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Hydration Behaviour and Infrared Spectroscopy of Pre-treatments Effect on Portland Cement-Eremospatha macrocarpa and Laccosperma secundiflorum Systems



O.O. Adefisan, J.S. Fabiyi and A.G. McDonald
 
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ABSTRACT

The effects of cold water extraction, incorporation of calcium chloride (CaCl2) and aluminium sulphate (Al2(SO4)3) on the setting time (tmax), maximum hydration temperature (Tmax), time ratio (tR) and surface chemistry of Eremospatha macrocarpa and Laccosperma secundiflorum particles mixed with Portland cement was investigated. The mixtures were placed in thermally sealed thermos flasks for 24 h after which tmax, Tmax and tR were measured. The tmax, Tmax and tR were 12.4 and 11.9 h, 59.1 and 58.3°C, 1.1 and 1.1, respectively for untreated E. macrocarpa and L. secundiflorum and ranged from 5.2 to 10.7 h, 57.7 to 83.7°C and 0.5 to 0.9, respectively when treated with cold water and chemical additives. Cold water extraction and chemical additives significantly improved the hydration parameters of rattan-cement system. CaCl2 performed better as a chemical accelerator than Al2(SO4)3 while L. secundiflorum inhibited cement setting more than E. macrocarpa. Infrared spectroscopy showed that incorporation of CaCl2 to L. secundiflorum particles helped expose cellulose to advance participation thereby enlarging its surface area for interpenetration networking with cement.

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O.O. Adefisan, J.S. Fabiyi and A.G. McDonald, 2012. Hydration Behaviour and Infrared Spectroscopy of Pre-treatments Effect on Portland Cement-Eremospatha macrocarpa and Laccosperma secundiflorum Systems. Journal of Applied Sciences, 12: 254-262.

DOI: 10.3923/jas.2012.254.262

URL: https://scialert.net/abstract/?doi=jas.2012.254.262
 
Received: November 25, 2011; Accepted: January 06, 2012; Published: February 22, 2012



INTRODUCTION

Production of Cement Bonded Boards (CBB) from untreated fibrous raw materials is faced with the problem of inhibitory effects of sugars, extractives and lignin in lignocellulosic materials (Moslemi and Lim, 1984; Hong and Lee, 1986). The disadvantages of inhibition include delayed setting, relatively lowered hydration temperature and prolonged time to attain maximum temperature (Moslemi and Lim, 1984). Addition of an accelerator into a mixture of cement-water paste could enhance the speed of hydration process to occur earlier (Nazerian et al., 2011). Several attempts have been made to overcome this challenge using cold or hot water extraction and/or incorporation of chemical additives such as calcium chloride (CaCl2), aluminium sulphate (Al2(SO4)3), magnesium chloride (MgCl2) prior CBB production (Hong and Lee, 1986; Olorunnisola, 2007). The chemical additives are usually added in quantity of less than 4% (by cement weight) and have been found to enhance many of the boards’ properties such as increased density, improved appearance, bending and compressive strength, dimensional stability and improved wood-cement bond due to its effect of accelerating the hydration of wood-cement mixtures (Olorunnisola, 2007). CaCl2 is the most commonly used among various available chemical additives. It accelerates the hydration of cement particularly the tri-calcium silicate phase (C3S), reduces the setting time and in some cases increases the maximum hydration temperature (Biblis and Lo, 1968; Moslemi et al., 1983; Lee and Short, 1989; Ramachandran, 1994; Olorunnisola and Adefisan, 2002). It improves the bending strength and dimensional stability attributable to increased board density and improved bonding between particles of lignocellulosics and cement (Badejo, 1989; Fabiyi, 2004; Olorunnisola, 2006). The internal bonding and direct screw withdrawal increased by 166 and 67%, respectively with the addition of CaCl2 to coconut cement boards while those of density were 64 and 45%, respectively (Almwdia et al., 2002).

However, CaCl2 may not be effective in overcoming severe inhibitions of cement hydration due to heartwood polyphenols of some certain wood species. Compounds that can accelerate cement hydration and also chelate or chemically modify polyphenols are more effective than CaCl2 at improving the cement compatibility of inhibitory wood species (Semple and Evans, 2000). Semple and Evans (2000) found that although CaCl2 performed well as an accelerator in the presence of wood-wool of Acacia mangium wood, it was not as effective as other compounds like tin chloride (SnCl4), aluminium chloride (AlCl3) and sodium silicate (Na2O.3SiO3). This finding suggests that different lignocellulosics depending on their constituent would react differently when incorporated in cement mixes. Therefore, it is important to understand the effect of various chemical additives on different lignocellulosic fibres sources for making CBB.

In Nigeria, several studies have been conducted on the hydration of rattan canes (Dahunsi, 2000; Olorunnisola and Adefisan, 2002; Olorunnisola, 2005; Adefisan and Olorunnisola, 2007; Olorunnisola, 2007). The reason for this is because rattans have short rotation and can be harvested in less than seven years after planting and processed with simple and relatively cheap technology. Also, the assembly line from rattan harvesting to CBB production involves low capital investment (Olorunnisola and Adefisan, 2002; Olorunnisola, 2005; Olorunnisola, 2008). There are three major rattan species namely: Eremospatha macrocarpa, Laccosperma secundiflorum and Calamus deerratus that are found in Nigeria (Dahunsi, 2000). Adefisan (1999) reported that E. macrocarpa has diameter of 10-17 mm and stem length of 20-25 mm while L. secundiflorum has diameter of 10-20 mm and stem length of 10 mm. The sugar contents of both species differed with L. secundiflorum having the highest carbohydrate content (over 70%) which may cause it to have the highest probability of inhibiting cement hydration (Dahunsi, 2000).

These rattan species respond to pre-treatments differently. Olorunnisola and Adefisan (2008) reported that hot water extraction improved the compatibility of the C. deerratus while L. secundiflorum was more amenable to cold water extraction. Hot water extraction of C. deerratus cement mix had higher hydration temperature and lower setting time than those soaked in cold water. However, cold water extraction resulted in higher hydration temperature and lower setting time in the L. secundiflorum cement mix than hot water (Olorunnisola and Adefisan, 2008). Unfortunately, most of the hydration studies conducted on rattan canes by several researchers have centred on L. secundiflorum and C. deerratus while it is rare to find information on E. macrocarpa. Since both E. macrocarpa and L. secundiflorum are widely spread and common in Nigeria, it is very important to investigate the hydration behaviour of both rattan species under same laboratory conditions and experimental procedures. This step would enhance comparative analysis of hydration behaviour between both species. Apart from the traditional chemical pre-treatments that have been used so far, there is no available information on the use of Al2(SO4)3 as chemical additive in relation to rattan canes.

The use of infrared spectroscopy to monitor the chemical structure of different polymers is widely explored. Its versatility is due to the fact that it requires minimum sample preparation, not tedious and not time consuming. However, its use for monitoring the changes that occur when cement, lignocellulosic fibres and chemical additives are mixed together is limited in literature. This study therefore aimed at investigating the effects of cold water extraction and incorporation of CaCl2 and Al2(SO4)3 on the hydration behaviour and infrared spectroscopy of E. macrocarpa and L. secundiflorum mixed portland cement.

MATERIALS AND METHODS

Matured stems of E. macrocarpa and L. secundiflorum canes were harvested from Gambari Forest Reserve located between longitude 50°44' E and latitude 7°14’ N in Ibadan, Oyo state, Nigeria. The canes were converted into billets of about 6 cm and hammer milled. The milled particles were sieved using a set of 1.18, 0.85 and 0.60 mm sieves. Particles that passed through the 0.85 mm sieve and were retained in the 0.60 mm sieve were collected and dried to 10% moisture content. These particles were divided into four sets with the first set mixed with cement but no additive incorporation (henceforth called untreated), the second set was soaked in distilled water for 30 min at room temperature, drained and dried to 10% moisture content (henceforth referred to as cold water treated), the third set pre-treated with CaCl2 and the fourth set pre-treated with Al2(SO4)3 before mixed with cement.

Hydration test: For the hydration tests, 15 g of the E. macrocarpa or L. secundiflorum particles, 200 g of Portland cement (purchased at a local hardware store, Moscow, Idaho state, USA) and 93 ml of distilled water were mixed in a polyethylene bag to form homogeneous slurry following the method developed by Adefisan and Olorunnisola (2007). The neat cement was mixed with 90 mL of distilled water while 3% CaCl2 or Al2(SO4)3 (by cement weight) was added.

Table 1: Cement compatibility assessment schemes
Image for - Hydration Behaviour and Infrared Spectroscopy of Pre-treatments Effect on Portland Cement-Eremospatha macrocarpa and Laccosperma secundiflorum Systems

However, untreated and 30 min cold water extracted samples were mixed with the neat cement and 90 mL of distilled water only prior hydration characterisation. Hydration characterisation was performed in a set of well insulated thermos flasks. The temperature rise was monitored for 24 h using thermocouples (J-type) connected to an 8-channel datalogger (USB TC-08, Pico Technology). Three sampled specimens of each mixture were prepared. The compatibility of E. macrocarpa and L. secundiflorum with cement was assessed using the compatibility indices (Table 1).

Chemical characterization: Specimens for the chemical analysis were obtained from each of the untreated and pre-treated rattan/cement mixes and ground into fine powder using pestle and mortar. Fourier Transform Infrared (FTIR) spectra were measured directly from the powder (1% w/w basis) thoroughly dispersed in KBr (99% w/w basis). Spectra were recorded using a Thermo Scientific Nicolet 8700 spectrometer equipped with a DTGS detector. Each spectrum was taken as an average of 64 scans at a resolution of 4 cm-1.

RESULTS AND DISCUSSION

Setting time of rattan-cement composites: The results of the hydration tests are presented in Table 2 and Fig. 1. The setting times of the E. macrocarpa and L. secundiflorum cement mixes without pre-treatment were 12.4 and 11.9 h, respectively. Based on the classification of Hofstrand et al. (1984), the untreated E. macrocarpa and L. secundiflorum were very suitable for Cement Bonded Board (CBB) production. Generally, the incorporation of chemical additives and 30 min cold water extraction of the two fibrous materials resulted in reduced setting time that ranged from 5.2 to 9.4 and 5.6 to 10.7 for the E. macrocarpa and L. secundiflorum cement composites, respectively. In addition, the setting time for 30 min. cold water extraction and 3% Al2(SO4)3 were very similar for the two rattan species (Table 2). The greatest improvement in the setting time was observed for rattan/cement/water mix treated with CaCl2.

Rattan species (E. macrocarpa and L. secundiflorum) did not significantly affect the setting times of the rattan/cement/water mix but incorporation of different chemical additives significantly influenced the setting time of the rattan/cement/water mix (Table 3). CaCl2 significantly reduced the setting time of the rattan/cement/water mix than Al2(SO4)3. Olorunnisola (2008) reported the setting time of 10.3 h for 30 min cold water extracted L. secundiflorum (sieved) mixed with cement. This is agreement with 10.7 h obtained in this study for same condition (Table 2).

Maximum hydration temperature of the rattan-cement composites: The maximum hydration temperatures (Tmax) attained by the untreated E. macrocarpa and L. secundiflorum cement mixes were 59.1 and 58.3°C (Table 2). The Tmax for CaCl2, Al2(SO4)3 and 30 min cold water extraction pre-treated E. macrocarpa/cement mix were 83.7, 60.4 and 65.1°C, respectively. In addition, Tmax for CaCl2, Al2(SO4)3 and 30 min cold water extraction pre-treated L. secundiflorum/cement mix were 78.6, 57.7 and 63.3°C, respectively (Table 2). Based on the Sandermann and Kohler (1964) index, the untreated E. macrocarpa and L. secundiflorum could be classified as intermediately suitable for the production of CBB. The chemical pre-treated E. macrocarpa and L. secundiflorum could be classified as suitable except the Al2(SO4)3 pre-treated L. secundiflorum which ranked as intermediately suitable for the production of CBB. Hence, the addition of chemical additives significantly improved the Tmax of the rattan/cement mixes with those treated with CaCl2 having highest maximum hydration temperature than those pre-treated with Al2(SO4)3 and 30 min cold water extraction.

In addition, E. macrocarpa/cement mix had higher Tmax than L. secundiflorum/cement mix. This indicates that CaCl2 was more effective than Al2(SO4)3 or 30 min water extraction in minimising the inhibitory effects of sugars and extractives present in the rattan/cement mixtures. The practical implication of this study is that the use of Al2(SO4)3 to pre-treat E. macrocarpa or L. secundiflorum is not economical since 30 min water extraction gave the same Tmax; hence cold water extraction is preferred because water is readily available and affordable. In addition, L. secundiflorum particles however inhibited cement setting more than E. macrocarpa particles. Higher sugar contents in the L. secundiflorum canes may contribute to its low Tmax.

Image for - Hydration Behaviour and Infrared Spectroscopy of Pre-treatments Effect on Portland Cement-Eremospatha macrocarpa and Laccosperma secundiflorum Systems
Fig. 1: Hydration behaviour of Eremospatha macrocarpa and Laccosperma secundiflorum/cement mixes

Table 2: Hydration parameters of Eremospatha macrocarpa and Laccosperma secundiflorum/cement mixes
Image for - Hydration Behaviour and Infrared Spectroscopy of Pre-treatments Effect on Portland Cement-Eremospatha macrocarpa and Laccosperma secundiflorum Systems
Means with the same letters in the same column for each of the rattan species are not statistically different

Table 3: Duncan’s multiple range tests of the effects of pre-treatment and rattan species on the hydration parameters of rattan/cement mixes.
Image for - Hydration Behaviour and Infrared Spectroscopy of Pre-treatments Effect on Portland Cement-Eremospatha macrocarpa and Laccosperma secundiflorum Systems
Means with the same letters in the same column for either pre-treatment or rattan species are not statistically different

Olorunnisola (2008) reported that the maximum hydration temperature of 30 min cold water extracted L. secundiflorum (sieved) mixed with cement was 51°C. This is contrary to 63.3°C obtained in this study for same condition (Table 2). This contradiction may be due to differences in the sources of Portland cement used. Olorunnisola (2008) used Portland cement produced in Nigeria while Portland cement used in the present study was purchased at a local hardware store, Moscow, Idaho state, USA. The study conducted by Olorunnisola (2008) ranked 30 min cold water extracted L. secundiflorum as intermediately suitable while the present study conducted at Idaho ranked it suitable for CBB production.

The choice of any of these two rattan species (without pre-treatment) did not significantly affect the Tmax of the rattan/cement mixes. However, the application of chemical additives significantly influenced the maximum hydration temperatures of the E. macrocarpa and L. secundiflorum/cement mixes (Table 3). This implies that different chemical additives had different effects on the hydration behaviour of the rattan/cement mixes.

Time ratio indices of the rattan-cement composites: The time ratio indices (tR) of the rattan/cement mixes are presented in Table 2. The time ratio indices for both untreated rattan species cement mixes were the same (1.1). Similarly, the tR for CaCl2 pre-treated E. macrocarpa/cement mix and L. secundiflorum/cement mix were the same (0.5). The tR for Al2(SO4)3 and 30 min cold water were 0.9 and 0.9-1.0, respectively for pre-treated E. macrocarpa/cement mix and L. secundiflorum/cement mix. Therefore, pre-treating either of the two rattan species with CaCl2, Al2(SO4)3 or 30 min cold water extraction did not make any difference, hence tR is not rattan species dependent but chemical additive dependent.

Image for - Hydration Behaviour and Infrared Spectroscopy of Pre-treatments Effect on Portland Cement-Eremospatha macrocarpa and Laccosperma secundiflorum Systems
Fig. 2: FTIR spectra of two rattan species: Eremospatha macrocarpa and Laccosperma secundiflorum. Each spectrum is an average of spectra from two specimens

Based on the classification of Olorunnisola (2008), the untreated rattans are suitable for CBB production. The incorporation of chemical additives significantly improved the tR of the rattan/cement mixes. The greatest improvement was observed for rattan/cement mixes pre-treated with CaCl2 (Table 3). Therefore, it suggests that CaCl2 improved the compatibility of the rattan/cement mixes more than Al2(SO4)3 or 30 min cold water extraction.

Olorunnisola et al. (2005) reported that incorporation of 3% CaCl2 to L. secundiflorum-cement system gave setting time and maximum hydration temperature as 9 h and 53.3°C, respectively. Their data showed that only the setting time support the suitability of 3% CaCl2 pre-treated L. secundiflorum-cement system but the present study show that both the setting time and maximum hydration temperature ranked 3% CaCl2 pre-treated L. secundiflorum-cement system as suitable for CBB production. The compatibility ranking of fibrous material based on the time ratio index shows 30 min cold water extracted L. secundiflorum is suitable for CBB production. Hence, the present study and the report of Olorunnisola (2008) support this finding.

Chemical characterisation: Figure 2 shows the FTIR spectra of E. macrocarpa and L. secundiflorum without cement. Infrared bands observed in the various treatments with their peak assignments and structural polymers are presented in Table 4 and 5. There are similarities and a few dissimilarities in the positions and intensities of the infrared spectra of the two rattan species investigated. Peaks numbered 2, 6, 8, 10, 14, 15, 17 and 20 have the same band frequencies for both E. macrocarpa and L. secundiflorum (Table 4, 5). However, the band frequencies for peaks numbered 3, 4, 11, 12, 13, 17, 18, 21, 23, 24 and 25 for E. macrocarpa differed from that of L. secundiflorum. Majorly, the carbonyl band for xylan differed by 3 cm-1 with E. macrocarpa occurring at 1737 cm-1 and L. secundiflorum at 1734 cm-1.

The lignin assigned peak for E. macrocarpa and L. secundiflorum occurred around 1506/1608 cm-1. However, some peaks occurred at higher frequency for E. macrocarpa than L. secundiflorum. Examples of these are peaks at 698, 1113, 1162, 1463 and 3412 cm-1 for E. macrocarpa compared with L. secundiflorum at 695, 1110, 1161, 1457 and 3407 cm-1. The band at 3540-3000 cm-1 which was assigned to O-H groups in the rattans emerged due to the combination of cellulose, hemicelluloses and lignin (Faix, 1992). This band is broader with higher intensity for L. secundiflorum than E. macrocarpa. Likewise the intensities for peaks numbers 10, 11, 12, 13, 15, 17, 19 and 20 are higher for L. secundiflorum than E. macrocarpa. Generally, there is no difference in the chemical functional groups that were present in both rattan species.

Table 4: Summary of infrared bands observed in Eremospatha macrocarpa and the untreated and pre-treated E. macrocarpa/cement mixes. The wavenumber of the 30 min cold water extraction is not presented because they are similar to that of Al2(SO4)3
Image for - Hydration Behaviour and Infrared Spectroscopy of Pre-treatments Effect on Portland Cement-Eremospatha macrocarpa and Laccosperma secundiflorum Systems

Table 5: Summary of infrared bands observed in Laccosperma secundiflorum and the untreated and pre-treated L. secundiflorum/cement mixes. The wavenumber of the 30 min cold water extraction is not presented because they are similar to that of Al2(SO4)3
Image for - Hydration Behaviour and Infrared Spectroscopy of Pre-treatments Effect on Portland Cement-Eremospatha macrocarpa and Laccosperma secundiflorum Systems

Therefore, the peak intensity, band width and b and frequency from the spectra can only be used to differentiate the two rattan species under investigation.

Chemical changes that occurred due to the blending of untreated, 30 min cold water extracted, Al2(SO4)3 or CaCl2 pre-treated E. macrocarpa or L. secundiflorum mixed with cement after the hydration testing had been terminated are illustrated in Fig. 3 and 4. The addition of Portland cement caused the appearance of some peaks in the spectra (numbers 1, 5, 7, 22 and 26).

Image for - Hydration Behaviour and Infrared Spectroscopy of Pre-treatments Effect on Portland Cement-Eremospatha macrocarpa and Laccosperma secundiflorum Systems
Fig. 3: FTIR spectra of (A) Eremospatha macrocarpa, (B) E. macrocarpa/cement mix, (C) E. macrocarpa/cement/CaCl2, (D) E. macrocarpa/cement/Al2(SO4)3 and (E) E. macrocarpa/cement/30 min cold water extraction. Each spectrum is an average of spectra from two specimens. Peak position and assignment as well as structural polymer for each peak are presented in Table 1

Image for - Hydration Behaviour and Infrared Spectroscopy of Pre-treatments Effect on Portland Cement-Eremospatha macrocarpa and Laccosperma secundiflorum Systems
Fig. 4: FTIR spectra of (A) Laccosperma secundiflorum, (B) L. secundiflorum/cement mix, (C) L. secundiflorum/ cement/CaCl2, (D) L. secundiflorum/cement/ Al2(SO4)3 and E) L. secundiflorum/cement/30 min cold water extraction. Each spectrum is an average of spectra from two specimens. Peak position and assignment as well as structural

The formation of the band at 3643 cm-1 in the untreated, 30 min cold water extracted and chemically treated rattan/cement mixes remained unchanged; indicating that its emergence is due to the chemical constituent of cement. It was due to the metal-bonded hydroxide (Mollah et al., 1992). This indicates the OH band from Ca(OH)2. The band at 3407/3414 cm-1 which was assigned to O-H groups in lignocellulosic materials, was affected by the pre-treatment and incorporation of cement to the rattan species. The blending of the rattan particles with cement and the incorporation of chemical additives and 30 min cold water extraction caused the band to be become narrower than in the ordinary rattan particles. In addition, peaks 23 and 24 at 2853 and 2926-2918 cm-1, respectively drastically decreased due to the addition of cement. This implies that the cement suppressed the methylene and methyl stretching frequencies that occurred in the rattan species.

The lignin assigned peaks (1506/1507 and 1608/1609 cm-1) did not appear in the rattan/cement mix but were masked due to the presence of broader band with peaks at 1426 and 1457 cm-1. In addition, the peak at 1047 cm-1 disappeared when cement was mixed with rattan particles. There were many bands that disappeared due to the addition of cement namely: peaks numbers 21, 15, 14, 13 and 6 which are xylan in hemicelluloses, cellulose, syringyl, guaiacyl and arabinogalactan, respectively (Table 4, 5). Addition of CaCl2 to L. secundiflorum particles helped expose cellulose to advance participation probably by enlarging its surface area for interpenetration networking with cement. Chemical reactivity of this peak (number 17) is rattan species dependent. The region between 1750 and 750 cm-1 was drastically affected (reduced the peaks’ intensities) by the incorporation of CaCl2 while Al2(SO4)3 and 30 min cold water extraction had little effect on this region for E. macrocarpa. However, 30 min cold water extraction drastically reduced the peaks’ intensities in the region between 1510 and 1300 cm-1 for L. secundiflorum.

CONCLUSIONS

The effects of cold water extraction and chemical additives on the setting time (tmax), maximum hydration temperature (Tmax), time ratio (tR) and surface chemistry of Eremospatha macrocarpa and Laccosperma secundiflorum particles mixed with Portland cement was investigated. Hydration behaviour showed that E. macrocarpa and L. secundiflorum canes are suitable for CBB production based on its setting time and time ratio index. However, maximum hydration temperature only ranked E. macrocarpa and L. secundiflorum as intermediately suitable. Cold water extraction (for 30 min) and chemical additives improved the hydration behaviour of the rattan cement mixes. Calcium chloride was a better chemical accelerator for the rattan cement mixes than aluminium sulphate. Cold water extraction had little advantage over aluminium sulphate for the species. L. secundiflorum inhibited cement setting more than E. macrocarpa. The surface chemistry studied using infrared spectroscopy showed that addition of cement to rattan fibre caused the suppression of methylene and methyl stretching frequencies that occurred in the rattan species. Addition of CaCl2 to L. secundiflorum particles helped expose cellulose to advance participation probably by enlarging its surface area for interpenetration networking with cement.

ACKNOWLEDGMENT

This study was conducted at the Forest Products Laboratory, University of Idaho, Moscow, USA with a grant received from John D. and Catherine T. MacArthur Foundation through University of Ibadan, Nigeria. The support is acknowledged with thanks.

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