Tests on Portland Cement

Dr. Kimberly Kurtis

School of Civil Engineering
Georgia Institute of Technology
Atlanta, Georgia

Composition
Shorthand Mass
Chemical Name Chemical Formula Notation (%)
Tricalcium silicate 3CaO•SiO2 C3S 50 - 70

Dicalcium silicate 2CaO• SiO2 C2S 15 - 30

Tricalcium aluminate 3CaO•Al2O3 C3A 5 - 10

Tetracalcium aluminoferrite 4CaO•Al2O3•Fe2O3 C4AF 5 - 15

Calcium sulfate dihydrate CaSO4•2H2O CSH2 ~5

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 Composition
The relative quantities of each of these phases affects:
• setting time
• rate of strength development
• overall strength
• durability
• color

It is important, then, to know the composition of the

cement.

Tests on Portland, Blended & Hydraulic Cements

Chemical Properties Physical Properties

Chemical analysis Fineness
Compound composition Soundness
Chemical limits Consistency
Setting time
False set and flash set
Compressive strength
Heat of hydration
Loss on ignition
Density
Bulk density
Sulfate expansion

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Belite, C2S

Alite, C3S

Width of field = 0.31 mm

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 /
http://www.bruker-axs.de

Chemical Analysis
ASTM C 114 Standard Test
SiO2 Silicon dioxide
Methods for Chemical Analysis
Al2O3 Aluminum oxide
of Hydraulic Cement
Fe2O3 Ferric oxide
CaO Calcium oxide Major components
MgO Magnesium oxide Separate determinations
SO3 Sulfur trioxide • Insoluble residue
LOI Loss on ignition • Free calcium oxide
• CO2 (carbon dioxide)
Na2O Sodium oxide
• Water-soluble alkali
K2O Potassium oxide
• Chloroform – soluble organic
TiO2 Titanium dioxide substances
P2O5 Phosphorus pentoxide Minor components
ZnO Zinc oxide
Mn2O3 Manganic oxide
Sulfide sulfur

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 ASTM C114
Oxide Analysis Oxide Shorthand Common Name
Oxide %
CaO C lime

SiO2 S silica
SiO2 20.6
Al2O3 5.07 Al2O3 A alumina
90 – 95%
Fe2O3 2.90 Fe2O3 F ferric oxide
CaO 63.9
MgO M magnesia
MgO 1.53
K2O K
K2O 0.73 alkalis
Na2O 0.15 Na2O N

SO3 2.53 SO3 S sulfate

LOI 1.58 CO2 C carbonate

+ other trace elements H2O H water

Compound Composition

Bogue Composition

C3S = 4.07C – 7.60S – 6.72A – 1.43F – 2.85S

C2S = 2.87S – 0.75C3S
C3A = 2.65A – 1.69F
C4AF = 3.04F

(Only valid when A/F ≥ 0.64)

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 Bogue Composition: Example
Oxide Analysis Calculated Phase Composition
Oxide %
C3S = 4.07(63.9) – 7.60(20.6) – 6.72(5.07)
– 1.43(2.90) - 2.85(2.53) = 58.1
SiO2 20.6
Al2O3 5.07 C2S = 2.87(20.6) – 0.754(58.1) = 15.6
Fe2O3 2.90
CaO 63.9 C3A = 2.65(5.07) – 1.69(F 2.90) = 8.5
MgO 1.53
K2O 0.73
C4AF = 3.04(2.90) = 8.8

Na2O 0.15 Bogue Potential Composition: C3S 58%

SO3 2.53 C2S 16%
LOI 1.58
C3A 9%
C4AF 9%

Typical Chemical Composition of Portland Cement

Oxide Analysis
Oxide %
Sodium equivalent, Na2Oe

SiO2 20.6
Na2Oe = Na2O + (0.658 x K2O)
Al2O3 5.07
Fe2O3 2.90
CaO 63.9
MgO 1.53 Na2Oe = 0.15 + (0.658 x 0.73)
K2O 0.73
Na2Oe = 0.63%
Na2O 0.15
SO3 2.53
LOI 1.58

+ other trace elements

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 Bogue Composition
The Bogue equations are based on the following assumptions:
1) All 4 phases are pure
2) All the F present occurs as C4AF, and the quantities of A =
0.64(%F) and C = 1.40 (%F) are subtracted from the
appropriate totals.
3) The remaining Al2O3 is combined as C3A and a further quantity
of C = 1.65 (% Al2O3) is subtracted fromt eh total remaining
CaO.
4) The SiO2 combines initially with CaO to form C2S giving a
provisional C2S figure. The CaO combining with SiO2 =
2.87%(SiO2) is subtracted from the total CaO figure, and the
remaining CaO is then combined with a part of the C2S =
4.07(%CaO) to form C3S.
As a result, Bogue compositions may be “off” by as much as
10% compared to XRD-determined compositions.

Bogue XRD

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 Chemical Limits
ASTM C 150 Portland Cement - Chemical Requirements

Cement Type
I II III IV V
SiO2, min. % - 20.0 - - -

Al2O3, max. % - 6.0 - - -

Fe2O3, max. % - 6.0 - 6.5 -
MgO, max. % 6.0 6.0 6.0 6.0 6.0
SO3, max. %
C3A ≤ 8% 3.0 3.0 3.5 2.3 3.0
C3A > 8% 3.5 n/a 4.5 n/a n/a
LOI, max. % 3.0 3.0 3.0 2.5 3.0
Insoluble residue, 0.75 0.75 0.75 0.75 0.75
max. %

Chemical Limits
ASTM C 150 Portland Cement - Chemical Requirements

Cement Type
I II III IV V
C3S, max. % - - - 35 -

C2S, min. % - - - 25 -
C3A, max. % - 8 15 7 5
C4AF + 2 C3A, - - - - 25
max. %

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 Chemical Limits
ASTM C 150 Portland Cement – Optional Chemical Requirements

Cement Type
I II III IV V
C3A, max. % - - 8 - -

C3A, max. % - - 5 - -
C33 + C3A, max. % - 58 - - -
Na2Oe, max. % 0.60 0.60 0.60 0.60 0.60

Chemical Limits
ASTM C 595 Blended Cement - Chemical Requirements

Cement Type
I(SM), I(SM)- S, SA I(PM),
A, IS, IS-A I(PM)-A, P,
PA,
IP, IP-A
MgO, max. % - - 6.0
Sulfur reported as SO3, max. 3.0 4.0 4.0
%
Sulfide sulfur (S), max. % 2.0 2.0 -
Insoluble residue, max. % 1.0 1.0 -
LOI, max. % 3.0 4.0 5.0
Water-soluble alkali, max. % - 0.03* -

*Only required when cement is specified to be nonstaining to limestone

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 Fineness

Fineness of cement is also important; it affects:

• rate of hydration
• rate of setting
• rate of hardening
• durability (ASR)
• rate of carbonation during storage
• cost
• rate of gypsum addition
• bleeding

Fineness

However, later strength is not directly affected.

Neville, Fig. 1.5

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 Fineness

Approx. 95% ≤ 45 microns

Average diameter ~ 15
microns

Those retained on the No 200

sieve (75 microns) will never
hydrate completely

Those retained on the No 325

sieve (45 microns) will be
difficult to hydrate completely

Type III >> Type I, II, V > Type IV

Fineness is generally described as the specific surface of the

cement, which is the surface area expressed in m2/kg

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 Lea and Nurse Air Permeability

Relates flow of fluid (air)

through a bed of granular
material (cement) to the specific
surface area of that granular
material

By knowing ρcement, a bed 10mm

thick with porosity of 4.75% is
made; air is passed through at
constant velocity; pressure drop
is measured.

Sw= 14 [(ε3Ah1)/(KLh2)]0.5
ρ(1-ε)

Blaine Air Permeability

• With the Lea Nurse method, air

passes through the bed at a constant
rate

• In the Blaine test, a known volume of

air passes at a constant pressure
through the bed
• The rate of flow decreases steadily
• The time for flow to occur is
measured for a given apparatus and a
Blaine Air Permeability
standard porosity of 5% (0.500).
(ASTM C 204)
Sw = K2t0.5

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 Wagner Turbidimeter

• Uses a photoelectric cell to

measure light passing through
cement particles suspended
in kerosene
• Test is based on Stoke’s Law
that states that a sphere will
obtain a constant velocity
under the action of gravity
• Allows calculation of particle-
size distribution (psd)
Wagner Turbidimeter
(ASTM C 115)
Blaine, in general, is 1.8X Wagner

Laser Particle Size Analyzer

•Laser particle size

analyzer
•Particle-size distribution
(psd)

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 Cement Fineness

ASTM C 430
• Sample washed over 45-µm (# 325) sieve
• Used in production
• Limits for pozzolans and slag (ASTM C 595)

Cement Fineness

Requirements for Type I, II, IV & V

(No requirements for Type III)

Air Permeability Turbidimeter

ASTM C 150 &

Minimum, m2/kg 280 160
AASHTO M 85

Maximum, m2/kg AASHTO M 85 400 220

Typical values, m2/kg 350-380 Type I

450-600 Type III

No limits for blended cement (ASTM C 595) or hydraulic cements

(ASTM C 1157) but values must be reported on mill test reports

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 Soundness

Soundness - ability of hardened paste to

maintain volume after setting

Unsoundness (abnormal expansion)

caused by hard-burned CaO or MgO

CaO + H 2O → Ca (OH ) 2
MgO + H 2O → Mg (OH ) 2

ASTM C 151 Standard Test Method for

Autoclave Expansion of Portland Cement

Expansion for all portland,

≤ 0.80%
blended & hydraulic cements

Consistency

Consistency of Cement Paste

• Penetration of 10 ± 1 mm of Vicat plunger
• ASTM C 187 Standard Test Method for
Normal Consistency of Hydraulic Cement

Consistency of Mortar
• Flow table
• ASTM C 1437 Standard Test Method for
Flow of Hydraulic Mortar

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 Setting Time

Initial Set Time from moment water is added until the paste
ceases to be fluid and plastic

Final Set Time from moment water is added for the paste to
acquire a certain degree of hardness

Setting Time: Standard Test

Vicat Needle
• ASTM C 191 Standard Test Method for
Time of Setting of Hydraulic Cement by
Vicat Needle
• Initial set occurs when needle penetrates
- after 30s - 25 mm (1 inch) into paste
• Final set occurs when there is no visible
penetration

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Setting Time: Field Measurements

• Concrete penetrometer, measures

resistance to penetration in sieved mortar
samples
• Pocket penetrometers

Setting Time: Standard Test

Gillmore Needles
• ASTM C 266 Standard Test
Method for Time of Setting of
Hydraulic-Cement Paste by
Gillmore Needles
• Setting determined as time when
paste resists indentation by
needles

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 Setting Time

Vicat Needle Gillmore Needles

ASTM C 150 Portland Cement

Initial Set, not less than (h:min) 0:45 1:00

Final Set, not more than (h:min) 6:15 10:00

ASTM C 595 Blended Cement

Initial Set, not less than (h:min) 0:45

Final Set, not more than (h:min) 7:00

ASTM C 1157 Hydraulic Cement

Initial Set, not less than (h:min) 0:45

Final Set, not more than (h:min) 7:00

Setting Time

Type I

Type II Initial
Final
Type III

Type IV

Type V

0 100 200 300 400

Time of Set (Minutes) - Vicat Method

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 False Set and Flash Set
“Early Stiffening”

False Set • Loss of plasticity shortly after mixing – little heat

• Due to hemihydrate (plaster) in cement –
hydrating to gypsum
• Workability restored by additional mixing

False Set and Flash Set

“Early Stiffening”

False Set • Loss of plasticity shortly after mixing – little heat

• Due to hemihydrate (Plaster) in cement –
hydrating to Gypsum
• Workability restored by additional mixing

Flash Set • Rapid & early loss of workability – significant heat

• Due to rapid reaction of aluminates – when
insufficient sulfate present
• Workability cannot be restored

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 Compressive Strength

ASTM C 109 Standard Test Method

for Compressive Strength of Hydraulic
Cement Mortars.

• 50-mm (2-inch) mortar cubes

• Sand:Cement = 2.75:1
• Water/Cement = 0.485 for portland
cement (0.460 for air-entraining
portland cement)
• Sufficient water for flow 110 ± 5 for
blended (ASTM C 595) and
hydraulic (ASTM C 1157) cements

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 Compressive Strength

ASTM C 150 Standard Specification for Portland Cement

Minimum Strength Requirements, MPa (psi)
Age Cement Type

I II III IV V

1 day - - 12.0 - -
(1740)
3 days 12.0 10.0 24.0 - 8.0
(1740) (1450) (3480) (1160)
7 days 19.0 17.0 - 7.0 15.0
(2760) (2470) (1020) (2180)
28 days - - - 17.0 21.0
(2470) (3050)

Lower strengths permitted for air-entraining cements (Types IA, IIA & IIIA)
and when heat of hydration option is specified for Type II cement

Compressive Strength

ASTM C 595 Standard Specification for Blended Hydraulic Cements

Minimum Strength Requirements, MPa (psi)
Age Cement Type

I(SM), IS, IS(MS), S P

I(PM), IP IP(MS)
3 days 13.0 11.0 - -
(1890) (1600)
7 days 20.0 18.0 5.0 11.0
(2900) (2610) (720) (1600)
28 days 25.0 25.0 11.0 21.0
(362) (3620) (1600) (3140)

Lower strengths permitted for air-entraining cements (with suffix –A)

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 Compressive Strength

ASTM C 1157 Standard Specification for Hydraulic Cement

Minimum Strength Requirements (MPa)

Age Cement Type

GU HE MS HS MH LH

1 day - 10 - - - -

3 days 10 17 10 5 5 -

7 days 17 - 17 10 10 5

28 days - - - 17 - 17

Compressive Strength

ASTM C 1157 Standard Specification for Hydraulic Cement

Minimum Strength Requirements (MPa)

Strength Range 5 10 17 25 35 45

Minimum Strength, 5 10 17 25 35 45
MPa (psi) (725) (1450) (2465) (3625) (5075) (6525)
Maximum Strength, 15 20 30 40 60 -
MPa (psi) (2175) (2900) (4350) (5800) (8700)

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 Heat of Hydration

Heat evolution in portland cement – tested by conduction calorimetry

Heat of Hydration

Heat of Solution Test

ASTM C 186 Standard Test Method for

Heat of Hydration of Portland Cement

Conduction Calorimetry

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 Heat of Hydration

Moderate Heat Low Heat of

of Hydration Hydration

ASTM C 150 Type II (Option) Type IV

Portland Cement 290 kJ/kg at 7 days 250 kJ/kg at 7 days
290 kJ/kg at 28 days

Heat of Hydration

Moderate Heat Low Heat of

of Hydration Hydration

ASTM C 150 Type II (Option) Type IV

Portland Cement 290 kJ/kg at 7 days 250 kJ/kg at 7 days
290 kJ/kg at 28 days

ASTM C 595 Suffix -MH Suffix -LH

Blended Cement 290 kJ/kg at 7 days 250 kJ/kg at 7 days
330 kJ/kg at 28 days 290 kJ/kg at 28 days

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 Heat of Hydration

Moderate Heat Low Heat of

of Hydration Hydration

ASTM C 150 Type II (Option) Type IV

Portland Cement 290 kJ/kg at 7 days 250 kJ/kg at 7 days
290 kJ/kg at 28 days

ASTM C 595 Suffix -MH Suffix -LH

Blended Cement 290 kJ/kg at 7 days 250 kJ/kg at 7 days
330 kJ/kg at 28 days 290 kJ/kg at 28 days

ASTM C 1157 Type MH Type LH

Hydraulic Cement 290 kJ/kg at 7 days 250 kJ/kg at 7 days
290 kJ/kg at 28 days

Loss on Ignition

ASTM C 114 Standard Test Methods

for Chemical Analysis of Hydraulic
Cement

• Loss on ignition – LOI

• Sample ignited at 900 to 1000°C
(1650 to 1830°F)
• High LOI indicates prehydration
and/or carbonation
• Improper or prolonged storage
(transportation)

ASTM C 150 Portland Cement LOI ≤ 3.0% (2.5% for Type IV)
ASTM C 595 Blended Cement LOI ≤ 3.0 – 5.0%
ASTM C 1157 Hydraulic Cement No limit – must be reported

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 Density

Le Chatelier flask - ASTM C 188 Standard

Test Method for Density of Hydraulic Cement
• Range= 3100 to 3250 kg/m3
• Average = 3150 kg/m3 (196 lb/ft3)
• Not indicator of quality
• Used for mixture proportioning
calculations

Relative density (specific gravity) = 3.15

Helium pycnometer

Bulk Density

Bulk density of cement varies

between
830 kg/m3 (52 lb/ft3)
and
1650 kg/m3 (103 lb/ft3).

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 Sulfate Expansion

ASTM C 452 Standard Test Method for Potential Expansion of

Portland-Cement Mortars Exposed to Sulfate
• Gypsum added to cement to yield 7.0% SO3 (by mass of
cement + gypsum)
• Mortar bars stored in water
• Length change monitored periodically
• Only applicable to portland cements

ASTM C 150 Portland Cement

Optional requirement for Limits for C3A, C4AF

Expansion ≤ 0.040%
Type V Sulfate-Resisting + 2C3A, SiO2 & Fe2O3
at 14 days
Portland Cement not required

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