ASTM C-114 Qualification for Cement Analysis

Cement industries, including various other factories that manufacture products from raw materials, are expected to meet extremely rigorous quality standards. Changes that occur during the fabrication process can influence the physical properties of the final products.

The maximum quality of the final product can be ensured with standards that are available that guarantee minimal differences in the analytical process.

What is ASTM C-114?

This standard is dedicated to the analysis of hydraulic cement. It provides limit values to conform to, ensuring that the analytical process is completely monitored and produces minimal variations in results.

Reference test methods that are ideal for individual elements of interest during the analysis of cement are suggested by this standard. A ''rapid test method'' can be used if the difference in results complies to the limitation projected by this norm.

This ''rapid test method'' refers to any method that has the potential to determine the analyte concentration that meets the ASTM C-114 validation requirements. This is the possibility of using fusion as a rapid test method if the resulting differences are found to be below the allowed values specified by ASTM C-114 for the suitable elements.

It is important to validate the method with certified reference materials (CRMs) provided by National Institute of Standard and Technology (NIST) as indicated in the ASTM C-114 standard.

Given below are seven Portland cement CRMs that have all the target elements essential for this study. The NIST website offers a list of the certified values.

  • SRM1880b
  • SRM1881a
  • SRM1884b
  • SRM1888b
  • SRM1889a
  • SRM 1886a
  • SRM1887b

ASTM C-114 accreditation for cement analysis

Figure 1. ASTM C-114 accreditation for cement analysis

Sample Preparation

Seven CRM C-114 standards were used to describe the performance of the rapid test method by fusion using the Katanax K2 Prime* six-position fusion fluxer.

NIST provided the CRMs, which served as Portland cement samples. They consist of varied concentrations of elements in a particular range, based on the typical composition of Portland cement.

A CRM sample weighing 0.8 g was mixed with 30 mg of LiBr as a non- wetting agent and 7 g of flux 50/50 Lithium Tetraborate/Lithium Metaborate (LiT/LiM) to create beads of 32 mm in diameter.

A Sartorius weighting cell WZ224-N with a precision of ±0.1 mg was used to weigh the components. A secondary container was used, where all of the products were mixed together and then shifted into a platinum crucible.

The applied parameters are shown in Table 1.

Table 1. Method used on the Katanax K2 Prime* fluxer

STEP TEMPERATURE TIME RAMP OF TEMPERATURE CRUCIBLE MIXING AMPLITUDE CRUCIBLE MIXING SPEED
1 1050°C 0:00 Fast 0%
2 1050°C 0:00 Fast 0%
3 1050°C 4:00 Fast 20° 90%
4 1050°C 6:00 Fast 25° 5%
Pouring 120° 50%
1 1:00 120° 80%
2 5:00 90° 80%

The XRF analysis was performed by an independent mineral laboratory (Corem). A WDXRF spectrometer with a scintillation detector, multi crystals (LiF, Ge) and an Rh X-ray tube of 2.4 kW was used by the laboratory.

It is necessary to run seven standards in duplicate on two different days in order to meet the ASTM C-114 requirements. The average of those duplicates helps to determine the accuracy results.

The values need to achieve the ASTM C-114 limits in terms of accuracy and precision for all of the elements that need to be analyzed by XRF.

Table 2. lists the allowed values provided by ASTM in terms of accuracy and precision for each target element in the analysis of Portland cement. Table 2 also shows the results derived for the standards used to perform the test.

The average of all the standard materials are listed based on the accuracy and precision of the related element. Annex 1 shows the details of the results of each standard (Table 3).

Table 2. ASTM C-114 limits compared to the results of the CRMs samples by fusion (percentage values)

Elements ASTM C-114 limits Average of the seven standards by fusion
Precision Accuracy Precision Accuracy
SiO2 0.16 0.2 0.047 0.054
Al2O3 0.2 0.2 0.038 0.059
Fe2O3 0.1 0.1 0.036 0.046
CaO 0.2 0.3 0.089 0.163
MgO 0.16 0.2 0.009 0.019
SO3 0.1 0.1 0.077 0.032
Na2O 0.03 0.05 0.014 0.006
K2O 0.03 0.05 0.008 0.018
TiO2 0.02 0.03 0.005 0.003
P2O5 0.03 0.03 0.002 0.008
ZnO 0.03 0.03 0.002 0.002
Mn2O3 0.03 0.03 0.003 0.011

Table 3. Precision and accuracy results for the seven CRMs used for the accreditation

Element Limits SRM1880b SRM1881a SRM1884b SRM1886a SRM 1887b SRM1888b SRM 1889a
Precision Accuracy Precision Accuracy Precision Accuracy Precision Accuracy Precision Accuracy Precision Accuracy Precision Accuracy Precision Accuracy
SiO2 0,16 0,2 0,08 0 0,002 0,06 0,04 0,02 0,05 0,02 0,01 0,04 0,12 0,13 0,03 0,11
AI2O3 0,2 0,2 0 0,09 0,003 0,07 0,07 0,04 0,11 0,1 0,001 0,03 0,004 0,08 0,08 0,00008
Fe2O3 0,1 0,1 0,01 0,03 0,004 0,08 0,02 0,01 0,0002 0,05 0,001 0,05 0,2** 0,08 0,02 0,02
CaO 0,2 0,3 0,02 0,17 0,09 0,16 0,16 0,22 0,05 0,23 0,06 0,14 0,14 0,18 0,1 0,04
MgO 0,16 0,2 0,016 0,02 0,004 0,01 0,0008 0,02 0,02 0,002 0,01 0,03 0,006 0,02 0,005 0,03
SO3 0,1 0,1 0,05 0,02 0,18 0,02 0,09 0,001 0,04 0,05 0,09 0,06 0,05 0,01 0,04 0,06
Na2O 0,03 0,05 0,01 0,005 0,02 0,001 0,01 0,0007 0,01 0,02 0,04 0,01 0,01 0,0002 0,001 0,007
K2O 0,03 0,05 0,008 0,02 0,01 0,05 0,003 0,007 0,01 0,003 0,01 0,01 0,01 0,005 0,004 0,03
TiO2 0,02 0,03 0 0,003 0,0003 0,004 0,002 0,003 0,01 0,008 0,0004 0,001 0,01 0,004 0,01 0,0003
P2O5 0,03 0,03 0 0,01 0,0006 0,02 0,0006 0,006 0,00007 0,002 0,01 0,008 0,00008 0,002 0,0006 0,009
ZnO 0,03 0,03 0 0,0005 0,0002 0,001 0 0,004 0 0,001 0,01 0,0005 0,00003 0,002 0 0,005
Mn2O3 0,03 0,03 0,001 0,02 0,0004 0,01 0,01 0,009 0 0,007 0,00001 0,005 0,00006 0,004 0,009 0,02
Cl 0,003 NA 0* 0,02 0* NA 0* 0,007 0* 0,004 0* 0,01 0* 0,01 0* 0,002
Final results - > Passed Passed Passed Passed Passed Passed Passed

Passed
Failed (but remain under twice permissible value, so acceptable)
* Detection limit of the instrumentation is over the value of chlorine in the sample.
** At least six of the seven CRM are within the prescribed limits for iron, so acceptable (according to ASTM-C114 requirement)

All of the results exist within the limits projected by ASTM C-114. This points out that the rapid test method using fusion with the Katanax K2 Prime* fluxer fulfills the ASTM C-114 requirements.

Katanax X-600 X-Fluxer

Figure 2. Katanax X-600 X-Fluxer

Conclusion

ASTM C-114 requirements are considered to be a standard measure of performance. It is possible to validate the ASTM C-114 method by using fusion, and in this case the data reveals that the Katanax fusion fluxer fulfills these requirements.

The Katanax fusion instrument can be used as a part of an analytical technique that meets the ASTM C-114 accreditation. The analysis of the beads was provided by an independent laboratory that also fulfilled the demands for C-114 analysis.

The use of fusion with the Katanax K2 Prime* instrument will help in successfully yielding accurate and precise results.

*The Katanax K2 Prime has now been replaced by the X-600 shown in figure 2

This information has been sourced, reviewed and adapted from materials provided by SPEX SamplePrep.

For more information on this source, please visit SPEX SamplePrep.

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