Mass spectrometric study of nanofilm products Chemistry, exposure and health effects

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1 Mass spectrometric study of nanofilm products Chemistry, exposure and health effects Ph.D. thesis Asger W. Nørgaard, 2010 National Research Centre for the Working Environment, Denmark Department of Chemistry, University of Copenhagen, Denmark ISBN nr I

2 PhD thesis for public defence February 4 th 2011 at in Auditorium 2, at the H.C. Ørsted Insitute, Univeristy of Copenhagen. Evaluation Committee Associate Professor Bo Svensmark, Chairman, Department of Chemistry, University of Copenhagen, Denmark Associate Professor Marianne Glasius, Aarhus University, Denmark Professor Risto Kostiainen, University of Helsinki, Finland Supervisors Professor Peder Wolkoff, National Research Centre for the Working Environment, Denmark Professor Frants R. Lauritsen, Department of Pharmaceutics and Analytical Chemistry, University of Copenhagen, Denmark II

3 Preface With this thesis, I conclude my work as a PhD student at the National Research Centre for the Working Environment and Department of Chemistry, University of Copenhagen. The PhD program was initiated in October 2007 and has proceeded until December The period from January 2010 to April 2010 was spent at the Department of Chemistry, State University of Campinas (UNICAMP), Brazil in the research group headed by Professor Marcos N. Eberlin. My work has centred on the utilization of several mass spectrometric techniques to study coating products claiming to be based on nano- technology, namely the nanofilm products (NFPs). The thesis comprises two parts. In the first part, I am intending to give an introduction to NFPs as well as the techniques I used in my work. This is in order to give the reader a basic understanding of both the NFPs and how the results presented in my papers were obtained. The last part of the thesis contains résumés of the five manuscripts prepared during the PhD programme. The résumés are meant as quick overviews of the main results and are presented in a more accessible way than the, sometimes, rigid manuscripts. I wish to express my deepest gratitude to my supervisor at the National Research Centre for the Working Environment, Peder Wolkoff, for his incredibly kind and competent guidance and support. Likewise, I thank my supervisor at the University of Copenhagen, Frants R. Lauritsen, for being a great source of inspiration. Our discussions always left me in high spirits and with a clear sense of purpose. Special thanks to my colleagues at National Research Centre for the Working Environment, Per Axel Clausen, Vivi Kofoed- Søresen, Anni Vibenholt, Keld Alstrup Jensen, Ismo Koponen, Yahia Kembouche, Marcus Levin and Larisa Jelezneacova you guys are amazing! III

4 I also wish to thank Søren Thor Larsen, Maria Hammer and Gunnar D. Nielsen for their outstanding work elucidating the health aspects of NFPs. Christian Janfelt and Mario Benassi deserve my most sincere gratitude for sharing their knowledge on ambient mass spectrometric techniques, in addition to being very dear friends and colleagues. I look forward to our future adventures into mass spectrometry and allied topics. My visit to Marcos N. Eberlin s group at UNICAMP was the experience of a lifetime. Never have I experienced such a welcoming attitude; it was simply amazing! The three months I spent in Brazil were very rewarding - both personally and professionally. I am most grateful to Marcos and all the great people in and around the Thomson Lab, for making my stay in Brazil one of the absolute apexes of my time as a PhD student. Finally, I express my endless love and gratitude to my wife Maria and my little son Carl for enduring these past three years - especially the periods of my absence. Asger W. Nørgaard December 2010 IV

5 Abstract Nanofilm products (NFPs) are a relatively new type of surface coating for domestic and industrial use. NFPs are sprayed onto a surface, and a thin film is formed by self- organization during evaporation of the solvent. NFP induces non- stick properties in the treated surfaces, which reduce post- treatment cleaning efforts considerably. The formulation of the NFPs does not appear in the product information available from the distributors. Consequently, knowledge about the products was limited and insufficient for risk assessment when the products were introduced in the early 2000s. In order to provide information about the chemistry, exposure and health effects of NFPs, the National Research Centre for the Working Environment initiated a research project in The major part of this project focused on a thorough chemical analysis, which would form a basis for subsequent toxicological studies. The mass spectrometric investigations of NFPs, assessment of exposure during use and their health effects are included in this thesis. The results obtained are presented in five papers, which are summarized below. Exposure assessment (paper 1). NFPs were sprayed towards a target plate inside a closed stainless steel chamber with no air exchange. Released VOCs were measured by a combination of air sampling on a Tenax TA adsorbent, followed by thermal desorption GC/MS and GC/FID analysis and real- time measurements using a miniature membrane inlet mass spectrometer. Particles were measured using a Fast Mobility Particle Sizer and an Aerosol Particle Sizer. A number of VOCs were identified, including small alcohols, ketones and ethers, chlorinated acetones, a perfluorinated silane, limonene and cyclic siloxanes. The number of particles generated was of the order of to particles/cm 3 per g sprayed NFP and nano- size particles (diameter less than 100 nm) dominated. Identification of the film- forming components (paper 2). Ten NFPs from three different suppliers, analysed by ESI- MS/MS and GC- MS/MS, could be classified into three major groups (NFP 1-3). NFP 1 and NFP 2 contained hydrolysates and condensates of the organofunctionalized silanes 1H,1H,2H,2H- perfluorooctyl triisopropoxysilane and hexadecyl triethoxysilane, respectively. NFP 3 contained non- ionic detergents and abrasives as active ingredients. To verify the fluorosilane solution in NFP 1, a synthetic NFP 1 was prepared by hydrolysis and condensation of 1H,1H,2H,2H- perfluorooctyl triethoxysilane. After about 1 month in acidic 2- propanol, substitution of the ethoxy groups with isopropoxy groups had taken place and all silane was converted to di-, tri- and tetrasiloxanes. V

6 Evaluation of health effects (paper 3). NFP 1 and NFP 2 were investigated for airway irritation, airway inflammation and lung damage in a mouse inhalation model. BALB/cJ mice were exposed for 60 min to the aerosolized products at mg/m 3. NFP 1 induced a lasting concentration- dependent decrease of the tidal volume. A narrow interval between the no- effect level (16.1 mg/m 3 ) and lethal concentrations (18.4 mg/m 3 ) was observed. NFP 2 had no effect at the concentrations studied. Experiments with different types of perfluorinated silanes and siloxanes showed that the toxic effects did not arise solely from the perfluorination. The number of free hydroxyl groups in the silanes/siloxanes was also critical for the observed toxicity. Real- time monitoring of the film formation (paper 4). NFP 1 and NFP 2 were applied to glass, filter paper or cotton surfaces and the progress of the polymerization was monitored via easy ambient sonic spray ionization (EASI). Significant changes in the composition of hydrolysates and condensates of 1H,1H,2H,2H- perfluorooctyl triisopropoxysilane (NFP 1) and hexadecyl triethoxysilane (NFP 2) were observed over time. The abundances of the hydrolysed species decreased compared to the non- hydrolysed species and the heavier oligomers became relatively more abundant over a period of min. Analysis of NFPs by nebulization ionization and desorption ionization (paper 5). Electrospray ionization (ESI), atmospheric pressure chemical ionization (APCI), transmission- mode desorption electrospray ionization (TM- DESI), low temperature plasma (LTP) and nano- assisted laser desorption ionization (NALDI), were utilized for the analysis of NFP 1 and NFP 2. This was done to make a comparison and to characterize the NFPs in different states from liquid product to film. LTP was superior in showing the non- reacted content of the NFPs, while ESI, APCI and TM- DESI seemed to be characterized by artefact formation of condensation products during the ionization processes. NALDI was ideal for showing the larger siloxane structures formed during film formation. In general, the versatility of each of the methods was demonstrated, in addition to the advantage of utilizing more than one method for the analysis of reactive species. VI

7 Dansk Resumé (abstract in Danish) Nanofilm produkter (NFPer) er en relativ ny type af overfladebehandlingsprodukter til både industriel og privat anvendelse. NFPerne sprøjtes på en overflade og en tynd film dannes efterhånden som opløsningsmidlet fordamper. Den påførte film tilfører den behandlede overflade non- stick egenskaber, som reducerer efterfølgende rengøringsarbejde betragteligt. Den fornødne viden om produktformuleringerne til brug for risikovurdering af NFPerne, var ikke tilgængelig, da de blev introduceret på det danske marked i begyndelsen af 2000 erne. Derfor påbegyndte Det Nationale Forskningscenter for Arbejdsmiljø i 2006 et projekt, som havde til formål at tilvejebringe viden om NFPernes kemi og eventuelle helbredseffekter. Hovedparten af projektet var fokuseret på gennemgribende kemiske analyser, som skulle danne grundlag for toksikologiske studier. Denne afhandling omfatter massespektrometriske undersøgelser af NFPerne samt vurderinger af eksponering og helbredseffekter. De opnåede resultater er præsenteret i fem videnskabelig artikler, hvis indhold er summeret neden for. Eksponeringstudie (artikel 1). For at vurdere frigivelsen af VOCer og partikler under anvendelse af NFPerne, blev der udført en række spraytests i et lukket stålkammer. VOCer blev målt med både et direkte visende membran- inlet massespektrometer (MIMS) og sampling på Tenax TA adsorbent efterfulgt af termisk desorption GC/MS og GC/FID. Partikler blev målt med to direkte visende partikelmålere (fast mobility particle sizer og aerodynamic particle sizer). En række VOCer blev identificeret, herunder alkoholer, ketoner, kloracetoner, perfluorosilan, limonen samt cykliske siloxaner. Partikelfasen var domineret af nanopartikler (diameter under 100 nm) og der blev målt partikelkoncentrationer på mellem 3x10 2 og 2x10 4 partikler/cm 3 for hvert gram NFP frigivet i kammeret. Identifikation af de filmdannende forbindelser (artikel 2). Ti NFPer fra tre forskellige leverandører blev analyseret via ESI- MS/MS og GC- MS/MS. Da adskillige af produkterne tilsyneladende var ens, kunne de inddeles i tre overordnede grupper: NFP 1, NFP 2 og NFP 3. NFP 1 og NFP 2 indeholdt hydrolysater og kondensater af henholdsvis 1H,1H,2H,2H- perfluorooctyl triisopropoxysilan og hexadecyl triethoxysilan. NFP 3 indeholdt non- ioniske tensider og slibemiddel. NFP 1 blev syntetiseret ud fra 1H,1H,2H,2H- perfluorooctyl triethoxysilan i 2- propanol tilsat en lille mængde myresyre. Efter ca. 1 måned var alle ethoxygrupper udskiftet med isopropoxygrupper og alt silan var omdannet til di-, tri og tetrasiloxan. VII

8 Vurdering af helbredseffekter (artikel 3). NFP 1 og NFP 2 blev undersøgt for luftvejs irritation, luftvejs inflammation og lunge skader i en muse- inhalationsmodel. BALB/cJ mus blev eksponeret i 60 min til aerosoliseret NFP i koncentrationer fra 3,3 til 60 mg/m 3. NFP 1 resulterede i en varig koncentrationsafhængig reduktion af musenes lunge funktion (tidal volume). Endvidere blev der observeret et snævret interval mellem no- effect level (16,1 mg/m 3 ) og dødelig koncentration (18,4 mg/m 3 ). NFP 2 havde ingen effekt inden for det valgte koncentrationsinterval (3.3 til 60 mg/m 3 ). Yderligere inhalationsforsøg med forskellige typer af perfluorerede silaner og siloxaner viste, at de toksiske effekter ikke udelukkende kunne tilskrives perfluoreringen. Antallet af hydroxylgrupper i silan/siloxan strukturerne var også af afgørende betydning for den observerede toksicitet. Direkte monitering af filmdannelsen (artikel 4). NFP 1 og NFP 2 blev påført glas, filter papir og bomuld og filmdannelserne blev moniteret via easy ambient sonic spray ionization (EASI). Signifikante ændringer i forholdene mellem hydrolysater og kondensater for de tilstedeværende silaner/siloxaner kunne observeres over tid. De hydrolyserede species aftog i forhold til de ikke- hydrolyserede og større oligomerer blev relativt mere hyppige over en periode på min. Analyse af NFPer via ESI, APCI og desorptions ionisering (artikel 5). Electrospray ionization (ESI), atmospheric pressure chemical ionization (APCI), transmission- mode desorption electrospray ionization (TM- DESI), low temperature plasma (LTP) og nano- assisted laser desorption ionization (NALDI) blev anvendt til analyse af NFP 1 og NFP 2. Formålet var en sammenligning af de fem metoder samt karakteristik af NFPerne på forskellige stadier fra væskeprodukt til film. LTP viste sig at være de andre metoder overlegen mht. at vise begge NFPer i deres ureagerede form. Medens analyse med ESI, APCI og TM- DESI tilsyneladende afstedkom dannelse af kondensater i forbindelse med ioniseringsprocesserne. NALDI viste sig ideel til analyse af større siloxan- strukturer dannet under hærdningen af produkterne. Anvendeligheden af alle fem metoder blev demonstreret foruden fordelene ved at have flere metoder til rådighed ved analyse af reaktive forbindelser. VIII

9 Table of contents Introduction... 1 Nanofilm products... 1 Organosilanes: Applying functionality to inorganic structures... 3 Health effects of coating products... 5 Considerations on exposure and characterization... 6 Mass spectrometry... 9 Ionization techniques Electron and chemical ionization Electrospray ionization Atmospheric pressure chemical ionization Ambient desorption ionization techniques Desorption electrospray ionization Easy ambient sonic spray ionization Low temperature plasma Laser desorption ionization techniques Nano- assisted laser desorption ionization Mass analysers The quadrupole mass analyser The Time- of- flight mass analyser The quadrupole time- of- flight hybrid mass spectrometer (QqTOF) Mass accuracy Collision induced dissociation Other techniques Original research Exposure Assessment (paper 1) Identification of film- forming components (paper 2) Evaluation of health effects (paper 3) Real- time monitoring of the film formation (paper 4) Analysis of NFPs by ESI and desorption ionization (paper 5) Conclusions List of abbreviations References Included papers 1: Release of VOCs and particles during use of nanofilm spray products : Characterization of nanofilm spray products by mass spectrometry : Lung damage in mice after inhalation of nanofilm spray products : Real- time monitoring of the progress of polymerizationreactions directly on surfaces at open atmosphere by ambient mass spectrometry : Nebulization ionization and desorption ionization analysis of reactive organo- functionalized silanes in nano film products...92 IX

10 Introduction Nanofilm products Introduction Nanofilm products Consumer products for the treatment of shoes and textiles to obtain water and dirtrepellence have been available for many years. They usually appear as aerosol sprays for easy application to both absorbent and non- absorbent surfaces and may contain active ingredients such as wax and paraffins, siloxanes or fluorine polymers (1,2). In the early 2000s a new type of coating product was introduced in the Danish market. These products were marketed as being based on highly sophisticated nanotechnology and their range of applications was impressive. Everything from bathroom tiles and taps to shirts and ties could be treated, and the effects appeared almost magical (Fig. 1). The coatings induce water- pearling effects and considerably less cleaning is required since dirt, soap film and limescale cannot stick to the treated surfaces. The products are mainly delivered as pump- sprays for easy application and the treatment is very simple: clean the surface, apply the product, polish off residue after 30 min and let the coating seal for hours. The effects may last for 12 months or more. The easy- to- clean effect arises from a hydrophobic functionality incorporated in the film. The hydrophobicity (or surface free energy) of a surface can be visualized by the contact angle between a water droplet and a surface (Fig. 2). When the contact angle is below 90 the surface is hydrophilic and thus wettable for water. When the contact angle is above 90, the surface is characterized as hydrophobic, while it is ultra hydrophobic for contact angles of 150 and above. Water will, in the latter case, form small spheres on the non- wettable, water- repellent surface. Figure 1. Water droplets on cotton, wood and concrete surfaces treated with NFP. Figure 2. Contact angle (Θ), adhesiveness, wettability and surface free energy of a hydrophobic surface compared to a hydrophilic surface. Reprinted with permission from Ramé- hart instruments co. (www.ramehart.com) 1

11 Introduction Nanofilm products The high contact angle is possible since water molecules may have stronger interactions between themselves, namely hydrogen bonds, than with a hydrophobic, non- polar surface with which only van- der- Waals interactions are possible. So the cohesion of the water droplet outweighs its adhesion with a surface. Thus, a surface is said to have a high surface free energy if it is polar (facilitation of strong interactions with a liquid) and a low surface free energy if it is non- polar (weak interactions with a liquid). Alkane-, silicone- and fluorine- based materials are among the best known high- contact angle substances. The values for water contact angles on polypropylene (PP), poly(dimethylsiloxane) (PDMS) and poly(tetrafluoroethylene) (PTFE or Teflon) are 96.4, 95.8 and 104, respectively (3). The highest obtainable contact angle for water on a smooth surface is 120, obtained by regularly aligned and close- packed CF 3 groups (4). Higher contact angles can only be obtained if the hydrophobic surface is roughened. The combination of hydrophobicity and roughness for obtaining an ultra hydrophobic surface is known from the leaves of the lotus flower, hence the term Lotus effect (5). The lotus flower, a symbol of purity for religions in Asia, always appears clean and untouched by dirt and pollutants since its micro- structured, hydrophobic surface (Fig. 3) results in contact angles greater than 150. As a result, water droplets form pearls, touching the leaves with only a few percent of their surface, and this enables them to roll off very easily. Accumulated dirt is carried away as the drops roll off, thus making the leaves self- cleaning. In order to make a coating system that simulates the effects of the lotus leaves it is necessary to induce both hydrophobicity and roughness to a surface. One way of doing this is summarized in Fig. 4. This procedure involves a complex mixture containing epoxy- and perfluorinated silanes for the formation of a coating with hydrophobic functionality and nano particles to create a roughed surface structure. Figure 3. Computer- generated illustration of the micro- structured surface of a lotus leaf (top) and the self- cleaning leaf (bottom). From and www. futureprospects.wordpress.com Figure 4. Process for the preparation of low surface free energy coatings. Reprinted with permission from (6). 2

12 Introduction Nanofilm products Once the mixture is applied to a surface, the individual components are self- aligning during evaporation of the solvent (Fig. 5) by a thermodynamic process to minimize the free surface energy of the coating formed. For fluorine- containing compounds, the minimum free surface energy is achieved when they are at the interface towards the atmosphere, thus causing a diffusion of fluorinated silanes towards the surface during the tempering process of the coating. A coating produced in this manner is completely transparent and exhibits contact angles relative to water of up to 160, in addition to hardness and therefore high scratch resistance (6). However, it was later realized that simple alcohol solutions of hydrolysed alkyl- or perfluoralkylsilanes could be used as coating systems for a wide range of substrates. These simplified coating systems proved to be superior to those of the more complex mixtures containing nano particles. This enabled easy and relatively cheap production of coating products inducing easy- to- clean effects to a substrate by means of a ca. 20 nm film based on organosilanes (8). Thus, these products are referred to as nanofilm products (NFPs). Organosilanes: applying functionality to inorganic structures Organosilanes are a group of hybrid compounds comprising a structure- forming inorganic part and an organic part with a desired functionality (Fig.6). Silicon, a metalloid with the atomic number 14, is the base atom of the organosilane. Silicon is unique since, apart from forming partly ionic bonds with oxygen, it forms stable covalent bonds with carbon and thus bridges inorganic structures with organic functionality (8,9). Figure 5. Illustration of an evaporation- induced self assembly (EISA) process taking place after the application of an initial sol (bottom). The components of the initial sol are self- aligning into a final film (top) as the solvent evaporates. The inorganic precursor could be a silane with perfluorinated functionality. Reprinted with permission from (7). Figure 6. Model of an organosilane. Modified from (8). 3

13 Introduction Nanofilm products The reactions of silanes to form networks or nanoscale structures are referred to as the sol- gel process (10). Sol- gel is a wet- chemical technique used for the fabrication of materials starting from a chemical solution (sol). The solution acts as a precursor for structures (gel) of either discrete particles or polymeric networks. An example of a typical precursor is tetraethoxyorthosilicate (TEOS), which then undergoes hydrolysis and condensation reactions during the structure formation (Scheme 1). Hydrolysis occurs by the nucleophilic attack of the oxygen atom in water on silicon, forming silanols and alcohols as products. Hydrolysis is fastest and most complete when an acid or base catalyst is employed. The condensation reactions run in parallel, immediately after the start of hydrolysis, and the reaction rates are maximized at alkaline ph (11). The course of a sol- to- gel conversion is summarized in Fig. 7. The incorporation of organic functionality into inorganic structures by using organosilanes has been utilized in the development of a range of products for surface coating (12-14). These coating systems are applicable on a broad range of surfaces, ranging from metal and ceramics to textiles and wood. Their properties are mainly non- stick or easy- to- clean effects but other properties reported include scratch and abrasion resistance, corrosion protection for metals and anti fogging effects on glass surfaces (15-17). Figure 7. Sol- gel process. From alkoxysilane precurser to fully formed film. From Scheme 1. Hydrolysis and condensation of TEOS. 4

14 Introduction Nanofilm products Health effects of coating products Coating products have been associated with acute respiratory illness and poisoning. In the period from 1991 to 2007, 84 cases of varying degrees of poisoning related to using textile proofing sprays were reported in Demark (1). The only common feature of the reported cases was that 15 out of 17 proofing agents causing the observed health effects contained fluorocarbon polymers. A number of cases have been reported worldwide after application of spray products to leather and textiles (18-24). The symptoms were dyspnea, breast pain, coughing, headache, and fever. There were also severe reactions, e.g. lung inflammation with pulmonary edema and hemorrhage, and reduced alveolar oxygen uptake resulting in reduced blood oxygen tension. On the basis of 102 cases with waterproofing spray products it was recently concluded that no threshold could be found to define a safe level of exposure (24). Further, it was concluded that improvement of the occupational and environmental conditions provided insufficient prevention of future outbreaks of waterproofing- spray toxicity, because the cause- effect relationship is unknown. The manufactures represent a major obstacle in the process of clarifying the toxicological effects of coatings. In order to prevent their products from being copied, they are reluctant to inform about the exact formulations. As a result there is limited knowledge on which to base a meaningful toxicological assessment. One lead, however, is the high number of products utilizing perfluorinated polymers among those reported to have health effects (1). It has been postulated that perfluorinated compounds (e.g. silanes) may alter the surface properties of the lung lining fluid, e.g. by increasing the surface tension of the lung lining fluid (25). This could counteract the effects of lung surfactants, resulting in alveolar collapse with the consequence of a cascade of potential lung- damaging effects. This is partly supported by the fact that per- fluorinated polymers appear to be potentially more toxic than non- fluorinated polymers (25). In 2006, the Federal Institute for Risk Assessment in Germany registered at least 153 severe cases associated with the use of a new coating product claiming to be based on nanotechnology. The individuals had used the product Magic NANO, a spray product for coating glass and ceramic tiles (Fig.8), and their symptoms were severe coughing, dyspnea and lung edema (26). The product was classified as toxic by the German authorities and withdrawn from the market. In addition, a warning was placed through the European rapid alert system for non- food products (RAPEX) (27). Figure 8. The Magic NANO product. From Analysis of Magic NANO revealed that it did not contain nano particles. However the delivery system was changed from pump spray to propellant spray prior to the appearance of the health effects. Propellant sprays yield finer aerosols during spraying, allowing them to stay in the air longer and to penetrate deeper into the airways. Like in the other cases mentioned above, the causative agent(s) in the Magic NANO product have not been identified. 5

15 Introduction Nanofilm products The Magic NANO case received a lot of attention in both the German and Danish media, causing politicians in the Danish Parliament to debate the hazards of nanotechnology. Several politicians raised demands for more strict guidelines for the use of nano- technology- based products (28) and urged for more knowledge on possible health hazards in order to make knowledge- based decisions. Considerations on exposure and characterization NFPs may be used to coat a broad range of different surfaces, both indoors and outdoors. As a result several different exposure scenarios may be hypothesized e.g. treatment of tiles in a small bathroom with poor ventilation, impregnation of a cotton sofa in a living room, coating of floor materials in an office building, or spraying of an outer concrete wall. Table 1 (page 8) shows a list of selected consumer NFPs from three suppliers in Denmark. The majority of the NFPs are delivered as pump sprays, which typically result in release of larger aerosols that are deposited more efficiently on an absorbing surface than the smaller aerosols from propellant sprays. Due to differences in formulation of the products, the possible exposures will differ substantially in both type and concentration. Alcohol- and kerosene- based NFPs may release both aerosols and gas- phase products, while mainly aerosols are expected from the water- based products. The amount of product needed to cover a surface, logically, depends on the surface to be treated. In the case of an absorbent surface, such as a concrete wall, up to 100 ml/m 2 is needed, while as little as 10 ml/m 2 may be enough for bathroom tiles. The treated area is another factor; there is a rather big difference between spraying a t- shirt and a floor of several thousand m 2 in a large production facility. While the pump spray is convenient in the first case, it is completely unrealistic in the second. Coating surfaces at industrial scale demands automated application methods such as floor- washing machines or spray guns. Chemical characterization of the relatively complex aerosol and gas- phase compound mixture released during use of spray products is a challenging analytical task and calls for several advanced analytical techniques. In the few reported studies on the subject, methods such as x- ray fluorescence for elemental analysis and GC/MS for screening volatile organic compounds have been used to analyse proofing sprays for shoes and textiles (1,2). These methods are ideal to identify solvents and to screen for elements of interest (e.g. fluorine). However, they are inadequate for the possible identification of non- volatile active substances. Thus, it has not been possible to elucidate exact identities for active compounds in proofing spray products and this makes the task of carrying out a meaningful toxicological evaluation difficult. NFPs represent an even more demanding analytical task, given the level of knowledge at the beginning of this project. Information on the chemical compositions was restricted to some vague phrases about silanes and their hydrolysates and condensates in the material safety data sheets (MSDS) issued by one of the Danish suppliers. Search in the literature gave the impression that NFPs consisted of complex sol- gel systems containing several different organosilanes as well as silica nano particles (12,14). Usually, characterization of nano particles and thin, solid films is carried out using methods such as atomic force microscopy (AFM) or scanning/transmission electron microscopy (STEM), often combined with energy- dispersive x- ray fluorescence (XRF) (8). These techniques are useful tools that can yield information on surface morphology and the presence of 6

16 Introduction Nanofilm products specific elements (29), e.g. for the producer of a coating product who needs information about the physical properties of a synthesized nanomaterial and/or the film it forms on a surface. But if the film- forming components themselves are unknown and the task at hand is to identify them, mass spectrometry (MS) is the best option. Within the field of MS there are several powerful techniques for identification of unknowns as well as quantification and generation of molecular images and/or profiles of solid surfaces (30). In combination with chromatography (gas or liquid), MS represents the most widely used method for analysis of complex mixtures. Ideally, the components are introduced one at a time into the mass spectrometer, resulting in both qualitative and quantitative data. GC/MS and LC/MS are the methods of choice for analysis of the gas- phase compounds released during application and the liquid product, respectively. However, since NFPs have to react in order to form a functional film after application, they may react during liquid separation e.g. in the stationary phase in a LC column. This will hamper the analysis and destroy the analytical column. Therefore, other approaches for mass spectrometric analysis are relevant for NFP analysis. Recently developed ambient mass spectrometric techniques represent interesting alternatives, since they can be used with existing LC/MS equipment. They facilitate direct analysis of liquids and/or solids without pre- treatment or separation. In addition, they enable assessment of surfaces treated with NFPs under ambient conditions. Thus, an approach including several different mass spectrometric techniques, both traditional and new, is considered optimal and with the highest probability of yielding results to characterise the NFPs. Further, methods to measure particle concentration and size distribution in addition to methods for quantitative air sampling are necessary to evaluate the exposure risk during application. 7

17 Introduction Nanofilm products Product name (translated from Danish) Product designation Solvent Active compounds Non- absorbing floor materials 1 NFP 1 2- propanol $ Fluorosilanes/siloxanes a Rim coating 2 NFP 1 2- propanol $ Fluorosilanes/siloxanes a Bath and tiles 1 NFP 2 Ethanol $ Alkylsilanes/siloxanes a Coating for synthetic materials 2 NFP 2 Ethanol $ Alkylsilanes/siloxanes a Bath and tiles 2 NFP 2 Ethanol $ Alkylsilanes/siloxanes a Coating for concrete 2 NFP 2 Ethanol $ Alkylsilanes/siloxanes a Glass and tiles 3 NFP 2 Ethanol $ Alkylsilanes/siloxanes a Multipurpose coating 1 NFP 3 Kerosene # Abrasive/non- ionic tensides a Chromium and mirror finish 2 NFP 3 Kerosene # Abrasive/non- ionic tensides a Multipurpose coating 3 NFP 3 Kerosene # Abrasive/non- ionic tensides a Self- cleaning glass 1* NFP 4 Ethanol $ Titanium dioxide (anatase) Textile and leather 1 NFP 5 Water $ Fluorosilanes/siloxanes a Non- absorbent floor materials 1 NFP 5 Water $ Fluorosilanes/siloxanes a Wood and stone 1 NFP 5 Water $ Fluorosilanes/siloxanes a 1NFPs from Nanocover; 2 NFPs from NanoLotus; 3 NFPs from NanoNordisk $Pump spray, # Propellant spray aactive compounds identified/confirmed with mass spectrometry *This product was withdrawn from the Danish market in 2008 Table 1. Examples of NFPs from three different suppliers in Denmark. The product designations according to the contents of active compounds are, except for NFP 4, based on mass spectrometric analysis (see paper 2). The analysis of NFP 5 products has not been published. 8

18 Introduction Mass spectrometry Mass spectrometry Since the first mass spectrometric studies carried out by J.J. Thomson in 1912, mass spectrometry (MS) has been undergoing continuous development, following the general innovation in science. During the last 20 years, the big and user- unfriendly instruments, typically located in the cellars of a university s chemical department, have been transformed into bench- top instruments that can be operated by non- experts. At the same time, phenomenal increases in resolution, sensitivity and speed have been achieved. Development of the atmospheric pressure inlet as well as new ionization techniques, have widened the area of application for MS significantly. In particular, electrospray ionization (ESI) and matrix- assisted laser desorption ionization (MALDI) enabling ionization at atmospheric pressure, interfacing of liquid chromatography (LC) and analysis of high mass compounds, have contributed significantly to spreading use of the technique (31-33). The recent appearance of ambient ionization techniques enables direct mass spectrometric analysis of a wide range of different samples, without preparation (34,35). This was inconceivable just 10 years ago. A mass spectrometer (see graphical outline in Fig. 9) is a sophisticated instrument for the determination of masses of atoms and molecules. In the inlet/ion source the sample is introduced and ionized; this may take place at either atmospheric pressure or in a vacuum. The ions formed are then transferred to the mass analyser, and this separates them according to their mass- to- charge ratio m/z by the means of electric and/or magnetic fields. The ions are counted as they arrive at the detector and the resulting signals are converted into a mass spectrum by the data system. Both mass separation and detection always takes place in a vacuum (10-6 to Bar). The information obtained from the mass spectrometer can be used to determine the elemental composition of a molecule and elucidate its structure. Figure 9. Universal schematic of a mass spectrometer. Modified from (36). Ionization techniques The ionization step is essential for successful performance of a mass spectrometric experiment, since the mass spectrometer can only measure ions. Through ionization, analyte molecules become either positively or negatively charged ions and are thus made available for mass measurements. The charges can be visualized as small handles by which analyte molecules can be captured by an electrical field and introduced into the mass spectrometer. Once inside, the ions are secured by electrical fields while non- ionized species are pumped away by the vacuum system. There are several different ionization techniques that function at either atmospheric pressure or in a vacuum. 9

19 Introduction Mass spectrometry They produce gas- phase ions from neutral molecules by ejection or capture of an electron, protonation or deprotonation, adduct formation or by liquid- to- gas phase transfer of charged species in solution. A number of different ionization techniques were utilized for the analysis of the NFPs. These are described in the following; some of them in brief and some in more detail. Electron and chemical ionization Electron ionization (EI) takes place in a vacuum, where analyte molecules are subjected to a flux of electrons, which usually have energies of 70 ev (see Fig. 10). This causes ejection of one electron from each ionized molecule: M + e - M e - The resulting radical cations (M + ) will often have excess internal energy and will fragment readily to yield fragment ions (x,z), radicals (y) and neutrals (n): M + X + + Y M + Z + + N EI works well for almost all organic compounds but extensive fragmentation may conceal information on molecular mass. However, since the fragmentation is characteristic for each molecule and further, relatively reproducible between instruments, it can be used for identification. The EI spectrum of a compound represents, in most cases, a unique chemical fingerprint and thus enables identification of an unknown compound by comparing its spectrum with a reference. This is done on a routine basis by most modern EI mass spectrometers by using the NIST and Wiley databases that contain thousands of reference spectra. Figure 10. Schematic of an EI source. From The sample is usually introduced into the EI ion source via a thin capillary (e.g. from a GC system). However, introduction may also take place by diffusion through a silicone membrane. The membrane is impermeable to air and water but allows small, non- polar analytes to pass through into the ion source. Thus direct introduction of a sample from ambient surroundings (1 Bar) into the mass spectrometer (< 10-5 Bar) can be carried out in a simple manner without the need for pre- treatment. This technique is referred to as membrane- inlet mass spectrometry (MIMS) (37-39). Chemical ionization (CI) (40) is often utilized as a supplement to EI in order to provide information on molecular mass. It is carried out in a slightly modified EI source by the means of a reagent gas (e.g. methane, isobutene or ammonia) at a partial pressure (1 to 5x10-3 Bar) that is much higher than that of the analyte molecules. 10

20 Introduction Mass spectrometry The flux of electrons emitted from the filament (Fig. 10) will ionize the reagent gas rather than the analyte molecules and thus form an ionization plasma through a series of reactions facilitated by the relatively high pressure in the ion source (30). An analyte molecule is then ionized by protonation, deprotonation or adduct formation. The resulting ions (e.g. [M + H] +, [M - H] - ) have less internal energy than the radical cations formed by EI and are therefore less prone to fragmentation. Electrospray ionization (ESI) ESI has become one of the most commonly used ionization techniques since its development in the late 1980s, and it is now standard on all commercial mass spectrometers with an atmospheric pressure inlet. ESI has a broad range of applications for analysis of polar and medium polar compounds and its unique capability to form multiple charged ions enables analysis of large bio- molecules using instruments with limited mass ranges (33,41). The liquid is passed through a capillary, which is held at a potential difference of 3-6 kv relative to the inlet of the mass spectrometer (See Fig. 11). This results in an accumulation of charges at the surface of the liquid exiting from the capillary. Consequently, the liquid is drawn out and, eventually, broken up into highly charged droplets. These droplets will shrink in size as the liquid contained in them evaporates, leading to an increase in the surface- charge to surface- area ratio. This continues until the repulsion between charges of the same polarity overcomes the surface tension (Rayleigh limit) and the droplet breaks apart into a cascade of smaller droplets in a Coulomb explosion (41,42). The ESI process will proceed until, in principle, all ions have been desolvated and thus transferred to the gas phase (See illustration Fig. 12). This takes in the order of one to a few milliseconds depending on the design of the ESI source. The solvent evaporation process is accelerated by a counter flow of heated nitrogen (up to 350 C) exiting from the inlet. In addition a nebulizing gas may be utilized to increase the formation of fine droplets, thereby allowing a higher flow of liquid (up to 1 ml/min). Thus ESI is ideal as an interface between an LC and a mass spectrometer. Figure 11. Diagram of an electrospray source. Reprinted with permission from (85). In the most general case, electrospray is a method for generating a fine aerosol from a low flow of liquid (usually 1-10 µl/min) by means of a strong electrical field. Figure 12. Schematic of the ESI process. N is the number of charges, R is the droplet radius in µm and Δt is the time between Rayleigh limits. Reprinted with permission from (42). 11

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