Presenter: Safwan Darwish El-Far Laboratory Supervisor / Chemist Qatar National Cement Company

Introduction: All of the calculation used for modules and mix design is based on the oxides obtained from the chemical analysis of the samples; great care must be taken for sampling to have the most representative sample.

What is sampling? Sampling is the process to collect a representative & sufficient quantity of material (sample) to be analyzed. Generally there are two types of samples

Spot sample

Representative sample

Spot sample: samples that is collected at a certain moment or the portion taken from the collected material (i.e. un-homogenized). Representative sample: samples that represent the full quantity or a full period of time. In both cases the sample can be collected manually or automatically, but representative sample is our aim.

Once the representative sample is guaranteed, accurate & precise analysis must also be ensured before necessary corrective actions.

Result Sample Material

Its a sequence: Material, Sample, Analysis & action

There are three possibilities:

Wrong sample + correct analysis = wrong action Correct sample + wrong analysis = wrong action Correct sample + correct analysis = right action

Representative Manual samples

Following are the common manual samples, in cement industry
Quarry samples: bore holes samples during survey/before blasting. Crusher samples: during stacking the piles. Clinker samples: after cooler crusher from the pan conveyer. Cyclone # 5 sample. By Pass sample. Electrostatic precipitator sample. Conditioning tower sample.

For the first three samples sufficient quantity including all the particle sizes shall be crushed, quartered & grinded to ensure the sampling accuracy. For the last four samples sufficient quantity must be collected many times but no need for quartering or grinding, as its a fine powder.

Representative auto samples:

Common automatic sample is cement industry Are auto samples always representative?

Raw Mill: including raw mill output & returned dust.

Kiln feed: from homo silo output

Well, all the automatically collected samples from the chute are shown below in the following chart:

Cement

From the chart the sample pass though the screw to the mixer then portion of mixed samples is transported to the lab via sample carrier. The mixer filling should be according to the sampling intervals: The collection of the sample must be continuous to ensure representative auto sampling.
Chute

Air slide

Mixer

Sample carrier

Screw

Qualitative

Sample analysis:
To identify the sample contents, acidic (carbonate, sulfate etc) & Basic (Ca, Mg, Na etc).
Qualitative

Quantitative
Sample Analysis

Determine the percentage of the identified contents. The quantitative analysis is based on the knowledge of the sample contents from the qualitative analysis.

Quantitative

Based on Geology the chemical composition of raw materials is identified: Limestone - mainly CaCO3. Clay - mainly SiO2, Al2O3 & Fe2O3. Bauxite - mainly Al2O3 Hematite - mainly Fe2O3 So according to this knowledge the quantitative analysis is performed directly.

There are different methods to perform the quantitative analysis

Complexometri c.

Gravimetric.

Potentiometric.

Spectroscopy

Flame photometer Spectrometer X-Ray Gamma rays IR & UV

The common method of analysis in cement industry is by using the X-Ray florescence. What is X-Ray? Its electromagnetic wave, having high energy, high frequency & low wavelength. When these waves strike the atom of the element transferring its energy to the inner electron leading to a vacancy in the internal shell, so electron from the upper shell migrate to the lower shell and giving the orbital energy difference as florescence.

There is a unique florescence for each element, as we can measure the intensity of the florescence for each element individually the concentration can be quantified according to the florescence intensity.

To achieve the best accurate results separate calibrations of different material are advised to avoid the wide range calibration line.
The wide range calibration line could lead to more errors in the lower or higher concentrations of the elements.

For raw material: Based in major component ((When ever major component increase the other component decrease.) Limestone CaCO3 43~55 %
(CaO)

Clay-shale SiO2 30~44 %

Iron ore Fe2O3 80~99 %

For Raw Meal

The range is similar to limestone but differs in SiO2, Al2O3 & Fe2O3. For clinker & Cement the concentration jump up due to burning.

The sample preparation

For raw meal the pressed pellets preparation is faster and also accurate method, but for clinker & cement its better to use fused bead method so as to avoid the crystal effect on the analysis The calibration standard preparation method must be the same, which should be used for routine samples. The calibration must be checked time to time to ensure the accuracy.

Conclusion: The calculations & actions related to the production process are based on both sampling & analysis. Great care must be given for both so as to take right actions during operation.