extraneous material
present on the glass that is not removed before digestion maycan result in inaccurate concentrations of the measured elements.
4.5 The precision and accuracy of the method should be established in each laboratory that employs the method.
5. Apparatus
5.1 ICP-MS—An ICP-MS Inductively Coupled Plasma Mass Spectrometer (ICP-MS) instrument is employed. Since there are
several manufacturers for ICP-MS instruments, the instrument maker, model, configuration, and major operational parameters
should be noted within the analysis results.
5.2 Standard Reference Glasses—A minimum of two different standard reference glasses of known elemental composition
should be used. Examples suitable for this analysis include NIST 1831 and NIST 612 Reference Glasses.
5.3 Non-Glass Laboratory Ware—Ware. for digestion.
5.4 Micro-Balance, Micro-Balance—A microbalance with a precision of 61 μg or better.61 μg or better is necessary for the
accurate weighing of the glass samples.
5.5 High Purity Reagents, Reagents—ICP-MS grade acids and reagents shall be used for digestion and dilution.
5.6 Laboratory Oven or Dry Bath Block,Block. for digestion.
5.7 Micropipettes,Micropipettes. used for the addition of reagents.
5.8 Fume Hood,Hood. for work with acids and removal of HF fumes.
6. Hazards
6.1 Hydrofluoric acid (HF) is corrosive to all body tissues and bone. Skin, eye or respiratory contact with HF presents a
significant health hazard that requires immediate first aid and possibly specialized medical care. Extreme care must be exercised
in the presence of this acid. Calcium gluconate gel should be kept in the immediate area of HF use in the event of a potential skin
exposure. See the chemical manufacturer’s Safety Data Sheet for more information.
6.2 The argon plasma should not be observed directly without protective eyewear. Potentially hazardous UV light may be
emitted.
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’sstandard’s Document Summary page on the ASTM website.
Available from National Institute of Standards and Technology (NIST), 100 Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http://www.nist.gov.
E2330 − 19
6.3 ICP-MS instruments generate high amounts of radio-frequency energy in their RF power supply and torch boxes that is
potentially hazardous if allowed to escape. Safety devices and safety interlocks should not be bypassed or disconnected.
7. Sample Preparation
7.1 The sample set for analysis willshall include all known samples, questioned samples and at least two standard reference
glasses. Prior to crushing the glass sample for the digestion, soak samples in concentrated HNO , rinse 3 times with high purity
water, and allow the samples to dry.
7.2 The samples are crushed Crush the samples between clean polymeric materials, such as polystyrene weighing boats or
glassine sheets, taking care not to puncture the materials.
7.3 Approximately Accurately weigh approximately 2 to 3 mg of each sample should be accurately weighed using a
microbalance (with a precision of 61 μg or better) and quantitatively transferredtransfer into a labeled non-glass tube with a cap.
At least three weighings per glass source shouldshall be made for a minimum of three analytical samples per glass source for
digestion. Empty Prepare empty labeled non-glass tubes should be prepared for reagent blanks.
7.4 All volumes are delivered using micropipettes.micropipets. Add concentrated hydrofluoric acid, concentrated hydrochloric
acid, and concentrated nitric acid to each tube to make a 2:1:1 2 to 1 to 1 mixture of the acids in the tubes.
7.5 The tubes are capped, vortex mixed, and Cap and vortex mix the tubes. The tubes may be placed in an ultrasonic bath to
assist in the digestion for approximately one hour. The tubes are then uncapped and placedUncap the tubes and place in a dry bath
block or an oven, at 80°C or greater (but below the softening temperature of the digestion tubes), and taken to dryness.until dry.
-1
7.6 The samples are reconstituted Reconstitute the samples by adding 500 μL of 50 % HNO (8.0 molLmol/L). ). The tubes
are re-capped. Recap the tubes and vortex mix.
7.7 The tubes are vortex mixed and ultrasonicated may be placed in an ultrasonic bath for at least one hour or left to stand
overnight.
7.8 Add 50 μlμL of a 10 ppmmg/L Rh internal standard solution and 4450 μlμL of ultrapure water to each tube and vortex mix
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contents. Each tube will contain a 5 mlmL solution with 100 ppbμg/L Rh internal standard in 5 % HNO (8.0 molL. ).
8. Instrument Set-Up and Calibration
8.1 The instrument should be tuned Tune the instrument prior to the analysis using the manufacturer’smanufacturer’s
recommendations covering the mass range of the identified elements. The instrument shouldshall be adjusted for maximum
sensitivity, best precision, and to minimize oxides and doubly charged ion interferences.
8.2 Calibration standards are prepared Prepare calibration standards from pure element standards traceable to accepted
metrological sources (NIST, etc.) covering the expected range of concentrations of the glass samples.
8.3 Two Prepare two calibration curves as well as two check standards are used. standards. The first calibration curve consists
24 27 47 57 55 88 90 138 206, 207, 208
shall consist of Mg, Al, Ti, Fe, Mn, Sr, Zr, Ba, and Pb with a concentration range of 0.0, 1.0, 10.0, 50.0,
85 139 140 146 148 206, 207,
75.0, and 150.0 ppb.μg/L. The second calibration curve consists shall consist of Rb, La, Ce, Nd, Sm, and Sm
208Pb with a concentration range of 0.0, 0.1, 0.5, 1.0, 5.0, and 50 ppb.μg/L. An internal standard of 100 ppbμg/L Rh is shall be
used in each standard sample.
8.4 The check standard (continuing calibration verification or CCV) for the element standards calibration is shall be 50.0
ppbμg/L for the first group and 5.0 ppbμg/L for the second group.
8.5 The Analyze the standard samples are analyzed using the ICP-MS and calibration curves established for each group of
elements. The Analyze the continuing calibration verification (CCV) samples are analyzed. samples. The system is should be
recalibrated any time that the CCV falls outside the acceptable parameters established by the laboratory or analyst for this
procedure.
9. Sample Analysis
9.1 A Analyze a reagent blank will be analyzed with every sample set.
9.2 Blanks will be analyzed Analyze blanks between replicate groups.
9.3 Two Analyze two Standard Reference Glasses (NIST 1831, NIST 612, etc.) will be analyzed as a part of the sample set.
9.4 All Analyze all blanks and digested glass samples are analyzed by the ICP-MS using the instrument parameters established
during tuning. The data are compared to the calibration curves, concentration values are determined, and corrected for the weight
of the glass sample used. Final concentration values should be reported as milligram of element per kilogram of glass (mg/kg).
10. Quality Control
10.1 Continuing Calibration Verification (CCV)—After measuring the standards and periodically throughout the analysis, a
CCV sample is measured to determine if the calibration is valid. The CCV sample is another solution containing all of the elements
E2330 − 19
of interest at a known concentration (50.0 ppbμg/L and 5.0 ppb).μg/L). The system is recalibrated any time one or more element
concentrations measured for the CCV sample fall outside the acceptable concentration ranges for the actual concentration of the
elements in the CCV. The acceptable ranges of the concentrations of the elements in the CCV and the frequency of CCV sample
measurements should be determined by each laboratory using this method.
10.2 Method Detection Limit (MDL) and Limit of Quantitation (LOQ)—The MDL for each element is determined by measuring
the concentrations of the elements of interest in three procedure blanks on two non-consecutive days. The MDL is the standard
deviation of the concentration of each element in the three procedure blanks times three. The LOQ is the standard deviation of the
concentration of each element in the three procedure blanks times ten. To calculate these limits of detection and quantitation, the
average from the results for the two days is taken.
NOTE 1—TableTable X2.1 X2.1 illustrates the values for MDL, LOQ, and range of concentrations found in a set of 50 soda-lime glass samples all
expressed as ppbug/L of the elemental concentration in the final solution.
10.3 Accuracy of Standard Reference Material (SRM)—SRMs with known concentrations of elements in glass are measured
with the Known source fragments to assess the accuracy of the method. If one or more element concentrations fall outside of the
acceptable ranges of concentrations (as determined by each laboratory), the sample analysis maycan yield inaccurate
concentrations. Corrective actions should be taken to address the source of the inaccuracy prior to additional analysis.
11. Calculation and Interpretation of Results
11.1 The procedure below sh
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