ASTM C1875-18(2024)
(Practice)Standard Practice for Determination of Major and Minor Elements in Aqueous Pore Solutions of Cementitious Pastes by Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES)
Standard Practice for Determination of Major and Minor Elements in Aqueous Pore Solutions of Cementitious Pastes by Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES)
SIGNIFICANCE AND USE
5.1 The chemical composition of the liquid in cementitious pastes is an important indicator of the solid component reactivity at early times, being influenced by the content and rate of reaction of readily soluble alkali components, lime, and other soluble phases. Monitoring the solution composition with time can provide valuable diagnostic information about cement quality and reactivity to supplement other sources of characterization data. This practice is intended to aid in the interpretation of the concentrations of readily soluble components in cement paste solutions, which may include portland cement, limestone, fly ash, ground granulated blast furnace slag, or other components. It provides guidance for measuring the time dependence of the concentrations of one or more components, on an elemental basis, including, but not limited to, aluminum, calcium, potassium, silicon, sodium, and sulfur.
SCOPE
1.1 This practice describes a procedure for collection, sample preparation and analysis of aqueous pore solutions obtained from cementitious materials at different hydration times when analyzed by ICP-OES for the six most common readily soluble elements aluminum, calcium, potassium, silicon, sodium and sulfur.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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.
1.4 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: C1875 − 18 (Reapproved 2024)
Standard Practice for
Determination of Major and Minor Elements in Aqueous
Pore Solutions of Cementitious Pastes by Inductively
Coupled Plasma Optical Emission Spectroscopy (ICP-OES)
This standard is issued under the fixed designation C1875; 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 D7111 Test Method for Determination of Trace Elements in
Middle Distillate Fuels by Inductively Coupled Plasma
1.1 This practice describes a procedure for collection,
Atomic Emission Spectrometry (ICP-AES)
sample preparation and analysis of aqueous pore solutions
E1479 Practice for Describing and Specifying Inductively
obtained from cementitious materials at different hydration
Coupled Plasma Atomic Emission Spectrometers
times when analyzed by ICP-OES for the six most common
readily soluble elements aluminum, calcium, potassium,
3. Terminology
silicon, sodium and sulfur.
3.1 Definitions:
1.2 The values stated in SI units are to be regarded as
3.1.1 Unless otherwise specified, for definitions of terms
standard. No other units of measurement are included in this
used in this practice refer to Terminology C1738/C1738M.
standard.
1.3 This standard does not purport to address all of the 4. Summary of Practice
safety concerns, if any, associated with its use. It is the
4.1 This document describes practice for determining the
responsibility of the user of this standard to establish appro-
concentration of multiple dissolved components in the pore
priate safety, health, and environmental practices and deter-
solution of cementitious pastes as a function of time using
mine the applicability of regulatory limitations prior to use.
inductively coupled plasma optical emission spectroscopy
1.4 This international standard was developed in accor-
(ICP-OES). A cementitious material is mixed with water at a
dance with internationally recognized principles on standard-
desired water to solid ratio using a Practice D1129 certified
ization established in the Decision on Principles for the
constant mixer. Aliquots of the mix are divided into centrifuge
Development of International Standards, Guides and Recom-
tubes and stored in a water bath or environmental chamber at
mendations issued by the World Trade Organization Technical
constant temperature. The samples centrifuged at different
Barriers to Trade (TBT) Committee.
times. The extracted pore solution is filtered and diluted with a
5 % nitric acid solvent. The prepared test solutions flow into
2. Referenced Documents
the plasma torch of the ICP instrument where it is vaporized
2.1 ASTM Standards:
and ionized, producing characteristic atomic wavelength emis-
C25 Test Methods for Chemical Analysis of Limestone,
sion spectra. The spectra are dispersed by a high resolution
Quicklime, and Hydrated Lime
grating and the intensities of the individual wavelengths are
C114 Test Methods for Chemical Analysis of Hydraulic
measured. Elemental concentrations are determined by relating
Cement
the emission intensities at specific wavelengths for an unknown
C1738/C1738M Practice for High-Shear Mixing of Hydrau-
sample to analytical curves made from reference standards of
lic Cement Pastes
known composition. The concentration of the elements in the
D1129 Terminology Relating to Water
solutions can then be calculated. Internal standards compensate
D1193 Specification for Reagent Water
for variations in test sample flow rates in the instrument.
D5673 Test Method for Elements in Water by Inductively
5. Significance and Use
Coupled Plasma—Mass Spectrometry
5.1 The chemical composition of the liquid in cementitious
pastes is an important indicator of the solid component
This practice is under the jurisdiction of ASTM Committee C01 on Cement and
reactivity at early times, being influenced by the content and
is the direct responsibility of Subcommittee C01.23 on Compositional Analysis.
rate of reaction of readily soluble alkali components, lime, and
Current edition approved April 1, 2024. Published April 2024. Originally
other soluble phases. Monitoring the solution composition with
approved in 2018. Last previous edition approved in 2018 as C1875 – 18. DOI:
10.1520/C1875-18R24. time can provide valuable diagnostic information about cement
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1875 − 18 (2024)
quality and reactivity to supplement other sources of charac- 7.6 Calibration Blank Solution—5 % (v/v) HNO .
terization data. This practice is intended to aid in the interpre-
7.7 Nitric Acid—5 % (v ⁄v).
tation of the concentrations of readily soluble components in
7.8 Check Standards—Quality control certified NIST trace-
cement paste solutions, which may include portland cement,
able samples that are stable and representative of the samples
limestone, fly ash, ground granulated blast furnace slag, or
of interest. These check standard samples represent ground
other components. It provides guidance for measuring the time
truth samples and are used to check that the measurement
dependence of the concentrations of one or more components,
process is in control.
on an elemental basis, including, but not limited to, aluminum,
calcium, potassium, silicon, sodium, and sulfur.
7.9 Internal Standards—Internal standards are used to cor-
rect for instrument drift and physical interferences. Refer to
6. Apparatus
instrument operating manual for suggested internal standards.
6.1 Spectrometer—Spectrometer-An inductively coupled Add internal standards to blanks, samples, and standards in a
plasma emission spectrometer of the simultaneous or sequen-
like manner.
tial type including RF generator, torch, nebulizer, connector
7.10 Membrane Filter—Nylon 25 mm diameter, 0.2 μm.
tube, spray chamber, recommended peristaltic pump and host
7.11 Syringe and Needle—Capacity of at least 2 mL.
computer. Sample uptake is done by self-aspiration, or with a
peristaltic pump.
7.12 Centrifuge Tubes—Clean plastic centrifuge tubes the
appropriate size for centrifuge.
6.2 Mass Flow Controllers—A mass-flow controller to regu-
late the nebulizer gas may be used as recommended by the
7.13 Glassware—Volumetric flasks complying with the re-
instrument manufacturer. quirements of ISO 1042, made of borosilicate glass complying
with the requirements of ISO 3585. Glassware should be
6.3 Balance—Top loading or analytical, with automatic tare,
cleaned before each use by soaking in nitric acid and then
with capacity of at least 500 g and a sensitivity of at least 0.1 g
rinsing thoroughly with deionized water.
to weigh paste mix components.
7.14 Pipette—Calibrated volumetric pipettes and pipette
6.4 Centrifuge—Use a centrifuge capable of accommodat-
tips, for dispensing.
ing two or more 50 mL centrifuge tubes at rotational speeds up
-1
to 5000 min .
8. Hazards
6.5 Timer—Calibrated timer for use of tracking blending
8.1 The toxicity or carcinogenicity of each reagent used in
and reaction times.
this practice has not been precisely defined; however, each
chemical should be treated as a potential health hazard.
7. Reagents and Materials
Adequate precautions should be taken to minimize exposure of
7.1 Ordinary laboratory apparatus are not listed, but are
personnel to chemicals used in this practice.
assumed to be present.
8.2 Gases under high pressure are used in this practice. Use
7.2 Purity of Reagents—At a minimum, reagent grade or
only apparatus rated for handling the high gas pressures that
better chemicals shall be used in all tests.
occur in this practice.
7.3 Purity of Water—References to water shall be under-
stood to mean deionized water. Tap water may be used only to
9. Sample Handling
prepare cement paste mixes if desired. If tap water is used for
9.1 Powder Homogenization—A uniform distribution of
mixing the composition of the water itself must be separately
powder components is essential to ensure representative sam-
measured as a test sample as described in Section 11.
pling during the mixing process, especially for blended powder
7.4 Argon—High purity grade (99.99 %).
components such as portland cement and fly ash. Powders
should therefore be homogenized for 30 min with a planetary
7.5 Calibration Standards—Single-element or multi-
mixer or similar device.
element calibration reference solutions that combine appropri-
ate volumes of the stock solutions or weighed reagent-grade
10. Sample Preparation and Collection
chemicals in acid-rinsed volumetric flasks. Dilute to the
volume of the flask using a 5 % (v/v) nitric acid solution. Prior 10.1 High Shear Mixing:
to preparing the multi-element solutions, analyze each stock 10.1.1 Blend the solid and liquid components to make a
solution separately to check for strong spectral interference and paste according the standard practice described in Practice
the presence of impurities. Take care when preparing the D1129.
multi-element solutions to verify that the components are 10.1.2 Set a timer to mark the end of mixing. The time on
compatible and stable (that is, that they do not interact to cause this timer will serve as the total reaction time for the remainder
precipitation) and that none of the elements present will of the procedure.
contribute to mutual spectral interference. Calibration refer- 10.1.3 Stir the paste with the spatula for no more than 15 s
ence solutions must be verified initially using a quality control ensure homogeneity.
sample and monitored periodically for stability. Mixed calibra- 10.1.4 Transfer (25 6 1) g of the paste into each of twelve
tion standards will vary, depending on the number of elements centrifuge tubes with secured lids in the minimum amount of
being determined. time possible, preferably les
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