International Journal of Materials Science and Applications
Volume 6, Issue 2, March 2017, Pages: 83-87

X Ray and Inductively Coupled Plasma Atomic Emission Spectroscopy Analysis of Cristallographic Structure And Composition of Pavement Based Clay Materials

Hilaire Elenga1, *, Timothée Nsongo1, Bernard Mabiala2, David Bilembi2, Ferland Ngoro Elenga1, Balla Diop Ngom3, Aboubaker Chedikh Beye3

1Faculty of Sciences and Technics, University of Marien NGOUABI, Brazzaville, Congo

2Laboratory of Mechanic, Energy and Engineering, National Polytechnic School, University of Marien GOUABI, Brazzaville, Congo

3Department of Physic, Faculty of Sciences and Technologies, University of Cheikh Anta Diop of Dakar, Dakar, Senegal

Email address:

(H. Elenga)
(B. D. Ngom)

*Corresponding authors

To cite this article:

Hilaire Elenga, Timothée Nsongo, Bernard Mabiala, David Bilembi, Ferland Ngoro Elenga, Balla Diop Ngom, Aboubaker Chedikh Beye. X Ray and Inductively Coupled Plasma Atomic Emission Spectroscopy Analysis of Cristallographic Structure And Composition of Pavement Based Clay Materials. International Journal of Materials Science and Applications. Vol. 6, No. 2, 2017, pp. 83-87. doi: 10.11648/j.ijmsa.20170602.13

Received: December 29, 2016; Accepted: January 12, 2017; Published: February 10, 2017

Abstract: In order to predicttechnological properties of local clay based materials mixed to wood waste and to prevent human health andenvironment, experimental mineral structure and composition study were conducted. The influence of wood waste on the structural properties of clay samples were also investigated. Non and stabilized clay sample at 4% of cement were made at different conditions and waste wood at different content have been incorporated. Mineralogical X-ray analysis was carried out using X- raydiffractometer with Geiger counter usingcobalt Kα radiationwith wavelength l=1,789 Å. inductively coupled plasma atomic emission spectroscopy (ICP/AES) and inductively coupled plasma optical emission spectroscopy (ICP/OES) were used respectively to determine major, Minor and trace elements. The results showed that incorporation of wood waste has a strong effect on the crystallographic structure, making partially amorphous clay structure. It is found that the waste wood incorporating influence the lattice constants of the components of the clay and must be correlated to acid interaction. Chemical analysis of clay sample indicates kaolinite and SiO2 as a dominant clay minerals. The results has shown some trace and heavy metal contamination for human and environment.

Keywords: Clay, Cement, Waste, Wood, Mineral Structure, Structure, Lattice Parameter, X-ray Diffraction

1. Introduction

With the development of the wood industry, the abundance of waste wood generate an important environment pollution. A wide range of studies has been reported to recycle wood waste in clay materials in order to improve technological properties [1, 2, 4]. Most of studies focused on mechanical properties and have shown that the addition of wood waste in clay considerably reduced the mechanical strength of the materials [5], [6], [7], [8], [9]. Knowledge of the composition and structural properties of clays mixed with wood waste remains unclear. Most of the research work has been done in order to make bricks [4, 6, 8, 9], pavements [16, 17], to study the influence of wood waste on acoustic and magnetic properties [15] or mechanical resistance of bricks or geotechnical structures [6, 8, 9]. There are very few studies in the literature related to the structural properties of clay materials with wood waste incorporating. The results of the study of the structure of clays mixed with wood waste have scientific interest for understanding the physical phenomena observed in the behavior of clay based structures but also to explore new technological applications. To understand the obtained results, chemical analysis should be associated with this study.

Knowledge of the microscopic properties such as structure and composition of clay materials used in construction may have technological interest [3], [10]. This work studies the composition of the clay and the influence of waste wood on the structure in order to improve technological properties

2. Apparatus and Experimental Conditions

A diffractometerautomated X type Siemens D5000 equipped with a cobalt anticathode was used the K of cobalt with .10-10m wavelength. The diffracted rays following the Bragg angle was recorded by a counter type GEIGER MULLER. This counter is placed in order to receive the rays diffracted by the sample in terms. The BRAGG law

2dhklsin=was used to determine the inter-reticular distances. The crystal lattice can be deduced from the expressions (6) and (7). The scanning angle varied between 4 to 84°2, the scanning speed was about 0.02°2/second.

2.1. X Ray Mineral Powder Analysis

For carrying out the analyzes, the samples were previously dried and ground into powder particle size less than 80 mm. The counting time for this test was about 5 seconds when the sample was turning from 4 to 84°2θ. The crystallized fraction of the samples was determined by X-ray diffractometry from their powder diffractogram. This technique is mainly qualitative and can only give a semi quantitative result. The detection limit is about 5% and can vary widely depending on the nature of the different phases.

2.2. X ray Mineral Analysis Using Oriented Blade

The counting time for this test was about 2 seconds in the rotating sample from 4 to 36°2θ.

The phylliteuse fraction of the samples was determined by diffraction from normal oriented blades glycollées for 12 hours in steam pressure and heated up to 490°C for 4 hours. The composing proportions were estimated from peak areas

2.3. Method of Identifying Crystal Phases

Generally the identification of a crystallized phase is made by comparison of the experimental with the theoretical diffractogram. The content of mineral components is estimated from peak areas.

Match 2 software FotoMix!, XRD2DScan were used to analyze the diffraction patterns.

The crystal lattice of α quartz is hexagonal. The values of the lattice constants are obtained after indexing peaks using the expression linking to the interplanar spacing dhkl.

Kaolinite crystallizes in the triclinic system.

Montmorillonite crystallizes in the monoclinic system

Chlorite also crystallizes in the monoclinic system.

2.4. Spectroscopy Analysis

Inductively coupled plasma atomic emission spectroscopy (ICP/AES) and inductively coupled plasma optical emission spectroscopy (ICP/OES) were used respectively to determine major, minor and trace elements. The ICP-MS X7 and ICP OES Icap 6500 equipment was used with the following:

RF power ~1200 W, Plasma argon gas ~ 15 l min-1), Auxiliary gas ~ 0.4 l min-1), Sample gas ~ 0.9 l min-1), Dwell time ~100 ms.

3. Results and Discussion

3.1. X Ray Analysis of Clay Sample

3.1.1. Raw Clay Sample Structure

The X ray pattern of analyzed clay sample before incorporating wood waste are shown in the figure 1.

Figure 1. X- ray pattern of raw clay sample.

The results reveals the presence of kaolinite with formula Al2H4Si2O9 and quartz, formula SiO2 in raw clay sample.

Estimates of the concentrations of mineral components obtained using the method of "Peak-height ratio" is as follows:

Quartz alpha: 51%;

Kaolinite: 43%.

interstratifiedmontmorillonite/chlorite: 6%

3.1.2. Clay Sample at 4% Content of Cement After Acajou Waste Wood Incorporation

The phases identified are: alpha quartz (Q), formula SiO2; kaolinite, formula

Al 2 (Si2O5)(OH)4; traces of calcite of formula CaCO3 and anatase of formula TiO2. Traces of calcite and anatase are due to the presence of the cement used to stabilize the mixture clay- soil-cement-woodchips

Quartz alpha: 58%;

Kaolinite: 24%;

Some traces of anatase: 8.88% and calcite: 8.31%.

By comparing the concentrations of mineral components of the crude clay and clay after incorporation of wood waste, we find that:

The concentration of SiO2 (quartz) in the crude clay (51%) is weaker than that with the clay after incorporating of mahogany wood waste (58%). Chemical reactions between clay and cement with high levels (pozzolanic reactions) form of new products that contribute to the strength of a cement stabilized earth [Akpodje 1985]; [Bell 1996].

Clay paved samples were analyzed by X-ray, after incorporating wood waste. The obtained results are shown in Figure 2.

The results showed that incorporation of wood waste has a strong effect on the crystallographic structure, making partially amorphous clay structure.

Figure 2. X Ray pattern after wood waste of limba incorporation.

3.2. Determination of Lattice Constants of Clay Components

Experimental lattice constants before and after waste wood incorporation was measured using dhkl, the results are summarized in the table 3

Table 1. Theoretical experimental lattice constants before and after waste wood incorporation.

  Quartz α Kaolinite
  Before incorporating waste After incorporating waste Before incorporating waste After incorporating waste

Experimental lattice constants

a=b=4,92 a=b=5,52 a=5,14 a=5,59
c=5,66 c=5,68 b=8,86 b=9,68
    c=7,50 c=7,31

Theoretical lattice constants

a=b=4,91 a=b=4,91 a=5,13 a=5,13
c=5,40 c=5,40 b=8,89 b=8,89
    c=7,25 c = 7,25

For the parameters a and b, the resulting values are identical to the results achieved by [12] in the case of α quartz, kaolinite and montmorillonite. There is no change on a and c lattice constant of chlorite conversely to lattice parameter a, c of quartz, kaolinite and montmorillonite. So then we can say that there has been an expansion of the crystal lattice; while in the case of chlorite this variation is observed in the parameter b, in this case we see a compression which results in a reduction of the volume of the crystal lattice.

A very little change of the experimental lattice constant was observed both for quartz and kaolinite. These results is in agreement with those obtained by [13] and are discussed as interactions of heavy metals cations with kaolinite could affect the structure of kaolinite.

"a" and "b" lattice constants were found to be high after waster wood incorporating. It was found [4] that waste wood incorporating in clay make it highly acidic, according. Dorothy Carroll et al [14] have shown that the acid attach has an influence in clay structure. The lattice constant expansion must be interpreted in acid reaction.

3.3. Composition Determination of Clay Sample

Chemical composition was determined by spectroscopy following the procedure NF P94-048.

The results obtained are summarized in the tables 2 and 3.

The results indicated the presence of SiO2, Al2O3 and Fe2O3 as major oxides.

And some traces of MnO, MgO, CaO, Na2O, K2O, TiO2, P2O5 in the form of impurities.

Table 2. Values of traceelements.

As Ba Be Bi Cd Ce Co Cr
ppm ppm ppm ppm ppm ppm ppm ppm
0,8007 117,1714 0,7561 0,2981 0,0743 40,2884 4,26 70,5524
Cs Cu Dy Er Eu Ga Gd Ge
ppm ppm ppm ppm ppm ppm ppm ppm
3,3022 11,9149 1,8503 0,9722 0,6891 35,7462 2,1793 2,1976
Hf Ho In La Lu Mo Nb Nd
ppm ppm ppm ppm ppm ppm ppm ppm
7,1513 0,3574 0,0476 28,9338 0,1652 1,4584 18,1847 16,9186
Ni Pb Pr Rb Sc Sb Sm Sn
ppm ppm ppm ppm ppm ppm ppm ppm
22,3332 18,9889 4,9762 15,2104 10,3 0,1421 2,9101 2,4378
Sr Ta Tb Th Tm U V W
ppm ppm ppm ppm ppm ppm ppm ppm
33,4639 1,6413 0,3112 6,7255 0,146 2,1038 74,7965 2,4262
Y Yb Zn c
ppm ppm ppm ppm
8,6069 1,0443 56,3158 269,7383

Fourty four trace elements were determinated using ICP/AES, the obtained results are in agreement with those published by Jean Carignan et al. [11]. Among all these impurities, Heavy metals such Sb, Cr, Cu, Pb, Zn Co and Ni has found to be toxic for human and environment [12].

The table 3 show the analysis results of major and minor elements, most of them like ceramics are very useful for industry applications.

Table 3. Values of major and minor constituents.

Eléments chimiques SiO2 Al2O3 Fe2O3 MnO MgO CaO Na2O K2O TiO2 P2O5 PF Total
  % % % % % % % % % % % %
  55,22 25,91 2,90 < L.D. 0,20 0,09 < L.D. 0,31 1,27 < L.D. 13,90 99,80

These results can be discussed according the experimental lattice constant values and can affect clay properties after waste wood incorporating. Recently the research work of SOUMIKA MBAYA [15] has shown the incorporation of waste wood in clay increase the magnetic induction. The determination of the trace element must have a correlation with magnetic properties.

4. Conclusion

At the end of this study, these conclusions can be drawn: Makoua clay consists of the following minerals unevenly distributed: the quartz α, kaolinite, and interstratified chlorite/ montmorillonite which crystallize respectively in the hexagonal, triclinic and monoclinic system.

In this study, we have determined the mineralogical structure of the Makoua clay and the lattice constant of the components of this clay using the mineralogical analysis by X-ray powder and oriented blades.

The results showed that incorporation of wood waste has a strong effect on the crystallographic structure, making partially amorphous clay structure. It is found that the lattice constants increase of quartz and kaolinite after waste wood incorporating must be correlated to the acid interaction.

Chemical analysis of clay sample indicates kaolinite and SiO2 as predominant component.

Some trace and heavy contamination has been identified to be toxic for some industry activities.


The authors would like to express their gratitude to Research Center of Geological and Mining Research for the financial support of the project.


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