Examples for adsorption of environmental pollutants on carbon nanotubes.
\\n\\n
Released this past November, the list is based on data collected from the Web of Science and highlights some of the world’s most influential scientific minds by naming the researchers whose publications over the previous decade have included a high number of Highly Cited Papers placing them among the top 1% most-cited.
\\n\\nWe wish to congratulate all of the researchers named and especially our authors on this amazing accomplishment! We are happy and proud to share in their success!
\\n"}]',published:!0,mainMedia:null},components:[{type:"htmlEditorComponent",content:'IntechOpen is proud to announce that 179 of our authors have made the Clarivate™ Highly Cited Researchers List for 2020, ranking them among the top 1% most-cited.
\n\nThroughout the years, the list has named a total of 252 IntechOpen authors as Highly Cited. Of those researchers, 69 have been featured on the list multiple times.
\n\n\n\nReleased this past November, the list is based on data collected from the Web of Science and highlights some of the world’s most influential scientific minds by naming the researchers whose publications over the previous decade have included a high number of Highly Cited Papers placing them among the top 1% most-cited.
\n\nWe wish to congratulate all of the researchers named and especially our authors on this amazing accomplishment! We are happy and proud to share in their success!
\n'}],latestNews:[{slug:"intechopen-authors-included-in-the-highly-cited-researchers-list-for-2020-20210121",title:"IntechOpen Authors Included in the Highly Cited Researchers List for 2020"},{slug:"intechopen-maintains-position-as-the-world-s-largest-oa-book-publisher-20201218",title:"IntechOpen Maintains Position as the World’s Largest OA Book Publisher"},{slug:"all-intechopen-books-available-on-perlego-20201215",title:"All IntechOpen Books Available on Perlego"},{slug:"oiv-awards-recognizes-intechopen-s-editors-20201127",title:"OIV Awards Recognizes IntechOpen's Editors"},{slug:"intechopen-joins-crossref-s-initiative-for-open-abstracts-i4oa-to-boost-the-discovery-of-research-20201005",title:"IntechOpen joins Crossref's Initiative for Open Abstracts (I4OA) to Boost the Discovery of Research"},{slug:"intechopen-hits-milestone-5-000-open-access-books-published-20200908",title:"IntechOpen hits milestone: 5,000 Open Access books published!"},{slug:"intechopen-books-hosted-on-the-mathworks-book-program-20200819",title:"IntechOpen Books Hosted on the MathWorks Book Program"},{slug:"intechopen-s-chapter-awarded-the-guenther-von-pannewitz-preis-2020-20200715",title:"IntechOpen's Chapter Awarded the Günther-von-Pannewitz-Preis 2020"}]},book:{item:{type:"book",id:"2224",leadTitle:null,fullTitle:"New Advances in Vehicular Technology and Automotive Engineering",title:"New Advances in Vehicular Technology and Automotive Engineering",subtitle:null,reviewType:"peer-reviewed",abstract:"An automobile was seen as a simple accessory of luxury in the early years of the past century. However, in the present days it's undeniable the amount of technology and human effort applied by the vehicular industry for developing high?quality vehicles, but still, cheap for the common person. In this context, this book tries not only to fill a gap by presenting new and updated subjects related to the vehicular technology and to the automotive engineering but also to provide guidelines for future research. This book is a result of many valuable contributions from worldwide experts of automotive's field. The amount and type of contributions were judiciously selected to cover as possible the widest range of research. 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He graduated in 1993 and received his MSc degree in 2002, both in Electrical Engineering from the University of Porto, Porto, Portugal. In 2011 he also obtained the graduation recognition in Electrical Engineering from the Federal University of Pernambuco (UFPE), Recife, Brazil. In 2007, he obtained the PhD degree in Industrial Electronics from the University of Minho, Guimarães, Portugal. His PhD thesis was on RF transceivers for integration in microsystems to be used in wireless sensors network applications.\nFrom 1999 to 2008 he was a Lecturer at Polytechnic Institute of Braganca. Since 2008, he is a Principal Rearcher at the University of Minho, where he is involved in the research on optical and microwave metamaterials, micro/nanofabrication technologies for mixed-mode/RF systems, solid state integrated sensors, microactuators, micro/nanodevices for wireless and biomedical applications, and milimetric-THz wave-systems.\nDoctor Carmo is also a Member of the IEEE Industrial Electronics Society. Also, he performs regular reviewes on these publications: Optics & Laser Technology, Microelectronics Journal, Journal of Sensors and Actuators A, IEEE Sensors Journal, IEEE Transactions on Industrial Electronics, Journal of Measurement Science and Technology, Journal of Physiological Measurement, among many more not listed. 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Solid phase extraction (SPE) is an effective sample handling method and is used as an enrichment technique when low concentrations of analytes need to be determined. SPE provides higher enrichment efficiency and requires a lower volume of solvent than the traditional method of liquid-liquid extraction.In addition, SPE is simpler and easily to be automated and operated.In the procedure of SPE, the type of sorbent, its structure and its interactions with the solute play an important role in obtaining higher enrichment efficiency of analytes. Until now, several kinds of materials such as C18, Oasis HLB, bonded silica, styrenedivinyl-benzen (SDB), zeolites, carbonaceous materials have been proposed as adsorbents for SPE cartridge.
\n\t\t\tIn recent years, carbon nanotubes (CNTs), a novel member in the carbon family, have attracted great attention due to its advantages that can be used for many different applications in terms of its chemical, electronic and mechanical properties as well as the unique tubular structures and large length / diameter ratio. CNTs are to be considered as a sheet of graphite that has been rolled into a tube and be classified as single – walled carbon nanotubes (SWCNTs) and multiwalled carbon nanotubes (MWCNTs). Over the past 20 years, CNTs have been exploited in analytical and other fields such as biosensors with immobilized biomolecules, electrochemical detectors, gas sensor, catalyst supports and so on. Because CNTs surfaces have a strong interaction with other molecules, particularly with those containing benzene rings, they possess excellent adsorption ability and substitute active carbon. CNTs as SPE adsorbents has been investigated to extract organic compounds such as pesticides (carbofuran, iprobenfos, parathion-methyl, prometryn, fenitrothion etc.), polycyclic aromatic hydrocarbons, antibiotics, sulphonylurea herbicides, sulfonamides, phthalate esters, endocrine disruptors, triazines, microcystines, pyrethroids and polybrominated diphenyl ethers. In several comparative studies CNTs exhibit similar or higher adsorption capacity for environmental pollutants than silica-based sorbents or macroporous resins. CNTs can also preconcentrate volatile organic compounds.CNTs were used as SPE adsorbents for preconcentration of metal ions, such as copper, nichel, cobalt, vanadium, silver, cadmium, rare earth elements etc.
\n\t\t\tThis chapter is organized in four sections including the introduction. Section 2 is devoted to the sorption properties of CNTs. Section 3 summarize the most important applications of CNTs for the enrichment of environmental pollutants.The potential factors affecting SPE and the sorption capacities of CNTs are also disscussed. The whole chapter is then concluded in Section 4.
\n\t\tCNTs usually have a diameter in the range comprized within a tenth to tens nanometers and a length of up to centimeters. The ends of CNTs are normally capped by a fullerene-like structure. As fullerene, CNTs also exhibit limited solubility. Depending on their diameter and helicity of the graphitic sheets CNTs can be either metallic or semi-conducting (Valcarcel et al., 2008). The characteristic structures of carbon nanotubes allow a strong interaction with organic molecules via non-covalent forces, such as hydrogen bonding, π -π stacking, electrostatic forces, van der Waals forces and hydrophobic interactions (Pyrzynska et al., 2008). The presence of functionalized carbon nanotubes allows the possibility of incorporating one or more of these interactions which increase the selectivity and the stability of the system.
\n\t\t\tIt was stated that CNT derivatization is required when developing special applications (e.g. retention of metals). CNTs were purified by sodium hypochlorite solutions and were employed as adsorbents to study the adsorption characteristics of zinc in water (Lu & Chiu, 2006). The properties of CNTs such as purity, structure and nature of the surface were considerably improved after purification by sodium hypochlorite which made CNTs become more hydrophilic and suitable for adsorption of Zn2+ from water. The adsorption of Zn2+ onto CNTs rises proportional to the pH increase within 1- 8 range, fluctuates very slight and reaches a maximum in the pH range of 8-11; the adsorption curve decreases at a pH of 12. The contact times to reach equilibrium are 60 min for SWCNTs and MWCNTs. The maximum adsorption capacities of Zn2+ calculated by the Langmuir model are 43.66 and 32.68 mg / g with SWCNT and MWCNT, respectively, at an initial Zn2+ concentration range of 10-80 mg/ L.
\n\t\t\tIt was found that the acid treatment with a mixture of nitric acid and sulfuric acid made CNTs become more hydrophilic and suitable for adsorption of low molecular weight and relatively polar trihalomethanes (THMs) in water (Lu et al., 2005). The adsorption of THMs onto CNTs can be suitably described by both Langmuir and Freundlich models. The smallest molecule CHCl3 is the most preferentially adsorbed onto CNTs, followed by CHBrCl2, CHBr2Cl and then by CHBr3. THMs absorption onto CNTs fluctuates very slightly in the pH range of 3 –7 but decreases with pH value when pH exceeds 7.
\n\t\t\tIt was shown that carbon nanotubes can also be used as supports for adsorption materials, and the new composites have a good affinity to many metals. MWCNTs filled with Fe2O3 nanoparticles have been prepared and employed as adsorbent for the magnetic separation of dye contaminants (Methylene Blue and Neutral Red) in water (Qu et al., 2008). The magnetic nanoparticles have been prepared via hydrothermal reaction of shortened MWCNTs in ferric nitrate solution and subsequent calcinations. The prepared magnetic MWCNTs can be well dispersed in water and easily magnetic separated from the medium after adsorption. As compared with other adsorbents, the magnetic nanoparticles not only have high adsorption efficiency to dyes, but can also be easily manipulated by external magnetic field.
\n\t\t\tMWCNT / iron oxide magnetic composites were prepared and used for adsorptions of Ni (II) and Sr (II) (Chen et al., 2009). Scan electronic microscopy (SEM) image shows an entangled network of MWCNTs with clusters of iron oxides attached to them suggesting the formation of MWCNTs / iron oxide magnetic composites. Ni (II) adsorption on the magnetic nanoparticles is pH and ionic strength dependent and can be easily desorbed from the magnetic nanoparticles by adjusting the solution pH values.The Langmuir model fitted the adsorption isotherm data of Ni (II) better than the Freundlich model.
\n\t\t\tMnO2 / CNTs composites were efficient for Pb (II) ion removal from aqueous solution (Wang et al., 2007b). The optimum MnO2 loading indicating the best performance of Mn O2 on the Pb(II) removal is 30 wt %.The application to experimental results of the Langmuir and Freundlich models show that the Langmuir model gives a better correlation coefficient.
\n\t\t\tIt was found that CNTs present a marked tendency to aggregation, which negatively affects adsorption by reducing their active surface (Valcarcel et al., 2008). In addition, when cartridges or home-made columns are employed, this tendency may increase pressure in the flow systems.
\n\t\t\tSpecial configurations are developed for specific applications. A complex sheet of SWCNT and polyaniline was used as a new adsorbent to remove bilirubin from plasma (Ando et al., 2009). Bilirubin, a red- brown bile pigment, is a metabolite of heme produced from the senescent hemoglobin. If a bilirubin concentration exceeds a certain level in blood, it may cause kernicterus or liver diseases. Bilirubin CNTs adsorption capacity has been found to be much higher versus the conventional materials because of their large surface area and considerable adsorption capability for polycyclic compound molecules due to their structure similar to graphite.
\n\t\t\tA recently introduced immobilization method to link the aminoacid L-tyrosine to CNTs was described (Pacheco et al., 2009). The amount of aminoacid immobilized on CNTs surface was 3174 μmol / g. The material was tested for Co retention using a minicolumn inserted in a flow system. A 10 % (v/v) HNO3 solution was chosen as eluent. The pH study revealed that Co binding increased at elevated pH values. The retention capacity was compared to other bivalent cations and showed the following tendency : Cu2+> Ni2+> Zn2+>> Co2+.
\n\t\t\tThe influence of the surface functionalization on the colloidal stability of CNTs, as well as on the sorption of heavy metals was investigated (Schierz & Zanker, 2009). Uranium (VI), a chemical element of considerable public concern, was chosen as an example of a toxic heavy metal. The results indicated that acid treatment increases the amount of acidic surface groups on the CNTs. Acid treatment has an intensifying effect upon the colloidal stability of the CNTs, and on their adsorption capacity for U (VI).
\n\t\t\tThe analytical potential of MWCNTs modified with a Schiff base ligand was examined for simultaneous preconcentration of Au (III) and Mn (II) in aqueous samples prior to their flame atomic adsorption spectrometric assessment (Shamspur & Mostavafi, 2009). It was found that the sorption is quantitative in the pH range 5.0- 7.5, whereas quantitative desorption occurs instantaneously with 4.0 mL of 0.1 mol / L Na2S2O3.
\n\t\t\tThe application of the hemimicelle capped carbon nanotubes–based nanosized SPE adsorbents in environmental analysis is reported for the first time using arsenic as model target (Li et al., 2009a). The end functionalized of CNTs can introduce oxygen-containing negatively functional groups such as – COOH, - OH, or - C= O on their surface site. If cationic surfactant, such as cetyltrimethylammonium chloride (CTAC) was added to the functionalized CNTs, interactions like hydrophobic and ionic may lead to the formation of hemimicelle / admicelle aggregates on the CNTs ; this way, a new kind of adsorbents is acquired, namely hemimicelle capped CMMWCNTs. Arsenic can be quantitatively retained on the hemimicelle capped CMMWCNT at pH 5 – 6 from sample volume up to 500 mL, and subsequently eluted completely with 2 mol/ L HNO3 in the presence of 10 mg / L CTAC.
\n\t\t\tCarbon nanotubes have also been proposed as material coatings in SPME fibers for the determination of flame retardants like polybrominated diphenyl ethers (PBDEs) in environmental and food samples (Wang et al., 2006a). The home-made fibers, which were prepared according to the method used for constructing composite electrodes, were evaluated quantitatively and compared with commercial fibers. The results demonstrated that the MWCNT coating was effective for extracting the analytes described above, and provided better enhancement factors than activated carbon and poly (5 % dibenzene- 95 % dimethylsiloxane) coatings.
\n\t\tMost CNT applications published have been developed for the extraction of water samples, which are probably the less complex samples to work with. Up to now, only few works have used CNTs (basically MWCNTs) for the extraction of environmental pollutants from matrices different than waters.
\n\t\t\tSome reprezentative examples of the use of carbon nanostructures as sorbent materials in SPE and solid phase microextraction (SPME) are given in Table 1 for an easier approach and comparison.
\n\t\t\tCarfentrazone-ethyl (a relatively novel triazolinone herbicide) residue in water was enriched by use of MWCNTs (Dong et al., 2009a). Relevant studies were developed to examine several factors affecting the recovery of the analyte, for example the pH of the water samples, sample volume, polarity and volume of eluents. It was found that MWCNT was an effective SPE adsorbent for preconcentration of carfentrazone-ethyl in water and the recovery of this herbicide from fortified water was 81.49-91.08 %.The detection limits and quantification were 0.01 and 0.03 μg / L. It was also shown that under the optimized SPE procedure, the MWCNT-packed cartridge needed only 100 mg adsorbent.
\n\t\t\tThe extraction efficiency of MWCNT as a new SPE adsorbent followed by GC-ECD for the analysis of chloroacetanilide herbicides (alachlor, acetochlor, metolachlor and butalochlor) was investigated (Dong et al. 2009b). It was found that the amount of adsorbent was much less for MWCNT in comparison with the commonly used adsorbent, such as C18. As an example, in this method were used only 100 mg MWCNT, whereas for the environmental analysis routine work were applied 500 mg to 1000 mg C18 cartridges. The detection limits were situated within the range of 0.01-0.03 μg / L.
\n\t\t\tThe adsorptive potential of MWCNTs was used for the extraction and clean up of eight pesticides in agricultural, ornamental and forestal soils (Asensio- Ramos et al., 2009). Soils were first ultrasound extracted with a mixture of methanol/ acetonitrile and the evaporated
\n\t\t\tAnalyte | \n\t\t\t\t\t\tSample | \n\t\t\t\t\t\tCombined technique and detection limit ( ng / mL ) | \n\t\t\t\t\t\tRemarks | \n\t\t\t\t\t\tReferences | \n\t\t\t\t\t
Carfentrazone-ethyl | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tGC-ECD 0.01-0.03 | \n\t\t\t\t\t\tOnly 100 mg of MWCNTs as adsorbent was needed Comparison with C 18 silica | \n\t\t\t\t\t\tDong et al. , 2009a | \n\t\t\t\t\t
Pesticides | \n\t\t\t\t\t\tAgricultural, ornamental, forestal soils | \n\t\t\t\t\t\tGC- NPD 2.97- 72.4 | \n\t\t\t\t\t\tLow cost CNTs were used (10-15 nm o.d., 2-6 nm i.d. and 0.1-10 μm length ) Satisfactory recovery values ( 54-91 % ) were obtained | \n\t\t\t\t\t\tAsensio-Ramos et al., 2009 | \n\t\t\t\t\t
Amines | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tGC-MS 0.005-0.016 | \n\t\t\t\t\t\tComparison with Lichrolut EN ,Oasis HLB , RP-C18 , graphitized carbon black and fullerenes | \n\t\t\t\t\t\tJurado-Sanchez et al., 2009 | \n\t\t\t\t\t
Pesticides | \n\t\t\t\t\t\tOlive oils | \n\t\t\t\t\t\tGC-MS 1.5-3.0 | \n\t\t\t\t\t\tOnly 30 mg of MWCNTs as adsorbent was needed | \n\t\t\t\t\t\tLopez-Feria et al., 2009 | \n\t\t\t\t\t
Phenols | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tHPLC-DAD 0.9-3.8 | \n\t\t\t\t\t\tThe SPME-Pt fiber coated with SWCNTs was prepared by electrophoretic deposition Linear range of 10- 300 ng / mL | \n\t\t\t\t\t\tLi et al., 2009b | \n\t\t\t\t\t
Oxygenated ethers | \n\t\t\t\t\t\tUrine | \n\t\t\t\t\t\tGC-MS 0.003-0.01 | \n\t\t\t\t\t\tThe SWCNT fiber exhibited higher sensitivity and longer life span ( over 150 times ) than CAR / PDMS fiber | \n\t\t\t\t\t\tRastkari et al., 2009 | \n\t\t\t\t\t
Atrazine, propoxur and methidathion | \n\t\t\t\t\t\tReservoir waters | \n\t\t\t\t\t\tHPLC-UV 2-3 | \n\t\t\t\t\t\tAt flow rate higher than 5.0 mL / min the enrichment efficiencies decreased for all pesticides Linear ranges of 5-30, 3-60 and 5-40 μg / L for atrazine, methidathion and propoxur | \n\t\t\t\t\t\tAl- Degs et al., 2009 | \n\t\t\t\t\t
Chloroacetanilide herbicides | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tGC-ECD 0.01-0.03 | \n\t\t\t\t\t\tThe recoveries were steady in the range of 200-1000 mL sample volume Linear range of 2.5-2500 μg /L | \n\t\t\t\t\t\tDong et al., 2009b | \n\t\t\t\t\t
Cobalt | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tFAAS 0.05 | \n\t\t\t\t\t\tL-tyrosine was immobilized on CNTs and used as sorbent for SPE Adsorption capacity of 37.58 μmol Co / g CNTs | \n\t\t\t\t\t\tPacheco et al., 2009 | \n\t\t\t\t\t
Uranium | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tICP-MS | \n\t\t\t\t\t\tCNTs were modified by heating in a mixture of HNO 3 / H 2 SO 4 The Langmuir model fitted the experimental data better than the Freundlich model | \n\t\t\t\t\t\tSchierz et al., 2009 | \n\t\t\t\t\t
Arsenic | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tFI-AFS 0.002 | \n\t\t\t\t\t\tCarboxyl modified MWCNTs with cation surfactant CTAC were used as adsorbent The recoveries remain stable when the flow rate was below 6 mL / min | \n\t\t\t\t\t\tLi et al., 2009a | \n\t\t\t\t\t
Analyte | \n\t\t\t\t\t\tSample | \n\t\t\t\t\t\tCombined technique and detection limit (ng / mL) | \n\t\t\t\t\t\tRemarks | \n\t\t\t\t\t\tReferences | \n\t\t\t\t\t
Bilirubin | \n\t\t\t\t\t\tPlasma apheresis | \n\t\t\t\t\t\tVIS spectro-photometer | \n\t\t\t\t\t\tMWCNTs exhibit greater adsorption for bilirubin than SWCNTs | \n\t\t\t\t\t\tAndo et al., 2009 | \n\t\t\t\t\t
Organophosphate pesticides (MP) | \n\t\t\t\t\t\tGarlic | \n\t\t\t\t\t\tSWV 5 | \n\t\t\t\t\t\tThe strong affinity of MWCNTs for phosphoric group allow extracting a large amount of MP | \n\t\t\t\t\t\tDu et al., 2008 | \n\t\t\t\t\t
Linear alkylbenzene sulfonates | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tHPLC-UV 0.02-0.03 | \n\t\t\t\t\t\tCarboxyl modified MWCNTs were used as adsorbents Comparison with C8 and C18 | \n\t\t\t\t\t\tGuan et al., 2008 | \n\t\t\t\t\t
Pesticides | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tHPLC 0.036-0.22 | \n\t\t\t\t\t\tMWCNTs have better ability for the extraction than C 18 silica and activated carbon | \n\t\t\t\t\t\tEl-Sheikh et al., 2008 | \n\t\t\t\t\t
Diazinon | \n\t\t\t\t\t\tTap water | \n\t\t\t\t\t\tHPLC 0.06 | \n\t\t\t\t\t\tPreconcentration factor of 200 was achieved for 1000 mL of sample volume Linear range of 0.3-10000 ng / mL | \n\t\t\t\t\t\tKatsumata et al.,2008 | \n\t\t\t\t\t
Organophosphorus pesticides | \n\t\t\t\t\t\tFruit juices | \n\t\t\t\t\t\tGC-NPD 1.85-7.32 | \n\t\t\t\t\t\tLow sample pretreatment prior to the SPE procedure Only 40 mg of MWCNTs as adsorbent was needed | \n\t\t\t\t\t\tRavelo-Perez et al., 2008 | \n\t\t\t\t\t
Aromatic amines | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tHPLC-UV 0.04-0.13 | \n\t\t\t\t\t\tAutomated in- tube SPME using carboxylated MWCNTs Linear range of 1.02-102 μg /mL | \n\t\t\t\t\t\tLiu et al., 2008 | \n\t\t\t\t\t
Pyrethroids | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tHPLC ?UV 1.3- 4.3 | \n\t\t\t\t\t\tThe recoveries decreased except fenpropathrin when the flow rate was over 3 mL/ min | \n\t\t\t\t\t\tZhou et al., 2008 | \n\t\t\t\t\t
Methylene Blue Neutral Red | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tUV-VIS spectrophoto-meter | \n\t\t\t\t\t\tMWCNTs filled with Fe 2 O 3 nanoparticles were used as adsorbent The magnetic MWCNTs have high adsorption efficiency to dyes and can be manipulated by external magnetic field | \n\t\t\t\t\t\tQu et al., 2008 | \n\t\t\t\t\t
Non-steroidal anti- inflammatory drugs | \n\t\t\t\t\t\tUrine | \n\t\t\t\t\t\tCapillary electrophoresis- MS 1.6-2.6 | \n\t\t\t\t\t\tCarboxylated SWCNTs (c-SWCNT ) were chemically immobilized on porous glass.High sorption capacity was related with the special orientation of c-SWCNTs | \n\t\t\t\t\t\tSuarez et al., 2007 | \n\t\t\t\t\t
Pesticides | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tGC-MS 0.01-0.03 | \n\t\t\t\t\t\tThe recoveries were constant at the flow rate in the range of 1.5- 3 mL / min Only 100 mg MWCNTs adsorbent per extraction | \n\t\t\t\t\t\tWang et al., 2007a | \n\t\t\t\t\t
Analyte | \n\t\t\t\t\t\tSample | \n\t\t\t\t\t\tCombined technique and detection limit (ng / mL) | \n\t\t\t\t\t\tRemarks | \n\t\t\t\t\t\tReferences | \n\t\t\t\t\t
Barbiturates | \n\t\t\t\t\t\tPork | \n\t\t\t\t\t\tGC/MS/MS 0.1-0.2 | \n\t\t\t\t\t\tMWCNTs showed better ability for the extraction of phenobarbital than C 18 Linear range 0.5-50μg / Kg | \n\t\t\t\t\t\tZhao et al., 2007 | \n\t\t\t\t\t
Cephalosporins Sulfonamides Phenolic compounds | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tHPLC-PDA 0.027-0.038 | \n\t\t\t\t\t\tCNTs were much superior to C18 for the extraction of the highly polar analytesThe recoveries decreased at solution pH "/ 8. | \n\t\t\t\t\t\tNiu et al., 2007 | \n\t\t\t\t\t
Volatile organic compounds (VOCs) | \n\t\t\t\t\t\tAmbient air | \n\t\t\t\t\t\tGC-FID | \n\t\t\t\t\t\tComparison with Tenax TA High adsorption efficiency for collecting VOCs with low boiling points and strong volatility | \n\t\t\t\t\t\tJie-Min et al., 2007 | \n\t\t\t\t\t
Polycyclic aromatic hydro-carbons | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tHPLC-UV 0.005-0.058 | \n\t\t\t\t\t\tThe recoveries were steady in the range of 250-1000 mL sample volume MWCNTs have better ability for the extraction than C18 | \n\t\t\t\t\t\tWang et al., 2007c | \n\t\t\t\t\t
Fungicides Prometryn | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tHPLC-UV 0.003-007 | \n\t\t\t\t\t\tSample volume up to 1500 mL Linear range of: 0.2-80 μg / L ( fungicides ) 0.05-20 μg /L ( prometryn ) | \n\t\t\t\t\t\tZhou et al., 2007 | \n\t\t\t\t\t
Chromium | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tFAAS 0.90 | \n\t\t\t\t\t\tThe procedure is based on SPE of the Cr ( VI ) -APDC chelate on MWCNTs Adsorption capacity of Cr ( VI ) was 9.5 mg/ g | \n\t\t\t\t\t\tTuzen & Soylak, 2007 | \n\t\t\t\t\t
Lead | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tICP | \n\t\t\t\t\t\tCNTs were coated with Mn oxide and used as adsorbent The Langmuir equation fitted the experimental data more closely than the Freundlich model | \n\t\t\t\t\t\tWang et al., 2007b | \n\t\t\t\t\t
Polybrominated diphenyl ethers | \n\t\t\t\t\t\tWater Milk | \n\t\t\t\t\t\tGC-ECD 0.0036-0.0086 | \n\t\t\t\t\t\tMWCNTs coated fibers for SPME were compared with activated carbon and PDMS-DB coated fibers | \n\t\t\t\t\t\tWang et al., 2006 a | \n\t\t\t\t\t
Microcystins ( MCs ) | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tHPLC-DAD | \n\t\t\t\t\t\tThe size of CNTs tube pore that is fit for molecular dimension of MCs plays a dominante role Adsorption capacity of MCs was 14.8 mg / g | \n\t\t\t\t\t\tYan et al., 2006 | \n\t\t\t\t\t
Sulfonamides | \n\t\t\t\t\t\tEggs Pork | \n\t\t\t\t\t\tHPLC-UV 0.004-0.010 | \n\t\t\t\t\t\tSample loading time up to 23 min for the flow rate of 4.5 mL / min MWCNTs gave lower detection limits, higher enrichment factors and better precisions than C18 silica | \n\t\t\t\t\t\tFang et al., 2006 | \n\t\t\t\t\t
Analyte | \n\t\t\t\t\t\tSample | \n\t\t\t\t\t\tCombined technique and detection limit (ng / mL) | \n\t\t\t\t\t\tRemarks | \n\t\t\t\t\t\tReferences | \n\t\t\t\t\t
Benzodiazepines | \n\t\t\t\t\t\tPork | \n\t\t\t\t\t\tGC-MS 2-5 | \n\t\t\t\t\t\tStatic adsorption experiments 0.2 g MWCNTs were superior to 0.5g C18 for the extraction of diazepam | \n\t\t\t\t\t\tWang et al., 2006b | \n\t\t\t\t\t
Atrazine and simazine | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tHPLC-DAD 0.009-0.033 | \n\t\t\t\t\t\tThe recoveries were constant at the flow rate of 2-7 mL/ min Linear range of 0.2-100 (atrazine) and 0.02-100 ng / mL (simazine) | \n\t\t\t\t\t\tZhou et al., 2006b | \n\t\t\t\t\t
Organochlorine pesticides | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tHPLC-UV 0.004-0.013 | \n\t\t\t\t\t\tThe recoveries were almost constant when the flow rate was change over the range of 2-8 mL / min for sampling loading Linear range of 0.2-60 μg / L | \n\t\t\t\t\t\tZhou et al., 2006a | \n\t\t\t\t\t
Sulfonylurea herbicides | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tHPLC-DAD 5.9 ? 11.2 | \n\t\t\t\t\t\tThe recoveries were constant at the flow rate in the range of 2-8 mL / min Sample volume up to 2000 mL | \n\t\t\t\t\t\tZhou et al., 2006c | \n\t\t\t\t\t
Zinc | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tFAAS | \n\t\t\t\t\t\tThe Langmuir equation is more appropriate to describe the adsorption of Zn 2+ onto CNTs than the Freundlich model.Comparison with powdered activated carbon | \n\t\t\t\t\t\tLu et al., 2006 | \n\t\t\t\t\t
Chlorophenols | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tHPLC-UV 0.08-0.8 | \n\t\t\t\t\t\tThe recoveries decreased slightly with the increase of sample volume higher than 200 mL Linear range of 1-200 ng/ mL | \n\t\t\t\t\t\tCai et al., 2005 | \n\t\t\t\t\t
Volatile organic compounds | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tGC-FID | \n\t\t\t\t\t\tComparison with Carbopack B and VOCARB 3000 | \n\t\t\t\t\t\tLi et al., 2004 | \n\t\t\t\t\t
Phthalate esters | \n\t\t\t\t\t\tWater | \n\t\t\t\t\t\tHPLC-DAD 0.18-0.86 | \n\t\t\t\t\t\tSample volume up to 3000 mL Linear range 2-100 ng / mL | \n\t\t\t\t\t\tCai et al., 2003 | \n\t\t\t\t\t
Examples for adsorption of environmental pollutants on carbon nanotubes.
extract redissolved in water was passed through 100 mg MWCNT of 2-6 nm i.d. and 0,1- 10 μm length.Dichloromethane was used for the elution of analytes. In the three types of soils satisfactory recovery values (54-91 %) were registered for several pesticides (diazinon, ethoprophos, fenitrothion, malathion and phosmet).
\n\t\t\tThe comparison of MWCNTs, graphitized carbon black, fullerenes, Lichrolut EN, Oasis HLB, RP- C 18 in terms of sensitivity, selectivity and reliability has been made for the retention of amine compounds including anilines, chloroanilines, N-nitrosoamines and aliphatic amines (Jurado- Sanchez et al., 2009).The analytes were retained on a SPE sorbent column and after elution, 1 μL of the extract was analysed by gas chromatography coupled with electron impact ionization. MWCNTs are adequate to retain aromatic compounds such as aromatic N-nitrosamines and despite amine aromaticity, they only interact with trichloroanilines and 2-nitroaniline, through π- π interactions, and with some dichloroanilines that contain chlorine atoms in accessible positions for establishing anion- π interactions, and are thus highly selective.
\n\t\t\tSimultaneous determination of three toxic pesticides (atrazine, methidathion and propo- xur) in tap and reservoir waters using MWCNT as solid phase extractant was developed (Al-Degs et. al, 2009). MWCNT adsorbent showed excellent extraction/ pre-concentration of pesticides present at trace levels.The experimental factors that affect pesticides extraction by MWCNTs adsorbent such as sample volume, eluent volume, solution pH and extraction flow rate were studied and optimized. The pesticides were reproducibly detected with a detection limit of 3,2 and 3g / L and linear ranges of 5-30, 3-60 and 5-40 g / L for atrazine, methidathion and propoxur. In tap water, the percent recoveries for pesticides were extended from 95 to 104 % while lower recoveries were observed in reservoir water : 84-93 %.
\n\t\t\tA new kind of carbon nanotubes application to the determination of several pesticides in virgin oil samples was developed (Lopez- Feria et al., 2009). Two carbon nanotubes, MWCNT and carboxylated SWCNT were evaluated. The sorbent (30 mg) was packed in 3-mL commercial cartridge and the virgin oil samples diluted in hexane were passed through it. After a washing step with hexane to remove the sample matrix, the pesticides were eluted with ethyl acetate and analysed by GC-MS.The low limits of detection achieved (between 1.5-3.0 μg / L) afford the application of the method to control the presence of these pollutants in very restrictive samples such as the ecological virgin oil. The method involves a single preconcentration-elution step, which allows sample processing in less than 8 min.The cartridge can be reused at least 100 times without losing performance.
\n\t\t\tA new kind of solid –phase microextraction (SPME) Pt fiber coated with SWCNT was prepared by electrophoretic deposition (EPD) and applied to the assessement of phenols in aqueous samples (Li et al., 2009b). The results revealed that EPD was a simple and reproducible technique for the preparation of SPME fibers coated with SWCNTs without the use of adhesive. The obtained SWCNT coating did not swell in organic solvents nor strip off from substrate, and possessed high mechanical strength due to the strong Van der Waals attractions between the surface of the SWCNTs. The prepared SPME fiber was conductive since both SWCNTs coating and Pt wire were conductive. Using Pt wire as substrate, the fiber was unbreakable. Owing to the presence of oxygenated groups on SWCNTs and the high surface area of SWCNTs, the SWCNT fiber was similar or superior to commercial PA fibers in extracting the studied phenols from aqueous sample. The detection limits for the phenols varied between 0.9 and 3.8 ng / mL and linear ranges were within 10 and 300 ng / mL.
\n\t\t\tA SWCNT fiber was prepared by binding the SWCNT to the surface of stainless steel wire and used as adsorbents for solid phase microextraction of several oxygenated ethers in human urine (Rastkari N. et al., 2009). SWCNTs were attached onto a stainless steel wire through organic binder. Compared with the commercial carboxen / polydimethylsiloxane (CAR / PDMS) fiber, the SWCNT fiber showed better thermal stability and longer life span (over 150 times). For all analytes the detection limits were 10 ng / L.
\n\t\t\tA sensitive method was developed using MWCNTs as SPE adsorbents followed by HPLC with UV detection for determination of six pyrethroid pesticides at trace level in environmental water samples (Zhou et al., 2009). MWCNTs showed more powerful adsorption properties than C18 in the extraction procedure, because they possess a higher capability to extract the six pyrethroids in larger volume solutions. The detection limits for the six target compounds were in the range of 0.7-5.0 ng / L.
\n\t\t\tA novel carbon nanotubes based micro-scale phase extraction ( - SPE) has been developed by incorporating CNTs in the needle of a syringe in packed, as well as in self assembled format (Sae-Khow & Mitra, 2009). The analytes were concentrated by drawing several milliliters of water into the syringe through the needle, and then desorbing/ concentrating them in a few microliters of solvent. The CNTs served as a high performance sorbents, where a relatively high enrichment could be achieved using small quantities of sorbent. The obtained data suggested that the applied method had a low detection limit ranging between 0.1 and 0.3 ng / mL. The enrichment on CNTs were significantly higher as compared to the amount achieved on C18 under similar conditions.
\n\t\t\tMWCNTs were used as sorbent for flow injection (FI) on-line microcolumn pre-concentration coupled with flame atomic adsorption spectrometry (FAAS) for the evaluation of trace cadmium and copper in environmental and biological samples (Liang & Han, 2009). An effective preconcentration of trace cadmium and copper was achieved in a pH range of 4.5-6.5, and 5.0-7.5, respectively.The retained cadmium and copper were efficiently eluted with 0.5 mol/ L HCl for on-line FAAS determination. The MWCNTs packed column exhibited fairly fast kinetics for the adsorption of cadmium and copper which explain the use of high sample flow rates up to at least 7.8 mL / min for the FI on line microcolumn preconcentration system without losing the retention efficiency. The detection limits were 0.30 and 0.11 μg /L for Cd and Cu, respectively.
\n\t\t\tCarboxyl modified multi-walled carbon nanotubes (CMMWCNT s) were used as SPE adsorbents to extract linear alkylbenzen sulfonates (LAS) from water samples (Guan at al., 2008). The effect of eluent and its volume, sample pH and flow rate, sample volume, the content of the electrolyte (NaCl) were investigated and optimized. The limit of detection for LAS homologues was 0.02-0.03 μg / L and the recoveries of LAS homologues in the spiked environmental water samples ranged from 84.8 to 106.1 %.A comparison study with CMMWCNTs, C8 and C18 as adsorbents for LAS was also conducted.CMMWCNTs car-tridge showed stronger retention ability than C8 and C18 cartridges for target com-pounds.
\n\t\t\tA combination of SPE using MWCNT as sorbent and square–wave voltammetric analysis resulted in a fast and selective electrochemical method for the assessement of orga-nophosphate (OP) pesticides using methyl parathion (MP) as a representative (Du at al., 2008). Due to the strong affinity of MWCNT for phosphoric group, nitroaromatic OP compounds can strongly bind to the MWCNT surface.The macroporosity and heterogeneity of MWCNTs allow the extraction of a large amount of MP in less than 5 min. The limit of detection for MP was 0.005 μg / mL. The MP assessement in garlic samples showed acceptable accuracy.
\n\t\t\tA comparison study of three different sorbents (MWCNTs, C18 silica and activated car -bon) in terms of analytical performance, application to environmental waters, cartridge re-use, adsorption capacity and cost of adsorbent has been made for propoxur, atrazine and methidathion pesticides (Sheikh at al., 2008). The adsorption capacity of MWCNTs was almost three times that of activated carbon and C 18, while activated carbon with various surface properties was often preferred to the other two adsorbents due to its low cost.
\n\t\t\tA sensitive and selective column method was proposed for the preconcentration of diazinon –one of the reprezentative compounds of organophosphorus pesticides – in water by using MWCNTs as an adsorbent and then determined by HPLC (Katsumata et al., 2008). The obtained data showed that it is possible to have quantitative analysis when the solution pH was 6 using 200 mL of validation solution and acetonitrile as an eluent.The maximum preconcentration factor was 200 for diazinon when 1000 mL of sample solution volume was used. The limit of detection was 0.06 ng / mL.
\n\t\t\tMWCNTs have been used for the first time as SPE adsorbents for the extraction of eight organophosphorus pesticides from different fruit juices (apple, grape, orange and pine apple) (Ravelo-Perez et al., 2008).The developed method is simple and cost-effective :only 1:1 dilution with Milli- Q Water and pH adjustement to 6.0 of 10 mL of juice is necessary prior to a quick MWCNTs-SPE procedure that used only 40 mg of stationary phase (MWCNT of 10-15 nm o.d., 2-6 nm i.d. and 0.1-10 μm lenght). Mean recovery values were above 73 % for all the pesticides and fruit juices. Limits of detection ranged between 1.85 and 7.32 μg / L.
\n\t\t\tFor the determination of substituted aniline compounds in water samples a simple and sensitive pretreatment technique was advanced by in-tube SPME with MWCNT-COOH adsorbent (Liu et al. 2008). High extraction capacity was achieved for the investigated analytes and great improvement of the limits of detection were obtained in comparison with other methods.The detection limit ranged from 0.04 ng /mL to 0.13 mg / mL.
\n\t\t\tA new method for the trace determination of fenpropathrin, cyhalothrin and deltametrin in environmental water was proposed using MWCNTs cartridge prior to HPLC (Zhou et al., 2008).Detailed analysis were performed concerning several parameters such as the sample pH, eluent and its volume, sample flow rate and sample volume. The linear ranges and the detection limits were in the range of 0.1-40 μg / L and 1.3-4.3 ng / L respectively. The increase of the pH value was conversely proportional to the recovery decline, requiring the adjustement to 7 of the solution pH for a better extraction based on the characteristics of analytes.
\n\t\t\tCarboxylated SWCNTs (c-SWCNTs) have shown a high sorption capacity to retain non-steroidal anti- inflammatory drugs (NSAIDs) and tetracyclines in urine (Suarez et al., 2007). Purified samples were analysed by capillary electrophoresis- mass spectrometry detection allowing the determination of 1.6 to 2.6 μg / L of NSAIDs with only 5 mL of sample.
\n\t\t\tSome factors that affect the MWCNTs enrichment efficiency in relation to some pesticides in environmental waters were investigated (El-Sheick et al., 2007). Model pesticides were selected from various common categories of pesticides, e.g. atrazine, propoxur, methidathion. The effect of MWCNTs oxidation with various oxidizing agents and the effect of length and external diameter of MWCNTs were assessed. Variables optimized included external diameter and length of the MWCNTs, oxidation of the MWCNT, mass of the MWCNT, volume and pH of water sample, composition and volume of eluting solvent and washing solvent. It was found that short –nitric acid oxidized –MWCNT exhibited higher enrichment efficiency especially for methidathion, than non-oxidized long MWCNT.
\n\t\t\tSPE with MWCNT as adsorbent was developed for determination and quantification of 12 pesticides in surface area by gas chromatography – mass spectrometry (GC-MS) (Wang et al., 2007a). Parameters that might influence the extraction efficiency such as the eluent volume, sample volume, sample flow rate and sample loading volume were optimized. The detection limits of proposed method could reach 0.01-0.03 g / L. The experimental results showed the excellent linearity of 12 pesticides over the range of 0.04-4 g / L. Good recoveries achieved with spiked water samples were in the range of 82.0- 103.7 %. The advantages of this SPE method are its simplicity, speediness and the economic consumption of only 0.1 g MWCNT adsorbent per extraction.
\n\t\t\tThe feasibility on the clean-up of three barbiturates (barbital, amobarbital and phenobarbital) from the complex matrix of pork utilizing MWCNTc SPE was also studied (Zhao et al., 2007). The residual barbiturates in pork were extracted by ultrasonic extrac-tion, cleaned up on a MWCNTs packed SPE cartridge and derivatized with methyl iodide under microwave irradiation. Ion trap GC/ MS/MS method eliminates the sample matrix interference. The detection limit of barbital was 0.2 μg/ kg and that of amobarbital and phenobarbital were both 0.1 μg / kg. Limit of quantification was 0.5 μg/ kg for three barbiturates.
\n\t\t\tThe adsorptive potential of SWCNTs and MWCNTs for SPE of three groups of highly polar compounds (namely cefalosporin antibiotics, sulfonamides and phenolic compounds) was tested (Niu et al., 2007). It was found that the analytes were strongly retained by carbon nanotubes.Acceptable recoveries were obtained by adding ammonium acetate into the elu-ents. The performed comparative studies showed that the carbon nanotubes were superior to C18 for the extraction of the highly polar analytes. For the cephalosporins antibiotics and sulfonamides, the carbon nanotubes showed stronger retention capability than graphitized carbon blacks ; however, for some of the phenolic compounds graphitized carbon blacks seemed to be more suitable, indicating different mechanisms of these analytes. MWCNTs packed cartridge was selected to preconcentrate sulfonamide compounds from several real water samples.The detection limits of sulfonamides were in the range of 27-38 ng/ L.
\n\t\t\tA simple and efficient method was developed to determine polycyclic aromatic hydrocarbons (PAHs) in environmental waters using MWCNTs as SPE adsorbents coupled with HPLC (Wang et al., 2007c). The detection limits for the studied PAHs were 0.005-0.058 μg /L. The recoveries of PAHs spiked in environmental water samples ranged from 78.7 to 118.1 %.
\n\t\t\tInvestigations were carried out to characterize the thermally treated CNTs and their adsorption properties of natural organic matter (NOM) (Lu & Su, 2007). After the thermal treatment the structure and nature of carbon surface were changed including the increase in graphitized structure and the decrease in surface functional groups and negative charges; these properties made CNTs to adsorb more NOM. The adsorption capacity of NOM increased with initial NOM concentration and ionic strength but decreased with initial pH. A comparative analysis on the NOM adsorption capacities of CNTs and granular activated carbon (GAC) revealed that the CNTs has superior adsorption performance as compared with the GAC.
\n\t\t\tThe characteristics of SWCNTs as novel adsorbent for collecting volatile organic compounds (VOCs) in ambient air have been studied (Jie-Min et al., 2007). The results reveal that SWCNTs have a large surface area and high adsorption and desorption efficiencies for collecting VOCs with low boiling points and strong volatility. The performed blank experiments show that the background of SWCNTs is very low owing to its chemical inertia. The effect of water can be neglected by increasing humidity in the sampling process because of its particular hydrophobicity. SWCNTs have large breakthrough volumes, as well as safe sampling volume.
\n\t\t\tA simple and sensitive method with MWCNT as SPE adsorbents coupled to HPLC for the determination of several fungicides and prometryn (triazine herbicide) in environmental waters was proposed (Zhou et al., 2007). The detection limits for the studied fungicides and prometryn were in the range of 2.99- 6.94 ng /L, respectively. The results indicated that this method could be used as a reliable alternative for the environmental routine analysis.
\n\t\t\tInvestigation studies were carried out regarding the trapping efficiency of MWCNTs for the analysis of several sulfonylurea herbicides (nicosulfuron, thifensulfuron- methyl and metsulfuron – methyl) in water samples (Zhou et al., 2006c).The possible parameters influencing the enrichment (eluent, sample pH, flow rate and sample volume) were optimized. The registered data showed that MWCNT has exhibited notable merits for trapping sulfonylurea herbicides at low ng / mL levels.
\n\t\t\tAn on-line SPE method using MWCNT as adsorbent coupled with HPLC for simultaneous determination of 10 sulfonamides in eggs and pork was developed (Fang et al., 2006). At the level of the on-line interface SPE with HPLC, a conventional sample loop on the six-port injector valve of the HPLC was replaced by a preconcentration column packed with carbon nanotubes. The analytes in water solution were preconcentrated onto the preconcentration column and subsequently eluted with mobile phase of methanol-water.The results showed that the proposed method was simple, cost efective and sensitive.
\n\t\t\tA new procedure utilizing ultrasonic assistant extract method for the extraction, MWCNTs SPE columns for the clean–up and GC/ MS for the simultaneous determination of four benzodiazepines in pork was developed (Wang et al., 2006b).The adsorption capability of MWCNTs was proved to be obviously higher in comparison with C18. Factors that presumably affect the enrichment efficiency of MWCNT such as the volume of eluent, sample flow rate, sample pH, and volume of the water samples were optimized.The detection limits were 2 g/kg for diazepam and 5 g /kg for estalozam, alprazolam and triazolam in pork, respectively.
\n\t\t\tIt was demonstrated that carbon nanotubes as SPE adsorbents can preconcentrate atrazine and simazine in environmental samples prior to HPLC with diode array detector (Zhou et al., 2006b).The detection limits of the atrazine and simazine were 33 and 9 ng / L, respectively.The spiked recoveries of the two analytes were over the range of 82.6- 103.7 % in most cases.
\n\t\t\tThe feasibility of MWCNTs used as SPE adsorbent to enrich dichlorodiphe-nyltrichloroethane (DDT) and its metabolites at trace level in water samples was investigated (Zhou et al., 2006a). The detection limits were in the range 4-13 ng / L.
\n\t\t\tAmong the newly developed procedures it must be mentioned the MWCNTs – supported micro solid phase extraction (μ- SPE) promoted by Basheer et al., 2006. A 6 mg sample of MWCNTs was packed inside a (2cm x 1.5 cm) sheet of porous polypropylene membrane whose edges were heat-sealed to secure the contents. The μ- SPE device, which was wetted with dichlormethane, was then placed in a stirred sewage sludge sample solution to extract organophosphorous pesticides, used as a model compounds. After extraction, analytes were desorbed in hexane and analyzed using GC / MS. Since the porous membrane afforded protection of the MWCNTs no further cleanup of the extract was required. The π-π electrostatic interactions with the analytes and the large surface area of MWCNTs facilitated the adsorption of the analytes, with good selectivity and reproducibility. The comparison with hollow fiber protected (HFM-SPME) and headspace solid phase microextraction (HS-SPME) showed that this procedure is accurate and fast. -SPE is more sensitive in comparison with the other two procedures. The limits of detection were in the range 1-7 pg / g ; in comparison, for HFM-SPME and HS-SPME, LOD values were 10-67 pg / g and 21-93 pg / g, respectively. Potentially, this developed microextraction technique can be used to extract complex matrices, such as sewage sludge, sludge samples and biological fluids,while preventing coextraction of extraneous materials.
\n\t\t\tCarbon nanotubes with the range of outside diameters from 2 to 10 mm were found to have a strong capacity in the adsorption of cyanobacterial toxins microcystins (MCs) (Yan et al., 2006). Cyanobacteria blooms in natural waters have become a growing environmental issue worldwide due to the increased discharge into rivers and lakes of wastewater containing nitrogen and phosphorus. MCs are stable in the water body and resistant to removal from drinking water by traditional water treatment technology. The adsorption amounts of MCs from lake water were about four times higher than those by activated carbon and clays tested.
\n\t\t\tA type of purified multi-walled carbon nanotubes (PMWCNTs) prepared by catalytic decomposition of methane was evaluated as an adsorbent used for trapping volatile organic compounds (VOCs) from environmental samples (Li et al., 2004). The performance in evaluation was based on breakthrough volumes (BTVs) and recoveries of selected VOCs. PMWCNTs were found to have much higher BTVs in comparison with Carbopack B, a graphitized carbon black with the same surface area as PMWCNTs. The recoveries of the tested VOCs trapped on PMWCNTs ranged from 80 to 110 %, and was not affected by the humidity of purge gas.The results indicate that PMWCNTs are a potential useful adsorbent for direct trapping VOCs from air samples.
\n\t\t\tMWCNTs possess remarkable potential for SPE of trace di-ethyl-phthalate, di-n-propyl-phthalate, di-iso-butyl-phthalate and dicyclohexyl-phthalate from tap water, river water and sea water samples. (Cai et al., 2003). The four analytes were quantitatively adsorbed on MWCNT packed cartridge, then the analytes in acetonitrile eluate were determined by HPLC. Detection limits of 0.18-0.86 ng / mL were achieved for four phthalate esters.The recoveries of SPE using MWCNT cartridge were compared with several SPE adsorbents such as C18, C8 and PS-DVB, the results showed that MWCNT were more effective than or as effective as these adsorbents for SPE of the four analytes.
\n\t\tSPE is an increasingly useful technique for sample concentration and clean-up in environmental applications and can be easily incorporated into automated analytical procedures. The future of SPE is closely related to improvement of sorbents that can be more effective in obtaining high enrichment efficiency of analytes. The unusual properties of CNTs, their large sorption capacity, wide surface area and the presence of a wide spectrum of surface functional groups have generated a great interest in their use as sorbent materials in a wide variety of analytical processess. The presence of the inner cavities, active sites on the surface and internanotube space can contribute to the high pollutants removal capability of CNTs. In several comparative studies the results showed that CNTs were more effective than or as effective as other commonly used adsorbents such as C 18 bonded silica, activated carbon or macroporous resins. It was reported that CNTs may be re-used more than 100 times after proper cleaning and reconditioning (Pyrzynska et al., 2008).
\n\t\t\tCarbon nanotubes have excellent adsorption ability for many kinds of substances such as inorganic and organic compounds (particularly those containing benzene rings) but lesser selectivity. It still needs to explore new chemical functionalization of CNTs to increase its selectivity for highly complexe samples in the future (Liu et al., 2008). Moreover, the development of new synthetic and purification procedures will contribute to the development of new microseparation methods and techniques. In a near future, it will be possible to perform chiral separation or to extract analytes selectively using chiral CNTs Another possibility will be the combination of carbon nanotubes with other new materials (e.g. quantum dots or ionic liquids) (Valcarcel et al., 2008).
\n\t\t\tCarbon nanotubes are relatively expensive and until recently, could only be obtained from a small number of suppliers. Improvements in synthesis methods and control of conditions which can develop a cost effective way of CNTs production are recommended.
\n\t\t\tSeveral authors suggest the need for more CNTs toxicological tests before introducing products containing CNTs into the market because these nanotubes are small enough to have the potential to enter the respiratory system and the detrimental effects are similar to those associated with asbestos. Functionalized CNTs (f-CNTs) are found to be safe while raw carbon nanotubes may possess some degree of toxicity, in vitro and in vivo. F-CNTs are employed in experimental treatment of cancer and as drug- delivery vehicles at the target without any toxic effects.
\n\t\tThe amount of energy consumed in the world has been steadily increasing in the recent decades, and the nonrenewable fossil energy sources account for over 80% of it [1]. In view of this, the search for efficient, environmentally appropriate methods for the generation of renewable energy is a vital present-day scientific problem [2]. One such promising trends is fuel cells [3, 4], the operation of which is directly bound up with the availability of high-purity hydrogen.
\nAt the present time, the wide use of pure hydrogen is economically inexpedient in comparison, e.g., with the use of natural gas, because of the high cost of its production. The industrial method for hydrogen production by the electrolysis of alkaline aqueous solutions [5] has a number of disadvantages, such as the large expenditure of energy, low efficiency of the process, and the necessity of using noble metals as catalysts. Low carbon steel, which is corrosion-nonresistant in alkaline medium, and nickel also possess a catalytic effect in the hydrogen evolution reaction [6]; nevertheless, the problem of search for electrode materials with lower hydrogen evolution overpotential and high corrosion resistance remains vital. For instance, platinum group catalysts can be replaced by cheaper materials, such as nickel, molybdenum, and iron-chromium and iron-manganese alloys, in electrolysis in ionic liquids [7]. However, if the high cost of ionic liquids themselves is taken into account, there is no considerable reduction in the cost of materials for pure hydrogen production.
\nIn the general form, the hydrogen electroreduction process in an alkaline medium is described by the Volmer (1)—Heyrovsky (2)—Tafel (3) mechanism with the following stages:
\nThe rate of electrocatalytic reaction depends on the energy of adsorbed species, i.e., on the energy of hydrogen atoms. The plot of the exchange current density of hydrogen evolution reaction against hydrogen-metal bond energy passes through a maximum and has a volcano-like shape (Figure 1).
\nDependence of the exchange current density of hydrogen evolution reaction in acid solutions against hydrogen-metal bond energy. Reprinted with permission from Ref. [8].
At low Ме▬Н bond energy, the process is controlled by the discharge step, reaction (1). At very high Ме▬Н bond energy, the process is controlled by the electrochemical desorption step, reaction (2). On nickel, cobalt, and iron, the rate-determining step changes from reaction (1) to (2) with increasing polarization. Thus, the most important parameter that determines electrocatalytic activity is the energy of bonding of adsorbed species to the catalyst [9]. When catalysts consisting of two metals are used, the formation of several alloy types, such as mechanical mixtures, solid solutions, and intermetallics is possible. From an analysis of the mechanism of electrocatalytic processes, metal-metal bond energy, and the properties of different alloy types, the authors of [9] conclude that the alloys formed by the metals that are on the different branches of the volcano plot and especially the alloys formed by d-metals with unoccupied d-orbitals (of groups IV–VI) and d-metals of group VIII with a large number of filled d-orbitals possess electrocatalytic activity.
\nIt is known from literature that transition-metal alloys, viz. alloys of iron subgroup metals with molybdenum and tungsten, which show electrocatalytic properties with respect to hydrogen reduction reaction both in acidic [10, 11, 12, 13] and in alkaline aqueous solutions [14, 15, 16, 17], meet these requirements, and that the use of the electrochemical method for the deposition of thin alloy coatings makes it possible to reduce the cost of electrode materials and hence the cost of produced hydrogen.
\nThe synergetic action of alloys in comparison with individual metals is explained by researchers not only by the type of formed alloy and its chemical composition but also by the difference in the mechanism of hydrogen electroreduction on the metals, as well as by the phenomenon of interfacial diffusion of adsorbed hydrogen, hydrogen spillover. The authors of [18] showed the frequent occurrence of this phenomenon in various catalytic processes and catalyst types. Spillover is called the transport of active species, sorbed or formed on one phase, to another phase, which does not sorb and form these species. A study of the synergetic effect of alloys of cobalt and nickel with molybdenum and tungsten with allowance for hydrogen spillover was carried out in [19] for hydrodesulphurization reaction as an example, and it was suggested that different process stages occur on different catalyst phases, between which hydrogen spillover takes place. The spillover phenomenon is of great practical importance, the study of which will help to design new multiphase catalysts, where the catalytic reaction takes place by interfacial diffusion.
\nAs applied to the alloys of molybdenum and tungsten with iron group metals, the spillover phenomenon can account for the synergetic effect of these alloys, in the case of which the discharge step on Mo(W) takes place quickly, and on Co(Ni, Fe), the electrochemical desorption step is fast. Thus, in order that this mechanism may be effected, the active centers of different nature must be at the distance from one another that makes possible the surface diffusion of hydrogen adatoms, and hence the alloy must be a solid solution or an intermetallic.
\nNickel is the most commonly used cathode material in electrolyzers for hydrogen production [20] due to its catalytic properties, corrosion resistance in alkaline medium, and low cost. A possible way of intensifying the process and improving the required properties is electrode surface modification by molybdenum and tungsten alloys; therefore, many papers are devoted to the study of the electrodeposition and catalytic activity of NiMo and NiW alloys. For instance, the authors of [21] studied the electrodeposition of a NiMo alloy on a copper and a nickel substrate from a citrate electrolyte with рН 9.5 and a concentration ratio of the metals of 1/12. The best catalytic activity was found for a coating containing 41 wt.% molybdenum, and it was shown that the hydrogen evolution overpotential at the obtained alloy is lower compared with pure nickel in the model 1 М NaOH solution. In the study [22], a citrate electrolyte with рН 6.0 was also used, and it was shown that it is possible to deposit an alloy containing 28.5 аt.% Мо, which reduces the hydrogen evolution overpotential in 8 M NaOH at 90°С from 122 to 21 mV·dec-1 relative to nickel. The authors of [23] found that when a SAS is added to a citrate-ammonia electrolyte for deposition, nanocrystalline coatings having catalytic activity at a molybdenum content of 19.59 аt.% can be obtained. Chialvo and co-authors [24] studied the catalytic activity of thermal NiMo alloys as a function of the amount of molybdenum (0–25 аt.%) and showed that the higher the Мо content, the lower the hydrogen overpotential. From an analysis of literature data, it can be concluded that there is no unambiguous dependence of electrocatalytic activity on the chemical composition of the coating; for each particular deposition electrolyte, activity is proportional to the molybdenum content, but from the comparison of a large number of papers, it becomes clear that the determining factor is electrolysis conditions, which determine the morphology, the true surface area, the presence of cracks, or an oxide phase on the alloy surface. Therefore, the catalytic properties of electrocatalytic alloys are determined experimentally in each particular case.
\nOn the basis of investigations carried out by the authors of [25], it was concluded that molybdenum-bearing alloys are more active in the hydrogen evolution reaction in alkaline medium than tungsten-bearing alloys. When investigating the properties of Ni-Mo, Ni-W, Co-Mo, and Co-W alloys, it was also found that cobalt alloys show a higher catalytic activity than nickel alloys.
\nThe main characteristics of electrocatalytic activity in HER are reaction exchange current and hydrogen reduction overpotential. Therefore, the main method for studying this process is voltammetry.
\nIn the study [26], an investigation on the electrocatalytic properties of Co-W alloys electrodeposited from a polyligand citrate-pyrophosphate electrolyte had been carried out. The coatings were deposited in a solution containing 0.1 mol L−1 of CoSO4, 0.2 mol L−1 of Na2WO4, 0.2 mol L−1 of Na3Cit (where Cit—citrate ions), 0.2 mol L−1 of K4P2O7, 0.5 mol L−1 of Na2SO4 and in solutions containing SASs: 2 mL L−1 of water-soluble resin neonol, whose efficiency was shown when electrodepositing Co-W alloys from a citrate-ammonia electrolyte [27], and 1.5 g L−1 and 4.5 g L−1 of a nonionic SAS, OP-10 emulsifier. All experiments were performed under forced convection conditions in a current density range of 5.0–30.0 mА сm−2 at 50°С and electrolyte рН 8.5.
\nIt can be seen from Figure 2 that the composition of the coatings deposited from a citrate-pyrophosphate electrolyte is constant regardless of deposition current density and addition of SASs. All coatings containing on an average 22 аt.% W, nevertheless, differ in the current efficiency of their deposition and in the morphology of the produced surface. A small increase in current efficiency for alloys is observed in the case of adding a SAS (neonol or OP-10) to the electrolyte. For instance, at 5.0 mА сm−2 in the presence of neonol, the current efficiency reaches 68%, and a compact, bright, adherent coating is formed. The addition of OP-10 has a noticeable effect only at a concentration of 4.5 g L−1.
\nDependence of the composition (a) and current efficiency (b) of Co-W alloys obtained from electrolyte: 1—without additives; 2—neonol; and 3 and 4—OP-10 (1.5 and 4.5 g L−1) on the deposition current density.
The addition of SASs to the electrolyte and deposition current density affects greatly the quality and morphology (Figure 3). For instance, in the electrolyte without additives at a current density of 5.0 mА сm−2, compact bright coatings are deposited. When the current density is increased to 10.0 mА сm−2, the coating becomes more stressed, and microcracks appear, and at 30.0 mА сm−2, the formation of spherulites is observed. The addition of neonol makes it possible to obtain high-quality fine-crystalline deposits in a wider current density range, and the addition OP-10, on the contrary, facilitates the formation of spherulites and favors surface development.
\nMicrophotographs of the surface of alloys obtained from electrolytes (a) without additives and (b) neonol at a current density of 10.0 mА сm−2 and (c) OP-10 at 30.0 mА сm−2.
The electrocatalytic properties of СоW coatings in the hydrogen reduction reaction were investigated by stationary voltammetry in 1.0 and 6.0 mol L−1 KОН solutions because KOH is used in industrial water electrolysis, and under experimental conditions, i.e., at room temperature, the solution has a maximum electrical conductivity at 28 wt.% KОН.
\nFigure 4a shows a considerable decrease in hydrogen overpotential on CoW alloys relative to electrolytic cobalt. For instance, at the current density of 30.0 mА сm−2, the overpotential decreases by 360 mV. As one would expect, a higher electrocatalytic activity is observed for the coating with more developed surface with spherulites morphology.
\n(a) Volt-ampere curves for the electroreduction of hydrogen in a solution of 1.0 mol L−1 KOH on cobalt (1) and CoW alloys (2 and 3) electrodeposited from the electrolyte without additives at 10.0 and 20.0 mA cm−2, respectively. (b) Volt-ampere curves for the electroreduction of hydrogen in 6.0 mol L−1 KOH solution on CoW alloys, obtained from electrolytes: 1—without additives; 2—neonol; and 3 and 4—OP-10 (1.5 and 4.5 g L−1) at a current density of 10.0 mA cm−2.
Figure 4b shows the effect of SASs added to an electrolyte for the deposition of CoW alloys on their electrocatalytic properties in a solution analogous to industrial electrolyte for hydrogen production. It can be seen that in this particular case, the addition of SAS rather has adverse effects, i.e., smoothing the surface during electrodeposition improves the mechanical and corrosive properties of the coating, but reduces its true surface area.
\nIn the study [28], cobalt and Со-Мо alloys were deposited from a citrate-pyrophosphate electrolyte, proposed earlier [29], with the different concentration ratio of the metals in the solution: [Co]:[Mo] = 20:1; 10:1: 5:1; 1:1 in a current density range of 10–100 mА сm−2 at 50°С. The studies of hydrogen electroreduction on Со-Мо alloys were carried out in solutions with different mineralization and рН, viz. 0.01 mol L−1 H2SO4; 0.5 mol L−1 Na2SO4; and 1.0 mol L−1 KOH. The voltammetric measurements for the determination of the kinetic parameters of hydrogen reduction were made at 25°С. The current-potential curves were recorded under potentiostatic conditions with a step of 20 mV. Before each experiment, argon was passed through the solution for 30 min.
\nIn order to show clearly the catalytic effect of the alloy in comparison with an individual metal, current-potential curves of hydrogen reduction on pure cobalt deposited from a citrate-pyrophosphate electrolyte at a current density of 30 mА сm−2 and a temperature of 50°С have been obtained.
\nFigure 5 shows current-potential curves of hydrogen electroreduction in an acidic, an alkaline, and a neutral medium on electrolytic cobalt cathodes and cathodes made of Со-Мо alloys electrodeposited at the same current density and temperature.
\nStationary current-potential curves of the electroreduction of hydrogen evolution on electrolytic cobalt (a) and Co-Mo alloys (b) with the ratio [Mo]/[Mo] + [Co] = 0.33 electrodeposited at the current density 30 mA cm−2, in media with different pH: 1—H2SO4, 2—KOH, and 3—Na2SO4.
Because of differences in electroreduction mechanism at different pH values, the lowest hydrogen evolution overpotential on cobalt is observed in an acidic medium and the highest in a neutral medium, as is the case with the dependence obtained for a mercury electrode and described in [30]. In the case of cobalt cathode, the coefficient b of the Tafel portion of the polarization curve for the acidic, alkaline, and neutral media was 0.122, 0.142, and 0.125 V, and the exchange current density was 1.93, 4.59 × 10−2 and 6.31 × 10−3 mА сm−2, respectively.
\nFigure 5 shows a considerable decrease in hydrogen evolution overpotential on the alloy. For instance, at the current density of 10 mА сm−2, the overpotential value in the alkaline medium is lower by over 200 mV.
\nThe plots shown in Figure 6 have been obtained on alloys electrodeposited at different current densities of 10–100 mА сm−2. The abscissa of the figure gives the ratio of the amounts of the metals in the alloy, and not the exact percentage because of the peculiarities of EDX analysis, in which the coating surface layer, on which a large amount of oxygen and carbon are adsorbed. The adsorbed light elements can be removed by polishing the surface or treating it with argon ions. Both in this and in the initial case, the ratio of the metals in the alloy remains constant, as was shown in [17], with a coating depth of up to 100 nm. Thus, the ratio of molybdenum and cobalt in the surface layer, determined by EDX analysis, corresponds to the volumetric chemical composition of the alloy.
\nDependence of the exchange current densities of the hydrogen electroreduction reaction on the ratio of molybdenum to cobalt in alloys electrodeposited at current densities of 10, 30, and 100 mA cm−2 from the solution with a [Co]:[Mo] ratio of 1:1 in various media: 1—H2SO4, 2—KOH, and 3—Na2SO4.
In the alloys deposited from an electrolyte with the concentration ratio [Co]:[Mo] = 1:1, the amount of molybdenum decreases and the exchange current density of the hydrogen reduction reaction increases with increasing deposition current density, which can be accounted for in terms of the value which the surface morphology and the true electrode area have, as was shown in [17]. Figure 7 shows surface micrographs of alloys electrodeposited at two current densities of 10 and 100 mА сm−2. It can be seen that at a low current density, smooth, fine-crystalline, and bright coatings are deposited in spite of the presence of microcracks. Increasing the deposition current density to 100 mА сm−2 results in the formation of spherulites and considerable surface development. This regularity is observed for all investigated solutions.
\nThe morphology of Co-Mo alloys precipitated from electrolytes [Co]:[Mo] = 1:1 (a and b) and [Co]:[Mo] = 5:1 (c and d) at current densities of: a and c—10 mA cm−2; b and d—100 mA cm−2 and the ratio of metals [Mo]/[Mo] + [Co] equal to 0.39, 0.27, 0.28, and 0.21, respectively.
The conclusion that the electrocatalytic activity decreases with increasing refractory metal content may contradict papers, published earlier, on the properties of Co-Mo coatings [17, 14]. However, attention should be called on how the coating composition was changed. There are several ways of influencing the chemical composition of alloys, viz. changing the electrolyte composition and pH, temperature, current density, hydrodynamic regime, etc. For instance, in the study [14], a change in alloy composition is achieved by changing both deposition current density and electrolyte composition and in the study [17], by changing pH and, hence, the concentration ratio of different complex species that are able to be discharged to form an alloy. Thus, it is impossible to obtain a rigorous dependence of catalytic activity on the composition of coating deposited under different conditions, because the electrolysis conditions influence not only chemical but also phase composition, which in turn influences the properties of the alloy as a whole.
\nThe effect of change in the composition of the solution for alloy electrodeposition on the electrocatalytic properties is clearly seen in Figure 8, which shows current-potential curves of hydrogen electroreduction on cobalt and alloys deposited at a current density of 30 mА сm−2 from electrolytes containing different sodium molybdate concentrations. It is seen from the figure that the highest hydrogen evolution overpotential is observed on cobalt deposits and the lowest on the alloy deposited from the electrolyte with [Co]:[Mo] = 10:1. The kinetic parameters of hydrogen electroreduction in an alkaline medium are presented in Table 1.
\nPolarization curves obtained in KOH solution on cobalt (1) and Co-Mo alloys with the ratio of metals [Mo]/[Mo]+[Co] equal to (2)—0.11, (3)—0.19, (4)—0.23, and (5)—0.33, respectively, electrodeposited at 30 mA∙cm−2 from electrolytes [Co]:[Mo] = 20:1, 10:1, 5:1, 1:1, respectively.
Electrolyte | \njdep. (mА сm−2) | \nЕ0 (V) | \nа | \nb | \nj0 (mА сm−2) | \n[Мо]/([Мо] + [Со])* | \n
---|---|---|---|---|---|---|
Co | \n30 | \n−0.821 | \n0.190 | \n0.142 | \n4.59 × 10−2 | \n— | \n
[Co]:[Mo] = 20:1 | \n10 | \n−0.910 | \n0.181 | \n0.134 | \n4.46 × 10−2 | \n0.22 | \n
30 | \n−0.985 | \n0.038 | \n0.077 | \n3.21 × 10−1 | \n0.11 | \n|
[Co]:[Mo] = 10:1 | \n10 | \n−0.940 | \n0.125 | \n0.091 | \n9.23 × 10−2 | \n0.25 | \n
20 | \n−1.005 | \n0.045 | \n0.058 | \n1.67 × 10−1 | \n0.23 | \n|
30 | \n−1.025 | \n0.025 | \n0.056 | \n3.58 × 10−1 | \n0.19 | \n|
[Co]:[Mo] = 5:1 | \n10 | \n−0.920 | \n0.130 | \n0.155 | \n1.25 × 10−1 | \n0.28 | \n
30 | \n−0.980 | \n0.050 | \n0.062 | \n1.56 × 10−1 | \n0.23 | \n|
100 | \n−1.000 | \n0.035 | \n0.053 | \n2.19 × 10−1 | \n0.21 | \n|
[Co]:[Mo] = 1:1 | \n10 | \n−0.900 | \n0.189 | \n0.146 | \n5.08 × 10−2 | \n0.39 | \n
20 | \n−0.935 | \n0.110 | \n0.089 | \n5.81 × 10−2 | \n0.37 | \n|
30 | \n−0.980 | \n0.083 | \n0.080 | \n9.17 × 10−2 | \n0.33 | \n|
40 | \n−0.965 | \n0.069 | \n0.077 | \n1.27 × 10−1 | \n0.30 | \n|
100 | \n−1.010 | \n0.043 | \n0.068 | \n2.33 × 10−1 | \n0.27 | \n
Kinetic parameters of hydrogen reduction reaction in a 1 mol L−1 KОН.
The ratio of the metals was calculated based on their atomic fraction in alloys.
Here, jdep. is the current density of alloy deposition; Е0 is the stationary potential of the alloy in a КОН solution; а and b are coefficients in the Tafel equation; and j0 is hydrogen exchange current density.
The difference in the value of hydrogen exchange current on alloys with the same chemical composition is seen in Figure 9.
\nThe dependence of the exchange current of the hydrogen reduction in a 1.0 mol L−1 KOH solution (1 and 2) and the current efficiency (3 and 4) of the Co-Mo alloys electrodeposited in the electrolytes [Co]:[Mo] = 5:1 and [Co]:[Mo] = 1:1 on the ratio of metals in the alloy.
In Figure 9, attention should be called on how the current efficiency of the deposition of the alloy and its electrocatalytic activity correlate with each other. In spite of the fact that the current efficiency was measured for a citrate-pyrophosphate electrolyte for deposition, this electrolyte is a weakly alkaline salt solutions, in which the alloys that are formed also exhibit electrocatalytic activity against the parallel cathodes process, with hydrogen electroreduction; therefore, the plots shown in Figure 9 are of antibate character. Therefore, alloys, electrodeposited at high current densities up to 100 mA cm−2 and having the highest catalytic activity (for all deposition electrolytes) are deposited with the lowest current efficiency.
\nFrom the obtained data, it can be concluded that in the case of Со-Мо alloys electrodeposited from citrate-pyrophosphate electrolytes, the hydrogen exchange current decreases for each particular electrolyte with increasing amount of molybdenum in the alloy. However, in a series of electrolytes with the different concentration ratio of the discharging metals, the alloys that differ greatly in chemical composition can have the same electrocatalytic activity; this can be seen in Figure 10, which shows values of hydrogen exchange currents and stationary potentials for alloys deposited at the same current density, but from different electrolytes.
\nThe dependence of the exchange current (1 and 2) and the stationary potential (3 and 4) in the KOH solution on the molybdenum and cobalt ratio in alloys deposited at current densities, mА cm−2. 1: 3—30; and 2: 4—10.
An extreme form is typical both of the plots of hydrogen exchange current density vs. the ratio of the alloy components and of the stationary potential values of the alloy in the КОН solution.
\nThus, the optimal electrolyte for the making of electrocatalytic Со-Мо alloys is the electrolyte with a cobalt and molybdenum concentration ratio of 10:1, which occupies an intermediate position in the series of investigated solutions; so, increasing or decreasing the concentration of sodium molybdate and hence of molybdenum in the alloy results in the deterioration of the catalytic properties of the coating.
\nIt is known [10] that the electrocatalytic activity of electrode material can be increased by several ways, e.g., by increasing the true working surface area of the catalyst, viz. by making the catalyst not in the form of a continuous film, but in the form of nanofibers [31]. The true surface area must be estimated when fabricating continuous alloy coatings, as this was done in [17]; it should be noted, however, that the factor of surface development is not determining in the ascertainment of the causes of the electrocatalytic activity of the materials under investigation. Another important factor is the nature of the metals comprising the alloy, which was shown in [25], but the physicochemical properties of one metal do not account for the synergetic effect in the use of alloys. The phenomenon that describes most reliably the synergetic action of two or more metals is spillover effect, which was described in [10, 11, 12]. Since hydrogen evolution occurs on Со and Мо with different rate-determining steps, as was said above, the occurrence of hydrogen spillover makes it possible to bring about a fact reaction (1) on molybdenum atoms and a rapid electrochemical desorption (2) on cobalt atoms.
\nBecause of this, the synergetic effect of the alloy will manifest itself when the atoms are arranged in an optimal manner to perform sequential reaction steps. This is possible when the alloy is an intermetallic, an amorphous phase, or solid solutions with nanosized crystals.
\nWhen we attempted to investigate the coatings obtained by us by X-ray phase analysis, we have not obtained somewhat well-defined peaks of phases, i.e., the coatings were either very fine-crystalline, below the device sensitivity level, or amorphous. However, different properties (e.g., corrosion or magnetic properties) of Co-Mo alloys of the same composition have also been obtained by us earlier. Their phase composition has been studied by us by stripping analysis and shown in [32].
\nSome of the main characteristics of modern catalytic materials are not only their activity in the desired reaction but also mechanical strength and corrosion resistance in aggressive media; therefore, the comprehensive investigation of the physicochemical properties of the electrode material is an important scientific and technical problem.
\nIn the study [26], the corrosion characteristics of electrolytic Co-W alloys deposited from a citrate-pyrophosphate electrolyte in 3.5% NaCl and 6 mol L−1 KOH solutions at 25°С have been determined by EIS and stationary voltammetry (Figure 11).
\nElectrochemical impedance spectra (a) and current-potential curves (b) obtained in the case of corrosion of coatings electrodeposited from a citrate-pyrophosphate electrolyte at the current densities mА cm−2: 1—5.0; 2—10.0; and 3—20.0.
The impedance hodographs obtained at a stationary potential in a corrosive medium can be described by a circuit comprising the ohmic resistance of the solution, charge transfer (corrosion) resistance, and a constant phase element. The corrosion parameters calculated in accordance with this equivalent circuit are listedTable 2.
\n\n | j (mА сm−2) | \nW (аt.%) | \nR (kОhm сm−2) | \nRp (kОhm сm−2) | \nЕcorr (V) | \nJcorr × 105 (А сm−2) | \n
---|---|---|---|---|---|---|
1 | \n5.0 | \n23.3 | \n18.0 | \n41.2 | \n−0.782 | \n1.35 | \n
2 | \n10.0 | \n24.0 | \n18.8 | \n6.9 | \n−0.834 | \n8.53 | \n
3 | \n20.0 | \n20.8 | \n12.8 | \n16.6 | \n−0.786 | \n5.24 | \n
Corrosion parameters of alloys in a 3.5% NaCl solution.
Here, j is alloy deposition current density; W is tungsten content, аt.%; R is corrosion resistance determined by the impedance method; Rp is corrosion resistance determined by voltammetry; Еcorr is corrosion potential; and jcorr is corrosion current density.
The coating deposited at a current density of 5.0 mА сm−2 has the highest corrosion stability because in the region of kinetic control of electrochemical reaction, most fine-crystalline and compact deposits are formed. Since the chemical composition of the coatings deposited from a citrate-pyrophosphate electrolyte is almost constant, the dependence of polarization resistance on deposition current density can be attributed to a difference in surface morphology and the appearance of microcracks on increasing the deposition current. On the whole, the corrosion rate of the obtained alloys is comparable with that in an analogous solution of electrolytic chromium deposited from Cr(III) and Cr(VI) baths in the study [33] (Figure 12).
\nSpectra of electrochemical impedance (a) and current-potential curves (b), obtained in the case of corrosion in a 6.0 mol L−1 KOH solution, for coatings electrodeposited at a current density of 10.0 mA cm−2 from electrolytes 1—no additives; 2—neonol; 3 and 4—OP-10 (1.5 and 4.5 g L−1).
The parameters of the corrosion process, determined by the electrochemical impedance method, have been calculated on the basis of an equivalent circuit comprising the ohmic resistance of the solution, corrosion resistance, a constant phase element, and Warburg impedance (Table 3).
\nElectrolyte | \nW (аt.%) | \nR (kOhm сm−2) | \nRp (kOhm сm−2) | \nЕcorr (V) | \nJcorr × 103 (А сm−2) | \n
---|---|---|---|---|---|
1 | \n24.0 | \n0.92 | \n0.58 | \n−1.03 | \n0.84 | \n
2 | \n23.7 | \n0.46 | \n0.37 | \n−1.05 | \n0.11 | \n
3 | \n24.0 | \n0.34 | \n0.40 | \n−1.04 | \n0.17 | \n
4 | \n22.6 | \n0.40 | \n0.48 | \n−1.03 | \n0.12 | \n
Corrosion parameters of alloys in a 6 mol L−1 КОН solution.
The corrosion studies, carried out by us, of CoW alloys in a 6.0 mol L−1 КОН solution showed that the corrosion resistance in a concentrated КОН solution (Figure 12) is two order of magnitude lower than in a model NaCl solution; nevertheless, the coatings can be considered corrosion proof. It was noted that the coatings obtained for the experiment are of the worst quality in comparison with others, since they are intermediate at the transition from fine crystalline to spherulite deposits. The deposits of these two types are dense and smooth, and only at 10.0 mА сm−2, the largest number of cracks is observed, which accordingly affects the properties of coatings; nevertheless, the coatings have a low corrosion rate and are passivated in alkaline solution.
\nTo determine the corrosion properties of electrolytic Со-Мо alloys in the study [34], the coatings were deposited from a citrate-pyrophosphate electrolyte with different concentration ratios of the metals: [Co]/[Mo] = 1/1 and [Co]/[Mo] = 5/1. The aim of the authors was a large percentage of a component having ferromagnetic properties, i.e., cobalt. To fabricate cobalt-rich alloys, electrolytes with low sodium molybdate content and, hence, with small amount of molybdenum in the coating are used.
\nAs is seen from Figure 13, the amount of molybdenum in the alloy electrodeposited from an electrolyte at [Co]/[Mo] = 5/1 decreased relative to the alloy deposited from an electrolyte with [Co]/[Mo] = 1/1; in this case, however, no direct proportionality between the molybdenum content of the alloy and solution is observed. For instance, the concentration ratio of molybdate and cobalt in the electrolyte was 0.2 and changed from 0.4 to 0.27 in the coating. The amount of cobalt in the deposit changes only slightly on increasing the current density, but the percentage of nonmetallic impurities, mainly oxygen, increases, which affect the internal stresses in the deposit. Nevertheless, this change in the concentration ratio of the metals in the solution leads to a great increase in current efficiency for the alloy at low current densities (Figure 13b). Thus, it can be stated that in terms of the cobalt content of the alloy, the most optimal conditions for the deposition of magnetic coatings are current densities of 10–50 mА сm−2.
\nDependence of the ratio of the metals content (a) and current efficiency (b) for alloys electrodeposited from electrolytes with a concentration ratios [Co]/[Mo] = 1/1 and [Co]/[Mo] = 5/1 on current density.
The corrosion test of the obtained coatings was carried out in a sulfate-chloride solution. The calculation of corrosion resistance from electrochemical impedance data has been performed on the basis of an equivalent circuit comprising the ohmic resistance of the solution, charge transfer resistance, and a constant phase element.
\nAlloy samples electrodeposited from an electrolyte with [Co]/[Mo] = 5/1 with increasing current density, i.e., with decreasing molybdenum content (Figure 13, curve 2), and an alloy electrodeposited from an analogous citrate electrolyte containing no pyrophosphate at 30 mА сm−2, have been investigated. Figure 14 and Table 4 show no clear correlation between the molybdenum content of the alloy and corrosion resistance. Besides, the coatings deposited from solutions with the same ratio of the metals in the presence and absence of pyrophosphate are similar in anticorrosion properties despite the difference in their chemical composition.
\nStationary current-potential curves (a) and electrochemical impedance spectra (b) of the corrosion of alloys deposited from polyligand electrolyte (1–3) and a citrate electrolyte (4) at the deposition current densities, mА cm−2: 1—10; 2 and 4—30; and 3—50.
Electrolyte | \nj (mА сm−2) | \nМо (аt.%) | \nR (Оhm) | \nRp (Оhm) | \nЕcorr (V) | \nJcorr (А сm−2) | \n
---|---|---|---|---|---|---|
Citrate-pyrophosphate | \n10 | \n21.5 | \n5.05 × 102 | \n2.97 × 103 | \n−0.627 | \n3.58 × 10−4 | \n
30 | \n17.4 | \n5.71 × 103 | \n1.77 × 104 | \n−0.804 | \n829 × 10−6 | \n|
50 | \n16.0 | \n7.02 × 102 | \n3.55 × 102 | \n−0.677 | \n6.40 × 10−4 | \n|
Citrate | \n30 | \n23.9 | \n4.57 × 103 | \n8.06 × 103 | \n−0.804 | \n2.83 × 10−5 | \n
Dependence of the corrosion parameters of Со-Мо alloys on alloy composition.
Here, j is deposition current density.
The anticorrosion resistance of Co-Mo coatings is usually associated with the percentage content of molybdenum in them as a more corrosion-resistant metal, and the magnetic properties of coatings—with a cobalt content as a metal with ferromagnetic properties. However, the functional properties of coatings can depend not only on the chemical composition of the alloy but also on its phase composition, morphology, thickness, porosity, and other factors.
\nWhen studying the corrosion and magnetic properties of Со-Мо coatings [32] deposited from a citrate-pyrophosphate electrolyte, it was found that for the coatings obtained under different electrolysis conditions and having the same chemical composition, the corrosion stability and magnetic parameters are different; it was suggested that the properties of the alloy largely depend on its phase composition.
\nIn the study, the corrosion and magnetic properties of coatings with same Mo content of the alloy (21.2 аt.%), deposited from a citrate-pyrophosphate electrolyte under different electrolysis conditions, have been investigated. The corrosion stability of the coatings was studied in a solution containing 7 g L−1 Na2SO4 and 7 g L−1 NaCl at рН 6.0 and 24 ± 1°С (Table 5). The magnetic properties (Table 6) of the obtained deposits were determined by means of a vibrating sample magnetometer in fields of up to 20 kOe at room temperature (Table 5).
\nDeposition electrolyte | \nj (mА сm−2) | \nt (°С) | \nRр (Оhm) | \nЕcorr (V) | \nJcorr (А сm−2) | \n
---|---|---|---|---|---|
[Co]/[Mo] = 1/1 | \n30 | \n25 | \n2.71 × 103 | \n−0.804 | \n8.44 × 10−5 | \n
[Co]/[Mo] = 1/1 | \n40 | \n50 | \n9.82 × 102 | \n−0.808 | \n2.54 × 10−4 | \n
[Co]/[Mo] = 5/1 | \n10 | \n50 | \n2.97 × 103 | \n−0.627 | \n3.58 × 10−4 | \n
Corrosion properties of alloys having the same chemical composition (21.2 аt.% Мо).
The magnetic characteristics of such Alloys are also given. Their calculated values are listed in Table 6. The main criteria for evaluating the properties of soft-magnetic materials are low coercive force, low remanent magnetization and high saturation magnetization, as well as the ability to reach saturation magnetization in low intensity fields. It is evident from Table 6 that the largest saturation magnetization values—927 Gs were obtained at a magnetic field intensity of 3 kOe for the alloys deposited from an electrolyte with a ratio of 5:1. For the coatings deposited from an electrolyte with a ratio of 1:1, no saturation magnetization is observed even at 20 kOe; the maximum value obtained under experimental conditions for alloys deposited at 25° and 50°С was 113 and 290 Gs, respectively. Thus, it can be concluded that the alloy deposited from an electrolyte with the concentration ratio of the metals [Co]/[Mo] = 5/1. We assumed that such a difference in functional properties for the coatings having the same chemical composition may be due to a difference in their phase composition.
\nDeposition electrolyte | \nj (mА сm−2) | \nt (°С) | \nН (Oe) | \nMR (Gs) | \nМS (Gs) | \n
---|---|---|---|---|---|
[Co]/[Mo] = 1/1 | \n30 | \n25 | \n155 | \n5.0 | \n113 | \n
[Co]/[Mo] = 1/1 | \n40 | \n50 | \n117 | \n20.0 | \n290 | \n
[Co]/[Mo] = 5/1 | \n10 | \n50 | \n102 | \n252 | \n927 | \n
Magnetic properties of alloys having the same chemical composition (21.2 аt.% Мо).
Here, Н is coercive force, MR is remanent magnetization, and МS is saturation magnetization.
To study the phase composition, the electrochemical method of linear stripping voltammetric analysis (LSVA) was used [35]. An advantage of this method, besides simplicity, is the possibility to follow the dissolution dynamics of the alloy. Before the stripping analysis, a 0.5 μM thick layer of Co or Co-Mo alloys were deposited onto the working electrode from a citrate-pyrophosphate electrolyte with the concentration ratios of the metals [Co]/[Mo] = 1/1 and [Co]/[Mo] = 5/1 at a current density of 10–100 mА сm−2 and a temperature of 25 and 50°С.
\nThe electrolyte for the anodic dissolution of the obtained alloy deposits must meet the following requirements: it must have a high electrical conductivity, be nonaggressive toward the coating, and not cause spontaneous chemical dissolution. In this electrolyte, an electrochemical side reaction paralleling the anodic dissolution of the deposit under investigation must be ruled out. The use of various acids as working solutions was considered inexpedient since the electrochemical process in such electrolytes is paralleled by the chemical dissolution of the coating under analysis. Alkaline solutions are unsuitable for use as working electrolytes because of passivation processes on the surface of samples under investigation. The optimal solution for the anodic dissolution of coatings under investigation is NaCl solution, which makes it possible to obtain on the current-potential curves clear peaks corresponding to the dissolution potentials of the various phases of the alloy. The stripping analysis of coatings was performed in a 0.5 М NaCl solution at 25°С on a rotating disk electrode at a rotational speed of 774 rpm.
\nFigure 15 shows a current-potential curve of the dissolution of freshly deposited cobalt (curve 1) in a 0.5 М NaCl solution. The observed dissolution peaks are traditionally attributed to the complex phase structure of metals and alloys, but their number depends on the electrolyte in which dissolution is performed [35]. The plot of cobalt dissolution current vs. potential exhibits three peaks, which we further use in order to distinguish the peaks of dissolution of the alloy from the peaks of cobalt dissolution. The figure shows plots except the oxygen and chlorine evolution curve. It can be seen that in the case of dissolution of alloys, the magnitude of the peaks and their number are different. For instance, for the alloys deposited from an electrolyte with the same concentration ratio of the metals, the magnitude of peak 1 is the same, but besides it, only one large peak is observed for the alloy obtained at 50°С and 40 mА сm−2, whereas two peaks are observed for the alloy obtained at 25°С and 30 mА сm−2. However, for the alloy deposited from an electrolyte with lower molybdate content, the magnitude of peak 1 is much larger than for other alloys. Based on the potentials of the peaks, the known cathodic quantity of electricity, the phase diagram of the double layer, and stoichiometry, it can be suggested that peaks 1 and 3 relate to cobalt dissolution and peak 2 to the dissolution of a solid solution of the chemical compound СоМо in cobalt.
\nAnodic dissolution curves for pure cobalt (curve 1) and Co-Mo alloys (21.1 at.% Mo) deposited under the following conditions: 2—Co:Mo = 5:1, 50°C, 10 mA cm−2; 3—Co:Mo = 1:1, 25°C, 30 mA cm−2; 4—Co:Mo = 1:1, 50°С, 40 mА сm−2.
Thus, the alloy deposited from an electrolyte containing a small amount of molybdate contains a larger amount of cobalt bound into neither a chemical compound nor a solid solution; this can explain the 200 mV shift of the corrosion potential of this alloy to positive values, i.e., cobalt is a more electropositive metal than molybdenum, as well as the improvement of the magnetic properties of the alloy. The increase in peak 2 indicates an increase in the percentage of the molybdenum-rich phase, which results in the improvement of the corrosion properties of alloys.
\nStripping analysis of alloys deposited from an electrolyte with [Co]/[Mo]=1/1 at different current densities is shown in Figure 16. It is seen from the figure that for the coatings obtained at lower deposition current densities 10–20 mА сm−2, three dissolution peaks are observed. For the alloys deposited at 30 and 40 mА сm−2, only two dissolution peaks are observed. The magnitude of peak 1 remains unchanged, and it can be assumed to correspond to the amount of cobalt that is directly on the electrode surface, i.e., dissolution of the less corrosion-resistant component than the alloy takes place, and since the electrode geometry does not change, the quantity of electricity for dissolution remains constant too. In the remaining alloy phase at different current densities, different redistribution of cobalt between the solid solution and the free α-phase takes place.
\n(a) Anodic current-potential curves of the dissolution of Co-Mo alloys deposited from an electrolyte at [Co]/[Mo] = 1/1 at 50°C at different current densities, mA cm−2: 1—10, 2—20, 3—30, 4—40 and (b) The magnitude of anodic dissolution peaks.
To study the alloy formation process, anodic polarization curves have been obtained for Со-Мо alloys deposited from an electrolyte with [Co]/[Mo] = 1/1 under the conditions corresponding to the maximum current efficiency: a current density of 30 mА сm−2 and at temperature of 50°С [36]. The coatings were deposited during 30, 60, 120, and 210 s (Figure 17). All current-potential curves of the dissolution of Со-Мо alloys exhibit two peaks. As one would expect, the quantity of electricity for the dissolution of the solid solution increases linearly with deposition time. We failed, however, to determine the order of deposition of the components; using this method, it is impossible to either confirm or refute the hypothesis that cobalt deposits first, which catalyzes later the reduction of molybdenum. Under our experimental conditions, an alloy phase which grows uniformly with increasing deposition time is present in the alloy even within a deposition time of 30 s.
\n(a) Anodic current-potential curves of the dissolution of Co-Mo alloys deposited from an electrolyte with [Co]/[Mo]=1/1 at 30 mA∙cm−2 and 50°C at different deposition time, s: 1—30, 2—60, 3—120, 4—210. (b) The magnitude of the anodic dissolution peaks: 1—the first peak, and 2—the second peak.
Electrolytic alloys of molybdenum and tungsten with iron subgroup metals possess catalytic properties in the hydrogen evolution reaction and can be used as a coating which improves the properties of exiting nickel cathodes.
\nFor each particular electrolyte and particular deposition conditions, the activity of the alloy and its corrosion stability increase with the amount of molybdenum, but the comparison of data obtained by different authors does not give a clear correlation.
\nThe properties of alloys depend not only on their chemical composition but also on their phase composition. The alloy containing the same amount of molybdenum, but fabricated under different conditions, has different corrosion and magnetic properties.
\nThe amorphous and nanocrystalline structure of electrolytic alloys makes hydrogen spillover possible, which greatly accelerates the hydrogen reduction process in alkaline electrolytes.
\nElectrolytic coatings of refractory metals alloys have a wide range of physicochemical properties. Controlling the electrolysis modes allows precipitating and accurately controlling the chemical and phase composition of the coatings, and hence producing corrosion-resistant materials for soft magnetic materials, electrocatalysts, and wear-resistant coatings.
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