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

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)1
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 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-
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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
Coupled Plasma—Mass Spectrometry 5. Significance and Use
D7111 Test Method for Determination of Trace Elements in 5.1 The chemical composition of the liquid in cementitious
pastes is an important indicator of the solid component
1
reactivity at early times, being influenced by the content and
This test method is under the jurisdiction of ASTM Committee C01 on Cement
rate of reaction of readily soluble alkali components, lime, and
and is the direct responsibility of Subcommittee C01.23 on Compositional Analysis.
Current edition approved July 1, 2018. Published August 2018. DOI: 10.1520/ other soluble phases. Monitoring the solution composition with
C1875-18 time can provide valuable diagnostic information about cement

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 C1875 − 18
quality and reactivity to supplement other sources of charac-
terization data. This practice is intended to aid in the interpre-
tation 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.
6. Apparatus
6.1 Spectrometer—Spectrometer-An inductively coupled
plasma emission spectrometer of the simultaneous or sequen-
tial type including RF generator, torch, nebulizer, connector
tube, spray chamber, recommended peristaltic pump and host
computer. Sample uptake is done by self-aspiration, or with a
peristaltic pump.
6.2 Mass Flow Controllers—A mass-flow controller to regu-
late the nebulizer gas may be used as recommended by the
instrument manufacturer.
6.3 Balance—Top loading or analytical, with automatic tare,
with capacity of at least 500 g and a sensitivity of at least 0.1
g to weigh paste mix components.
6.4 Centrifuge—Use a centrifuge capable of accommodat-
ing two or more 50 mL centrifuge tubes at rotational speeds up
to 5000 min-1.
6.5 Timer—Calibrated timer for use of tracking blending
and reaction times.
7. Reagents and Materials
7.1 Ordinary laboratory apparatus are not listed, but are
assumed to be present.
7.2 Purity of Reagents—At a minimum, reagent grade or
better chemicals shall be used in all tests.
7.3 Purity of Water—References to water shall be under-
stood to mean deionized water. Tap water may be used only to
prepare cement paste mixes if desired. If tap water is used for
mixing the composition of the water itself must be separately
measured as a test sample as described in Section 11.
7.4 Argon—High purity grade (99.99 %).
7.5 Calibration Standards—Single-element or multi-
element calibration reference solutions that combine appropri-
ate volumes of the stock solutions or weighed reagent-grade
chemicals in acid-rinsed volumetric flasks. Dilute to the
volume of the flask using a 5 % (v/v) nitric acid solution. Prior
to preparing the multi-element solutions, analyze each stock
solution separately to check for strong spectral interference and
the presence of impurities. Take care when preparing the
multi-element solutions to verify that the components are
compatible and stable (i.e., that they do not interact to cause
precipitation) and that none of the elements present will
contribute to mutual spectral interference. Calibration refer-
ence solutions must be verified initially using a quality control
sample and monitored periodically for stability. Mixed calibra-
tion standards will vary, depending on the number of elements
being determined.
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7.6 Calibration Blank Solution—5 % (v/v) HNO3.
7.7 Nitric Acid—5 % (v ⁄v).
7.8 Check Standards—Quality control certified NIST trace-
able samples that are stable and representative of the samples
of interest. These check standard samples represent ground
truth samples and are used to check that the measurement
process is in control.
7.9 Internal Standards—Internal standards are used to cor-
rect for instrument drift and physical interferences. Refer to
instrument operating manual for suggested internal standards.
Add internal standards to blanks, samples, and standards in a
like manner.
7.10 Membrane Filter—Nylon 25 mm diameter, 0.2 µm.
7.11 Syringe and Needle—Capacity of at least 2 mL.
7.12 Centrifuge Tubes—Clean plastic centrifuge tubes the
appropriate size for centrifuge.
7.13 Glassware—Volumetric flasks complying with the re-
quirements of ISO 1042, made of borosilicate glass complying
with the requirements of ISO 3585. Glassware should be
cleaned before each use by soaking in nitric acid and then
rinsing thoroughly with deionized water.
7.14 Pipette—Calibrated volumetric pipettes and pipette
tips, for dispensing.
8. Hazards
8.1 The toxicity or carcinogenicity of each reagent used in
this practice has not been precisely defined; however, each
chemical should be treated as a potential health hazard.
Adequate precautions should be taken to minimize exposure of
personnel to chemicals used in this practice.
8.2 Gases under high pressure are used in this practice. Use
only apparatus rated for handling the high gas pressures that
occur in this practice.
9.1 Powder Homogenization—A uniform distribution of
powder components is essential to ensure representative sam-
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pling during the mixing process, especially for blended powder
components such as portland cement and fly ash. Powders
should therefore be homogenized for 30 minutes with a
planetary mixer or similar device.
10. Sample Preparation and Collection
10.1 High Shear Mixing:
10.1.1 Blend the solid and liquid components to make a
paste according the standard practice described in Practice
D1129.
10.1.2 Set a timer to mark the end of mixing. The time on
this timer will serve as the total reaction time for the remainder
of the procedure.
10.1.3 Stir the paste with the spatula for no more than 15 s
ensure homogeneity.
10.1.4 Transfer (25 6 1) g of the paste into each of twelve
centrifuge tubes with secured lids in the minimum amount of
time possible, preferably less than 2 min.
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 C1875 − 18
10.1.5 Place the twelve centrifuge sample tubes upright in
sample holders and place them in the temperature control
device (water bath or environmental chamber).
10.2 Liquid Solution Extraction:
10.2.1 Refer to manufacturerâs manual for instructions
on safe and optimal operation of centrifuge.
10.2.2 Set centrifuge parameters to 5000 rpm for approxi-
mately 1 min, and load one centrifuge tube filled with (25 6 1)
g of solid to serve as a counterweight.
10.2.3 Within the first 10 min on the timer, select one of the
samples and place it into the centrifuge opposite the preloaded
counterweight. Begin centrifuging. Record the time indicated
on the timer when the centrifuge started.
10.2.4 Immediately after the centrifuge comes to a complete
stop, remove sample centrifuge tube.
10.2.5 Using a needle tip syringe, extract pore solution from
sample without disturbing solid material in tube.
10.2.6 Invert syringe and cautiously remove needle tip and
add a 0.20 µm nylon membrane filter at the syringe opening.
10.2.7 Transfer pore solution from syringe through filter
into a clean empty plastic sample container. Label and note
centrifugation time recorded in 10.2.3.
10.2.8 Repeat 10.2.2 through 10.2.7 at different desired
times, based on the running time being kept on the timer set in
10.1.2.
NOTE 1—Many cement pastes will begin to harden after three hours, or
perhaps even sooner, making extraction of the liquid by a centrifuge
difficult or impossible.
11. Preparation of Test Solutions and Standards
11.1 Preparation of Test Sample:
11.1.1 Transfer appropriate amount of a filtered sample into
a volumetric flask then dilute to volume with 5 % HNO3.
Repeat for each filtered pore solution from 10.2.
NOTE 2—Appropriately dilute samples to within the calibration range of
each chosen element.
11.2 Preparation of Calibration Standard:
11.2.1 Blank—Prepare a blank solution by adding same
concentration of diluted acids as used in the sample dissolution
(usually 5 % nitric acid).
11.2.2 Calibration Standards—repare known concentrations
of single-element or multi- element calibration reference solu-
tions by combining appropriate volumes of the stock solutions
in acid-rinsed volumetric flasks. Add sufficient 5 % nitric acid
to dilute to volume. Take care when preparing the multi-
element solutions to verify that the components are compatible
and stable (they do not interact to cause precipitation) and that
none of the elements present exhibit mutual spectral interfer-
ence. Calibration reference solutions must be verified initially
using a quality control sample and monitored periodically for
stability.
11.3 Preparation of Check Standard:
11.3.1 Prepare the same way as the calibration standards
11.2.2 specifically using NIST traceable certified reference
solutions.
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12. Interfaces
12.1 Refer to ICP-OES operating manual for instructions on
minimizing and checking for interferences.
13. Preparation of ICP-OES Apparatus
13.1 Prepare and operate the spectrometer in accordance
with the manufacturerâs instructions. The present practice
assumes that good operating procedures are followed. Design
differences between spectrometers make it impractical to
specify the required steps in detail.
13.2 Peristaltic Pump—If a peristaltic pump is used, inspect
the pump tubing and replace it, if necessary, before starting
each day. Verify the solution uptake rate and adjust it to the
desired rate.
13.3 ICP Excitation Source—Initiate the plasma source at
least 30 min before performing an analysis. During this warm
up period, nebulize either water or a dilute (5 %) acid solution.
NOTE 3—Some instrument manufacturers recommend even longer
warm-up periods to minimize changes in the slopes of calibration curves.
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13.4 Wavelength Profiling—Perform any wavelength profil-
ing that is specified in the normal operation of the instrument.
13.5 Operating Parameters—Assign the appropriate oper-
ating parameters to the instrument task file so that the desired
elements can be determined. Parameters to be included are
element, wavelength(s), background correction points
(optional), inter-element correction factors, and integration
time. Multiple integrations (typically three) are required for
each measurement. A typical measurement time is 10 s.
14. Calibration and Standardization
14.1 Allow the ICP-OES instrument to warm up for at least
30 min. Operate the spectrometer according to the operation
manual for the instrument.
14.2 Calibrate the instrument for the elements chosen over a
suitable concentration range by atomizing the calibration blank
and mixed calibration standard solutions, including any inter-
nal standards, and recording their concentrations and signal
intensities. A minimum of six standards and a blank should be
used for calibration with one of the standards. The computer
software will establish the slope, intercept and correlation
coefficients for each element. Use manufacture suggested
wavelengths each element. The calibration correlation coeffi-
cient shall be equal to or greater than 0.990. It is recommended
that the calibration blank and standards be matrix matched with
the same acid concentration contained in the samples. Analyze
appropriate reference solutions to validate the calibration of the
instrument before proceeding to the sample analysis.
14.3 Alternatively, calibrate according to the manufacturer’s
instructions if equivalent results are achieved.
15. Analysis by Inductively Coupled Plasma Optical
Emission Spectroscopy
15.1 Aspirate the prepared samples into the calibrated
instrument using the same conditions established for the
calibration procedure. Rinse sufficiently to prevent carryover
between samples.
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 C1875 − 18
15.2 Run a blank and a check standard (certified NIST
traceable solution) every few samples or as established to be
necessary for the instrument. Analyze a blank and check
standard at the end of each run. The concentration shall be
within 610 % of the expected value and the internal standard
should fall within established limits of deviation. If the
concentration is out of range, correct the problem, recalibrate
the instrument and rerun the samples in question.
15.3 Perform the corrections and calculations, including
dilution factors, using the instrument host computer.
16. Quality Control
16.3.2 The result obtained for the LCS shall fall within the
limit of 610 % of the expected value, or meets the desired
limits. If the result is not within these limits, reporting of
results should be halted until the problem causing the deviation
is identified and resolved. An indication of the occurrence
should accompany the reported results.
17. Calculations
17.1 To calculate the concentration of each element in the
original undiluted solution, multiply the measured concentra-
tion of that element by the dilution factor.

16.1 Confirm the performance of the instrument and cali-
bration curve by analyzing a quality control sample.
16.2 Internal Standard:
16.2.1 Select the appropriate internal standard element(s)
for the capabilities (mass availability, sensitivity) of the ICP-
OES instrument available. Yttrium is often used as an internal
standard for this purpose. The element(s) chosen for the
internal standard should not be a component of the test
specimen or calibration standard. Add internal standards to
blanks, samples, and standards in a like manner.
16.3 Laboratory Check Standard (LCS):
16.3.1 To ensure that the test method is in control, analyze
a certified NIST traceable standard solution every few samples
or as established to be necessary for the instrument. The
standard added to 5 % HNO3 (v/v) should be appropriate for
the type of samples analyzed and should produce results of
sufficient precision to ensure meaningful assessment of accu-
racy. The LCS must be taken through all the steps of the
analytical method including sample preservation and pretreat-
ment.
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18. Report
18.1 Data to report shall include the following:
18.1.1 All sample and standard information including
source details;
18.1.2 Sample analysis results;
18.1.3 Quality assurance and quality control data;
18.1.4 Identity of laboratory analysts;
18.1.5 Information on instrumentation operation and equip-
ment used;
18.1.6 Any other information that may help identify the
specimen preparation conditions or measurement conditions.
19. Precision and Bias
19.1 This practice is provided for users to develop their own
precision and bias statements when using this method.
20. Keywords
20.1 atomic emission; cementitious; chemical analysis; hy-
dration; ICP; inductively coupled plasma; optical emission;
pore solution; spectroscopy

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