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ASTM C114, 2007

Erick Josue Villa Lun Anwar Mussaddad Anthony Gonzalez

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C 114 – 07

APPENDIXES

(Nonmandatory Information)

X1. EXAMPLE OF DETERMINATION OF EQUIVALENCE POINT FOR THE CHLORIDE DETERMINATION

(Column 1) (Column 2) (Column 3) (Column 4)

AgNO3, mL Potential, mV D  mV A D2 mVB 

1.60 125.3
5.8
1.80 119.5 1.4
7.2
2.00 112.3 1.3
8.5
2.20 103.8 1.3
9.8
2.40 94.0 0.6
9.2
2.60 84.8 2.3
6.9
2.80 77.9 0.8
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3.00 71.8 1.3   ,

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4.8   ,
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3.20 67.0     -

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The equivalence point is in the maximum  D  mV interval (Column 3) and thus between 2.20 and 2.40 mL. The exact equivalence point in this 0.20 increment is cal-   ,
        `
  ,
  ,

culated from the  D 2 mV (Column 4) data as follows:

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E  5  2.20  1 ~ 1.3 / ~1.3 1  0.6 ! ! 3  0.20  5  2.337 mL. Round to 2.34.

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A
Differences between successive readings in Column 2.
B 
Differences between successive  D  readings in Column 3 “second differentials”.

X2. CO2   DETERMINATIONS IN HYDRAULIC CEMENTS

X2.1 Scope X2.1.5 The split loss on ignition method in X2.2.1 can give
X2.1.1 This appendix contains information about methods misleading results when used with materials containing CaOH 2
for determination of carbon dioxide (CO 2) in hydraulic cement. (calcium hydroxide). This can occur with aged cement, cement
The methods listed received a favorable evaluation by Task  made from aged clinker, or high free lime clinker, in addition
Group C01.23.04. to cements with a lime or hydrated lime ingredient.
X2.1.2 Section   X2.2   lists the analytical methods that re-
ceived a favorable evaluation, briefly describes each method, X2.2 Analytical Methods
suggests analytical techniques or cautions that may be useful, X2.2.1   Split Loss on Ignition—This procedure is compa-
and indicates limitations to some of the methods. rable to the analytical method described in Test Methods
X2.1.3 The methods listed as   X2.2.1,   X2.2.4,   X2.2.5,   and C 114, Section  3.3.1.1,  with the following modifications:
X2.2.6   determine total carbon calculated as CO 2. For that
1. A crucible of known mass and containing a sample of 
reason, they are not appropriate for determination of carbon
known mass is initially heated at 550 °C for 2 h.
dioxide in fly ash, limestones containing carbon in the form of 
graphite or kerogen, in other carbon bearing materials, or in 2. After being cooled to room temperature in a desiccator,
blended cements produced from these materials. and its mass determined, the crucible with sample is then
X2.1.4 The methods listed in  X2.2.2 and X2.2.3 can deter- heated at 950 °C for 2 h.
mine actual CO2   directly rather than by calculation from total 3. Finally, the crucible with sample is cooled and its mass is
carbon. They are suggested for analysis of blended cements determined as per Step No. 2.
and blended cement ingredients which are likely to contain 4. The difference in residue masses after the respective heat
non-carbonate carbon. treatments is assumed to be carbon dioxide.

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C 114 – 07
TGA results indicated that CaOH 2   can lose a significant TABLE X2.1 Cooperative Test Series No. 1
portion of its mass above 500 °C. Thus, the Split Loss on Single Determinations
Ignition procedure should not be used when situations de- Carbon Determinations Added Added
scribed in  X2.1.5  exist. Dioxide Base CO2, c% CO2,
UnknownA Cement B  Determined C  % KnownD 
X2.2.2   Thermogravimetric Analysis (TGA)—This method
Split LOI 2.40 0.45 1.97 2.00
involves the determination of sample mass loss at various
2.52 0.56 1.99
temperatures. The heating of a sample through a temperature 2.41 0.36 2.07
range allows for mass loss differentiation based on mineral 2.39 0.32 2.09
2.41 0.36 2.07
form (for example, CaCO3, MgCO3, CaOH2, etc.). Specific
2.28 0.27 2.02
operational information is provided by the equipment manu- Test Methods 2.00 0.02 1.98
facturers. If free carbon is present, an inert atmosphere (for E 350
2.00 0.02 1.98
example, nitrogen) should be used for sample analysis. Induction 2.46 0.40 2.07
X2.2.3   Test Methods   C 25 , Section 22—“Standard Test Furnace/IR
Methods for Chemical Analysis of Limestone, Quicklime, and 2.53 0.48 2.08
2.38 0.40 2.00
Hydrated Lime.” This method involves decomposition of the 2.42 0.48 1.97
sample with HCl. The liberated CO 2  is then passed through a Average Standard 2.02
series of scrubbers to remove water and sulfides. The CO 2  is Deviation
0.05
absorbed with special Sodium Hydroxide Absorbent (Ascar-
A
The Unknown was prepared by blending/grinding a mixture of 5.00 % NIST
ite). The gain in mass of the absorption tube is determined and SRM 1C Argillaceous Limestone and 95.00 % CCRL Portland Cement Reference
calculated as percent CO 2. Calcium carbonate, for instance, Sample No. 85.According to the Certificate of Analysis, the SRM 1C had a loss on
can be calculated by multiplying the determined CO 2  content ignition of 39.9 %. For the purpose of the cooperative test series, the loss on
ignition was assumed to be CO 2  only.
by a conversion factor (for example, CO 2 3 2.2742 = CaCO3). B 
The Base Cement was CCRL Portland Cement Reference Sample No. 85.
X2.2.4   X-ray Fluorescence Spectroscopy —In this method C 
The Determined % Added CO2  was obtained by subtracting the Base Cement
the sample is ground to a fine particle size, pressed into a flat % CO2  from the Unknown % CO 2.
D 
The addition of 5.00 % NIST SRM 1C (with a loss on ignition value of 39.9 %)
pellet and irradiated with the chosen instrument. Carbon would provide 2.00 % Added CO 2. (Again, it was assumed that the SRM 1C loss
content is determined by comparing the collected carbon on ignition was only carbon dioxide.)
emissions to calibration standards.
X2.2.5   Combustion by Induction Furnace/IR—This method TABLE X2.2 Cooperative Test Series No. 2
involves volatilization by induction furnace and detection by Averages from Three Determinations
infrared absorption. Suitable calibration standards (for ex- Carbon Determinations Added CO2,
Added CO2
ample, calcium carbonate and synthetic carbon) are available Dioxide Base %
% KnownD 
UnknownA Cement B  Determined C 
from some instrument manufacturers. NIST cement SRMs
with known additions of NIST argillaceous limestone (or other Split LOI 2.00 0.41 1.59 1.60
1.65 0.32 1.33
suitable standards) should also be considered to check instru- 2.02 0.46 1.56
ment calibration. 1.91 0.35 1.56
2.10 0.43 1.67
X2.2.6   “Test Methods  E 350—This method, Total Carbon
1.91 0.41 1.50
by the Combustion Gravimetric Method from Test Methods for 1.98 0.46 1.52
Chemical Analysis of Carbon Steel, Low-Alloy Steel, Silicon XRFA 1.68E  0.00E  1.68E 
Induction Furnace/IR 2.23 0.28 1.95
Electrical Steel, Ingot Iron, and Wrought Iron,” is suitable for
1.96 0.28 1.68
the determination of carbon in concentrations from 0.05 to 1.95 0.40 1.55
1.80 % (as carbon dioxide 0.18 to 6.60 %). The test method TGA 1.77 0.20 1.57
1.87 0.25 1.62
involves burning the sample in a stream of oxygen; the carbon Average Standard Deviation 1.60
dioxide in the evolved gases is then collected in a suitable 0.14
absorbent and its mass determined. Time of analysis is less A
The Unknown was prepared by blending/grinding a mixture of 4.00 % NIST
than 10 min. SRM 1C Argillaceous Limestone and 96.00 % CCRL Portland Cement Reference
Sample No. 85.According to the Certificate of Analysis, the SRM 1C had a loss on
ignition of 39.9 %. For the purpose of the cooperative test series, the loss on
X2.3 Cooperative Test Results ignition was assumed to be CO 2  only.
B 
The Base Cement was CCRL Portland Cement Reference Sample No. 85.
X2.3.1   Tables X2.1 and X2.2 list results from two series of  C 
The Determined % Added CO2  was obtained by subtracting the Base Cement
cooperative tests using several of the analytical methods % CO 2  from the Unknown % CO  2  .
D 
evaluated by the Task Group. In all, five of the six methods The addition of 4.00 % NIST SRM 1C (with a loss on ignition value of 39.9 %)
would provide 1.60 % Added CO  2  . (Again, it was assumed that the SRM 1C loss
receiving favorable ratings were included. The sixth method, on ignition was only carbon dioxide.)
Test Methods  C 25, was specifically not tested in these coop- E 
The XRF instrument was calibrated using standards composed of the Base
erative series, but was rated favorably because of long history Cement (that is, CCRL No. 85) and NIST SRM 1C. It was assumed that the Base
Cement contained 0 % CO 2  .
of use with related materials.
X2.3.2   Table X2.1 includes results of single determinations
using three of the different analytical methods. The methods X2.3.3   Table X2.2  includes results based on average of 
used were Split Loss on Ignition, Test Methods  E 350, and three determinations. Results from four of the different ana-
Combustion by Induction Furnace with Infra-Red Detection. lytical methods are included. Methods used were Split Loss on

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C 114 – 07
Ignition, X-Ray Fluorescence Analysis, Induction furnace with
Infra-Red Detection, and Thermo-Gravimetric Analysis. Test
Methods E 350 was not used in this series of tests.

For additional useful information on details of cement test methods, reference may be made to the “Manual of Cement Testing,”
which appears in Vol 04.01 of the  Annual Book of ASTM Standards.

SUMMARY OF CHANGES

Committee C01 has identified the location of selected changes to these test methods since the last issue,
C 114 – 06 1, that may impact the use of these test methods. (Approved July 15, 2007)
e

(1) Revised 3.3.2.4. (3) Editorially corrected the equation at the bottom of the table
(2) Revised 19.1. Added new  Note 64 and renumbered subse- in  Appendix X1.
quent notes.

Committee C01 has identified the location of selected changes to these test methods since the last issue,
C 114 – 05, that may impact the use of these test methods. (Approved November 1, 2006)

(1) Revised X2.2.1.

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