The authors would like to acknowledge the support from the Department of Earth Sciences, Uppsala University for supporting part of this research.

1. A funcionalização de multiwalled Nanotubos de Carbono <ol><li> Realizar toda a etapa de funcionalização dentro de um exaustor, usando óculos de segurança, luvas e jaleco. Medir 24 ml de ácido sulfúrico e 8 ml de ácido nitrato utilizando um cilindro graduado, e depois transferi-los para um copo. Adicionar 32 mg de MWCNTs não tratados para uma proveta de usar estanho recipiente de alumínio em uma balança analítica (concentração final deve ser de 1 mg / ml de mistura de ácido). </li><li> Em primeiro lugar, manter o copo com MWCNT e mistura de ácido no produto de limpeza de ultra-sons (banho) durante 2 horas à temperatura ambiente. Então, o calor e agita-se a solução MWCNT-ácido durante 5 h a 90 ° C utilizando uma placa quente. </li><li> Filtra-se a suspensão com um CNT dos poros da membrana de 0,2 um filtro de PTFE de diâmetro colocado sobre um suporte de filtro, e usar a vácuo para ajudar a filtração. Realize a porção de filtração por porção e use várias membranas de filtro (aproximadamente 1/4 th de mistura acima por parte de um filtro). Adicione a água ferventedurante o processo de filtração para filtrar a solução de ácido até que o pH da mistura torna-se maior do que 5. </li><li> Sempre quebrar o vácuo antes de ser desligado e não introduzir qualquer coisa no sistema de vácuo. Use um copo cônico para recolher o líquido de resíduos. </li><li> Derrame de ácido filtrado em um recipiente de resíduos (enviar o recipiente de resíduos para uma instalação de tratamento de resíduos ou diluir o líquido antes de despejá-la na pia, adicionando pelo menos dez vezes de água da torneira). </li><li> Transfira as membranas filtrantes com MWCNTs retidos em evaporando pratos e colocar os pratos em exsicador (contém cerca de 100 g de gel de sílica) e criar um ambiente de vácuo (deixar o vácuo durante cerca de 1 hora) para o CNT para completar a secagem (cerca de 24 horas ). <ol><li> Raspe os nanotubos de carbono fora das membranas cuidadosamente usando uma espátula e transferir as partículas dentro de um recipiente limpo. Pesa-se o pó MWCNTs e identificar o recipiente, para uso futuro. </li></ol></li></ol> 2. Poronos meios de transporte para Experiments <ol><li> Prepare uma solução de HCl 0,1 M por lavagem ácida de areia de sílica. <ol><li> Executar todas as etapas dentro de um exaustor com óculos de segurança, luvas e jaleco. Adicionar 1 L de água desionizada para um balão de 2 L. Medida 8 ml de HCl a 37% utilizando um cilindro graduado. </li><li> Adicionar o HCl na água desionizada cuidadosamente. Agitar o frasco cuidadosamente para ajudar a mistura. </li></ol></li><li> Lava-se a areia com a solução de HCl preparado. <ol><li> Pesar cerca de 1.000 g de areia. Adicione 1/3 de areia para o balão com a solução de HCl e agitar o frasco duas vezes para ajudar a mistura, em seguida, adicionar o resto da areia (1/3 de areia de cada vez). </li><li> Agitar o frasco três vezes e deixar o ácido com areia durante 30 min. </li><li> Despeje o líquido para fora do balão ao recipiente de resíduos de ácido e lavar a areia com água deionizada pelo menos 8 vezes. </li></ol></li><li> Lava-se a areia com uma solução de H 2 O 2. <ol><li> Adicione 700 ml de água deionizada emo balão com areia, em seguida, medir 40 ml de 30% de H 2 O 2 solução usando um cilindro graduado. </li><li> Adicione o 2 O 2 solução H na garrafa com areia e apertar duas vezes para ajudar a mistura. Em seguida, adicionar mais 40 mL de 30% de H 2 O 2 a solução 3 vezes até que não é de 160 ml no total de H 2 O 2 no frasco. </li><li> Agitar e homogeneizar a solução e areia de cada vez e deixar o H 2 O 2 com solução de areia durante 40 min para permitir que a reacção se completou. Agitar o frasco e agita-se a areia com uma vareta de plástico a cada 10 min. </li><li> Decantar o líquido até a pia e correr água da torneira durante 30 segundos. </li></ol></li><li> Lavar e secar a areia. <ol><li> Lavar areia com água deionizada pelo menos 8 vezes para se livrar de qualquer solução ou esquerda sobre produtos de reacção. Agitar e mexa bem quando enxaguar. </li><li> Coloque a garrafa com areia lavada em um forno (105 ° C) por 24 horas para secar, em seguida, tomar a areia fora do forno usandoforno-luva e deixar no balcão para 2 horas para a areia para se refrescar. </li><li> Transfira a areia limpa em um recipiente de plástico. Marque o recipiente e coloque-o em uma prateleira apropriado para estar pronto para o uso. </li></ol></li></ol> 3. Experimentos Coluna <ol><li> Preparação da solução de fundo. <ol><li> Prepare apropriado química solução de fundo para o experimento coluna. </li><li> Use 0,1 M HCl e 0,1 M NaOH soluções para ajustar o pH e o sal de NaCl para conseguir a força iónica adequada para a experiência seguinte. </li></ol></li><li> Seleção de coluna. <ol><li> Escolha uma coluna de vidro de 2,5 cm de diâmetro e 15 cm de comprimento para este experimento (pH: 5 e força iônica: 2 mM no estudo atual). Use de um filtro de malha de aço (0,2 mm) em ambos os lados da coluna de vidro. </li><li> Lave os tubos ligados à coluna e encher com solução de fundo (ou solução MWCNTs até que a válvula de 3 vias para controlar o tipo de fluxo de líquido (MWCNTs solution ou solução de fundo), conforme mostrado na Figura 1. </li></ol></li><li> Wet-embalagem da coluna. <ol><li> Pesar a areia limpa em escala e tomar 124 g de areia limpa para o tamanho da coluna selecionada. </li><li> Use uma bomba peristáltica de alta precisão. Calibrar a bomba para atingir 2 ml / min de fluxo de líquido. </li><li> Iniciar a bomba para encher a coluna a partir do fundo até que o nível de água é um par de centímetros acima do fundo da coluna. Coloque cerca de 1/10 da areia, medida de cada vez para a coluna, mas certifique-se que o nível de areia não vem acima do nível da água na coluna. Continuar o fluxo de água para a coluna continuamente para ficar acima do nível de areia. </li><li> Feche a tampa da coluna com tela de filtro adequado, após o preenchimento completo. </li><li> Permitir que a coluna de enchimento para fluir durante pelo menos 1 hr. Os parâmetros individuais da coluna são indicadas na Tabela 1. </li></ol></li><li> Tracer teste. <ol><li> Start o experimento de coluna com um traçador de teste antes das experiências de solução MWCNT. </li><li> Alterne a válvula de 3 vias para a solução marcador (o uso de alimentos de cor marcador a 20 mg / L) para iniciar o experimento. </li><li> Recolher as amostras de saída a partir da coluna a cada 2 minutos (ou seja, 4 ml / amostras em cada tubo de ensaio), utilizando o colector de fracções ligado conforme mostrado na Figura 1. </li><li> Continuar para injectar a solução de traçador para um volume de poro de 4,32 (isto é, solução passa de 4,32 vezes o espaço vazio de poros total na coluna empacotada areia), que também é chamado de fase I do experimento. </li><li> Alterne a válvula de 3 vias para solução do fluxo de fundo (água DI no caso de experimento tracer) para outro volume 4,32 poros. </li></ol></li><li> Preparação da solução de MWCNT. <ol><li> Adicione uma disperso, solução MWCNTs funcionalizado colocando 15 mg de MWCNTs funcionalizados em um copo de 300 ml contendo 200 ml de solução aquosa (com soluçã o desejarn química ou seja, pH 5 e 2 mM de força iónica na condição experimental corrente) e utilizando um homogeneizador de ultra-sons de sonda colocada no copo de vidro (com 40% de potência, durante 15 min). Misture a solução MWCNTs disperso com mais 800 ml da mesma solução aquosa para se atingir a concentração MWCNT de 15 mg / L. </li><li> Realizar microscopia de varrimento electrónico (SEM) de análise de imagem de solução estoque para o seu tamanho e forma das nanopartículas depois de funcionalização. </li></ol></li><li> Experimento transporte MWCNT. <ol><li> Alterne a válvula de 3 vias para solução MWCNT para iniciar o experimento coluna. </li><li> Recolher as amostras de saída a partir da coluna a cada 2 min utilizando o colector de fracções ligado. </li><li> Injectar a solução MWCNT para um volume de 4,32 poro (fase I do experimento). </li><li> Alterne a válvula de 3 vias para fluir solução de fundo para outro volume de poros 4,32, o que é chamado de fase II do experimento. </li><li> Alterar o tubo de injecção de background solução para o frasco de água DI (depois de parar a bomba, por um momento, para evitar a entrada de ar a partir do tubo) e continuar o fluxo para outro volume de poro de 4,32, que é chamada a fase III do experimento. </li></ol></li><li> As análises das amostras. <ol><li> Transferir todas as amostras de tubos de coletor de fração em um suporte de tubos. </li><li> Prepare um espectrofotômetro UV / VIS para a análise da amostra, ou seja, descobrir o comprimento de onda de leitura adequado para a quantificação das amostras coletadas. Use 400 nm para uma solução MWCNT e um comprimento de onda de 333 nm para a solução do marcador. </li><li> Digitalizar todas as amostras recolhidas a partir da coluna durante as fases I, II, III e utilizando uma cuvete a 400 nm de comprimento de onda (ou um comprimento de onda diferente, se for considerado mais apropriado na etapa anterior) e armazenar os dados. </li><li> Coletar os dados do espectrofotômetro e traçá-los vs tempo ou volume de poros para obter curvas de ruptura como mostram os resultados representativos (por exemplo, a Figura3). </li><li> Realizar análise de tamanho (diâmetro hidrodinâmico) de entrada e saída amostras usando zeta sizer e conduzir a visualização estudou tanto para entrada e saída amostras usando microscopia eletrônica de varredura. </li></ol></li></ol>

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The authors declare that they have no competing financial interests.

Efeito de funcionalização MWCNT Como a Figura 2 confirma a estabilidade do MWCNTs funcionalizados, a diferença observada no volume de eluído de MWCNT foi devido a funcionalização e particularmente, devido à adição de carboxilo (-COOH) grupos à superfície das MWCNTs (Figuras 3 e 4). No processo de funcionalização semelhante, a presença de oxigênio foi confirmada pelo raio-X espectroscopia de fotoelétrons ...

Com o recente desenvolvimento em nanotecnologia que utiliza vários tipos de nanopartículas para melhorar uma série de tecnologias em setores como tecnologia da informação, energia, ciência ambiental, medicina, segurança interna, a segurança alimentar, e transporte; uma compreensão completa do transporte e retenção de nanopartículas em solo e água subterrânea é fundamental para a avaliação de riscos, bem como aplicações ambientais de nanopartículas 1-3. Nanotubos de carbono (CNT) são uma das nanopartículas à base de carbono mais produzidos 2,4. Nanotubos de carbono são a forma cilíndrica longa e de grafeno com um diâmetro geralmente inferior a 100 nm e um comprimento na gama de 100 nm a 50 um. Eles têm propriedades únicas, que aceleraram a sua utilização em diversas aplicações, tais como a eletrônica, ótica, cosméticos e tecnologia biomédica (por exemplo, materiais compósitos) 5. Com o aumento do uso, há também um aumento da risk à exposição humana e efeitos sobre a saúde, bem como as consequências ecológicas negativas seguintes CNT e disposição outras nanomateriais à base de carbono para o meio ambiente 5-8. Com nenhuma modificação de superfície (não funcionalizados), nanotubos de carbono são extremamente hidrofóbico e tendem a agregar em solução aquosa. Nanotubos de carbono funcionalizadas podem, no entanto, permanecem dispersos e estável em soluções aquosas e são utilizados para fins biomédicos, tais como a entrega de drogas 9. Aqui, é essencial que os nanotubos de carbono permanecem dispersos e mobilização, de modo que o fármaco pode ser entregue no interior do corpo humano 10. Por outro lado, para reduzir os riscos ambientais, não há a necessidade de estudos com foco em como imobilizar os nanotubos de carbono, a fim de evitar a sua entrada em aquíferos e dos recursos de água potável 11. Estudos recentes têm demonstrado o efeito tóxico do CNT em organismos vivos e também os riscos para os ecossistemas em termos de nanotubos de carbono que entram e que se acumulam nas cadeias alimentares, uma vez queNanotubos de carbono são difíceis de biodegradar 5,8. Mesmo com sistemas de barreira em aterros contendo os nanotubos de carbono, que pode ser possível para os nanotubos de carbono de passar através das barreiras. Nesses casos, os nanotubos de carbono poderia entrar em reservatórios de água subterrânea e corpos de água superficiais. Como regulamentos de eliminação da CNT não estão bem definidos e mecanismos de transporte são mal compreendidos, uma melhor compreensão da mobilidade dos nanotubos de carbono é necessário para a formulação e concepção de sistemas de escoamento adequado 12. Portanto, é importante estudar e compreender o destino e transporte de nanotubos de carbono em meios porosos e o efeito de fatores físicos e químicos comumente presentes no ambiente de subsuperfície na superfície modificada retenção CNT. Uma série de pesquisas têm sido realizadas sobre o efeito do tamanho do coletor de grão 13-15, caudal 16, e propriedades de superfície dos grãos de 17 sobre o transporte de nanopartículas em meios porosos. Entretanto, as investigações sistemáticas sobre o efeito da solutquímica de iões (tais como o pH e força iónica) sobre possível deposição sobre a superfície do colector são ainda limitados 18-20. Além disso, o efeito combinado de factores físicos, solução química do meio e propriedades de superfície dos nanotubos de carbono não é bem compreendida e variam na literatura diferente. Neste estudo, um método de preparação para a modificação da superfície de MWCNTs será demonstrada, juntamente com uma coluna sistemática à escala laboratorial embalado com areia de quartzo limpo com ácido vai ser utilizado para investigar o transporte, a manutenção e remobilização de nanotubos de carbono de superfície modificada em meios porosos saturados .

<table border="0" cellpadding="0" cellspacing="0" width="750">
	<tbody>
		<tr height="43">
			<td height="43" style="height:43px;width:183px;">Name of Material/ Equipments</td>
			<td style="width:228px;">Company</td>
			<td style="width:169px;">Catalog Number</td>
			<td style="width:171px;">Comments/Description</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:183px;">MWCNT</td>
			<td style="width:228px;">Cheap Tubes Inc., USA</td>
			<td style="width:169px;">sku-03040304</td>
			<td style="width:171px;">Purchased as semi-functionlized powder</td>
		</tr>
		<tr height="148">
			<td height="148" style="height:148px;width:183px;">Quartz sand</td>
			<td style="width:228px;">Sibelco Nordic, Baskarp, Sweden</td>
			<td style="width:169px;">B44</td>
			<td style="width:171px;">Purchased with more than 91% silica sand</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:183px;">H2SO4</td>
			<td style="width:228px;">VWR</td>
			<td style="width:169px;">1.01833.2500</td>
			<td style="width:171px;">95-97% purity</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:183px;">HNO3</td>
			<td style="width:228px;">VWR</td>
			<td style="width:169px;">1.00441.1000</td>
			<td style="width:171px;">70% purity</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:183px;">HCl</td>
			<td style="width:228px;">VWR</td>
			<td style="width:169px;">1.00317.2500</td>
			<td style="width:171px;">37-38% purity</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:183px;">H2O2</td>
			<td style="width:228px;">VWR</td>
			<td style="width:169px;">23615.248</td>
			<td style="width:171px;">30% purity</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:183px;">NaCl</td>
			<td style="width:228px;">VWR</td>
			<td style="width:169px;">1.06404.0500</td>
			<td style="width:171px;">99.5% purity</td>
		</tr>
		<tr height="64">
			<td height="64" style="height:64px;width:183px;">NaOH</td>
			<td style="width:228px;">Sigma-Aldrich</td>
			<td style="width:169px;">S8045-500G</td>
			<td style="width:171px;">99.99% pur pellets&#160;</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:183px;">Ultrasonic Homogenizer</td>
			<td style="width:228px;">Biologics Inc. Manassas, Virginia</td>
			<td style="width:169px;">Model 3000, 0-127-0002</td>
			<td style="width:171px;">Operated for fix time interval</td>
		</tr>
		<tr height="22">
			<td height="22" style="height:22px;width:183px;">Sonicator (bath)</td>
			<td style="width:228px;">Kerry Ultrasonic Ltd</td>
			<td style="width:169px;">1808</td>
			<td style="width:171px;">Common bath sonicator</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:183px;">Peristaltic pump</td>
			<td style="width:228px;">Ismantec, Glattbrugg, Switzerland</td>
			<td style="width:169px;">ISM931</td>
			<td style="width:171px;">Work with tygon tubing in the pump</td>
		</tr>
		<tr height="64">
			<td height="64" style="height:64px;width:183px;">Spectrophotometer</td>
			<td style="width:228px;">Hach Lange</td>
			<td style="width:169px;">DR500, LPV408.99.0001</td>
			<td style="width:171px;">Operate with manual cuvette as well as automated sampling</td>
		</tr>
		<tr height="22">
			<td height="22" style="height:22px;width:183px;">pH meter</td>
			<td style="width:228px;">Metrohm</td>
			<td style="width:169px;">781</td>
			<td style="width:171px;">pH analysis</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:183px;">Glass column</td>
			<td style="width:228px;">Chromaflex</td>
			<td style="width:169px;">420830-1510</td>
			<td style="width:171px;">Column with adjustable cap</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:183px;">Fraction collector</td>
			<td style="width:228px;">Spectrum Labs Europe</td>
			<td style="width:169px;">CF-2, 124846</td>
			<td style="width:171px;">Fixed at regular interval of time</td>
		</tr>
		<tr height="22">
			<td height="22" style="height:22px;width:183px;">Fraction collector tubes</td>
			<td style="width:228px;">VWR</td>
			<td style="width:169px;">212-9599</td>
			<td style="width:171px;">6 ml volume glass tube</td>
		</tr>
		<tr height="22">
			<td height="22" style="height:22px;width:183px;">Hot plate stir</td>
			<td style="width:228px;">Thermo Scientific</td>
			<td style="width:169px;">SP131320-33</td>
			<td style="width:171px;">Adjustable tempurature</td>
		</tr>
		<tr height="22">
			<td height="22" style="height:22px;width:183px;">Oven</td>
			<td style="width:228px;">Elektro Helios</td>
			<td style="width:169px;">259</td>
			<td style="width:171px;">For oven dry of sand</td>
		</tr>
		<tr height="22">
			<td height="22" style="height:22px;width:183px;">Balance</td>
			<td style="width:228px;">Mettler Toledo</td>
			<td style="width:169px;">AE 160</td>
			<td style="width:171px;">For accurate weight</td>
		</tr>
	</tbody>
</table>

transport of surface-modified carbon nanotubes through a soil column

Carbon nanotubes (CNTs) are widely manufactured nanoparticles, which are being utilized in a number of consumer products, such as sporting goods, electronics and biomedical applications. Due to their accelerating production and use, CNTs constitute a potential environmental risk if they are released to soil and groundwater systems. It is therefore essential to improve the current understanding of environmental fate and transport of CNTs. The transport and retention of CNTs in both natural and artificial media have been reported in literature, but the findings widely vary and are thus not conclusive. There are a number of physical and chemical parameters responsible for variation in retention and transport. In this study, a complete procedure of selected multiwalled carbon nanotubes (MWCNTs) is presented starting from their surface modification to a complete set of laboratory column experiments at critical physical and chemical scenarios. Results indicate that the stability of the commercially available MWCNTs are critical with their attached surface functional group which can also influence the transport and retention of MWCNT through the surrounding medium.

Efeito de funcionalização MWCNT A solução MWCNT funcionalizado e disperso foi selado no recipiente para permitir que a solução atinja o equilíbrio. Não houve sedimentação nem agregação observada na solução estoque após sonicação, como o diâmetro hidrodinâmico da MWCNT (1.619 ± 262 nm) da solução manteve-se a mesma durante seis meses de ultra-sons (Figura 2). Para investigar o efeito de funcionalização de MWCNTs à sua mobilidade, dois...

Watch this Scientific Journal Video about Transport of Surface-modified Carbon Nanotubes through a Soil Column at JoVE.com

Transport of Surface-modified Carbon Nanotubes through a Soil Column

Surface properties of a nanoparticle are important for their interaction with the surrounding medium. Therefore the surface modification of carbon nanotubes can be critical for their transport and retention through porous media. Here, lab scale column experiments are used to understand the possible transport and retention of these nanoparticles.

Transporte de nanotubos de carbono de superfície modificada através de uma coluna de solo

Carbon nanotubes (CNTs) are widely manufactured nanoparticles, which are being utilized in a number of consumer products, such as sporting goods, ...

transport-of-surface-modified-carbon-nanotubes-through-a-soil-column

Research

JoVE Journal

Chemistry

9.4K visualizações.  Nalanda University. Surface properties of a nanoparticle are important for their interaction with the surrounding medium. Therefore the surface modification of carbon nanotubes can be critical for their transport and retention through porous media. Here, lab scale column experiments are used to understand the possible transport and retention of these nanoparticles. 

Vídeo: Transport of Surface-modified Carbon Nanotubes through a Soil Column

Dependence of Laser-induced Breakdown Spectroscopy Results on Pulse Energies and Timing Parameters Using Soil Simulants

The dependence of some LIBS detection capabilities on lower pulse energies (&lt;100 mJ) and timing parameters were examined using synthetic silicate samples. These samples were used as simulants for soil and contained minor and trace elements commonly found in soil at a wide range of concentrations. For this study, over 100 calibration curves were prepared using different pulse energies and timing parameters; detection limits and sensitivities were determined from the calibration curves. Plasma temperatures were also measured using Boltzmann plots for the various energies and the timing parameters tested. The electron density of the plasma was calculated using the full-width half maximum (FWHM) of the hydrogen line at 656.5 nm over the energies tested. Overall, the results indicate that the use of lower pulse energies and non-gated detection do not seriously compromise the analytical results. These results are very relevant to the design of field- and person-portable LIBS instruments.

LIBS detection capabilities on soil simulants were tested using a range of pulse energies and timing parameters. Calibration curves were used to determine detection limits and sensitivities for different parameters. Generally, the results showed that there was not a significant reduction in detection capabilities using lower pulse energies and non-gated detection.

Dependência da induzida por laser Resultados Breakdown Spectroscopy sobre Energias de pulso e parâmetros de tempo utilizando simuladores de solo

The  dependence of some LIBS detection capabilities on lower pulse energies (&lt;100  mJ) and timing parameters were examined using synthetic silicate ...

Química

An Inverse Analysis Approach to the Characterization of Chemical Transport in Paints

The ability to directly characterize chemical transport and interactions that occur within a material (i.e., subsurface dynamics) is a vital component in understanding contaminant mass transport and the ability to decontaminate materials. If a material is contaminated, over time, the transport of highly toxic chemicals (such as chemical warfare agent species) out of the material can result in vapor exposure or transfer to the skin, which can result in percutaneous exposure to personnel who interact with the material. Due to the high toxicity of chemical warfare agents, the release of trace chemical quantities is of significant concern. Mapping subsurface concentration distribution and transport characteristics of absorbed agents enables exposure hazards to be assessed in untested conditions. Furthermore, these tools can be used to characterize subsurface reaction dynamics to ultimately design improved decontaminants or decontamination procedures. To achieve this goal, an inverse analysis mass transport modeling approach was developed that utilizes time-resolved mass spectroscopy measurements of vapor emission from contaminated paint coatings as the input parameter for calculation of subsurface concentration profiles. Details are provided on sample preparation, including contaminant and material handling, the application of mass spectrometry for the measurement of emitted contaminant vapor, and the implementation of inverse analysis using a physics-based diffusion model to determine transport properties of live chemical warfare agents including distilled mustard (HD) and the nerve agent VX.

In this paper, a procedure for quantifying the mass transport parameters of chemicals in various materials is presented. This process involves employing an inverse-analysis based diffusion model to vapor emission profiles recorded by real-time, mass spectrometry in high vacuum.

Uma abordagem de análise inversa à caracterização dos Transportes Química em Tintas

The ability to directly characterize chemical transport and interactions that occur within a material (i.e., subsurface dynamics) is a vital component in ...

Tuning a Parallel Segmented Flow Column and Enabling Multiplexed Detection

Active flow technology (AFT) is new form of column technology that was designed to overcome flow heterogeneity to increase separation performance in terms of efficiency and sensitivity and to enable multiplexed detection. This form of AFT uses a parallel segmented flow (PSF) column. A PSF column outlet end-fitting consists of 2 or 4 ports, which can be multiplexed to connect up to 4 detectors. The PSF column not only allows a platform for multiplexed detection but also the combination of both destructive and non-destructive detectors, without additional dead volume tubing, simultaneously. The amount of flow through each port can also be adjusted through pressure management to suit the requirements of a specific detector(s). To achieve multiplexed detection using a PSF column there are a number of parameters which can be controlled to ensure optimal separation performance and quality of results; that is tube dimensions for each port, choice of port for each type of detector and flow adjustment. This protocol is intended to show how to use and tune a PSF column functioning in a multiplexed mode of detection.

Here, we present a protocol for the operation and tuning of parallel segmented flow chromatography columns to enable multiplexed detection.

Sintonizar um paralelo Coluna Segmentada fluxo e permitindo a detecção multiplexada

Active flow technology (AFT) is new form of column technology that was designed to overcome flow heterogeneity to increase separation performance in terms ...

Curtain Flow Column: Optimization of Efficiency and Sensitivity

Active Flow Technology (AFT) is a form of column technology that increases the separation performance of a HPLC column through the use of a specially purpose built multiport end-fitting(s). Curtain Flow (CF) columns belong to the AFT suite of columns, specifically the CF column is designed so that the sample is injected into the radial central region of the bed and a curtain flow of mobile phase surrounding the injection of solute prevents the radial dispersion of the sample to the wall. The column functions as an 'infinite diameter' column. The purpose of the design is to overcome the radial heterogeneity of the column bed, and at the same time maximize the sample load into the radial central region of the column bed, which serves to increase detection sensitivity. The protocol described herein outlines the system and CF column set up and the tuning process for an optimized infinite diameter 'virtual' column.

Here, we present a protocol for the operation and optimization of Active Flow Technology (AFT) column in Curtain flow (CF) mode for enhanced separation performance.

Cortina Fluxo Coluna: Optimização da Eficiência e Sensibilidade

Active Flow Technology (AFT) is a form of column technology that increases the separation performance of a HPLC column through the use of a specially ...

Facile Preparation of Internally Self-assembled Lipid Particles Stabilized by Carbon Nanotubes

We present a facile method to prepare nanostructured lipid particles stabilized by carbon nanotubes (CNTs). Single-walled (pristine) and multi-walled (functionalized) CNTs are used as stabilizers to produce Pickering type oil-in-water (O/W) emulsions. Lipids namely, Dimodan U and Phytantriol are used as emulsifiers, which in excess water self-assemble into the bicontinuous cubic Pn3m phase. This highly viscous phase is fragmented into smaller particles using a probe ultrasonicator in presence of conventional surfactant stabilizers or CNTs as done here. Initially, the CNTs (powder form) are dispersed in water followed by further ultrasonication with the molten lipid to form the final emulsion. During this process the CNTs get coated with lipid molecules, which in turn are presumed to surround the lipid droplets to form a particulate emulsion that is stable for months. The average size of CNT-stabilized nanostructured lipid particles is in the submicron range, which compares well with the particles stabilized using conventional surfactants. Small angle X-ray scattering data confirms the retention of the original Pn3m cubic phase in the CNT-stabilized lipid dispersions as compared to the pure lipid phase (bulk state). Blue shift and lowering of the intensities in characteristic G and G&#39; bands of CNTs observed in Raman spectroscopy characterize the interaction between CNT surface and lipid molecules. These results suggest that the interactions between the CNTs and lipids are responsible for their mutual stabilization in aqueous solutions. As the concentrations of CNTs employed for stabilization are very low and lipid molecules are able to functionalize the CNTs, the toxicity of CNTs is expected to be insignificant while their biocompatibility is greatly enhanced. Hence the present approach finds a great potential in various biomedical applications, for instance, for developing hybrid nanocarrier systems for the delivery of multiple functional molecules as in combination therapy or polytherapy.

We report on a smart application of carbon nanotubes for kinetic stabilization of lipid particles that contain self-assembled nanostructures in their cores. The preparation of lipid particles requires rather low concentrations of carbon nanotubes permitting their use in biomedical applications such as drug delivery.

Preparação Facile da Internamente auto-montados Lipid partículas estabilizada por nanotubos de carbono

We present a facile method to prepare nanostructured lipid particles stabilized by carbon nanotubes (CNTs). Single-walled (pristine) and multi-walled ...

Preparation of Carbon Nanosheets at Room Temperature

Amphiphilic molecules equipped with a reactive, carbon-rich "oligoyne" segment consisting of conjugated carbon-carbon triple bonds self-assemble into defined aggregates in aqueous media and at the air-water interface. In the aggregated state, the oligoynes can then be carbonized under mild conditions while preserving the morphology and the embedded chemical functionalization. This novel approach provides direct access to functionalized carbon nanomaterials. In this article, we present a synthetic approach that allows us to prepare hexayne carboxylate amphiphiles as carbon-rich siblings of typical fatty acid esters through a series of repeated bromination and Negishi-type cross-coupling reactions. The obtained compounds are designed to self-assemble into monolayers at the air-water interface, and we show how this can be achieved in a Langmuir trough. Thus, compression of the molecules at the air-water interface triggers the film formation and leads to a densely packed layer of the molecules. The complete carbonization of the films at the air-water interface is then accomplished by cross-linking of the hexayne layer at room temperature, using UV irradiation as a mild external stimulus. The changes in the layer during this process can be monitored with the help of infrared reflection-absorption spectroscopy and Brewster angle microscopy. Moreover, a transfer of the carbonized films onto solid substrates by the Langmuir-Blodgett technique has enabled us to prove that they were carbon nanosheets with lateral dimensions on the order of centimeters.

We present the synthesis of an amphiphilic hexayne and its use in the preparation of carbon nanosheets at the air-water interface from a self-assembled monolayer of these reactive, carbon-rich molecular precursors.

Preparação de Nanofolhas de Carbono à Temperatura Ambiente

Amphiphilic molecules equipped with a reactive, carbon-rich "oligoyne" segment consisting of conjugated carbon-carbon triple bonds self-assemble into ...

Functionalization of Single-walled Carbon Nanotubes with Thermo-reversible Block Copolymers and Characterization by Small-angle Neutron Scattering

We demonstrate a protocol for single-walled carbon nanotube functionalization using thermo-sensitive PEO-PPO-PEO triblock copolymers in an aqueous solution. In a carbon nanotube/PEO105-PPO70-PEO105 (poloxamer 407) aqueous solution, the amphiphilic poloxamer 407 adsorbs onto the carbon nanotube surfaces and self-assembles into continuous layers, driven by intermolecular interactions between constituent molecules. The addition of 5-methylsalicylic acid changes the self-assembled structure from spherical-micellar to a cylindrical morphology. The fabricated poloxamer 407/carbon nanotube hybrid particles exhibit thermo-responsive structural features so that the density and thickness of poloxamer 407 layers are also reversibly controllable by varying temperature. The detailed structural properties of the poloxamer 407/carbon nanotube particles in suspension can be characterized by small-angle neutron scattering experiments and model fit analyses. The distinct curve shapes of the scattering intensities depending on temperature control or addition of aromatic additives are well described by a modified core-shell cylinder model consisting of a carbon nanotube core cylinder, a hydrophobic shell, and a hydrated polymer layer. This method can provide a simple but efficient way for the fabrication and in-situ characterization of carbon nanotube-based nano particles with a structure-tunable encapsulation.

A method for the functionalization of carbon nanotubes with structure-tunable polymeric encapsulation layers and structural characterization using small-angle neutron scattering is presented.

Funcionalização da murada-Single nanotubos de carbono com termo-reversível copolímeros em bloco e caracterização por Small-angle Neutron Scattering

We demonstrate a protocol for single-walled carbon nanotube functionalization using thermo-sensitive PEO-PPO-PEO triblock copolymers in an aqueous ...

Characterizing Electron Transport through Living Biofilms

Here we demonstrate the method of electrochemical gating used to characterize electrical conductivity of electrode-grown microbial biofilms under physiologically relevant conditions.1 These measurements are performed on living biofilms in aqueous medium using source and drain electrodes patterned on a glass surface in a specialized configuration referred to as an interdigitated electrode (IDA) array. A biofilm is grown that extends across the gap connecting the source and drain. Potentials are applied to the electrodes (ES and ED) generating a source-drain current (ISD) through the biofilm between the electrodes. The dependency of electrical conductivity on gate potential (the average of the source and drain potentials, EG = [ED + ES]/2) is determined by systematically changing the gate potential and measuring the resulting source-drain current. The dependency of conductivity on gate potential provides mechanistic information about the extracellular electron transport process underlying the electrical conductivity of the specific biofilm under investigation. The electrochemical gating measurement method described here is based directly on that used by M. S. Wrighton2,3 and colleagues and R. W. Murray4,5,6 and colleagues in the 1980&#39;s to investigate thin film conductive polymers.

A protocol for measuring electrical conductivity of living microbial biofilms under physiologically relevant conditions is presented.

Caracterizando o transporte de elétrons através de biofilmes vivos

Here we demonstrate the method of electrochemical gating used to characterize electrical conductivity of electrode-grown microbial biofilms under ...

Grafting Multiwalled Carbon Nanotubes with Polystyrene to Enable Self-Assembly and Anisotropic Patchiness

We demonstrate a straightforward protocol to graft pristine multiwalled carbon nanotubes (MWCNTs) with polystyrene (PS) chains at the sidewalls through a free-radical polymerization strategy to enable the modulation of the nanotube surface properties and produce supramolecular self-assembly of the nanostructures. First, a selective hydroxylation of the pristine nanotubes through a biphasic catalytically mediated oxidation reaction creates superficially distributed reactive sites at the sidewalls. The latter reactive sites are subsequently modified with methacrylic moieties using a silylated methacrylic precursor to create polymerizable sites. Those polymerizable groups can address further polymerization of styrene to produce a hybrid nanomaterial containing PS chains grafted to the nanotube sidewalls. The polymer-graft content, amount of silylated methacrylic moieties introduced and hydroxylation modification of the nanotubes are identified and quantified by Thermogravimetric Analysis (TGA). The presence of reactive functional groups hydroxyl and silylated methacrylate are confirmed by Fourier Transform Infrared Spectroscopy (FT-IR). Polystyrene-grafted carbon nanotube solutions in tetrahydrofuran (THF) provide wall-to-wall collinearly self-assembled nanotubes when cast samples are analyzed by transmission electron microscopy (TEM). Those self-assemblies are not obtained when suitable blanks are similarly cast from analogous solutions containing non-grafted counterparts. Therefore, this method enables the modification of the nanotube anisotropic patchiness at the sidewalls which results into spontaneous auto-organization at the nanoscale.

A procedure for the synthesis of polystyrene-grafted multiwalled carbon nanotubes using successive chemical modification steps to selectively introduce the polymer chains to the sidewalls and their self-assembly via anisotropic patchiness is presented.

Enxertia de nanotubos de carbono de Multiwalled com poliestireno para habilitar auto-montagem e anisotrópica Patchiness

We demonstrate a straightforward protocol to graft pristine multiwalled carbon nanotubes (MWCNTs) with polystyrene (PS) chains at the sidewalls through a ...

Electrochemical Impedance Spectroscopy as a Tool for Electrochemical Rate Constant Estimation

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). In the case of fast reversible electrochemical processes, current is predominantly affected by the rate of diffusion, which is the slowest and limiting stage. EIS is a powerful technique that allows separate analysis of stages of charge transfer that have different AC frequency response. The capability of the method was used to extract the value of charge transfer resistance, which characterizes the rate of charge exchange on the electrode-solution interface. The application of this technique is broad, from biochemistry up to organic electronics. In this work, we are presenting the method of analysis of organic compounds for optoelectronic applications.

Electrochemical impedance spectroscopy (EIS) of species that undergo reversible oxidation or reduction in solution was used for determination of rate constants of oxidation or reduction.

Espectroscopia de impedância eletroquímica como uma ferramenta para estimativa de constante taxa eletroquímica

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). ...