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    Dr. Kimberly KurtisSchool of Civil Engineering

    Georgia Institute of TechnologyAtlanta, Georgia

    Tests on Portland Cement

    Composition

    ~ 5CSH2CaSO42H2OCalcium sulfate dihydrate

    5 - 15C4AF4CaOAl2O3Fe2O3Tetracalcium aluminoferrite

    5 - 10C3A3CaOAl2O3Tricalcium aluminate

    15 - 30C2S2CaO SiO2Dicalcium silicate

    50 - 70C3S3CaOSiO2Tricalcium silicate

    Mass

    (%)

    Shorthand

    NotationChemical FormulaChemical Name

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    CompositionThe 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.

    Physical Properties

    Fineness

    Soundness

    Consistency

    Setting time

    False set and flash set

    Compressive strength

    Heat of hydration

    Loss on ignition

    Density

    Bulk density

    Sulfate expansion

    Tests on Portland, Blended & Hydraulic CementsTests on Portland, Blended & Hydraulic Cements

    Chemical Properties

    Chemical analysis

    Compound composition

    Chemical limits

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    Alite, C3S

    Belite, C2S

    Width o f field = 0.31 mm

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

    Chemical AnalysisChemical Analys is

    ASTM C 114 Standard Test

    Methods for Chemical Analysis

    of Hydraulic Cement

    Manganic oxideMn2O3

    Sulfide sulfur

    Titanium dioxideTiO2

    Phosphorus pentoxideP2O5

    Zinc oxideZnO

    Potassium oxideK2O

    Sodium oxideNa2O

    Loss on ignitionLOI

    Sulfur trioxideSO3

    Magnesium oxideMgO

    Calcium oxideCaO

    Ferric oxideFe2O3

    Aluminum oxideAl2O3

    Silicon dioxideSiO2

    Major components

    Minor components

    Separate determinations

    Insoluble residue

    Free calcium oxide

    CO2 (carbon dioxide)

    Water-soluble alkali

    Chloroform soluble organic

    substances

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    ASTM C114

    Oxide %

    SiO2 20.6

    Al2O3 5.07

    Fe2O3 2.90

    CaO 63.9

    MgO 1.53

    K2O 0.73

    Na2O 0.15SO3 2.53

    LOI 1.58

    Oxide Analysis

    + other trace elements

    Oxide Shorthand Common Name

    CaO C lime

    SiO2 S silica

    Al2O3 A alumina

    Fe2O3 F ferric oxide

    MgO M magnesia

    H2O H water

    K2O Kalkalis

    Na2

    O N

    SO3 sulfateS

    CO2 carbonateC

    90 95%

    (Only valid when A/F 0.64)

    C2S = 2.87S 0.75C3S

    C3A = 2.65A 1.69F

    C4AF = 3.04F

    Bogue Composition

    Compound CompositionCompound Composition

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

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    Bogue Composition: ExampleOxide Analysis

    C3S = 4.07(63.9) 7.60(20.6) 6.72(5.07)

    1.43(2.90) - 2.85(2.53) = 58.1

    C2S = 2.87(20.6) 0.754(58.1) = 15.6

    C3A = 2.65(5.07) 1.69(F 2.90) = 8.5

    C4AF = 3.04(2.90) = 8.8

    Calculated Phase Composition

    Oxide %

    SiO2 20.6

    Al2O3 5.07

    Fe2O3 2.90

    CaO 63.9

    MgO 1.53

    K2O 0.73

    Na2O 0.15

    SO3 2.53

    LOI 1.58

    9%C4AF

    9%C3A

    16%C2S

    58%C3SBogue Potential Composition:

    Oxide %

    SiO2 20.6

    Al2O3 5.07

    Fe2O3 2.90

    CaO 63.9

    MgO 1.53

    K2O 0.73

    Na2O 0.15

    SO3 2.53

    LOI 1.58

    Typical Chemical Composition of Portland Cement

    Oxide Analysis

    + other trace elements

    Sodium equivalent, Na2Oe

    Na2Oe = Na2O + (0.658 x K2O)

    Na2Oe = 0.15 + (0.658 x 0.73)

    Na2Oe = 0.63%

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    Bogue CompositionThe Bogue equations are based on the following assumptions:

    1) All 4 phases are pure2) 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 resul t, Bogue composi tions may be of f by as much as

    10% compared to XRD-determined compositions.

    BogueXRD

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    Chemical LimitsChemical Limits

    6.06.06.06.06.0MgO, max. %

    3.02.53.03.03.0LOI, max. %

    0.750.750.750.750.75Insoluble residue,

    max. %

    Cement Type

    3.0

    n/a

    2.3

    n/a

    3.5

    4.5

    3.0

    n/a

    3.0

    3.5

    SO3, max. %

    C3A 8%

    C3A > 8%

    -6.5-6.0-Fe2O3, max. %

    ---6.0-Al2O3, max. %

    ---20.0-SiO2, min. %

    VIVIIIIII

    ASTM C 150 Portland Cement - Chemical Requirements

    Chemical LimitsChemical Limits

    Cement Type

    25----C4AF + 2 C3A,

    max. %

    57158-C3A, max. %

    -25---C2S, min. %

    -35---C3S, max. %

    VIVIIIIII

    ASTM C 150 Portland Cement - Chemical Requirements

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    Chemical LimitsChemical Limits

    Cement Type

    0.600.600.600.600.60Na2Oe, max. %

    ---58-C33 + C3A, max. %

    --5--C3A, max. %

    --8--C3A, max. %

    VIVIIIIII

    ASTM C 150 Portland Cement Optional Chemical Requirements

    Chemical LimitsChemical Limits

    5.04.03.0LOI, max. %

    -0.03*-Water-soluble alkali, max. %

    6.0--MgO, max. %

    -2.02.0Sulfide sulfur (S), max. %

    -1.01.0Insoluble residue, max. %

    Cement Type

    4.04.03.0Sulfur reported as SO3, max.

    %

    I(PM),

    I(PM)-A, P,

    PA,

    IP, IP-A

    S, SAI(SM), I(SM)-

    A, IS, IS-A

    ASTM C 595 Blended Cement - Chemical Requirements

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

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    FinenessFineness

    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

    However, later strength is not directly affected.

    Neville, Fig. 1.5

    FinenessFineness

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    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

    FinenessFineness

    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 PermeabilityLea 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 cement, a bed 10mmthick with porosity of 4.75% is

    made; air is passed through at

    constant velocity; pressure drop

    is measured.

    Sw= 14 [(3Ah1)/(KLh2)]

    0.5

    (1-)

    Blaine Air PermeabilityBlaine Air Permeabili ty

    Blaine Air Permeability

    (ASTM C 204)

    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

    standard porosity of 5% (0.500).

    Sw = K2t0.5

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    WagnerWagner TurbidimeterTurbidimeter

    Wagner Turbidimeter

    (ASTM C 115)

    Uses a photoelectric cell to

    measure light passing through

    cement particles suspended

    in kerosene

    Test is based on Stokes Law

    that states that a sphere will

    obtain a constant velocity

    under the action of gravity

    Allows calculation of particle-

    size distribution (psd)

    Blaine, in general, is 1.8X Wagner

    Laser Particle Size AnalyzerLaser Particle Size Analyzer

    Laser particle sizeanalyzer

    Particle-size distribution

    (psd)

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    Cement FinenessCement Fineness

    ASTM C 430

    Sample washed over 45-m (# 325) sieve Used in production

    Limits for pozzolans and slag (ASTM C 595)

    Cement FinenessCement Fineness

    Requirements for Type I, II, IV & V

    (No requirements for Type III)

    Minimum, m2/kg

    Air Permeability Turbidimeter

    ASTM C 150 &

    AASHTO M 85280 160

    Maximum, m2/kgAASHTO M 85 400 220

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

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

    Typical values, m2/kg 350-380 Type I

    450-600 Type III

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    SoundnessSoundness

    Soundness - ability of hardened paste to

    maintain volume after setting

    Unsoundness (abnormal expansion)

    caused by hard-burned CaO or MgO

    22 )(OHCaOHCaO +

    22 )(OHMgOHMgO +

    ASTM C 151 Standard Test Method for

    Autoclave Expansion of Portland Cement

    Expansion for all portland,

    blended & hydraulic cements 0.80%

    ConsistencyConsistency

    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 TimeSetting Time

    Initial Set

    Final Set

    Time from moment water is added until the paste

    ceases to be fluid and plastic

    Time from moment water is added for the paste to

    acquire a certain degree of hardness

    Setting Time: Standard TestSetting 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 MeasurementsSetting Time: Field Measurements

    Concrete penetrometer, measures

    resistance to penetration in sieved mortar

    samples

    Pocket penetrometers

    Setting Time: Standard TestSetting 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 TimeSetting Time

    ASTM C 150 Por tland Cement

    Initial Set, not less than (h:min)

    Final Set, not more than (h:min)

    Vicat Needle Gillmore Needles

    0:45

    6:15

    1:00

    10:00

    ASTM C 595 Blended Cement

    Initial Set, not less than (h:min)

    Final Set, not more than (h:min)

    0:45

    7:00

    ASTM C 1157 Hydrau lic Cement

    Initial Set, not less than (h:min)

    Final Set, not more than (h:min)

    0:45

    7:00

    Setting TimeSetting Time

    0 100 200 300 400

    Type V

    Type IV

    Type III

    Type II

    Type I

    Time of Set (Minutes) - Vicat Method

    Initial

    Final

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    False Set and Flash SetFalse Set and Flash Set

    False Set Loss of plasticity shortly after mixing little heat

    Due to hemihydrate (plaster) in cement

    hydrating to gypsum

    Workability restored by additional mixing

    Early Stiffening Early Stiffening

    False Set and Flash SetFalse Set and Flash Set

    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

    Early Stiffening Early Stiffening

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    Compressive StrengthCompressive 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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    ASTM C 150 Standard Specification for Portland Cement

    Cement Type

    21.0

    (3050)

    17.0

    (2470)

    ---28 days

    15.0

    (2180)

    7.0

    (1020)

    -17.0

    (2470)

    19.0

    (2760)

    7 days

    8.0

    (1160)

    -24.0

    (3480)

    10.0

    (1450)

    12.0

    (1740)

    3 days

    --12.0

    (1740)

    --1 day

    VIVIIIIII

    Age

    Minimum Strength Requirements, MPa (psi)

    Compressive StrengthCompressive Strength

    Lower strengths permitted for air-entraining cements (Types IA, IIA & IIIA)

    and when heat of hydration option is specified for Type II cement

    ASTM C 595 Standard Specification for Blended Hydraulic Cements

    Cement Type

    21.0

    (3140)

    11.0

    (1600)

    25.0

    (3620)

    25.0

    (362)

    28 days

    11.0

    (1600)

    5.0

    (720)

    18.0

    (2610)

    20.0

    (2900)

    7 days

    --11.0

    (1600)

    13.0

    (1890)

    3 days

    PSIS(MS),

    IP(MS)

    I(SM), IS,

    I(PM), IP

    Age

    Minimum Strength Requirements, MPa (psi)

    Compressive StrengthCompressive Strength

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

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    ASTM C 1157 Standard Specification for Hydraulic Cement

    Cement Type

    17-17---28 days

    5101017-177 days

    -551017103 days

    ----10-1 day

    LHMHHSMSHEGU

    Age

    Minimum Strength Requirements (MPa)

    Compressive StrengthCompressive Strength

    ASTM C 1157 Standard Specification for Hydraulic Cement

    -60

    (8700)

    40

    (5800)

    30

    (4350)

    20

    (2900)

    15

    (2175)

    Maximum Strength,

    MPa (psi)

    45

    (6525)

    35

    (5075)

    25

    (3625)

    17

    (2465)

    10

    (1450)

    5

    (725)

    Minimum Strength,

    MPa (psi)

    45352517105Strength Range

    Minimum Strength Requirements (MPa)

    Compressive StrengthCompressive Strength

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    Heat of HydrationHeat of Hydration

    Heat evolution in portland cement tested by conduction calorimetry

    Heat of Solution Test

    ASTM C 186 Standard Test Method for

    Heat of Hydration of Portland Cement

    Conduction Calorimetry

    Heat of HydrationHeat of Hydration

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    Heat of HydrationHeat of Hydration

    Moderate Heat

    of Hydration

    Low Heat of

    Hydration

    ASTM C 150

    Portland Cement

    Type II (Option)

    290 kJ/kg at 7 days

    Type IV

    250 kJ/kg at 7 days

    290 kJ/kg at 28 days

    Heat of HydrationHeat of Hydration

    Moderate Heat

    of Hydration

    Low Heat of

    Hydration

    ASTM C 150

    Portland Cement

    Type II (Option)

    290 kJ/kg at 7 days

    Type IV

    250 kJ/kg at 7 days

    290 kJ/kg at 28 days

    ASTM C 595

    Blended Cement

    Suffix -MH Suffix -LH

    250 kJ/kg at 7 days

    290 kJ/kg at 28 days

    290 kJ/kg at 7 days

    330 kJ/kg at 28 days

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    Heat of HydrationHeat of Hydration

    Moderate Heat

    of Hydration

    Low Heat of

    Hydration

    ASTM C 150

    Portland Cement

    Type II (Option)

    290 kJ/kg at 7 days

    Type IV

    250 kJ/kg at 7 days

    290 kJ/kg at 28 days

    ASTM C 595

    Blended Cement

    Suffix -MH Suffix -LH

    250 kJ/kg at 7 days

    290 kJ/kg at 28 days

    290 kJ/kg at 7 days

    330 kJ/kg at 28 days

    ASTM C 1157

    Hydraulic Cement

    Type MH Type LH

    250 kJ/kg at 7 days

    290 kJ/kg at 28 days

    290 kJ/kg at 7 days

    Loss on IgnitionLoss on Ignition

    ASTM C 114 Standard Test Methods

    for Chemical Analysis of Hydraulic

    Cement

    Loss on ignition LOI

    Sample ignited at 900 to 1000C

    (1650 to 1830F)

    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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    DensityDensity

    Le Chatelier flask - ASTM C 188 Standard

    Test Method for Density of Hydraulic Cement

    HeliumHelium pycnometerpycnometer

    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

    Bulk DensityBulk Density

    Bulk density of cement varies

    between

    830 kg/m3 (52 lb/ft3)

    and

    1650 kg/m3 (103 lb/ft3).

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    ASTM C 452 Standard Test Method for Potential Expansion ofPortland-Cement Mortars Exposed to Sulfate

    Sulfate ExpansionSulfate Expansion

    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

    Type V Sulfate-Resisting

    Portland Cement

    Expansion 0.040%

    at 14 days

    Limits for C3A, C4AF

    + 2C3A, SiO2 & Fe2O3not required