ASTM C1608-23

Standard Test Method for Chemical Shrinkage of Hydraulic Cement Paste

SIGNIFICANCE AND USE
4.1 Numerous properties of cementitious materials are controlled by their initial hydration rate. Examples include early-age strength development, heat release, and crack resistance. One direct and convenient measure of this initial hydration rate is provided by the measurement of the chemical shrinkage of the cement paste during its hydration. As cement hydrates, the hydration products occupy less volume than the initial reacting materials (cement and water). Due to this volume change, a hydrating cement paste will sorb water from its immediate surroundings, when available. At early times, this sorption is in direct proportion to the amount of hydration that has occurred.5 This method is based on the one developed by Geiker.6 The results are relevant to understanding the hydration behavior of cements. This method does not measure the bulk volume changes (autogenous shrinkage) associated with chemical shrinkage nor the cracking potential of concretes produced with the evaluated cement.
SCOPE
1.1 This test method measures the internal (absolute) volume change of hydraulic cement paste that results from the hydration of the cementitious materials. This volume change is known as chemical shrinkage.  
1.1.1 Procedure A, volumetric method.  
1.1.2 Procedure B, the density method.  
1.2 The values stated in SI units are to be regarded as the 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. (Warning—Fresh hydraulic cementitious mixtures are caustic and may cause chemical burns to skin and tissue upon prolonged exposure.2)  
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

• Status: Published
• Publication Date: 30-Nov-2023
• ICS: 91.100.10 - Cement. Gypsum. Lime. Mortar
• Technical Committee: C01 - Cement
• Drafting Committee: C01.31 - Volume Change

Relations

• Replaces: ASTM C1608-17 - Standard Test Method for Chemical Shrinkage of Hydraulic Cement Paste
• Effective Date: 01-Dec-2023
• Refers: ASTM C219-24 - Standard Terminology Relating to Hydraulic and Other Inorganic Cements
• Effective Date: 01-Apr-2024
• Refers: ASTM C670-24a - Standard Practice for Preparing Precision and Bias Statements for Test Methods for Construction Materials
• Effective Date: 01-Feb-2024
• Refers: ASTM C670-24 - Standard Practice for Preparing Precision and Bias Statements for Test Methods for Construction Materials
• Effective Date: 01-Jan-2024
• Refers: ASTM C219-20a - Standard Terminology Relating to Hydraulic and Other Inorganic Cements
• Effective Date: 01-Aug-2020
• Refers: ASTM C670-15 - Standard Practice for Preparing Precision and Bias Statements for Test Methods for Construction Materials
• Effective Date: 15-Jun-2015
• Referred By: ASTM C1761/C1761M-23 - Standard Specification for Lightweight Aggregate for Internal Curing of Concrete
• Effective Date: 01-Dec-2023

Overview

ASTM C1608-23, "Standard Test Method for Chemical Shrinkage of Hydraulic Cement Paste," provides a standardized approach for measuring the internal (absolute) volume change-known as chemical shrinkage-that occurs when hydraulic cement paste hydrates. Chemical shrinkage is a crucial parameter in understanding the early-age properties of cementitious materials, including early strength development, heat evolution, and resistance to cracking. This standard, issued by ASTM International, aids laboratories, researchers, and manufacturers in accurately and consistently evaluating cement hydration behavior.

Key Topics

• Chemical Shrinkage: Refers to the absolute volume reduction accompanying the hydration of cement, as the hydration products typically occupy less volume than the original reactants (cement and water). This shrinkage influences water sorption from the paste’s surroundings.
• Test Methods:
  • Procedure A (Volumetric Method): Utilizes a glass vial, rubber stopper, and graduated capillary tube to monitor water level changes as an indicator of volume loss.
  • Procedure B (Density Method): Involves weighing density bottles containing cement paste at regular intervals to determine internal volume changes based on mass differences.
• Measurement Precision: The standard specifies repeatability and reproducibility criteria, contributing to robust, comparable results.
• Hydration Rate: Provides direct measurement of initial hydration rate, which governs key properties such as strength and risk of early-age cracking.

Applications

• Material Development and Quality Control: Enables manufacturers and engineers to assess and compare the hydration characteristics of different cementitious materials, ensuring product consistency and suitability for various construction applications.
• Research and Mix Design: Facilitates investigation into new cement formulations, supplementary cementitious materials, and additives by offering insight into how changes affect early hydration and associated physical behavior.
• Durability and Crack Resistance Assessment: Understanding chemical shrinkage helps in forecasting the likelihood of early-age cracking and in designing cementitious mixtures that better withstand crack formation.
• Education and Training: Serves as a reference method for academic and industrial training in cement chemistry and material science laboratories, promoting best practices in measurement and safety.
• Compliance and International Trade: As an internationally recognized standard, ASTM C1608-23 supports regulatory compliance and acceptance in global supply chains.

Related Standards

Users of ASTM C1608-23 may also refer to related ASTM testing and terminology standards to ensure comprehensive evaluation and compatibility:

• ASTM C114: Test Methods for Chemical Analysis of Hydraulic Cement
• ASTM C188: Test Method for Density of Hydraulic Cement
• ASTM C219: Terminology Relating to Hydraulic and Other Inorganic Cements
• ASTM C305: Practice for Mechanical Mixing of Hydraulic Cements and Mortars
• ASTM C511: Specification for Mixing Rooms and Water Storage Used in Cement Testing

Practical Value

Adopting ASTM C1608-23 standardizes the measurement of chemical shrinkage in hydraulic cement paste, directly supporting the development of durable, high-performance cementitious materials. This standard ensures repeatable and reliable results across laboratories and projects, enhances the understanding of hydration kinetics, and plays a vital role in quality assurance and construction innovation. By following this method, organizations can better anticipate early-age behavior and optimize their cement-based products for a wide range of practical applications.

Keywords: ASTM C1608-23, chemical shrinkage, hydraulic cement paste, cement hydration, cement testing, volumetric method, density method, quality control, cement standards, concrete durability, ASTM International.

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: C1608 − 23
Standard Test Method for
Chemical Shrinkage of Hydraulic Cement Paste
This standard is issued under the fixed designation C1608; 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* C219 Terminology Relating to Hydraulic and Other Inor-
ganic Cements
1.1 This test method measures the internal (absolute) vol-
C305 Practice for Mechanical Mixing of Hydraulic Cement
ume change of hydraulic cement paste that results from the
Pastes and Mortars of Plastic Consistency
hydration of the cementitious materials. This volume change is
C511 Specification for Mixing Rooms, Moist Cabinets,
known as chemical shrinkage.
Moist Rooms, and Water Storage Tanks Used in the
1.1.1 Procedure A, volumetric method.
Testing of Hydraulic Cements and Concretes
1.1.2 Procedure B, the density method.
C670 Practice for Preparing Precision and Bias Statements
1.2 The values stated in SI units are to be regarded as the
for Test Methods for Construction Materials
standard.
3. Terminology
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3.1 Definitions:
responsibility of the user of this standard to establish appro-
3.1.1 chemical shrinkage, n—the absolute (internal) vol-
priate safety, health, and environmental practices and deter-
ume change accompanying the hydration of cement, due to the
mine the applicability of regulatory limitations prior to use.
fact that the cement hydration products occupy less physical
(Warning—Fresh hydraulic cementitious mixtures are caustic
volume than the reactants.
and may cause chemical burns to skin and tissue upon
2 3.1.2 All other terms are as defined in Terminology C219.
prolonged exposure. )
1.4 This international standard was developed in accor-
4. Significance and Use
dance with internationally recognized principles on standard-
4.1 Numerous properties of cementitious materials are con-
ization established in the Decision on Principles for the
trolled by their initial hydration rate. Examples include early-
Development of International Standards, Guides and Recom-
age strength development, heat release, and crack resistance.
mendations issued by the World Trade Organization Technical
One direct and convenient measure of this initial hydration rate
Barriers to Trade (TBT) Committee.
is provided by the measurement of the chemical shrinkage of
the cement paste during its hydration. As cement hydrates, the
2. Referenced Documents
3 hydration products occupy less volume than the initial reacting
2.1 ASTM Standards:
materials (cement and water). Due to this volume change, a
C114 Test Methods for Chemical Analysis of Hydraulic
hydrating cement paste will sorb water from its immediate
Cement
surroundings, when available. At early times, this sorption is in
C186 Test Method for Heat of Hydration of Hydraulic
4 direct proportion to the amount of hydration that has occurred.
Cement (Withdrawn 2019)
This method is based on the one developed by Geiker. The
C188 Test Method for Density of Hydraulic Cement
results are relevant to understanding the hydration behavior of
cements. This method does not measure the bulk volume
1 changes (autogenous shrinkage) associated with chemical
This test method is under the jurisdiction of ASTM Committee C01 on Cement
and is the direct responsibility of Subcommittee C01.31 on Volume Change.
shrinkage nor the cracking potential of concretes produced
Current edition approved Dec. 1, 2023. Published December 2023. Originally
with the evaluated cement.
approved in 2005. Last previous edition approved in 2017 as C1608 – 17. DOI:
10.1520/C1608-23.
See the section on Safety, Manual of Cement Testing, Annual Book of ASTM
Standards, Vol. 04.01. L.J. Parrott, M. Geiker, W.A. Gutteridge, and D. Killoh, “Monitoring Portland
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Cement Hydration: Comparison of Methods,” Cement and Concrete Research, Vol.
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM 20, 919-926, 1990.
Standards volume information, refer to the standard’s Document Summary page on M. Geiker, “Studies of Portland Cement Hydration: Measurements of Chemical
the ASTM website. Shrinkage and a Systematic Evaluation of Hydration Curves by Means of the
The last approved version of this historical standard is referenced on Dispersion Model,” Ph.D. Thesis, Technical University of Denmark, Copenhagen,
www.astm.org. Denmark, 1983.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1608 − 23
5. Apparatus 7. Procedure
5.1 Devices for Determining Mass, conforming to the re-
7.1 Preparation of Cement Paste—Prepare the cement paste
quirements of Test Methods C114 and evaluated for precision
in accordance with the proportions and procedure described in
and accuracy at a total load of 100 g.
Test Method C186 (Note 1). The pastes shall be prepared in a
mixing room meeting the temperature and humidity require-
5.2 Constant Temperature Water Bath—a water bath ca-
ments outlined in Specification C511. Record to the nearest
pable of maintaining a temperature of 23.0 °C 6 0.5 °C, with
minute the time when the water first contacts the dry cement
a sufficient capacity to hold the specimens being evaluated. To
powder.
avoid evaporative cooling, the surface of the water in the bath
shall be covered with floating plastic balls or fitted with an
NOTE 1—Other mixing procedures such as mixing in a Hobart mixer
insulated lid. (see Practice C305) or kneading by hand in a sealed plastic bag may be
used. The standard paste mixture uses 150 g of cement and 60 mL of water
5.3 Timing Device—Clock that can measure time to the
(water-cement ratio of 0.40). Adjust the volume of paste mixed to match
nearest minute.
the mixing equipment used. Other water-cement ratios may be used as
long as they are stated in the test report; higher water-cement ratios may
5.4 For Procedure A
produce significant bleeding of the cement paste which will influence the
5.4.1 Capillary Tube—A graduated glass capillary tube with
results (by changing the effective water-cement ratio, and so forth); lower
graduations of 0.01 mL or smaller, and typically a capacity of
water-cement ratios may lead to difficulties in preparing a fully
1.0 mL. compacted, homogeneous paste for subsequent evaluation and self-
desiccation may occur.
5.4.2 Small Glass Vials (for example, 22 mm diameter and
55 mm height) with Rubber Stoppers that fit tightly into the
7.2 Prepare a minimum of two replicate specimens as
glass vials and have a hole placed in each stopper with the
described below for either Procedure A or Procedure B.
graduated capillary tube inserted through the hole (as shown in
7.3 Procedure A
Fig. 1). Fix the capillary tube in the stopper using a two-
7.3.1 Determine the mass of each empty glass vial to the
component epoxy or other suitable adhesive applied at the
nearest 0.01 g.
stopper’s top and bottom surfaces.
7.3.2 Carefully place the prepared cement paste into the
5.5 For Procedure B
glass vial to achieve a paste height between 5 mm and 10 mm
5.5.1 Density bottle, glass, capacity approximately 20 mL
in the vial (Note 2). Consolidate the paste in the vial by tapping
with internally conical glass stopper as shown in Fig. 2.
the vial on a laboratory countertop, or placing it on a vibrating
table, or some similar procedure.
6. Reagents and Materials
NOTE 2—For applications requiring a water-cement ratio or water-
6.1 Paraffin oil.
cementitious material ratio of less than 0.40, it is recommended that the
6.2 De-aerated water (prepared by boiling water and sealing
paste height be reduced to 3 mm or less. Thicker samples can experience
it in a closed container before it has cooled.) a process called depercolation, resulting in the measured chemical
FIG. 1 Illustration of One Experimental Setup for Monitoring Chemical Shrinkage of Hydrating Cement Paste Using Procedure A.
C1608 − 23
6,7
shrinkage being less than the true value.
7.3.3 Determine the mass of each glass vial with the cement
paste to the nearest 0.01 g.
7.3.4 Carefully, without disturbing the cement paste, add
clean, de-aerated water to fill the glass vial to the top.
7.3.5 Place the rubber stopper with the inserted capillary
tube tightly into the glass vial. Be careful to avoid the
entrapment of air bubbles when the bottom rubber stopper
surface encounters the water in the glass vial. As the rubber
stopper is inserted, the water level in the graduated capillary
tube will rise. Optimally, the water level should rise near to but
FIG. 2 Illustration of Density Bottle
...

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: C1608 − 17 C1608 − 23
Standard Test Method for
Chemical Shrinkage of Hydraulic Cement Paste
This standard is issued under the fixed designation C1608; 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 This test method measures the internal (absolute) volume change of hydraulic cement paste that results from the hydration of
the cementitious materials. This volume change is known as chemical shrinkage.
1.1.1 Procedure A, volumetric method.
1.1.2 Procedure B, the density method.
1.2 The values stated in SI units are to be regarded as the 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 and healthsafety, health, and environmental practices and determine
the applicability of regulatory limitations prior to use. (Warning—Fresh hydraulic cementitious mixtures are caustic and may
cause chemical burns to skin and tissue upon prolonged exposure. )
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.
2. Referenced Documents
2.1 ASTM Standards:
C114 Test Methods for Chemical Analysis of Hydraulic Cement
C186 Test Method for Heat of Hydration of Hydraulic Cement (Withdrawn 2019)
C188 Test Method for Density of Hydraulic Cement
C219 Terminology Relating to Hydraulic and Other Inorganic Cements
C305 Practice for Mechanical Mixing of Hydraulic Cement Pastes and Mortars of Plastic Consistency
C511 Specification for Mixing Rooms, Moist Cabinets, Moist Rooms, and Water Storage Tanks Used in the Testing of Hydraulic
Cements and Concretes
C670 Practice for Preparing Precision and Bias Statements for Test Methods for Construction Materials
3. Terminology
3.1 Definitions:
This test method is under the jurisdiction of ASTM Committee C01 on Cement and is the direct responsibility of Subcommittee C01.31 on Volume Change.
Current edition approved Aug. 1, 2017Dec. 1, 2023. Published August 2017December 2023. Originally approved in 2005. Last previous edition approved in 20122017
as C1608 – 12.C1608 – 17. DOI: 10.1520/C1608-17.10.1520/C1608-23.
See the section on Safety, Manual of Cement Testing, Annual Book of ASTM Standards, Vol. 04.01.
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.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1608 − 23
3.1.1 chemical shrinkage, n—the absolute (internal) volume change accompanying the hydration of cement, due to the fact that
the cement hydration products occupy less physical volume than the reactants.
3.1.2 All other terms are as defined in Terminology C219.
4. Significance and Use
4.1 Numerous properties of cementitious materials are controlled by their initial hydration rate. Examples include early-age
strength development, heat release, and crack resistance. One direct and convenient measure of this initial hydration rate is
provided by the measurement of the chemical shrinkage of the cement paste during its hydration. As cement hydrates, the hydration
products occupy less volume than the initial reacting materials (cement and water). Due to this volume change, a hydrating cement
paste will sorb water from its immediate surroundings, when available. At early times, this sorption is in direct proportion to the
5 6
amount of hydration that has occurred. This method is based on the one developed by Geiker. The results are relevant to
understanding the hydration behavior of cements. This method does not measure the bulk volume changes (autogenous shrinkage)
associated with chemical shrinkage nor the cracking potential of concretes produced with the evaluated cement.
5. Apparatus
5.1 Devices for Determining Mass, conforming to the requirements of Test Methods C114 and evaluated for precision and
accuracy at a total load of 100 g.
5.2 Constant Temperature Water Bath—a water bath capable of maintaining a temperature of 23.0 6 0.5°C,23.0 °C 6 0.5 °C, with
a sufficient capacity to hold the specimens being evaluated. To avoid evaporative cooling, the surface of the water in the bath shall
be covered with floating plastic balls or fitted with an insulated lid.
5.3 Timing Device—Clock that can measure time to the nearest minute.
5.4 For Procedure A
5.4.1 Capillary Tube—A graduated glass capillary tube with graduations of 0.01 mL or smaller, and typically a capacity of 1.0 mL.
5.4.2 Small Glass Vials (for example, 22-mm22 mm diameter and 55-mm55 mm height) with Rubber Stoppers that fit tightly into
the glass vials and have a hole placed in each stopper with the graduated capillary tube inserted through the hole (as shown in Fig.
1). Fix the capillary tube in the stopper using a two-component epoxy or other suitable adhesive applied at the stopper’s top and
bottom surfaces.
5.5 For Procedure B
5.5.1 Density bottle, glass, capacity approximately 20 mL with internally conical glass stopper as shown in Fig. 2.
6. Reagents and Materials
6.1 Paraffin oil.
6.2 De-aerated water (prepared by boiling water and sealing it in a closed container before it has cooled.)
7. Procedure
7.1 Preparation of Cement Paste—Prepare the cement paste in accordance with the proportions and procedure described in Test
L.J. Parrott, M. Geiker, W.A. Gutteridge, and D. Killoh, “Monitoring Portland Cement Hydration: Comparison of Methods,” Cement and Concrete Research, Vol. 20,
919-926, 1990.
M. Geiker, “Studies of Portland Cement Hydration: Measurements of Chemical Shrinkage and a Systematic Evaluation of Hydration Curves by Means of the Dispersion
Model,” Ph.D. Thesis, Technical University of Denmark, Copenhagen, Denmark, 1983.
C1608 − 23
FIG. 1 Illustration of One Experimental Setup for Monitoring Chemical Shrinkage of Hydrating Cement Paste Using Procedure A.
Method C186 (Note 1). The pastes shall be prepared in a mixing room meeting the temperature and humidity requirements outlined
in Specification C511. Record to the nearest minute the time when the water first contacts the dry cement powder.
NOTE 1—Other mixing procedures such as mixing in a Hobart mixer (see Practice C305) or kneading by hand in a sealed plastic bag may be used. The
standard paste mixture uses 150 g of cement and 60 mL of water (water-cement ratio of 0.40). Adjust the volume of paste mixed to match the mixing
equipment used. Other water-cement ratios may be used as long as they are stated in the test report; higher water-cement ratios may produce significant
bleeding of the cement paste which will influence the results (by changing the effective water-cement ratio, and so forth); lower water-cement ratios may
lead to difficulties in preparing a fully compacted, homogeneous paste for subsequent evaluation and self-desiccation may occur.
7.2 Prepare a minimum of two replicate specimens as described below for either Procedure A or Procedure B.
7.3 Procedure A
7.3.1 Determine the mass of each empty glass vial to the nearest 0.01 g.
7.3.2 Carefully place the prepared cement paste into the glass vial to achieve a paste height between 55 mm and 10 mm in the
vial (Note 2). Consolidate the paste in the vial by tapping the vial on a laboratory countertop, or placing it on a vibrating table,
or some similar procedure.
NOTE 2—For applications requiring a water-cement ratio or water-cementitious material ratio of less than 0.40, it is recommended that the paste height
be reduced to 3 mm or less. Thicker samples can experience a process called depercolation, resulting in the measured chemical shrinkage being less than
6,7
the true value.
7.3.3 Determine the mass of each glass vial with the cement paste to the nearest 0.01 g.
7.3.4 Carefully, without disturbing the cement paste, add clean, de-aerated water to fill the glass vial to the top.
7.3.5 Place the rubber stopper with the inserted capillary tube tightly into the glass vial. Be careful to avoid the entrapment of air
bubbles when the bottom rubber stopper surface encounters the water in the glass vial. As the rubber stopper is inserted, the water
Sant, G., Bentz, D., and Weiss, J., “Capillary porosity depercolation in cement-based materials: Measurement techniques and factors which influence their interpretation,”
Cemen
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