**Author details**

Rafael Vasconcelos Oliveira and Valfredo Azevedo Lemos *Universidade Estadual do Sudoeste da Bahia, Laboratório de Química Analítica (LQA), Campus de Jequié, Jequié, Bahia, Brazil* 

#### **5. References**

276 Polyurethane

Cd

Pb

\* µg g-1.

**4. Conclusion** 

laboratory.

**Author details** 

Rafael Vasconcelos Oliveira and Valfredo Azevedo Lemos

*Laboratório de Química Analítica (LQA), Campus de Jequié, Jequié, Bahia, Brazil* 

*Universidade Estadual do Sudoeste da Bahia,* 

**Element Process of extraction Enrichment**

Solid phase extraction

Ionic liquid dispersive

liquid–liquid microextraction

Cd Dispersive liquid-liquid

**factor** 

Pb 35 1.0 14.0

**Limit of detection (�g L-1)** 

30 0.8 9.0

Pb Solid phase extraction 2.1 ----- Yalcinkaya et al, 2011)

microextraction 55 0.4 ----- (Rojas et al., 2011)

Cd Solid phase extraction 19 0.77 ----- (Tang & Hu, 2011)

Cd Ion-flotation Separation 45 1.2 ----- (Tavallali et al., 2011)

Cd Cloud point extraction 29 0.1\* ----- (Moghimi & Tajodini,

Pb Cloud point extraction 56 and 42 1.14 ----- (Shah *et al.*, 2011)

Pb Solid phase extraction 50 0.65 ----- (Melek et al., 2006)

**Table 4.** Analytical characteristics of various procedures for the determination of Cd and Pb by FAAS,

The PUF grafted with Me-BTAP was successfully applied to the preconcentration of cadmium and lead. The sorbent showed characteristics that are desirable for materials used in solid phase extraction systems, such as resistance to swelling and changes in pH, low resistance to flow passage and simplicity in preparation. Moreover, when applied to the preconcentration system, the solid phase provided a simple and sensitive method for the determination of cadmium and lead by FAAS. The synthesized material is a good alternative for the determination of these elements. The extraction of other elements will be tested using this sorbent, and further work in this area is currently being conducted in our

**Sample volume (mL)** 

40 1.5 20.0 (Soylak & Yilmaz,

2011)

2010)

**Reference** 

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**Chapter 13** 

© 2012 El-Shahawi et al., licensee InTech. This is an open access chapter distributed under the terms of the Creative Commons Attribution License (http://creativecommons.org/licenses/by/3.0), which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

© 2012 El-Shahawi et al., licensee InTech. This is a paper distributed under the terms of the Creative Commons Attribution License (http://creativecommons.org/licenses/by/3.0), which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

**Fast, Selective Removal and Determination of** 

**Total Bismuth (III) and (V) in Water by Procaine** 

**Hydrochloride Immobilized Polyurethane Foam** 

Bismuth is found in nature in trivalent state as bismuthinite, Bi2S3, bismite, Bi2O3 and bismuth sulfide- telluric, Bi2Te2S. It is also found as a secondary component in some lead, copper and tin minerals [1]. Bismuth (V) compounds do not exist in solution and are important in the view of pharmaceutical analytical chemistry [1]. In the Earth's crust, bismuth presents at trace concentration (8 μg Kg-1) while, bismuth minerals rarely occur alone and are almost associated with other ores [2]. Bismuth appears to be environmentally significant because its physical and chemical properties have led it to be used in different areas of life. Pamphlett et al, 2000 [3] have reported that, bismuth compounds after oral intake enter the nervous system of mice, in particular, in motor neurons [3]. Hence, bismuth

The development of selective, separation, pre-concentration and determination method for bismuth at sub-micro levels is a challenging problem because of its extremely low concentrations in natural samples and of its strong interference from the sample matrices. Several methods e.g. hydride generation atomic absorption spectrometry [4], electro thermal atomic absorption spectrometry [5], atomic fluorescence spectrometry [6], hydride generation atomic absorption spectrometry [7], and cathotic and anodic adsorptive stripping voltammetry [8 - 10] have been reported for bismuth determination. Most of these methods require preconcentration of bismuth for precise determination because most analytical

**Packed Column Prior to Inductively Coupled** 

**Plasma – Optical Emission Spectrometry** 

M.S. El-Shahawi, A.A. Al-Sibaai, H.M. Al-Saidi and E.A. Assirey

Additional information is available at the end of the chapter

species are included in the list of potential toxins [3].

techniques do not possess adequate sensitivity for direct determination.

http://dx.doi.org/10.5772/47962

**1. Introduction** 


**Fast, Selective Removal and Determination of Total Bismuth (III) and (V) in Water by Procaine Hydrochloride Immobilized Polyurethane Foam Packed Column Prior to Inductively Coupled Plasma – Optical Emission Spectrometry** 

M.S. El-Shahawi, A.A. Al-Sibaai, H.M. Al-Saidi and E.A. Assirey

Additional information is available at the end of the chapter

http://dx.doi.org/10.5772/47962

**1. Introduction** 

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FAAS. *Current Analytical Chemistry*, Vol.7, No.3, p.p.225-234.

gold(III). *Microchimica Acta*, Vol.174, No.3-4, p.p.391-398.

Bismuth is found in nature in trivalent state as bismuthinite, Bi2S3, bismite, Bi2O3 and bismuth sulfide- telluric, Bi2Te2S. It is also found as a secondary component in some lead, copper and tin minerals [1]. Bismuth (V) compounds do not exist in solution and are important in the view of pharmaceutical analytical chemistry [1]. In the Earth's crust, bismuth presents at trace concentration (8 μg Kg-1) while, bismuth minerals rarely occur alone and are almost associated with other ores [2]. Bismuth appears to be environmentally significant because its physical and chemical properties have led it to be used in different areas of life. Pamphlett et al, 2000 [3] have reported that, bismuth compounds after oral intake enter the nervous system of mice, in particular, in motor neurons [3]. Hence, bismuth species are included in the list of potential toxins [3].

The development of selective, separation, pre-concentration and determination method for bismuth at sub-micro levels is a challenging problem because of its extremely low concentrations in natural samples and of its strong interference from the sample matrices. Several methods e.g. hydride generation atomic absorption spectrometry [4], electro thermal atomic absorption spectrometry [5], atomic fluorescence spectrometry [6], hydride generation atomic absorption spectrometry [7], and cathotic and anodic adsorptive stripping voltammetry [8 - 10] have been reported for bismuth determination. Most of these methods require preconcentration of bismuth for precise determination because most analytical techniques do not possess adequate sensitivity for direct determination.

© 2012 El-Shahawi et al., licensee InTech. This is an open access chapter distributed under the terms of the Creative Commons Attribution License (http://creativecommons.org/licenses/by/3.0), which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. © 2012 El-Shahawi et al., licensee InTech. This is a paper distributed under the terms of the Creative Commons Attribution License (http://creativecommons.org/licenses/by/3.0), which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

Solvent extraction in the presence of co-extractant ligands e.g. bis (2, 4, 4-trimethyl pentyl) monothiophosphinic acid [11], pyrolidine dithocarbamate [12] etc has received considerable attention. However, these methods are too expensive, suffer from the use of large volumes of toxic organic solvents, and time-consuming. Thus, recent years have seen considerable attention on preconcentration and/ or monitoring of trace and ultra trace concentrations of bismuth by low cost procedures in a variety of samples e.g. fresh, marine and industrial wastewater [13]. Solid phase extraction (SPE) techniques have provided excellent alternative approach to liquid – liquid extraction for bismuth preconcentration prior to analyte determination step [14 -18].

Polyurethane foams (PUFs) sorbent represent an excellent solid sorbent material due to their high available surface area, cellular and membrane structure and extremely low cost [19]. Thus, several liquid solid separation involving PUFs methods have been employed successfully for separation and sensitive determination of trace and ultra trace levels of metal ions including bismuth (III) [19-29]. The membrane like structure and the available surface area of the PUFs make it a suitable stationary phase and a column filling material [25, 27]. Thus, the main objectives of the present chapter are focused on: i. developing of a low cost method for the removal of bismuth(III) and (V) species after reduction of the latter to tri valence state employing PUFs impregnated PQ+.Cl- ; ii. Studying the kinetics, and thermodynamic characteristics of bismuth (ІІІ) sorption by trioctylamine plasticized PQ+.Cltreated PUFs and finally iii. Application of the developed method in packed column for complete removal and / or determination of bismuth (III &V) species in wastewater by PQ+.Cl treated PUFs sorbent.
