Particle size of minerals participating into the reverse flotation.
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More than half of the publishers listed alongside IntechOpen (18 out of 30) are Social Science and Humanities publishers. IntechOpen is an exception to this as a leader in not only Open Access content but Open Access content across all scientific disciplines, including Physical Sciences, Engineering and Technology, Health Sciences, Life Science, and Social Sciences and Humanities.
\\n\\nOur breakdown of titles published demonstrates this with 47% PET, 31% HS, 18% LS, and 4% SSH books published.
\\n\\n“Even though ItechOpen has shown the potential of sci-tech books using an OA approach,” other publishers “have shown little interest in OA books.”
\\n\\nAdditionally, each book published by IntechOpen contains original content and research findings.
\\n\\nWe are honored to be among such prestigious publishers and we hope to continue to spearhead that growth in our quest to promote Open Access as a true pioneer in OA book publishing.
\\n\\n\\n\\n
\\n"}]',published:!0,mainMedia:null},components:[{type:"htmlEditorComponent",content:'
Simba Information has released its Open Access Book Publishing 2020 - 2024 report and has again identified IntechOpen as the world’s largest Open Access book publisher by title count.
\n\nSimba Information is a leading provider for market intelligence and forecasts in the media and publishing industry. The report, published every year, provides an overview and financial outlook for the global professional e-book publishing market.
\n\nIntechOpen, De Gruyter, and Frontiers are the largest OA book publishers by title count, with IntechOpen coming in at first place with 5,101 OA books published, a good 1,782 titles ahead of the nearest competitor.
\n\nSince the first Open Access Book Publishing report published in 2016, IntechOpen has held the top stop each year.
\n\n\n\nMore than half of the publishers listed alongside IntechOpen (18 out of 30) are Social Science and Humanities publishers. IntechOpen is an exception to this as a leader in not only Open Access content but Open Access content across all scientific disciplines, including Physical Sciences, Engineering and Technology, Health Sciences, Life Science, and Social Sciences and Humanities.
\n\nOur breakdown of titles published demonstrates this with 47% PET, 31% HS, 18% LS, and 4% SSH books published.
\n\n“Even though ItechOpen has shown the potential of sci-tech books using an OA approach,” other publishers “have shown little interest in OA books.”
\n\nAdditionally, each book published by IntechOpen contains original content and research findings.
\n\nWe are honored to be among such prestigious publishers and we hope to continue to spearhead that growth in our quest to promote Open Access as a true pioneer in OA book publishing.
\n\n\n\n
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Avci",slug:"munevver-ertek-avci",email:"Munevver.ErtekAvci@calikdenim.com",position:null,institution:null}]},book:{id:"7242",title:"Engineered Fabrics",subtitle:null,fullTitle:"Engineered Fabrics",slug:"engineered-fabrics",publishedDate:"February 13th 2019",bookSignature:"Mukesh Kumar Singh",coverURL:"https://cdn.intechopen.com/books/images_new/7242.jpg",licenceType:"CC BY 3.0",editedByType:"Edited by",editors:[{id:"36895",title:"Dr.",name:"Mukesh Kumar",middleName:null,surname:"Singh",slug:"mukesh-kumar-singh",fullName:"Mukesh Kumar Singh"}],productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"}}},ofsBook:{item:{type:"book",id:"8807",leadTitle:null,title:"Organic Synthesis",subtitle:null,reviewType:"peer-reviewed",abstract:"
\r\n\tOrganic synthesis has always been one of the central topics of research for the scientific community in the academic laboratories and industrial world. Many striking journal articles and remarkable reviews and books have been published in the past year describing the practicability and applications of the subject demonstrating the importance of organic synthesis. In the present book, we will be putting together the topics in organic synthesis which may include but not limited to, (1) the basic terms and concepts, (2) various organic reactions including reduction, oxidation, addition, elimination, rearrangements, and cycloadditions, (3) Total Synthesis of Natural products, (4) transition metal catalysts, organocatalysts, enzymes and biotransformations, (5) applications in medicinal chemistry and drug design and development, (6) purification methods and characterization techniques, etc. To set a limit and to increase the scope of the book, author(s) are encouraged to send the chapters that include selected examples with practical applications and good yielding reactions reported within the past decade. Older topics with significant findings or their essence to prepare the foundation may be included in the chapter are welcomed as well.
",isbn:null,printIsbn:"979-953-307-X-X",pdfIsbn:null,doi:null,price:0,priceEur:null,priceUsd:null,slug:null,numberOfPages:0,isOpenForSubmission:!1,hash:"f3bbbd989d0896f142d317ccb8abcc35",bookSignature:"Dr. Prashant S Deore",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/8807.jpg",keywords:"Natural Product Synthesis, Organic Reaction Mechanism, Stereoselective synthesis, Chirality, C-H Functionalization, Cross-Coupling Reactions, Heterogeneous Catalysis, Homogeneous Catalysis, Green Synthesis, Green Solvents and Reagents, Bioorganic synthesis, Click Chemistry",numberOfDownloads:null,numberOfWosCitations:0,numberOfCrossrefCitations:0,numberOfDimensionsCitations:null,numberOfTotalCitations:null,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"December 10th 2018",dateEndSecondStepPublish:"January 14th 2019",dateEndThirdStepPublish:"March 15th 2019",dateEndFourthStepPublish:"May 20th 2019",dateEndFifthStepPublish:"July 19th 2019",remainingDaysToSecondStep:"2 years",secondStepPassed:!0,currentStepOfPublishingProcess:5,editedByType:null,kuFlag:!1,biosketch:null,coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"251769",title:"Dr.",name:"Prashant",middleName:"S",surname:"Deore",slug:"prashant-deore",fullName:"Prashant Deore",profilePictureURL:"https://mts.intechopen.com/storage/users/251769/images/system/251769.png",biography:"Dr. Prashant S. Deore was born in India. He received a Master’s degree in organic chemistry from Pune University in 2007. In the same year, he qualified with the SET and CSIR-NET (JRF) and joined in the group of Prof. Narshinha P. Argade for the doctoral studies in National Chemical Laboratory, India. In 2014, he awarded with a Ph. D. in Chemistry and was a recipient of the 2nd prize in “2014 Eli Lilly and Company Asia Outstanding Thesis Awards”. In July 2014 he moved to Canada and joined as a postdoctoral researcher in the group of Prof. Richard Manderville at the University of Guelph, Canada. Presently, Dr. Deore is working on the collaborative project between the University of Guelph and Aterica health Inc., and providing consulting to the company. His research interest includes organic synthesis, fluorescent probes development, nucleic acid synthesis and modifications, and aptasensor development for proteins and food toxins.",institutionString:"University of Guelph",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"0",totalChapterViews:"0",totalEditedBooks:"0",institution:null}],coeditorOne:null,coeditorTwo:null,coeditorThree:null,coeditorFour:null,coeditorFive:null,topics:[{id:"8",title:"Chemistry",slug:"chemistry"}],chapters:null,productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"},personalPublishingAssistant:{id:"270935",firstName:"Rozmari",lastName:"Marijan",middleName:null,title:"Ms.",imageUrl:"https://mts.intechopen.com/storage/users/270935/images/7974_n.png",email:"rozmari@intechopen.com",biography:"As an Author Service Manager my responsibilities include monitoring and facilitating all publishing activities for authors and editors. From chapter submission and review, to approval and revision, copyediting and design, until final publication, I work closely with authors and editors to ensure a simple and easy publishing process. I maintain constant and effective communication with authors, editors and reviewers, which allows for a level of personal support that enables contributors to fully commit and concentrate on the chapters they are writing, editing, or reviewing. I assist authors in the preparation of their full chapter submissions and track important deadlines and ensure they are met. I help to coordinate internal processes such as linguistic review, and monitor the technical aspects of the process. As an ASM I am also involved in the acquisition of editors. Whether that be identifying an exceptional author and proposing an editorship collaboration, or contacting researchers who would like the opportunity to work with IntechOpen, I establish and help manage author and editor acquisition and contact."}},relatedBooks:[{type:"book",id:"1591",title:"Infrared Spectroscopy",subtitle:"Materials Science, Engineering and Technology",isOpenForSubmission:!1,hash:"99b4b7b71a8caeb693ed762b40b017f4",slug:"infrared-spectroscopy-materials-science-engineering-and-technology",bookSignature:"Theophile Theophanides",coverURL:"https://cdn.intechopen.com/books/images_new/1591.jpg",editedByType:"Edited by",editors:[{id:"37194",title:"Dr.",name:"Theophanides",surname:"Theophile",slug:"theophanides-theophile",fullName:"Theophanides Theophile"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"3092",title:"Anopheles mosquitoes",subtitle:"New insights into malaria vectors",isOpenForSubmission:!1,hash:"c9e622485316d5e296288bf24d2b0d64",slug:"anopheles-mosquitoes-new-insights-into-malaria-vectors",bookSignature:"Sylvie Manguin",coverURL:"https://cdn.intechopen.com/books/images_new/3092.jpg",editedByType:"Edited by",editors:[{id:"50017",title:"Prof.",name:"Sylvie",surname:"Manguin",slug:"sylvie-manguin",fullName:"Sylvie Manguin"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"3161",title:"Frontiers in Guided Wave Optics and Optoelectronics",subtitle:null,isOpenForSubmission:!1,hash:"deb44e9c99f82bbce1083abea743146c",slug:"frontiers-in-guided-wave-optics-and-optoelectronics",bookSignature:"Bishnu Pal",coverURL:"https://cdn.intechopen.com/books/images_new/3161.jpg",editedByType:"Edited by",editors:[{id:"4782",title:"Prof.",name:"Bishnu",surname:"Pal",slug:"bishnu-pal",fullName:"Bishnu Pal"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"72",title:"Ionic Liquids",subtitle:"Theory, Properties, New Approaches",isOpenForSubmission:!1,hash:"d94ffa3cfa10505e3b1d676d46fcd3f5",slug:"ionic-liquids-theory-properties-new-approaches",bookSignature:"Alexander Kokorin",coverURL:"https://cdn.intechopen.com/books/images_new/72.jpg",editedByType:"Edited by",editors:[{id:"19816",title:"Prof.",name:"Alexander",surname:"Kokorin",slug:"alexander-kokorin",fullName:"Alexander Kokorin"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"1373",title:"Ionic Liquids",subtitle:"Applications and Perspectives",isOpenForSubmission:!1,hash:"5e9ae5ae9167cde4b344e499a792c41c",slug:"ionic-liquids-applications-and-perspectives",bookSignature:"Alexander Kokorin",coverURL:"https://cdn.intechopen.com/books/images_new/1373.jpg",editedByType:"Edited by",editors:[{id:"19816",title:"Prof.",name:"Alexander",surname:"Kokorin",slug:"alexander-kokorin",fullName:"Alexander Kokorin"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"57",title:"Physics and Applications of Graphene",subtitle:"Experiments",isOpenForSubmission:!1,hash:"0e6622a71cf4f02f45bfdd5691e1189a",slug:"physics-and-applications-of-graphene-experiments",bookSignature:"Sergey Mikhailov",coverURL:"https://cdn.intechopen.com/books/images_new/57.jpg",editedByType:"Edited by",editors:[{id:"16042",title:"Dr.",name:"Sergey",surname:"Mikhailov",slug:"sergey-mikhailov",fullName:"Sergey Mikhailov"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"371",title:"Abiotic Stress in Plants",subtitle:"Mechanisms and Adaptations",isOpenForSubmission:!1,hash:"588466f487e307619849d72389178a74",slug:"abiotic-stress-in-plants-mechanisms-and-adaptations",bookSignature:"Arun Shanker and B. Venkateswarlu",coverURL:"https://cdn.intechopen.com/books/images_new/371.jpg",editedByType:"Edited by",editors:[{id:"58592",title:"Dr.",name:"Arun",surname:"Shanker",slug:"arun-shanker",fullName:"Arun Shanker"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"878",title:"Phytochemicals",subtitle:"A Global Perspective of Their Role in Nutrition and Health",isOpenForSubmission:!1,hash:"ec77671f63975ef2d16192897deb6835",slug:"phytochemicals-a-global-perspective-of-their-role-in-nutrition-and-health",bookSignature:"Venketeshwer Rao",coverURL:"https://cdn.intechopen.com/books/images_new/878.jpg",editedByType:"Edited by",editors:[{id:"82663",title:"Dr.",name:"Venketeshwer",surname:"Rao",slug:"venketeshwer-rao",fullName:"Venketeshwer Rao"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"4816",title:"Face Recognition",subtitle:null,isOpenForSubmission:!1,hash:"146063b5359146b7718ea86bad47c8eb",slug:"face_recognition",bookSignature:"Kresimir Delac and Mislav Grgic",coverURL:"https://cdn.intechopen.com/books/images_new/4816.jpg",editedByType:"Edited by",editors:[{id:"528",title:"Dr.",name:"Kresimir",surname:"Delac",slug:"kresimir-delac",fullName:"Kresimir Delac"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"3621",title:"Silver Nanoparticles",subtitle:null,isOpenForSubmission:!1,hash:null,slug:"silver-nanoparticles",bookSignature:"David Pozo Perez",coverURL:"https://cdn.intechopen.com/books/images_new/3621.jpg",editedByType:"Edited by",editors:[{id:"6667",title:"Dr.",name:"David",surname:"Pozo",slug:"david-pozo",fullName:"David Pozo"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}}]},chapter:{item:{type:"chapter",id:"59758",title:"Reverse Flotation",doi:"10.5772/intechopen.74082",slug:"reverse-flotation",body:'\nCoal is a type of sedimentary rock, which exists in nature in the form of black-dark gray and brown-black color and consumed as fossil fuel. Besides, coal possesses carbonated plants, and its proportions in terms of weight and volume are more than 50 and 70%, respectively [1].
\nRaw coal is enriched by different beneficiation methods that are mainly gravity-based separation and flotation. In gravity-based separation, undesired substances, which are not compound of coal, might be reduced but it could not be effective on ingredients being in internal structure of coal. It is dangerous to consume raw coal as fossil fuel for environment due to high amount of sulfur ingredients, because impurities like sulfur produces harmful gases after heating process. Therefore, in order to remove these undesired contents, flotation is applied as an enrichment method.
\nFlotation, as the name implies, is expressed like separation of substance in compound form by floating process. Floatability of material is crucial aspect for efficiency of flotation. For coal mineral, some of them have natural floatable properties because of its nature, but some others do not possess an inherent floatability because of its internal structure properties [2, 3, 4]. The surface texture of coal particle may involve both hydrophobic and hydrophilic zones. Thus, domination of this zones is one of the criteria which decides whether coal is floatable or not [5, 6].
\nAnother criterion for defining floatability of coal particle is moisture content. For example, lignite, which involves 70–80% carbon, has high moisture content and extremely less hydrophobic disposition. The chemical structure of lignite is altering due to elimination of polar groups like hydroxyl and carboxyl groups, and natural moisture content decreases during the transition from lignite to bituminous coal. As a result, coal comes in position of more hydrophobic. Moreover, the content of carbon is in relation with hydrophobicity of coal, too. In the range of 81–89% of carbon content, polar character loses its influence, and coal becomes more hydrophobic. Hydrophobicity of coal reaches its maximum level in 89% of carbon content, and it decreases slightly when the carbon content climbs up from this level. The flotation is directly related with the floatability of particles, so higher carbon content makes conventional flotation process easier [7, 8].
\nIn addition, flotation efficiency is directly related with the properties of the inorganic and organic mineral impurities existed in coals and amount and dispersion of gangue mineral inclusion. It is not possible to remove these finely dispersed impurities inclusion by applying physical methods [9], so flotation should be taken in consideration inevitably in the manner of protecting environment and recovering valuable minerals.
\nIn this respect, flotation is playing significant role in supplying raw materials for various industries. More than 2 billion tons of minerals and fine coals are being processed annually by using flotation in worldwide [10]. For this reason, flotation becomes one of the most important methods for enrichment of minerals and is commonly used in the world [10, 11, 12, 13]. At the same time, flotation is utilized for finely-grain-sized coal upgrading [14, 15, 16, 17, 18], fly ash decarburization [19], and wastewater treatment [20]. Since coals and ore are liberated in fine grain size, tendency to flotation in mineral processing increases [21].
\nFor environment, sulfur and ash content of coal is too important because heating process leads to propagate harmful gases to the environment. Flotation is one of the effective methods for desulfurization and deashing of raw coal having high ash and sulfur content [22]. Flotation properties depend on the surface texture and other features of particle, so to make particle float or depress in pulp, some different reagents are governed. In conventional flotation, oily collector and frother are used, and these reagents are conditioned in a period of time [23, 24]. In flotation of low rank coal, it is difficult to obtain good result using oily collector due to surface of minerals with low surface hydrophobicity [23]. For this reason, collector consumption is much more in flotation of low rank coal compared with high rank ones [25]. In low rank coal flotation, in order to increase performance, parameters like grain size, pulp density, reagents type and dosage, pulp pH, flotation and time conditioning, and air entrainment rate should be investigated, and [9, 22, 26, 27] most proper condition should be determined with respect to results of them. In addition to conventional flotation method, reverse flotation is also applied on enrichment of minerals.
\nThe reverse flotation was commenced to investigate in 1950s [28, 29]. In following studies after 1950s, different researchers also continued to work on that concept [30, 31, 32, 33, 34] and still have been proceeding [4, 25, 27, 35, 36, 37, 38, 39, 40, 41, 42, 43]. However, researchers have not understood completely how particles inside the pulp interact with each other, yet because there are many uncertain factors that influence the surface of minerals and coal existing in pulp. Foremost among these factors is that coal possesses different type of elements and behavior of these elements has not been identified; thus, theoretical and experimental verification of interaction between elements is difficult. For that reason, more researches should be performed in that regard. Studies until current time are generally associated with reduction of pyrite and ash. However, recovery of valuable elements in coal should also be taken into consideration in the environmental aspect as well, so the objective of this study is to discuss the benefits of reverse flotation of coal for environment on the behalf of past researches.
\nAsh content is important for both environment and flotation efficiency. Ash content in coal can be eliminated by both physical methods and flotation process, but the presence of ash in internal structure of coal particle could not be removed by physical methods. To be able to remove impurities inside coal particle, reverse flotation is applied on coal. In reverse flotation, tailing is taken as clean coal, and concentrate is accepted as gangue minerals.
\nAsh content is crucial for coal flotation efficiency. Froth is the key element of determining flotation concentrate, and between concentrate froth and the ash content, there is a strong relation [44].
\nAsh reduction in reverse flotation of coal subjects have been developed for 30 years by some important researchers. Stonestreet, Pawlik, and Ding have performed intensive studies on ash reduction in reverse coal flotation. Stonestreet and Pawlik prepared their PhD thesis on reverse flotation of coal separately [4, 45] and continued his studies with Franzidis in advance [39, 40, 41]. In their experiment, clean coal with 7% ash and silica were mixed as a feed, and quantity of each element was same. From the results of experiments, reverse flotation process, 92% ash reduction was achieved from feed in which ash content was 54%. In depressed coal, ash content was 12%, whereas the recovery of coal is 27%. Results of experiment show that recovery of coal was not good even it was achieved that high ash reduction was obtained [39]. They continued their experiments to increase the recovery of coal by using three stage addition process, and for same substance, a product of 86% coal throughput involving 12% ash was obtained [40]. Within the matter of improving reverse flotation, they extended their studies and compared the laboratory column cell using synthetic feed mixture consisting coal and quartz. Thus, recovery capacity of coal was much better than in normal flotation [41].
\nLater, Ding and Laskowski took Stonestreet’s studies step further by adding dolomite and calcite as gangue minerals and surveyed the effects of factors on separation. They used dodecyl trimethyl ammonium chloride (DTAC) as a collector whose properties of separation are good when it is used minimum 6 kg/t [2]. After, Ding further continued to study on reverse flotation using DTAC on subbituminous coal, too. DTAC consumption was dramatically descended from 6 to 1.375 kg/t by applying polyacrylamide (PAM) and zero-conditioning time method. Besides, in order to improve selectivity, dextrin was governed, and the addition of tannic acids as a dispersant improved the quality of concentrate. For the feed ash content of 34.6%, the concentrate of 16.7% ash at 50.4% yield was acquired [36].
\nOn the other hand, Patil and Laskowski carried out their studies regarding to enhancing reverse flotation of coal. Patil drew on dodecyl trimethyl ammonium chloride (DTAB) in reverse flotation as collector, but used no depressant, first. Also, zero-conditioning time method was applied in their studies. Zero conditioning was accomplished by adding necessary quantity of DTAB in one step, immediately after system was exposed to the air. The logic behind the zero-conditioning time is that continuity of reverse flotation should not be interrupted in any case. Air bubbles formed from air introducing carried collectors, DTAB, during the flotation process. The entrainment of DTAB carried in air bubble demonstrated that reduction of ash from sub-bituminous coal (LS-26) from 34.7 to 22.9% with gangue yield of 36.8% by using any depressant. In the existence of depressant which was dextrin with 0.5 kg/t, the ash substance of LS-26 was reduced from 34.7 to 16.5% at the clean coal yield 55% [46].
\nGenerally, researchers have been seeking the behavior of ash particles under the participation of different reagents. They mainly focused on low rank coal like lignite due to their hydrophilic properties. Vamvuka also studied on lignite and oxidized coals and used dodecyl amine (DDA) with kerosene in flotation. Ash reduction of 18% with coal recovery of 80% was achieved [47]. Ozturk also proceeded their studies on reverse flotation of Turkish lignite samples involving high ash and sulfur content. They used ionic collector (Aero 3477) and obtained clean coal product of 29.04% ash at a combustible yield of 78.14%, while with non-ionic collector [kerosene], these values altered to 27.04 and 81.19%, respectively [27]. On the other hand, Zhang et al. also worked on reverse flotation, but used different reagents, as a collector dodecyl amine chloride (DAH), as a depressant corn starch, and as a further methyl isobutyl carbinol (MIBC), and observed the effect of particle size in the presence of soluble salt. When the highest reverse flotation performance was achieved, concentrate ash content of 11.30% was obtained with a combustible recovery of 65.29% [43]. Finally, Xia et al. applied reverse flotation on taixi oxidized coals. Dextrin was used as depressant, whereas hexadecyl trimethyl ammonium bromide (HTAB) was oriented as collector [42].
\nAlternatively, Li studied with sub-bituminous coal involving a significant amount of oxygen which causes to decreasing hydrophobicity. Due to being difficult to upgrade fine fraction in normal flotation, reverse flotation method in which minerals was made hydrophobic by adding collector, whereas coal was made hydrophilic by adding depressants. Li commenced experiments preparing mixture from coarse coal with fine quartz and medium size coal with fine silica. Ash content was dropped around 35% while recovering nearly 85% of combustible material by reverse flotation. The obtained results were much better than that acquired from conventional flotation method. However, when same procedure was applied to fine coal and quartz, separation was not as effective as tests prepared with coarse coal due to influence of hydraulic entrainment [48].
\nIn the early age of 1960s, Eveson was the first person who took attention on reverse flotation by removing shale from bituminous coal. After, reverse flotation had become popular among other researchers, and they started to focus on desulfurization of coal by using this method [30, 31, 32, 49].
\nThe presence of sulfur in coal might be found in three forms which can be categorized as organic sulfur, metallic sulfur, and sulfatic sulfur [9, 50, 51, 52, 53]. Organic sulfur in coal originates from carbonated plant, while metallic and sulfatic ones’ source is inorganic sulfur which exists among mineral compounds. The most common example of metallic sulfur is pyrite and it is called as pyritic sulfur. In addition to pyrite, other minerals may be involved in coal structure such as marcasite, galena, sphalerite, etc. For sulfatic ones, gypsum may be illustrated [54].
\nThe sulfur content is varying by different types of coal, and sulfur content accounts for pyritic and organic sulfur amount in coals. Even coal substances might be extracted from same ore bed, they possess different sulfur content. Pyritic sulfur may represent 20–80% of total sulfur content [38, 50]. Like ash, pyrite particles may also exist in internal structure of coal, so physical methods are becoming nonfunctional in removal of pyrite from coal substance [28]. Flotation was started to be applied to achieve desulfurization as well.
\nEach type of pyrite mineral shows different floatability properties, and the reason of that was investigated by some important researchers. Feurstenau considered that the cause of that variation is related with the formation of elemental sulfur. Because of being naturally hydrophobic [37, 55, 56], elemental sulfur can conduct with the surface of pyrite, and then, it may behave like a collector for pyrite. Oxidation of pyrite under proper condition forms elemental sulfur, and it is frequently observed in weathered coal, not in fresh coal [57]. Two basic reactions are standing below for expressing elemental sulfur formation from pyrite. These are as follows:
\nEq. (1) accounts for formation of elemental sulfur under microbial oxidation of pyrite, i.e. pyrite oxides in moist. To proceed the process of oxidation, acidic environment is necessary because pyrite-oxidizing bacteria can grow under this circumstance [37, 38]; that means, during the pyrite oxidation, iron sulfates, type of salts, constitutes, and these are known as flotation depressant [55]. These depressants can only be dissolved when acidic conditions are satisfied in pulp. On the other hand, unlike formation of sulfate format, if elemental sulfur formation is obtained at the end of oxidation, it is assumed that reaction of coal pyrite is similar to reaction of mineral pyrites, and flotation can be carried out on neutral pH range [37]. Second oxidation reaction may take place with water [58], and it is expressed in the form of;
\nIn both cases, if conditions are suitable, substantial quantity of elemental sulfur formation on pyrite sulfur can be observed even the elemental sulfur is normally an intermediate product in a series of reactions that are over with producing sulfate (\n
Pyrite has small hydrophobic tendency [55, 59, 60, 61] when its surface is unoxidized. With the presence of water, oxidation takes place on surface of pyrite and forms ferric hydroxide, which leads to decreasing hydrophobicity [62, 63, 64]. In pH range of 4.5–6.9, oxidation products of pyrite act like strong depressant [60], as it was mentioned before. In order to enhance hydrophobic tendency of pyrite, it is required to add some collector like xanthate [65] since floatability of pyrite intimately depends on pH, and highest floatability might be obtained in acidic pulp [38].
\nKawatra performed experiments on fresh coal and 1-year aged coal for different conditions. Fresh coal substances were exposed to different pH levels, and the percentage of froth weight being in directly proportional with floatability of pyrite were investigated. pH levels were defined as 8.3, 7.5, 2.3,2.2, and 2.0, and froth weights were found as 5, 4, 98, 98, and 99%, respectively. On the other hand, same procedure was applied on 1-year aged coal at -15°C, and lowest weight was attained around 37% when pH was almost equal to 6.8, whereas pH was dropped to 2.0, achieved weight dramatically increased, and equal to 92%. Lastly, 1-year aged coal substances were heated up to 100°C and tested in pH level 6.2 and 2.0, and results were 7% and 82%, respectively. From the results, it can be understood that freshly ground mineral pyrite is not readily floatable at neutral pH despite of being highly floatable in acidic pH. On the other hand, pyrite oxidation concludes with sulfate formation, which is not hydrophobic. If necessary conditions might be satisfied for forming elemental sulfur, pyrite can be floated. Also, it is shown that under certain condition, pyrite can be floated at neutral pH, but that is not a normal case. [37]
\nVanadium is strategic metal and has been extensively used in the field of steel and alloy industry. Tensile strength capacity of vanadium is too high, so 80% of vanadium are utilized for alloy steels, whereas remaining portion is applied in chemical industry [66, 67, 68].
\nVanadium is another element that might be recovered from coal by using reverse flotation. Coal vanadium element can be found in some coal minerals such as illite, muscovite, roscoelite, and kaolin in the form of isomorphism, whereas tantalite and garnet are appeared in the form of absorption [69]. In addition, quartz, calcite, and carbonaceous are found to be main gangues in stone coal [68]. For many studies, flotation has been popular topic for many years, but there are not much more available studies on pre-concentration of vanadium in low-grade coal by the method [70].
\nStone coal was exposed to the two stages of flotation processes to recover vanadium microelement. Mineral composition of coal was calcite, barite, quartz, and V-minerals. Reagents were sulfuric acid (pH regulator), oleic acid (Ca minerals collector), sodium silicate (dispersant), sodium fluorosilicate (SFF and depressant), melamine (EA and V minerals collector), dodecyl amine (DDA and V minerals collector), octadecylamine (DC and V minerals collector, terpenic oil (frother)). pH was kept between 7 and 8, and water glass was used as depressant (2000 g/t). Besides, oleic acid was taken 200 g/t as collector [70].
\nAt the end of this study, selective separation of vanadium-bearing minerals can be achieved in pH 3 using melamine (EA). The final vanadium concentrates with V2O5 grade of 1.88% and recovery rate of 76.58% are obtained by desliming-flotation process and 72.51% of the raw ore is rejected as tailings [70]. Also, results of other tests demonstrate that grade and recovery of V2O5 concentrate are 1.32% and 88.38, respectively, and tailing yield is 38.36%. On the other hand, recovery and grade of carbon mineral which may be used as fossil fuels are 75.10 and 30.08%, respectively [71].
\nAlthough vanadium recovery from stone coal is exploring recently by researchers, studies have already been demonstrated how well vanadium is recovered and obtained clean coal simultaneously.
\nCoal quality is determined by many properties, but major factor is coal rank. The rank of coal is identified by the percentage of fixed carbon, moisture (water), volatile matter, and calorific value in British thermal units after sulfur and mineral matter content have been subtracted. Coal types that might be ordered from lowest to the highest rank are lignite, sub-bituminous coal, bituminous coal, and anthracite [72]. Rank directly influences floatability of the coal since chemical structure changes due to elimination of polar groups during coalification process. At the end of this process, carbon content increases, and result in increasing hydrophobicity [73, 74]. Although, rank and floatability are directly proportional, highest hydrophobicity is achieved in bituminous coal, not anthracite, which has highest coal rank, but difference in floatability is not significant between them [75, 76]. Bituminous coals are enough hydrophobic to be floated in further without collector, but in order to improve coal recovery, collector oil is governed [77] even it reduces the coal rank [78].
\nMoreover, degree of the oxidation of the coal surface is essential for hydrophobicity. It leads coal to act like lower rank coal whose hydrophobicity is lower [4, 79, 80]. However, there are some cases that oxidation increases in the floatability of coal like freshly cleaved coal surfaces. Short-time air exposure may increase hydrophobicity due to drying of the coal surfaces which then becomes more difficult to wet [9].
\nCoal is composed of many different minerals that influence type of beneficiation method and its applications. These materials cannot be removed from coal totally by using conventional method [81]. Coal has heterogeneous structure, but is mainly formed from inorganic materials such as clay, quartz, sulfides, and sulfates [82, 83]. Mineral content determines the coal grade, and its rate should be less than 50% to be accepted as coal [54]. There are more than 120 minerals involved in coal, and primary ones regarding their degree of presence are quartz, kaolinite, illite, montmorillonite, chlorite (may contain Mn), clays (may also contain Be, Ni, and other trace elements), pyrite (may contain As, Cd, Co, Hg, Ni, Sb, and Se), calcite, and siderite (may contain Mn); not common ones are analcime, apatite, barite, chalcopyrite, clausthalite, crandallite, floricide, gorseksit, goyasite, dolomite, feldspar, galena, marcasite (may contain same elements as pyrite), monazite, rutile, sphalerite (may contain Cd), xenotime, and zircon; and rare ones are chromite, gypsum, gold, gibbsite, rock salt, magnetite, and muscovite [72]. Seventy-six elements of periodic table can be found in coal substance. Some of these are trace elements and their ratios are expressed with ppm. Some trace elements may be concentrated in specific coal bed, which make that bed a valuable resource for those elements such as silver, zinc, or germanium [84]. However, some elements have potential to damage environment like cadmium or selenium if their concentrates are more than trace amounts. Trace elements associated with clays or pyrite are removed from coal by flotation process, and it is significant to dispose all trace element with in the manner of environment and recovery of valuable elements. Nevertheless, except for gypsum, the various forms of ash and germanium, recovered minerals have not been used commonly [72].
\nIn addition to rank and mineral matter, maceral also affects the flotation of coal since coal hydrocarbon structure and hydrophobicity are influenced by maceral content [78, 85]. The macerals consist of lithotypes, and their proportions vary. The properties of lithotypes also differ from each other. Macerals are classified into groups according to dominant components, which are vitrine, inertinite, or liptinite, and has different hydrophobicity. For example, the lithotype fusain involving inertinite group macerals is generally the least floatable, whereas vitrian involving vitrinite group macerals is the most floatable [75]. Studies associated with maceral recovery proved that it is possible to regain good volume macerals without much loss of combustible value [83]. The studies on floatability of coal macerals were appeared at the beginning of 1950 by Horsley [8] and Sun [86]. According to Burdon, maceral content changed with increasing time flotation [87]. Even in same flotation cell, maceral content could vary when samples were taken from different place of it [3] because the macerals are the basic microscopic, physically distinct, and chemically different constituents of the carbonaceous matter in coal, which originate from material deposited in the primeval swamps [83]. Due to variance in maceral content, it is essential to define coal nature and response each maceral during the flotation. Based on maceral content in clean coal, the use of coal can be optimized. For example, high liptinite content increases the calorific value, whereas high inertinite content in concentrate stimulates increase in fixed carbon [88].
\nRank, mineral content and macerals are influencing the flotation performance and type because these are essential parameters for floatability of coal. Reverse flotation can be optimized for low rank coal because low rank coal can be suppressed more easily since hydrophobicity of low rank coals are more less due to its polar structures. In order to recover valuable minerals and remove hazardous minerals at the same time, reverse flotation is again proper way because mineral content of low rank coal is more compared to high rank coal, so minerals might be floated without taking much more effort. Lastly, macerals can be divided into some groups according to compounds content as it was mentioned before. Coal with lowest floatable maceral, fusain, may be upgraded by using reverse flotation, too.
\nThe pH has great importance in flotation because pH of liquid phase influences the surface characteristics and behavior of mineral and induces minerals to absorb all types of reagents on the surface. Response of reagents to the pH is essential for flotation, and there are no standard pH values for particular minerals in flotation. Instead, it is generally expressed with range for flotation of specific minerals, and it may differ according to participating reagents. For this reason, this may become complicated and needed to perform sensitive when highly selective products are required. Like coal reverse flotation, effects of hydroxide ions (OH−) and hydrogen ions (H+) ions are not only important for floating mineral matter but also important for suppressing coal [89]. Mineral surface can be altered with adjusting these ions in pulp. Minerals in pulp can be charged positively or negatively by arranging pH regarding the isoelectric point (IEP). When the pH is higher than IEP, minerals charge negatively, on the contrary, opposite actions will take place in mineral charging. Zeta potential is related with absolute changing in pH with respect to IEP, so it increases slowly [90, 91].
\nThe pH plays important role in pyrite removal, which is hazardous mineral for environment. Mineral pyrite and coal pyrite act different. Inherently, mineral pyrite is floatable, and it loses its floatability when pH is greater than 5.0. When the pH range is between 5 and 9, the recovery of mineral pyrite is not noticeable even neutral oil collectors are utilized to render mineral pyrite floatable. Although same fashion is used for coal pyrite, it does not act as mineral pyrites. In the pH range of 2.2–8.8, coal pyrite can be recovered 31–43%, whereas mineral matter pyrite can be achieved to regain 99% over the same pH range. Kawatra carried out microscopic examination of coal pyrite flotation and resulted in floated materials that were coal and locked coal/pyrite particles. Therefore, it is assumed that coal pyrite was floated due to attachment to coal [38]. Chander and Aplan performed studies to prove that pyrite is inherently less floatable due to exposed oxidation during purifying from coal which may result in destroying floatability of pyrite [34]. The studies show that coal pyrite may be floated due to locked or entrained particles [38]. Some experiments were handled by Kawatra to examine the effects of pH with using different reagents. In the first experiment, the pulp pH was arranged lower than 4.0, and fuel oil was used as collector for mineral pyrite. Flotation could be achieved with the range of that pH, but native floatability was entirely lost with higher pH values. In second trial, coal pyrite was tried to be floated. However, coal pyrite may behave like mineral pyrite, and it was not recovered at neutral pH range [38].
\nThe effects of surface and solution chemistry of Fe(II) and Fe (III) ions on the flotation of both mineral and coal pyrite with xanthate were investigated based on flotation output, zeta point measurements, and thermodynamic calculations. The results showed that existence of ferrous and ferric ions induced pyrite depress in pH range 6–9.5. Coal pyrite was recognized non-floatable above pH 6 due to large number of ferrous ions resulted from pyrite oxidation. Moreover, thermodynamic calculations demonstrated that formation of ferric hydroxyl xanthate leads to reducing floatability of pyrite when the pH is greater than 6.0 [92].
\nOn the other hand, some additional experiments have been performed for different types of minerals existing in coal structure. As it is well known that materials vary between each other with respect to their properties. Like pyrite, ash also can be recovered by reverse flotation along the different pH ranges. Stonestreet performed studies on ash reduction by applying reverse flotation method on quartz coal mixtures with same amount. The result of their studies showed that maximum ash reduction was succeeded using talk water whose pH was equal to 7.6 [4]. After, Pawlik also touched upon ash reduction with different coal substances. Sub-bituminous, bituminous, and oxidized bituminous coal were objective of reverse flotation with different pH ranges. At first, bituminous coal were exposed to different pH ranges, and optimal results for normal and oxidized coal differed. For normal bituminous coal, the flotation yield went into decline for higher pH values than 9.5. However, sharp decrease was observed when pH level becomes higher than 4.0 for oxidized bituminous coal sample. Besides, different tests were performed for sub-bituminous coal/silica mixtures, and for these tests, optimum pH range was determined between 8.3 and 8.6 [25]. Moreover, Ozturk mainly focused on ash reduction by reverse flotation of lignite, and they achieved maximum level of reduction at neutral pH range around 8 [27]. Same with Ozturk, Zhang also implemented reverse flotation on lignite sample at neutral pH level [73]. Lastly, sub-bituminous coal/quartz mixture with ratio 7:3 was subjected to the test, and all tests were done at neutral pH level [48]. Some additional examples are given from different pH ranges to represent bad results. For example, the low ash content of concentrate was obtained around 10.5 pH value due to optimum flotation of calcite and dolomite around this pH [93].
\nAs well as ash and pyrite, some other valuable minerals can also be regained by reverse flotation throughout different pH levels. Ding worked on sub-bituminous coal sample with 48.5% ash content and gangue minerals such as calcite dolomite and silica with the ratio of 7:1:1:1, respectively. These gangue minerals were intended to be floated. In first study, when pH was 10.4, these gangue minerals can be floated [35], whereas in second test, zero-time conditioning was also taken into consideration, and maximum yield was achieved at the 7.5–8.4 pH range [36]. Wang also tried to float calcite as well as vanadium, which has great value in industry. For calcite, pH level varied between 7 and 8, while it was 3.0 for vanadium [70].
\nTherefore, importance of pH is clearly explained by studies, and more research should be carried out to take a step further in reverse flotation.
\nThe most important criteria of mineral processing is associated to size of liberated mineral particle. The performance of flotation process depends on the degree of liberation of mineral in fine fraction. For this reason, flotation is applied to minerals that are intended to recover or remove from coal. Coal has a complex structure and possesses various minerals. Although the particle size of coal is generally less than 0.5 mm, liberation may not be achieved in that fraction size, so grinding may become inevitably for well separation. Hence, it is compulsory to apply flotation on coal due to liberation in fine fraction phase. However, finer fraction does not always mean that every parameter related with flotation is obtained in well range. There is a trade of between fraction size and performance of flotation. In Table 1, some studies with different coal type associated with various fraction size are demonstrated.
\nCoal type | \nParticle size (micron) | \nFloated minerals | \nReference | \n
---|---|---|---|
Sub-bituminous coal/quartz | \n150–200 (coarse coal), 74–120 (medium size coal) | \nMineral matter | \n[50] | \n
\n | −38 (fine coal), −200 (raw coal) | \n\n | \n |
\n | −56 (fine silica), −200 (coarse silica) | \n\n | \n |
Lignite with 42.34% ash content | \n−425, 250–425, 150–250, 150–74, 74–45, −45 | \nAsh | \n[43] | \n
Lignite | \n100 (86% of material finer mineral than 100 micron) | \nAsh | \n[27] | \n
Low grade stone coal (mass fraction) | \n−38, 38–50, 50–74, 74–154, 154–300, +300 | \nCarbon, vanadium | \n[71] | \n
Low grade stone coal | \n−38, 38–50, 50–74, 74–154, 154–600, 600–1500, +1500 | \nCarbon, vanadium | \n[70] | \n
Taixi oxidized coal | \n250–500, 250–125, 125–74, −74 | \nMineral matter | \n[42] | \n
Lignite | \n+300, 300–75, −75 | \nAsh | \n[47] | \n
Particle size of minerals participating into the reverse flotation.
Zhang et al. studied on lignite which possessed 42.34% ash content by applying reverse flotation. Recovery amount and flotation performance can differ with respect to particle size. Maximum performance was obtained for −74-micron fraction size with the combustible recovery of 65.29% and ash content of 11.30% after 20 minutes flotation. However, maximum flotation rate constant was achieved in 150–250-micron range, and the maximum reverse flotation index efficiency was attained for −425 microns. Hence, combustible recovery increased with increasing size fraction but meanwhile the concentrate ash content also increased particularly for finer particle sizes [73]. For finer fraction, slime problem appears. Because of that reason, there must be performed detailed studies for finer fraction flotation in order to obtain optimum results.
\nThe purpose of using reagents is to change the surface properties of minerals to adjust which material is floated and depressed. In this concept, regulator reagents (pH adjustor, activator, depressants, and dispersants) are entrained into flotation process to improve quality of selectivity and separation. In Table 2, reagents are demonstrated in three groups: depressants, collectors, and frothers. Most of reverse flotation experiments are listed, and for each test, available used reagents are indicated (Table 3).
\nCoal type | \nDepressant | \nCollector | \nFrother | \nReference | \n
---|---|---|---|---|
Bituminous coal | \nInorganic oxidants | \nOctylamine, CTAC, FAA, CTAB, CDBAC, LPC | \nMIBC | \n[29] | \n
Subbituminous coal | \nNot used | \nDTAB | \nMIBC* | \n[45] | \n
Bituminous & sub-bituminous coal | \nDextrin | \nDTAB, PAM | \nDTAB | \n[94] | \n
Bituminous & sub-bituminous coal | \nDextrin | \nDTAB | \nMIBC | \n[46] | \n
Sub-bituminous coal | \nDextrin | \nDTAC | \nnot used | \n[36] | \n
Sub-bituminous coal | \nDextrin | \nLilaflot D817M | \nMIBC | \n[48] | \n
Clean coal and silica mixture | \nHumic acids (HA) | \nDTAB | \nMIBC* | \n[45] | \n
Calcite, dolomite, silica, and raw coal | \nDextrin | \nDTAC | \nNot used | \n[35] | \n
Quartz and clean cooking coal mixture | \n\n | HTAB, HPYC | \n\n | [39, 40] | \n
Taixi oxidized coal | \nDextrin | \nHTAB | \n– | \n[42, 95] | \n
Quartz and clean cooking coal mixture | \n\n | HPYB | \n\n | [39] | \n
Lignite coal | \nNot used | \nAero-3477 (anionic collector), kerosene | \nPine oil | \n[27] | \n
Mineral pyrite | \nNot used | \nFuel oil | \nMIBC | \n[37] | \n
Pittsburgh coal | \nNot used | \nFuel oil | \nDowfroth 200 | \n[37] | \n
Mineral pyrite, coal | \nNot used | \nFuel oil | \nDowfroth 200 | \n[48] | \n
Quartz and clean cooking coal mixture | \nDextrin | \nDTAB | \nMIBC | \n[39, 40] | \n
Lignite coal | \nNot used | \n(Cationic; DDA, TTAB) | \nMIBC | \n[47] | \n
\n | \n | Anionic; SDS, non-ionic (2-ethyhexanol)/kerosene | \n\n | \n |
Lignite coal | \nCorn starch | \nDAH | \nMIBC | \n[43] | \n
Low grade stone coal | \nSodium silicate | \noleic acid, EA, DDA, DC, Mixed Alimine | \nTerpenic oil | \n[70, 71] | \n
Silica and raw coal mixture | \nHumic acids (HA) | \nDTAB | \nMIBC* | \n[25] | \n
Use of reagents in reverse flotation.
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Abbreviations.
Collectors are the reagents, which cause to arranging hydrophobicity of material. Collectors can be observed into two main topics that are ionic and non-ionic collectors. Non-ionic collectors are organic compounds formed from hydrocarbon chains having no neutral and polar groups, whereas ionic collectors are divided into two groups, anionic and cationic. The surface properties of minerals determine the reagents selections, and after necessary conditioning is done, flotation process starts. Some of the preferred collectors in reverse flotation are DTAB, HTAB, DTAC, and so on. On the other hand, PAM and ferric silicate were governed besides collector in order to increase activation of them. On the other hand, depressants are the reagents which are added to the pulp to make mineral surface more hydrophobic. As depressants, commonly used reagents in coal reverse flotation are dextrin, humic acids, and corn starch. Frothers are utilized for forming small size bubbles and durable forth which can bear floated minerals without getting any damage during transportation process. In reverse flotation, most common reagents are MIBC, and pine oil, terpenic oil, and Dowfroth 200 follows it. On the other hand, the use of frothers is not compulsory for reverse flotation because some collectors possess foaming agents.
\nAlternatively, Yi et al., stated that waste cooking oil (WCO) can be converted into a bio-flotation agent (BFA), which can be replaced with diesel improves a new coal flotation agent with Zr-SBA-15 catalyst. Pilot program data demonstrated that WCO to BFA brings saving energy by 13%, and CO2 emission by 76% as well as production cost when compared with petro-diesel use [96]. As a new trend, environmental aspects should be considered so that less harmful collectors should be employed within the manner of reducing the damage to environment, and in this respect, more studies should be handled to overcome environmental issues.
\nFlotation was developing at the end of 1800s, and reverse flotation was first tried in 1960s. Although not much researcher paid attention on reverse flotation issue, they contributed to literature significantly through past 50 years. With respect to these results, it is inevitable to reach success by reverse flotation.
\nSO2 gases are the main triggering factor of acid rains due to propagating toxic gases after burning treatment. Sulfur gases may be found in coal in the form of organic and mineral sulfur (pyrite, marcasite, galena, and sphalerite) and sulfate (Gypsum—CaSO4\n
I would like to express my appreciation to Bilal Umut Ayhan (Master of Science student at Middle East Technical University) who provided great help on preparation process of this chapter.
\nPhotoacoustic imaging (PAI) is a novel method of obtaining spectral images of chemical constituents of a sample or a scene, to gain valuable insight into its structure and dynamics. It is based on the technique of photoacoustic spectroscopy (PAS) and covers the entire spectral range from the ultraviolet to the infrared. When light is incident on a sample, photons can be either absorbed, transmitted, or reflected, and the PAS technology focuses on the amount of absorption and its subsequent release as heat. PAS is an extremely sensitive detection technique as it can detect molecular concentrations below the parts per billion (ppb) level. This technique emerged from the discovery of the photoacoustic effect by Graham Bell in 1880 during his attempt to transmit sound over a beam of sunlight [1]. However, it remained dormant for almost a century until the advent of tunable lasers in the 1970s and was successfully used by Kreuzer and Patel for the trace detection of atmospheric pollutants [2].
Bell succeeded in wireless audio communication about two decades before the radio transmission. He used the newly discovered selenium cell in the receiver in view of selenium’s property to react to modulated intensity of sunlight incident on it, as the resistance of selenium crystal depends on the incident light. A flexible mirror was attached at the speaking end of the photophone that created slight deviation of the beam of light reaching the receiver end. This led to variation of intensity at the selenium receiver, which acted like an optical version of the electric coil in the telephone receiver, converting the intensity modulated light back into sound. Bell performed many experiments and observed that sound waves were also produced directly from a solid sample when exposed to a periodically modulated beam of sunlight as illustrated in Figure 1. A hearing tube, whose other end was tightly attached to the open end of a transparent glass test tube with sample placed at its closed end, could be used as a photophone. When a beam of sunlight focused on the sample was rapidly interrupted with a rotating slotted wheel at an audible frequency, the intensity of sound in the hearing tube was dependent on the type of material. The loudest sound was heard when the sample was carbon black, leading to the conclusion that photoacoustic effect was caused by the absorbed light energy which subsequently heats the sample.
Illustration of photoacoustic effect with periodically chopped light incident on carbon black sample cell fitted with a hearing tube.
During Bell’s visit to England in 1880, John Tyndall performed the photoacoustic experiment in gases, and although the photoacoustic effect was confirmed, Tyndall was of the view that it was caused mainly by the radiant heat [3]. Bell was driven by rare intellectual curiosity to learn, and it led him to invent the spectrophone to find out the wavelengths that were more efficient for the radiant heat [4]. For this purpose he converted a prism spectroscope into a spectrophone by replacing the eyepiece of the telescope with a hearing tube in which a thin wire mesh coated with lampblack was fitted in the position of the cross wires (see Figure 2). When the incident sunlight was interrupted by a mechanical chopper, the hearing tube produced sound whose frequency was equal to the periodic intermittence of light. The loudness of sound, however, varied in accordance with the intensity of the solar spectrum, being maximum in the green-yellow region and decreasing at both the red and violet ends, and observations were made by fixing the position of the telescope in different spectral regions of the solar spectrum. These observations confirmed the fact that the photoacoustic effect is due to optical absorption, since lampblack totally absorbs light at each wavelength. On the basis of his observations, Bell made the prophetic statement about the great importance of photoacoustic spectroscopy in the infrared.
Alexander Graham Bell and his spectrophone.
The interaction between light and matter giving rise to photoacoustic effect has three distinct features. (1) The absorbed energy of optical radiation is converted into heat. (2) At the site of optical absorption, there is a temporal rise and fall of temperature. (3) The expansion and contraction following these temperature changes lead to periodic pressure variation to generate sound.
The heat generation following optical absorption is caused by internal motions in molecules or those of the matrix in which atoms are imbedded in condensed matter. In the quantum mechanical description, an excited molecular state reached by the optical absorption has two channels of relaxation. The radiative decay leads to optical emission, whereas the nonradiative decay causes heating. Thus a molecule, optically excited to a vibronic or a rovibrational state, loses a part of its excitation energy as heat leading to the photoacoustic signal. The photoacoustic spectrum is similar to the absorption spectrum, but its intensity at the exciting wavelength is proportional to the product of the absorption coefficient and the probability of nonradiative decay of the excited state.
Figure 3 shows the energy level diagram, in the Born-Oppenheimer approximation, of a typical organic molecule with an even number of electrons where total internal energy
Typical energy level diagram of an organic molecule where radiative processes A, F, and P stand for absorption, fluorescence, and phosphorescence, respectively. The nonradiative processes IC and ISC refer to internal conversion (IC) and intersystem crossing (ISC), respectively.
The rate of radiative transition
where
Two-level molecular model showing the rate of radiative rij and nonradiative cijtransitions between energy states E0 and E1.
Suppose the number density of molecules in the ground and excited states of Figure 4 is
We define the radiative and nonradiative lifetimes to be
In a similar manner, we find the following expression for the rate of change of ground state population density:
Hence from Eqs. (3) and (4), we get
In a photoacoustic experiment, we assume the incident light intensity I to vary slowly so that we may consider the upper and lower state population density changes to be an adiabatic interchange. Under this approximation we can set the left-hand side of Eq. (5) to zero. Since the total molecular density for the two-level system is
The spectral radiant energy density is directly proportional to the intensity I of the light source, and we define a constant
Mechanical chopping of the light source at a frequency ω can be expressed as the periodic “on” and “off” of the intensity by
If the gas is very weakly absorbing, we assume that most of the molecules are in state
For a molecular gas, its kinetic energy (K) has to be considered to get the total internal energy density
The rate of change of energy is given by
This change of energy is equal to the difference between the absorbed and radiated optical energy so that
We know that
Since the volume of the photoacoustic cell does not change in the experiment, and thermodynamic evaluation of the change in kinetic energy at constant volume gives
Since the specific heat capacity of gas
where
The pressure of the ideal gas
Since
Substituting for
Integrating Eq. (19) we get the following expression for photoacoustic signal, which is detected by a sensitive microphone:
Let us consider a cylindrical photoacoustic cell shown in Figure 5 where the light-absorbing solid sample is surrounded by optically transparent gas (air) on the front side and the backing material is a poor conductor of heat. The absorption of light, of a particular wavelength in the sample, generates heat by nonradiative transitions. The acoustic signal produced in the coupling gas is due to periodic heat flow from the sample. Rosencwaig-Gersho model for
Photoacoustic cell for a solid sample. Thermal waves originate from the point of absorption and travel toward the solid–gas interface to periodically heat a thin layer of gas (shown in red).
where
The temperature variation in the gas dies out within a thickness of
The temperature and pressure changes involved in the process of PA signal generation are extremely small, typically a micro- to millidegree and nano- to microbar, respectively. This was the reason that the field of PAS remained dormant till the advent of tunable laser sources and of sensitive audio detectors. A piezoelectric transducer or a sensitive microphone serves as the acoustic detector in photoacoustic cells used during the laboratory experiments. Recent developments in the field of miniaturization and the related progress in computer software have made it possible to use tiny quartz-based acoustic detection devices like cantilever and crystal tuning forks. The photoacoustic spectrometer using miniature lasers fitted with these novel detectors can be easily packed in a small box and can be used in the laboratory or in the field for standoff detection of hazardous materials. The heat generated by the photoacoustic effect produces density changes caused by temperature fluctuations in liquid and gaseous samples. In such cases, photoacoustic spectroscopy is carried out by detection of thermal lens formation using a probe laser. In the present case, however, we will confine to the detection of acoustic vibrations in the analysis of PA spectra.
One of the simplest PA cells for measurements on gases and vapors is made from a Pyrex tube fitted with quartz windows at the two ends. The length of the tube and location of the microphone are chosen to maximize the PA signal using the resonance of sound generated by the modulated light beam. The design of such a cell made from 62.5-cm-long Pyrex tube of 2.5 cm diameter and fitted with quartz windows at Brewster’s angle is shown in Figure 6(a). The cell was resonant at 335 Hz with maximum signal in the middle port for the microphone, and it was resonant at 669 Hz, rendering maximum signal at two ports symmetrically located on either side of the middle port. The microphone ports correspond to the positions of three possible antinodes of the stationary acoustic waves formed at the two resonant frequencies. Acoustic isolation was achieved by putting the cell in a wooden box filled with sand. Two of the ports, not in use during the measurement, were sealed using O-rings and flat Teflon disks. PA measurements were carried out with iodine vapor at room temperature in the presence of air at atmospheric pressure using 20 milliwatt Argon laser light at 514.5 nm. The chopping frequency of the laser light was varied between 27 and
Longitudinally resonant PA cell with three ports for microphone (a). PA signal for resonance at 335 Hz (b) and those for resonance at 669 Hz (c) and (d).
The photoacoustic spectrum of iodine vapor recorded using a Nd:YAG laser pumped tunable dye laser in the presence of atmospheric air and at 15 Torr is shown in Figure 7. Dye laser pulses used for the measurements were of 7 ns duration, 0.05 nm bandwidth, and
Photoacoustic spectra of I2 vapor in the wavelength region 492–552 nm (20,300–18,100 cm−1). The little downward arrow indicates the wavelength of exciting radiation that dissociates I2 into two iodine atoms (20,043 cm−1).
To make photoacoustic measurements on a flowing gas sample, such as in the case of pollution monitoring, one needs a different type of acoustic resonant PA cell as schematically illustrated in Figure 8. The U-shaped cell has a total length
The U-shaped resonant PA cell for detection of PA signal in a flowing air sample with special orifice for controlling the pressure inside the cell.
The airborne particulate matter (aerosols) remains suspended in air inside the PA cell shown in Figure 8 and has enough time to absorb radiation from the tunable laser beam. The absorbed optical energy is transferred as heat to the surrounding air, before the next laser pulse arrives, to build the stationary pressure wave in the PA cell. An instrument of this type can directly measure light absorption by aerosols over the entire range of sunlight entering the atmosphere. This type of PA cell has been used with a single laser as well as with two lasers of different wavelengths impacting the same gaseous sample [10, 11].
PA cells fitted with microphone, for recording PA spectra of solid samples, have been routinely used in the laboratory for almost four decades. One of the important aspects of homemade cells is to choose a material for effective shielding from extraneous sound. The design of a nonresonant PA cell is schematically shown in Figure 9. The main body of the cell has been constructed from a single block of aluminum with a cavity made from the bottom side for fixing the microphone along with its preamplifier. A cavity is made on the top of the block to put the sample cuvette whose open end is in the same horizontal plane as the microphone surface. A flat aluminum plate with double quartz windows in front of the sample cuvette is tightly fixed at the top of the main body with a very thin, suitably cut rubber sheet to make the chamber airtight. The thickness of the air duct connecting the sample and microphone is about 1 mm, and its total volume is less than 1 cc. The exterior dimensions of the stainless steel sample cuvettes are identical so as to tightly fit into their designated cavity. The sample cuvettes are, however, of varying depths to make measurements on powder samples of different thicknesses. Carbon black is used as the standard sample for recording the power spectrum of the excitation source of light to normalize the PA signals of the sample under investigation.
Design of nonresonant PA cell. (1) the main body of aluminum, (2) microphone and preamplifier chamber, and (3) sample cuvette.
The PA spectra of powder samples of RDX and TNT recorded with a PA cell of the above type are shown in Figure 10. The source of excitation used in these experiments was a rotational line tunable cw
CO2 laser-excited PA spectra of RDX and TNT powders. The persistent vibrational bands of the two molecules are seen for highly diluted samples in the lower half of the figure.
PA instrumentation for detection of liquid samples is somewhat complicated. A schematic diagram of the experimental setup for detection of harmful and dangerous pollutants in water is shown in Figure 11. The tunable dye laser beam, pumped by an excimer laser or a Nd:YAG laser, is focused into a 600 micron core multimode optical fiber for investigation on remotely located samples. The polluted water is kept in a quartz cuvette which is acoustically coupled to a piezoelectric transducer. The light exiting from the optical fiber is collimated into the quartz cuvette by means of a
Schematic PA spectroscopy system for trace detection of chemical species in polluted water.
In a PA cell, the acoustic energy is accumulated in a resonant cavity, but the principle of PA detection by a quartz tuning fork (QTF) involves the accumulation of the acoustic energy in a sharply resonant acoustic transducer [16, 17, 18]. Crystal quartz is an easy material for such a transducer because of its low loss piezoelectric property, and QTFs can be designed to resonate at any frequency between 4 Hz and 200
When a laser beam is focused at the center between the two prongs of the QTF placed in a gaseous sample, the absorbed optical energy converted into heat generates a weak acoustic pressure wave. When the laser beam is modulated at half the QTF resonant frequency (f), the pressure wave makes the two prongs move apart two times during each acoustic cycle. In this situation the QTF detects sound oscillations at the second harmonic of the modulation frequency due to two absorption events during each modulation period. The laser light is modulated at “
Experimental setup for gas phase PA spectroscopy with QTF detector. The excitation diode laser source is currently modulated at half of the QTF resonant frequency (f).
The use of QTF for solid phase PA detection in the laboratory requires a very thin film of the molecular sample to be adsorbed on the outer surface of one of the prongs. The absorbed laser light heats the sample, generating an acoustic wave at the prong’s surface interface with air. When the frequency of repetition of the incident laser pulse coincides with the mechanical resonant frequency of the QTF, the localized pressure variation sets the latter into vibration. The amplitude of this vibration and the resulting piezoelectric voltage are proportional to the amount of heat produced by optical absorption at the surface.
An experimental arrangement using the above concept is schematically shown in Figure 13 using a quantum cascade laser (QCL). The large wavelength coverage in the mid-IR region combined with narrow linewidth and powering up to tens of
Schematic experimental arrangement for solid phase PA spectroscopy using QTF detector with sample adsorbed on one of the QTF prongs. The function generator controls the pulse repetition rate of the quantum cascade laser (QCL) to be in resonance with the symmetric vibration of the QTF.
PA spectroscopy has been widely used in chemical sensing applications in environmental science and medical diagnostics. It is useful in rapid detection of illicit drugs, nerve agents, and hazardous biological materials. In a typical hospital environment, there is a need for evaluation of anesthetic gaseous components. Although hospital staff are exposed to much lower anesthetic concentration than the patients, this exposure extends over many years. Under inadequate hygiene conditions, people working in hospitals or factories often complain of headaches and fatigue due to traces of harmful gases in the environment. Illicit drug trafficking poses many challenges for detection of dangerous chemicals that threaten life and property. In the following sections, we will present examples of point detection as well as standoff detection of chemical compounds using PA spectroscopy.
Ethylene
The smells emanating from various parts of the body are unique to an individual, made up of specific chemical compounds that vary depending on age, diet, metabolism, and health. Near-IR diode laser at
Trace level detection of nitric oxide has many applications in medicine, biology, and environmental science. CO laser was the first to be used by Kreuzer and Patel [2] for PA detection of NO concentrations of 0.01 ppmV. Since its first detection in exhaled air [23], NO has been found to be a sensitive marker for asthmatic airway inflammation [24]. A QCL-based PA cell has been developed by Elia et al. [25], while Spagnolo et al. have reported a minimum NO concentration limit of 15 ppbV [26].
A
Morphine is the prototype narcotic drug, and it is the standard against which all other opioids are tested. An acetylated form of morphine, almost two times more potent than morphine itself, is known as heroin. Animal and human studies and clinical experience back up the contention that morphine is one of the most euphoric drugs on earth. Both morphine and heroin are used for pain medication, but both are addictive and identified as illegal drugs.
Microgram quantities of powders of morphine and heroin were used in a PA cell shown in Figure 9 and fitted with
CO2 laser-excited PA spectra of powders of heroin (on the left) and morphine (on right).
Photoacoustic imaging is an emerging technique that combines the high resolution of light and deep imaging capability of ultrasound. It is similar to hyperspectral imaging except for the fact that optical sensors are replaced by ultrasonic detectors that convert the sound waves into images. It has many applications as a noninvasive technique in medicine to produce molecular images of internal organs. It is based on the rapid production of heat, when the optical energy from a nanosecond laser pulse is absorbed in the tissue, causing thermal expansion and the generation of ultrasonic waves. The processes involved in the image formation are schematically illustrated in Figure 15, which show that it is a hybrid technique making use of optical absorption and ultrasonic wave propagation.
Schematic illustration of the principle and processes involved in photoacoustic image formation.
There are two basic conditions for efficient generation of the PA signal for imaging. The condition of “thermal confinement” requires the laser pulse duration
It can be shown that a nanosecond laser pulse impacting a biological tissue sample satisfies the conditions for PA imaging. Thermal diffusion length during the laser pulse is given by
Photoacoustic tomography (PAT) and photoacoustic microscopy (PAM) are the two methods of PA imaging. In the PAT mode, an expanded laser beam illuminates the whole sample, and laser photons are absorbed at various points in the sample generating ultrasonic waves. PAT acquires depth-dependent information by time-of-flight measurements of the acoustic waves. An ultrasonic transducer placed outside the sample detects the PA signal, which is measured either by moving a single transducer around the sample or by using an array of transducers. PA image is obtained from the data set of PA signals by using appropriate reconstruction algorithms in the computer. In the case of PAM, the laser beam is focused into a tiny volume, and ultrasonic waves from this localized region are imaged by the detector. To obtain a
Fluorescence microscopy is an effective tool in thin biological samples like single-celled organisms, but with slightly thicker samples, it becomes difficult to know where exactly the fluorescence originates. In a complex organism, like zebra fish, it is crucial to image deeper and deeper while the organism is kept alive. Fluorescent light emerging from the point of absorption suffers multiple scattering in the tissue on its way to the optical detector. This leads to loss of information on the origin and propagation path of the fluorescent light, giving rise to a blurred image and destruction of the spatial resolution. PA detection of optical absorption circumvents these limitations, because the sound waves travel through the diffuse biological media with much less distortion than light.
The experimental components used in PAM by Harrison et al. [30] are shown in Figure 16a. The laser beam, from a tunable source (L), is diverted down the
(a) Experimental setup for combined photoacoustic (PA) and ultrasound (US) imaging (with permission from Ref. [30]). (b) In vivo image of a section of the zebra fish brain and five transverse image slices through the hindbrain (with permission from Ref. [31]).
In the recording of images of Figure 16b, the zebra fish was held on a rotating platform immersed in water. The position of the laser focus was fixed at a particular depth inside the body of the sample, and the platform was rotated through 360° to record the two-dimensional sections [31]. The location of fluorescent protein mCherry (in red) is clearly seen in the image of the zebra fish brain at the top, and transverse image slices of the zebra fish hindbrain are shown in the lower half of Figure 16b, where each slice is separated by a depth of 0.5 mm inside the tissue.
PA imaging is emerging as a new diagnosis technique with specificity, high resolution, and enough imaging depth for early detection of prostate cancer. Ex vivo multispectral PA imaging has been carried out to differentiate between malignant prostate tissue, benign prostatic hyperplasia (BPH), and normal human prostate tissue. The preliminary results of investigations carried out by Dogra et al. [32] show that there was a significant difference in the mean PA intensity of dehydroxy hemoglobin (dHb) and lipid between malignant and normal prostate. There was also a significant difference in the mean intensity of dHb between malignant prostate and BPH. There was, however, no significant difference in HbO2, dHb, and lipid between normal prostate tissue and BPH. Laser radiation at 1064 nm and 1197 nm has been used to obtain PAT images, corresponding to optical absorption of hemoglobin and lipid, to determine the clustering prostate cancer tissue at each wavelength [33]. It was found that 1064 nm PAT in conjunction with ultrasound image is more effective in identifying prostate cancer biopsy targets than the PAT at 1197 nm.
This chapter starts with a brief history of photoacoustic effect and photoacoustic spectroscopy. A simple mathematical derivation for the generation of PA signal in gaseous and solid samples is followed by experimental methods. The design and construction of a variety of PA cells and detectors have been described along with their use in the investigation of gaseous, solid, and liquid samples. Some illustrative examples of trace detection of explosives and harmful chemicals have been discussed. A brief account of the principle and application of the emerging technique of PA imaging is discussed at the end of the chapter.
I am grateful to all the authors and scientists whose results have been cited to make the presentation meaningful. I am thankful to Dr. Punam Rai for taking care of my health, Sudheer for the help with the computer, and to my grandchildren, Leo and Mia, for their innocent inquiries during the course of my writing.
IntechOpen implements a robust policy to minimize and deal with instances of fraud or misconduct. As part of our general commitment to transparency and openness, and in order to maintain high scientific standards, we have a well-defined editorial policy regarding Retractions and Corrections.
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\\n\\nA Statement of Concern detailing alleged misconduct will be issued by the Academic Editor or publisher following a 3rd party report of scientific misconduct when:
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\\n\\nA Correction will be issued by the Academic Editor when:
\\n\\n3.1. ERRATUM
\\n\\nAn Erratum will be issued by the Academic Editor when it is determined that a mistake in a Chapter originates from the production process handled by the publisher.
\\n\\nA published Erratum will adhere to the Retraction Notice publishing guidelines outlined above.
\\n\\n3.2. CORRIGENDUM
\\n\\nA Corrigendum will be issued by the Academic Editor when it is determined that a mistake in a Chapter is a result of an Author’s miscalculation or oversight. A published Corrigendum will adhere to the Retraction Notice publishing guidelines outlined above.
\\n\\n4. FINAL REMARKS
\\n\\nIntechOpen wishes to emphasize that the final decision on whether a Retraction, Statement of Concern, or a Correction will be issued rests with the Academic Editor. The publisher is obliged to act upon any reports of scientific misconduct in its publications and to make a reasonable effort to facilitate any subsequent investigation of such claims.
\\n\\nIn the case of Retraction or removal of the Work, the publisher will be under no obligation to refund the APC.
\\n\\nThe general principles set out above apply to Retractions and Corrections issued in all IntechOpen publications.
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\\n\\nPolicy last updated: 2017-09-11
\\n"}]'},components:[{type:"htmlEditorComponent",content:'IntechOpen’s Retraction and Correction Policy has been developed in accordance with the Committee on Publication Ethics (COPE) publication guidelines relating to scientific misconduct and research ethics:
\n\n1. RETRACTIONS
\n\nA Retraction of a Chapter will be issued by the Academic Editor, either following an Author’s request to do so or when there is a 3rd party report of scientific misconduct. Upon receipt of a report by a 3rd party, the Academic Editor will investigate any allegations of scientific misconduct, working in cooperation with the Author(s) and their institution(s).
\n\nA formal Retraction will be issued when there is clear and conclusive evidence of any of the following:
\n\nPublishing of a Retraction Notice will adhere to the following guidelines:
\n\n1.2. REMOVALS AND CANCELLATIONS
\n\n2. STATEMENTS OF CONCERN
\n\nA Statement of Concern detailing alleged misconduct will be issued by the Academic Editor or publisher following a 3rd party report of scientific misconduct when:
\n\nIntechOpen believes that the number of occasions on which a Statement of Concern is issued will be very few in number. In all cases when such a decision has been taken by the Academic Editor the decision will be reviewed by another editor to whom the author can make representations.
\n\n3. CORRECTIONS
\n\nA Correction will be issued by the Academic Editor when:
\n\n3.1. ERRATUM
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\n\nA published Erratum will adhere to the Retraction Notice publishing guidelines outlined above.
\n\n3.2. CORRIGENDUM
\n\nA Corrigendum will be issued by the Academic Editor when it is determined that a mistake in a Chapter is a result of an Author’s miscalculation or oversight. A published Corrigendum will adhere to the Retraction Notice publishing guidelines outlined above.
\n\n4. FINAL REMARKS
\n\nIntechOpen wishes to emphasize that the final decision on whether a Retraction, Statement of Concern, or a Correction will be issued rests with the Academic Editor. The publisher is obliged to act upon any reports of scientific misconduct in its publications and to make a reasonable effort to facilitate any subsequent investigation of such claims.
\n\nIn the case of Retraction or removal of the Work, the publisher will be under no obligation to refund the APC.
\n\nThe general principles set out above apply to Retractions and Corrections issued in all IntechOpen publications.
\n\nAny suggestions or comments on this Policy are welcome and may be sent to permissions@intechopen.com.
\n\nPolicy last updated: 2017-09-11
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