Indo. J. Chem., 2009, 9 (2), 184 - 188 Paulina Taba 184 * Corresponding author. Email address : ultita@yahoo.com.au FTIR AND NMR STUDIES OF ADSORBED TRITON X-114 IN MCM-41 MATERIALS Paulina Taba Department of Chemistry, Hasanuddin University Jl. Perintis Kemerdekaan Km 10 Tamalanrea, Makassar, South Sulawesi, Indonesia 90245 Received February 26, 2009; Accepted May 12, 2009 ABSTRACT One source of water pollutions is caused by the high use of surface-active agents (surfactants) by industries and households. As a consequence, it is required to remove such substances from the environment One of the important and widely used methods for removal of substances from solution is adsorption. In this research, MCM-41 and its modification MCM41-TMCS were used to adsorb nonionic surfactant, Triton X-114. FTIR and NMR methods were used to study the interaction between the surfactants and the adsorbents. MCM-41 was synthesized hydrothermally at 100 o C and its modification was conducted by silylation of MCM-41 with trimethylchloro silane (MCM41-TMCS). Both unmodified and modified MCM-41 can adsorb the surfactant. The amount adsorbed in the unmodified material is higher than that in the modified one. The interaction of Triton X-114 with MCM-41 was hydrogen bonding between the silanol groups in MCM-41 and hydroxyl groups of Triton X-114. For modified samples, Triton X-114 interacted with alkylsilyl groups mostly through hydrophobic interaction. It is more likely that the interaction was through C12, C13, C26 and C27 of Triton X-114. Keywords: FTIR, NMR, adsorbed Triton X-114, MCM-41 materials INTRODUCTION The widespread use of surfactants in industries as well as at home is producing an important environmental impact, especially in aquatic media. As a consequence, it is required to remove such substances from the environment. Non-ionic surfactants, such as Triton X- 114, have found widespread use in several domestic and industrial applications such as cleaning, personal care, crop protection, paint and coating, textile finishing, emulsion stabilization, food and leather processing, and ore refining. One of the largest applications of these surfactants is in petroleum industries where they find use in the operations involving foams, emulsions and liquid– solid operations such as stabilization of fine particles and sludge displacement [1]. It is well known that surfactants with ramified hydrocarbon chains show high resistance to biodegradation in aqueous media, leading to the formation of long-standing foams. Several days or weeks are required for the complete biodecomposition of surfactants, which often leads to the formation of persistent and even toxic metabolites. Adsorption is one of the important and widely used methods for removal of substances including surfactants from solution. It has been reported that activated carbon and graphite [2,3], unmodified and modified silica [4], silica gel [5,6], mica [7], clays [8], polymers [9-12], and modified zeolite [13] have all previously been used as adsorbents for the removal of surfactants from aqueous environments. Mesoporous materials, such as mesoporous silica with diameters of 2 to 50 nm, show high promise to be used as adsorbents for such organic materials because of their high porosity and their large surface areas. One example of mesoporous silica is MCM-41, discovered in 1992 by Mobil Corporation [14,15]. In this research, adsorption of nonionic surfactant (Triton X-114) in MCM-41 and its modification will be discussed. The molecular structure of the surfactant is given as follows: The amount of surfactants adsorbed was measured from the carbon content of the adsorbent following adsorption. 13 C CP MAS NMR and FTIR spectroscopy was used to study the mechanism of interaction between the surfactant and mesoporous materials. The method used for adsorption of the surfactant in mesoporous materials was the stirring method, which has been described in detail elsewhere [16], in aqueous solutions for periods of 5 hours. EXPERIMENTAL SECTION A hydrothermal method was used to synthesize MCM-41 as described in elsewhere [17] and trimethylchloro silane (TMCS) were used as reagents for silylation of MCM-41 using the procedure of [18] with some modification to produce MCM41-TMCS. Hydrostability of MCM-41 was tested by making use of a Siemens D500 diffractometer using CuK ( = 1.5412 Å) as a radiation source. For in-situ