Breve Historia de los Aerogeles de Sílice

Un gran número de personas da por sentado que los aerogeles son productos
recientes de la tecnología moderna. En realidad, los primeros aerogeles se
prepararon en 1931. Por aquel entonces, Steven. S. Kistler del College of the
Pacific de Stockton (California) consiguió demostrar que un «gel» contenía una red
sólida y continua del mismo tamaño y forma que un gel húmedo.
La forma más lógica de demostrar esta hipótesis consistía en extraer el líquido del
gel húmedo sin dañar el componente sólido.
Como suele ocurrir, esa forma lógica incluía muchos obstáculos. Si dejamos que
un gel se seque por sí solo, éste encogería, a menudo hasta alcanzar una fracción
de su tamaño original. Esta reducción de tamaño normalmente iba acompañada
de un fuerte craquelado del gel. Kistler supuso, correctamente, que el componente
sólido del gel era microporoso, y que el punto de contacto entre el líquido y el
vapor del líquido en evaporación empleaba grandes fuerzas de tensión superficial
que colapsaban la estructura del poro. Kistler entonces descubrió el aspecto
fundamental de la producción del aerogel: [«Obviamente, para producir un aerogel
[Kistler acuñó este término], hay que reemplazar de algún modo el líquido por aire
sin permitir que la superficie del líquido se pierda por el interior del gel. Si
mantenemos el líquido bajo una presión siempre superior a la presión del vapor y
aumentamos la temperatura, dicho líquido se convertirá, al alcanzar la temperatura
crítica, en un gas sin que se den dos fases de manera simultánea» (S.S. Kistler, J.
Phys. Chem. 34, 52, 1932).]
Los primeros geles que estudió Kistler eran geles de sílice preparados mediante la
condensación ácida de silicato de sodio acuoso. Sin embargo, los intentos de
preparar aerogeles mediante la conversión del agua de estos geles en un fluido
supercrítico no tuvieron éxito. En vez de formarse un aerogel de sílice, el agua
supercrítica redisolvió la sílice, que después precipitó mientras se evaporaba el
agua. Entonces se sabía que el agua de los geles acuosos se podía sustituir con
líquidos orgánicos miscibles. Kistler lo intentó de nuevo, lavando bien los geles de
sílice con agua (para retirar las sales del gel) y sustituyendo el agua por alcohol. Al
convertir el alcohol en un fluido supercrítico y permitir su evaporación, se formaron
los primeros verdaderos aerogeles. Los aerogeles de Kistler eran muy similares a
los aerogeles de sílice que se preparan en la actualidad. Eran materiales
transparentes, de baja densidad y muy porosos que despertaban un gran interés
académico.
Durante los años siguientes, Kistler caracterizó completamente los aerogeles de
sílice y preparó aerogeles con muchos otros materiales, incluyendo alúmina, óxido
de tungsteno, óxido de hierro, óxido de estaño, tartrato de níquel, celulosa, nitrato
de celulosa, gelatina, agar-agar, albúmina de huevo y caucho.
Algunos años después Kistler abandonó el College of the Pacific y consiguió un
puesto en la empresa Monsanto Corp.
Monsanto comenzó a comercializar un producto conocido simplemente como
«aerogel». El Aerogel de Monsanto era un material de sílice granular. Poco se
sabe sobre las condiciones de procesamiento que se utilizaron para este material,
pero se asume que su producción seguía los métodos de Kistler. El Aerogel de
Monsanto fue utilizado como agente aditivo o tixotrópico en cosméticos y
dentífricos. Durante las tres décadas siguientes se avanzó poco en el campo de
los aerogeles. Al cabo del tiempo, en los años sesenta, el desarrollo de la
económica sílice «ahumada» debilitó el comercio del aerogel, por lo que Monsanto
dejó de producirlo.
Los aerogeles ya habían pasado a la historia cuando, a finales de los años
setenta, el gobierno francés mantuvo contactos con
Stanislaus Teichner de la Université Claude Bernard (Lyon) buscando un método
para almacenar oxígeno y carburante de misiles dentro de materiales porosos.
Hay una leyenda transmitida entre los investigadores pertenecientes a la
comunidad de los aerogeles sobre lo que sucedió después. Teichner le confirió a
uno de sus pupilos licenciados el trabajo de preparar y estudiar los aerogeles con
el objetivo mencionado anteriormente. Sin embargo, siguiendo el método de
Kistler, que incluía dos laboriosos y prolongados pasos de intercambio de
solvente, se necesitaron varias semanas para preparar el primer aerogel.
Teichner le comunicó a su pupilo que necesitaría un gran número de muestras de
aerogel para completar su trabajo. Al comprobar que para llevar a cabo tal tarea,
necesitaría muchos, muchos años, el estudiante abandonó el laboratorio de
Teichner sufriendo un ataque de nervios. Cuando regresó al laboratorio después
de un descanso tenía una gran motivación por descubrir un mejor proceso
sintético. El resultado fue uno de los mayores avances dentro de la ciencia del
aerogel, concretamente en cuanto a la aplicación de la química sol-gel en la
preparación del aerogel de sílice. Este proceso reemplazó el silicato de sodio que
utilizaba Kistler por un alcoxilo (tetrametilortosilicato, TMOS). Al hidrolizar TMOS
en una solución de metanol se producía un gel en sólo un paso (denominado
«alcogel»). Con ello se eliminaron dos de los inconvenientes del método de Kistler,
más concretamente, el paso del intercambio de agua por alcohol y la presencia de
sales inorgánicas en el gel. Al secar los alcogeles bajo unas condiciones de
alcohol supercrítico se produjeron aerogeles de sílice de calidad óptima.
Durante los años siguientes, el grupo de trabajo de Teichner y otros investigadores
utilizaron este método para preparar otros aerogeles de gran variedad con óxidos
metalicos.
Tras este descubrimiento los avances dentro del campo de los aerogeles se
sucedieron de forma rápida a medida que aumentaba el número de investigadores
en la materia. Algunos de los logros notables son:
• Durante la primera mitad de los años ochenta los investigadores de física de
partículas se dieron cuenta de que los aerogeles de sílice serían un medio ideal
para la producción y la detección de la radiación de Cherenkov. Para realizar estos
experimentos se necesitaban grandes losas transparentes de aerogel de sílice.
Utilizando el método del TMOS, se fabricaron dos detectores de gran tamaño. Uno
utilizaba 1700 litros de aerogel de sílice en el detector TASSO de la
Deutsches Elektronen Synchrotron (DESY) de Hamburgo y otro en CERN utilizaba
1000 litros de aerogel de sílice preparado en la Universidad de Lund de Suecia.
• La primera planta piloto para la producción de bloques de aerogel de sílice que
utilizaba el método del TMOS fue establecida por miembros del grupo Lund de
Sjobo (Suecia). Dicha planta incluía una autoclave diseñada para soportar las
altas presiones y temperaturas que se dan con el metanol supercrítico (240ºC y 80
atmósferas). No obstante, en 1984 la autoclave desarrolló un escape durante una
secuencia de producción. La habitación donde se encontraba el recipiente se llenó
rápidamente de vapores de metanol y posteriormente explotó. Afortunadamente
no hubo que lamentar víctimas mortales, aunque las instalaciones quedaron
totalmente destrozadas. La planta se volvió a construir y aún hoy en día produce
aerogeles de sílice utilizando el proceso del TMOS. La planta es controlada en la
actualidad por Airglass Corp.
• En 1983 Arlon Hunt y el Microstructured Materials Group del Laboratorio de
Berkeley (California) descubrieron que el compuesto TMOS, muy tóxico, podría
sustituirse con tetraetilortosilicato (TEOS), que es un reactivo mucho más seguro.
La calidad de producción de los aerogeles no disminuyó.
• Al mismo tiempo el Microstructured Materials Group del Laboratorio de Berkeley
descubrió que el alcohol del interior del gel podría reemplazarse por dióxido de
carbono líquido antes de llevarse a cabo el secado supercrítico sin dañar el
aerogel. Este hecho significaba un avance importante en cuanto a la seguridad, ya
que el punto crítico del CO2 (31ºC y 1050psi) tiene lugar bajo unas condiciones
mucho menos agudas que el punto crítico del metanol (240ºC y 1600psi).
Además, a diferencia del alcohol, el dióxido de carbono no representa ningún
peligro de explosión. Este proceso se utilizó por primera vez para producir placas
de aerogel de sílice transparente a partir de TEOS.
• La empresa alemana BASF desarrolló simultáneamente métodos de sustitución
de CO2 para la preparación de perlas de aerogel a partir de silicato de sodio. Este
material se ha estado produciendo hasta 1996 con el nombre comercial de
«BASOGEL».
• En 1985 el Catedrático Jochen Fricke organizó el primer Simposio Internacional
sobre Aerogeles (ISA) en Würzburg (Alemania). En esta conferencia científicos de
todo el mundo presentaron hasta un total de 25 ponencias. Se celebraron
posteriores ISAs en los años 1988 en Montpellier (Francia), 1991 en Würzburg, y
1994 en Berkeley (California). La cuarta ISA estableció un récord de asistencia
con 151 participantes, 10 ponencias invitadas, 51 ponencias de contribución y 35
exposiciones de cartel. La quinta ISA se celebró recientemente en Montpellier y
contó con casi 200 asistentes.
• A finales de los años ochenta científicos del Laboratorio Internacional de
Lawrence Livermore (LLNL) dirigidos por Larry Hrubesh prepararon el aerogel de
sílice de menor densidad del mundo (y el material sólido de menor densidad).
Dicho aerogel tenía una densidad de 0,003g/cm3, sólo tres veces mayor que la del
aire.
• Poco después, Rick Pekala, miembro también del LLNL, siguiendo las técnicas
utilizadas para preparar aherrójeles inorgánicos, preparó aerogeles de polímeros
orgánicos. Entre éstos estaban los aerogeles de resorcinol-formaldehido y de
melamina-formaldehido. Los aerogeles de resorcinol-formaldehido se podían
pirolizar para producir aerogeles de carbón puro. Este hecho abrió nuevas
expectativas dentro de la investigación del aerogel.
• Thermalux, L.P. fue fundada en 1989 por Arlon Hunt, y por otros colaboradores,
en Richmond (California). Thermalux operaba una autoclave de 300 litros para la
producción de bloques de aerogel de sílice a partir de TEOS utilizando el proceso
de sustitución del dióxido de carbono. Thermalux preparó una gran cantidad de
aerogeles, pero, desafortunadamente, dejó de funcionar en 1992.
• El aerogel de sílice, preparado en el Jet Propulsion Laboratory (Laboratorio de
Propulsión a Chorro), ha ido a bordo del Space Shuttle en varias misiones. En
estos vuelos se utiliza el aerogel de muy baja densidad para recoger y traer a la
tierra muestras de polvo cósmico de alta velocidad.
• Investigadores de la University of New Mexico, dirigidos por C. Jeff Brinker y por
Doug Smith, y de otras instituciones cada vez están más cerca de eliminar el paso
de secado supercrítico utilizado en la producción de aerogel mediante la
modificación química de la superficie del gel previa al secado. Esta investigación
tuvo como consecuencia la fundación de Nanopore para comercializar aerogeles
de bajo coste.
• En 1992, Hoechst Corp. también inició en Francfort un programa de aerogeles
granulares de bajo coste.
• En 1994, la Aerojet Corp. inició en Sacramento (California) un proyecto
cooperativo con el Laboratorio de Berkeley, el LLNL y otros para comercializar los
aerogeles utilizando el proceso de sustitución del dióxido de carbono. Aerojet
consiguió la autoclave de 300 litros antiguamente controlada por Thermalux,
produciendo así varias formas de aerogeles de sílice de resorcinol-formaldehido y
de carbono. Sin embargo, abandonaron el programa en 1996.
Cada vez es mayor el número de investigaciones y desarrollos, por lo que, en un
futuro muy cercano, seguramente habrá muchas más aplicaciones y avances en la
tecnología de los aerogeles.
Cómo se Preparan los Aerogeles de Sílice
(Translation from English by "mailto:chicken17@arrakis.es" , University of
Granada, Spain)
La discusión posterior se basa en los siguientes términos:
Hidrólisis:
Reacción de un alcoxilo metálico (M-OR) con el agua, formándose un hidróxido
metálico (M-OH).
Condensación:
Una reacción de condensación tiene lugar cuando dos hidróxidos metálicos (M-OH
+ HO-M) se combinan para producir una especie de óxido metálico (M-O-M). Esta
reacción forma una molécula de agua.
Sol:
Solución de varios reactivos que sufren reacciones de hidrólisis y de
condensación. El peso molecular del tipo de óxido que se produce no deja de
aumentar. A medida que crecen, estas especies suelen empezar a unirse unas a
otras formando una red tridimensional.
Punto de gel:
Momento en que la red de partículas de óxido unidas abarca el contenedor donde
se encuentra el sol. Cuando se alcanza el punto de gel, el sol se convierte en
Alcogel.
Alcogel (gel húmedo):
Cuando se alcanza el punto de gel, la mezcla forma una sustancia rígida
denominada alcogel. El alcogel puede extraerse del contenedor original donde se
encuentra, y mantenerse fuera de éste. Un alcogel consta de dos partes, una
sólida y otra líquida. La parte sólida es la red tridimensional de partículas de óxido
unidas. La parte líquida (el solvente original del sol) rellena el espacio libre que
queda alrededor de la parte sólida. Aparentemente ambas partes de un alcogel
ocupan el mismo volumen.
Fluido supercrítico:
Sustancia que se encuentra por encima de su presión y temperatura críticas. Un
fluido supercrítico cuenta con algunas propiedades en común con los líquidos
(densidad y conductividad térmica) y otras con los gases (abarca el volumen del
contenedor donde se encuentra y no tiene tensión superficial).
Aerogel:
Sobrante de un alcogel cuando se le extrae la parte líquida sin dañar la parte
sólida (esto se consigue normalmente mediante la extracción supercrítica). Si se
hace correctamente, el aerogel conserva la forma original del alcogel y como
mínimo un 50% (normalmente>85%) del volumen del alcogel.
Xerogel:
Remanente cuando se extrae la parte líquida de un alcogel mediante evaporación
o mediante métodos similares. Los xerogeles pueden conservar su forma original,
aunque a menudo se agrietan. Normalmente, en el caso de los xerogeles, la
reducción de tamaño que se produce durante el secado es extrema (-90%).
Química sol-gel
Por lo general, la formación de aerogeles comprende dos pasos principales: la
formación de un gel húmedo y el secado del gel húmedo para formar un aerogel.
En un principio, los geles húmedos se preparaban mediante la condensación
acuosa del silicato de sodio o de un material similar. A pesar del buen
funcionamiento de este proceso, la reacción formaba sales dentro del gel que sólo
se podían extraer lavándo el gel una y otra vez (procedimiento largo y laborioso).
Gracias al rápido desarrollo de la química sol-gel durante las últimas décadas, la
gran mayoría de los aerogeles de sílice que se preparan en la actualidad utiliza
precursores de alcoxilo de silicona. Los más utilizados son el tetrametil ortosilicato
(TMOS, Si(OCH3)4) y el ortosilicato tetraetilo (TEOS, Si(OCH2CH3)4). Sin
embargo, se pueden utilizar muchos otros alcoxilos que contengan varios grupos
funcionales orgánicos para que el gel adquiera propiedades diferentes. La química
sol-gel basada en alcoxilos evita la formación de los poco deseados productos
derivados de la sal, además de posibilitar un control mucho mayor sobre el
producto final. La ecuación química equilibrada para la formación de un gel de
sílice a partir de TEOS es:

Si(OCH2CH3)4 (líquido) = SiO2 (sólido) + 4HOCH2CH3 (líquido)

Esta reacción normalmente se lleva a cabo en etanol; la densidad final del aerogel
depende de la concentración de los monómeros de alcoxilo de silicona que hay en
la solución. Cabe destacar que la estoiquiometría de la reacción precisa dos moles
de agua por cada mol de TEOS. En la práctica, esta cantidad de agua tiene como
consecuencia una reacción incompleta y unos aerogeles débiles y empañados. La
mayoría de las fórmulas para preparar aerogeles utiliza por tanto un mayor
porcentaje de agua del que aconseja la ecuación equilibrada (entre 4 y 30
equivalentes).
Catalizadores
La cinética de la reacción anterior es poco práctica por su lentitud a temperatura
ambiente, por lo que a menudo se necesitan varios días para llevarla a cabo
totalmente. Para acortar el proceso se añaden catalizadores ácidos o básicos a la
fórmula. Las propiedades microestructurales, físicas y ópticas del producto de
aerogel final dependerán de la cantidad y el tipo de catalizador que se emplee.
Los catalizadores ácidos pueden consistir en un ácido prótido cualquiera, como el
HCl. Los catalizadores básicos por lo general utilizan amoníaco o amoníaco
amortiguado con fluoruro amónico. Los aerogeles preparados con catalizadores
ácidos normalmente encogen más durante el secado supercrítico y pueden ser
menos transparentes que los aerogeles preparados con un catalizador básico. La
descripción precisa de los efectos microestructurales de varios catalizadores es
bastante compleja, ya que la subestructura de las partículas primarias de los
aerogeles puede ser difícil de distinguir con un microscopio electrónico.
Todos contienen unas partículas pequeñas (2-5nm de diámetro), normalmente
esféricas o con forma de huevo. Por el contrario, en el caso de los catalizadores
ácidos, estas partículas pueden resultar «menos sólidas» (con la apariencia de
una bola de cuerda) que las obtenidas en los geles preparados con catalizadores
básicos.
A medida que progresan las reacciones de condensación, el sol se convertirá en
un gel rígido. Es en este punto cuando normalmente se extrae el gel del molde,
aunque hay que mantener cubierto el gel con alcohol para evitar que evapore el
líquido contenido dentro de los poros del gel. La evaporación puede dañar
seriamente el gel y disminuir la calidad del aerogel resultante.
Aerogeles de un paso frente a aerogeles de dos pasos
Los geles normales preparados a partir de TEOS con catalizadores ácidos o con
catalizadores básicos suelen encuadrarse dentro de los geles «de un paso» (para
la reacción sólo se necesita «un recipiente»). Un método desarrollado
recientemente emplea TEOS pre-polimerizado como fuente de sílice. El TEOS
pre-polimerizado se prepara calentando una solución de etanol de TEOS con una
cantidad sub-estoiquiométrica de agua y un catalizador ácido. El solvente se
extrae mediante destilación, quedando un fluido viscoso que contiene óxido-
alcoxilo de silicona de un peso molecular superior. Este material se redisuelve en
etanol y reacciona con el agua restante bajo condiciones básicas hasta que se
produce la gelatinación. Los geles que se preparan siguiendo este método se
denominan geles catalizados ácidos/ básicos «de dos pasos». El TEOS pre-
polimerizado se encuentra disponible en los EEUU y es comercializado por
Silbond Corp. (Silbond H-5).
Estas condiciones de procesamiento ligeramente distintas provocan unos
pequeños pero importantes cambios en el producto final de aerogel. Normalmente,
los aerogeles preparados mediante un catalizador básico de un paso son
mecánicamente más fuertes, aunque también más quebradizos, que los aerogeles
de dos pasos. Sin embargo, los aerogeles de dos pasos tienen una distribución del
tamaño de los poros más pequeña y estrecha, además de ser normalmente más
transparentes óptimamente que los aerogeles de un solo paso.
Maduración y remojo
Las reacciones de hidrólisis y de condensación del reactivo alcoxilo de silicona a
menudo se consideran completas cuando el sol alcanza el punto de gel, aunque
no suele ser este el caso. El punto de gel no es más que el momento en que las
especies de sílice que se encuentran bajo el proceso de polimerización abarcan el
volumen del contenedor donde está el sol. En ese momento la columna de sílice
del gel contiene una importante cantidad de grupos alcoxilos sin reaccionar. De
hecho, aún puede darse hidrólisis y condensación hasta que se complete la
gelatinación. Uno de los errores más comunes en la preparación de aerogeles de
sílice se comete al no tener en cuenta ese aspecto. La solución es fácil, hay que
tener paciencia. La red de sílice será más fuerte si se le da el tiempo suficiente.
Este proceso puede tener un mejor resultado controlando el pH y el contenido de
agua de la solución que cubre el aerogel. Uno de los procedimientos que se
suelen utilizar para la maduración de los geles catalizados básicos consiste en
remojar el gel en una mezcla de alcohol y agua proporcional al sol original bajo un
pH de 8-9 (amoníaco). Es recomendable dejar reposar los geles en esta solución
hasta un máximo de 48 horas.
Este paso, así como los posteriores pasos de procesamiento, es controlado
mediante difusión. O sea que la introducción o extracción de material dentro o
fuera del gel no se ve afectada por convección o mezcla (debido a la solidez de la
red de sílice).
Sin embargo, la difusión sí se ve afectada por el grosor del gel. En breve, el
tiempo necesario para cada paso de procesamiento aumenta de forma radical a
medida que aumenta el grosor del gel. Este hecho limita la producción práctica de
los aerogeles a piezas de 1 a 2 centímetros de grosor.
Una vez haya madurado el gel y antes de proceder al secado, se debe extraer
todo el agua que queda dentro de los poros. Para ello, se debe remojar el gel
varias veces en alcohol puro hasta que no quede nada de agua. Una vez más, el
tiempo que se necesita para este proceso depende del grosor del gel. Si se deja
agua dentro del gel, ésta no podrá ser extraída mediante el secado supercrítico,
por lo que el resultado será un aerogel opaco, blanco y muy denso.
Secado supercrítico
El último proceso y el más importante a la hora de preparar aerogeles de sílice es
el secado supercrítico. Durante este proceso se extrae el líquido remanente dentro
del gel, dejando sólo la red de sílice entrelazada. El proceso se puede llevar a
cabo mediante la evaporación de etanol por encima de su punto crítico (altas
temperaturas, o sea muy peligroso) o mediante un intercambio del solvente con
CO2 seguido de una evaporación supercrítica (bajas temperaturas, o sea menos
peligroso). Este proceso se debe llevar a cabo en una autoclave especialmente
diseñada para este fin (en el caso del secado de CO2 se pueden utilizar las
autoclaves de poco tamaño que emplean los usuarios de microscopios
electrónicos para preparar muestras biológicas). El proceso consiste en los pasos
siguientes: los alcogeles se colocan en la autoclave (previamente rellenada con
etanol). Después se presuriza el sistema a una presión de al menos 750-850psi
con CO2 y se enfría hasta alcanzar los 5-10ºC.
Se introduce CO2 líquido dentro del recipiente hasta que se haya extraído todo el
etanol de dicho recipiente y del interior de los geles. Cuando ya no quede etanol
en los geles, se calienta el recipiente hasta una temperatura superior a la
temperatura crítica del CO2 (31ºC). A medida que se calienta el recipiente,
aumenta la presión del sistema. Se suelta el CO2 con cuidado para mantener una
presión ligeramente superior a la presión crítica del CO2 (1050psi). El sistema
debe mantenerse bajo estas condiciones durante un corto periodo de tiempo. A
continuación se suelta de forma lenta y controlada el CO2 a temperatura
ambiente. Como en los pasos anteriores, el tiempo que se necesita para llevar a
cabo este proceso depende del grosor de los geles. El proceso puede durar entre
12 horas y 6 días. Tras este proceso se puede abrir el recipiente y admirar así la
belleza intrínseca de los aerogeles.
La gráfica siguiente muestra las condiciones del proceso de sustitución/ secado
con dióxido de carbono y las del proceso de secado con alcohol.
Fórmulas generales
Aerogel de sílice catalizado básico de un paso
Para preparar un aerogel con una densidad aproximada de 0,08g/cm3, el tiempo
de gel debería estar entre los 60 y los 120 minutos, dependiendo de la
temperatura.
1. Mezclar dos soluciones:
1. Solución de sílice con 50mL de TEOS y 40mL de etanol.
2. Solución catalizadora con 35mL de etanol, 70mL de agua, 0,275mL de
amoníaco 30% acuoso y 1,21mL de fluoruro amónico de 0,5M.
2. Añadir lentamente la solución catalizadora a la solución de sílice mientras se
remueve.
3. Verter la mezcla dentro de un molde apropiado y esperar a que se produzca la
gelatinación.
4. Proceder siguiendo los pasos descritos en los apartados anteriores.
Aerogel de sílice catalizado básico de dos pasos
Para preparar un aerogel con una densidad aproximada de 0,08g/cm3, el tiempo
de gel debería estar entre los 30 y los 90 minutos, dependiendo de la temperatura.
1. Mezclar dos soluciones:
1. Solución de sílice con 50mL de sílice precondensada (Silbond H-5, o un
equivalente) y 50mL de etanol.
2. Solución catalizadora con 35mL de etanol, 75mL de agua y 0,35mL de
amoníaco 30% acuoso.
2. Añadir lentamente la solución catalizadora a la solución de sílice mientras se
remueve.
3. Verter la mezcla dentro de un molde apropiado y esperar a que se produzca la
gelatinación.
4. Proceder siguiendo los pasos descritos en los apartados anteriores.
"http://www.lbl.gov/http://www.lbl.gov"
Cómo Manejar los Aerogeles de Sílice sin Romperlos
Lo primero que hace la mayoría de la gente cuando toca aerogeles de sílice por
primera vez es romperlos en un millón de trozos. En la radio y televisión de vez en
cuando se oyen cosas como: «Un nuevo material de la Era Espacial que aguanta
hasta 1000 veces su propio peso…». Esto quizás sea verdad, pero no hay que
olvidar que, para un material de tan baja densidad, «1000 veces su propio peso»
no es en absoluto mucho peso. Además, también es importante destacar que el
aerogel de sílice no es más que otro tipo de cristal. Si el aerogel no se maneja con
cuidado, se romperá, aunque, si se tiene cuidado, este material se puede manejar
y se le puede dar forma de manera muy eficaz. Algunas sugerencias son:
• No se deben levantar piezas grandes de aerogel por las esquinas. Pasar una
plancha fina de metal o de otro material consistente por debajo del aerogel para
desplazarlo.
• El aerogel de sílice dura mucho más si se encuentra bajo compresión. Para
ponerlo bajo compresión, se puede simplemente sellar al vacío el aerogel dentro
de una bolsa de plástico (un envasador de alimentos al vacío funciona bien). Este
método es muy útil cuando se quieren enviar muestras por correo.
• La mejor herramienta para cortar un aerogel de sílice es una sierra con filo de
diamante, similar a la que se utiliza para cortar gemas y piedras. Lo más difícil es
mantener inmóvil el material. Una herramienta de succión es muy útil.
• La mayor parte del aerogel de sílice se destruye al entrar en contacto con
líquidos, aunque se puede proteger con agua
• Los cambios momentáneos de presión ambiental pueden provocar que el
aerogel se rompa debido a la posible salida o entrada de gases en la estructura
porosa. Hay que tener cuidado si se pone el aerogel a altas presiones.
Un gran número de personas se pregunta si existen peligros tóxicos asociados
con el manejo del aerogel de sílice. Manejar un aerogel con las manos al
descubierto podría dañar la piel. Esto se debe a la absorción de humedad y
aceites de la piel que ejercen los poros del aerogel. Es más una molestia que un
problema tóxico, y puede evitarse con un par de guantes. Al cortar y darle forma a
un aerogel se suele producir una nube de polvo fino. Las partículas del aerogel
que hay en el polvo son homogéneas y redondas, por lo que no suponen un daño
de laceración (a diferencia de los asbestos, por ejemplo). No obstante, sería
recomendable trabajar con ropa aislante o con un buen respirador para no inhalar
el polvo de aerogel.
Silica Aerogels for Absorbing Kinetic Energy
When someone who has never seen a piece of silica aerogel holds some for the
first time, the following chain of events usually results. The observer first notices
the transparency and light weight of the aerogel and makes some sort of remark
about these properties. Then the piece is held between two fingers and gently
squeezed. The aerogel gives a little, and springs back. Then a little more force is
applied and...pffttt, the piece shatters into a thousand pieces, most of which find a
home deep in the carpeting, never to be seen again. Not surprisingly, researchers
who have spent the time and effort required to make silica aerogels are usually
very reluctant to hand them out to just anyone. Because of this, an application of
silica aerogels that has been largely overlooked is their use as an absorber of
kinetic energy (impacts) in safety and protective devices.
Energy Absorbing Materials
In very simplified terms, materials absorb kinetic energy by plastic deformation,
elastic deformation, brittle fracture, or by the fluid dynamics of gases or liquids
within the material. Materials used today for absorbing impacts are commonly
organic foams, such as expanded polystyrene, polyurethanes, polyethers, or
polyethylene. These typically show elastomeric or plastic behavior. Silica aerogels,
being an inorganic solid, are inherently brittle. A brittle material would, at first, seem
to be a poor choice for a cushioning material. However, as silica aerogels are
usually very low density materials, the collapse of the solid network occurs
gradually, spreading the force of impact out over a longer time. Additionally, as
silica aerogels are an open-pored material, the gas contained within the bulk of the
solid in forced outwards as the material collapses. In doing so, the gas must pass
through the "http://eande.lbl.gov/ECS/aerogels/sapore.htm" of the aerogel. The
frictional forces caused as a gas passes through a restricted opening are indirectly
proportional to the square of the pore diameter. As silica aerogels have very
narrow pores (~20-50 nm), gases rapidly passing through the material will absorb a
considerable amount of energy. Therefore, the energy of an object impacting a
silica aerogel is taken up by the aerogel by the collapse of its solid structure and
the release of gas from within the material.
An effective material for use in safety devices will serve to minimize the force felt
by the object (or person) to be protected. This is usually done by spreading the
deceleration of the impacting object over a longer period of time. The graphic
below shows load versus time for a silica aerogels sample, and two other
materials. The samples were cubes 5 cm on a side and were crushed by an 8 lb.
weight traveling at 11 ft/sec. The red curve represents a silica aerogel with a
density of 0.1g/cm3, the yellow curve is expanded polystyrene, and the green is
an elastomeric polypropylene foam. The plots show that both the aerogel and the
polystyrene foam reduce the maximum load produced to a very low level. It may,
therefore, seem that readily available polystyrene foam may be a more appropriate
material than the more unusual silica aerogel.
The situation is not as straightforward as this. Many organic foams produce a
significant amount of rebound when they are impacted. This transfers a portion of
the energy absorbed by the material back into the object that impacted it (such as
a human head). This rebound effect can often do further damage to the object
being protected. The plot of deflection (distance moved by the impacting object) vs.
time for silica aerogel and polystyrene shown below demonstrates the differences
of these materials
(Note: Deflection data are derived from measured load values and are for
comparison purposes only). The polystyrene (yellow), which behaves elastically
and plastically, is crushed by the impacting weight (positive deflection) but then
springs back to a considerable fraction of its original volume. Conversely, the
weight that impacts the silica aerogel (red) travels a certain distance into the
material and then comes to a complete stop without bouncing. This is an important
phenomenon to consider when developing materials for safety and protective
devices.
These data were collected using a Dynatup Drop-Weight System with the kind
assistance of "http://www.grci.com/grcinst" ,
Santa Barbara, CA, a division of "http://www.grci.com/" .
Environmental Concerns
The production and use of silica aerogels is environmentally benign. No
significantly hazardous wastes are produced during their production. The disposal
of silica aerogels is perfectly natural. In the environment, they quickly crush into a
fine powder that is essentially identical to one of the most common substances on
Earth, namely, sand. Additionally, silica aerogels are completely non-toxic and non-
flammable. If they eventually find their way into widespread use as protective
materials, they could eliminate a very large amount of unwanted plastic materials.
Potential Uses
The attractive energy absorbing properties of silica aerogels may lead to their use
in various applications. These may include personal protection in motor vehicles,
protection of sensitive equipment such as aircraft flight data recorders, and
protection of electronic equipment such as laptop computer hard drives.
The Surface Chemistry of Silica Aerogels
Silica aerogels contain primary particles of 2-5 nm in diameter. Silica particles of
such a small size have an extraordinarily large surface-to-volume ratio (~2 x 109
m-1) and a corresponding high specific surface area (~900 m2/g). It is not
surprising, therefore, that the chemistry of the interior surface of an aerogel plays a
dominant role in its chemical and physical behavior. It is this property that makes
aerogels attractive materials for use as catalysts, catalyst substrates, and
adsorbents.
The nature of the surface groups of a silica aerogel are strongly dependent on the
conditions used in its preparation. For example, if an aerogel is prepared using the
supercritical alcohol drying process, its surface may consist primarily of alkoxy-
(-OR) groups. On the other hand, with the carbon dioxide drying process the
surface is almost exclusively covered with hydroxyl (-OH) groups. The extent of
hydroxyl- coverage is ~5 -OH/nm2, a value consistent with other forms of silica.
This value, combined with their high specific surface area, means that silica
aerogels present an extremely large number of accessible hydroxyl groups. Silica
aerogels are therefore a somewhat acidic material. A more striking effect of the
hydroxyl surface is seen the physical behavior of silica aerogels. As with most
hydroxyl surfaces, the surface of silica aerogels can show strong hydrogen-
bonding effects. Because of this, silica aerogels with hydroxyl surface are
extremely hygroscopic. Dry silica aerogels will absorb water directly from moist air,
with mass increases of up to 20%. This absorption has no visible effect on the
aerogel, and is completely reversible. Simply heating the material to 100-120
degrees C will completely dry the material in about an hour (or longer, depending
on thickness). As the sample cools, water will reabsorb quickly (mass increases
can be seen almost immediately).
While the adsorption of water vapor does not harm silica aerogels, contact with
liquid water has disastrous results. The strong attractiveforces that the hydroxyl
surface exerts on water vapor also attracts liquid water. However, when liquid
water enters a nanometer-scale pore, the surface tension of water exerts capillary
forces strong enough to fracture the solid silica backbone.
The net effect is a complete collapse of the aerogel monolith. The material
changes from a transparent solid with a definite shape to a fine white powder. The
powder has the same mass and total surface area as the original aerogel, but has
lost its solid integrity. Silica aerogels with fully hydroxylated surfaces are, therefore,
classified as "hydrophilic".
This would appear to pose a significant problem to using silica aerogels in exposed
environments. Fortunately, this problem can be easily circumvented by converting
the surface hydroxyl (-OH) groups to a non-polar (-OR) group. This is effective
when R is one of many possible aliphatic groups, although trimethylsilyl- groups
are the most common. The derivitization can be performed before (on the wet gel)
or after (on the aerogel) supercritical drying. This completely protects the aerogel
from damage by liquid water by eliminating the attractive forces between water and
the silica surface. In fact, silica aerogels treated in this way can not
be wet by water, and will float on its surface indefinitely. Silica aerogels that have
been derivitized in this way are classified as "hydrophobic".
The illustrations below demonstrate the interaction of water with the pore structure
and solid backbone of silica aerogels.
The Pore Structure of Silica Aerogel
The pore structure of silica aerogels is difficult to describe in words. Unfortunately,
the available methods of characterizing porosity do only a slightly better job. The
International Union of Pure and Applied Chemistry has recommended a
classification for porous materials where pores of less than 2 nm in diameter are
termed "micropores", those with diameters between 2 and 50 nm are termed
"mesopores", and those greater than 50 nm in diameter are termed "macropores".
Silica aerogels possess pores of all three sizes. However, the majority of the pores
fall in the mesopore regime, with relatively few micropores. The pore size
distribution of a single-step silica aerogel is shown below:
It is very important when interpreting porosity data to indicate the method used to
determine the data. Various measurement techniques can give differing results for
the same sample. The entire range of characterization methods has been applied
to silica aerogels, including:
Gas/Vapor adsorption
This is the most widely available and utilized method for determining aerogel
porosity. In this technique a gas, usually nitrogen, at its boiling point, is adsorbed
on the solid sample. The amount of gas adsorbed depends of the size of the pores
within the sample and on the partial pressure of the gas relative to its saturation
pressure. By measuring the volume of gas adsorbed at a particular partial
pressure, the Brunauer, Emmit and Teller (BET) equation gives the specific surface
area of the material. At high partial pressures the hysteresis in the
adsorption/desorption curves (called "isotherms"), the Kelvin equation gives the
pore size distribution of the sample. The pore size distribution shown above was
determined using a 40-point nitrogen adsorption/desorption analysis. Gas
adsorption methods are generally applicable to pore in the mesopore range.
However, microporosity information can be inferred through mathematical analyses
such as t-plots or the Dubinin-Radushevich method.
Gas adsorption can not effectively determine macropores. For a detailed
description of this procedure, see the IUPAC guidelines for "Reporting
Physisorption Data for Gas/Solid Systems" in Pure and Applied Chemistry, volume
57, page 603, (1985).
Mercury Porosimetry: This technique is generally not effective for
aerogels. The high compressive forces encountered in forcing mercury into the
pores of an aerogel cause its structure to collapse.
Scattering Methods (x-ray, neutron and visible light):
Scattering methods involve the angle dependent deflection of radiation
by features within the sample. These features can be solid particles or pores.
Scattering efficiency is greatest when the wavelength of the radiation used is
comparable to the features being studied. X-ray and neutron scattering are
particularly well suited for determining the fractal geometry of the aerogel pore
network. See the section on "file:///C|/Mis documentos/saoptic.htm" for a
discussion of visible light scattering.
Other methods: Gas/solid NMR, electron microscopy of replicants, and
atomic force microscopy have also been used to characterize the pore network of
silica aerogels with limited success.
Because of the limitations of these methods, a major problem in aerogel science
remains unresolved. If the mass, density, and total pore volume of an aerogel are
measured, it is apparent that there is a substantial amount of porosity that is not
accounted for. This obviously results from the drawbacks of using gas adsorption
to determine the pore volume. It is assumed that the "missing porosity" lies in the
micro- or macropore regimes, areas not measured effectively by this method.
One final important aspect of the aerogel pore network is its "open" nature and
interconnectedness. Pores in various materials are either open or closed
depending on whether the pore walls are solid or themselves porous (or at least
"holey"). A macroscopic example of a open-pored material is a common sponge,
while "bubble wrap" packaging is an example of a closed-pore material. In a
closed-pore material, gases or liquids can not enter the pore without breaking the
pore walls. This is not the case with an open-pore structure. In this instance, gases
or liquids can flow from pore to pore, with limited restriction, and eventually through
the entire material. It is this property that makes silica aerogels effective materials
for gas phase catalysts, microfiltration membranes, adsorbents, and substrates for
chemical vapor infiltration.
Physical Properties of Silica Aerogels
Note: Most of the properties listed here are significantly affected by the
conditions used to prepare the aerogel and any subsequent post-processing.
Physical properties of silica aerogels
Property Value Comments
Apparent Density 0.003-0.35 g/cm3
Most common density is ~0.1g/cm3
Internal Surface Area 600-1000 m2/g As determined by nitrogen
adsorption/desorption
% Solids 0.13-15% Typically 5% (95% free space)
Mean Pore Diameter ~20 nm As determined by nitrogen adsorption/desorption
(varies with density)
Primary Particle Diameter 2-5 nm Determined by electron microscopy
Index of Refraction 1.0-1.05 Very low for a solid material
Thermal Tolerance to 500 C Shrinkage begins slowly at 500 C, increases with inc.
temperature. Melting point is >1200 C
Coefficient of Thermal Expansion 2.0-4.0 x 10-6 Determined using ultrasonic
methods
Poisson's Ratio 0.2 Independent of density. Similar to dense silica.
Young's Modulus 106-107 N/m2 Very small (<104x) compared to dense silica
Tensile Strength 16 kPa For density = 0.1 g/cm3.
Fracture Toughness ~0.8 kPa*m1/2 For density = 0.1 g/cm3. Determined by 3-
point bending
Dielectric Constant ~1.1 For density = 0.1 g/cm3. Very low for a solid material
Sound Velocity Through the Medium
100 m/sec For density = 0.07 g/cm3. One of the lowest velocities for a solid
material
Optical Properties of Silica Aerogels
The optical properties of silica aerogels are best described by the phrase "silica
aerogels are transparent". This may seem obvious, as silica aerogels are made of
the same material as glass. However, the situation is not as simple as that
comparison.
While distant objects can be viewed through several centimeters of silica aerogel,
the material displays a slight bluish haze when an illuminated piece is viewed
against a dark background and slightly reddens transmitted light. These effects are
a result of Rayleigh scattering effects. The various aspects of optical transmission
through silica aerogel are discussed below.
Rayleigh Scattering
The vast majority of the light that we see when we look at objects is scattered light
(light that reaches our eyes in an indirect way). The phenomenon of scattering
leads to several well known natural effects, such as blue skies, red sunsets, the
white (or gray) color of clouds, and poor visibility on foggy days. Scattering results
from the interaction of light with inhomogeneities in solid, liquid, or gaseous
materials. The actual entity that causes scattering, called the scattering center, can
be as small as a single large molecule (with an inherent inhomogeneity) or clusters
of small molecules arranged in a non-uniform way. However, scattering becomes
more effective when the size of the scattering center is similar to the wavelength of
the incident light. This occurs in small particles (~400-700 nm in diameter for
visible light) that are separated from on another, or by larger, macroscopic,
particles with inherent irregularities. When scattering centers are smaller in size
than the wavelength of the incident light, scattering is much less effective. In silica
aerogels, the primary particles have a diameter of ~2-5 nm, and do not contribute
significantly to the observed scattering. However, scattering does not necessarily
arise from solid structures. There is in silica aerogels, a network of pores which can
act, themselves, as scattering centers. The majority of these are much smaller
(~20 nm) than the wavelength of visible light. There are, however, invariably a
certain number of larger pores that scatter visible light. Control of the number an
size of these larger pores is, to a certain degree, possible by modifying the sol-gel
chemistry used to prepare the aerogel. As scattering efficiency is dependent on the
size of the scattering center, different wavelengths will scatter with varying
magnitudes. This causes the reddening of transmitted light (red light has a longer
wavelength, and is scattered less by the fine structure of aerogels) and the blue
appearance of the reflected light off silica aerogels.
A simple method can be used to quantitatively measure the relative contributions of
Rayleigh scattering and the wavelength-independent transmission factor (due to
surface damage and imperfections) for silica aerogels prepared with different
recipes and/or drying procedures. Briefly, the transmission spectrum of an aerogel
slab of known thickness is measured and the transmission is plotted against the
inverse fourth power of the wavelength. These data are fit to the equation: where T
= transmittance, A = wavelength independent transmission factor, C = intensity of
Rayleigh scattering, t = sample thickness, and Lambda = wavelength. From this
plot A and C can be determined. Aerogels with a high value of A and a low value of
C will be the most transparent. Scattering may also be accompanied by
absorbance which will further attenuate the transmitted light.
Visible Transmission Spectrum
The intrinsic absorbance of silica is low in the visible region. Therefore the
tranmittance in this region is primarily attenuated by scattering effects. As
wavelengths become progressively shorter, scattering increased, eventually cutting
off transmission near 300 nm. Weak absorbances begin to appear in the near
infrared, and again cuts off transmission around 2700-3200 nm.
There is then a "visible window" of transmission through silica aerogel that is an
attractive feature of this material for daylighting applications.
Infrared Spectrum
As the spectrum moves into the infrared, scattering becomes less important, and
standard molecular vibrations account for the spectral structure. A strong, broad
absorbance band is usually observed at 3500 cm-1, due to O-H stretching
vibrations. A weaker O-H bending vibration band is seen at 1600 cm-1. Both
adsorbed water and surface -OH groups contribute to these bands. Thoroughly
drying the sample before analysis will eliminate vibrations due to water, while
surface -OH groups can be significantly eliminated by firing the aerogel at 500
degrees C. The Si-O-Si fundamental vibration gives the strong band at ~1100 cm-
1. There is a region of high infrared transparency between 3300 and 2000 cm-1.
This allows a certain amount of thermal radiation to pass through silica aerogel and
lower its thermal insulative performance. Addition of additives that absorb radiation
in this region can remedy this problem.
Thermal Properties of Silica Aerogels
After preparing the first silica aerogels, Kistler proceeded to characterize them as
thoroughly as possible. One of the extraordinary properties that he discovered was
their very low thermal conductivity. Kistler also found that the thermal conductivity
decreased even further under vacuum. However, in the 1930's thermal insulation
was a low priority and applications of aerogels in insulation systems was not
pursued. The renaissance of aerogel technology around 1980 coincided with an
increased concern for energy efficiency and the environmental effects of
chlorofluorocarbons (CFC's). It was then readily apparent that silica aerogels were
an attractive alternative to traditional insulation due to their high insulating value
and environment-friendly production methods. Unfortunately, the production costs
of the material were prohibitive to cost-sensitive industries such as housing. A
significant research effort was undertaken, and is continuing, at several institutions
worldwide (including Berkeley Lab) to circumvent this problem by increasing the
insulative performance and lowering the production costs of silica aerogels.
The passage of thermal energy through an insulating material occurs through three
mechanisms; solid conductivity, gaseous conductivity, and radiative (infrared)
transmission. The sum of these three components gives the total thermal
conductivity of the material. Solid conductivity is an intrinsic property of a specific
material. For dense silica, solid conductivity is relatively high (a single-pane
window transmits a large amount of thermal energy). However, silica aerogels
possess a very small (~1-10%) fraction of solid silica. Additionally, the solids that
are present consist of very small particles linked in a three-dimensional network
(with many "dead-ends"). Therefore, thermal transport through the solid portion of
silica aerogel occurs through a very tortuous path and is not particularly effective.
The space not occupied by solids in an aerogel is normally filled with air (or
another gas) unless the material is sealed under vacuum. These gases can also
transport thermal energy through the aerogel. The pores of silica aerogel are open
and allow the passage of gas (albeit with difficulty) through the material.
The final mode of thermal transport through silica aerogels involves infrared
radiation. A advantage of silica aerogels for insulation applications is their visible
transparency (which will allow their use in windows and skylights). However, they
are also reasonably transparent in the infrared (especially between 3-5 microns).
At low temperatures, the radiative component of thermal transport is low, and not a
significant problem. At higher temperatures, radiative transport becomes the
dominant mode of thermal conduction, and must be dealt with. The infrared
spectrum of silica.Attempting to calculate the total thermal conductivity arising from
the sum of these three modes can be difficult, as they modes are coupled
(changing the infrared absorbency of the aerogel also changes the solid
conductivity, etc.). It is generally easier to measure the total thermal conductivity
directly rather than predict the effect of changing one component. To achieve this,
the Microstructured Materials Group at Berkeley Lab designed and built an
economical, but accurate instrument for measuring the thermal conductivity of
large aerogel panels. The Vacuum Insulation Conductivity Tester (On Rollers)
-VICTOR, is a thin-film heater based device that can measure the thermal
conductivity of panels up to 26 cm on edge, with pressures of various gases down
to 0.01 Torr.
Minimizing the solid component of thermal conductivity
There is little that can be done to reduce thermal transport through the solid
structure of silica aerogels. Lower density aerogels can be prepared (as low as
0.003 g/cm3), which reduces the amount of solid present, but this leads to aerogels
that are mechanically weaker. Additionally, as the amount of solids decreases the
mean pore diameter increases (with an increase in the gaseous component of the
conductivity). These are, therefore, generally not suitable for insulation
applications. However, as noted above, the tortuous solid structure of silica
aerogels leads to a intrinsically low thermal transport. Granular aerogels have an
extremely low solid conductivity component. This is due to the small point of
contact between granules in an aerogel bed.
However, in granular aerogel, the inter-granule voids increase the overall porosity
of the material thereby requiring a higher vacuum to achieve the maximum
performance (see below).
Minimizing the gaseous component of thermal
conductivity.
A typical silica aerogel has a total thermal conductivity of ~0.017 W/mK
(~R10/inch). A major portion of this energy transport results from the gases
contained within the aerogel. This is the transport mode that is most easily
controllable. As a consequence of their fine pore structure, the mean pore diameter
of an aerogel is similar in magnitude to the mean free path of nitrogen (and
oxygen) molecules at standard temperatures and pressures. If the mean free path
of a particular gas were longer than the pore diameter of an aerogel, the gas
molecules would collide more frequently with the pore walls than with each other. If
this were the case, the thermal energy of the gas would be transferred to the solid
portion of the aerogel (with its low intrinsic conductivity).
Lengthening the mean free path relative to the mean pore diameter can be
accomplished in three ways; by filling the aerogel with a gas with a lower molecular
mass (and a longer mean free path) than air, by reducing the pore diameter of the
aerogel, and by lowering the gas pressure within the aerogel.
The first of these methods is generally not practical, as light gases are relatively
expensive and would eventually escape the system. The mean pore diameter can
be reduced by increasing the density of the aerogel. However, any benefit from a
lower gaseous conductivity component is counteracted by an increase in the solid
conductivity component. The pore diameter can be reduced somewhat (while
keeping the aerogel's density constant) by using the two-step process to prepare
the aerogel. The greatest improvement is found by reducing the gas pressure.
Vacuum insulations are commonplace in various products (such as Thermos
bottles). These systems generally require a high vacuum to be maintained
indefinitely to achieve the desired performance. In the case of aerogels, however, it
is only necessary to reduce the pressure enough to lengthen the mean free path of
the gas relative to the mean pore diameter. This occurs for most aerogels at a
pressure of about 50 Torr. This is a very modest vacuum that can be easily
obtained and maintained (by sealing the aerogel in a light plastic bag).
The graphic below shows Thermal Conductivity vs. Pressure curves obtained on
VICTOR for single-step and two-step silica aerogels. The minimum value of ~0.008
W/mK corresponds to ~R20/inch.
Minimizing the radiative component of thermal conductivity
As noted above, radiative component of thermal conductivity becomes more
important as temperatures increase. If silica aerogels are to be used at
temperatures above 200 degree C, this mode of energy transport must be
suppressed. This can be accomplished by adding an additional component to the
aerogel, either before or after supercritical drying. The second component must
either absorb or scatter infrared radiation. A major challenge for this process is to
add a component that does not interfere with the mechanical integrity of the
aerogel or increase its solid conductivity. One of the most promising additives is
elemental carbon. Carbon is an effective absorber of infrared radiation and, in
some cases, actually increases the mechanical strength of the aerogel.
The graphic below shows Thermal Conductivity vs. Pressure curves obtained on
VICTOR for pure single-step silica aerogel and single-step silica aerogel with 9%
(wt/wt) carbon black. At ambient pressure the addition of carbon lowers the
thermal conductivity from 0.017 to 0.0135 W/mK. The minimum value for the
carbon composite of ~0.0042 W/mK corresponds to ~R30/inch.
Silica Aerogel Nanocomposite Materials
It was readily apparent to early researchers working on aerogels that they were
ideal for use in composite materials. However, with much fundamental research
needed into the preparation and properties of aerogels, this area has only recently
been explored. In this discussion "composite" is used in the broadest sense of the
term, where the final product consists of a "substrate" (the silica aerogel) and one
or more additional phases (of any composition or scale). As all the materials
considered here have a silica aerogel substrate, there is always at least one phase
with physical structures with dimensions on the order of nanometers (the particles
and pores of the aerogel). The additional phases may also have nanoscale
dimensions, or may be larger (up to centimeters). Because of this the materials can
legitimately be classified as "nanocomposites". There are generally three routes to
aerogel nanocomposites: addition of the second component during the sol-gel
processing of the material (before supercritical drying), addition of the second
component through the vapor phase (after supercritical drying), and chemical
modification of the aerogel backbone through reactive gas treatment.
Aerogel nanocomposites through Sol-Gel processing
This approach is the logical first route to aerogel nanocomposites and can produce
many varieties of composites. There are, however, limitations to these procedures.
Simply stated, a non-silica material is added to the silica sol before gelation. This
added material may be a soluble organic or inorganic compound, insoluble
powders, polymers, biomaterials, bulk fibers, woven cloths, or porous preforms. In
all cases, the additional components must withstand the subsequent process steps
used to form the aerogel (alcohol soaking, and supercritical drying). The conditions
encountered in the CO2 drying process are milder than the alcohol drying process
and are more amenable to forming composites. If the added components are bulk,
insoluble materials (such as carbon fibers or mineral powders), steps must be
taken to prevent the settling of the insoluble phase before gelation.
This can often be accomplished by gently agitating the mixture until gelation is
imminent. The silica aerogel with the best results from the addition of a small
amount of carbon black to the sol using this technique.
The addition of soluble inorganic or organic compounds to the sol provides a
virtually unlimited number of possible composites.
There are two criteria that must be met to prepare a composite by this route. First,
the added component must not interfere with the gelation chemistry of the silica
precursor. This is difficult to predict in advance, but rarely a problem if the added
component is reasonably inert. The second problem encountered in this process is
the leaching out of the added phases during the alcohol soak or supercritical drying
steps. This can be a significant impediment if a high loading of the second phase is
desired in the final composite. When the addend component is a metal complex, it
is often useful to use a binding agent, such as
(CH3O)3SiCH2CH2NHCH2CH2NH2.
This can bind with the silica backbone through the hydrolysis of its methoxysilane
groups and chelate the metal complex with its dangling diamine. This general
approach has been used by several research groups to prepare nanocomposites
of silica aerogels or xerogels. After the gel has been dried, the resulting composite
consists of a silica aerogel with metal ions atomically dispersed throughout the
material. Thermal post-processing induces thermal diffusion and reduction of the
metal ions, forming nanometer-scale metal particles within the aerogel matrix.
These composites are being extensively studies for use a catalysts for gas-phase
reactions. There is a photograph of composites prepared in this way in
Aerogel nanocomposites through Chemical Vapor Infiltration
The open of silica aerogels allows for easy transport of vapors throughout the
entire volume of the material. This provides another route to an aerogel
nanocomposite. Virtually any compound with at least a slight vapor pressure can
be deposited throughout a silica aerogel. In fact, silica aerogels should be stored in
a clean environment to prevent the unwanted absorption of volatile pollutants. To
prevent subsequent desorption of the added phase, it is useful to convert the
adsorbed material into a non-volatile phase by thermal or chemical decomposition.
This can be done during, or after the initial deposition. The Microstructured
Materials Group has prepared a wide variety of aerogel nanocomposites using this
process, including:
Silica aerogel-Carbon composites
These have been prepared through the decomposition of various hydrocarbon
gases at high temperatures. However, due to the fine structure of silica aerogels,
the decomposition take place at a much lower temperature (200-450 degrees C)
than the corresponding decomposition in the absence of the aerogel. Carbon
loadings ranging from 1-800% have been observed. Surprisingly, at lower loadings,
the carbon deposition is relatively uniform throughout the volume of monolithic
aerogel slabs. At higher loadings, the carbon begins to localize at the exterior
surface of the composite monolith. Interesting aspects of these composites include
electrical conductivity at higher loadings, and mechanical strengthening of the
composite relative to the original aerogel.
Silica aerogel-Silicon composites
The thermal decomposition of various organosilanes on a silica aerogel forms
deposits of elemental silicon. In this case the rapid decomposition of the silane
precursor leads to deposits localized near the exterior surface of the aerogel
substrate. Thermal annealing of the composite induces crystallization of the silicon.
The resulting composite, with 20-30 nm diameter silicon particles, exhibits strong
visible photoluminescence at 600 nm.
Silica aerogel-Transition Metal composites
Organo-transition metal complexes are idea precursors for this type of composite.
Even the least volatile of these possess a sufficient vapor pressure to be deposited
within an aerogel. Under controlled conditions, these deposit uniformly throughout
the entire volume of the aerogel monolith. Typically, the metal compounds are then
thermally degraded to their base metals. These intermediate composites are
generally highly reactive, due to the disperse nature of the metallic phase, and can
be easily converted to metal oxides, sulfides, or halides. This process can be
repeated several times to increase the loading of the metallic phase. Typically
composites prepared in this way possess crystals of the desired metal compound
on the order of 5-100 nm in diameter.
The graphic below displays the magnetization/demagnetization curve for a silica
aerogel/Fe3O4 composite prepared by this process. The curve shows that the
composite is a "soft" ferromagnetic material. The magnetite crystals in this
composite are 20-60 nm in diameter. Many appear to be single domain, as
observed by electron microscopy.The Microstructured Materials
Group has a patent pending on various aspects of this process.
Aerogel nanocomposites through Energized Gas
Treatment
The Microstructured Materials Group has recently discovered a simple process that
can alter the chemical structure of the silica(or other oxide) backbone of an
aerogel. This process utilizes an energized reducing (or other) gas to form thin
films of new material on the interior surface of the aerogel. The techniques used in
this case are similar to standard plasma methods.
However, the nanoscale pore structure of silica aerogels prohibit the formation of a
plasma within an aerogel.Nevertheless, the centers of thick monoliths are affected
by this process. In the simplest case, silica aerogel monoliths are partially reduced
by energized hydrogen. The resulting composite consists of a silica aerogel with a
thin layer of oxygen-deficient silica (SiOx) on the interior surface. As with other
reduced silica materials, this material exhibits strong visible photoluminescence at
490-500 nm when excited by ultraviolet (330 nm) light. However, the process used
in this case is relatively gentle, and does not alter the physical shape or optical
transparency of the original aerogel. This composite is the basis for the aerogel.
There is a photograph of this composite.
The Microstructured Materials Group has a patent pending on this process ".
As noted above, several aerogel nanocomposites exhibit strong visible
photoluminescence. The spectra shown below are for the silicon
nanoparticles/silica aerogel (red emitter) and gas-treated reduced silica aerogel
composite (blue-green emitter)
Optical Oxygen Sensor Based on Silica Aerogel
Silica aerogels are ideal materials for active and passive components in optical
sensors. Their visible transparency, high surface area, facile transport of gases
through the material, thermal and chemical stability, and ability to be filled with
additional active phases are the key properties that aerogels bring to sensor
applications. The Microstructured Materials Group has recently discovered a new
process that induces a permanent, visible photoluminescence in silica aerogels
(see the section on aerogel composite materials). Shortly after these materials
were prepared, it was observed that the intensity of the photoluminescence was
indirectly proportional to the amount of gaseous oxygen within the aerogel. The
quenching of photoluminescence by oxygen is a phenomenon that is frequently
observed in many luminescent materials.
In simple terms, photoluminescence occurs when a material absorbs a photon of
sufficient energy. The entity that absorbs the photon may be a discrete molecule,
or a defect center in a solid-state material, and if often referred to a "carrier". When
the photon has been absorbed, the carrier is moved into a high energy, "excited"
state. The carrier will then relax back to its ground state after certain length of time.
This "lifetime" of the excited state is usually on the order of nanoseconds to
microseconds. The mechanism by which the carrier relaxes determines whether
the photoluminescence is termed "fluorescence" or "photoluminescence". If an
oxygen molecule collides with a carrier while it is in its excited state, the oxygen
molecule will absorb the excess energy of the carrier and quench the
photoluminescence. The oxygen molecule absorbs the energy and undergoes a
triplet-to-singlet transition, while the carrier undergoes a non-radiative relaxation.
The efficiency of the photoluminescence quenching is , therefore, determined by
the number of collisions between the material containing the carrier, and oxygen
molecules. As the collision frequency of gases is determined by the number of
molecules present, the pressure (P), and temperature (T), at a given P and T, the
quenching efficiency, and, consequently, the photoluminescence intensity will be
determined by the concentration of oxygen in the atmosphere surrounding the
material.
Oxygen sensors based on this principle have been extensively studied. The most
common sensor elements studied are those based on an organic or inorganic
compound suspended in a thin silicone membrane. Advantages of using an
aerogel-based sensor element over these systems include a more rapid response
time (due to rapid diffusion of gases through the aerogel pore network), and
improved resistance to photo-bleaching (as the photoluminescence is caused by
stable defect centers in SiO2).
The Microstructured Materials Group has built a prototype oxygen sensor based on
this technology. The sensor is intended to perform as low cost, moderate sensitivity
device operating most effectively in the concentration range of 0-30% oxygen. The
sensor operates independently of the nature of the other gases present in the feed
gas and of the feed gas flow rate. The prototype sensor has been sensor has been
successfully operated over a temperature range of -25 to +85 degrees C (this
range is based on other experimental limitations of the system, the actual usable
range is larger). The highest sensitivity is observed at lower temperatures.The
prototype sensor uses a Hg-arc lamp for excitation (330 nm), and a Si photodiode
for detection of the emission (500nm). The prototype design can be easily
miniaturized, and a device can be designed with built-in pressure and temperature
compensation.
This sensor is available for technology-transfer. The graphic below plots the
measured photoluminescence intensity (irradiance) vs oxygen pressure
(concentration gives a similar plot) at two temperatures using the prototype sensor.
Silica Aerogels: Technology-Transfer Opportunities/Commercial
AvailabilityTechnology Transfer
As an institution funded by the U. S. Government, Berkeley Lab actively seeks
technology-transfer arrangements that will be mutually beneficial to Berkeley Lab
and commercial entities. The following technologies developed by the
Microstructured Materials Group are available for direct transfer:
• Methods of producing aerogel-based via chemical vapor infiltration methods.
• Methods of producing and other aerogels with altered chemical compositions.
• based on photoluminescent silica aerogel.
For details on how to begin a partnership with Berkeley Lab, visit the
http://www.lbl.gov/Tech-Transfer
Commercial Availability
In 1994, the Microstructured Materials Group entered into a Cooperative Research
And Development Agreement with http://www.aerojet.com/ .of Sacramento,
California, USA and several other partners. This agreement was supported by an
ARPA-TRP grant and focused on development of a pilot-scale aerogel production
plant. At the completion of the project in 1995, Aerojet idled this facility and has no
current plans to continue in this area.
Other potential U.S. sources of aerogels are http://www.nanopore.com , in
Albuquerque, N.M. which focuses on lower-cost granular aerogels and
http://www.aspensystems.com/ , in Marlboro, MA which produces flexible aerogel-
based insulation for cryogenic systems.
A new venture, Ocellus, in the San Fransisco area, is currently selling small
quantities of R-F, carbon and silica aerogels. They are available through
http://www.mkt-intl.com/aerogels/index.html In Europe, http://www.airglass.se/ in
Lund, Sweden has made batch quantities of aerogels for many years, focusing on
serving the needs of the high energy physics community.
"http://www.cabot-corp.com/cabot will soon introduce commercial-scale quantities
of granular, ambient-pressure dried aerogel products.
The http://www.taasi.com/ company in Ohio is developing various oxide materials
for uses such as air purification and catalysis.
Note: The Microstructured Materials Group has a limited, and ever decreasing,
stock of silica aerogel monoliths of various sizes.
In the past we have provided demonstration samples to interested parties.
Regrettably, we can no longer continue this practice.
We may provide samples to organizations interested in collaborative research with
Berkeley Lab, or to assist in development of applications of aerogels with realistic
commercial potential. We are sorry that we will not be able to help artists,
designers, high schools, etc. unless there are extraordinary circumstances. To
contact Microstructured Materials Group members go to the
A Partial Bibliography for Silica Aerogels
Note: There are well over one thousand scholarly papers dealing with aerogels.
The partial list below gives representative examples and an indication of the
breadth of this field.
• THE INTERNATIONAL SYMPOSIA ON AEROGELS (ISA)
• 1st ISA: Wurzburg, Germany September 23-25 1985 Proceedings: "Aerogels"
Ed. J. Fricke Springer Proceedings in Physics 6, Springer-Verlag (Berlin) 1986
• 2nd ISA: Montpellier, France September 21-23, 1988
Proceedings: Colloque de Physique (Supplement au Journal de Physique, FASC.
4), C4-1989
• 3rd ISA: Wurzburg, Germany September 30 - October 2, 1991
Proceedings: http://www.elsevier.com/locate/jnoncrysol vol. 145, 1992
• 4th ISA: Berkeley, California, USA. September 19-21, 1994
Proceedings: http://www.elsevier.com/locate/jnoncrysol vol. 185-6, 1995
• 5th ISA: Montpellier, France September 8-10, 1997
Proceedings:http://www.elsevier.com/locate/jnoncrysol vol. 225, 1998
• 6th ISA: Albuquerque, N.M., USA October 8-11, 2000
Proceedings:http://www.elsevier.com/locate/jnoncrysol vol. 285, 2001
•
• PAPERS BY MICROSTRUCTURED MATERIALS GROUP MEMBERS
• Ayers, M.R. and Hunt. A.J.
2001 Observation of the Aggregation Behavior of Silica Sols Using Laser Speckle
Contrast Measurements.Journal of Non-Crystalline Solids, 290:122-128
• Ayers, M.R. and Hunt. A.J.
2001 Synthesis and Properties of Chitosan-Silica Hybrid Aerogels. Journal of Non-
Crystalline Solids, 285:123-127
• Hunt. A.J., and Ayers, M.R.
2001 Investigations of Silica Alcogel Using Coherent Light. Journal of Non-
Crystalline Solids, 285:162-166.
• Hunt. A.J.
1998 Light Scattering for Aerogel Characterization Journal of Non-Crystalline
Solids, 225:303-306
• Ayers, M.R. and Hunt. A.J.
1998 Molecular Oxygen Sensor Based on Photoluminescent Silica Aerogel.
Journal of Non-Crystalline Solids,
225:343-347
• Ayers, M.R. and Hunt. A.J.
1998 Light Scattering Studies of UV-Catalyzed Gel and Aerogel Structure, Journal
of Non-crystalline Solids , 225:325-329
• Ayers, M. R. and Hunt A.J.
1998 Titanium Oxide Aerogels Prepared from Titanium Metal and Hydrogen
Peroxide. Materials Letters, 34:290-293
• Ayers, M. R. and Hunt A.J.
1998 Visibly Photoluminescent Silica Aerogels. Journal of Non-Crystalline Solids,
217:229-235
• Ayers, M. R. Song, X. Y., and Hunt A. J.
1996 Preparation of Nanocomposite Materials Containing WS2, d-WN, Fe3O4, or
Fe9S10 in a Silica Aerogel Host. Journal of Materials Science 31:6251-6257.
• Zeng, S. Q., A. Hunt, and R. Greif
1995 Theoretical Modeling of Carbon Content to Minimize Heat Transfer In Silica
Aerogel. Journal of Non-Crystalline Solids, 186: 271-277.
• Song, X. Y., W. Q. Cao, M. R. Ayers, and A. J. Hunt
1995 Carbon Nanostructures In Silica Aerogel Composites. Journal of Materials
Research 10: 251-254.
• Zeng, S. Q., A. Hunt, and R. Greif
1995 Transport Properties of Gas In Silica Aerogel. Journal of Non-Crystalline
Solids 186: 264-270.
• Hunt, A. J., M. R. Ayers, and W. Q. Cao
1995 Aerogel Composites Using Chemical Vapor Infiltration. Journal of Non-
Crystalline Solids 185: 227-232.
• Lee, D., P. C. Stevens, S. Q. Zeng, and A. J. Hunt
1995 Thermal Characterization of Carbon-Opacified Silica Aerogels. Journal of
Non-Crystalline Solids 186: 285-290.
• Cao, W. Q., and A. J. Hunt
1994 Photoluminescence of Chemically Vapor Deposited Si On Silica Aerogels.
Applied Physics Letters 64: 2376-2378.
• Song, X. Y., W. Cao, and A. J. Hunt
1994 AEM and HREM evaluation of carbon nanostructures in silica aerogels,
Spring meeting of the Materials Research Society; pp. (6 p). San Francisco, CA
(United States): Lawrence Berkeley Lab., California (United States)
• Cao, W. Q., and A. J. Hunt
1994 Improving the Visible Transparency of Silica Aerogels. Journal of Non-
Crystalline Solids 176: 18-25.
• Cao, W. Q., and A. J. Hunt
1994 Thermal Annealing of Photoluminescent Si Deposited On Silica Aerogels.
Solid State Communications 91: 645-648.
• Zeng, S. Q., A. J. Hunt, W. Cao, and R. Greif
1994 Pore size distribution and apparent gas thermal conductivity of silica aerogel.
Journal of Heat Transfer 116: 756-759.
• Hunt, A. J., C. A. Jantzen, W. Cao, R. S. Graves, and D. C. Wysocki
1991 Aerogel. Gatlinburg, TN (United States): Philadelphia, PA (United States)
ASTM (Symposium on insulation materials: testing and applications,
• Hunt, A., K. Lofftus, W. H. Bloss, and F. Pfisterer
1988 Silica aerogel, a transparent high performance insulator. Hamburg, F.R.
Germany: Pergamon Press,Oxford, GB (International Solar Energy Society
biennial congress on advances in solar energy technology,
• Tewari, P. H., A. J. Hunt, K. D. Lofftus, J. G. Lieber, C. J. Brinker, D. E.
Clark, and D. R. Ulrich
1986 Microstructural studies of transparent silica gels and aerogels. Palo Alto, CA,
USA: Materials Research Society,Pittsburgh, PA (Materials Research Society
spring meeting
• Tewari, P. H., K. D. Lofftus, and A. J. Hunt
1985 Structure and chemistry of sol-gel derived transparent silica aerogel, 2.
international conference on ultrastructure processing of ceramics, glasses and
composites; pp. 17. Daytona Beach, Florida, USA: Lawrence Berkeley Lab.,
California (USA)
• Hunt, A. J., R. E. Russo, P. H. Tewari, and K. D. Lofftus
1985 Aerogel: a transparent insulator for solar applications, INTERSOL '85 - Solar
energy--the diverse solution; pp. 8. Montreal, Canada: Lawrence Berkeley Lab.,
California (USA)
• Hunt, A., P. Berdahl, K. Lofftus, R. Russo, and P. Tewari
1985 Advances in transparent insulating aerogels for windows, Solar buildings:
realities for today - trends for tomorrow; pp. 138-141. Washington, DC, USA:
Lawrence Berkeley Lab., California, MCC Associates, Inc., Silver Spring, MD
(USA)
• Hunt, A., R. Russo, P. Tewari, K. Lofftus, E. Bilgen, and K. G. T. Hollands
1985 Aerogel: A transparent insulator for solar applications. Montreal, Canada:
Pergamon Books Inc.,Elmsford,NY (INTERSOL '85 - Solar energy--the diverse
solution,
• Selkowitz, S. E., A. Hunt, C. M. Lampert, and M. D. Rubin
1984 Advanced optical and thermal technologies for aperture control, Passive and
hybrid solar energy update;pp. 10-19. Washington, DC, USA: Lawrence Berkeley
Lab., Californialifornia, U.S. Department of Energy Assistant Secretary for
Conservation and Renewable Energy, Washington, DC. Passive and Hybrid Solar
Energy Division
• Hunt, A. J., and P. Berdahl
1984 Structure data form light scattering studies of aerogel. Mater. Res. Soc.
Symp. Proc. : 275-280.
• Hunt, A., P. Berdahl, K. Lofftus, R. Russo, and P. Terwari
1984 Advances in transparent insulating aerogels for windows,Passive and hybrid
solar energy update; pp.47-50. Washington, DC, USA: Lawrence Berkeley Lab.,
Californialifornia, U.S. Department of Energy Assistant Secretary for Conservation
and Renewable Energy, Washington, DC. Passive and Hybrid Solar Energy
Division
• Hunt, A. J.
1983 Light-scattering studies of silica aerogels, International conference on
ultrastructure processing of ceramics, glasses and composites; pp. 15. Gainesville,
FL, USA: Lawrence Berkeley Lab., California (USA)

THERMAL PROPERTIES
• Rettelbach, R., J. Sauberlich, S. Korder, and J. Fricke
1995 Thermal Conductivity of Ir-Opacified Silica Aerogel Powders Between 10 K
and 275 K. Journal of Physics
D-Applied Physics 28: 581-587.
• Rettelbach, T., J. Sauberlich, S. Korder, and J. Fricke
1995 Thermal Conductivity of Silica Aerogel Powders At Temperatures From 10 to
275 K. Journal of
Non-Crystalline Solids 186: 278-284.
• Hrubesh, L. W., and J. F. Poco
1995 Thin Aerogel Films For Optical, Thermal, Acoustic and Electronic
Applications. Journal of Non-Crystalline Solids 188: 46-53.
• Hrubesh, L. W., and R. W. Pekala
1994 Thermal properties of organic and inorganic aerogels. Journal of Materials
Research 9: 731-738.
• Zeng, S. Q., A. J. Hunt, W. Cao, and R. Greif
1994 Pore size distribution and apparent gas thermal conductivity of silica aerogel.
Journal of Heat Transfer 116: 756-759.
• Reiss, H.
1992 Heat transfer in thermal insulations. Physikalische Blaetter 48: 617-622.
• Bernasconi, A., T. Sleator, D. Posselt, J. K. Kjems, and H. R. Ott
1992 Low-Temperature Specific Heat and Thermal Conductivity of Silica Aerogels.
Journal of Non-Crystalline Solids 145: 202-206.
• Scheuerpflug, P., M. Hauck, and J. Fricke
1992 Thermal Properties of Silica Aerogels Between 1.4-K and 330-K. Journal of
Non-Crystalline Solids 145: 196-201.
• Bernasconi, A., T. Sleator, D. Posselt, J. K. Kjems, and H. R. Ott
1992 Dynamic Properties of Silica Aerogels As Deduced From Specific-Heat and
Thermal-Conductivity
Measurements. Physical Review B-Condensed Matter 45: 10363-10376.
• Posselt, D., J. K. Kjems, A. Bernasconi, T. Sleator, and H. R. Ott
1991 The Thermal Conductivity of Silica Aerogel In the Phonon, the Fracton and
the Particle-Mode Regime. Europhysics Letters 16: 59-65.
• Scheuerpflug, P., H. J. Morper, G. Neubert, and J. Fricke
1991 Low-Temperature Thermal Transport In Silica Aerogels. Journal of Physics
D-Applied Physics 24: 1395-1403.
• Xianping, Lu, Wang Peng, D. Buettner, U. Heinemann, O. Nilsson, J. Kuhn,
and J. Fricke
• 1991 Thermal transport in opacified monolithic silica aerogels. High
Temperatures High Pressures 23: 431-436.
• Sleator, T., A. Bernasconi, D. Posselt, J. K. Kjems, and H. R. Ott
1991 Low-Temperature Specific Heat and Thermal Conductivity of Silica Aerogels.
Physical Review Letters 66: 1070-1073.
• Caps, R., G. Doll, J. Fricke, U. Heinemann, and J. Hetfleisch
1989 Thermal Transport In Monolithic Silica Aerogel. Journal De Physique 50:
C4113-C4118.
• Fricke, J.
1989 Thermal insulation without CFC. Physik in Unserer Zeit 20: 189-191.
• Fricke, J., E. Hummer, H. J. Morper, and P. Scheuerpflug
1989 Thermal Properties of Silica Aerogels. Journal De Physique 50: C487-C497.
• Buettner, D., R. Caps, U. Heinemann, E. Huemmer, A. Kadur, and J. Fricke
1988 Thermal loss coefficients of low-density silica aerogel tiles. Sol. Energy 40:
13-15.
• Fricke, J., R. Caps, D. Buettner, U. Heinemann, E. Huemmer, and A. Kadur
1987 Thermal loss coefficients of monolithic and granular aerogel systems. Sol.
Energy Mater. 16: 267-274.
OPTICAL PHENOMENA
• Hrubesh, L. W., and J. F. Poco
1995 Thin Aerogel Films For Optical, Thermal, Acoustic and Electronic
Applications. Journal of Non-Crystalline Solids 188: 46-53.
• Zhu, L., Y. F. Li, J. Wang, and J. Shen
1995 Structural and Optical Characteristics of Fullerenes Incorporated Inside
Porous Silica Aerogel. Chemical Physics Letters 239: 393-398.
• Emmerling, A., R. Petricevic, A. Beck, P. Wang, H. Scheller, and J. Fricke
1995 Relationship Between Optical Transparency and Nanostructural Features of
Silica Aerogels. Journal of
Non-Crystalline Solids 185: 240-248.
• Beck, A., W. Koerner, and J. Fricke
1994 Optical investigations of granular aerogel fills. Journal of Physics. D, Applied
Physics 27: 13-18.
• Hotaling, S. P.
1993 Ultra-Low Density Aerogel Optical Applications. Journal of Materials
Research 8: 352-355.
• Emmerling, A., P. Wang, G. Popp, A. Beck, and J. Fricke
1993 Nanostructure and Optical Transparency of Silica Aerogels. Journal De
Physique Iv 3: 357-360.
• Platzer, W. J., and M. Bergkvist
1993 Bulk and surface light scattering from transparent silica aerogel. Solar
Energy Materials and Solar Cells 31: 243-251.
• Wang, P., W. Korner, A. Emmerling, A. Beck, J. Kuhn, and J. Fricke
1992 Optical Investigations of Silica Aerogels. Journal of Non-Crystalline Solids
145: 141-145.
• Beck, A., O. Gelsen, P. Wang, and J. Fricke
1989 Light Scattering For Structural Investigations of Silica Aerogels and Alcogels.
Journal De Physique 50: C4203-C4208.
• Lampert, C. M.
1987 Advanced optical materials for energy efficiency and solar conversion. Sol.
Wind Technol. 4: 347-379.
• Hunt, A. J., and P. Berdahl
1984 Structure data form light scattering studies of aerogel. Mater. Res. Soc.
Symp. Proc. : 275-280.
• Lampert, C. N.
1983 Solar optical materials for innovative window design. Int. J. Energy Res. 7:
359-374.

MECHANICAL PROPERTIES
• Hunt. A.J., and Ayers, M.R.
2001 Investigations of Silica Alcogel Using Coherent Light. Journal of Non-
Crystalline Solids, 285:162-166.
• Woignier, T., J. Phalippou, H. Hdach, G. Larnac, F. Pernot, and G. W.
Scherer
1992 Evolution of Mechanical Properties During the Alcogel Aerogel Glass
Process. Journal of Non-Crystalline Solids 147: 672-680.
• Armand, A. C., and D. Guyomar
1992 Acoustic and Mechanical Characterization of Silica Aerogels. Journal De
Physique Iii 2: 759-762.
• Hdach, H., T. Woignier, J. Phalippou, and G. W. Scherer
1990 Effect of Aging and pH On the Modulus of Aerogels. Journal of Non-
Crystalline Solids 121: 202-205.
• Woignier, T., and J. Phalippou
1989 Scaling Law Variation of the Mechanical Properties of Silica Aerogels.
Journal De Physique 50:
C4179-C4184.
• Phalippou, J., T. Woignier, and R. Rogier
1989 Fracture Toughness of Silica Aerogels. Journal De Physique 50: C4191-
C4196.
• Cross, J., R. Goswin, R. Gerlach, and J. Fricke
1989 Mechanical Properties of SiO2 - Aerogels. Journal De Physique 50: C4185-
C4190.

CHERENKOV RADIATION COUNTER APPLICATIONS

• Adachi, I., T. Sumiyoshi, K. Hayashi, N. Iida, R. Enomoto, K. Tsukada, R.
Suda, S. Matsumoto, K. Natori, M. Yokoyama, and H. Yokogawa
1995 Study of a threshold Cherenkov counter based on silica aerogels with low
refractive indices. Nuclear Instruments and Methods in Physics Research, Section
A 355: 390-398.
• Ganezer, K. S., W. E. Keig, and A. F. Shor
1994 A simple high efficiency Cherenkov counter. IEEE Transactions on Nuclear
Science 41: 336-342.
• Hasegawa, T., O. Hashimoto, T. Nagae, and M. Sekimoto
1994 A large silica aerogel Cherenkov counter for SKS. Nuclear Instruments and
Methods in Physics Research, Section A 342: 383-388.
• Brajnik, D., S. Korpar, G. Medin, M. Staric, and A. Stanovnik
1994 Measurement of Sr-90 Activity With Cherenkov Radiation In a Silica Aerogel.
Nuclear Instruments &
Methods In Physics Research Section a-Accelerators Spectrometers Detectors
and Associated Equipment
353: 217-221.
• Fields, D. E., H. Vanhecke, J. Boissevain, B. V. Jacak, W. E. Sondheim, J. P.
Sullivan, W. J. Willis, K.
Wolf, E. Noteboom, P. M. Peters, and R. Burke
• 1994 Use of Aerogel For Imaging Cherenkov Counters. Nuclear Instruments &
Methods In Physics Research Section a-Accelerators Spectrometers Detectors
and Associated Equipment 349: 431-437.
• Adachi, Ichiro
1994 R and D on Cherenkov counter based on silica aerogel with low refractive
index. Hoshasen 20: 21-30.
• Lippert, C., R. Siebert, J. P. Didelez, J. Ernst, R. Frascaria, J. Y. Martel, and
R. Skowron
1993 Particle discrimination in medium energy physics with an aerogel Cherenkov
detector. Nuclear Instruments and Methods in Physics Research, Section A 333:
413-421.
• Onuchin, A., A. Shamov, Yu Skovpen, A. Vorobiov, A. Danilyuk, T.
Gorodetskaya, and V. Kuznetsov
1992 The aerogel Cherenkov counters with wavelength shifters and phototubes.
Nuclear Instruments and Methods in Physics Research, Section A 315: 517-520.
• Miskowiec, D., W. Ahner, E. Grosse, P. Senger, and W. Walus
1990 Aerogel Cherenkov detectors for the Kaon spectrometer. Verhandlungen der
Deutschen Physikalischen Gesellschaft 25: 1520.
• Vincent, P., R. Debbe, A. Pfoh, and M. Abreu
1988 E802 aerogel Cherenkov detector. Nucl. Instrum. Methods Phys. Res. 272:
660-668.
• Carlson, P.
1986 Aerogel Cherenkov counters: Construction principles and applications. Nucl.
Instrum. Methods Phys. Res. 248: 110-117.
• Poelz, G.
1986 Aerogel Cherenkov counters at DESY. Nucl. Instrum. Methods Phys. Res.,
Sect. A. 248: 118-129.
• Kawai, H., J. Haba, T. Homma, M. Kobayashi, K. Miyake, T. S. Nakamura, N.
Sasao, Y. Sugimoto, M. Yoshioka, and M. Daigo
1985 Tests of a silica aerogel Cherenkov counter. Nucl. Instrum. Methods Phys.
Res., Sect. A 228: 314-322.
• Maurer, K., G. Koebschall, K. Roehrich, C. Schmitt, and V. H. Walther
1984 Silica aerogel threshold Cherenkov counters for use at intermediate energies.
Nucl. Instrum. Methods
Phys. Res., Sect. A 224: 110-111.
• Fernandez, C., K. E. Johansson, M. Schouten, S. Tavernier, P. Ladron de
Guevara, P. Herquet, J.Kesteman, and O. Pingot
1984 Performance of the silica aerogel Cherenkov detector used in the European
Hybrid Spectrometer. Nucl. Instrum. Methods Phys. Res., Sect. A 225: 313-318.
• Yasumi, Shinjiro, and Hideyuki Kawai
1983 Silica aerogel Cherenkov counter. Nippon Butsuri Gakkaishi 38: 671-676.
• Poelz, G., and R. Riethmueller
1982 Preparation of silica aerogel for Cherenkov counters. Nucl. Instrum. Methods
Phys. Res. 195: 491-503.
• Carlson, P. J., K. E. Johansson, J. Norrby, J. Kesteman, O. Pingot, S.
Tavernier, and L. van Lancker
1982 Tests of an 18 module silica aerogel Cherenkov detector to be used in the
European hybrid spectrometer. Nucl. Instrum. Methods Phys. Res. 192: 209-216.
• Burkhardt, H., P. Koehler, R. Riethmueller, B. H. Wiik, R. Fohrmann, J.
Franzke, H. Krasemann, R. Maschuw, G. Poelz, and J. Reichardt
1981 TASSO gas and aerogel Cherenkov counters. Nucl. Instrum. Methods 184:
319-331.
• Trachsel, C., D. Perrin, and R. Schwarz
1981 Study of an aerogel Cherenkov detector with indirect light collection. Helv.
Phys. Acta 53: 655-661.
• de Brion, J. P., A. Caillet, J. B. Cheze, J. Derre, G. Marel, E. Pauli, and C.
Pigot
1981 Silica aerogel Cherenkov counter in a missing-mass experiment K/sup -/d ..--
>.. K/sup +/ + X at 1.4 GeV/c. Nucl. Instrum. Methods 179: 61-65.
• Carlson, P. J., K. E. Johansson, J. Kesteman, O. Pingot, J. Norrby, S.
Tavernier, F. van den Bogaert, and
L. van Lancker
1979 Increased photoelectron collection efficiency of a photomultiplier in an
aerogel Cherenkov counter. Nucl. Instrum. Methods 160: 407-410.
• Bourdinaud, M., J. B. Cheze, and J. C. Thevenin
1976 Use of silica aerogel for Cherenkov radiation counter. Nucl. Instrum. Methods
136: 99-103.

MISCELLANEOUS
• Coddens, G., J. Dekinder, and R. Millet
1995 Time-of-Flight Inelastic Neutron Scattering Study of Liquid He-4 In Silica
Aerogels. Journal of Non-Crystalline Solids 188: 41-45.
• Ehrburgerdolle, F., J. Dallamano, E. Elaloui, and G. M. Pajonk
1995 Relations Between the Texture of Silica Aerogels and Their Preparation.
Journal of Non-Crystalline Solids 186: 9-17.
• Hua, D. W., J. Anderson, J. Digregorio, D. M. Smith, and G. Beaucage
1995 Structural Analysis of Silica Aerogels. Journal of Non-Crystalline Solids 186:
142-148.
• Jarzebski, A. B., and J. Lorenc
1995 Pore Network Connectivity and Effective Diffusivity of Silica Aerogels.
Chemical Engineering Science 50:
357-360.
• Rogacki, G., and P. Wawrzyniak
1995 Diffusion of Ethanol-Liquid CO2 In Silica Aerogel. Journal of Non-Crystalline
Solids 186: 73-77.
• Tsou, P.
1995 Silica Aerogel Captures Cosmic Dust Intact. Journal of Non-Crystalline Solids
186: 415-427.
• Yokogawa, H., and M. Yokoyama
1995 Hydrophobic Silica Aerogels. Journal of Non-Crystalline Solids 186: 23-29.
• Zhu, L., Y. F. Li, J. Wang, and J. Shen
1995 Intense Visible Light Emission From Fullerene-Doped Silica Aerogel. Journal
of Applied Physics 77: 2801-2803.
• Zhu, L., Y. F. Li, J. Wang, and J. Shen
1995 Structural and Optical Characteristics of Fullerenes Incorporated Inside
Porous Silica Aerogel. Chemical Physics Letters 239: 393-398.
• Schaefer, D. W., B. J. Olivier, C. Ashley, G. Beaucage, D. Richter, B. Farago,
B. Frick, and D. A. Fischer
1994 Structure and Topology of Silica Aerogels During Densification. Journal of
Non-Crystalline Solids 172: 647-655.
• Bruesch, P., F. Stucki, T. Baumann, P. Klugeweiss, B. Bruhl, L. Niemeyer,
R. Strumpler, B. Ziegler, and M. Mielke
1993 Electrical and Infrared Dielectrical Properties of Silica Aerogels and of Silica
Aerogel-Based Composites. Applied Physics a-Solids and Surfaces 57: 329-337.
• Gross, J., T. Schlief, and J. Fricke
1993 Ultrasonic Evaluation of Elastic Properties of Silica Aerogels. Materials
Science and Engineering a-Structural Materials Properties Microstructure and
Processing 168: 235-238.
• Igarashi, K., K. Tajiri, Y. Tai, and S. Tanemura
1993 Structural Study By Dsc, Saxs, and Raman Spectroscopy of Silica Aerogel.
Zeitschrift Fur Physik D-Atoms Molecules and Clusters 26: S207-S209.
• Kralj, S., G. Lahajnar, A. Zidansek, N. Vrbancickopac, M. Vilfan, R. Blinc,
and M. Kosec
1993 Deuterium Nmr of a Pentylcyanobiphenyl Liquid Crystal Confined In a Silica
Aerogel Matrix. Physical Review E 48: 340-349.
• Pauthe, M., F. Despetis, and J. Phalippou
1993 Hydrophobic Silica CO2 Aerogels. Journal of Non-Crystalline Solids 155:
110-114.
• Buckley, A. M., and M. Greenblatt
1992 The Preparation and Characterisation of Silica Aerogels and Xerogels Doped
With Transition Metal Species. Journal of Non-Crystalline Solids 146: 97-110.
• Buckley, A. M., and M. Greenblatt
1992 A Comparison of the Microstructural Properties of Silica Aerogels and
Xerogels. Journal of Non-Crystalline Solids 143: 1-13.
• Courtens, E., and R. Vacher
1992 Structure and Dynamics of Silica Aerogels. Philosophical Magazine B-
Physics of Condensed Matter Structural Electronic Optical and Magnetic
Properties 65: 347-355.
• Damrau, U., H. C. Marsmann, O. Spormann, and P. Wang
1992 Si-29 Mas-Nmr Investigations of Silica Aerogels. Journal of Non-Crystalline
Solids 145: 164-167.
• Dasilva, A., P. Donoso, and M. A. Aegerter
1992 Properties of Water Adsorbed In Porous Silica Aerogels. Journal of Non-
Crystalline Solids 145: 168-174.
• Duval, E., A. Boukenter, T. Achibat, B. Champagnon, J. Serughetti, and J.
Dumas
1992 Structure of Silica Aerogels and Vibrational Dynamics In Fractal Materials
and Glasses – Electron Microscopy and Low-Frequency Raman Scattering.
Philosophical Magazine B-Physics of Condensed Matter Structural Electronic
Optical and Magnetic Properties 65: 181-189.
• Ehrburgerdolle, F., M. Holz, C. Mauzac, J. Lahaye, and G. M. Pajonk
1992 Characterization of the Porous Texture of Aerogel, Precipitated and
Pyrogenic Silicas. Journal of Non-Crystalline Solids 145: 185-190.
• Foret, M., A. Chougrani, R. Vacher, and J. Pelous
1992 From Colloidal-Silica Sols to Aerogels and Xerogels. Journal De Physique Iv
2: 135-139.
• Gross, J., and J. Fricke
1992 Ultrasonic Velocity Measurements In Silica, Carbon and Organic Aerogels.
Journal of Non-Crystalline Solids 145: 217-222.
• Posselt, D., J. S. Pedersen, and K. Mortensen
1992 A Sans Investigation On Absolute Scale of a Homologous Series of Base-
Catalysed Silica Aerogels. Journal of Non-Crystalline Solids 145: 128-132.
• Schaefer, D. W., B. J. Olivier, C. S. Ashley, D. Richter, B. Farago, B. Frick, L.
Hrubesh, M. J. Vanbommel, G. Long, and S. Krueger
1992 Structure and Topology of Silica Aerogels. Journal of Non-Crystalline Solids
145: 105-112.
• Emmerling, A., R. Gerlach, R. Goswin, J. Gross, G. Reichenauer, J. Fricke,
and H. G. Haubold
1991 Structural Modifications of Highly Porous Silica Aerogels Upon Densification.
Journal of Applied Crystallography 24: 781-787.
• Crowell, P. A., G. K. S. Wong, and J. D. Reppy
1990 Measurement of the Superfluid Density In Silica Aerogels. Physica B 165:
549-550.
• Devreux, F., J. P. Boilot, F. Chaput, and B. Sapoval
1990 Nmr Determination of the Fractal Dimension In Silica Aerogels. Physical
Review Letters 65: 614-617.
• Jang, K. Y., and K. Kim
1990 Study of sol--gel processing for fabrication of hollow silica--aerogel spheres.
Journal of Vacuum Science and Technology, A 8: 1732-1735.
• Jang, K. Y., K. Kim, and R. S. Upadhye
1990 Study of Sol-Gel Processing For Fabrication of Hollow Silica-Aerogel
Spheres. Journal of Vacuum Science & Technology a-Vacuum Surfaces and Films
8: 1732-1735.
• Phalippou, J., T. Woignier, and M. Prassas
1990 Glasses From Aerogels .1. the Synthesis of Monolithic Silica Aerogels.
Journal of Materials Science 25: 3111-3117.
• Schaefer, D. W., C. J. Brinker, D. Richter, B. Farago, and B. Frick
1990 Dynamics of Weakly Connected Solids - Silica Aerogels. Physical Review
Letters 64: 2316-2319.
• Woignier, T., J. Phalippou, R. Vacher, J. Pelous, and E. Courtens
1990 Different Kinds of Fractal Structures In Silica Aerogels. Journal of Non-
Crystalline Solids 121: 198-201.
• Boukenter, A., D. Champagnon, J. Dumas, E. Duval, J. F. Quinson, J. L.
Rousset, J. Serughetti, S. Etienne, and C. Mai
1989 A Saxs Study of Silica Aerogels. Journal De Physique 50: C4133-C4136.
• Kim, N. K., K. Kim, D. A. Payne, and R. S. Upadhye
1989 Fabrication of hollow silica aerogel spheres by a droplet generation method
and sol--gel processing. J. Vac. Sci. Technol., A 7: 1181-1184.
• Maynard, R., R. Calemczuk, A. M. Degoer, B. Salce, J. Bon, E. Bonjour, and
A. Bourret
1989 Low Energy Excitations In Silica Aerogels. Journal De Physique 50: C4107-
C4112.
• Schaefer, D. W.
1989 What Factors Control the Structure of Silica Aerogels. Journal De Physique
50: C4121-C4126.
• Mukherjee, S. P., J. F. Cordaro, and J. C. Debsikdar
1988 Pore structures and microstructures of silica gel monoliths at different stages
of sintering. Advanced Ceramic Materials 3: 463-467.
• Fearon, E. M., P. R. Coronado, R. G. Garza, D. H. Darling, and P. C. Souers
1987 Shrinkage and opacity of 100 kg/m3 silica aerogel foam in liquid deuterium-
tritium. J. Nucl. Mater. 149: 105-108.

ZERO-GRAVITY AEROGEL FORMATION:

The Effects of Reduced Gravity on the Clarity and Pore Structure of Aerogels
Produced by a Rapid Gelation Two-Step Catalysis
Test Equipment Data Package
Stephen Steiner
Principal Investigator
Zero-G Aerogel Team
Project ID: 2002-073
University of Wisconsin–Madison
Chemistry Department
1101 University Ave.
Madison, WI 53706-1396
March 6, 2002
Quick Reference Sheet
Principle Investigator: Stephen Steiner
Contact Information:
Mailing Address 1001 W. Brentwood Lane Glendale, WI 53217
Phone (414) 732-5261 (Mobile)
Email mailto:ssteiner@zerogaerogel.com
Experiment Title: Zero-Gravity Aerogel Formation: The Effects of Reduced
Gravity on the Clarity and Pore Structures of Aerogels Produced Through a Rapid
Gelation Two- Step Catalysis
Flight Dates: Tuesday, April 23rd and Wednesday, April 24th 2002
Overall Assembly Weight: 190 lbs.
Assembly Dimensions (L x W x H): 22" x 21" x 51"
Proposed Floor Mounting Strategy: Straps
Gas Cylinder Requests: None
Overboard Vent Requests: No
Power Requirements: 115 VAC, 9.4 Amps max
Flyer Names for Each Proposed Flight Day: Tuesday Wednesday
Stephen Steiner David Meister
Lucas Heinkel Nicholas Kho
Table of Contents
Quick Reference Sheet 1
4. Flight Manifest 4
5. Experiment Background 5
5.1 Introduction 5
5.2 Preparation of Alcogels 6
5.3 Supercritical Extraction Process 7
5.4 Rayleigh Scattering in Silica Aerogels 8
5.5 Effects of Gravity on the Formation of Aerogel 8
5.6 Other Reduced Gravity Experiments 9
5.7 Uses of Aerogel 10
5.8 Experimental Objectives 10
5.9 Description of Follow-up Flight 11
6. Experiment Description 12
6.1 Expectations of Experiment 12
6.2 Expectations of Corresponding Ground Experiments 13
7. Equipment Description 14
7.1 Introduction 14
7.2 Containment Unit 14
7.3 Glassware 16
7.4 Glassware Controls and Sensors 16
7.5 Computer Controls 19
7.6 Molds 20
7.7 Liquid Containment and Delivery 20
8. Structural Analysis 22
8.1 Overview 22
8.2 Centers of Gravity 22
8.3 Summary 28
8.4 Structural Integrity 28
9. Electrical Analysis 30
9.1 Electrical Schematic 30
9.2 Load Analysis 31
9.3 Emergency Shutdown Procedures 31
10. Pressure Vessel Certification 32
10.1 Schematic 33
10.2 MAWP Table 34
11. Laser Certification 35
12. Parabola Details and Crew Assistance 36
13. Free Float Requirements 37
14. Institutional Review Board 38
15. Hazard Analysis Report 39
16. Tool Requirements 52
17. Photo Requirements 53
18. Aircraft Loading 54
19. Ground Support Requirements 55
20. Hazardous Materials 56
21. Material Safety Data Sheets 57
22. Procedures 80
22.1 Shipping Equipment to Ellington Field 80
22.2 Ground Operations 80
22.3 Loading 80
22.4 Pre-Flight 80
22.5 In-Flight 80
22.6 Post-Flight 81
23. Bibliography 82
Figure 5-1: Silica Aerogel on a Hand 5
Figure 5-2: Silica Aerogel on a Penny 5
Figure 5-3: Steel Supercritical Drying Vessel 7
Figure 7-1: Containment Unit Inner and Outer Boxes 15
Figure 7-2: Glassware and Pipetting Apparatus 15
Figure 7-3: Syringe-Molds 17
Figure 7-4: Laser Diode Photocell Assembly Across Zypette 18
Figure 7-5: Motor and Gear Assembly for Moving Microstopcock 18
Figure 7-6: Contacts on Microstopcocks 19
Figure 7-7: Liquid Delivery and Containment (not shown with sensors) 21
Figure 8-1: Showing center of gravity of entire system (outer case, inner case,
internal components). 24
Figure 8-2: Total Structure from Side 24
Figure 8-3: Total Structure Under G-Load Conditions (Front) 25
Figure 8-4: Inner Box Under G-Load Conditions (Side) 25
Figure 8-5: Inner Box Under G-Load Conditions (Front) 26
Table 8-1: Summary of calculated factors of safety for fastening of the equipment
under all g-load specifications 28
Table 8-2: Induced G-Loads and Factors of Safety 29
Figure 9-1: Electrical Schematic 30
Table 9-1: Load Table 31
Table 18-1: Weight Table 54
4. Flight Manifest
Stephen Steiner
Flight Date: Tuesday, April 23rd
Previous Flights: July 2001
Lucas Heinkel
Flight Date: Tuesday, April 23rd
Previous Flights: None
David Meister
Flight Date: Wednesday, April 24th
Previous Flights: None
Nicholas Kho
Flight Date: Wednesday, April 24th
Previous Flights: None
Alternate
Michael Fidler
Flight Date: As Needed
Previous Flights: None
5. Experiment Background
5.1 INTRODUCTION
Aerogel is a low-density, nanoporous, polymer solid that is typically 50-99% air. It
is formed by extracting the liquid solvent from a gel in such a way that the gel's
solid component is left behind without collapsing due to capillary action. The
remaining solid component retains most or all of the gel's original volume. This
solid material is aerogel.
A gel is a colloidal system in which a network of interconnected solid particles
spans the volume of a liquid medium. If the liquid solvent in a gel is evaporated, the
gel's solid particle matrix will collapse by capillary forces and form a dense glass-
like polymer. It is possible, however, to extract the liquid from a gel without causing
the matrix to collapse. This is typically done by supercritically extracting the liquid
from the gel. The result is a low-density solid polymer in the shape of the original
precursor gel. This solid is aerogel.
Figure 5-1: Silica Aerogel on a Hand Figure 5-2: Silica Aerogel on a Penny
The most heavily researched type of aerogel is silica aerogel. Silica aerogels are
typically transparent with a distinct bluish tint. Their densities range from 0.1 g/cc to
0.001 g/cc and, as previously mentioned, are 50-99% air. Although aerogels are
extremely low in density, they can withstand 500 to 4,000 times their weights in
applied force. In addition, silica aerogels have very high internal surface areas,
ranging from 250 m2/g to 4,000 m2/g.
Because of their low densities and high surface areas, aerogels also have unusual
thermal, electrical, and insulative properties. Silica aerogel is the best thermally
insulating material that has ever been produced, and because of this, has been
used by NASA as lightweight insulation for spacecraft. Aerogel could potentially be
used as superinsulating window inserts for industry, commercial, and aerospace
applications. Although silica aerogel is transparent, its noticeable blue color
prevents it from being used in such applications. In addition to its lengthy
processing times and high cost of production, aerogel is not currently commercially
practical.
5.2 Preparation of Alcogels
The physical and chemical properties of aerogel are determined during the
formation of the aerogel precursor gel, called alcogel. Alcogel is typically formed by
the sol-gel process. In this process, a solution of monomer molecules begins to
react to form oligomeric species (prepolymer particles) by a chemical reaction. This
solution of oligomeric species is called a sol. As the chemical reaction continues,
these oligomeric particles become larger and eventually interconnect. The
polymerization of these particles results in the formation of a solid particle matrix in
the solvent and eventually forms a gel. The manner in which these oligomeric
species interconnect defines the pore structure of the derivative aerogel.
Moreover, the amount of solvent present in the solution will determine the density
of the derivative aerogel.
The overall reaction by which the formation of the gel occurs is shown below (1,2).
Silica alcogel is typically formed by hydrolyzing a silicon alkoxide with water and
polymerizing the partially hydrolyzed species by condensation reactions.
nMe(OR)4 + 4nH2O nMe(OH)4 + 4nROH Hydrolysis (1)

nMe(OH4) nMeO2 + 2nH2O Condensation (2)

R=alkyl group (like C2H5), Me=metal (like silicon)
The sol-gel polymerization has three steps--hydrolysis, alcohol condensation, and
water condensation. These three reactions form siloxane bonds from hydrolyzed
alkoxide molecules, eventually forming a polymer across the liquid medium.
≡ MeOR + HOH ≡ MeOH + ≡ ROH Hydrolysis (3)
≡ MeOR + HOMe ≡ MeOMe≡ + ≡ ROH Alcohol Condensation (4)
≡ MeOH + HOSi ≡ MeOMe≡ + HOH Water Condensation (5)

5.3 Supercritical Extraction Process

Once an alcogel has been formed, it is usually soaked in a pure organic solvent to
remove any excess reagents and catalyst from the gel. This solvent must be
miscible with polar and non-polar solvents, since both are present in the alcogel.
After an alcogel has been adequately diffused with the pure organic solvent, it is
placed inside a high-pressure vessel and soaked several more times in liquid
carbon dioxide. Most organic solvents (like ethanol) have high critical points and
are extremely flammable at those conditions. Instead, a solvent exchange with
liquid CO2 can be utilized.
The CO2 solvent exchange reduces the risk of explosion associated with the high
critical points of organic solvents. Carbon dioxide has the benefits of being non-
flammable, miscible with organics, and having a low critical point of 31.1°C at 75
atmospheres. For the solvent exchange to succeed, the alcogel must be soaked in
liquid CO2 long enough for the CO2 to completely diffuse through the gel and take
the place of the organic solvent. At that point, the CO2 can be brought to
supercritical temperatures and pressures for solvent extraction.
After the gel has been Figure 5-3: Steel Supercritical Drying Vessel completely
diffused with CO2, (A Manuclave) it can be supercritically dried. This process is
done by heating the gel past its solvent's critical pointthe temperature and
pressure beyond which a substance cannot be condensed into a liquid by
increasing pressure. For CO2, this is done by heating the alcogel past 31.1°C and
1,050 psi.
Supercritical fluids are semi-liquids/semi-gases that possess some properties
similar to those of gases (such as expansion) and other properties like liquids
(such as viscosity). By heating the gel to its solvent's critical point, the solvent can
be extracted from the gel as a supercritical fluid without causing the gel's solid
particle matrix to collapse. Once the solvent has diffused out of the gel, the vessel
is depressurized, the gaseous solvent vented off, and the newly formed aerogels
can be taken out.
5.4 Rayleigh Scattering in Silica Aerogels
It has been proposed that formation of aerogel in microgravity could allow for the
production of non-blue aerogels. The blue color aerogels show is a result of
Rayleigh scattering of white light as it passes through the aerogel's nanopores.
These nanopores, sized from 5 to 15 nm across, are much smaller than the
wavelengths of visible light, yet large enough to act as particles for Rayleigh
scattering. The larger of these pores scatter light more easily, and are thus
responsible for the blue color in the aerogel. Shorter wavelengths are diffracted
more than longer wavelengths, and therefore blue and violet light are diffracted the
most. Although both blue and violet light are diffracted by these nanopores, only a
blue color is seen. This is because the human eye is more sensitive to blue light
than any other color, and so the violet light scattered by the aerogel is perceived to
be mostly blue.
5.5 Effects of Gravity on the Formation of Aerogel
The effect of gravity is usually negligible in systems affected only by Brownian
motion; however, as a solution begins to polymerize, oligomeric species with
considerable mass are formed, and can be affected by the force of gravity through
buoyancy.
The polymerization process in the formation of a sol is random, and thus the
weights of the oligomeric species (which will later polymerize to form the gel) can
vary considerably. Heavier oligomers have lower buoyancies, and thus, are
affected by gravity more than lighter species. This does not mean that heavier
oligomers sink to the bottom of the gel, but rather that they are not affected solely
by Brownian motion. The influence of gravity on the buoyancies of oligomeric
species in the sol prevents uniform interconnection during gelation. This non-
uniform polymerization in the gel causes the formation of larger nanopores
throughout the gel due to a downward bias of gravity on the heavier oligomeric
species.
The downward push of gravity on the forming gel also causes a "Venetian blind"
effect, observed by the fact that alcogels are more opaque through the side
(looking at the Venetian blinds) then through the top (looking down through them).
Previous studies of the effects of microgravity on the formation of silica alcogels
have been inconclusive. Lawrence Berkeley under the direction of Arlon Hunt
reported that aerogels formed in microgravity show higher surface areas and
different pore structures than aerogels formed in 1 G of gravity, but not necessarily
more or less blue in color.
5.6 Other Reduced Gravity Experiments
Experiments aboard the space shuttle utilized a slow gelation process to form
alcogels in zero-gravity, which were then brought to Earth and analyzed. The first
mission produced inconclusive results because of human and experimental error.
The second mission did not produce any aerogels, but silica Stober particles
(microscale alcogels) for pore structure analysis. The long gel times required to
produce silica alcogel mean that testing the effects of microgravity on its formation
require an environment where zero-gravity is sustainable for several hours.
Arlon Hunt did an experiment aboard the KC-135A analyzing the species in a silica
sol by X-ray scattering techniques. He found a difference in the formation of pre-gel
silica clusters that led him to do an experiment forming alcogel aboard a Saturn V
rocket a year later. The results showed that the lack of gravity affected the
formation of aerogel in such a way that it may be possible to make it completely
transparent if grown in zero-gravity. The Saturn V and KC-135A experiments were
limited to short amounts of time--too short for the formation of a substantial alcogel
sample, only long enough to produce pre-gel sols. These sols showed different
light scattering properties than those produced in 1 G of gravity, and so
microgravity would most likely also influence the formation of gels in similar
settings.
The formation of silica alcogel on a Saturn V rocket or the KC-135A was not
practical, however, since an extremely rapid gel time would be required.
5.7 Uses of Aerogel
Aerogel is currently only commercially available on a limited scale. Although it has
many potential applications including superinsulating window inserts, its noticeable
bluish tint and high cost of production prevent it from being commercially viable.
Aerogel has been used by NASA on various spacecraft including Stardust and
several Mars probes to collect high-velocity micrometeorites in outer space.
In order for aerogel to become a commercially viable product, several issues must
be addressed.
First, there must be a way to reduce the Rayleigh scattering in silica aerogel so
that it can be made optically transparent.
Second, there must be an inexpensive way to make it transparent. Currently, there
is no completely effective way of making clear silica aerogels.
5.8 Experimental Objectives
The objective of the experiment is to test if the absence of gravitational pull on
forming alcogels will have an influence on the pore structure of the resulting
aerogels. For silica aerogels, a more uniform pore structure may improve the clarity
of the derivative aerogel, possibly to the point where most of the Rayleigh
scattering in the aerogel could be eliminated.
The experiment is testing if reduced gravity can allow for an increase in surface
area in the resulting aerogels, and if so, by how much.
In addition to these objectives, we will be testing the effectiveness of microgravity
as a dispersion technique for embedding solid materials into aerogel matrices, for
the production of composite silica aerogels. We will be embedding iron, palladium,
and buckminsterfullerenes into several alcogels and will evaluate their uniformity in
comparison with composite aerogels formed by other techniques.
5.9 Description of Follow-up Flight
This experiment is our second attempt at forming aerogels in reduced gravity on
board the KC-135A. We have made numerous modifications and several complete
redesigns to our previous experiment, which was flown in July 2001.
6. Experiment Description
The experiment is testing the effects of reduced gravity on the formation of the
silica matrix of silica alcogels. This is done by mixing two liquids in reduced gravity
that form a gel upon being mixed. The liquids will be set to gel within 15 to 20
seconds after being mixed and, once the gel has solidified, the gel will remain
unaffected by reduced or induced gravity for the rest of the flight.
The two liquids required to form the alcogels are a base solution of
tetramethoxysilane, ethanol, and water and a catalyst solution of ethanol and
ammonium hydroxide. The volume of ammonium hydroxide in the catalyst solution
may vary from 50 to 100%, and will be added in 15 M concentration.
For each flight, 18 gels will be produced. The gels will then be taken back to the
ground and stored under ethanol in a sealed plastic container for shipment back to
the University of Wisconsin. The gels will then be supercritically dried and
analyzed. Analysis will be done using spectrophotometry, surface area
measurements, density measurements, tensile strength analysis, and compressive
modulus analysis.
In some of the gels for both flights, the molds will contain a small amount of a
fluorescent dye, palladium metal, iron metal, or buckminsterfullerenes. This is to
form composite alcogel materials by using microgravity to disperse solid particles
throughout the alcogel precursor liquid, allowing it to be trapped and evenly
dispersed throughout the alcogel when it forms. Doing so will illustrate the
dispersion process of liquids and solids in our gel apparatus and trap the
dispersion in a gel. In addition, a number of composite aerogel materials will be
produced.
6.1 Expectations of Experiment
The expectations of the experiment are that aerogels produced in microgravity will
show reduced scattering the blue-violet region of the spectrum compared with
aerogels produced in 1 G. We believe that between 30 and 36 alcogels of various
types will be safely and effectively formed in reduced gravity. It is also believed that
these gels will form within 5 to 15 seconds, which will be 5 seconds faster than the
target gel times that will be observed in 1 G.
The main objective of the experiment is to test to see if the pore structures of such
gels will be different than similar gels produced in 1 G. It is believed that analysis of
these gels will show them to be of significantly higher surface area than aerogels
produced in 1 G, as well as being more transparent (less blue) than silica aerogels
produced in 1 G.
These differences are expected to result in aerogels with surface areas between
1,000 m2/g to 2,000 m2/g higher, with more even nanoporosities and narrower
distributions of pore sizes, focused mainly between 5 to 15 nm.
More even nanoporosity in the silica alcogels may result in a reduction in the
visible effects of Rayleigh scattering in the resulting aerogels. It is believed that
aerogels produced in reduced gravity will have densities similar to aerogels
produced on the ground.
In addition to these expectations, it is also believed that composite alcogels of
silica and other materials can be formed with a microscopically even dispersal of
material throughout the gel.
6.2 Expectations of Corresponding Ground Experiments
Aerogels produced on the ground in the same manner are expected to have
surface areas of 500 m2/g to 2,500 m2/g, with nanoporosities typical of normal
aerogels and a broad distribution of pore sizes, from 5 to 65 nm.
7. Equipment Description
7.1 Introduction
The equipment in the experiment is used to pipette specific amounts of catalyst
solution into cylindrical glass molds that have been pre-filled (before the zero-g
flight) with base solution. The catalyst and base react in zero-g to form a gel in the
mold. The apparatus is designed to prevent and eliminate air bubbles in the gels by
using syringes, collapsible bags, and rubber o-ring sealed molds to handle the
liquids, allowing for liquid-tight reactions. The apparatus is computer controlled to
minimize human error and to minimize risk in breaking equipment due to
mishandling in zero-g.
Figure 7-1: Containment Unit Inner and Outer Boxes
7.2 Containment Unit
The equipment used in the experiment is housed in a glove box made of aluminum
frame and polycarbonate windows. The box consists of an inner glove box nested
in a larger glove box (see Figure 7-1) giving two solid, global layers of protection
around our apparatus. The glassware is our first layer of protection.
Figure 7-2: Glassware and Pipetting Apparatus
The inner aluminum-polycarbonate box is vibrationally isolated from the outer box
by 1.5 to 2.5 inches of damping foam on the bottom of the outer box and on all
corners. This foam protects the gelation reaction from low frequency vibrations
caused by the KC-135A and by the environment around the boxes.
The boxes are equipped with gloves to allow for manipulation of objects (such as
molds) in the box. The inner box is equipped with butyl dry-box gloves, which are
chemically resistant to all chemicals being used in the system. The outer box
gloves, which fit into the inner box gloves, are made of neoprene and lined with
cotton.
The inner box top is lined with two layers of 1/8" rubber and locked shut with Nylon
buckles. The outer box is also lined with rubber and locked shut with steel latches
on the front of the box. The lids are not airtight but can contain a liquid spill or glass
break.
7.3 Glassware
The apparatus housed by the boxes consists of a modified gas-tight borosilicate
syringe, called a zypette (a zero-gravity syringe-pipette, see Figure 7-2). The
zypette is used to measure out specific amounts of liquid for dispensing catalyst
into the molds. The zypette is connected to a borosilicate 4-way connection called
a "micro-t," to allow for three-way direction of the liquid flow. The micro-t is
encased in epoxy for structural support. Both the zypette and micro-t were
professionally manufactured.
The micro-t has three microstopcocks that branch from it, each connected to a
Luer lock to allow for attachment of needles to the zypette. On one connection of
the micro-t is connected a Mylar bag filled with catalyst. On another connection, an
empty Mylar bag is connected for dumping and flushing of waste. The third
connection is an open Luer lock to allow for a mold equipped with a Luer needle
(see Figure 7-3) to be attached to the apparatus.
7.4 Glassware Controls and Sensors
The zypette is operated by a 25-lb. actuator that pushes and pulls the zypette
piston up and down to aspirate and dispense liquid as instructed. The amount of
liquid in the zypette is monitored by a set of 3 laser diode/photocell assemblies,
placed at the 0 mL, 2.5 mL, and 5 mL positions on the zypette (see Figure 7-4).
The assemblies are connected to a computer which interprets the status of the
photocells (exposed to light or blocked by the piston) to determine the height of the
piston and the volume of the liquid in the zypette. The laser/photocell assemblies
are made of
Figure 7-3: Syringe-Molds polycarbonate and shielded by opaque plastic to
prevent laser light from shining outside of the assembly.
The microstopcocks are opened and shut by 12VDC motors, turning the handles of
the microstopcocks by a gear mechanism (see Figure 7-5). The motors are
controlled by the computer. Two aluminum contacts placed on the handles and
bases of the microstopcocks connect when the microstopcocks are open,
instructing the computer the stopcock is open. When the contacts do not touch, the
stopcock is closed and the circuit is broken (see Figure 7-6).
The actuator is operated by two circuits that are controlled by the computer, a push
circuit that supplies positive voltage to the actuator and a
Figure 7-4: Laser Diode Photocell Assembly Across Zypette
Figure 7-5: Motor and Gear Assembly for Moving Microstopcock pull circuit that
supplies negative voltage to the actuator (see Electrical Analysis).
7.5 Computer Controls
The glassware is operated by three motors and an actuator that are controlled by
optically isolated relay circuits interfaced with the parallel port of the computer. The
computer runs a program called ZGel, written by our team, that has subroutines
designed to operate the glassware with composite functions. For example, the
computer can be instructed to inject liquid into a Figure 7-6: Contacts on
Microstopcocks mold by aspirating 5 mL, waiting 2 seconds, and dispensing it in
small bursts, which involves several separate mechanical steps, like opening
stopcocks and pulling the actuator. The program has built-in safety controls, for
example, preventing the actuator from operating when all microstopcocks are
closed, to prevent pressure build-up or strain (see Figure 7-6). If the computer
malfunctions, the system can be switched to manual mode, which relies on a panel
of switches located inside the inner box connected in parallel to the optical relays
that power the devices. These switches perform individual functions such as
opening motors and moving the actuator arm, but not composite functions.
If power fails to the system, the experiment is not operated.
7.6 Molds
The gelation reaction is carried out by injecting 2.5 or 5.0 mL of catalyst into molds
pre-filled with base (prior to the flight). The molds are glass cylinders clamped shut
with glass plates and sealed by rubber gaskets, equipped with Nylon syringes that
expand when liquid is injected, to accommodate for the volume of liquid. The molds
are housed in a plastic shelving unit that contains 18 boxes, fitted with foam
cutouts for the molds to rest in. The drawers are snapped into place with a
magnetic snap.
7.7 Liquid Containment and Delivery
Liquid reagents used for the experiment are kept in 30 mil, 500 mL Mylar bags with
special septum seals. The septum seal is comprised of a Nylon gasket epoxied to
the inside of the Mylar bags, sandwiched against a second Nylon gasket epoxied
to the outside of the Mylar bag (see Figure 7-7). Through the gaskets is epoxied
and sealed a 0.25"-diameter 3"-long PTFE tube. To the top of the tube is a rubber
septum sealed in place. The liquid reagent is introduced and extracted from the
Mylar bag by injection with a syringe needle.
Liquid is pulled out of the bags by steel needles connected to the micro-t, by the
slight pressure differential caused by the actuator pulling the zypette piston
upwards. Liquid is injected into the bags by the actuator pushing down. Two bags
are used for the experiment–a catalyst source bag and a waste bag. The bags are
secured in aluminum boxes and strapped in place with Velcro straps. Two straps
that strap over the top of the bag, two straps secure it to a side of the aluminum
box, and one strap secures it to the bottom.
Figure 7-7: Liquid Delivery and Containment (not shown with sensors)
8. Structural Analysis
Structural analysis of all components involved revealed that the apparatus is
sufficiently designed to withstand all g-load specifications required by NASA. First,
calculations of g-loads of the entire system are discussed showing that the
apparatus is securely fastened to the fuselage of the KC-135A. Next, calculations
are presented showing that all internal components will be isolated from the cabin
of the aircraft via the outer case. Free-body diagrams (FBDs) are included for each
calculation. Factors of safety for all critical components show that the equipment
built for this experiment is safe for all persons and aircraft components.
8.1 Overview
Two cases, one outer and one inner separated by a layer of energy-absorbing
foam, are used to provide containment for chemicals in the experiment. Internal
glass, Mylar, and cell (mold) components provide the third layer of containment.
The frames for the outer and inner case are made of aluminum L-beams
("angles"). The L-beams are 1/8" thick, 90o bend, with 1½" legs. Sides of each
case are made of ¼" polycarbonate sheets bolted to the aluminum L-beams with
¼" steel bolts. The upper lids of each case are made of 1/8" polycarbonate sheets
with hinges attached by 5/16" steel bolts. The bottoms of each case consist of ¼"
aluminum sheets. The outer case is attached to the fuselage of the aircraft with two
2"-wide cargo straps and 3/8" steel bolts.
8.2 Centers of Gravity
The entire system has left-right and front-back symmetry. All calculations for the
centers of gravity use a 3-D right-handed coordinate system with the "origin"
located at the bottom-left-rear corner of the outer case. To calculate the centers of
gravity (CG), we used individual component weights and positions relative to the
origin. For the structural analysis, we calculated two CGs: one for the inner case
containing all inner components and one for the entire system.
The total weight (at 1g) of the inner box with internal components is 80 lbs. The
total weight of the internal components is less than 10 lbs. We will assume this
weight to be concentrated at the CG of the inner box due to relatively symmetrical
weight distribution among the internal components. The outside edges of the inner
case have dimensions 19" x 49" x 17" (x, y, z l, h, w). After considering left-right
and front-back symmetry and the 1½" foam layer between the inner and outer
cases, we can see that the CGx and CGz of the inner case with all internal
components are located at 11 (19/2 + 1.5) and 10 (17/2 + 1.5) inches, respectively.
CGy is a slightly more complicated calculation. The inner case has an aluminum
sheet 1" from the bottom as well as an aluminum sheet 10" from the bottom that
serves as a shelf for the internal components of the experiment. Each aluminum
sheet weighs 8 lbs. CG in the vertical direction is calculated as follows:
CGy = [24.5*64 + 10*8 + 1*8] / 80 + 1.5 (foam) = 22.2"
Hence, the CG of the inner case with all internal components is (11, 22.2, 10).
The center of gravity of the entire apparatus is required for calculations to show
that the equipment will be securely fastened to the aircraft under all g-load
specifications. The weight of the outer case including foam is 81 lbs.
CGx for the outer case alone is 22.75/2 = 11.4 inches. CGz for the outer case is
21/2 = 10.5 inches. CGy for the outer case, with an 8-lb bottom aluminum plate is
[25.5(81-8) + 1(8)] / 81 = 23 inches. Below are the calculations of the CG for the
entire system (i.e., outer box + inner box + internal components):
CGx = [11*80 + 11.4*81] / 161 = 11.2"
CGy = [22.2*80 + 23*81] / 161 = 22.6"
CGz = [10*80 + 10.5*81] / 161 = 10.3"
Here we can see that the center of gravity for the entire system is located at (11.2,
22.6, 10.3). The weight of the equipment will be assumed to be concentrated at the
center of mass for all moment and factor of safety calculations.
Figure 8-1: Showing center of gravity of entire system (outer case, inner case,
internal components).
Figure 8-2: Total Structure from Side (Note: Straps extend behind handle over
box)
Figure 8-3: Total Structure with Center of Gravity (Front)
Figure 8-4
Figure 8-5
9-g's Forward
Under an induced gravity of 9-g's forward, the entire system will experience a
weight of 1449 lbs.
(161*9). The reaction force to this weight in the horizontal direction will be provided
by the two-2" wide cargo straps attached to the handle of the outer case (bolted to
the aircraft via 3/8" steel bolts). Summing the forces in the x-direction we can see
that the straps will each need to provide a reaction force of 725 lbs in the negative
x-direction. Each strap is capable of supplying 5000*cos(58o) = 2650 lbs. This
results in a factor of safety of 3.66 for the entire apparatus in 9-g's forward in the
horizontal direction. Taking the moments about the point (0, 0, 10.3) we can see
that the reaction moment for each strap will need to be 1449*22.6 / 2 = 16400 lb-in.
The straps are each capable of providing a moment of 5000*sin(58) * 18.5 = 78400
lb-in. This results in a factor of safety of 4.78. We can see that the equipment will
remain static under 9-g's forward.
3-g's Aft
Under an induced gravity of 3-g's aft, the entire system will experience a weight of
483 lbs.
(161*3). The reaction force to this weight will be provided by the two-2" wide cargo
straps attached to the handle of the outer case (bolted to the aircraft via 3/8" steel
bolts). Summing the forces in the x-direction we can see that the straps will each
need to provide a reaction force of 242 lbs in the positive x-direction. Each strap is
capable of supplying 5000*cos(58o) = 2650 lbs.
This results in a factor of safety of 11.0 in the horizontal direction for the entire
apparatus in 3-g's aft. Taking moments about the position (22.75, 0, 10.3) we can
see that each strap will need to provide a reaction moment of 483*22.6 / 2 = 5460
in-lbs.. Each strap is capable of supplying a 5000*sin(58)*18.5 = 78400 in-lbs..
This results in a factor of safety of 14.3.
6-g's Down
While experiencing an induced gravity of 6-g's down, the equipment will experience
an induced weight of 966 lbs. The area of the bottom of the equipment is 3.32 ft^2.
This results in a stress of 291 lbs/ft^2.This exceeds the acceptable in-flight floor
loading specification of 200 lbs/ft^2. Hence our experiment will need to be provided
floor shoring of at least 5 square feet to satisfy the g-load specifications in the 6'g's
down situation.
2-g's Lateral
The equipment will experience an induced weight of 322 lbs. in the lateral direction.
To avoid translational motion in the z-direction, the outer case will need to be
ratcheted down with enough force so that the frictional force generated against the
foam is significantly greater than the 322 lbs. of induced force. If the case were to
rotate, the cargo straps would need to counter the moment induced about the
position (11.4, 0, 0). The moment that needs to be countered would be 322*22.6 =
7,300 lb.-in. The tether strap going over the top of the outer case would need to
provide a force of 7,300 / 21 = 350 lbs. Since the strap is capable of providing a
force of up to 5,000 lbs., the factor of safety for 2'g's in the lateral direction would
be 14.3.
2-g's Up
Under an induced gravity of 2'g's, the weight of the equipment would be 322 lbs.
This weight will be countered by reaction forces provided by the straps over the top
of the outer case. Each strap is capable of providing up to 5000 lbs. of reaction
force when in tension.This results in a factor of safety of 5000*2 / 322 = 31.
8.3 Summary
All of the calculations for the entire system used in the formation of aerogel will
remain in static equilibrium for all g-load specifications. The use of two cargo straps
will provide sufficient reaction forces to secure the apparatus to the fuselage of the
KC-135A.
Table 8-1: Summary of calculated factors of safety for fastening of the equipment
under all g-load specifications.Forces and moments shown are the reactions that
need to be provided by one cargo strap.
Case Force (lbs.) Force FS Moment (lb-in.) Moment FS
9 g's forward 725 3.66 16400 4.78
3 g's aft 242 11 5460 14.3
6 g's down 966 on aircraft floor see text N/A N/A
2 g's lateral Need more info see text 7300 14.3
2 g's up 161 31 N/A N/A
8.4 Structural Integrity
Under an induced acceleration, the outer box will contain all components within it
and not come apart or deform. We intentionally over-engineered the outer box so
that it could safely contain everything within it. The shear strength for
polycarbonate is 7,000 psi. The area being stressed is 0.196 in2. If the entire mass
of the inner box applies a force on any vertical face of the outer box, it force will be
evenly applied over 18 bolts.That gives the box's faces a strength of 24,000 lbs.
each at minimum. In the up direction there are 2 latches and 2 hinges, with 2 bolts
connecting each latch and 5 bolts connecting each hinge. The reaction forces of
the bolts will counter the induced force on the lid. The weakest component of the
lid is the hinges, and each are rated at 5,000 lbs. each in shear. The loads and
factors of safety are shown in the following table.
Table 8-2: Induced G-Loads and Factors of Safety
G-Load Direction Induced Force Structural Strength of Box Factor of Safety
9g's Forward 720 lbs. 24,000 lbs. 33.3
3g's Aft 240 lbs. 24,000 lbs. 100
6g's Down 480 lbs. 16,488 lbs. 34.4
2g's Lateral Left (Back of box)
160 lbs. 24,000 lbs. 150
2g's Lateral Right (Front of box)
160 lbs. 24,000 lbs. 150
2g's Up 160 lbs. 10,000 lbs. 62.5
9. Electrical Analysis
9.1 Electrical Schematic
Figure 9-1: Electrical Schematic
The system shows the block arrangement for the relays, sensors, and computer
used in the system. The relays, in addition to being optically activated, can be
activated by pushing a button parallel with the optical sensors.
The power supply provides +5VDC, +12VDC, and +24VDC power to the relays
and the system. The computer is a Gateway Solo laptop, 1.0 GHz, Pentium 4
processor, 128 MB RAM, running an MS-DOS based program called ZGel that
controls the system.
9.2 Load Analysis
The electronic sensors on the microstopcocks, LEDs, and the photocells on the
zypette do not use any substantial current and are powered off of the computer's
parallel port. The relays power the laser diodes, motors, and actuator.
Table 9-1: Load Table
Wire Gauge Current Drawn
Max Current Voltage Devices Current
1 Power Strip
Cord
14 9.4 Amps Max 20 Amps 115 VAC @ 60Hz
Laser control module and laser x 3
250 mA x 3 =750 mA
Motor control module and motor x 3
1.2 A x 3 = 3.6A
Actuator control module x 2
250 mA x 2 = 500 mA
Computer 2.5 A Actuator 2.0 A
Total 9.4 A
9.3 Emergency Shutdown Procedures
Emergency shutdown can be performed by pressing the power switch on the main
power strip. This switch will deactivate all electronics in the system, and cut power
to the computer. The computer will then go into battery mode, so our data will be
saved. The electronics can be repaired if necessary during a portion of 1-g or zero-
g, and can be reinitiated.
10. Pressure Vessel Certification
The system uses glassware that utilizes slight pressure differentials to draw liquids
into the apparatus and dispense them into the molds. All reagent bags and molds
are volume expandable and collapsible, so no pressure can build up during
nominal operation
The system is comprised of standard steel needles, Luer locks, a modified
borosilicate syringe, and a modified set of microstopcocks. The system has been
classified as Category E by JSC Personnel.
10.1 Schematic
Consult the Equipment Description for more detailed description of the glassware
apparatus.
The apparatus is comprised of a borosilicate syringe, modified with a standard
ground-glass connection for a tip and a pipette-fit head. The piston in the syringe
has been cut short and is fitted with a stainless steel rod secured by a threaded set
screw that screws into the piston. The piston is pulled up and down by an actuator
to which the steel rod is screwed.
The modified zero-gravity syringe-pipette, or zypette, is fit into a four-way micro-t
connection by a standard ground glass joint and sealed with silicone grease. The
zypette is clipped to the joint with a Keck clip. The four-way joint, or micro-t, has
three Luer lock connections for attaching syringe needles to. The micro-t has three
microstopcocks to control where the liquid goes.
One Luer lock is connected to a liquid-filled Mylar bag for pulling catalyst. A second
Luer lock is connected to an empty Mylar bag for dumping waste.
To attach molds to the apparatus, the molds, equipped with Luer needles
(connector side is exposed and cannot be removed), can be snapped onto the third
lock. Molds are volume expandable by Nylon syringes.
10.2 MAWP Table
Component MAWP are provided by their manufacturers, with the exception of the
Mylar bags which were tested with a nitrogen tank to determine burst pressure
along the edges, and divided by 2.
Component MAWP
Zypette, borosilicate glass 200 psi
Micro-T, borosilicate glass 200 psi
Syringe needles 2,000 psi
Mylar bags 50 psi
Nylon syringes 100 psi
MAWP for entire system: 125 psi–calculated by dividing the 25 lbs. of force the
actuator can exert by the surface area of the zypette piston.
This is only reached when all stopcocks are closed and actuator is pushing down.
This case has been prevented by safety controls, and would not affect the Mylar
bags or Nylon syringes because they are expandable. The Mylar bags have a
volume of 500 mL, 100 times greater than the volume of the zypette and more than
95 greater than the entire system. Any high pressure in the system would be
resolved by volume expansion into the Mylar bags, as long as it did not occur more
than 20 times. This is not the normal function of the system, and will not occur. The
syringe pistons would pop out if 125 psi was attained, which cannot occur when the
microstopcock to the syringe is open.
11. Laser Certification
Three shielded laser diodes will be used to monitor the level of the piston in the
zypette during the experiment.
a) Lasers are Class II, red laser diodes (similar to those used in laser pointers), 6
mm dot @ 3 meters, <1 mW optical power, 60 mA maximum current, made by
National Semiconductor for the Tandy Corporation.
b) Lasers are used to shine light through the zypette (across the diameter of the
zypette, not across the length of it) onto photocells to electronically monitor the
position of the piston.
c) Lasers will be active during the entire flight.
d) Lasers are shielded in opaque plastic casings and can be deactivated by a
switch in the box or by the master kill switch on the power strip outside of the box.
12. Parabola Details and Crew Assistance
The experiment will try to produce 18 gels over the 30 parabolas of zero-gravity
during each flight.
The first two parabolas will be used to get accustomed to the zero-gravity
environment and to ensure all equipment is operating within normal parameters.
The last 10 parabolas will be used in case of a malfunction or to retry forming gels
that did not form, and to do outreach for our video and the National Geographic
Channel. No crew assistance is requested.
13. Free Float Requirements
The experiment has no free float requirements.
14. Institutional Review Board
The experiment has no IRB requirements.
15. Hazard Analysis Report
The experiment uses a number of hazardous chemicals and one toxic chemical
that need to be specially contained. The equipment used to form aerogels in
microgravity has been designed to minimize hazards involving the release or
leakage of these chemicals. The supercritical drying process mentioned in the
Experiment Background is not being done in microgravity. The supercritical
drying process is being done after the flight outside of NASA's facilities.
DETAILED HAZARD DESCRIPTIONS
Hazard Number 1:
Flammable/combustible material, fluid (liquid, vapor, or gas).
Description: Base solution for silica alcogels is composed of flammable liquids
(ethanol and tetramethoxysilane/tetraethoxysilane); danger with eye/skin contact,
inhalation, ingestion.
Causes: Liquid escapes from syringe or cell (mold), ignites from spark or fire.
Controls: All liquids are triple-contained. Even if liquid escapes from a cell or the
connected syringe, it will be contained by the inner and outer case. No sparking
electrical equipment is being used (all wires are thoroughly insulated), and all
apparati are bolted firmly inside to the case. All cells are firmly stored in their
respective dense foam containers. No ignition sources will be used in the
experiment.
Hazard Number 2:
Toxic/noxious/corrosive/hot/cold material, fluid (liquid, vapor, or gas).
Description: Tetramethoxysilane is toxic, ammonium hydroxide is corrosive.
Noncontained liquids pose health hazards/danger to equipment, danger of contact
with eyes/skin, inhalation.Ingestion.
Causes: Liquid escapes from Mylar bags, case breaks/leaks, glass components
crack and leak.
Controls: All liquids are triple contained. Even if liquid escapes from a Mylar bag or
any glass components, it will be contained by the inner and outer case. However,
toxic chemicals will be used in extremely small/dilute quantities. Applicable
temperature range for polycarbonate thermal applications: 0 – 200oF.
Polycarbonate is resistant to all chemical components used in this project.
Hazard Number 3:
Flammable/combustible material, fluid ignition source (i.e,short circuit;under-sized
wiring/fuse/circuit breaker).
Description: Base solution for silica alcogels is composed of flammable liquids
(ethanol and tetramethoxysilane/tetraethoxysilane), spark ignites noncontained
liquid; burns, suffocation.
Causes: Structural failure of experimental case, linear actuator may spark from
overload in power supply. Wiring insulation degradation.
Controls: Liquids are triple-contained. Power supply is limited to maximum of 12
Volts.Power supply significant distance from experimental case and chemical
solutions. Wiring insulation is resistant to chemicals used in this experiment.
Hazard Number 4:
Glass apparatus comes unclamped from case / steel ring stand.
Description: Glassware becomes unclamped from case, free floats.
Causes: Excessive structural loads, team members hands knock these clamps
loose.
Controls: Clamps will be tightened and thoroughly inspected prior to each flight.
Each glass component is relatively short and thick, unlikely to crack. Pipetting
glass components are not directly in user's range of motion.
Hazard Number 5:
Mylar bags become unattached to the micro-T, or a Mylar bag is cut.
Description: Steel connection to the Mylar bag becomes loose.Threat of exposure
to toxic liquids. Thin steel rod may puncture other materials, including gloves.
Causes:User's hands accidentally disrupts steel-Mylar bag connection. Micro-T
breaks/shatters, resulting in sharp glass particles that may puncture bag.
Controls: Steel-Mylar bag connection is tightened by rubber o-ring. Micro-T is
manufactured to minimize possibility of breaking, designed as short, thick glass. All
other components inside of inner case have blunt edges. User must be aware of
this potential hazard.
Hazard Number 6:
Syringe pistons on cells come out of syringe chassis.
Description: The piston of the syringe is somehow removed and hazardous liquids
can leak out. Danger of contact with eyes/skin, inhalation, ingestion.
Causes: The syringe is pushed too far, comes out of the shell, and allows
hazardous fluids to leak out.
Controls: Syringe piston is cut-off so that external forces may not introduce torque.
Maximum volumedisplacement from the cell will is 5 ml (actuator is fully extended
at displacing 5ml of liquid). Syringe is built to allow 7 ml of liquid. Cover slip is
bolted at end of syringe so that piston cannot be removed.
Hazard Number 7:
Syringe connection to the aerogel cell comes loose.
Description: Hazardous liquids leak out of apparatus. Presents danger of eye/skin
contact, inhalation, ingestion.
Causes: Connection badly assembled, damaged.
Controls: Cells are securely fastened to syringes with Luer locks. Liquids are triple-
contained and cannot leak out into the air.
Hazard Number 8:
Steel tubing fractures, liquid leaks out of assembly.
Description: Hazardous liquids leak out of apparatus. Presents danger of eye/skin
contact, inhalation, ingestion.
Causes: Damaged steel tubing.
Controls: Steel tubing is built to withstand 70000 psi.Highly unlikely for the steel
tubing to break.
Hazard Number 9:
Aerogel cell is not adequately attached to micro-T.
Description: Glass tubing/ Luer lock is inadequately attached to aerogel mold,
assembly leaks. Presents danger of liquids leaking out of apparatus, danger of
contact with eyes/skin, inhalation, ingestion.
Causes: Glass tubing not properly secured onto aerogel mold, Luer lock is not set.
Controls: User will have to be sure to firmly connect the cell to the micro-T. Luer
lock has to be securely fastened. All chemicals are contained within double-walled
polycarbonate box.
Hazard Number 10:
Outer case cracks/becomes unbolted.
Description: Outer case bolt connections become loose, structural failure.
Cause: Extremely high-velocity impact to container chests, poor construction.
Controls: Structural analysis predicts all fastened components to the outer case to
withstand all g-load specifications. Inner case is initial barrier to experimental
apparatus, inner case would have to fail first.
Hazard Number 11:
Inner case cracks/becomes unbolted.
Description: Inner case bolt connections become loose, structural failure.
Cause: Extremely high-velocity impact to container chests, poor construction.
Controls: Structural analysis predicts all fastened components to the outer case to
withstand all g-load specifications. Outer case is designed to provide back-up to
the inner case.
Hazard Number 12:
Inner or outer case lid comes open.
Description: Aluminum/polycarbonate lid becomes loose and opens.
Cause: Lid insufficiently locked shut or hinges come unloose, rubber o-rings do not
adhere.
Controls: Hinges and clips are securely fastened to withstand all g-load
specifications. Lids will be securely fastened and tested directly prior to flight. If lids
need to be opened during flight, user needs to be absolutely sure to refasten clips.
Inner and outer cases complement each other so if one opens, the other should
remain closed.
Hazard Number 13:
Computer, sensor interface, accelerometer, or power strip shorts
out/sparks/breaks.
Description: Malfunction in power supply or computer causes a spark, power to
computer is lost. Poses risk of electric fire.
Cause: Power surge from aircraft power supply, damage to one of the components
causes it to malfunction.
Controls: A surge protector, equipped with a master kill switch, is used in the event
of electrical problems. If the computer or sensor interface shorted out, it would
merely shut off and would pose no real health hazard.
No software-controlled devices or procedures are utilized during the experiment
and so power failure does not pose a health risk to the researchers or the crew.
Sparks pose a risk of fire since flammable liquids are used in the formation of the
silica alcogels, but those liquids are triple-contained in sealed plastic containers
and are placed a sufficient distance from the power supply that risk of ignition of
the liquids is extremely improbable. In addition, the power strip is UL listed and is
unlikely to spark or malfunction.
Hazard Number 14:
Glass micro-T breaks.
Description: Glass micro-T fractures in one or more places, resulting in sharp
pieces of glass inside the inner case.May cut user's hands.
Cause: Excessive structural load, team member mishandles equipment, clamping
mechanism comes unloose.
Controls: Micro-T is designed to withstand all g-loads specified in structural
analysis. User must be aware to avoid any actions that may compromise integrity
of micro-T. Prior to flight, all clamping mechanisms will be thoroughly tested and
locked to avoid structural failure. PODs will be securely fastened in their holding
compartments and the POD in use will be secured to either the Luer lock and the
micro-T or the passive damping system (PDS). Elastic binding to the PDS will
ensure that the PDS will not contact the micro-T (indicated in structural analysis).
Two sets of gloves from the inner and outer case protect user's hands.
Hazard Number 15:
Linear actuator failure.Description: Actuator comes loose inside inner case,
breakage of other components, fire.
Cause: Clamping mechanism on actuator fails, free-floating actuator fractures
glass or steel components inside inner case, short-circuit or exposed wires may
cause sparks or even fire inside inner case.
Controls: Clamping mechanism is thoroughly inspected prior to each flight.
Actuator is calculated to withstand all g-load specifications. All wires are insulated
to avoid possible sparks. Polycarbonate is electrically (17 ohm-cm) and fire
(flammability = V-2) resistant on inner and outer case to avoid electrical
complications from the actuator.Double containment of linear actuator.
Hazard Number 16:
Cell casing comes apart.
Description: Toxic chemicals are released inside the inner case.
Cause: Clamps loosen,excessive pressure build-up. Cell edges leak noxious liquid
components.
Controls: Clamps are securely fastened and tightened prior to each flight. Edges of
each cell will be attached to the clamping mechanism via a rubber gasket material.
Attachments are designed to withstand all g-load specifications. Syringe attached
to cell dissipates majority of any pressure build-up from catalyst injection.
Hazard Number 17:
Catalyst does not flow well through the micro-T.
Description: Leakage of toxic chemicals into inner case.
Cause: Build-up of excessive fluids may increase micro-T pressure and cause
leakage. Poor flow, tubing too small. Undesired mixing of catalyst and base if base
leaks from cell into micro-T.
Controls: Second steel tube running from micro-T to another Mylar bag can allow
excess fluids through and release pressure build-up. Positive pressure from linear
actuator ensures that there will be very minimal leakage of base from cell into the
micro-T. Any base that does enter the micro-T can be flushed into the Mylar bag.
Also, manipulation of micro-stopcocks will not allow base to come into micro-T.
Micro-T has been designed and tested to allow catalyst to flow smoothly without
any turbulence or clotting.
Hazard Number 18: Laptop failure.
Description: Loss of automated experimental capabilities.
Cause: Low battery, computer virus, straps loosen and laptop begins to free float
and connection to apparatus is lost.
Controls: We will bring a back-up battery on each flight and use anti-virus software.
Straps will be securely fastened and tested prior to each flight. Connection to
apparatus has several points of attachment, ensuring that connection will remain
under all g-load specifications. Experiment may still operate under a manual mode.
Hazard Number 19:
Optoelectronics failure.
Description: Loss of automated experimental capabilities, excessive heating of
toxic/flammable chemicals.
Cause: Lasers may become loose, inoperable Controls: Lasers are certified for use
and emit low energy. Lasers are securely fastened to the zypettte and connections
are calculated to withstand all g-load specifications. Low energy dissipated from
both lasers makes the likelihood of igniting a fire extremely unlikely.
Hazard Number 20:
Glove openings from case to inside of apparatus ruptures.
Description: Exposure of user to potentially dangerous chemicals, broken glass,
sharp thin steel rods.
Cause: Glove material tears with excessive loading by user. Laceration of material
by sharp pieces from inside the inner case or outside of the outer case. Any
excessive puncturing force may rupture glove material.
Controls: Two sets of gloves are used; one set attached to the outer case, one set
attached to the inner case. No sharp objects will be allowed near the experiment.
Gloves are made of durable, chemically inert rubber. Attachments of gloves to their
respective cases can withstand all g-load specifications.
Hazard Number 21:
Steel-clamping rod (ring stand) dislodges from inner case.
Description: Equipment damage, broken glass and exposed sharp steel rods.
Cause: Bolts loosen, become unattached so that apparatus may free-float inside of
the inner case.
Controls: Connections of steel clamping rod to the inner case are designed to
withstand all g-load specifications. Inner and outer casing ensures that no parts of
apparatus will become exposed to cabin of the KC-135A. Bolted and epoxied in
place with 4 heavy bolts and ceramic-metal epoxy.
Hazard Number 22:
Connection between inner and outer casing fails.
Description: Inner case becomes a free-floating object, increasing likelihood of
toxic chemical exposure to cabin of KC-135A.
Cause: Bolts connecting the inner case to the outer case fail.
Controls: Bolt connections are designed to withstand all g-load specifications.
Outer case is structurally sound to withstand all possible external forces applied by
the inner case.
Hazard Number 23:
Outer case becomes loose.
Description: Outer case becomes a free-floating object in the KC-135A cabin.
Possible physical injury to team members or
any personnel in the vicinity of the experiment.
Cause: Failure of fastening devices and/or tether straps.
Controls: A thorough pre-flight test analysis will be conducted to ensure casing is
firmly fastened to the inside of the airplane. Structural analysis shows that
fastening mechanism is designed to withstand all g-loadspecifications.
Hazard Number 24:
Stopcock jams, unable to move.Description: Inability to move stopcock may result
in poor aerogel yields, back flow of base into the micro-T, excessive pressure
build-up, leakage of toxic chemicals into inner case.
Cause: Back flow of base into micro-T, solidifying connection of micro-T to the
stopcock. Dry glass-glass connection,no lubricant.Excessively cold temperatures.
Controls: All stopcocks will easily be accessible to team members for manual
adjustments. Glass-glass connections will be lubricated prior to use to minimize
chances of jamming. Temperatures will not drop below 32oF. Back flow of base
into micro-T will be minimized by careful user experimental technique; excessive
amounts may be flushed out of micro-T by the linear actuator and the Mylar waste
bag.
Hazard Number 25:
Aerogel foam shelving units become detached, cracked Description: Free-floating
PODs (protective outer devices) in the inner case, leakage of toxic chemicals.
Cause: Velcro straps holding the PODs in place may lose their adhesiveness, bolts
attaching foam to inner case may become loose, foam degrades or is pulled apart
from bolts/inner case.
Controls: Velcro straps are new and thoroughly tested to withstand all g-load
specifications. Pre-flight analysis will ensure POD shelving units are ready for use.
Bolt/epoxy attachment of foam to the inner case is designed to withstand all g-load
specifications. Foam is relatively dense, highly unlikely to degrade or come apart
from all connections. Inner and outer case ensures no toxic chemical exposure to
team members or any other personnel in the KC-135A.
Hazard Number 26:
Explosion in micro-T or zypette.
Description: Toxic chemicals released into the environment, loss of aerogel molds.
Cause: Temperatures exceeding boiling points of liquids used, gases causing
increased pressure in apparatus. Excessive liquid pressure build-up.
Controls: Temperatures will be well below the boiling points of our chemical liquids.
The syringe in the cell or the 2nd Mylar bag may dissipate any liquid pressure
build-up. Extremely unlikely that an explosion could occur, since chemicals being
used are in dilute solutions, and no off-gassing takes place.
Hazard Number 27:
Laser damages retina of team members.
Description: Temporary or permanent eye damage (i.e., retinal damage) to team
members.
Cause: Clamping mechanism failure, excessive structural loading, and high-
powered laser.
Controls: Power and intensity of lasers is much less than dangerous levels. Laser
clamping mechanisms can withstand all g-load specifications. Lasers are certified
for safety. Lasers are contained in opaque clamps and are not visible unless
clamps are taken apart. If a laser did come loose, it would detach from the
electrical connection before it would come out of the casing.
Hazard Number 28:
Velcro on Mylar bags becomes loose.
Description: Free-floating Mylar bags, collision with object in box, may release toxic
chemicals to the inside of the inner case.
Cause: Poor Velcro, worn out, dirty, bumped on accident.
Controls: New Velcro will be used, replaced if necessary. Back-up Velcro will be
carried onboard in case of failure. Plastic containers containing the Mylar bags are
securely fastened to the inner case and can withstand all g-load specifications.
Bags are secured by 5 Velcro straps, unlikely to all fail. Bags still held in place by
needles penetrating them.
Hazard Number 29:
Epoxy attachments become loose.
Description: Potential for toxic chemicals to become exposed to inside of KC-135A
cabin.
Cause: Epoxy attachments between polycarbonate and aluminum L-beams or
plates become loose or degrade.
Controls: All epoxy adhesive attachment sites use a thorough amount of epoxy.
Connections are strong enough to withstand all g-load specifications. No
connection is solely dependent on an epoxy bond, but a combination of bolts,
rubber seals and gaskets, and friction fits.
Hazard Number 32:
Linear actuator connection to the zypette breaks, comes off.
Description: Potential break on zypette, loss of automated dispensing.
Cause: Linear actuator spins, possibly causing excessive torque on the steel rod
connecting to the piston inside the zypette. Bolts on the actuator come loose,
clamping mechanism holding the bolts come loose.
Controls: Bolts and clamping mechanism are securely fastened and tested prior to
flight. Clamping mechanism is designed to withstand all g-load specifications and
torque introduced by the linear actuator.
Epoxy connection to the steel rod connected to the actuator is very strong, held in
place by threaded connection to the piston inside the zypette.
Hazard Number 33:
Luer locking mechanisms fail.
Description: Toxic chemicals released into inner case.
Cause: Luer locking mechanisms fail, poorly fastened, user mishandles apparatus.
Controls: Luer locking mechanisms connecting the zypette and Mylar bags to the
micro-T will be securely fastened and tested prior to flight. Luer locking
mechanisms between the micro-T and the individual cells have to be carefully
handled by a team member. Team member must be aware of always fastening the
Luer locking mechanism before initiating catalyst injection into the cell. Apparatus
is triple-contained so that even if liquid were released into the box, it would be
contained.
Hazard Number 34:
Electrical or computer failure causes uncontrolled mechanical stress
Description: Fire, breakages.
Cause: Unknown, possibly loose electrical connection, static discharge shorts out
circuitry, Microsoft product present on computer.
Controls: Master Kill Switch located on the outside of the outer case. Cuts power to
all systems, including computer and electronics.
Hazard Number 35:
Wire connection from laptop to apparatus becomes severed or exposed to
environment.
Description: Exposed electrical wires with active voltage source, toxic chemical
exposure to cabin of aircraft.
Cause: Epoxy covering holes for wire feeds comes loose, possibly from excessive
structural loads, disconnection of inner and outer case.
Controls: Power to all electronic equipment will be shut down if there are exposed
wires until the problem is remedied. Inner and outer cases are firmly bolted to each
other, ensuring wire connections will be maintained under all g-load specifications.
Hazard Number 38:
Opening of lid during flight may expose toxic chemicals to cabin environment.
Description: Exposure of toxic chemicals to the cabin of the aircraft.
Cause: Intentional opening of inner and outer case lids to fix problems that can't be
resolved with only gloves.
Controls: Permission will be asked before opening, lids will not be opened during
periods of reduced gravity, only during periods of 1-2 g's.
Hazard Number 39:
Handle on inner lid comes unloose.
Description: Free-floating handle in cabin poses risk of injury.
Cause: Poor lid handle attachment, excessive structural load applied by g-forces or
team member or other persons operating the equipment.
Controls: All bolts connecting handles to the inner and outer case lids can
withstand all g-load specifications and are reinforced by four other bolts.
Hazard Number 40:
Protective outer device (POD) for each cell may structurally fail.
Description: Release of breakable glass components / toxic chemicals into the
inside of the inner box.
Cause: Aluminum or Velcro or foam failure of the POD design from excessive
structural loads, user mishandling, abuse, external loading.
Controls: Four sides of a POD consist of aluminum that can resist considerable
amounts of structural loading. All Velcro components are new, with maximum
adhesive qualities. Foam maintains soft intermediate between fragile glass
components of the cell and any external pieces. User will be careful when handling
individual PODs. Only one POD will be handled at a time.
Hazard Number 41:
Clamping mechanism to the zypette fails, comes loose.
Description: Fragile glass components may free-float in inner case, potential for
shattering, and danger for user.
Cause: Loosening of clamping mechanism from external forces, possible by a
team member. Excessive loading. Excessive torque applied by the linear actuator.
Clamping mechanism itself may crush the zypette.
Controls: Zypette is securely fastened to two ring stands in two places. Clamping
mechanism is designed to withstand all g-load specifications. Clamping
mechanism may need to use cloth or double-sided sticky adhesive between the
clamp and the zypette to reduce the possibility of inwards crushing.
Hazard Number 42:
Clamping mechanism to the micro-T may fail.
Description: Fragile glass components may free-float in inner case, potential for
shattering, and danger for user.
Cause: Loosening of clamping mechanism from external forces, possible by a
team member.Excessive loading. Excessive torque applied by the linear actuator.
Clamping mechanism itself may crush the micro-T.
Controls: Clamps are strong enough to dissipate possible torque created by the
linear actuator, but not strong enough to crush the micro-T. All clamping of
glassware will be carefully constructed and tested prior to each flight.
Hazard Number 43:
Laceration of team member with sharp object.
Description: Team member needs medical attention, bleeding, etc.
Cause: Excessive structural loading, broken apparatus inside inner case, cuts
through gloves and team member's skin.
Controls: All materials inside inner case are designed to withstand all g-load
specifications without breaking, two layers of gloves are used, first-aid medical kit
is present onboard for any necessary medical attention.
Hazard Number 44:
Edges of outer case injure team members.
Description: Bruising, external/internal bleeding, broken bones.
Cause: Person cuts or falls onto the outer case. Edges may cut or bruise person
who is not careful and is near the outer case when the KC-135A enters 2-g from
reduced gravity.
Controls: Outer edges of outer case have foam duct-taped to each edge,
eliminating exposure to any sharp corners. First-aid kit is readily available for
anyone who needs medical attention.
16. Tool Requirements
All tools used will be for ground maintenance and will be contained in a composite
tool kit with Styrofoam cutouts for ease of inventory evaluation. All tools will be
marked with the initials UW for identification. This should provide a quick means of
discovering missing tools and minimize the risk of tools causing foreign object
damage (FOD) to aircraft. In addition, all aluminum foil, paper, and plastic sheet
products will be closely tracked to prevent any FOD to aircraft. The following tools
will be brought.
1. Standard flathead and Phillips screwdriver
2. (1) roll duct tape
3. (1) roll of resin core solder
4. Soldering iron
5. Needle nose pliers
6. (2) packs of epoxy
7. (2) tubes of gasket compound
8. Crescent wrench
9. Electric screwdriver/drill kit
10. Spare bolts, washers, and nuts for equipment

The following materials and equipment are part of the experiment apparatus.
1. 1/4" Drilled polycarbonate sheets
2. (2) Micro-T connectors (manufactured by UW Chemistry Department Glass
Shop)
3. (2) 5mL zypettes (zero-gravity syringe-pipettes, manufactured UW Chemistry
Department Glass Shop)
4. (2) 25-lb. 24VDC Actuators
5. (4) Steel Luer-lock needles (1/16" diameter)
6. (36) Alcogel syringe-molds (including glass plates, rubber O-rings, and syringes)
7. (20) 1/4" Drilled aluminum L-beams
8. (2) Pairs of drybox gloves, butyl and neoprene
9. (4) 6.0V 40mW Laser diodes
10. (4) Hinges for inner and outer casing lids
11. (2) Drilled ring stands
12. Laptop computer
13. Electronic interface for computer and apparatus
14. 24VDC power supply
15. 17. Photo Requirements
We will be using a journalist to take photographs and videotape of the experiment.
We will not require the usage of S-band downlink. Our journalist will use a MiniDV
camcorder to record video for the National Geographic Channel. We will be using a
Panasonic MiniDV camcorder to record our experiment. We will require camera-
mounting poles for the camcorder. In addition to bringing a MiniDV camcorder to
record our experiment, we will also bring our own 35mm camera.
18. Aircraft Loading
We will be using a forklift to carry the inner and outer casing and all equipment up
to the KC. After the forklift reaches the level of the entrance to the aircraft, two
people will be needed to carry the inner and outer casings and equipment aboard
the aircraft.
There will be 2 handles on either side of the two boxes so that the 4 people can lift
the boxes and equipment aboard the KC. The inner casing, outer casing, and
equipment in the boxes weigh less than 200 pounds. Shoring for the floor is
requested for the apparatus The boxes will contain the equipment that will be
brought aboard the KC for the experiment.
Note: See Procedures for detailed information about the loading process.
Table 18-1: Weight Table
Item Weight of Items
Laser Diodes and Electronics 0.5 lbs.
Glassware (not including molds) 0.5 lbs.
Actuator 1 lb. Camcorders (2) 6 lbs.
Ring Stands 4 lbs.
Spare Parts 1 lb.
Laptop Computer 5 lbs.
Inner Encasement 80 lbs.
Outer Encasement 80 lbs.
Molds (filled) 4 lbs.
Tool Kit 5 lbs.
Total Weight: 187 lbs.
Note: See Equipment Description section for pictures of the items described in
the weight table above.
19. Ground Support Requirements
Power Requirements:
Standard 120 VAC 60 Hz power is required for testing pipetting apparatus,
computer and sensor interfaces.
Hazardous Substance Requirements:
Storage for 15.1 M ammonium hydroxide, denatured ethanol, tetramethoxysilane,
and tetraethoxysilane is needed. Space to mix the chemicals is required, but no
ventilation is needed. Beakers, stirring rods, and bottles for storing the solutions in
will be brought by the researchers.
Access to Building 993 During Non-business Hours:
Access to Building 993 is not requested during non-business hours.
Pressurized Gas Requirements:
No pressurized gas requirements. Our project will not require the use of any
pressurized gas.
General Tool Requests:
No general tool requests.
20. Hazardous Materials
The experiment uses two liquids that both contain hazardous materials. The liquids
are both triple-contained within the equipment, and all materials used to build the
equipment are chemical resistant.
Catalyst Solution
Contains: water, ethanol, 15.1 M ammonium hydroxide
Hazard: toxic, corrosive, releases pungent odor Containment: Stored in Mylar
bags, handled within double-walled polycarbonate box, used in dilute solution, only
used in liquid-tight system
Base Solution
Contains: water, ethanol, tetramethoxysilane or tetraethoxysilane, 15.1 M
ammonium hydroxide
Hazard: toxic, lachrymator, targets organs, lungs, blood, kidneys
Containment: Stored in sealed glass molds in double-walled polycarbonate box,
becomes safe once gel is formed
21. Material Safety Data Sheets
Material Safety Data Sheet for 15.1 M Aqueous Ammonium Hydroxide
Solution
Valid 05/2001 - 07/2001
Riedel-de Haen
3050 Spruce St. St. Louis, MO 63178 USA Tel: 314-289-6000
MATERIALSAFETYDATASHEET
SECTION 1. - - - - - - - - - CHEMICAL IDENTIFICATION- - - - - - - - - -
CATALOG #: 05002
NAME: AMMONIA SOLUTION MAX. 33% NH3, EXTRA PURE
SECTION 2. - - - - - COMPOSITION/INFORMATION ON INGREDIENTS - - - - - -
CAS #: 1336-21-6
EC NO: 215-647-6
SYNONYMS
AMMONIA AQUEOUS * AMMONIA WATER 29% * AQUA AMMONIA *
SECTION 3. - - - - - - - - - - HAZARDS IDENTIFICATION - - - - - - - - -
LABEL PRECAUTIONARY STATEMENTS CORROSIVE DANGEROUS FOR THE
ENVIRONMENT TOXIC IF SWALLOWED. LACHRYMATOR.
IN CASE OF ACCIDENT OR IF YOU FEEL UNWELL, SEEK MEDICAL ADVICE
IMMEDIATELY (SHOW THE LABEL WHERE POSSIBLE).
IN CASE OF CONTACT WITH EYES, RINSE IMMEDIATELY WITH PLENTY OF
WATER AND SEEK MEDICAL ADVICE.
WEAR SUITABLE PROTECTIVE CLOTHING, GLOVES AND EYE/FACE
PROTECTION.
AVOID RELEASE TO THE ENVIRONMENT. REFER TO SPECIAL
INSTRUCTIONS/
SAFETY DATA SHEETS.
SECTION 4. - - - - - - - - - - FIRST-AID MEASURES- - - - - - - - - - -
IF SWALLOWED, WASH OUT MOUTH WITH WATER PROVIDED PERSON IS
CONSCIOUS.
CALL A PHYSICIAN.
DO NOT INDUCE VOMITING.
IF INHALED, REMOVE TO FRESH AIR. IF NOT BREATHING GIVE ARTIFICIAL
RESPIRATION. IF BREATHING IS DIFFICULT, GIVE OXYGEN.
IN CASE OF SKIN CONTACT, FLUSH WITH COPIOUS AMOUNTS OF WATER
FOR AT LEAST 15 MINUTES. REMOVE CONTAMINATED CLOTHING AND
SHOES. CALL A PHYSICIAN.
IN CASE OF CONTACT WITH EYES, FLUSH WITH COPIOUS AMOUNTS OF
WATER FOR AT LEAST 15 MINUTES. ASSURE ADEQUATE FLUSHING BY
SEPARATING
THE EYELIDS WITH FINGERS. CALL A PHYSICIAN.
SECTION 5. - - - - - - - - - FIRE FIGHTING MEASURES - - - - - - - - - -
EXTINGUISHING MEDIA NONCOMBUSTIBLE. USE EXTINGUISHING MEDIA
APPROPRIATE TO SURROUNDING FIRE CONDITIONS.
SPECIAL FIREFIGHTING PROCEDURES WEAR SELF-CONTAINED
BREATHING APPARATUS AND PROTECTIVE CLOTHING TO
PREVENT CONTACT WITH SKIN AND EYES.
UNUSUAL FIRE AND EXPLOSIONS HAZARDS EMITS TOXIC FUMES UNDER
FIRE CONDITIONS.
SECTION 6. - - - - - - - - ACCIDENTAL RELEASE MEASURES- - - - - - - - -
WEAR SELF-CONTAINED BREATHING APPARATUS, RUBBER BOOTS AND
HEAVY RUBBER GLOVES.
COVER WITH DRY LIME OR SODA ASH, PICK UP, KEEP IN A CLOSED
CONTAINER AND HOLD FOR WASTE DISPOSAL.
VENTILATE AREA AND WASH SPILL SITE AFTER MATERIAL PICKUP IS
COMPLETE.
EVACUATE AREA.
SECTION 7. - - - - - - - - - - HANDLING AND STORAGE- - - - - - - - - - -
REFER TO SECTION 8.
SECTION 8. - - - - - - EXPOSURE CONTROLS/PERSONAL PROTECTION- - - - -
SAFETY SHOWER AND EYE BATH.
USE ONLY IN A CHEMICAL FUME HOOD.
WASH CONTAMINATED CLOTHING BEFORE REUSE.
DISCARD CONTAMINATED SHOES.
WASH THOROUGHLY AFTER HANDLING.
DO NOT BREATHE VAPOR.
DO NOT GET IN EYES, ON SKIN, ON CLOTHING.
AVOID PROLONGED OR REPEATED EXPOSURE.
NIOSH/MSHA-APPROVED RESPIRATOR.
COMPATIBLE CHEMICAL-RESISTANT GLOVES.
CHEMICAL SAFETY GOGGLES.
FACESHIELD (8-INCH MINIMUM).
KEEP TIGHTLY CLOSED.
STORE IN A COOL DRY PLACE.
REFRIGERATE BEFORE OPENING.
SECTION 9. - - - - - - - PHYSICAL AND CHEMICAL PROPERTIES - - - - - - -
PHYSICAL PROPERTIES
MELTING POINT: -77 C
EXPLOSION LIMITS IN AIR:
UPPER 27 %
LOWER 16 %
VAPOR PRESSURE: 115 MMHG
SPECIFIC GRAVITY: 0.9 G
VAPOR DENSITY: 1.2 G/L
SECTION 10. - - - - - - - - -STABILITY AND REACTIVITY - - - - - - - - -
STABILITY
STABLE.
INCOMPATIBILITIES
COPPER, COPPER ALLOYS
GALVANIZED IRON
ZINC
HAZARDOUS COMBUSTION OR DECOMPOSITION PRODUCTS
AMMONIA
HAZARDOUS POLYMERIZATION
WILL NOT OCCUR.
SECTION 11. - - - - - - - - - TOXICOLOGICAL INFORMATION - - - - - - - -
ACUTE EFFECTS
MATERIAL IS EXTREMELY DESTRUCTIVE TO TISSUE OF THE MUCOUS
MEMBRANES
AND UPPER RESPIRATORY TRACT, EYES AND SKIN.
INHALATION MAY RESULT IN SPASM, INFLAMMATION AND EDEMA OF THE
LARYNX AND BRONCHI, CHEMICAL PNEUMONITIS AND PULMONARY
EDEMA.
SYMPTOMS OF EXPOSURE MAY INCLUDE BURNING SENSATION,
COUGHING,
WHEEZING, LARYNGITIS, SHORTNESS OF BREATH, HEADACHE, NAUSEA
AND VOMITING.
CAUSES BURNS.
MAY BE HARMFUL IF ABSORBED THROUGH THE SKIN.
LACHRYMATOR.
MAY BE HARMFUL IF INHALED.
MATERIAL IS EXTREMELY DESTRUCTIVE TO THE TISSUE OF THE MUCOUS
MEMBRANES
AND UPPER RESPIRATORY TRACT.
HARMFUL IF SWALLOWED.
RTECS #: BQ9625000
AMMONIUM HYDROXIDE
IRRITATION DATA
EYE-RBT 250 UG SEV AJOPAA 29,1363,1946
EYE-RBT 44 UG SEV AROPAW 25,839,1941
EYE-RBT 1 MG/30S RINSE SEV TXCYAC 23,281,1982
TOXICITY DATA
ORL-HMN LDLO:43 MG/KG 34ZIAG -,95,1969
IHL-HMN LCLO:5000 PPM 34ZIAG -,95,1969
ORL-RAT LD50:350 MG/KG JIHTAB 23,259,1941
IVN-MUS LD50:91 MG/KG JCINAO 37,497,1958
TARGET ORGAN DATA
BEHAVIORAL (CONVULSIONS OR EFFECT ON SEIZURE THRESHOLD)
BEHAVIORAL (COMA)
LUNGS, THORAX OR RESPIRATION (FIBROSIS, FOCAL)
LUNGS, THORAX OR RESPIRATION (ACUTE PULMONARY EDEMA)
LUNGS, THORAX OR RESPIRATION (RESPIRATORY STIMULATION)
GASTROINTESTINAL (OTHER CHANGES)
LIVER (OTHER CHANGES)
KIDNEY, URETER, BLADDER (OTHER CHANGES)
ONLY SELECTED REGISTRY OF TOXIC EFFECTS OF CHEMICAL
SUBSTANCES
(RTECS) DATA IS PRESENTED HERE. SEE ACTUAL ENTRY IN RTECS FOR
COMPLETE INFORMATION.
SECTION 12. - - - - - - - - - ECOLOGICAL INFORMATION - - - - - - - - - -
DATA NOT YET AVAILABLE.
SECTION 13. - - - - - - - - - DISPOSAL CONSIDERATIONS - - - - - - - - -
CONTACT A LICENSED PROFESSIONAL WASTE DISPOSAL SERVICE TO
DISPOSE OF THIS MATERIAL.
DISSOLVE OR MIX THE MATERIAL WITH A COMBUSTIBLE SOLVENT AND
BURN IN A
CHEMICAL INCINERATOR EQUIPPED WITH AN AFTERBURNER AND
SCRUBBER.
OBSERVE ALL FEDERAL, STATE AND LOCAL ENVIRONMENTAL
REGULATIONS.
SECTION 14. - - - - - - - - - - TRANSPORT INFORMATION - - - - - - - - -
CONTACT SIGMA CHEMICAL COMPANY FOR TRANSPORTATION
INFORMATION.
SECTION 15. - - - - - - - - - REGULATORY INFORMATION - - - - - - - - - -
EUROPEAN INFORMATION
EC INDEX NO: 007-001-01-2
CORROSIVE DANGEROUS FOR THE ENVIRONMENT
R 34
CAUSES BURNS.
R 50
VERY TOXIC TO AQUATIC ORGANISMS.
S 26
IN CASE OF CONTACT WITH EYES, RINSE IMMEDIATELY WITH PLENTY OF
WATER AND SEEK MEDICAL ADVICE.
S 36/37/39
WEAR SUITABLE PROTECTIVE CLOTHING, GLOVES AND EYE/FACE
PROTECTION.
S 45
IN CASE OF ACCIDENT OR IF YOU FEEL UNWELL, SEEK MEDICAL ADVICE
IMMEDIATELY (SHOW THE LABEL WHERE POSSIBLE).
S 61
AVOID RELEASE TO THE ENVIRONMENT. REFER TO SPECIAL
INSTRUCTIONS/
SAFETY DATA SHEETS.
REVIEWS, STANDARDS, AND REGULATIONS
OEL=MAK
NOHS 1974: HZD 06145; NIS 297; TNF 85664; NOS 161; TNE 735671
NOES 1983: HZD 06145; NIS 326; TNF 66188; NOS 188; TNE 1022551; TFE
379643
EPA TSCA SECTION 8(B) CHEMICAL INVENTORY
EPA TSCA SECTION 8(D) UNPUBLISHED HEALTH/SAFETY STUDIES
EPA TSCA TEST SUBMISSION (TSCATS) DATA BASE, JANUARY 2001
SECTION 16. - - - - - - - - - - OTHER INFORMATION- - - - - - - - - - - -
THE ABOVE INFORMATION IS BELIEVED TO BE CORRECT BUT DOES NOT
PURPORT TO
BE ALL INCLUSIVE AND SHALL BE USED ONLY AS A GUIDE. SIGMA,
ALDRICH,
FLUKA SHALL NOT BE HELD LIABLE FOR ANY DAMAGE RESULTING FROM
HANDLING OR FROM CONTACT WITH THE ABOVE PRODUCT. SEE
REVERSE SIDE OF INVOICE OR PACKING SLIP FOR ADDITIONAL TERMS
AND CONDITIONS OF SALE.
COPYRIGHT 2001 SIGMA-ALDRICH CO.
LICENSE GRANTED TO MAKE UNLIMITED PAPER COPIES FOR INTERNAL
USE ONLY
Material Safety Data Sheet for Ethanol, Denatured with 4.8% IPA
Valid 05/2001 - 07/2001
Fluka Chemical Corp. 1001 West St. Paul Milwaukee, WI 53233 USA
Tel: 414-273-3850
MATERIALSAFETYDATASHEET
SECTION 1. - - - - - - - CHEMICAL IDENTIFICATION- - - - - CATALOG #: 02853
NAME: ETHANOL, DENAT. WITH 4.8% ISOPROPANOL, 'F
25 IPA'
SECTION 2. - - - - - COMPOSITION/INFORMATION ON INGREDIENTS - - - - - -
CAS #: 64-17-5
EC NO: 200-578-6
HAZARDOUS INGREDIENTS
CONTAINS 2-PROPANOL (ISOPROPYL ALCOHOL), CHEMICAL ABSTRACTS
REGISTRY NUMBER 67-63-0.
SYNONYMS
ABSOLUTE ETHANOL * AETHANOL (GERMAN) * AETHYLALKOHOL
(GERMAN) *
ALCOHOL * ALCOHOL, ANHYDROUS * ALCOHOL DEHYDRATED * ALCOOL
ETHYLIQUE
(FRENCH) * ALCOOL ETILICO (ITALIAN) * ALGRAIN * ALKOHOL (GERMAN) *
ALKOHOLU ETYLOWEGO (POLISH) * ANHYDROL * COLOGNE SPIRIT *
ETANOLO
(ITALIAN) * ETHANOL (ACGIH:OSHA) * ETHYL ALCOHOL (DOT:OSHA) *
ETHYL
ALCOHOL ANHYDROUS * ETHYL HYDRATE * ETHYL HYDROXIDE *
ETYLOWY ALKOHOL
(POLISH) * FERMENTATION ALCOHOL * GRAIN ALCOHOL * JAYSOL *
JAYSOL S *
METHYLCARBINOL * MOLASSES ALCOHOL * NCI-C03134 * POTATO
ALCOHOL * SD
ALCOHOL 23-HYDROGEN * SPIRITS OF WINE * SPIRT * TECSOL *
SECTION 3. - - - - - - - - HAZARDS IDENTIFICATION - - - - - - -
LABEL PRECAUTIONARY STATEMENTS
FLAMMABLE (USA)
HIGHLY FLAMMABLE (EU)
IRRITANT
IRRITATING TO EYES, RESPIRATORY SYSTEM AND SKIN.
RISK OF SERIOUS DAMAGE TO EYES.
TARGET ORGAN(S):
NERVES
LIVER
KEEP AWAY FROM SOURCES OF IGNITION - NO SMOKING.
IN CASE OF CONTACT WITH EYES, RINSE IMMEDIATELY WITH PLENTY OF
WATER AND SEEK MEDICAL ADVICE.
WEAR SUITABLE PROTECTIVE CLOTHING.
SECTION 4. - - - - - - - - - - FIRST-AID MEASURES- - - - - - - - - - -
IF INHALED, REMOVE TO FRESH AIR. IF BREATHING BECOMES DIFFICULT,
CALL A PHYSICIAN.IN CASE OF CONTACT WITH EYES, FLUSH WITH
COPIOUS AMOUNTS OF WATER FOR AT LEAST 15 MINUTES. ASSURE
ADEQUATE FLUSHING BY SEPARATING THE EYELIDS WITH FINGERS. CALL
A PHYSICIAN.IF SWALLOWED, WASH OUT MOUTH WITH WATER PROVIDED
PERSON IS CONSCIOUS.
CALL A PHYSICIAN IMMEDIATELY.
IN CASE OF SKIN CONTACT, FLUSH WITH COPIOUS AMOUNTS OF WATER
FOR AT LEAST 15 MINUTES. REMOVE CONTAMINATED CLOTHING AND
SHOES. CALL A PHYSICIAN.
WASH CONTAMINATED CLOTHING BEFORE REUSE.
SECTION 5. - - - - - - - - - FIRE FIGHTING MEASURES - - - - - - - - - -
EXTINGUISHING MEDIA CARBON DIOXIDE, DRY CHEMICAL POWDER OR
APPROPRIATE FOAM.
SPECIAL FIREFIGHTING PROCEDURES
WEAR SELF-CONTAINED BREATHING APPARATUS AND PROTECTIVE
CLOTHING TO
PREVENT CONTACT WITH SKIN AND EYES.
USE WATER SPRAY TO COOL FIRE-EXPOSED CONTAINERS.
FLAMMABLE LIQUID.
UNUSUAL FIRE AND EXPLOSIONS HAZARDS
VAPOR MAY TRAVEL CONSIDERABLE DISTANCE TO SOURCE OF IGNITION
AND
FLASH BACK.
SECTION 6. - - - - - - - - ACCIDENTAL RELEASE MEASURES- - - - - - - - -
EVACUATE AREA.
SHUT OFF ALL SOURCES OF IGNITION.
WEAR SELF-CONTAINED BREATHING APPARATUS, RUBBER BOOTS AND
HEAVY RUBBER GLOVES.COVER WITH DRY-LIME, SAND, OR SODA ASH.
PLACE IN COVERED CONTAINERS USING NON-SPARKING TOOLS AND
TRANSPORT OUTDOORS.
VENTILATE AREA AND WASH SPILL SITE AFTER MATERIAL PICKUP IS
COMPLETE.
SECTION 7. - - - - - - - - - - HANDLING AND STORAGE- - - - - - - - - - -
REFER TO SECTION 8.
SECTION 8. - - - - - - EXPOSURE CONTROLS/PERSONAL PROTECTION- - - - -
-
WEAR APPROPRIATE NIOSH/MSHA-APPROVED RESPIRATOR, CHEMICAL-
RESISTANT GLOVES, SAFETY GOGGLES, OTHER PROTECTIVE CLOTHING.
USE ONLY IN A CHEMICAL FUME HOOD.
SAFETY SHOWER AND EYE BATH.
DO NOT BREATHE VAPOR.
DO NOT GET IN EYES, ON SKIN, ON CLOTHING.
AVOID PROLONGED OR REPEATED EXPOSURE.
WASH THOROUGHLY AFTER HANDLING.
KEEP TIGHTLY CLOSED.
KEEP AWAY FROM HEAT, SPARKS, AND OPEN FLAME.
STORE IN A COOL DRY PLACE.
SECTION 9. - - - - - - - PHYSICAL AND CHEMICAL PROPERTIES - - - - - - -
APPEARANCE AND ODOR
CLEAR, COLORLESS LIQUID
SECTION 10. - - - - - - - - -STABILITY AND REACTIVITY - - - - - - - - -
STABILITY
STABLE.
INCOMPATIBILITIES
OXIDIZING AGENTS
PEROXIDES
ACIDS
ACID CHLORIDES
ACID ANHYDRIDES
ALKALI METALS
AMMONIA
PROTECT FROM MOISTURE.
HAZARDOUS COMBUSTION OR DECOMPOSITION PRODUCTS
TOXIC FUMES OF:
CARBON MONOXIDE, CARBON DIOXIDE
HAZARDOUS POLYMERIZATION
WILL NOT OCCUR.
SECTION 11. - - - - - - - - - TOXICOLOGICAL INFORMATION - - - - - - - -
ACUTE EFFECTS
MAY BE HARMFUL BY INHALATION, INGESTION, OR SKIN ABSORPTION.
CAUSES SEVERE EYE IRRITATION.
VAPOR OR MIST IS IRRITATING TO THE EYES, MUCOUS MEMBRANES AND
UPPER
RESPIRATORY TRACT.
CAUSES SKIN IRRITATION.
CAN CAUSE CNS DEPRESSION.
EXPOSURE CAN CAUSE:
NAUSEA, HEADACHE AND VOMITING
NARCOTIC EFFECT
DAMAGE TO THE HEART
TARGET ORGAN(S):
NERVES
LIVER
KIDNEYS
CARDIOVASCULAR SYSTEM
G.I. SYSTEM
RTECS #: KQ6300000
ETHYL ALCOHOL
IRRITATION DATA
SKN-RBT 400 MG OPEN MLD UCDS** 7/22/1970
SKN-RBT 20 MG/24H MOD 85JCAE -,189,1986
EYE-RBT 500 MG SEV AJOPAA 29,1363,1946
EYE-RBT 500 MG/24H MLD 85JCAE -,189,1986
EYE-RBT 100 MG/4S RINSE MOD FCTOD7 20,573,1982
TOXICITY DATA
ORL-CHD LDLO:2 GM/KG ATXKA8 17,183,1958
ORL-HMN LDLO:1400 MG/KG NPIRI* 1,44,1974
SCU-INF LDLO:19440 MG/KG AJCPAI 5,466,1935
ORL-RAT LD50:7060 MG/KG TXAPA9 16,718,1970
IHL-RAT LC50:20000 PPM/10H NPIRI* 1,44,1974
IPR-RAT LD50:3600 UG/KG PHMGBN 2,27,1969
IVN-RAT LD50:1440 MG/KG TXAPA9 18,60,1971
IAT-RAT LD50:11 MG/KG TXAPA9 18,60,1971
ORL-MUS LD50:3450 MG/KG GISAAA 32(3),31,1967
IHL-MUS LC50:39 GM/M3/4H GTPZAB 26(8),53,1982
IPR-MUS LD50:528 MG/KG STRAAA 127,245,1965
SCU-MUS LD50:8285 MG/KG FAONAU 48A,99,1970
IVN-MUS LD50:1973 MG/KG HBTXAC 1,128,1955
ORL-RBT LD50:6300 MG/KG HBTXAC 1,130,1955
IPR-RBT LD50:963 MG/KG EVHPAZ 61,321,1985
IVN-RBT LD50:2374 MG/KG EVHPAZ 61,321,1985
ORL-GPG LD50:5560 MG/KG JIHTAB 23,259,1941
IPR-GPG LD50:3414 MG/KG EVHPAZ 61,321,1985
IPR-HAM LD50:5068 MG/KG EVHPAZ 61,321,1985
IPR-MAM LD50:4300 MG/KG TXAPA9 13,358,1968
TARGET ORGAN DATA
BEHAVIORAL (SLEEP)
BEHAVIORAL (CHANGE IN MOTOR ACTIVITY)
BEHAVIORAL (ATAXIA)
BEHAVIORAL (ANTIPSYCHOTIC)
BEHAVIORAL (HEADACHE)
BEHAVIORAL (CHANGE IN PSYCHOPHYSIOLOGICAL TESTS)
LUNGS, THORAX OR RESPIRATION (CHRONIC PULMONARY EDEMA OR
CONGESTION)
LUNGS, THORAX OR RESPIRATION (DYSPNAE)
LUNGS, THORAX OR RESPIRATION (OTHER CHANGES)
GASTROINTESTINAL (ALTERATION IN GASTRIC SECRETION)
GASTROINTESTINAL (HYPERMOTILITY, DIARRHEA)
GASTROINTESTINAL (NAUSEA OR VOMITING)
GASTROINTESTINAL (OTHER CHANGES)
LIVER (FATTY LIVER DEGENERATION)
LIVER (TUMORS)
ENDOCRINE (CHANGE IN GONADOTROPINS)
ENDOCRINE (OTHER CHANGES)
BLOOD (OTHER CHANGES)
BLOOD (LYMPHOMA INCLUDING HODGKIN'S DISEASE)
PATERNAL EFFECTS (TESTES, EPIDIDYMIS, SPERM DUCT)
EFFECTS ON FERTILITY (FEMALE FERTILITY INDEX)
EFFECTS ON FERTILITY (MALE FERTILITY INDEX)
EFFECTS ON FERTILITY (POST-IMPLANTATION MORTALITY)
EFFECTS ON FERTILITY (OTHER MEASURES OF FERTILITY)
EFFECTS ON EMBRYO OR FETUS (EXTRA EMBRYONIC STRUCTURES)
EFFECTS ON EMBRYO OR FETUS (CYTOLOGICAL CHANGES)
EFFECTS ON EMBRYO OR FETUS (FETOTOXICITY)
EFFECTS ON EMBRYO OR FETUS (FETAL DEATH)
EFFECTS ON EMBRYO OR FETUS (OTHER EFFECTS TO EMBYRO OR
FETUS)
SPECIFIC DEVELOPMENTAL ABNORMALITIES (EYE, EAR)
SPECIFIC DEVELOPMENTAL ABNORMALITIES (CRANIOFACIAL)
SPECIFIC DEVELOPMENTAL ABNORMALITIES (MUSCULOSKELETAL
SYSTEM)
SPECIFIC DEVELOPMENTAL ABNORMALITIES (RESPIRATORY SYSTEM)
EFFECTS ON NEWBORN (GROWTH STATISTICS)
TUMORIGENIC (EQUIVOCAL TUMORIGENIC AGENT BY RTECS CRITERIA)
ONLY SELECTED REGISTRY OF TOXIC EFFECTS OF CHEMICAL
SUBSTANCES
(RTECS) DATA IS PRESENTED HERE. SEE ACTUAL ENTRY IN RTECS FOR
COMPLETE INFORMATION.
SECTION 12. - - - - - - - - - ECOLOGICAL INFORMATION - - - - - - - - - -
DATA NOT YET AVAILABLE.
SECTION 13. - - - - - - - - - DISPOSAL CONSIDERATIONS - - - - - - - - -
BURN IN A CHEMICAL INCINERATOR EQUIPPED WITH AN AFTERBURNER
AND
SCRUBBER BUT EXERT EXTRA CARE IN IGNITING AS THIS MATERIAL IS
HIGHLY
FLAMMABLE.
OBSERVE ALL FEDERAL, STATE AND LOCAL ENVIRONMENTAL
REGULATIONS.
SECTION 14. - - - - - - - - - - TRANSPORT INFORMATION - - - - - - - - -
CONTACT FLUKA CHEMICAL COMPANY FOR TRANSPORTATION
INFORMATION.
SECTION 15. - - - - - - - - - REGULATORY INFORMATION - - - - - - - - - -
EUROPEAN INFORMATION
EC INDEX NO: 603-002-00-5
HIGHLY FLAMMABLE
IRRITANT
R1
HIGHLY FLAMMABLE
R 36/37/38
IRRITATING TO EYES, RESPIRATORY SYSTEM AND SKIN.
R 41
RISK OF SERIOUS DAMAGE TO EYES.
S 16
KEEP AWAY FROM SOURCES OF IGNITION - NO SMOKING.
S 26
IN CASE OF CONTACT WITH EYES, RINSE IMMEDIATELY WITH PLENTY OF
WATER AND SEEK MEDICAL ADVICE.
S 36
WEAR SUITABLE PROTECTIVE CLOTHING.
TLV AND SOURCE
FOR 2-PROPANOL (ISOPROPYL ALCOHOL):
ACGIH TLV-TWA: 400 PPM (983 MG/M3); STEL: 500 PPM (1230 MG/M3).
OSHA PEL: 8H TWA: 400 PPM (983 MG/M3); STEL: 500 PPM (1225 MG/M3).
REVIEWS, STANDARDS, AND REGULATIONS
OEL=MAK
ACGIH TLV-NOT CLASSIFIABLE AS A HUMAN CARCINOGEN DTLVS*
TLV/BEI,1999
ACGIH TLV-TWA 1000 PPM DTLVS* TLV/BEI,1999
IARC CANCER REVIEW:ANIMAL INADEQUATE EVIDENCE IMEMDT 44,35,1988
EPA FIFRA 1988 PESTICIDE SUBJECT TO REGISTRATION OR RE-
REGISTRATION
FEREAC 54,7740,1989
MSHA STANDARD-AIR:TWA 1000 PPM (1900 MG/M3)
DTLVS* 3,103,1971
OSHA PEL (GEN INDU):8H TWA 1000 PPM (1900 MG/M3)
CFRGBR 29,1910.1000,1994
OSHA PEL (CONSTRUC):8H TWA 1000 PPM (1900 MG/M3)
CFRGBR 29,1926.55,1994
OSHA PEL (SHIPYARD):8H TWA 1000 PPM (1900 MG/M3)
CFRGBR 29,1915.1000,1993
OSHA PEL (FED CONT):8H TWA 1000 PPM (1900 MG/M3)
CFRGBR 41,50-204.50,1994
OEL-AUSTRALIA: TWA 1000 PPM (1900 MG/M3), JAN1993
OEL-AUSTRIA: MAK 1000 PPM (1900 MG/M3), JAN1999
OEL-BELGIUM: TWA 1000 PPM (1880 MG/M3), JAN1993
OEL-DENMARK: TWA 1000 PPM (1900 MG/M3), JAN1999
OEL-FINLAND: TWA 1000 PPM (1900 MG/M3), STEL 1250 PPM (2400 MG/M3),
JAN1999
OEL-FRANCE: VME 1000 PPM (1900 MG/M3), VLE 5000 PPM, JAN1999
OEL-GERMANY: MAK 1000 PPM (1900 MG/M3), JAN1999
OEL-HUNGARY: TWA 1000 MG/M3, STEL 3000 MG/M3, JAN1993
OEL-THE NETHERLANDS: MAC-TGG 500 PPM (950 MG/M3), JAN1999
OEL-NORWAY: TWA 500 PPM (950 MG/M3), JAN1999
OEL-THE PHILIPPINES: TWA 1000 PPM (1900 MG/M3), JAN1993
OEL-POLAND: MAC(TWA) 1000 MG/M3, MAC(STEL) 3000 MG/M3, JAN1999
OEL-RUSSIA: STEL 1000 MG/M3, JAN1993
OEL-SWEDEN: NGV 500 PPM (1000 MG/M3), KTV 1000PPM (1900 MG/M3),
JAN1999
OEL-SWITZERLAND: MAK-W 1000 PPM (1900 MG/M3), JAN1999
OEL-THAILAND: TWA 1000 PPM (1900 MG/M3), JAN1993
OEL-TURKEY: TWA 1000 PPM (1900 MG/M3), JAN1993
OEL-UNITED KINGDOM: TWA 1000 PPM (1950 MG/M3), SEP2000
OEL IN ARGENTINA, BULGARIA, COLOMBIA, JORDAN, KOREA CHECK ACGIH
TLV;
OEL IN NEW ZEALAND, SINGAPORE, VIETNAM CHECK ACGIH TLV
NIOSH REL TO ETHYL ALCOHOL-AIR:10H TWA 1000 PPM
NIOSH* DHHS #92-100,1992
NOHS 1974: HZD 31500; NIS 430; TNF 157709; NOS 242; TNE 2088926
NOES 1983: HZD 31500; NIS 334; TNF 86077; NOS 222; TNE 2069125; TFE
1014002
EPA GENETOX PROGRAM 1988, POSITIVE: RODENT DOMINANT LETHAL
EPA GENETOX PROGRAM 1988, NEGATIVE: ASPERGILLUS-FORWARD
MUTATION;
SHE-CLONAL ASSAY
EPA GENETOX PROGRAM 1988, NEGATIVE: CELL TRANSFORM.-RLV F344
RAT EMBRYO
EPA GENETOX PROGRAM 1988, NEGATIVE: IN VITRO CYTOGENETICS-
NONHUMAN;
MAMMALIAN MICRONUCLEUS
EPA GENETOX PROGRAM 1988, NEGATIVE: N CRASSA-ANEUPLOIDY;
HISTIDINE
REVERSION-AMES TEST
EPA GENETOX PROGRAM 1988, NEGATIVE: IN VITRO SCE-HUMAN
LYMPHOCYTES; IN
VITRO SCE-HUMAN
EPA GENETOX PROGRAM 1988, NEGATIVE: IN VITRO SCE-NONHUMAN;
SPERM
MORPHOLOGY-MOUSE
EPA GENETOX PROGRAM 1988, NEGATIVE/LIMITED: CARCINOGENICITY-
MOUSE/RAT
EPA TSCA SECTION 8(B) CHEMICAL INVENTORY
EPA TSCA SECTION 8(D) UNPUBLISHED HEALTH/SAFETY STUDIES
EPA TSCA TEST SUBMISSION (TSCATS) DATA BASE, JANUARY 2001
NIOSH ANALYTICAL METHOD, 1994: ETHANOL IN BLOOD, 8002
NIOSH ANALYTICAL METHOD, 1994: ALCOHOLS I, 1400
NTP CARCINOGENESIS STUDIES; ON TEST (TWO YEAR STUDIES),
OCTOBER 2000
SECTION 16. - - - - - - - - - - OTHER INFORMATION- - - - - - - - - - - -
THE ABOVE INFORMATION IS BELIEVED TO BE CORRECT BUT DOES NOT
PURPORT TO
BE ALL INCLUSIVE AND SHALL BE USED ONLY AS A GUIDE. SIGMA,
ALDRICH,
FLUKA SHALL NOT BE HELD LIABLE FOR ANY DAMAGE RESULTING FROM
HANDLING
OR FROM CONTACT WITH THE ABOVE PRODUCT. SEE REVERSE SIDE OF
INVOICE OR
PACKING SLIP FOR ADDITIONAL TERMS AND CONDITIONS OF SALE.
COPYRIGHT 2001 SIGMA-ALDRICH CO.
LICENSE GRANTED TO MAKE UNLIMITED PAPER COPIES FOR INTERNAL
USE ONLY
Easy PDF copyright (C) 1998,2000 Visage Software - http://www.visagesoft.com
This document was created with Easy PDF unregistered version
This stamp will be removed with registered version of Easy PDF
Material Safety Data Sheet for Iron Powder
Valid 05/2001 - 07/2001
Riedel-de Haen
3050 Spruce St.
St. Louis, MO 63178 USA
Tel: 314-289-6000
MATERIALSAFETYDATASHEET
SECTION 1. - - - - - - - - - CHEMICAL IDENTIFICATION- - - - - - - - - -
CATALOG #: 12311
NAME: IRON
SECTION 2. - - - - - COMPOSITION/INFORMATION ON INGREDIENTS - - - - - -
CAS #:NONE
EC NO: 231-096-4
SYNONYMS
ANCOR EN 80/150 * ARMCO IRON * CARBONYL IRON * COPY POWDER CS
105-175
* DISEASES, IRON OVERLOAD * EFV 250/400 * EO 5A * FEROVAC E * GS 6 *
IRON FULLERIDE (FEC2O) * LOHA * MICROPOWDER R 2430 * NC 100 *
PZH2M *
PZHO * REMKO * SUY-B 2 * 3ZHP *
SECTION 3. - - - - - - - - - - HAZARDS IDENTIFICATION - - - - - - - - -
LABEL PRECAUTIONARY STATEMENTS
FLAMMABLE (USA)
HIGHLY FLAMMABLE (EU)
TOXIC
TOXIC IF SWALLOWED.
IRRITATING TO EYES.
TARGET ORGAN(S):
LIVER
G.I. SYSTEM
KEEP AWAY FROM SOURCES OF IGNITION - NO SMOKING.
IN CASE OF ACCIDENT OR IF YOU FEEL UNWELL, SEEK MEDICAL ADVICE
IMMEDIATELY (SHOW THE LABEL WHERE POSSIBLE).
IN CASE OF CONTACT WITH EYES, RINSE IMMEDIATELY WITH PLENTY OF
WATER AND SEEK MEDICAL ADVICE.
WEAR SUITABLE PROTECTIVE CLOTHING, GLOVES AND EYE/FACE
PROTECTION.
SECTION 4. - - - - - - - - - - FIRST-AID MEASURES- - - - - - - - - - -
IF SWALLOWED, WASH OUT MOUTH WITH WATER PROVIDED PERSON IS
CONSCIOUS.
CALL A PHYSICIAN IMMEDIATELY.
IF INHALED, REMOVE TO FRESH AIR. IF NOT BREATHING GIVE ARTIFICIAL
RESPIRATION. IF BREATHING IS DIFFICULT, GIVE OXYGEN.
IN CASE OF SKIN CONTACT, FLUSH WITH COPIOUS AMOUNTS OF WATER
FOR AT LEAST 15 MINUTES. REMOVE CONTAMINATED CLOTHING AND
SHOES. CALL A PHYSICIAN.
IN CASE OF CONTACT WITH EYES, FLUSH WITH COPIOUS AMOUNTS OF
WATER
FOR AT LEAST 15 MINUTES. ASSURE ADEQUATE FLUSHING BY
SEPARATING
THE EYELIDS WITH FINGERS. CALL A PHYSICIAN.
SECTION 5. - - - - - - - - - FIRE FIGHTING MEASURES - - - - - - - - - -
EXTINGUISHING MEDIA
WATER SPRAY.
CARBON DIOXIDE, DRY CHEMICAL POWDER OR APPROPRIATE FOAM.
SPECIAL FIREFIGHTING PROCEDURES
WEAR SELF-CONTAINED BREATHING APPARATUS AND PROTECTIVE
CLOTHING TO
PREVENT CONTACT WITH SKIN AND EYES.
UNUSUAL FIRE AND EXPLOSIONS HAZARDS
EMITS TOXIC FUMES UNDER FIRE CONDITIONS.
THIS MATERIAL, LIKE MOST MATERIALS IN POWDER FORM, IS CAPABLE OF
CREATING A DUST EXPLOSION.
SECTION 6. - - - - - - - - ACCIDENTAL RELEASE MEASURES- - - - - - - - -
WEAR SELF-CONTAINED BREATHING APPARATUS, RUBBER BOOTS AND
HEAVY
RUBBER GLOVES.
SWEEP UP, PLACE IN A BAG AND HOLD FOR WASTE DISPOSAL.
AVOID RAISING DUST.
VENTILATE AREA AND WASH SPILL SITE AFTER MATERIAL PICKUP IS
COMPLETE.
EVACUATE AREA.
USE NONSPARKING TOOLS.
SHUT OFF ALL SOURCES OF IGNITION.
SECTION 7. - - - - - - - - - - HANDLING AND STORAGE- - - - - - - - - - -
REFER TO SECTION 8.
SECTION 8. - - - - - - EXPOSURE CONTROLS/PERSONAL PROTECTION- - - - -
-
WASH CONTAMINATED CLOTHING BEFORE REUSE.
WASH THOROUGHLY AFTER HANDLING.
DO NOT BREATHE DUST.
DO NOT GET IN EYES, ON SKIN, ON CLOTHING.
AVOID PROLONGED OR REPEATED EXPOSURE.
NIOSH/MSHA-APPROVED RESPIRATOR. COMPATIBLE CHEMICAL-
RESISTANT GLOVES.
CHEMICAL SAFETY GOGGLES.
SAFETY SHOWER AND EYE BATH.
USE NONSPARKING TOOLS.
MECHANICAL EXHAUST REQUIRED.
KEEP TIGHTLY CLOSED.
KEEP AWAY FROM HEAT, SPARKS, AND OPEN FLAME.
STORE IN A COOL DRY PLACE.
STORE UNDER N2.
SECTION 9. - - - - - - - PHYSICAL AND CHEMICAL PROPERTIES - - - - - - -
APPEARANCE AND ODOR
SOLID.
PHYSICAL PROPERTIES
SPECIFIC GRAVITY: 7.86
SECTION 10. - - - - - - - - -STABILITY AND REACTIVITY - - - - - - - - -
STABILITY
STABLE.
INCOMPATIBILITIES
REACTS VIOLENTLY WITH:
HALOGENS
PHOSPHORUS
PROTECT FROM MOISTURE.
ACIDS
OXYGEN
STRONG OXIDIZING AGENTS
HAZARDOUS COMBUSTION OR DECOMPOSITION PRODUCTS
IRON OXIDES
HAZARDOUS POLYMERIZATION WILL NOT OCCUR.
SECTION 11 - - TOXICOLOGICAL INFORMATION - -
ACUTE EFFECTS
OVERDOSE OF IRON COMPOUNDS MAY HAVE A CORROSIVE EFFECT ON
THE GASTROINTESTINAL MUCOSA AND BE FOLLOWED BY NECROSIS,
PERFORATION AND STRICTURE FORMATION. SEVERAL HOURS MAY
ELAPSE BEFORE SYMPTOMS THAT CAN INCLUDE EPIGASTRIC PAIN,
DIARRHEA, VOMITING, NAUSEA AND HEMATEMESIS OCCUR. AFTER
APPARENT RECOVERY A PERSON MAY EXPERIENCE METABOLIC
ACIDOSIS, CONVULSIONS AND COMA HOURS OR DAYS LATER. FURTHER
COMPLICATIONS MAY DEVELOP LEADING TO ACUTE LIVER NECROSIS
THAT CAN RESULT IN DEATH DUE TO HEPATIC COMA.
LONG TERM INHALATION EXPOSURE TO IRON (OXIDE FUME OR DUST)
CAN CAUSE SIDEROSIS. SIDEROSIS IS CONSIDERED TO BE A BENIGN
PNEUMOCONIOSIS AND DOES NOT NORMALLY CAUSE SIGNIFICANT
PHYSIOLOGIC IMPAIRMENT. SIDEROSIS CAN BE OBSERVED ON X-RAYS
WITH THE LUNGS HAVING A MOTTLED APPEARANCE.
EXPOSURE CAN CAUSE:
STUPOR, SHOCK, ABDOMINAL CRAMPS, VOMITING, BURNING EPIGASTRIC
DISTRESS, CENTRAL NERVOUS SYSTEM AND CARDIOVASCULAR
DISTURBANCES, CYANOSIS, LEUKOCYTOSIS, HYPERGLYCEMIA,
LETHARGY, AND PULMONARY EDEMA. MAY CAUSE SKIN IRRITATION.
MAY BE HARMFUL IF ABSORBED THROUGH THE SKIN.
CAUSES EYE IRRITATION. MAY BE HARMFUL IF INHALED.
MATERIAL MAY BE IRRITATING TO MUCOUS MEMBRANES AND UPPER
RESPIRATORY TRACT.
TOXIC IF SWALLOWED.
CHRONIC EFFECTS
TARGET ORGAN(S):
LIVER
G.I. SYSTEM
BLOOD
CARDIOVASCULAR SYSTEM
RTECS #: NO4565500
IRON
TOXICITY DATA
ORL-RAT LD50:30 GM/KG IJPAAO 13,240,1951
ORL-GPG LD50:20 GM/KG IJPAAO 13,240,1951
TARGET ORGAN DATA
BEHAVIORAL (IRRITABILITY)
LUNGS, THORAX OR RESPIRATION (TUMORS)
GASTROINTESTINAL (NAUSEA OR VOMITING)
BLOOD (NORMOCYTIC ANEMIA)
TUMORIGENIC (EQUIVOCAL TUMORIGENIC AGENT BY RTECS CRITERIA)
ADDITIONAL INFORMATION
ORL-CHD LDL0:77 MG/KG
ORL-HMN LDLO:70 MG/KG
ONLY SELECTED REGISTRY OF TOXIC EFFECTS OF CHEMICAL
SUBSTANCES
(RTECS) DATA IS PRESENTED HERE. SEE ACTUAL ENTRY IN RTECS FOR
COMPLETE INFORMATION.
SECTION 12. - - - - - - - - - ECOLOGICAL INFORMATION - - - - - - - - - -
DATA NOT YET AVAILABLE.
SECTION 13. - - - - - - - - - DISPOSAL CONSIDERATIONS - - - - - - - - -
MATERIAL IN THE ELEMENTAL STATE SHOULD BE RECOVERED FOR
REUSE OR
RECYCLING.
OBSERVE ALL FEDERAL, STATE AND LOCAL ENVIRONMENTAL
REGULATIONS.
SECTION 14. - - - - - - - - - - TRANSPORT INFORMATION - - - - - - - - -
CONTACT SIGMA CHEMICAL COMPANY FOR TRANSPORTATION
INFORMATION.
SECTION 15. - - - - - - - - - REGULATORY INFORMATION - - - - - - - - - -
EUROPEAN INFORMATION
HIGHLY FLAMMABLE TOXIC
R 25
TOXIC IF SWALLOWED.
R 36
IRRITATING TO EYES.
S 16
KEEP AWAY FROM SOURCES OF IGNITION - NO SMOKING.
S 45
IN CASE OF ACCIDENT OR IF YOU FEEL UNWELL, SEEK MEDICAL ADVICE
IMMEDIATELY (SHOW THE LABEL WHERE POSSIBLE).
S 26
IN CASE OF CONTACT WITH EYES, RINSE IMMEDIATELY WITH PLENTY OF
WATER AND SEEK MEDICAL ADVICE.
S 36/37/39
WEAR SUITABLE PROTECTIVE CLOTHING, GLOVES AND EYE/FACE
PROTECTION.
REVIEWS, STANDARDS, AND REGULATIONS
OEL=MAK
NOHS 1974: HZD 91095; NIS 160; TNF 13096; NOS 115; TNE 207672
NOES 1983: HZD T0176; NIS 130; TNF 13865; NOS 72; TNE 204603; TFE 16574
NOES 1983: HZD X3724; NIS 1; TNF 122; NOS 2; TNE 1670
NOES 1983: HZD X5910; NIS 1; TNF 3; NOS 1; TNE 400; TFE 400
NOES 1983: HZD X5996; NIS 1; TNF 45; NOS 1; TNE 179
NOES 1983: HZD 91095; NIS 364; TNF 103949; NOS 174; TNE 1312446; TFE
116899
EPA TSCA SECTION 8(B) CHEMICAL INVENTORY
EPA TSCA SECTION 8(D) UNPUBLISHED HEALTH/SAFETY STUDIES
EPA TSCA TEST SUBMISSION (TSCATS) DATA BASE, JANUARY 2001
NIOSH ANALYTICAL METHOD, 1994: METALS IN URINE, 8310
NIOSH ANALYTICAL METHOD, 1994: ELEMENTS IN BLOOD OR TISSUE, 8005
SECTION 16. - - - - - - - - - - OTHER INFORMATION- - - - - - - - - - - -
THE ABOVE INFORMATION IS BELIEVED TO BE CORRECT BUT DOES NOT
PURPORT TO
BE ALL INCLUSIVE AND SHALL BE USED ONLY AS A GUIDE. SIGMA,
ALDRICH, FLUKA SHALL NOT BE HELD LIABLE FOR ANY DAMAGE
RESULTING FROM HANDLING OR FROM CONTACT WITH THE ABOVE
PRODUCT. SEE REVERSE SIDE OF INVOICE OR PACKING SLIP FOR
ADDITIONAL TERMS AND CONDITIONS OF SALE.
COPYRIGHT 2001 SIGMA-ALDRICH CO.
LICENSE GRANTED TO MAKE UNLIMITED PAPER COPIES FOR INTERNAL
USE ONLY
Material Safety Data Sheet for Palladium Powder
Valid 05/2001 - 07/2001
Riedel-de Haen 3050 Spruce St. St. Louis, MO 63178 USA Tel: 314-289-6000
MATERIALSAFETYDATASHEET
SECTION 1. - - - - - - - - - CHEMICAL IDENTIFICATION- - - - - - - - - -
CATALOG #: 64149
NAME: PALLADIUM (PALLADIUM BLACK) 98%
SECTION 2. - - - - - COMPOSITION/INFORMATION ON INGREDIENTS - - - - - -
CAS #: 7440-05-3
MF: PDM
EC NO: 231-115-6
SYNONYMS
PALLADEX 600 * PALLADIUM BLACK * PALLADIUM ELEMENT *
SECTION 3. - - - - - - - - - - HAZARDS IDENTIFICATION - - - - - - - - -
LABEL PRECAUTIONARY STATEMENTS
PYROPHORIC (USA DEFINITION)
HIGHLY FLAMMABLE (EUROPEAN DEFINITION)
IRRITANT
IRRITATING TO EYES, RESPIRATORY SYSTEM AND SKIN.
KEEP AWAY FROM SOURCES OF IGNITION - NO SMOKING.
IN CASE OF CONTACT WITH EYES, RINSE IMMEDIATELY WITH PLENTY OF
WATER AND SEEK MEDICAL ADVICE.
WEAR SUITABLE PROTECTIVE CLOTHING.
KEEP CONTAINER TIGHTLY CLOSED AND IN WELL-VENTILATED PLACE.
SECTION 4. - - - - - - - - - - FIRST-AID MEASURES- - - - - - - - - - -
IF SWALLOWED, WASH OUT MOUTH WITH WATER PROVIDED PERSON IS
CONSCIOUS.
CALL A PHYSICIAN.
IF INHALED, REMOVE TO FRESH AIR. IF NOT BREATHING GIVE ARTIFICIAL
RESPIRATION.IF BREATHING IS DIFFICULT, GIVE OXYGEN.
IN CASE OF SKIN CONTACT, FLUSH WITH COPIOUS AMOUNTS OF WATER
FOR AT LEAST 15 MINUTES. REMOVE CONTAMINATED CLOTHING AND
SHOES. CALL A PHYSICIAN.
IN CASE OF CONTACT WITH EYES, FLUSH WITH COPIOUS AMOUNTS OF
WATER
FOR AT LEAST 15 MINUTES. ASSURE ADEQUATE FLUSHING BY
SEPARATING THE EYELIDS WITH FINGERS. CALL A PHYSICIAN.
SECTION 5. - - - - - - - - - FIRE FIGHTING MEASURES - - - - - - - - - -
EXTINGUISHING MEDIA WATER SPRAY.
CARBON DIOXIDE, DRY CHEMICAL POWDER OR APPROPRIATE FOAM.
SPECIAL FIREFIGHTING PROCEDURES
WEAR SELF-CONTAINED BREATHING APPARATUS AND PROTECTIVE
CLOTHING TO
PREVENT CONTACT WITH SKIN AND EYES.
UNUSUAL FIRE AND EXPLOSIONS HAZARDS
PYROPHORIC MATERIAL.
EMITS TOXIC FUMES UNDER FIRE CONDITIONS.
CATCHES FIRE IF EXPOSED TO AIR.
SECTION 6. - - - - - - - - ACCIDENTAL RELEASE MEASURES- - - - - - - - -
WEAR SELF-CONTAINED BREATHING APPARATUS, RUBBER BOOTS AND
HEAVY
RUBBER GLOVES.
AVOID RAISING DUST.
COVER WITH DRY-LIME, SAND, OR SODA ASH. PLACE IN COVERED
CONTAINERS USING NON-SPARKING TOOLS AND TRANSPORT
OUTDOORS.
VENTILATE AREA AND WASH SPILL SITE AFTER MATERIAL PICKUP IS
COMPLETE.
EVACUATE AREA.
SHUT OFF ALL SOURCES OF IGNITION.
USE NONSPARKING TOOLS.
SECTION 7. - - - - - - - - - - HANDLING AND STORAGE- - - - - - - - - - -
REFER TO SECTION 8.
SECTION 8. - - - - - - EXPOSURE CONTROLS/PERSONAL PROTECTION- - - - -
-
SAFETY SHOWER AND EYE BATH.
USE NONSPARKING TOOLS.
MECHANICAL EXHAUST REQUIRED.
WASH THOROUGHLY AFTER HANDLING.
AVOID CONTACT WITH EYES, SKIN AND CLOTHING.
AVOID BREATHING DUST.
AVOID PROLONGED OR REPEATED EXPOSURE.
NIOSH/MSHA-APPROVED RESPIRATOR.
COMPATIBLE CHEMICAL-RESISTANT GLOVES.
CHEMICAL SAFETY GOGGLES.
KEEP CONTAINER CLOSED.
KEEP AWAY FROM HEAT, SPARKS, AND OPEN FLAME.
HANDLE AND STORE UNDER NITROGEN.
SECTION 9. - - - - - - - PHYSICAL AND CHEMICAL PROPERTIES - - - - - - -
APPEARANCE AND ODOR
SOLID.
SECTION 10. - - - - - - - - -STABILITY AND REACTIVITY - - - - - - - - -
STABILITY
STABLE.
INCOMPATIBILITIES
CATCHES FIRE IF EXPOSED TO AIR.
STRONG OXIDIZING AGENTS
HAZARDOUS COMBUSTION OR DECOMPOSITION PRODUCTS
CARBON MONOXIDE, CARBON DIOXIDE
HAZARDOUS POLYMERIZATION
WILL NOT OCCUR.
SECTION 11. - - - - - - - - - TOXICOLOGICAL INFORMATION - - - - - - - -
ACUTE EFFECTS
TO THE BEST OF OUR KNOWLEDGE, THE CHEMICAL, PHYSICAL, AND
TOXICOLOGICAL PROPERTIES HAVE NOT BEEN THOROUGHLY
INVESTIGATED.
MAY CAUSE SKIN IRRITATION.
MAY BE HARMFUL IF ABSORBED THROUGH THE SKIN.
MAY CAUSE EYE IRRITATION.
MAY BE HARMFUL IF INHALED.
MATERIAL MAY BE IRRITATING TO MUCOUS MEMBRANES AND UPPER
RESPIRATORY TRACT.
MAY BE HARMFUL IF SWALLOWED.
RTECS #: RT3480500
PALLADIUM
ONLY SELECTED REGISTRY OF TOXIC EFFECTS OF CHEMICAL
SUBSTANCES
(RTECS) DATA IS PRESENTED HERE. SEE ACTUAL ENTRY IN RTECS FOR
COMPLETE INFORMATION.
SECTION 12. - - - - - - - - - ECOLOGICAL INFORMATION - - - - - - - - - -
DATA NOT YET AVAILABLE.
SECTION 13. - - - - - - - - - DISPOSAL CONSIDERATIONS - - - - - - - - -
CONTACT A LICENSED PROFESSIONAL WASTE DISPOSAL SERVICE TO
DISPOSE OF
THIS MATERIAL.
BURN IN A CHEMICAL INCINERATOR EQUIPPED WITH AN AFTERBURNER
AND
SCRUBBER BUT EXERT EXTRA CARE IN IGNITING AS THIS MATERIAL IS
HIGHLY
FLAMMABLE.
OBSERVE ALL FEDERAL, STATE AND LOCAL ENVIRONMENTAL
REGULATIONS.
SECTION 14. - - - - - - - - - - TRANSPORT INFORMATION - - - - - - - - -
CONTACT SIGMA CHEMICAL COMPANY FOR TRANSPORTATION
INFORMATION.
SECTION 15. - - - - - - - - - REGULATORY INFORMATION - - - - - - - - - -
EUROPEAN INFORMATION
HIGHLY FLAMMABLE
IRRITANT
R 36/37/38
IRRITATING TO EYES, RESPIRATORY SYSTEM AND SKIN.
S 16
KEEP AWAY FROM SOURCES OF IGNITION - NO SMOKING.
S 26
IN CASE OF CONTACT WITH EYES, RINSE IMMEDIATELY WITH PLENTY OF
WATER AND SEEK MEDICAL ADVICE.
S 36
WEAR SUITABLE PROTECTIVE CLOTHING.
S 7/9
KEEP CONTAINER TIGHTLY CLOSED AND IN WELL-VENTILATED PLACE.
REVIEWS, STANDARDS, AND REGULATIONS
OEL=MAK
EPA TSCA SECTION 8(B) CHEMICAL INVENTORY
EPA TSCA TEST SUBMISSION (TSCATS) DATA BASE, JANUARY 2001
U.S. INFORMATION
THIS PRODUCT IS SUBJECT TO SARA SECTION 313 REPORTING
REQUIREMENTS.
SECTION 16. - - - - - - - - - - OTHER INFORMATION- - - - - - - - - - - -
THE ABOVE INFORMATION IS BELIEVED TO BE CORRECT BUT DOES NOT
PURPORT TO
BE ALL INCLUSIVE AND SHALL BE USED ONLY AS A GUIDE. SIGMA,
ALDRICH,
FLUKA SHALL NOT BE HELD LIABLE FOR ANY DAMAGE RESULTING FROM
HANDLING OR FROM CONTACT WITH THE ABOVE PRODUCT. SEE
REVERSE SIDE OF INVOICE OR PACKING SLIP FOR ADDITIONAL TERMS
AND CONDITIONS OF SALE.
COPYRIGHT 2001 SIGMA-ALDRICH CO.
LICENSE GRANTED TO MAKE UNLIMITED PAPER COPIES FOR INTERNAL
USE ONLY
Material Safety Data Sheet for Tetraethoxysilane (Tetraethyl Orthosilicate)
Valid 05/2001 - 07/2001
Aldrich Chemical Co., Inc. 1001 West St. Paul Milwaukee, WI 53233 USA Tel: 414-
273-3850
MATERIALSAFETYDATASHEET
SECTION 1. - - - - - - - - - CHEMICAL IDENTIFICATION- - - - - - - - - -
CATALOG #: 131903
NAME: TETRAETHYL ORTHOSILICATE, 98%
SECTION 2. - - - - - COMPOSITION/INFORMATION ON INGREDIENTS - - - - - -
CAS #: 78-10-4
MF: C8H20O4SI
EC NO: 201-083-8
SYNONYMS
ETHYL ORTHOSILICATE * ETHYL SILICATE (ACGIH:OSHA) * ETYLU
KRZEMIAN
(POLISH) * SILANE, TETRAETHOXY- * SILICATE D'ETHYLE (FRENCH) *
SILICATE TETRAETHYLIQUE (FRENCH) * TEOS * TETRAETHOXYSILANE *
TETRAETHYL ORTHOSILICATE * TETRAETHYLSILIKAT (CZECH) *
SECTION 3. - - - - - - - - - - HAZARDS IDENTIFICATION - - - - - - - - -
LABEL PRECAUTIONARY STATEMENTS
COMBUSTIBLE (USA)
FLAMMABLE (EU)
HARMFUL
HARMFUL BY INHALATION, IN CONTACT WITH SKIN AND IF SWALLOWED.
IRRITATING TO EYES, RESPIRATORY SYSTEM AND SKIN.
TARGET ORGAN(S):
LIVER
KIDNEYS
LUNGS
BLOOD
KEEP AWAY FROM SOURCES OF IGNITION - NO SMOKING.
IN CASE OF CONTACT WITH EYES, RINSE IMMEDIATELY WITH PLENTY OF
WATER AND SEEK MEDICAL ADVICE.
WEAR SUITABLE PROTECTIVE CLOTHING, GLOVES AND EYE/FACE
PROTECTION.
MOISTURE SENSITIVE
STORE UNDER NITROGEN.
SECTION 4. - - - - - - - - - - FIRST-AID MEASURES- - - - - - - - - - -
IN CASE OF CONTACT, IMMEDIATELY FLUSH EYES WITH COPIOUS
AMOUNTS OF
WATER FOR AT LEAST 15 MINUTES.
IN CASE OF CONTACT, IMMEDIATELY WASH SKIN WITH SOAP AND
COPIOUS
AMOUNTS OF WATER.
IF INHALED, REMOVE TO FRESH AIR. IF NOT BREATHING GIVE ARTIFICIAL
RESPIRATION. IF BREATHING IS DIFFICULT, GIVE OXYGEN.
IF SWALLOWED, WASH OUT MOUTH WITH WATER PROVIDED PERSON IS
CONSCIOUS.
CALL A PHYSICIAN.
REMOVE AND WASH CONTAMINATED CLOTHING PROMPTLY.
SECTION 5. - - - - - - - - - FIRE FIGHTING MEASURES - - - - - - - - - -
EXTINGUISHING MEDIA
CARBON DIOXIDE, DRY CHEMICAL POWDER OR APPROPRIATE FOAM.
SPECIAL FIREFIGHTING PROCEDURES
WEAR SELF-CONTAINED BREATHING APPARATUS AND PROTECTIVE
CLOTHING TO PREVENT CONTACT WITH SKIN AND EYES.
COMBUSTIBLE.
UNUSUAL FIRE AND EXPLOSIONS HAZARDS
VAPOR MAY TRAVEL CONSIDERABLE DISTANCE TO SOURCE OF IGNITION
AND FLASH BACK.
UNDER FIRE CONDITIONS, MATERIAL MAY DECOMPOSE
TO FORM FLAMMABLE AND/OR EXPLOSIVE MIXTURES IN AIR.
EMITS TOXIC FUMES UNDER FIRE CONDITIONS.
SECTION 6. - - - - - - - - ACCIDENTAL RELEASE MEASURES- - - - - - - - -
EVACUATE AREA.
WEAR SELF-CONTAINED BREATHING APPARATUS, RUBBER BOOTS AND
HEAVY
RUBBER GLOVES.
ABSORB ON SAND OR VERMICULITE AND PLACE IN CLOSED CONTAINERS
FOR
DISPOSAL.
VENTILATE AREA AND WASH SPILL SITE AFTER MATERIAL PICKUP IS
COMPLETE.
SECTION 7. - - - - - - - - - - HANDLING AND STORAGE- - - - - - - - - - -
REFER TO SECTION 8.
SECTION 8. - - - - - - EXPOSURE CONTROLS/PERSONAL PROTECTION- - - - -
-
WEAR APPROPRIATE NIOSH/MSHA-APPROVED RESPIRATOR, CHEMICAL-
RESISTANT
GLOVES, SAFETY GOGGLES, OTHER PROTECTIVE CLOTHING.
SAFETY SHOWER AND EYE BATH.
MECHANICAL EXHAUST REQUIRED.
DO NOT BREATHE VAPOR.
DO NOT GET IN EYES, ON SKIN, ON CLOTHING.
WASH THOROUGHLY AFTER HANDLING.
HARMFUL LIQUID.
IRRITANT.
KEEP TIGHTLY CLOSED.
MOISTURE SENSITIVE
KEEP AWAY FROM HEAT AND OPEN FLAME.
STORE UNDER NITROGEN.
STORE IN A COOL DRY PLACE.
SECTION 9. - - - - - - - PHYSICAL AND CHEMICAL PROPERTIES - - - - - - -
APPEARANCE AND ODOR
COLORLESS LIQUID
PHYSICAL PROPERTIES
BOILING POINT: 168 C
FLASHPOINT 116F
46.66C
VAPOR PRESSURE: <1MM 20 C
SPECIFIC GRAVITY: 0.934
VAPOR DENSITY: >1
SECTION 10. - - - - - - - - -STABILITY AND REACTIVITY - - - - - - - - -
INCOMPATIBILITIES
STRONG OXIDIZING AGENTS
STRONG ACIDS
MAY DECOMPOSE ON EXPOSURE TO MOIST AIR OR WATER.
HAZARDOUS COMBUSTION OR DECOMPOSITION PRODUCTS
TOXIC FUMES OF:
CARBON MONOXIDE, CARBON DIOXIDE
SILICON OXIDE
SECTION 11. - - - - - - - - - TOXICOLOGICAL INFORMATION - - - - - - - -
ACUTE EFFECTS
HARMFUL IF SWALLOWED, INHALED, OR ABSORBED THROUGH SKIN.
CAUSES SKIN IRRITATION.
VAPOR OR MIST IS IRRITATING TO THE EYES, MUCOUS MEMBRANES AND
UPPER
RESPIRATORY TRACT.
EXPOSURE CAN CAUSE:
NAUSEA, HEADACHE AND VOMITING
TO THE BEST OF OUR KNOWLEDGE, THE CHEMICAL, PHYSICAL, AND
TOXICOLOGICAL PROPERTIES HAVE NOT BEEN THOROUGHLY
INVESTIGATED.
CHRONIC EFFECTS
PROLONGED EXPOSURE CAN CAUSE:
LUNG IRRITATION, CHEST PAIN AND EDEMA WHICH MAY BE FATAL.
TARGET ORGAN(S):
LIVER
KIDNEYS
LUNGS
BLOOD
RTECS #: VV9450000
SILICIC ACID, TETRAETHYL ESTER
IRRITATION DATA
EYE-HMN 3000 PPM JIHTAB 22,288,1940
SKN-RBT 500 MG/24H MOD UCDS** 7/23/1970
EYE-RBT 100 MG MLD UCDS** 7/23/1970
EYE-RBT 500 MG/24H MLD 85JCAE -,1231,1986
EYE-GPG 2500 PPM/2H SEV JIHTAB 22,288,1940
TOXICITY DATA
ORL-RAT LD50:6270 MG/KG JIHTAB 31,60,1949
SKN-RBT LD50:6300 UL/KG UCDS** 7/23/1970
TARGET ORGAN DATA
BEHAVIORAL (GENERAL ANESTHETIC)
LUNGS, THORAX OR RESPIRATION (CHANGE IN TRACHEA OR BRONCHI)
LUNGS, THORAX OR RESPIRATION (ACUTE PULMONARY EDEMA)
LUNGS, THORAX OR RESPIRATION (PLEURAL EFFUSION)
KIDNEY, URETER, BLADDER (CHANGES IN TUBULES)
KIDNEY, URETER, BLADDER (INTERSTITIAL NEPHRITIS)
BLOOD (OTHER HEMOLYSIS WITH OR WITHOUT ANEMIA)
BLOOD (CHANGES IN SPLEEN)
NUTRITIONAL AND GROSS METABOLIC (WEIGHT LOSS OR DECREASED
WEIGHT GAIN)
ONLY SELECTED REGISTRY OF TOXIC EFFECTS OF CHEMICAL
SUBSTANCES
(RTECS) DATA IS PRESENTED HERE. SEE ACTUAL ENTRY IN RTECS FOR
COMPLETE INFORMATION.
SECTION 12. - - - - - - - - - ECOLOGICAL INFORMATION - - - - - - - - - -
DATA NOT YET AVAILABLE.
SECTION 13. - - - - - - - - - DISPOSAL CONSIDERATIONS - - - - - - - - -
THIS COMBUSTIBLE MATERIAL MAY BE BURNED IN A CHEMICAL
INCINERATOR
EQUIPPED WITH AN AFTERBURNER AND SCRUBBER.
OBSERVE ALL FEDERAL, STATE AND LOCAL ENVIRONMENTAL
REGULATIONS.
SECTION 14. - - - - - - - - - - TRANSPORT INFORMATION - - - - - - - - -
CONTACT ALDRICH CHEMICAL COMPANY FOR TRANSPORTATION
INFORMATION.
SECTION 15. - - - - - - - - - REGULATORY INFORMATION - - - - - - - - - -
EUROPEAN INFORMATION
EC INDEX NO: 014-005-00-0
FLAMMABLE
HARMFUL
R 10
FLAMMABLE.
R 20
HARMFUL BY INHALATION.
R 36/37
IRRITATING TO EYES AND RESPIRATORY SYSTEM.
REVIEWS, STANDARDS, AND REGULATIONS
OEL=MAK
ACGIH TLV-TWA 10 PPM DTLVS* TLV/BEI,1999
MSHA STANDARD-AIR:TWA 100 PPM (850 MG/M3)
DTLVS* 3,108,1971
OSHA PEL (GEN INDU):8H TWA 100 PPM (850 MG/M3)
CFRGBR 29,1910.1000,1994
OSHA PEL (CONSTRUC):8H TWA 100 PPM (850 MG/M3)
CFRGBR 29,1926.55,1994
OSHA PEL (SHIPYARD):8H TWA 100 PPM (850 MG/M3)
CFRGBR 29,1915.1000,1993
OSHA PEL (FED CONT):8H TWA 100 PPM (850 MG/M3)
CFRGBR 41,50-204.50,1994
OEL-AUSTRALIA: TWA 10 PPM (85 MG/M3), JAN1993
OEL-AUSTRIA: MAK 20 PPM (170 MG/M3), JAN1999
OEL-BELGIUM: TWA 10 PPM (85 MG/M3), JAN1993
OEL-DENMARK: TWA 10 PPM (85 MG/M3), JAN1999
OEL-FINLAND: TWA 10 PPM (85 MG/M3), STEL 20 PPM (170 MG/M3), JAN1999
OEL-FRANCE: VME 10 PPM (85 MG/M3), JAN1999
OEL-GERMANY: MAK 20 PPM (170 MG/M3), JAN1999
OEL-JAPAN: OEL 10 PPM (85 MG/M3), JAN1999
OEL-THE NETHERLANDS: MAC-TGG 10 PPM (85 MG/M3), JAN1999
OEL-NORWAY: TWA 10 PPM (85 MG/M3), JAN1999
OEL-THE PHILIPPINES: TWA 100 PPM (850 MG/M3), JAN1993
OEL-POLAND: MAC(TWA) 80 MG/M3, MAC(STEL) 250 MG/M3, JAN1999
OEL-RUSSIA: STEL 20 MG/M3, JAN1993
OEL-SWITZERLAND: MAK-W 10 PPM (85 MG/M3), JAN1999
OEL-TURKEY: TWA 100 PPM (850 MG/M3), JAN1993
OEL-UNITED KINGDOM: TWA 10 PPM (87 MG/M3), STEL 30 PPM, SEP2000
OEL IN ARGENTINA, BULGARIA, COLOMBIA, JORDAN, KOREA CHECK ACGIH
TLV;
OEL IN NEW ZEALAND, SINGAPORE, VIETNAM CHECK ACGIH TLV
NIOSH REL TO ETHYL SILICATE-AIR:10H TWA 10 PPM
NIOSH* DHHS #92-100,1992
NOES 1983: HZD X4097; NIS 22; TNF 721; NOS 26; TNE 10422; TFE 2566
EPA TSCA SECTION 8(B) CHEMICAL INVENTORY
EPA TSCA TEST SUBMISSION (TSCATS) DATA BASE, JANUARY 2001
SECTION 16. - - - - - - - - - - OTHER INFORMATION- - - - - - - - - - - -
THE ABOVE INFORMATION IS BELIEVED TO BE CORRECT BUT DOES NOT
PURPORT TO
BE ALL INCLUSIVE AND SHALL BE USED ONLY AS A GUIDE. SIGMA,
ALDRICH,
FLUKA SHALL NOT BE HELD LIABLE FOR ANY DAMAGE RESULTING FROM
HANDLING OR FROM CONTACT WITH THE ABOVE PRODUCT. SEE
REVERSE SIDE OF INVOICE OR PACKING SLIP FOR ADDITIONAL TERMS
AND CONDITIONS OF SALE.
COPYRIGHT 2001 SIGMA-ALDRICH CO.
LICENSE GRANTED TO MAKE UNLIMITED PAPER COPIES FOR INTERNAL
USE ONLY
Material Safety Data Sheet for Tetramethoxysilane
Valid 05/2001 - 07/2001
Fluka Chemical Corp.
1001 West St. Paul
Milwaukee, WI 53233 USA
Tel: 414-273-3850
MATERIALSAFETYDATASHEET
SECTION 1. - - - - - - - - - CHEMICAL IDENTIFICATION- - - - - - - - - -
CATALOG #: 87682
NAME: TETRAMETHOXYSILANE
SECTION 2. - - - - - COMPOSITION/INFORMATION ON INGREDIENTS - - - - - -
CAS #: 681-84-5
MF: C4H12O4SI
EC NO: 211-656-4
SYNONYMS
METHYL SILICATE (ACGIH) * SILICIC ACID, METHYL ESTER OF ORTHO- *
TETRAMETHOXYSILANE * TETRAMETHYL SILICATE * TETRAMETHYLSILIKAT
(CZECH)
* TL 190 *
SECTION 3. - - - - - - - - - - HAZARDS IDENTIFICATION - - - - - - - - -
LABEL PRECAUTIONARY STATEMENTS
FLAMMABLE
HIGHLY TOXIC (USA)
TOXIC (EU)
TOXIC BY INHALATION.
CAUSES BURNS.
TARGET ORGAN(S):
EYES
KIDNEYS
KEEP AWAY FROM SOURCES OF IGNITION - NO SMOKING.
IN CASE OF ACCIDENT OR IF YOU FEEL UNWELL, SEEK MEDICAL ADVICE
IMMEDIATELY (SHOW THE LABEL WHERE POSSIBLE).
IN CASE OF CONTACT WITH EYES, RINSE IMMEDIATELY WITH PLENTY OF
WATER AND SEEK MEDICAL ADVICE.
WEAR SUITABLE PROTECTIVE CLOTHING, GLOVES AND EYE/FACE
PROTECTION.
SECTION 4. - - - - - - - - - - FIRST-AID MEASURES- - - - - - - - - - -
IN CASE OF CONTACT, IMMEDIATELY FLUSH EYES OR SKIN WITH COPIOUS
AMOUNTS OF WATER FOR AT LEAST 15 MINUTES WHILE REMOVING
CONTAMINATED
CLOTHING AND SHOES.
IF SWALLOWED, WASH OUT MOUTH WITH WATER PROVIDED PERSON IS
CONSCIOUS.
CALL A PHYSICIAN IMMEDIATELY.
IF INHALED, REMOVE TO FRESH AIR. IF NOT BREATHING GIVE ARTIFICIAL
RESPIRATION. IF BREATHING IS DIFFICULT, GIVE OXYGEN.
ASSURE ADEQUATE FLUSHING OF THE EYES BY SEPARATING THE
EYELIDS
WITH FINGERS.
SECTION 5. - - - - - - - - - FIRE FIGHTING MEASURES - - - - - - - - - -
EXTINGUISHING MEDIA
CARBON DIOXIDE, DRY CHEMICAL POWDER OR APPROPRIATE FOAM.
WATER MAY BE EFFECTIVE FOR COOLING, BUT MAY NOT EFFECT
EXTINGUISHMENT.
SPECIAL FIREFIGHTING PROCEDURES
WEAR SELF-CONTAINED BREATHING APPARATUS AND PROTECTIVE
CLOTHING TO
PREVENT CONTACT WITH SKIN AND EYES.
USE WATER SPRAY TO COOL FIRE-EXPOSED CONTAINERS.
UNUSUAL FIRE AND EXPLOSIONS HAZARDS
FLAMMABLE LIQUID.
VAPOR MAY TRAVEL CONSIDERABLE DISTANCE TO SOURCE OF IGNITION
AND
FLASH BACK.
CONTAINER EXPLOSION MAY OCCUR UNDER FIRE CONDITIONS.
FORMS EXPLOSIVE MIXTURES IN AIR.
SECTION 6. - - - - - - - - ACCIDENTAL RELEASE MEASURES- - - - - - - - -
EVACUATE AREA.
SHUT OFF ALL SOURCES OF IGNITION.
WEAR SELF-CONTAINED BREATHING APPARATUS, RUBBER BOOTS AND
HEAVY
RUBBER GLOVES.
COVER WITH AN ACTIVATED CARBON ADSORBENT, TAKE UP AND PLACE
IN CLOSED
CONTAINERS. TRANSPORT OUTDOORS.
VENTILATE AREA AND WASH SPILL SITE AFTER MATERIAL PICKUP IS
COMPLETE.
SECTION 7. - - - - - - - - - - HANDLING AND STORAGE- - - - - - - - - - -
REFER TO SECTION 8.
SECTION 8. - - - - - - EXPOSURE CONTROLS/PERSONAL PROTECTION- - - - -
-
WEAR APPROPRIATE NIOSH/MSHA-APPROVED RESPIRATOR, CHEMICAL-
RESISTANT
GLOVES, SAFETY GOGGLES, OTHER PROTECTIVE CLOTHING.
FACESHIELD (8-INCH MINIMUM).
USE ONLY IN A CHEMICAL FUME HOOD.
SAFETY SHOWER AND EYE BATH.
USE NONSPARKING TOOLS.
DO NOT BREATHE VAPOR.
DO NOT GET IN EYES, ON SKIN, ON CLOTHING.
WASH THOROUGHLY AFTER HANDLING.
DISCARD CONTAMINATED CLOTHING AND SHOES.
KEEP TIGHTLY CLOSED.
KEEP AWAY FROM HEAT, SPARKS, AND OPEN FLAME.
STORE IN A COOL DRY PLACE.
SECTION 9. - - - - - - - PHYSICAL AND CHEMICAL PROPERTIES - - - - - - -
PHYSICAL PROPERTIES
BOILING POINT: 120 - 122 C
MELTING POINT: -4 C
FLASHPOINT 78.8 F
26 C
VAPOR PRESSURE: 274.527 MMHG
SPECIFIC GRAVITY: 1.032
VAPOR DENSITY: 5.25 G/L
SECTION 10. - - - - - - - - -STABILITY AND REACTIVITY - - - - - - - - -
STABILITY
STABLE.
CONDITIONS TO AVOID
MAY DECOMPOSE ON EXPOSURE TO MOIST AIR OR WATER.
INCOMPATIBILITIES
OXIDIZING AGENTS
ACIDS
BASES
HAZARDOUS COMBUSTION OR DECOMPOSITION PRODUCTS
CARBON MONOXIDE, CARBON DIOXIDE
SILICON OXIDE
METHANOL
HAZARDOUS POLYMERIZATION
WILL NOT OCCUR.
SECTION 11. - - - - - - - - - TOXICOLOGICAL INFORMATION - - - - - - - -
ACUTE EFFECTS
WARNING: AVOID EYE CONTACT BECAUSE TETRAMETHYL
ORTHOSILICATE
UNDERGOES HYDROLYSIS READILY, PRODUCING METHANOL WHICH
CAUSES
IRREVERSIBLE BLINDNESS.
CONTACT WITH MOISTURE LIBERATES METHANOL. INGESTION OF
METHANOL MAY
CAUSE BLINDNESS, NAUSEA, HEADACHE, VOMITING, GASTROINTESTINAL
UPSET,
DIZZINESS, IRREGULAR BREATHING, WEAKNESS, CONFUSION,
DROWSINESS,
UNCONSCIOUSNESS, AND DEATH.
MATERIAL IS EXTREMELY DESTRUCTIVE TO TISSUE OF THE MUCOUS
MEMBRANES
AND UPPER RESPIRATORY TRACT, EYES AND SKIN.
INHALATION MAY RESULT IN SPASM, INFLAMMATION AND EDEMA OF THE
LARYNX AND BRONCHI, CHEMICAL PNEUMONITIS AND PULMONARY
EDEMA.
SYMPTOMS OF EXPOSURE MAY INCLUDE BURNING SENSATION,
COUGHING,
WHEEZING, LARYNGITIS, SHORTNESS OF BREATH, HEADACHE, NAUSEA
AND
VOMITING.
TO THE BEST OF OUR KNOWLEDGE, THE CHEMICAL, PHYSICAL, AND
TOXICOLOGICAL PROPERTIES HAVE NOT BEEN THOROUGHLY
INVESTIGATED.
MAY BE HARMFUL IF ABSORBED THROUGH THE SKIN.
CAN CAUSE BLINDNESS.
TOXIC IF INHALED.
MAY BE HARMFUL IF SWALLOWED.
CHRONIC EFFECTS
TARGET ORGAN(S):
EYES
KIDNEYS
LUNGS
RTECS #: VV9800000
SILICIC ACID, TETRAMETHYL ESTER
TOXICITY DATA
IPR-RAT LD50:100 MG/KG 85JCAE -,1222,1986
IPR-MUS LD50:250 MG/KG CBCCT* 2,56,1950
SKN-RBT LD50:17 ML/KG AMIHBC 4,119,1951
ORL-MAM LD50:1 GM/KG GISAAA 39(4),86,1974
TARGET ORGAN DATA
SENSE ORGANS AND SPECIAL SENSES (OTHER EYE EFFECTS)
LUNGS, THORAX OR RESPIRATION (ACUTE PULMONARY EDEMA)
KIDNEY, URETER, BLADDER (CHANGES IN TUBULES)
MUSCULO-SKELETAL (OTHER CHANGES)
ADDITIONAL INFORMATION
IHL-RAT LC50:0.4 MG/L/4H
ONLY SELECTED REGISTRY OF TOXIC EFFECTS OF CHEMICAL
SUBSTANCES
(RTECS) DATA IS PRESENTED HERE. SEE ACTUAL ENTRY IN RTECS FOR
COMPLETE INFORMATION.
SECTION 12. - - - - - - - - - ECOLOGICAL INFORMATION - - - - - - - - - -
DATA NOT YET AVAILABLE.
SECTION 13. - - - - - - - - - DISPOSAL CONSIDERATIONS - - - - - - - - -
BURN IN A CHEMICAL INCINERATOR EQUIPPED WITH AN AFTERBURNER
AND
SCRUBBER BUT EXERT EXTRA CARE IN IGNITING AS THIS MATERIAL IS
HIGHLY
FLAMMABLE.
OBSERVE ALL FEDERAL, STATE AND LOCAL ENVIRONMENTAL
REGULATIONS.
SECTION 14. - - - - - - - - - - TRANSPORT INFORMATION - - - - - - - - -
CONTACT FLUKA CHEMICAL COMPANY FOR TRANSPORTATION
INFORMATION.
SECTION 15. - - - - - - - - - REGULATORY INFORMATION - - - - - - - - - -
EUROPEAN INFORMATION
FLAMMABLE
TOXIC
R1
FLAMMABLE
R 23
TOXIC BY INHALATION.
R 34
CAUSES BURNS.
S 16
KEEP AWAY FROM SOURCES OF IGNITION - NO SMOKING.
S 45
IN CASE OF ACCIDENT OR IF YOU FEEL UNWELL, SEEK MEDICAL ADVICE
IMMEDIATELY (SHOW THE LABEL WHERE POSSIBLE).
S 26
IN CASE OF CONTACT WITH EYES, RINSE IMMEDIATELY WITH PLENTY OF
WATER AND SEEK MEDICAL ADVICE.
S 36/37/39
WEAR SUITABLE PROTECTIVE CLOTHING, GLOVES AND EYE/FACE
PROTECTION.
REVIEWS, STANDARDS, AND REGULATIONS
OEL=MAK
ACGIH TLV-TWA 1 PPM DTLVS* TLV/BEI,1999
MSHA STANDARD:AIR-CL 5 PPM (30 MG/M3)
DTLVS* 3,169,1971
OSHA PEL (CONSTRUC):8H TWA 5 PPM (30 MG/M3)
CFRGBR 29,1926.55,1994
OSHA PEL (SHIPYARD):8H TWA 5 PPM (30 MG/M3)
CFRGBR 29,1915.1000,1993
OEL-AUSTRALIA: TWA 1 PPM (6 MG/M3), JAN1993
OEL-BELGIUM: TWA 1 PPM (6 MG/M3), JAN1993
OEL-DENMARK: TWA 1 PPM (6 MG/M3), JAN1999
OEL-FINLAND: TWA 5 PPM (30 MG/M3), STEL 10 PPM (60 MG/M3), JAN1999
OEL-FRANCE: VME 1 PPM (6 MG/M3), JAN1999
OEL-JAPAN: OEL 1 PPM (6 MG/M3), JAN1999
OEL-THE NETHERLANDS: MAC-TGG 1 PPM (6 MG/M3), JAN1999
OEL-NORWAY: TWA 1 PPM (6 MG/M3), JAN1999
OEL-SWITZERLAND: TWA 1 PPM (6 MG/M3), JAN1999
OEL-UNITED KINGDOM: TWA 1 PPM (6.3 MG/M3), STEL 5 PPM (32 MG/M3),
SEP2000
OEL IN ARGENTINA, BULGARIA, COLOMBIA, JORDAN, KOREA CHECK ACGIH
TLV;
OEL IN NEW ZEALAND, SINGAPORE, VIETNAM CHECK ACGIH TLV
NIOSH REL TO METHYL SILICATE-AIR:10H TWA 1 PPM
NIOSH* DHHS #92-100,1992
EPA TSCA SECTION 8(B) CHEMICAL INVENTORY
EPA TSCA TEST SUBMISSION (TSCATS) DATA BASE, JANUARY 2001
SECTION 16. - - - - - - - - - - OTHER INFORMATION- - - - - - - - - - - -
THE ABOVE INFORMATION IS BELIEVED TO BE CORRECT BUT DOES NOT
PURPORT TO
BE ALL INCLUSIVE AND SHALL BE USED ONLY AS A GUIDE. SIGMA,
ALDRICH,
FLUKA SHALL NOT BE HELD LIABLE FOR ANY DAMAGE RESULTING FROM
HANDLING
OR FROM CONTACT WITH THE ABOVE PRODUCT. SEE REVERSE SIDE OF
INVOICE OR
PACKING SLIP FOR ADDITIONAL TERMS AND CONDITIONS OF SALE.
COPYRIGHT 2001 SIGMA-ALDRICH CO.
LICENSE GRANTED TO MAKE UNLIMITED PAPER COPIES FOR INTERNAL
USE ONLY.
22. Procedures
22.1 Shipping Equipment to Ellington Field
Equipment will be shipped assembled, tested, and working!! to Ellington field on
April 10th, 2002,
via UPS. Two packages will arrive, one containing the nested containment units,
and one with miscellaneous other components.
Gabe Hoffmann's team will be bringing our chemicals with them to JSC and leaving
them there
until we arrive the next week. The chemicals will be accompanied by
documentation.
Equipment does not need any special storage requirements.
22.2 Ground Operations
The equipment will be set up and tested as it would be run on the KC. Reagent
bags will be filled
with catalyst and molds will be filled with base. Molds will be placed into their
drawers in the containment unit and tested.
Access to a standard 120 VAC power source is required.
22.3 Loading
The containment units, without the molds in them, will be loaded onto a forklift to
load it onto the
KC. The boxes will be strapped to the floor with two straps. The glassware, molds,
and computer will be brought on the plane
separately and installed.
22.4 Pre-Flight
The computer will be boot, the program ZGel will be run, and the equipment will be
tested.
22.5 In-Flight
Prior to each zero-gravity parabola, 5.0 mL of catalyst will be drawn. A mold will be
taken out of its
drawer and connected to the micro-t. In zero-g, the catalyst will be dispensed into
the mold and a gel will be allowed to form.
After 15 to 20 seconds, the gel will have formed and the mold will be put into a
drawer.
22.6 Post-Flight
The molds will be manually taken off the plane with the glassware and computer.
New molds will
be loaded into the equipment and the glassware will be cleaned.
22.7 Offloading
The molds will be manually taken off the plane again, as well as the glassware and
the computer.
The boxes will be taken off the plane by a forklift. The equipment will be shipped
out of Ellington Field on April 25th, 2002 and
sent back to Wisconsin by UPS.
23. Bibliography
Ayers, M. How Silica Aerogels are Made. http://eande.lbl.gov/ECS/Aerogels/
saprep.htm. (1998)
Campbell, J. A. in Chemical Systems: Energetics, Dynamics, Structure. J. H.
Freeman and Co. (1977)
Hrubesh, Lawrence W.and Poco, John F.Processing and Characterization of High
Porosity Aerogels. Lawrence Livermore National Laboratory Reports.(1994)
Hunt, Arlon. Telephone Interview, 20 May 2001.
Kong, Fung-Ming and Pekala, Richard W. A Synthetic Route to Organic Aerogels--
Mechanisms, Structure, and Properties. Lawrence Livermore National Laboratory
Reports. (1988)
Schaefer, Dale W. et al., "Origin of Porosity in Resorcinol-Formaldehyde Aerogels."
Journal of Non-Crystalline Solids, 186, 159-167. (1995)
Smith, David et al., "Effect of Microgravity on the Growth of Silica Nanostructures."
Langmuir, 16, 10055-10060. (2000)
Tillotson, T. M. and Hrubesh, L. Transparent Ultralow-density Silica Aerogels
Prepared by a Two-Step Sol-Gel Process. Reports from Third International
Symposium on Aerogels, Warzburg, Germany. (1991)
Weast, Robert ed. Handbook of Chemistry & Physics, 48th Edition. Chemical
Rubber Co. (1967)