Professional Documents
Culture Documents
TESIS
Presentada por:
Br. ROCIO MARIA TAMAYO CALDERON
AREQUIPA PER
2012
PRESENTACION
El presente trabajo consta de costa de seis captulos los cuales presentar a continuacin en
el orden siguiente:
2
AGRADECIMIENTOS
A mi asesor de tesis,
De forma muy especial al Ing. Rivalino Guzmn Al, ya que gracias a su
perseverante apoyo logr culminar el presente trabajo.
Al Dr. Acides Lpez Milla del Instituto Peruano de Energa Nuclear IPEN por
brindarme su apoyo para realizar parte de este trabajo en sus Laboratorios.
GRACIAS A TODOS
3
Dedicatoria
A Dios porque siempre est a mi lado.
Con mucho amor a mi madre y amiga Marcela, por su apoyo
incondicional, por sus sabios concejos, por ser ejemplo de sacrificio y
esfuerzo, por creer en m; este trabajo es para Usted.
A mis queridos hermanos a Carlos Daniel, Hugo, Marco
Antonio y Wilson Elard, por su ejemplo, por su amor y apoyo
en todo momento.
A mis sobrinos Samira, Hugo, Sofa, Sebastin y Diego por
ser el motivo de mi inspiracin.
A mi angelito potu perdn
De forma muy especial a mi compaero Elisban, por su apoyo
incondicional.
Roco Mara
4
INDICE GENERAL
PRESENTACIN.......... 2
AGRADECIMIENTOS 3
DEDICATORIA . 4
INDICE GENERAL.. 5
INDICE DE FIGURAS 8
INDICE DE TABLAS 10
INDICE DE ECUACIONES.. 12
ACRONIMOS 13
RESUMEN.. 14
ABSTRAC. 15
6
4.7.1 Anlisis de Fluorescencia de Rayos X .. 107
4.7.2 Anlisis de Difraccin de Rayos X .. 107
4.7.3 Microscopia Electrnica de Barrido.. .. 107
4.8 ANALISIS A MEJOR MUESTRA A DIFERENTES TEMPERATURAS............. 108
4.8.1 Anlisis Fsico... 108
4.8.2 Anlisis de Resistencia a la Compresin. 108
4.8.3 Anlisis con Microscopia ptica.. 108
4.8.4 Microscopia Electrnica de Barrido.. .. 109
7
INDICE DE FIGURAS
Figura 2.1 Unidad estructural de los silicatos..... 27
Figura 2.2 Esquema de la formacin de enlaces... 27
Figura 2.3 Configuracin espacial de un Neosilicatos.... 28
Figura 2.4 Configuracin espacial de un Sorosilicatos... 29
Figura 2.5. Configuracin de Ciclosilicatos.... 29
Figura 2.6 Configuracin de inosilicatos..... 30
Figura 2.7 Distribucin de los tetraedros de filosilicato... 31
Figura 2.8 Configuracin de Tectosilicatos..... 32
Figura 2.9 Unidad estructural de los filosilicatos..... 32
Figura 2.10 Estructuras de los filosilicatos....... 33
Figura 2.11 Politipos ms comunes...... 41
Figura 2.12 Red tridimensional infinita SiO2....... 44
Figura 2.13 Difractograma de muestra vidrio sodo-calcico..... 47
Figura 2.14 Esquema de la estructura del vidrio de cuarzo segn ZACHARIASEN.. 52
Figura 2.15 Sistema ternario de los feldespatos........ 58
Figura 2.16 Estructura de sanidina.... 59
Figura 2.17 Ubicacin del K en la estructura de sanidina... 60
Figura 2.18 Dos caminos posibles de partculas en Sinterizacin... 66
Figura 2.19 Angulo diedro de equilibrio... 67
Figura 2.20 Mecanismos atmicos bsicos.... 68
Figura 3.1 Composicin General de R.S. Domiciliarios del Distrito de Cayma 72
Figura 3.2 Caracterizacin de R.S. Urbanos Domiciliarios del Distrito de Cayma. 73
Figura 3.3 Potencial de arcilla comn en el Per..... 75
Figura 3.4 Canteras de arcilla comn de la regin Arequipa por provincias 76
Figura 3.5 Greda amarilla de Polobaya... 77
Figura 3.6 Tierra de chacra de Polobaya....... 78
Figura 3.7 Fabricacin artesanal de ladrillos...... 81
Figura 3.8 Moldeo manual de ladrillos.......... 82
Figura 3.9 Secado de ladrillos artesanales.......... 83
Figura 4.1 Diagrama de Flujo de los procesos realizados en ente estudio.. 89
Figura 4.2 Cuchara de casa grande con greda y tierra de chacra... 92
Figura 4.3 muestras de greda y tierra de chacra en la secadora.... 93
Figura 4.4 Diagrama de casa grande........... 94
Figura 4.5 Regin experimental de mezclas de las materias primas... 100
Figura 4.6 Las materias primas greda y tierra de chacra..... 101
Figura 4.7 Molino de barras, vidrio molido.... 102
Figura 4.8 Proceso de elaboracin de probetas.... 102
Figura 4.9 Codificacin de muestras....... 103
Figura 4.10 Maquina de ensayo universal SENCICO...... 107
Figura 4.11 Microscopio Electrnico de Barrido, Metalizador de la UNSA.. 108
Figura 4.12 Muestra cocidas a diferentes temperaturas.... 108
Figura 4.13 Muestra de secciones cocidas a diferentes temperaturas.. 109
Figura 4.14 Microscopio ptico IPEN.... 109
Figura 5.1 Resultados del Anlisis granulomtrico de las materias primas... 111
Figura 5.2 Porcentaje de Humedad de greda numero de golpes 112
Figura 5.3 Porcentaje de Humedad de Tierra de chacra numero de golpes 113
8
Figura 5.4 Representacin grafica del diagrama de casa grande... . 114
Figura 5.5 Comparacin Difractogramas de las Materias primas... 117
Figura 5.6 Porcentaje de contraccin total versus el tipo de muestra...... 118
Figura 5.7 Porcentaje de humedad total versus el tipo de muestra....... 119
Figura 5.8 Porcentaje de porosidad total versus el tipo de muestra...... 121
Figura 5.9 Resistencia a la compresin versus el tipo de muestra...... 123
Figura 5.10 Comparacin de DRX de muestra 302050 a 0 y 900C...... 123
Figura 5.11 Microfotografas SEM de muestra 305020 a 0 y 900C; 100, 50 y 5 m 125
Figura 5.12Resistencia a compresin, muestras 302050 diferentes temperaturas 126
Figura 5.13Microfotografas de MO de muestras 305020 a 10 y 30 aumentos de
diferentes temperaturas 127
Figura 5.14 Comparacin Difractogramas, muestras 302050 diferentes temperaturas 128
Figura 5.15 Superficie de respuesta estimada.. 132
Figura 5.16 Contornos de superficie de respuesta estimada 132
Figura 5.17 Grfica de diferencia mnima significativa (LSD) .. 134
Figura 5.18 Grfica de Caja y Bigotes... 135
9
INDICE DE TABLAS
10
ANEXOS
Tabla A.1 Anlisis Granulomtrico Vidrio........... 142
Tabla A.2 Anlisis Granulomtrico Greda........ 142
Tabla A.3 Anlisis Granulomtrico Tierra de Chacra........ 143
Tabla A.4 Resultados del las contracciones de las muestras..... 144
Tabla A.5 Resultados del las contracciones de las muestras..... 145
Tabla A.6 Resultados del porcentaje de humedad......... 146
Tabla A.7 Resultados del porcentaje de humedad......... 147
Tabla A.8 Resultados del porcentaje de porosidad...... 148
Tabla A.9 Resultados del porcentaje de porosidad...... 149
Tabla A.10 Resultados de la densidad aparente...... 149
Tabla A.11 Resultados de la densidad aparente...... 150
Tabla A.12 Resultado de Absorcin Mxima...... 150
Tabla A.13 Resultados de Absorcin Mxima....... 151
Tabla A.14 Resultado de Resistencia a la Compresin..... 152
Tabla A.15 Resultado de Resistencia a la Compresin...... 153
Tabla A.16 Resultados Estimados para Resistencia Compresin. 153
Tabla A.17 Resultados Estimados para Resistencia Compresin. 154
11
INDICE DE ECUACIONES
Ecuacin [2.1], Cambio de energa por Densificacin......... 65
Ecuacin [2.2], Energa de borde de grano........ 66
Ecuacin [4.1], Porcentaje de Humedad....... 91
Ecuacin [4.2], ndice de Plasticidad.......... 94
Ecuacin [4.3], Ecuacin de la lnea A........ 95
Ecuacin [4.4], Ecuacin de la lnea U........... 95
Ecuacin [4.5], Densidad Real............ 96
Ecuacin [4.6], Deteccin de inconsistencias..... 98
Ecuacin [4.7], Deteccin de inconsistencias L... 99
Ecuacin [4.8], Deteccin de inconsistencias U..... 99
Ecuacin [4.9], Numero de ensayos...... 99
Ecuacin [4.10], Contraccin Volumtrica seca....... 103
Ecuacin [4.11], Contraccin Volumtrica coccin........ 103
Ecuacin [4.12], Contraccin Volumtrica total....... 104
Ecuacin [4.13], Porcentaje de Humedad seco........... 104
Ecuacin [4.14], Porcentaje de Humedad coccin........... 104
Ecuacin [4.15], Porcentaje de Humedad total.......... 104
Ecuacin [4.16], Porcentaje de Porosidad.......... 105
Ecuacin [4.17], Densidad Aparente.......... 105
Ecuacin [4.18], Porcentaje de absorcin mxima........... 105
Ecuacin [4.19], Resistencia a la Compresin.......... 106
12
ACRONIMOS
13
RESUMEN
El presente trabajo tiene por objetivo la obtencin de ladrillos de arcilla cocida reforzados
con vidrio reciclado tipo sodo-clcico con mejores propiedades como resistencia a la
compresin y menor temperatura de coccin.
Se caracterizo la materia prima, las muestras obtenidas a 900 C y las muestras obtenidas a
diferentes temperaturas determinando las propiedades fsicas y qumicas como el anlisis
granulomtrico, porcentaje de humedad, limite de Atterberg, densidad, anlisis elemental
mediante Fluorescencia de Rayos X (FRX), anlisis mineralgico por Difraccin de Rayos X
(DRX), porcentaje de contraccin, Absorcin de agua, Microscopia ptica (MO), Microscopia
Electrnica de Barrido (MEB) y Resistencia a la Compresin.
14
ABSTRACT
The purpose of this research is to get fired-clay bricks reinforced with recycled sodium-calcic
glass with better properties such as compression resistance and lower firing temperature.
We applied the algorithm of McLean and Anderson to the experimental design of three-
component mixtures with some restrictions, which obtained 12 mixtures as well as an
additional sample without glass including their replicas. In order to manufacture the bricks,
the raw material was prepared according to the Granulometric analysis taking into account
some parameters of craftwork technique. Also a metallic mold was used to form the
samples. Once obtained the dried samples, they were taken to the muffla at 900C and at a
heating speed 3.33C min-1 to fire it.
The characteristics of raw material were that the samples were obtained at 900C and those
obtained at different temperatures determining physical and chemical properties such
Granulometric analysis, percentage of humidity, Atterberg limits, density, elemental analysis
by X-ray Fluorescence (FRX), mineralogical analysis by X-ray Diffraction (DRX), percentage of
contraction, water absorption, optic microscopy (MO), Electronic Microscopy for Sweeping
(MEB) and compression resistance.
15
CAPITULO I
ASPECTOS GENERALES
1.1. INTRODUCCION
El vidrio es un material que ha sido usado por el hombre desde hace milenios, posiblemente
sea el material ms viejo fabricado por el hombre y que an contina afectando la vida
presente. Los primeros egipcios consideraron a los vidrios como materiales preciosos, para
evidencia fueron encontradas restos de vidrio en tumbas y mscaras de Faraones, tambin
fueron usadas piezas de obsidiana como herramientas y armas, hemos estado produciendo
vidrios fusionando materias primas por miles de aos.
La presencia de los vidrios es tan comn que raramente notamos su existencia, el vidrio
est presente en formas tan diversas como: ventanas, vasos, envases de todo tipo,
telescopios, en la industria nuclear como escudo de radiacin, en electrnica como sustrato
slido para circuitos, en la industria del transporte, de la construccin etc. Por sus
caractersticas intrnsecas (brillantez, resistencia al uso, transparencia, etc.), el vidrio es un
material difcilmente sustituible (y a veces, realmente insustituible) en la mayora de sus
aplicaciones. Igualmente remarcable es la disponibilidad y bajo costo de las materias primas
usadas para producirlo, especialmente su componente ms importante, la slice (que se
encuentra en la arena).
El vidrio es 100% reciclable infinitas veces, sin embargo solo se reciclan botellas y envases,
siendo un problema ambiental los residuos de vidrios comunes (vidrios de ventanas sodo-
clcico, sector automotriz, etc.) no se reciclan, son llevados para su disposicin final a
botaderos y rellenos sanitarios. Considrese que en la ciudad de Arequipa se generan 0.76
kg/hab./da per cpita y un total 662.44 Tn/da de residuos slidos.
17
Agregando diferentes porcentajes de vidrio molido a mezclas de arcillas comunes se obtuvo
el mximo resultado de resistencia a la compresin de 28 MPa; y como agente fundente
con una temperatura de coccin de 800C; con una resistencia a la compresin de 17MPa y
segn la norma de Albailera E-007 seria catalogado tipo de ladrillo V mejor resistencia a la
compresin.
En el Capitulo III se ofrece el estudio de la materia prima desde el punto de vista general,
industrial, regional y distrital.
1.2. ANTECEDENTES
En trabajos anteriores fueron reportados diferentes componentes que mejoran las
propiedades de ladrillos de arcilla cocida como la resistencia a la compresin y que vidrios
reciclados pueden ser utilizados como un potencial agente fundente que ayuda a bajar la
18
temperatura de quemado de cuerpos de arcilla mejorando las propiedades fsicas es as
que tenemos:
Marin (2010), concluye que los relaves de mina pueden ser utilizados como un
componente en la fabricacin de arcilla cocida, mejora la resistencia a la compresin en
un 122.4 % comparado con un ladrillo artesanal, se obtuvieron mejores propiedades
con 40% de relave de mina, 40% de tierra de chacra y 20% de greda a una temperatura
de coccin de 950 C.[13]
Sivana y Velez (2008), concluyen que al agregar 10% de sillar en una mezcla de ladrillo
de arcilla cocida ayudan a mejorar sus propiedades fsicas y mecnicas. Las
propiedades que se mejoraron son la resistencia a la compresin y la contraccin
(%).[20]
Vorrada et al. (2009), Concluye que es factible destinar a vidrios reciclados planos
como un componente en la fabricacin de ladrillos de arcilla cocida. Los vidrios
reciclados pueden estar mezclados con arcilla en proporciones diferentes para preparar
ladrillos de buena calidad. La temperatura correcta de quemado es 1100 C, la adicin
de vidrio reciclado hasta 30 wt. % no le caus los efectos perjudiciales a las
propiedades de ladrillos de arcilla, y que los ladrillos de arcilla preparados con 15 a 30
wt % pudieran encontrar los requisitos mnimos en una gran variedad de aplicaciones y
aun en algunas estructuras que soportan carga. [24]
Tucci et al. (2004), demostrarn los beneficios de agregar polvos de vidrio sodo-clcico
en pequeas cantidades en mezclas de baldosas, vasijas de gres, porcelana, los cuales
generalmente requieren temperaturas altas de quemado. El estudio demostr que los
vidrios sodo-clcico podran actuar como un buen agente fundente y el reemplazo de
vidrios por 10 % en peso result con mejores caractersticas mecnicas.[23]
19
Luz y Ribeiro (2007) indicaron tambin que el vidrio reciclado fue un agente fundente
eficaz en mezclas de cermicas para la manufactura de baldosas, acelerando el proceso
de densificacin. Los resultados demostraron buenas propiedades mecnicas y fsicas
con cantidades pequeas de adicin de polvo del vidrio. [12]
Dondi (2009) demostr que los vidrios reciclados se comportan como un agente que
disminuye la plasticidad, facilitando la sinterizacion y bajando la temperatura de
coccin de la arcilla durante el quemado. La adicin de vidrios reciclados, deberan ser
mantenidas entre 2 y 4 % en peso, sin embargo esto depender de las caractersticas
de cuerpos de arcilla, para prevenir efectos destructivos en productos finales. [7]
Los residuos slidos industriales y domsticos, se han incrementado estos ltimos tiempos,
dentro de ellos tenemos los vidrios, de acuerdo a la Caracterizacin de Residuos Slidos
Domiciliarios de la Municipalidad de Cayma (junio 2011), el 2,8 % del total corresponde a
vidrios en general, de ellos el 1,5% corresponden a botellas y envases de vidrio que se
20
reciclan y el 1,3% corresponde a vidrios que no se reciclan, son desechados sin ningn
cuidado, los cuales atentan contra nuestra salud y al medio ambiente.
1.4. HIPOTESIS
Dado que agregando diferentes porcentajes de vidrio molido a mezclas de arcillas comunes
es posible producir ladrillos de arcilla cocida con elevada resistencia a la compresin y
menor temperatura de coccin.
1.5. OBJETIVOS
1.5.1 Objetivo General
1.6. JUSTIFICACIONES
21
estos residuos son llevados diariamente a los botaderos aumentando el volumen y
poniendo en riesgo la salud de las personas que trabajan directamente con los
residuos slidos, por ello el presente trabajo estudia a los vidrios reciclados sodo-
clcico para que pueda ser usado como reforzante en la produccin de ladrillos de
arcilla cocida, el cual nos permitir reducir el volumen de estos residuos slidos y por
lo tanto disminuir la contaminacin ambiental.
22
CAPITULO II
MARCO TEORICO
2.1. LAS ARCILLAS
El trmino arcilla presenta una cierta complejidad, ya que oscila en torno a dos conceptos,
fundamentados en la mineraloga y en el tamao de partcula. Segn el criterio
granulomtrico se considera arcilla toda fraccin integrada por minerales cuyo tamao de
grano (isodimetro) sea inferior a 2 m. Desde el punto de vista mineralgico, se considera
arcilla a aquellos minerales de la subclase filosilicatos cuyas capas de tetraedros de SiO4 y
octaedros de AlO6 estn apiladas y unidas por enlaces de tipo residual o por molculas de
agua y que en caso de presentar cationes entre estas capas, stos no constituyen elemento
estructural interlaminar.
La realidad nos muestra que en muchas ocasiones ambos criterios se solapan, toda vez que
los minerales que pertenecen a los filosilicatos arcillosos muestran siempre tamaos de
grano inferiores a 2 m, si bien otros minerales (cuarzo, por ejemplo) pueden ser
considerados arcilla granulomtricamente, aunque no lo sean mineralgicamente. Para
ordenar estas ideas, los comits de nomenclatura propusieron dos definiciones:
24
2.1.1. Clasificacin de Arcillas
Las arcillas se pueden clasificar desde distintos puntos de vista, segn sean los
criterios utilizados, geolgico, mineralgico, segn sus propiedades fisicoqumicas o
de acuerdo a su uso. No obstante, nos vamos a centrar en una clasificacin basada en
sus propiedades fsicas y en su aplicabilidad en la industria cermica. Las rocas
arcillosas estn compuestas adems por minerales de arcilla (caolinitas, illita,
montmorillonitas, cloritas e interestratificados de distintas composiciones), por
distintas proporciones de cuarzo, carbonatos, feldespatos, biotita, moscovita,
compuestos de hierro y titanio, sales solubles, materia orgnica y residuos
carbonosos. La naturaleza de los minerales de arcillas y las proporciones relativas del
resto de componentes condicionarn la respuesta de las arcillas durante el proceso
cermico. En funcin de esto, las arcillas utilizadas en la industria cermica se pueden
dividir en tres grandes grupos (Barba et al. 1997):
Caolines o China-clays
Tienen una composicin eminentemente caolintica, generalmente resultado de
un proceso de beneficio y concentracin de este mineral a partir de una roca
arcillosa rica en este mineral. Su caracterstica principal es su color blanco o
crema tras coccin y su refractariedad.
25
Arcillas de color rojo tras coccin
Arcillas refractarias: De propiedades muy variables, su nica caracterstica comn
es el comportamiento refractario.
Arcillas fundentes: Se clasifican segn su contenido en carbonatos en arcillas de
bajo (<5% en peso), medio (5-15%) y alto (>15%) contenido en carbonatos.
Arcillas comunes: Son arcillas impuras de mediana plasticidad, composicin y
mineraloga variable, tiles para la fabricacin de ladrillos. Generalmente no son
de color blanco y contienen hasta 5% de lcalis, 12% de alcalinotrreos y 8% de
xidos frricos.
El fuerte enlace que une los iones silicio y oxigeno es, literalmente, el cemento que
conglomera la corteza terrestre. Empleando el concepto de electronegatividad de PAULING
este enlace puede ser considerado como inico en un 50% y covalente en otro 50%. Es
decir, aunque el enlace es debido en parte a la atraccin de unidades inicas de cargas
contrarias, implica tambin el reparto de electrones y la interpenetracin de las
superestructuras electrnicas de los iones, estando el enlace intensamente localizado en la
proximidad de estos electrones compartidos. Cada in oxigeno, O2-, puede unirse a otro in
26
silicio y entrar en otra agrupacin tetradrica, en la que los grupos tetradricos estn
unidos por los oxgenos compartidos (puentes de oxgeno).
27
Si dos tetraedros adyacentes comparten uno, dos, tres o los cuatro oxgenos, resulta
estructuras con diversas configuraciones. La Figura 2.2 ilustra las diversas formas en las
cuales pueden combinarse los tetraedros SiO4.
28
Figura 2.4 Configuracin espacial de un Sorosilicatos
Fuente: SHACKELFORD, J., & DOREMUS, R., (2008) Ceramics and Glass
Materials Structure
29
2.3.4. Inosilicatos [Si2O6]4- ; [Si4O11]6- :
Son silicatos con estructuras en cadenas con una disposicin infinita de los tetraedros
segn una direccin. Los tetraedros SiO4 se disponen compartiendo dos oxgenos,
para formar cadenas sencillas, a su vez cadenas simples pueden unirse lateralmente a
travs de un oxigeno de tetraedros alternos, formando cadenas dobles. Esto confiere
a estos minerales su tpica exfoliacin en fibras. As tenemos dos grandes grupos que
constituyen esta clase y pueden ser:
Cadenas continuas sencillas de tetraedros unidos por un oxgeno comn. As
quedan dos O de cada tetraedro saturados por la unin, otro O se mantiene (con
una valencia libre) situado en el plano de los otros dos anteriores y el cuarto O se
sita alternativamente hacia un lado y otro de la cadena. Ejemplo: Piroxeno
MgSiO3.
Cadenas continas dobles de tetraedros, formados a partir de dos cadenas
sencillas unidas por oxgenos de tetraedros alternos. Ejemplo: Anfbol
Mg7Si8O22(OH)2.
30
Cada estrato, por medio de su superficie de iones O, se une a otro estrato de anloga
estructura mediante los cationes metlicos. La superficie no activa del estrato suele
unirse a la estructura general por dbiles fuerzas de Van der Waals (de ah la gran
facilidad de exfoliacin de estos minerales). Ejemplo: Mica, KMg 3(AlSi3O10)(OH)2.
31
Figura 2.8 Configuracin de Tectosilicatos. (a) Orden
espacial de un tectosilicato, consiste solamente de
tetraedros de slice (b) orden espacial de un tectosilicato
en el que algn Si4+ ha sido sustituido por Al3+.
Fuente: SHACKELFORD, J., & DOREMUS, R., (2008) Ceramics and Glass
Materials Structure
32
La relacin Si:O es de 2:5 o 4:10. Estas capas estn constituidas por unidades (SiO4)4- en las
que el Al puede llegar a sustituir al Si en una de cada de dos posiciones. A estas capas se las
denomina capas tetradricas.
Cada capa tetradrica en todos los filosilicatos (excepto en la apofilita) se asocia con otra
agrupacin tambin laminar de cationes (Fe2+, Mg2+, Al3+, Fe3+), en coordinacin octadrica
con aniones oxgeno y (OH). Los grupos (OH) se localizan en el centro de los anillos
hexagonales de tetraedros, a la misma altura que los vrtices no compartidos de los
tetraedros (SiO4)4-.Esta coordinacin octadrica se produce de forma que los aniones se
disponen en torno a cationes ocupando los vrtices de un octaedro en cuyo centro se sita
el catin. Mediante la comparticin de aniones entre los octaedros se origina una malla
plana que se denomina capa octadrica. En la naturaleza hay dos minerales que presentan
este tipo de estructura laminar con coordinacin octadrica:
33
Brucita, Mg3(OH)6, similar a la anterior excepto en que hay tres denomina
trioctadricos.
Para los trilaminares, si se conectan las capas tetradricas por ambos lados de la capa
octadrica se producen como emparedados T-O-T, que pueden dar lugar a estructuras
trilaminares (2 capas T y una capa O) dioctadricas [pirofilita, Al2Si4O10(OH)2)] o
trioctadricas [talco, Mg3Si4O10(OH)2)]. Las estructuras resultantes son elctricamente
neutras y forman unidades estructurales estables que se conectan entre s por
enlaces de Van der Waals. Como estos enlaces son muy dbiles, es lgico que los
filosilicatos sean minerales que presenten exfoliacin basal perfecta (paralela a la
disposicin de las lminas) y fcil deslizamiento de unas respecto a otras. Aunque
34
estas estructuras son elctricamente neutras, pueden existir sustituciones de Si 4+ por
Al3+ en la capa tetradrica, lo que provocar la aparicin de lminas cargadas
negativamente. Este dficit de carga es compensado por la entrada de cationes
monovalentes o divalentes (si es sustituido ms de un tomo de Si) entre las lminas
T-O-T. Estos cationes interlaminares hacen que las lminas se unan ms firmemente,
con lo que se produce un aumento de la dureza y disminuye la facilidad de
deslizamiento. Las estructuras que resultan de la intercalacin de cationes
monovalentes entre las lminas corresponden a las MICAS REALES, que comprenden
tanto trminos dioctadricos, en los que el catin interlaminar puede ser K o Na
(Moscovita-Paragonita), como trioctadricos (biotita-flogopita), en los que el catin
interlaminar slo puede ser K.
35
bructica adicional). Por lo tanto, en funcin del valor global en la lmina de las
estructuras 2:1 podemos distinguir los siguientes grupos:
Sustitucin de R3+ (normalmente Al3+ o Fe3+) o, ms raramente R2+ (Be) por Si4+ en
posiciones tetradricas.
Sustitucin de R+ o R3+ por R2+ o R3+ en posiciones octadricas.
Existencia de vacancias en las posiciones octadricas.
Deshidroxilacin de grupos (OH)-.
El resultado es una lmina cargada negativamente, que dependiendo del valor de esa
carga da lugar a los diferentes grupos de filosilicatos 2:1.
36
Tabla 2.2 Tipos de filosilicatos Dioctadricos
APILAMIENO DE PLANOS
DIOCTAEDRICOS (Capa tetradrica, 2 cationes por cada 6 aniones)
TIPO 1:1 BILAMINARES T-O (espaciado de 4-7 )
Caolinita Si2O5Mg3(OH)4
Caolinita triclnica, Dickita
monoclnica, Nacrita
monoclnica pseudorrmbica,
Metahalloysita, halloysita
parcialmente hidratada.
Margarita (Si2Al2)O10Al2(OH)2Ca
Fuente: Magdalena Rodas, Mineraloga 1, Universidad Complutense de Madrid, 2011.
37
Tabla 2.3 Tipos de filosilicatos trioctadricos
APILAMIENO DE PLANOS
TRIOCTAEDRICOS (Capa octadrica, 3 cationes por cada 6 aniones)
TIPO 1:1 BILAMINARES T-O (espaciado de 4-7 )
Serpentina Si2O5Al2(OH)4
Amesita, Antigorita, Berthierina, Crysotilo Lizardita,
Cronstedtita, Greenalita
Micas (Si3Al)O10Mg3(OH)2K
Mg-Fe, Flogopita, lepidolita, biotita.
Xantofilita (Si2Al2)O10Mg3(OH)2Ca
Fuente: Magdalena Rodas, Mineraloga 1, Universidad Complutense de Madrid, 2011.
38
Tabla 2.4 Tipos de filosilicatos Dioctadricos
TIPOS 2:1 TRILAMINARES T-O-T (espaciado de 7-14 )
DIOCTAEDRICOS
Esmectitas Si4O10 (Al2-x R 2+X) (OH)2nH2O
Al, montmorillonitas, beidelita.
Fe, nontronita
39
Tabla 2.5 Tipos de filosilicatos Trioctadricos
TIPOS 2:1 TRILAMINARES T-O-T (espaciado de 7-14 )
TRIOCTAEDRICOS
Esmectitas Si4O10 (Mg3-x R 2+X) (OH)
Mg, saponita, estevensita, hectorita.
VI IV
Vermiculitas (MG, Fe, Al) 3 (Al,Si4) O10 (OH)2 Mg0.35 4.5H2O
40
3. Si la secuencia de apilamiento consiste en dos vectores a 120 uno de otro
(p.ej., los vectores 1 y 2), se origina un politipo monoclnico, pero distinto del
primero, con grupo espacial C2/c. Es el politipo 2M1.
4. Apilamiento segn las direcciones de los tres vectores (1, 2 y 3), la simetra es
trigonal y origina el politipo 3T, que es compatible con dos grupos espaciales -
P3112 y P3212.
Aunque pueden existir otros politipos adems de los mencionados, los ms comunes
son los 1M, 2M y 3T.
41
Los cristales de denso empaquetamiento, por ejemplo los xidos SiO 2, MgO, a pesar de este
denso empaquetamiento poseen un elevado coeficiente de dilatacin, mientras ciertas
sustancias como el vidrio de cuarzo, de un reducido empaquetamiento estructural, poseen
un coeficiente de dilatacin muy pequeo. En estas sustancias una parte del calor de
dilatacin es consumido por el espacio libre interior. Los intensos enlaces entre los tomos
tienen como consecuencia la infusibilidad y dureza de los cristales. Los enlaces dbiles son
caractersticos para los cristales blandos de bajo punto de fusin.
Sin embargo, las formas estables por encima del punto de transicin (formas ), en
contraposicin a las formas estables por debajo del mismo punto (formas y ), en la
mayor parte de los casos poseen un empaquetamiento ms reducido y en consecuencia un
peso especifico ms pequeo que las formas estables debajo del punto de transicin:
Tambin se conocen algunos casos en que la forma estable por encima del punto de
transicin tambin es estable a temperaturas inferiores. Sin embargo, el anlisis, en casi
todos estos casos, ha permitido demostrar que existan impurezas que, en forma de
inclusiones o por formacin de cristales mixtos, rellenan los espacios libres del amplio
retculo de la forma estable por encima del punto de transicin. Estas impurezas impiden la
contraccin del retculo para que aparezca la forma estable por debajo del punto de
transicin al descender la temperatura por debajo del mismo.
42
Las valencias de un tomo central, por ejemplo de SiO4, quedan completamente saturadas
al combinarse con el oxigeno; ahora bien, a cada O le queda una valencia libre. Por eso este
radical ha de considerarse como ion (SiO4)4-. Las valencias del oxigeno han de saturarse de
alguna forma hacia el exterior. Un tetraedro SiO4 puede unirse por sus valencias libres a
otro tetraedro SiO4, o a dos octaedros de Al, o tambin a tres octaedros de Mg.
Por su inters petrolgico destacamos los siguientes grupos dentro de los tectosilicatos:
43
Figura 2.12 Red tridimensional infinita SiO2 (dixido de
silicio)
Fuente: Magdalena Rodas, Mineraloga 1, Universidad Complutense de
Madrid, 2011.
2.6.1. Polimorfa
Polimorfa es la propiedad por la que una sustancia es capaz de presentarse en
diversas formas cristalinas, llamadas modificaciones. Puede suceder que por el
aspecto exterior se consideren como diferentes, debido a sus propiedades
perfectamente distintas, las substancias que cientficamente son consideradas como
modificaciones de una misma por ejemplo, el grafito y el diamante o el fsforo rojo
y el blanco.
La definicin de polimorfa como una sustancia que presenta varias
modificaciones no puede considerarse tomando como unvoca tomando
sencillamente como caracterstica su composicin qumica, sino que se debe
enunciar en una forma ms precisa. Esta definicin ms precisa del concepto de
substancia polimorfa corresponde en general a la transformacin de una forma
usual en otra, y por lo tanto, est basada en la teora de las fases. Se entiende por
sustancia un constituyente independiente de un sistema que, por s solo, no forma
un sistema unitario, y que, en principio, queda caracterizado en los distintos estados
por sus propiedades. La ventaja de esta definicin consiste en que, de acuerdo con
ella, las modificaciones polimrficas se pueden estudiar de la misma manera que los
44
gases y los lquidos, la influencia de la temperatura y presin sobre la posicin de
equilibrio est relacionada con el calor de transformacin y con la variacin de
volumen al pasar de una modificacin a otra mediante ecuaciones termodinmicas.
Evidentemente, el estudio termodinmico slo comprende una parte del problema,
pues nos informa exclusivamente sobre los equilibrios y la estabilidad
termodinmica de cada una de las modificaciones en determinadas condiciones
exteriores.
Los polimorfos de una sustancia dada se efectan con una ligera variacin del
sistema cristalino, sin alteracin de la estructura reticular y conservando la forma
exterior. Por ejemplo:
2.7. EL VIDRIO
Los vidrios usados durante la mayor parte de nuestra historia se han basado en slice. Los
vidrios se forman tradicionalmente por el enfriamiento de una mezcla fundida. La mayora
45
de vidrios tradicionales son inorgnicos y poco metlicos. Actualmente usamos un nmero
enorme de vidrios orgnicos. Los vidrios metlicos se estn volviendo ms comunes cada
ao. Obviamente la naturaleza qumica del material no puede usarse para definir un vidrio.
Todos los vidrios encontrados hasta la fecha comparten dos caractersticas comunes:
Un vidrio as puede estar definido "un slido amorfo completamente carente de rango de la
peridica estructura atmica y exhibiendo una regin de comportamiento de
transformacin de vidrio". Cualquier material, inorgnico, orgnico, o metlico, formado
por cualquier tcnica, que exhibe comportamiento de transformacin de vidrio es un vidrio.
46
Figura 2.13 Difractograma de muestra vidrio sodo-clcico.
Fuente: Elaboracin Propia
47
promedio a la distribucin espacial en el retculo cristalino, las densidades del vidrio y
de la modificacin cristalina correspondiente sern aproximadamente las mismas. Si el
retculo es de mayores dimensiones, son de esperar diferencias en ellas. Comparando
las densidades y los volmenes del vidrio y del cristal se deducen las relaciones
existentes entre la estructura reticular ordenada del cristal.
La imagen estructural del vidrio as desarrollada permite explicar, por una parte, las
relaciones citadas entre el vidrio y el cristal, y por otra las diferentes caractersticas
entre ambos, o sea la ausencia de un punto de fusin definido en el vidrio. Ya que en
ste las partculas contiguas, an siendo de la misma especie, no tienen la misma
solidez que en el cristal. A causa de las irregularidades en la estructura reticular del
vidrio, los diferentes lugares de la red sufren, al calentarse ms o menos, las
consecuencias del incremento en las vibraciones de las partculas. En un lugar se
debilitan los enlaces ms que en otro, de manera que el retculo no se destruye a una
temperatura determinada, como los cristalinos, sino que pierden paulatinamente su
cohesin a medida que se van debilitando, primero, los enlaces ms dbiles, y luego,
los ms fuertes.
48
Ya que la teora estructural reticular exige que las relaciones geomtricas de un grupo
fundamental con los contiguos, es decir, su nmero de coordinacin en la sustancia
vtrea, sean las mismas que en la sustancia cristalina, quedan determinadas tambin
exactamente las condiciones geomtricas previas para la formacin de un retculo. Por
eso, al derivar el retculo irregular de un vidrio se toman como base los mismos
poliedros de coordinacin que al deducir las estructuras reticulares. En un retculo los
poliedros de coordinacin pueden unirse por una cara, por una arista se establece la
disposicin simtrica en el retculo, incluso para los grupos fundamentales ms
alejados: dos grupos unidos por una cara son rgidos, mientras que los unidos por un
vrtice no determinan el ngulo de este. En el caso de poseer un vrtice comn queda
as sin determinar el ngulo que forman los tomos centrales de los poliedros vecinos
con el tomo del vrtice compartido. Por esto, esencialmente slo se tomar en
consideracin, para la formacin de un retculo irregular, la unin de los poliedros de
coordinacin a travs de un vrtice. De la estructura cristalina de modificaciones
polimrficas se desprende que el ngulo en dicho vrtice puede variar: en la
cristobalita y en la tridimita el ngulo Si-O-Si es llano, mientras que en las otras
modificaciones del dixido de silicio es obtuso, pero an as, la disposicin tetradrica
regular del poliedro de coordinacin SiO4 es igual en todas ellas. A fin de que pueda
mantenerse la red tridimensional de los poliedros de coordinacin, cada uno de ellos
deber estar enlazado por lo menos con otros tres.
El nmero de coordinacin (NC) del tomo central de uno de estos poliedros deber
ser, pues, 3 mayor. Pero tampoco mucho mayor, porque de ser as se condicionaran
demasiadas direcciones en el espacio, segn las leyes de simetra vigentes para los
retculos, en cuyo caso slo se podra formar un retculo irregular cuando existieran
fuertes deformaciones irregulares de los poliedros, lo que no ocurre en las substancias
en que el NC del tomo central del poliedro de coordinacin en el cristal es 6 u 8, no
forman vidrios. El nmero de coordinacin en el vrtice comn del tomo que enlaza a
dos poliedros debe ser, naturalmente, 2.
49
Resumiendo, las condiciones geomtricas previas para la formacin de un retculo
irregular son, pues, las siguientes:
En general, las cuatro reglas deben ser satisfechas para que ocurra la formacin del
vidrio. Con estas conclusiones existe una base para las consideraciones estructurales en
substancias amorfas. As se pueden aplicar a los vidrios la concepcin terica
estructural conocida en Qumica orgnica, la teora de la coordinacin y la
Cristaloqumica. En ello estriba la gran ventaja que representa la teora estructural
reticular de ZACHARIASEN frente a las teoras sobre el estado vtreo que se apoyaban
en la Termodinmica y especialmente en la teora de las fases.
Las reglas de ZACHARIASEN se cumplen originando vidrios aluminosilicatos, con
importantes aplicaciones tecnolgicas. Estos xidos son llamados Formadores
Intermedios de vidrios; no forman vidrios por ellos mismos, pero actan como
formadores de vidrios combinados con otros (vidrios aluminosilicatos, alumino-
boratos, alumino-fosfatos).
50
2.7.3. Componentes de un Vidrio
De acuerdo a la teora estructural reticular de los vidrios formulada por ZACHARIASEN
podemos clasificar en tres grupos a los compuestos que forman el vidrio:
Generadores de Red de Vidrio: Todos los vidrios de inters para el ceramista son
combinaciones de xidos. Los xidos capaces de formar un vidrio por s mismos se
llaman generadores de red. ZACHARIASEN, en 1932, establece cuatro reglas que deben
cumplirse para que un oxido forme un vidrio:
Segn estos criterios, se vio que el SiO2, B2O3 y el P2O5 deban formar vidrios, como
ocurre en realidad. Otros varios xidos y el fluoruro de berilio tambin forman vidrios.
Modificadores de la Red de Vidrio: Los modificadores son xidos que rellenan los
huecos de la red y debilitan los enlaces. Su adicin debe ser limitada porque, s entran
en la red ms de los que pueden caber, toda la estructura se derrumba al estado
cristalino. Tales modificaciones pueden ser: Na2O, K2O, CaO, MgO, PbO. Por lo general
cuanto ms modificadores se aaden, menos viscosidad tiene el vidrio y menos
resistencia al ataque qumico.
51
Tabla 2.6 Los tres grupos de los compuestos que forman el vidrio de acuerdo a
la teora estructural reticular de los vidrios formulada por ZACHARIASEN.
FUNCION COMPUESTOS
Modificadores de red Na2O K2 O CaO MgO BaO PbO ZnO
Intermedios Al2O3 TiO ZrO
Formadores de Red SiO2 B2O3 GeO2 P2O5
Fuente: Shelby, E. Introduction to Glass Science and Technology 2005 USA
52
El vidrio no se desintegra ni explota sometido a las cargas de flexin, sino que la rotura
se origina en un punto especfico (donde hay una falla) la cual se convierte en una
pequea grieta y de all progresa extendindose rpidamente sobre el vidrio y
generando la rotura. En la resistencia del vidrio a la rotura tambin influye el tiempo
durante el cual se aplic la tensin. A mayor tiempo de aplicacin, la capacidad de
resistencia del vidrio disminuye respecto a la original.
53
de estao lquido, el cual posee una planimetra perfecta. El vidrio copia la superficie
plana del estao fundido, mientras se va enfriando, obteniendo as un vidrio con una
planimetra perfecta, sin ondulaciones. Las materias primas son fundidas en horno a
1500 C aproximadamente. Una vez lograda la homogeneizacin, la masa de vidrio es
vertida sobre un bao de estao fundido que avanza a una determinada velocidad
(aqu la temperatura es de aproximadamente 1050 C).
De este modo la cinta es producida con un espesor uniforme y las superficie pulidas
brillantes sin necesidad de posteriores procesos. El vidrio contina enfrindose
mientras avanza a lo largo del bao de estao fundido y entra al horno de recocido a
600C aproximadamente. Este proceso es necesario para bajar lentamente la
temperatura previniendo las tensiones internas que se produciran por un rpido
enfriamiento. El vidrio contina enfrindose a 200C.
Ahora est suficientemente fro para poder ser cortado, lo cual es realizado por rodillos
de corte montados sobre puentes de corte longitudinales y transversales, que permiten
obtener los tamaos individuales requeridos. Las piezas separadas son removidas de la
lnea de produccin por brazos robticos con ventosas que toman el vidrio. Previo al
corte se realiza una inspeccin con rayos lser para identificar posibles defectos en el
vidrio. Esta informacin es transmitida a una computadora que permite que se corte el
defecto y reenviar el trozo de vidrio defectuoso al horno de fusin. Los bordes
recortados de la cinta de vidrio tambin son reenviados al horno.
54
2.7.6. Vidrio Sodo Clcico
Este es el vidrio comercial ms comn y el menos costoso. El amplio uso de este tipo de
vidrio es debido a sus importantes propiedades qumicas y fsicas. El vidrio sodo-clcico
es usado para:
Envases (botellas, jarros, vasos de uso diario, etc.)
Vidrio para ventanas (en la industria de la construccin y en la industria
automotriz).
Para fabricarlo es necesario fundir la slice, la cual lo hace a una temperatura muy alta
(1500C). Para reducir esa temperatura de fusin y hacer a la masa ms manejable, se
le agrega sodio (NaO). Pero el vidrio as obtenido es suave y no muy durable, por lo que
se le agrega cal (CaO) para aumentar su dureza y durabilidad qumica. Otros xidos se
agregan por otras varias razones, o son impurezas naturales de las materias primas. Por
ejemplo, el aluminio aumenta la duracin qumica y aumenta la viscosidad en los
rangos de temperaturas ms bajos.
La composicin tpica de vidrios sodo-clcicos de slice se muestra la tabla 2.8.
Adems su superficie suave y no porosa lo hace especialmente apto para ser usado
como envases pues resulta fcil de limpiar, y debido a la inercia qumica del vidrio
sodo-clcico, ste no contaminar el contenido ni afectar el sabor de los elementos
55
guardados all. Un tpico vidrio sodo-clcico est compuesto de 71 a 75% en peso de
arena (SiO2), 12-16% de soda (xido de sodio del carbonato de sodio), 10-15% de cal
(oxido de calcio del carbonato de calcio) como se muestra en la tabla 2.8, y un bajo
porcentaje de otros materiales para propiedades especficas tales como el color. La
densidad y el ndice de refraccin del vidrio sodo-clcico son mayores en comparacin
de los vidrios de slice debido al relleno de intersticios en la red por iones de calcio y
sodio.
Como resultado la densidad llega a 2.5 g cm-3 y el ndice de refraccin a 1.51. Con
pequeas variaciones en la composicin, varan las propiedades tpicas de vidrios sodo-
clcicos. La presencia de NaO en vidrios sodo-clcicos da como resultado otro cambio
principal en las propiedades relativas a los vidrios de silicio.
56
Una de las mayores desventajas del vidrio sodo-clcico es su relativamente alta
expansin trmica de 8 a 9 ppm K-1, por lo que posee una resistencia relativamente
pobre a cambios sbitos de temperatura. Esta limitacin debe ser tomada en cuenta al
instalar un vidrio en una ventana, adems el vidrio sodo-clcico no es resistente a
qumicos corrosivos. Las propiedades de varios tipos de vidrio sodo-calcico se
presentan en la tabla 2.9.
Su caracterizacin deber hacerse por tanto desde un punto de vista qumico y estructural
ya que en rocas que muestran diferentes historias de enfriamiento puede encontrarse todo
el espectro de posibles estados estructurales. Esto proporciona una oportunidad nica para
estudiar el modo en que responde una estructura a un ambiente geolgico que cambia
lentamente.
Los feldespatos (Si3AlO8)1- que se han enfriado de tal manera que se mantiene la estructura
correspondiente a su alta temperatura de cristalizacin se denominan feldespatos de alta
temperatura. La mayora de los feldespatos de rocas volcnicas son de este tipo.
Los feldespatos de baja temperatura son aquellos que han cristalizado en condiciones de
temperatura ms baja o bien cuya cristalizacin se ha producido por un enfriamiento lento
a partir de condiciones de alta temperatura: son caractersticos de las rocas plutnicas.
57
2.8.1. Clasificacin de los Feldespatos
Los feldespatos naturales se pueden representar en el tringulo Feldespato potsico
(KAlSi3O8)-Albita (NaAlSi3O8)-Anortita (CaAl2Si2O8), en la que la regin sombreada de
la figura 2.15 corresponde a las soluciones slidas a alta temperatura.
Los feldespatos pueden ser clasificados como miembros del sistema ternario
feldespato sdico (albita) - feldespato potsico - feldespato clcico (anortita). Los
miembros de la serie feldespato K-albita se denominan feldespatos alcalinos. Los
de composicin comprendida entre albita y anortita se denominan plagioclasas.
58
Figura 2.16 Estructura de la sanidina con presencia de
anillos de cuatro tetraedros
Fuente: Magdalena Rodas, Mineraloga 1, Universidad Complutense de
Madrid, 2011.
Todos los feldespatos tienen una disposicin similar de los enlaces entre los
tetraedros, que puede sufrir diferentes tipos de distorsiones. El origen de estas
modificaciones estructurales y la interrelacin entre los distintos factores que
intervienen en la reduccin de simetra al disminuir la temperatura, ha recibido
una importante atencin durante muchos aos por parte de los mineralogistas.
Las estructuras de los feldespatos estn formadas por un armazn tridimensional
de tetraedros SiO4 y AlO4, que comparten sus cuatro oxgenos apicales con los
tetraedros contiguos, dando una red tridimensional en cuyos huecos se sitan los
cationes Na, K, Ca y Ba. Este armazn posee cierta elasticidad y puede ajustarse
59
al tamao de los cationes cuando estos son de mayor tamao (K y Ba), originando
una simetra monoclnica.
Cuando los cationes son de menor tamao (Na y Ca), la simetra es triclnica. El
tipo estructural a partir del cual se pueden derivar todas las dems estructuras de
los feldespatos es el sanidina KAlSi3O8, el Al y el Si estn distribuidos al azar, de tal
forma que la ocupacin media de cada tetraedro es 25%Al, 50%Si. La estructura
es bastante compleja, y se describe en trminos de unidades estructurales
ideales.
Feldespatos Alcalinos
La caracterstica bsica del armazn tridimensional es la presencia de anillos de
cuatro tetraedros de SiO4 y AlO4, que comparten cuatro oxgenos T1 y T2 alternan
pares de vrtices apuntando en direcciones opuestas dando una red
tridimensional en cuyos huecos se sitan los cationes Na, K, Ca, Ba, en el caso de
la sanidina solo K situados sobre los planos de simetra m ocupando los huecos de
mayor tamao como se muestra en la siguiente figura.
60
El armazn tiene gran elasticidad lo que posibilita su acoplamiento al tamao del
catin, como ya se ha mencionado. Cuando los cationes son grandes (K, Ba), la
simetra es monoclnica (C2/m) y cuando los cationes son ms pequeos (Na y Ca)
la simetra es triclnica (C1). Estos anillos estn unidos formando lminas, como se
muestra en la figura 2.18, en la que se ven las cadenas a lo largo del eje a. En la
sanidina (KAlSi3O8), que es como ya se ha dicho, es la forma monoclnica de alta
temperatura del KAlSi3O8 el gran tamao del K impide la transformacin (el
colapso en torno al catin K) y la estructura sigue siendo monoclnica hasta que
comienza el ordenamiento (Al, Si) a unos 450C. Este ordenamiento implica
ruptura de enlace fuertes Si-O y Al-O, y por ello tiene lugar muy lentamente.
Feldespatos Potsicos
En los feldespatos potsicos naturales existen varios estados de ordenamiento Al,
Si, que dependen de la historia de enfriamiento de la roca. Sobre estos estados
intermedios podemos hacer las siguientes consideraciones generales:
El ordenamiento en la estructura (C2/m) implica una discriminacin entre las
posiciones T.
La gran lentitud del proceso de ordenamiento, y el hecho de que las fuerzas que
producen el ordenamiento sean de carcter local, hacen que sea posible observar
un ordenamiento Al, Si a escala local mientras que la simetra total del cristal
permanece monoclnica.
Esto es lo que ocurre en la ortosa, una forma del feldespato potsico que aparece
en rocas que se han enfriado con una velocidad moderada.
Feldespatos Sdicos
La albita NaAlSi3O8 es monoclnica (C2/m) por encima de 980C (monalbita),
pero colapsa en torno al Na a una estructura triclnica (C1) por debajo de esta
temperatura. En esta etapa, mientras existe poco orden Al, Si se denomina albita
de alta, pero por debajo de los 700C comienza el ordenamiento Al, Si y puede
tener lugar sin ningn cambio en la simetra hasta que a bajas temperaturas se
forma una albita de baja temperatura totalmente ordenada.
Existe solucin slida completa, con estructura (C2/m), entre NaAlSi3O8 y KAlSi3O8
a altas temperaturas, pero al descender la temperatura la diferencia de tamaos
entre Na y K, as como la diferencia en el comportamiento estructural de los dos
trminos extremos, conduce a una reduccin en el grado de miscibilidad.
62
A temperaturas por debajo de unos 300C no existe posibilidad de solucin slida
en los feldespatos alcalinos. Los feldespatos alcalinos en los que los cristales
muestran inter-crecimientos de zonas ricas en Na y zonas ricas en K formadas
por enfriamiento de una solucin slida se denominan pertitas.
63
Tabla 2.10 Reaccin de Generales de arcillas a diferentes temperaturas
TEMPERATURA REACCIONES GENERALES
30-120 C Perdida de humedad higroscpica
120-300C Desprendimiento de agua absorbida
350C Oxidacin
Deshidroxilacin (perdida de agua de
250-650C cristalizacin)
400-650C Oxidacin de las materias orgnicas y de piritas
573-575C Inversin beta-alfa cuarzo sinterizacin
400-900C Descomposicin de los carbonatos
700C Se inicia la formacin de compuestos (frricos)
900C Se inicia la vitrificacin, seguida por la fusin
980C Formacin de la espinela en la arcilla
1000C Formacin de mullita primaria
1050-1100C Formacin de vidrio, crecimiento de mullita
1200C Mas vidrio, continua el crecimiento de la mullita
1250C Cristalizacin de la mullita secundaria
Fuente: Materiales cermicos Policristalinos de Al2O3 y YAG con
Funcionalidad ptica, tesis Doctoral CSIC CINN 2009 Universidad de Oviedo.
2.10.1. Secado
El propsito del secado de cermicos es eliminar agua del cuerpo cermico
plstico antes de ser sometida a altas temperaturas. Generalmente la eliminacin
de agua se lleva acabo a menos de 100 C y puede tardar alrededor de 24 horas
para un trozo de ceramica grande. La mayora de los cimentadores orgnicos
pueden extraerse de las piezas cermicas por calentamiento en el rango de 200 a
300 C, aunque unos residuos hidrocarbonados pueden requerir un
calentamiento a temperaturas ms elevadas.
64
2.10.2. Sinterizacin
La sinterizacin es un proceso por el que un polvo prensado, denominado cuerpo
verde, es transformado en un cuerpo cermico denso y resistente, despus de ser
calentado a una temperatura suficiente para estimular los mecanismos de
transporte de materia, pero inferior al punto de fusin del material.
La sinterizacin puede ocurrir tanto en presencia como en ausencia de una fase
liquida. En el primer caso se llama sinterizacin en fase liquida, donde las
composiciones y temperaturas de calentamiento son elegidas de tal forma que se
origine un liquido durante el procesamiento. En ausencia de fase liquida el
proceso es conocido como sinterizacion en estado slido y ser el tipo de
sinterizacin con el que nos encontramos en este trabajo.
Ecuacin [2.1]
Donde:
: energa superficial
A: rea superficial
(A): cambio de energa debido a la densificacin
(A): cambio de energa debido al crecimiento y coalescencia de granos
como se muestra en la figura 2.19.
65
Figura 2.18 Dos de los caminos posibles por los que un conjunto de
partculas puede disminuir su energa: (a) Densificacin seguido de un
crecimiento de grano, en este caso ocurre la contraccin. (b)
Aumento del tamao de grano, donde los granos crecen a expensas
de los ms pequeos
Fuente: Materiales cermicos Policristalinos de Al2O3 y YAG con Funcionalidad ptica,
tesis Doctoral CSIC CINN 2009 Universidad de Oviedo.
Ecuacin [2.2]
Donde:
66
bg: energa de borde de grano
sv: energa superficial solido-vapor
: ngulo diedro de equilibrio
67
de bajo potencial qumico y pueden conducir a densificacin. A
continuacin se clasifican los diferentes mecanismos en funcin de si
conducen al crecimiento de grano o a la densificacin del material.
68
La fuerza motriz en todos los casos es la diferencia en la presin que est
asociada con las variaciones locales en curvatura. Por ejemplo, la presin en el
punto s de la figura 2.20a con una curvatura positiva, es ms grande que la del
punto n con una curvatura negativa, que a su vez resulta en una transferencia de
masa de la superficie convexa a la cncava.
69
material y otras las relacionadas con el propio proceso de sinterizacin. En la
tabla 2.11 se recoge un resumen de dichas variables.
Las variables relacionadas con el material influyen fundamentalmente en la
compactacin y sinterizacin, es decir, en la densificacin y crecimiento de grano.
El resto de variables son de carcter termodinmico y su efecto ha sido
ampliamente estudiado sobre el proceso de sinterizacin.
2.10.3. Vitrificacin
Algunos productos cermicos tales como la porcelana, productos arcillosos
estructurales y algunos componentes electrnicos contienen una fase cristalina.
Esta fase cristalina sirve como medio de reaccin para que la difusin pueda
tener lugar a menor temperatura que en el resto de material slido cermico.
Durante el tratamiento a elevadas temperaturas de este tipo de materiales, tiene
lugar un proceso llamado vitrificacin; por medio de la cual la fase cristalina se
lica y rellena los porros del material. Esta fase cristalina liquida puede reaccionar
tambin con alguno de los slidos restantes del material refractario. Bajo
enfriamiento, la fase liquida solidifica para formar una matriz vtrea que une las
partculas que no han fundido.
70
CAPITULO III
ESTUDIO DE LA MATERIA
PRIMA
3.1 EL VIDRIO
La produccin nacional de vidrio, segn el ndice de Crecimiento Industrial (ICI), ha
registrado en varios aos de la dcada del 2000 variaciones anuales positivas, as en el ao
2010 registr un incremento de 29.52%; sin embargo en los aos 2006 y 2009 registr una
cada de 0.18% y 5.77%, respectivamente. En los primeros 8 meses del ao 2011 registr
un comportamiento positivo de 41.41%.
De acuerdo a la informacin del Censo Industrial 2007, la concentracin de
establecimientos productivos dedicados a la fabricacin de vidrio y productos de vidrio, se
localizan principalmente en la provincia de Lima (47.97%), Arequipa (5.91%), Junn (5.79%) y
Cajamarca (4.98%), de un universo total de 863 empresas.
RESIDUOS
REAPROVECHABLE
S ORGANICOS
35%
72
En la figura 3.1 se muestra la composicin general de los residuos slidos domiciliarios del
Distrito de Cayma, donde el 63% son residuos que se pueden volver a utilizar es decir
reciclables y el 36% son residuos para disposicin final donde se encuentran a los vidrios
tipo sodo-calcico el cual actualmente no es reciclado.
73
3.3 RECICLAJE DEL VIDRIO
El vidrio es un material que por sus caractersticas fsicas son 100 % reciclables, es decir,
que a partir de un resto de vidrio plano se puede fabricarse uno nuevo que puede tener las
mismas caractersticas del primero. Est facilidad de reutilizacin del vidrio abre un amplio
rango de posibilidades para que la sociedad y las administraciones afectadas puedan auto
gestionarse de una manera fcil para evitar impactos negativos a su medio ambiente. El
reciclaje ha sido practicado por industrias estadounidenses, alemanas, japonesas,
canadienses, daneses, francesas, y de otros pases hace ms de 20 aos.
Es importante sealar que el reciclaje de vidrio necesita un 26% menos de energa que la
produccin original, en la que para crear un kilo de vidrio se necesitan unas 4.200
kilocaloras de energa. Adems el material generado por reciclaje reduce en un 20% la
contaminacin atmosfrica que provocara por el proceso habitual, y disminuye en un 40%
la contaminacin de agua. Otro dato, la energa que se ahorra del procesamiento de una
botella de cristal puede mantener encendida una bombilla de 100 watts durante 4 horas.
El costo del reciclaje del vidrio es menor en comparacin con otros procesos. Botellas, vasos
y recipientes de alimentos son clasificados, triturados y el material resultante es fundido, lo
que permite darle nueva forma.
74
Estas cifras difieren de las estadsticas oficiales, puesto que la informacin consultada en
gabinete no es completa, debido a que gran parte de los fabricantes de ladrillos son
informales y muchos de ellos desconocen las propiedades y caractersticas de las arcillas
para su utilizacin. Se ha constatado que diversos productos no tienen medidas estndar y
el quemado no es uniforme, presentando deformaciones, ya que slo prevalece su
experiencia, excepto la industria ladrillera mecanizada que viene trabajando dentro de
estndares normados.
Lambayeque
2%
75
En la figura 3.4 podemos apreciar que el 67% de las canteras de arcillas de la regin estn
en Caylloma, y el resto en las dems provincias. Sin embargo, la actividad ladrillera que usa
estos recursos est concentrada en la provincia de Arequipa especialmente en las
localidades de Yarabamba, Mollebaya, Quequea, Characato, Yura y Uchumayo, en este
ltimo se encuentran la ladrillera Diamante y Unidas que son las nicas ladrilleras
mecanizadas y que en la ltima dcada han mejorado la calidad de sus productos, las
mismas fueron favorecidas con capacitacin de la Cooperacin Tcnica Peruana Alemana
en la dcada de los 90.
Caraveli
11%
Caman
Caylloma
11%
67%
76
La produccin de arcilla comn en la Regin Arequipa durante el periodo 2000-2009, segn
las fuentes de informacin de la Direccin General de Minera del Ministerio de Energa y
Minas e INGEMMET que la produccin durante este periodo experiment una tasa de
crecimiento promedio anual de 57%. Es necesario recalcar que en las zonas ya
mencionadas, los materiales arcillosos son escasos y no son de ptima calidad, por lo que
los productores tienen que realizar mezclas con diversos materiales, entre ellos las arcillas
provenientes de depsitos ubicados en Hornillos (Caylloma), estas arcillas se caracterizan
por su plasticidad, resultando ser materias adecuadas.
3.4.1 Greda
La greda es una arcilla comn de mediana plasticidad, de colores variados no
uniformes que van desde el amarillo hasta el marrn, como se puede apreciar en las
siguientes fotos, presentes restos orgnicos como races y otros. El contenido de
hierro favorece la coloracin rojiza del ladrillo y presenta mayor plasticidad en
comparacin con la tierra de chacra. En la industria ladrillera la greda es un
componente importante para la produccin de ladrillos teniendo la funcin de
compactante.
77
Tabla 3.1 Composicin qumica de la greda por fusin alcalina
COMPUESTO FORMULA %
Slice (anhdrido silcico) SiO2 42.67
Almina Al2O3 18.29
Hematina Fe2O3 7.65
Oxido de Magnesio MgO 0.86
Oxido de Calcio CaO 0.66
Oxido de Sodio Na2O 2.33
Oxido de Potasio K2 O 3.01
Oxido de Manganeso Mn2O3 0.89
Perdidas por calcinacin 6.85
Fuente: SIVANA, E. & VELEZ, J. tesis Estudio del sillar de la
Cantera de Aashuayco para utilizarlo en la fabricacin
de Ladrillos de Arcilla Cocida Universidad Nacional de San
Agustn, Arequipa, Per, 2008.
78
Tabla 3.2 Composicin qumica de la tierra de chacra por fusin alcalina
COMPUESTO FORMULA %
Slice (anhdrido silcico) SiO2 59.03
Almina Al2O3 16.12
Hematina Fe2O3 5.66
Oxido de Magnesio MgO 1.08
Oxido de Calcio CaO 0.83
Oxido de Sodio Na2O 2.68
Oxido de Potasio K2 O 2.64
Oxido de Manganeso Mn2O3 1.08
Perdidas por calcinacin 4.83
Fuente: SIVANA, E. & VELEZ, J. tesis Estudio del sillar
de la Cantera de Aashuayco para utilizarlo en la
fabricacin de Ladrillos de Arcilla Cocida Universidad
Nacional de San Agustn, Arequipa, Per, 2008.
3.5 EL LADRILLO
79
indgenas americanos de las civilizaciones prehispnicas. En regiones secas construan
casa de adobe secado al sol. Las grandes pirmides de los olmecas mayas y otros
pueblos fueron construidas con adobes revestidos de piedra. Pero fue en Espaa
donde por la influencia Musulmana, el uso del ladrillo alcanzo mas difusin sobre
todo en Castilla Aragn y Andaluca.
80
Mezclado
La mezcla a mano se realiza al final del da luego de concluir las labores de labranza.
Con ayuda de una lampa se prepara en las fosas de mezclado, una premezcla de
arcilla y arena humedecidas amasando con manos y pies hasta que desaparezcan los
terrones ms grandes de arcilla. Algunos artesanos aaden otros agregados que
pueden ser aserrn, cscara de arroz o de caf, cenizas. Se deja reposar esta masa
hasta el da siguiente para que los terrones ms pequeos se deshagan, la mezcla se
vuelva consistente y adquiera la textura requerida para el moldeo o labranza. Las
impurezas de la arcilla y tierra como races de plantas, restos de arbustos y piedras
son separadas manualmente. Algunas pocas veces se hace pasar la arena por un tamiz
para eliminar impurezas u obtener un grano ms homogneo. La materia prima no se
selecciona ni es sometida a molienda para control granulomtrico. La formulacin y
caractersticas finales de la mezcla son definidas en base a su consistencia segn la
experiencia, necesidades o disponibilidad de materiales de cada artesano.
81
Moldeo o Labranza
Se utilizan moldes metlicos o de madera. Los moldes no tienen tamaos
estandarizados, difieren de un artesano a otro y de una regin a otra. Generalmente
utilizan arena muy fina (cenicero) o agua como desmoldante para facilitar el retiro de
la mezcla del molde. En condiciones climticas normales, o sea sin lluvias, un labrador
rinde semanalmente en jornadas de 8 horas de lunes a sbado por cada tipo de
ladrillo.
Secado
Los ladrillos crudos recin moldeados se depositan en canchas de secado o tendales,
que son espacios de terreno plano habilitados para este fin generalmente lo ms
cerca posible a la zona de moldeo. Los ladrillos se secan aprovechando la accin
natural del sol y el viento. Cuando llueve y no estn bajo sombra, se cubren con
mantas de plstico para protegerlos aunque esto no siempre evita que se daen por
lo que es ms recomendable construir cobertizos techados para el secado.
83
en una disposicin apropiada una al lado de otra a casi todo lo largo y ancho de la
seccin del horno para conseguir un frente de fuego horizontal.
Las briquetas utilizadas generalmente son de forma cilndrica de 10cm de dimetro
por 14,0cm de alto con un agujero en el medio para favorecer su encendido. Por
encima de la bveda armada como malecn de encendido, los ladrillos son colocados
en capas horizontales sucesivas cada una transversal respecto a la anterior (en ngulo
de 90 grados), descansando sobre su lado ms largo hasta llenar toda la altura del
horno. En los techos abovedados se hace la misma disposicin pero siguiendo la
forma de la bveda. Otra manera de armar es en la secuencia 1 , que consiste en
colocar un ladrillo a lo largo seguido de un ladrillo a lo ancho, luego un ladrillo a lo
largo y as sucesivamente.
Entre ladrillo y ladrillo se deja una separacin de tres a cinco milmetros para permitir
el flujo de aire y de los gases calientes producto de la combustin, as como para
permitir la transmisin de fuego y calor durante la coccin.
El carguo y armado del horno se realiza en jornadas de uno a ms das dependiendo
del tamao y capacidad del horno. En promedio un horno de 10 millares se carga en
10 horas con cinco personas: cuatro para alcanzar los ladrillos (bolear) y una para el
armado.
Coccin
La coccin se realiza en los hornos ladrilleros. El horneado o quemado es una
operacin netamente artesanal que el Maestro Hornero va ajustando segn los
resultados que se van obteniendo. Los canales de encendido estn construidos a la
altura del piso, atraviesan el horno de lado a lado y sus ventanas o bocas estn en los
lados de mayor longitud. Las dimensiones y caractersticas de las bocas dependen del
tipo de combustible que se va a quemar.
84
3.5.4 Normatividad de Albailera
La Norma de Albailera E.070 establece los requisitos y las exigencias mnimas para el
anlisis, el diseo, los materiales, la construccin, el control de calidad y la inspeccin
de las edificaciones de albailera estructuradas principalmente por muros confinados
y por muros armados.
UNIDAD DE ALBAILERA
Se denomina ladrillo a aquella unidad cuya dimensin y peso permite que sea
manipulada con una sola mano. Las unidades de albailera a las que se refiere esta
norma son ladrillos en cuya elaboracin se utiliza arcilla, como materia prima.
Estas unidades pueden ser slidas, huecas, alveolares o tubulares y podrn ser
fabricadas de manera artesanal o industrial.
85
Tabla 3.3 Clase de unidad de albailera para fines estructurales
86
CAPITULO IV
DESARROLLO EXPERIMENTAL
4.1. DESARROLLO EXPERIMENTAL
Para la obtencin de ladrillos de arcilla cocida reforzado con vidrio reciclado tipo sodo-calcico
con resistencia a la compresin elevada y menor temperatura de coccin es necesario primero
caracterizar las materias primas para ello se determinaron las propiedades fsicas como el
anlisis granulomtrico, % de humedad, limite de Atterberg y densidad; el anlisis elemental
mediante Fluorescencia de Rayos X (FRX) y mineralgico por Difraccin de Rayos X (DRX).
Una vez caracterizada la materia prima se procedi con el diseo experimental y se aplico el
algoritmo de Mc Lean y Anderson para mezclas de tres componentes y la influencia de
adiciones de vidrio para una regin donde se deben cumplir condiciones dirigidas a seleccionar
la mejor mezcla para la fabricacin de ladrillos de arcilla cocida. Se prepar las materias primas
segn el anlisis granulomtrico, se tamiz la greda, la tierra de chacra y el vidrio pasados por la
malla 70. Una vez obtenida la materia prima se procedi a la fabricacin de ladrillos a nivel
laboratorio pero siguiendo los parmetros de la tcnica artesanal se mezclaron las materias
primas con agua y se amaso hasta obtener la pasta adecuada para moldear las muestras, se
utilizo un molde metlico cubico de 5.32 x 5.32 x 5.32 cm. Y de acuerdo al mtodo experimental
se fabrico ladrillos de arcilla cocida en 13 bloques y cada bloque con sus respectivas
repeticiones en diferentes concentraciones de vidrio molido en los cuales se evaluaron las
caractersticas fsicas en fresco y seco.
Una vez obtenidas las muestras secas se llevo a la mufla a 900 C con una velocidad de
calentamiento de 1C seg-1, luego se realizaron ensayos fsicos de los que se obtuvo para la
mezcla 503020 el mximo resultado en Resistencia a la Compresin 28 MPa y se volvieron a
fabricar tres bloques con tres repeticiones de igual mezcla (502030) las que se llevaron a
coccin a diferentes temperaturas 750, 800, 850 y 900C, se realiz anlisis microscpico MEB,
Difraccin de Rayos X para la caracterizacin mineralgica y Fluorescencia de Rayos X para el
anlisis elemental.
88
Diagrama de Flujo de Procesos para Obtencin de Ladrillos Reforzados con Vidrio
FRX
Granulometra
Caracterizacin de las DRX
Materias Primas
Humedad
Fsicas
Atterberg
Densidad
Molienda y Vidrio
Tamizado (-70)
Preparacin de la
Materia Prima Tamizado (-70)
Greda
T. Chacra
Mezclado
Amasado
Coccin
Resistencia a la compresin
Anlisis de ladrillos
Fsicas % Absorcin de agua
cocidos a 900C
% de Contraccin
FRX % Porosidad
Resistencia a la compresin
Coccin a diferentes Ladrillo
temperaturas 750, 800, Optimo
DRX
850 y 900 C.
MEB
89
4.2. CARACTERIZACIN DE LAS MATERIAS PRIMAS
Las Materias Primas utilizadas en esta investigacin fueron obtenidas, los vidrios reciclados
de los residuos urbanos del distrito de Cayma y las arcillas (Greda y tierra de chacra) de la
zona de Polobaya.
90
Es importante conocer la cantidad de humedad que tienen las, tericamente se sabe
que las arcillas ms plsticas son las que mayor humedad que retienen en su
composicin. El proceso se sigui de la siguiente manera:
Se pes una luna de reloj limpio y seco en una balanza analtica.
Luego se adicion la arcilla a la luna y se registr el peso total.
Se lleva a la estufa durante seis horas a 110 C.
Se enfra en un desecador la muestra y se registrar el peso total, a este peso se le
resta el peso de la luna y se determina la masa final de las muestras.
El porcentaje de humedad se calcula con la siguiente frmula:
Ecuacin [4.1]
Donde:
mh = masa hmeda
ms115C = masa de arcilla a 115 C
Los lmites se basan en el concepto de que en un suelo de grano fino solo pueden
existir 4 estados de consistencia segn su humedad. As, un suelo se encuentra
en estado slido, cuando est seco. Al agregrsele agua poco a poco va pasando
sucesivamente a los estados de semislido, plstico y finalmente lquido. Los
contenidos de humedad en los puntos de transicin de un estado al otro son los
denominados lmites de Atterberg en este caso vamos a determinar el ndice de
plasticidad.
Para determinar el lmite lquido y plstico de nuestras arcillas nos basamos en la NTP
339.129 o ASTM D 4318-00.
91
Determinacin de Lmite Lquido
El objetivo de hallar el lmite lquido es para conocer la cantidad de humedad
necesaria para que la arcilla en estudio pase del estado plstico al estado
semilquido.
Pesamos 100 g del material en estudio (greda y tierra de chacra).
Seguidamente procedemos a agregar agua hasta el punto donde la masa se
hace plstica.
Dejamos reposar la masa de la muestra de arcilla para que la humedad se
homogenice.
Procedemos a colocar la pasta en cuchara de casa-grande tomando en cuenta
la superficie sea plana con un espesor de 10mm. En su parte ms baja de la
cuchara.
Luego se procede hacer la marca con el acanalador teniendo en cuenta que no
tenga desprendimientos de material o porosidad en el caso de que ocurriera
se repetir el ensayo.
Para esto es necesario conformar una masa del suelo, de modo tal que
podamos amasar una esfera y posteriormente dar lugar a la formacin
de cilindros con la palma de la mano.
Unas vez amasadas (greda y tierra de chacra) procedemos a colocar la
bola en una superficie plana donde con la ayuda de la palma de la
mano podremos conseguir y dar forma de cilindro con un dimetro de
3mm.
La prueba continua con la misma metodologa hasta conseguir que al
formar el cilindro este se parta en pedazos 5 a 10mm
Seguidamente procedemos a calcular el porcentaje de humedad de la
muestra
El procedimiento de repite para 4 pruebas
El resultado final ser el promedio de las tres mediciones.
93
ndice de plasticidad (IP)
Con el ndice de plasticidad puede evaluarse el grado de amasado que
permite el suelo mientras se encuentre en su consistencia plstica, este
ndice se define como:
Ecuacin [4.2]
Donde:
IP, es ndice de plasticidad
LL, es lmite liquido
LP, es lmite plstico
La lnea A separa las arcillas inorgnicas de los limos inorgnicos, las arcillas
inorgnicas se encuentran por encima de esta lnea y los limos inorgnicos
por debajo de esta. Los limos inorgnicos estn situados por debajo de esta
lnea en el intervalo de 30 a 50 del lmite lquido, las arcillas inorgnicos se
ubican por debajo de esta lnea con un lmite lquido mayor a 50. La
ecuacin de la lnea A es:
94
Ecuacin [4.3]
Ecuacin [4.4]
Las muestras deben ser molida muy finamente para ello se uso un mortero.
Secar la muestra a 110 C por espacio de 2 horas aproximadamente.
Enfriar la muestra.
El vaso de precipitados (fiola) limpio y seco debe ser pesado. Anotar dicha
masa como M1.
El vaso (fiola) con la muestra se le llena de agua y se lleva a ebullicin, luego
se hace enfriar el vaso (fiola) para posteriormente volver a pesar, esta masa
ser M2.
Llenar el vaso de precipitados (fiola) con agua, pesar esta masa ser M3.
En el vaso (fiola) limpio y seco se introduce una pequea cantidad de muestra,
y se vuelve a pesar, esta masa ser M4.
95
El clculo de la densidad real es el siguiente:
Ecuacin [4.5]
96
provocara que los tomos que conforman a este dispersen a la onda incidente tal
que cada uno de ellos produce un fenmeno de interferencia que para
determinadas direcciones de incidencia ser destructivo y para otras constructivo
surgiendo as el fenmeno de difraccin. La informacin que proporciona el patrn
de difraccin de Rayos X, se puede ver como dos aspectos diferentes pero
complementarios: por un lado, la geometra de las direcciones de difraccin
(condicionadas por el tamao y forma de la celdilla elemental del cristal), nos
ofrecen informacin sobre el sistema cristalino. Y por otro lado la intensidad de los
rayos difractados, estn ntimamente relacionados con la naturaleza de los tomos y
las posiciones que ocupan en la red, talque su medida constituye la informacin
tridimensional necesaria para conocer la estructura interna del cristal.
97
4.3. DISEO EXPERIMENTAL
Para el estudio de la influencia de las adiciones de vidrio se hace mediante el diseo
experimental para Mezclas con restricciones de Mc Lean Anderson, para una regin donde
se deben cumplirlas las siguientes condiciones, dirigidas a seleccionar la mejor mezcla para
la fabricacin de ladrillos de arcilla cocida.
Las siguientes restricciones estn en base a las caractersticas y tipo de fabricacin que en
este caso es un procedimiento artesanal. Se debe de cumplir las siguientes restricciones:
RESTRICCIONES
0.50 X1 0.80
0.10 X2 0.20
0.10 X3 0.30
Fuente: Elaboracin Propia
Ecuacin [4.6]
Rx1 = 0.30
Rx2 = 0.10
Rx3 = 0.20
98
Ecuacin [4.7]
RL= 1-(0.50+0.10+0.10)
RL = 0.30
Entonces se cumple: Ri RL
Ecuacin [4.8]
RU = (0.80+0.20+0.30)-1
RU = 0.30
Entonces se cumple: Ri RU
Debido a que ningn Ri > RL y ningn Ri > RU para todo X1, X2, y X3 por lo tanto las
restricciones no presentan inconsistencias y se puede usar el algoritmo.
Ecuacin [4.9]
Donde:
N, es el nmero de ensayos
q, es el nmero de variables
Si:
Entonces: N
99
Tabla 4.3 Mezclas y numero de pruebas
N Mezclas X1 X2 X3
1 1 0.500 0.200 0.300
2 2 0.600 0.150 0.250
3 3 0.800 0.100 0.100
4 1-2 0.550 0.175 0.275
5 1-3 0.650 0.150 0.200
6 1-4 0.525 0.188 0.288
7 2-3 0.700 0.125 0.175
8 2-4 0.575 0.163 0.263
9 3-4 0.675 0.138 0.188
10 1-2-3 0.633 0.150 0.217
11 2-3-4 0.650 0.142 0.208
12 1-2-3-4 0.613 0.156 0.231
(*) 0.800 0.200 0
Fuente: Elaboracin Propia
(*)Mezcla patrn (sin vidrio)
100
4.3.2. Definicin de Variables
Para nuestra investigacin se plantean las siguientes variables dependientes e
Independientes:
101
Figura 4.7 Molino de barras, vidrio molido
Fuente: Elaboracin Propia
102
4.5.1. Codificacin de muestras
Como cada muestra tiene diferentes proporciones de materiales y para evitar la
confusin se codifico las muestras de la siguiente manera:
Ecuacin [4.10]
Ecuacin [4.11]
103
Ecuacin [4.12]
Donde:
Cs= Contraccin por secado.
Cc= Contraccin por cocido.
Ct= Contraccin total.
Vh= Volumen despus del moldeo.
Vs= Volumen despus del secado.
Vc= Volumen despus del cocido.
Ecuacin [4.13]
Ecuacin [4.14]
Ecuacin [4.15]
Donde:
: peso hmedo
: peso de la muestra seca
: peso de la muestra cocida
%Hs: porcentaje de humedad despus del secado
%Hc: porcentaje de humedad despus de la coccin
%Ht: porcentaje de humedad total
104
Ecuacin [4.16]
Ecuacin [4.17]
Donde:
%P: porcentaje de porosidad
: densidad real
: densidad aparente
: peso de la muestra seca
: peso saturado con agua
: peso suspendido
: densidad del agua
Ecuacin [4.18]
105
Donde:
%Absorcin mx.: porcentaje mximo de absorcin de agua
: Peso de las muestras secas
: Peso de agua saturada en 24 horas.
Luego se procedi a tomar las medidas loa lados de las caras de la muestra que
tendrn contacto con los vstagos de la mquina para determinar el rea en el que se
ejecutara la fuerza. Se prepara la mquina para el ensayo se coloca la muestra y se
ejecuta la fuerza en el que se rompe la muestra y se hace la respectiva lectura.
Ecuacin [4.19]
Donde:
: Resistencia a la compresin de las muestras (kgf cm-2)
: Carga de rotura ejercida por la maquina (kgf)
: rea promedio de las dos caras de la muestra (cm 2)
106
Figura 4.10 Maquina de ensayo universal SENCICO.
Fuente: Elaboracin Propia
Para realizar anlisis en MEB, por ser las muestras de ladrillo no conductoras, se
necesito realizar un tratamiento previo de dopa miento de oro a la superficies a
analizar para ello se utilizo un metalizador DESK II.
107
-
109
CAPITULO V
ANALISIS DE RESULTADOS
DISCUSIONES
5.1. RESULTADO DE CARACTERIZACION DE LAS MATERIAS PRIMAS
100
Passing (%)
60
20
0 100 200 300 400 500 600 700 800
Abertura (m)
Vidrio Greda T. Chacra
Como se puede observar en las tablas anteriores y en la grafica 5.1 las curvas
granulomtricas de las materias primas se intersecan alrededor de 70% de Passing y
con abertura de alrededor de 200 m, por lo que se elige una granulometra de malla
menos 70 (212 m) para elaborar nuestras muestras.
111
Tabla 5.2 Resultado del anlisis de % de humedad de la tierra de chacra
N Ensayo Masa hmeda Masa seca % Humedad
1 100 98.32 1.68
2 100 99.14 0.86
3 100 98.64 1.36
4 100 98.83 1.17
Promedio 1.27 0.34
Fuente: Elaboracin Propia
50
% de Humedad
40
30
y = -0.7065x + 52.965
R = 0.9368
20
5 50
Numero de golpes
% de humedad Greda Lineal (% de humedad Greda)
112
De acuerdo a la ecuacin de la figura 5.2 el limite liquido para la Greda con 25 golpes
seria 35.30% y reemplazando en la ecuacin 4.2 el IP es 11.17.
Tabla 5.4 Resultado del Lmite plstico de Greda
Tara + masa Tara + masa Masa Masa Masa de %
N Tara
hmeda seca hmeda seca agua Humedad
1 44.76 45.77 45.58 1.01 0.82 0.19 18.81
2 42.48 43.32 43.19 0.84 0.71 0.13 15.48
3 43.89 44.40 44.31 0.51 0.42 0.09 17.65
4 43.98 44.64 44.53 0.66 0.55 0.11 16.67
Promedios 0.762 0.622 0.14 18.28
Fuente: Elaboracin Propia
45
% de Humedad
35
25
y = -0.9887x + 51.068
R = 0.6459
15
5 Numero de golpes 50
% de humedad T. de chacra Lineal (% de humedad T. de chacra)
113
De acuerdo a la ecuacin de la figura 5.3 el limite liquido para la Tierra de chacra a
25 golpes seria 26.35% y reemplazando en la ecuacin 4.2 el IP es 4.64.
De la figura 5.4 y de acuerdo a los resultados antes demostrados tanto como para el
lmite liquido y plstico de la greda y tierra de chacra se puede indicar que la greda es
114
una arcilla inorgnica de mediana plasticidad y la tierra de chacra es una arcilla
inorgnica de baja plasticidad.
115
Tabla 5.9 Composicin elemental de las materias primas por FRX.
Tabla 5.10 Comparacin de los componentes de las materias primas por FRX.
116
5.1.6. Resultado de Anlisis de Difraccin de Rayos X
Desde el punto de vista mineralgico se pueden diferenciar los materiales en la figura
5.5 se muestra los diferentes difractogramas para las materias primas del anlisis
cualitativo. La greda presenta fases mineralgicas como la albita (a), anortita (A),
caolinita (K), (Q) cuarzo y ortoclasa (O), lo que indica la presencia de feldespatos y
filosilicatos; sin embargo en el difractograma de la tierra de chacra no estn presentes
caolinita (K), lo que indica la presencia mayoritaria de feldespatos y el difractograma
del vidrio indica que es amorfo por presentarse un cumulo de intensidades y no
presenta picos caractersticos.
DIFRACTOGRAMAS DE LAS MATERIAS PRIMAS
Figura 5.5 DRX de comparacin de las Materias Primas donde (a) albita, (A) anortita, (K)
caolinita, (Q) cuarzo y (O) ortoclasa.
Fuente: Elaboracin Propia
117
cocida (Cc) es la contraccin despus de haber sido cocida, y la contraccin total es la
contraccin de la fase hmeda a cocida (desde que fueron elaboradas las muestras
hasta despus de cocidas). De la tabla 5.11 se muestran los promedios de las
contracciones totales de los 13 combinaciones de las muestras donde se aprecia que
la ms alta contraccin la presenta la muestra patrn 005020 ( 10.17 1.24 %) y la
menor contraccin en la muestra 305020 (5.69 0.58 %).
CONTRACCION TOTAL
12
% de Contraccin Total
10
8
6
4
2
0
0 2 4 6 8 10 12 14
Tipo de Muestra
118
5.2.2. Resultado del porcentaje de Humedad
En este caso el mayor porcentaje de humedad es de la muestra 008020 (24.11 1.44
%) y de las muestras que llevan vidrio varan desde 10.32 % hasta 18.62 %.
Tabla 5.12 Promedios del porcentaje de humedad total
N Muestras Promedio Ht (%)
1 00_8020 24.11 1.44
2 1030_5020 10.32 2.53
3 2025_6015 15.53 3.37
4 3010_8010 18.62 2.18
5 4028_5517 13.58 2.22
6 5020_6515 15.92 1.60
7 6029_5219 12.19 1.98
8 7018_7012 16.39 2.33
9 8026_5713 12.90 1.91
10 9019_6714 14.86 1.57
11 10022_6315 12.72 2.31
12 11021_6514 15.47 3.27
13 12023_6114 14.20 1.63
Fuente: Elaboracin Propia
PORCENTAJE DE HUMEDAD
30
25
% de Humedad
20
15
10
0
0 2 4 6 8 10 12 14
Tipo de muestra
119
5.2.3. Resultados del anlisis del porcentaje de Porosidad
Tabla 5.13 Resultado del porcentaje de porosidad
Densidad Densidad Porosidad
Muestras
real aparente %
00_8020 1.87 1.48 0.04 20.93
1030_5020 2.27 0.33 2.03 10.64
2025_6015 2.02 0.01 1.79 0.16 11.58
3010_8010 1.96 0.06 1.65 0.12 15.68
4028_5517 2.10 0.51 1.86 0.11 11.38
5020_6515 2.08 0.17 1.80 0.10 13.24
6029_5219 2.14 0.03 1.91 0.21 10.79
7018_7012 2.03 0.02 1.75 0.09 13.76
8026_5713 2.01 0.01 1.75 12.94
9019_6714 2.05 0.04 1.71 0.12 16.58
10022_6315 2.07 0.02 1.78 0.05 14.18
11021_6514 2.06 0.02 1.73 0.25 16.12
12023_6114 2.04 0.01 1.72 0.16 15.56
Fuente: Elaboracin Propia
120
PORCENTAJE DE POROSIDAD
25
% de Absorcin 20
15
Mxima
10
0
0 2 4 6 8 10 12 14
Tipos de Mezclas
121
De los resultados se puede observar un mximo de 30.85 6.80 % de absorcin
mxima para la muestra 11021_6514 y un mnimo porcentaje de absorcin de
14.54 3.46 % para la muestras 6029_ 5219.
Del ensayo de compresin simple se puede decir que la mxima resistencia presento
la mezcla 1030_5020 con 28.39 2.04 MPa y la mnima resistencia la obtuvo la
muestra 3010_8010 con 18.01 5.31 MPa, la muestra patrn 00_8020 alcanzo
14.87 1.23 MPa.
122
RESISTENCIA A LA COMPRESION
30
Resistencia a la Compresin (MPa)
1030_5020, 25.04
25
6029_5219, 21.54
12023_6114, 20.69
3010_8010, 19.33 7018_7012, 20.57
20 9019_6714, 19.73
2025_6015, 19.85 5020_6515, 20.36 8026_5713, 20.08 11021_6514, 19.22
4028_5517, 19.04 10022_6315, 19.01
15 00_8020, 14.87
10
0 2 4 6 8 10 12 14
Tipo de Mezcla
COMPARACION DE DIFRACTOGRAMAS
123
5.3.2. Resultado de Fluorescencia de Rayos X
Tabla 5.17 Composicin elemental de la mezcla 305020
MEZCLA UNID.
K 1.8 0.2 %W
Ca 2.8 0.3 %W
Ti 3105 259 ppm
V < 150 ppm
Cr 65 25 ppm
Mn 511 38 ppm
Fe 3.3 1 %W
Cu 16 ppm
Zn 361 9 ppm
Ga < 12 ppm
As < 17 ppm
Br <3 ppm
Rb 42 2 ppm
Sr 213 9 ppm
Y 9 1 ppm
Zr 92 5 ppm
Nb 4.0 0.7 ppm
Ba < 3000 ppm
Pb 124 12 ppm
Th 6 1 ppm
U <2 ppm
Matriz 89.5 %
Fuente: Elaboracin Propia
Tabla 5.18 Comparacin de los componentes mayores de las materias primas por FRX.
124
5.3.3. Microscopia Electrnica de Barrido MEB
Muestra Sin Vidrio Muestra de mejor Resistencia
100 m 100 m
50 m 50 m
5 m 5 m
Figura 5.11 Microfotografas de MEB comparando la morfologa la muestra 305020 con la muestra
de referencia sin vidrio cocidas a 900C y a diferentes aumentos.
Fuente: Elaboracin Propia
125
5.4. RESULTADO DE LOS ANALISIS DE MUESTRAS COCIDAS A DIFERENTES TEMPERATURAS
5.4.1. Resistencia a la compresin
Tabla 5.19 Resistencia a la compresin a diferentes temperaturas
Promedio de Areas Carga RESISTENCIA RESISTENCIA
Muestras
cm2 pulg2 lb Lb pulg-2 Kgf cm-2 MPa Promedio
750130_5020 25.76 10.14 12600.00 1242.63 87.37 8.57
750230_5020 26.73 10.52 14400.00 1368.54 96.22 9.43 9.48
750330_5020 26.01 10.24 15500.00 1513.65 106.42 10.44
800130_5020 26.00 10.24 25500.00 2491.16 175.15 17.17
800230_5020 27.83 10.95 25600.00 2336.90 164.30 16.11 17.03
800330_5020 26.27 10.34 26700.00 2582.07 181.54 17.80
850130_5020 26.52 10.44 32400.00 3103.17 218.17 21.39
850230_5020 26.88 10.58 28900.00 2730.66 191.98 18.83 21.42
850330_5020 26.52 10.44 36400.00 3486.28 245.11 24.03
900130_5020 27.30 10.75 40600.00 3777.44 265.58 26.04
900230_5020 27.30 10.75 46300.00 4307.68 302.86 29.70 28.39
900330_5020 27.19 10.71 45700.00 4268.49 300.10 29.43
Fuente: Elaboracin Propia
20
(MPa)
10
0
700 750 800 850 900 950
Temperatura de Coccin
126
5.4.2. Microscopia ptica
10 X 30X
900 C 900 C
850 C 850 C
800 C 800 C
750 C 750 C
127
5.4.3. Difraccin de Rayos X
Figura 5.14 Comparacin secuenciales difractogramas de DRX de muestras cocidas con vidrio a
diferentes temperaturas donde (A) anortita, (a) albita y (Q) cuarzo.
Fuente: Elaboracin Propia
Tabla 5.21 Comparacin de resultados ladrillo sin vidrio- con 30% de vidrio sodo-calcico.
128
5.5. ANALISIS DE RESULTADOS
Tabla 5.22 Efectos Estimados Modelo Completo para Resistencia Compresin (MPa)
Suma de Cuadrado
Fuente Gl Razn-F Valor-P
Cuadrados Medio
Media 15645.0 1 15645.0
Lineal 198.03 2 99.0151 14.15 0.0000
Cuadrtico 61.5549 3 20.5183 3.63 0.0239
Cbico Especial 1.77623 1 1.77623 0.31 0.5835
Cbico 21.9044 3 7.30148 1.30 0.2945
Error 145.678 26 5.60301
Total 16074.0 36
Fuente: Elaboracin Propia
129
Tabla 5.24 ANOVA para Resistencia Compresin
Fuente Suma de Gl Cuadrado Razn-F Valor-P
Cuadrados Medio
Modelo 285.09 9 31.6767 5.73 0.0002
Cbico
Error total 143.854 26 5.53285
Total (corr.) 428.944 35
Fuente: Elaboracin Propia
Esta tabla muestra un anlisis de varianza para el modelo cbico, dado que el
valor-P para este modelo es menor que 0.05, existe una relacin estadsticamente
significativa entre Resistencia Compresin y los componentes, con un nivel de
confianza del 95.0%.
130
Donde:
R: Resistencia a la Compresion
G: porcentaje de greda
V: porcentaje de vidrio
T: porcentaje de tierra de chacra
Cada tem corresponde a los valores de los componentes en una fila especfica
del archivo de datos. Para generar pronsticos para combinaciones adicionales
de los componentes, agregue filas al final del archivo de datos. En cada fila,
introduzca los valores para los componentes pero deje vacas las celdas para la
respuesta. Cuando regrese a esta ventana, se habrn agregado pronsticos a la
tabla para las nuevas filas pero el modelo no se ver afectado.
131
Figura 5.15 Superficie de respuesta estimada
Fuente: Elaboracin Propia
132
5.5.2. Anlisis de Muestras a Diferentes Temperaturas
Variable dependiente: RESISTENCIA (MPa)
Factor: TEMPERATURA (C)
Nmero de observaciones: 12
Nmero de niveles: 4
133
Tabla 5.27 Rangos para COMPRESION por temperatura
temperatura Casos Media Grupos
Homogneos
750 3 9.48 X
800 3 17.026 X
7
850 3 21.416 X
7
900 3 28.39 X
Fuente: Elaboracin Propia
134
Figura 5.18 Grafica de Caja y Bigotes de la resistencia a La compresin (MPa) con
respecto a la temperatura de coccin (C)
Fuente: Elaboracin Propia
5.6. DISCUSIONES
Segn Vorrada et al. (2009), obtuvieron que con adiciones de vidrio menores al 30 % en
peso y temperatura de quemado de 1100C tuvieron resultado de resistencia a la
compresin de 16 a 41MPa y de acuerdo al desarrollo experimental del presente estudio
los resultados obtenidos para el uso de vidrio reciclado sodo-calcico como reforzante en
la elaboracin de ladrillos de arcilla cocida es de 30% en peso de vidrio sodo-calcico, 20%
de greda y 50% de tierra de chacra cocidas a una temperatura de 900C se tuvieron
resultados de 28 MPa y a 800C de 17 MPa en la resistencia a la compresin; por lo que
hay concordancia en las dos investigaciones ya que los resultados son similares, lo que
genera la confianza para utilizar el vidrio reciclado sodo-calcico como un componente
(reforzante) en la industria ladrillera.
135
CAPITULO VI
CONCLUSIONES
RECOMENDACIONES
5.1 CONCLUSIONES
5.2 RECOMENDACIONES
Tu vida tiene un propsito grandioso, viniste a este mundo a aprender, a ser un mejor
ser humano, a sanar, a compartir, a ser feliz, y ser un instrumento de amor en el
mundo
137
REFERENCIAS
BIBLIOGRAFICAS
REFERENCIAS BIBLIOGRAFICAS
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Materias primas para la fabricacin de soportes de baldosas cermicas. Castelln.
Instituto de Tecnologa Cermica-AICE. 292 p.
2. BOCH, P., & NIEPCE, J., (2001), Ceramic Materials Pocesses, Propertier and Aplications,
(1ra ed.) Great Britain, Antony Rowe Ltd.
3. CALLISTER, W., (2001) Fundamentals of Materials Science and Engineering (5ta ed.) USA,
Jhon Wiley & Sons.
4. CANAHUA, H., (2011) Diseos Experimentales en Medio Ambiente (1ra ed.) Tacna
Universidad Nacional Jorge Basadre Grohmann.
5. CHAWAKITCHAREON, P., TIANSIRI, W., (2008). Utilization of glass scrap as raw material
for ceramic tile production. Thai Environmental Engineering Journal 1, 103 112.
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Industriales de Arequipa y Alrededores Boletn 22 Serie B (8-58 pp.). Lima Geologa
Econmica INGEMMET.
7. DONDI, M., GUARINI, G., RAIMONDO, M., ZANELLI, C., (2009). Recycling PC and TV
waste glass in clay bricks and roof tiles. Waste Management 29, 19451951.
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the AIPEA Nomenclature and CMS Nomenclature Committees. Clays Clay Miner 43:255-256.
9. HUANG, W., (1968) Petrologa (1ra ed.). Mxico Unin Tipogrfica Hispano Americana
(199-230 pp.)
10. LAWSON, J., MADRIGAL, J., ERJAVEC, J., (1992) Estrategias Experimentales para el
Mejoramiento de la Calidad en la Industria (1era ed.) Mxico, Grupo Editorial
Iberoamericano.
11. LEVIN, E., ROBBINS, C., & McMurdie, (1964) Phase Diagrams for Ceramists (1ra ed.).
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139
13. MARIN, W., (2010). Uso de los Relaves Mineros en la fabricacin de Ladrillos de Arcilla
Cocida. Arequipa Universidad Nacional de San Agustn.
140
ANEXOS
141
ANEXO A
RESULTADO DE ENSAYOS
RESULTADOS DE CARACTERIZACION DE LA MATERIA PRIMA
142
Tabla A.3 Anlisis Granulomtrico Tierra de Chacra
Malla Abertura Retenido Retenido Acumulado Passing
# m (g) (%) (%) (%)
20 840 4.58 1.83 1.83 98.17
50 300 12.56 5.02 6.86 93.14
70 212 25.63 10.25 17.11 82.89
100 150 72.89 29.16 46.26 53.74
200 74 32.71 13.08 59.35 40.65
275 53 4.89 1.96 61.30 38.70
<275 <53 96.74 38.70 100.00 0.00
Total 250.00 100 0.00 100.00
Fuente: Elaboracin Propia
143
RESULTADOS DE MUESTRA DE LADRILLO
Tabla A.4 Resultados del las contracciones seca (Cs), cocida (Cc) y contraccin total (Ct).
Hmedo (h) Seco (s) Cocido (c) Promedios
Muestras Cs Cc Ct
l h a l h a l h a Ct
01_8020 5.33 5.31 5.32 5.28 5.26 5.25 5.18 5.15 5.18 3.16 5.23 8.22
02_8020 5.35 5.33 5.35 5.27 5.20 5.24 5.16 5.10 5.13 5.87 5.99 11.51
03_8020 5.34 5.29 5.33 5.29 5.25 5.16 5.19 5.18 5.05 4.82 5.26 9.83 10.17
04_8020 5.37 5.33 5.28 5.23 5.25 5.24 5.17 5.11 5.11 4.80 6.17 10.67
05_8020 5.38 5.40 5.27 5.29 5.36 5.21 5.18 5.14 5.14 3.51 7.36 10.61
1130_5020 5.34 5.31 5.29 5.28 5.25 5.20 5.25 5.20 5.15 3.90 2.46 6.27
1230_5020 5.32 5.33 5.30 5.26 5.27 5.25 5.23 5.22 5.20 3.16 2.45 5.54
1330_5020 5.30 5.28 5.34 5.28 5.24 5.22 5.26 5.17 5.15 3.35 3.03 6.28 5.69
1430_5020 5.29 5.30 5.28 5.25 5.25 5.26 5.20 5.18 5.20 2.06 3.39 5.38
1530_5020 5.31 5.40 5.34 5.28 5.35 5.31 5.24 5.28 5.26 2.04 2.98 4.96
2125_6015 5.36 5.33 5.30 5.33 5.30 5.18 5.20 5.26 5.14 3.36 3.92 7.15
2225_6015 5.44 5.38 5.35 5.35 5.34 5.29 5.30 5.22 5.19 3.48 4.99 8.30
2325_6015 5.38 5.30 5.36 5.34 5.24 5.31 5.28 5.24 5.21 2.78 2.99 5.69 7.53
2425_6015 5.40 5.33 5.37 5.37 5.24 5.25 5.26 5.17 5.18 4.42 4.65 8.86
2525_6015 5.30 5.40 5.34 5.26 5.34 5.27 5.21 5.26 5.15 3.14 4.66 7.65
3110_8010 5.43 5.40 5.38 5.38 5.35 5.20 5.29 5.22 5.10 5.12 5.91 10.73
3210_8010 5.38 5.35 5.36 5.31 5.29 5.31 5.25 5.12 5.24 3.32 5.57 8.70
3310_8010 5.40 5.39 5.40 5.35 5.33 5.32 5.15 5.21 5.20 3.48 8.03 11.23 9.83
3410_8010 5.36 5.33 5.30 5.30 5.28 5.25 5.18 5.16 5.17 2.97 5.94 8.74
3510_8010 5.34 5.40 5.36 5.30 5.32 5.22 5.25 5.18 5.13 4.77 5.21 9.74
4128_5517 5.35 5.30 5.33 5.31 5.25 5.29 5.30 5.20 5.10 2.42 4.69 7.00
4228_5517 5.41 5.38 5.40 5.28 5.35 5.26 5.35 5.15 5.10 5.46 5.43 10.60
4328_5517 5.30 5.33 5.35 5.26 5.28 5.27 5.22 5.21 5.22 3.16 3.01 6.07 7.73
4428_5517 5.36 5.33 5.30 5.30 5.25 5.23 5.25 5.15 5.16 3.89 4.13 7.86
4528_5517 5.33 5.31 5.35 5.28 5.27 5.29 5.21 5.18 5.21 2.79 4.48 7.14
5120_6515 5.37 5.30 5.33 5.32 5.27 5.28 5.35 5.15 5.12 2.42 4.70 7.01
5220-6515 5.40 5.36 5.37 5.36 5.30 5.31 5.30 5.20 5.10 2.95 6.82 9.57
5320_6515 5.38 5.35 5.33 5.33 5.26 5.27 5.25 5.21 5.20 3.69 3.73 7.29 8.60
5420_6515 5.35 5.30 5.36 5.31 5.27 5.31 5.24 5.25 5.05 2.23 6.51 8.59
5520_6515 5.42 5.40 5.38 5.36 5.34 5.28 5.25 5.22 5.14 4.02 6.79 10.54
5.33 5.32 5.29 5.28 5.26 5.20 5.24 5.20 5.15 3.72 2.83 6.45
6129_5219
5.32 5.33 5.30 5.26 5.27 5.25 5.23 5.22 5.16 3.16 3.20 6.26
6229_5219 5.31 5.27 5.34 5.28 5.22 5.22 5.26 5.17 5.15 3.72 2.66 6.28
6329_5219 5.29 5.30 5.28 5.25 5.25 5.26 5.20 5.18 5.21 2.06 3.20 5.20 6.15
6429_5219 5.34 5.38 5.34 5.28 5.34 5.28 5.24 5.28 5.18 2.96 3.73 6.58
6529_5219 5.33 5.32 5.29 5.28 5.26 5.20 5.24 5.20 5.15 3.72 2.83 6.45
Fuente: Elaboracin Propia
144
Tabla A.5 Resultados del las contracciones seca (Cs), cocida (Cc) y contraccin total (Ct).
Hmedo (h) Seco (s) Cocido (c) Promedios
Muestras Cs Cc Ct
l h a l h a l h a Ct
7118_7012 5.36 5.33 5.33 5.30 5.28 5.26 5.22 5.17 5.19 3.33 4.84 8.02
7218_7012 5.35 5.37 5.36 5.29 5.32 5.33 5.25 5.20 5.10 2.59 7.18 9.59
7318_7012 5.38 5.33 5.38 5.33 5.25 5.31 5.25 5.21 5.20 3.69 4.28 7.80 8.45
7418_7012 5.33 5.30 5.36 5.28 5.27 5.23 5.22 5.25 5.15 3.89 3.02 6.79
7518_7012 5.40 5.41 5.36 5.36 5.34 5.31 5.25 5.22 5.14 2.94 7.32 10.04
8126_5713 5.41 5.35 5.32 5.35 5.29 5.25 5.30 5.21 5.18 3.50 3.73 7.11
8226_5713 5.36 5.38 5.39 5.31 5.33 5.31 5.29 5.25 5.23 3.31 3.35 6.55
8326_5713 5.35 5.33 5.37 5.29 5.28 5.30 5.22 5.21 5.26 3.33 3.37 6.58 7.52
8426_5713 5.33 5.33 5.38 5.26 5.25 5.31 5.18 5.18 5.16 4.06 5.58 9.41
8526_5713 5.40 5.34 5.36 5.27 5.28 5.29 5.21 5.24 5.21 4.76 3.37 7.97
9119_6714 5.38 5.35 5.40 5.30 5.29 5.31 5.22 5.20 5.25 4.22 4.28 8.31
9219_6714 5.40 5.34 5.31 5.33 5.27 5.28 5.25 5.18 5.15 3.14 5.57 8.53
9319_6714 5.34 5.37 5.35 5.26 5.31 5.28 5.22 5.23 5.22 3.87 3.37 7.11 8.29
6419_6714 5.41 5.36 5.36 5.36 5.30 5.29 5.26 5.25 5.17 3.31 5.00 8.14
6419_6714 5.36 5.38 5.40 5.29 5.31 5.33 5.22 5.25 5.15 3.85 5.73 9.36
10122_6315 5.41 5.33 5.34 5.32 5.27 5.28 5.28 5.21 5.20 3.86 3.37 7.10
10222_6315 5.39 5.36 5.39 5.33 5.32 5.34 5.27 5.25 5.29 2.76 3.34 6.01
10322_6315 5.37 5.35 5.34 5.31 5.28 5.25 5.26 5.22 5.19 4.06 3.19 7.11 7.12
10422_6315 5.40 5.36 5.37 5.36 5.29 5.32 5.27 5.24 5.24 2.95 4.07 6.90
10522_6315 5.42 5.40 5.35 5.37 5.35 5.29 5.25 5.23 5.22 2.94 5.69 8.47
11121_6514 5.40 5.38 5.37 5.35 5.31 5.29 5.30 5.25 5.21 3.67 3.54 7.08
11221_6514 5.37 5.41 5.38 5.32 5.34 5.31 5.26 5.27 5.28 3.49 2.98 6.36
11321_6514 5.42 5.34 5.35 5.37 5.29 5.27 5.31 5.23 5.21 3.32 3.35 6.56 6.96
11421_6514 5.39 5.38 5.43 5.35 5.32 5.36 5.29 5.26 5.25 3.11 4.24 7.23
11521_6514 5.41 5.39 5.35 5.36 5.33 5.27 5.27 5.25 5.21 3.49 4.26 7.60
12123_6114 5.35 5.32 5.36 5.29 5.25 5.30 5.21 5.15 5.18 3.51 5.58 8.89
12223_6114 5.36 5.38 5.41 5.32 5.33 5.35 5.26 5.25 5.27 2.76 4.07 6.72
12323_6114 5.35 5.40 5.30 5.30 5.33 5.26 5.22 5.24 5.20 2.96 4.28 7.11 7.39
12423_6114 5.33 5.32 5.36 5.26 5.25 5.30 5.21 5.19 5.24 3.70 3.19 6.77
12523_6114 5.30 5.35 5.41 5.23 5.28 5.33 5.17 5.22 5.26 4.05 3.55 7.46
Fuente: Elaboracin Propia
145
Tabla A.6 Resultados del porcentaje de humedad seca (Hs), coccin (Hc) y total (Hs)
Hs H c H t Promedio
Muestras Wh Ws Wc
(%) (%) (%) H t (%)
01_8020 283.02 244.23 218.13 13.71 10.69 22.93
02_8020 299.24 256.47 232.67 14.29 9.28 22.25
03_8020 312.47 262.58 235.41 15.97 10.35 24.66 24.11
04_8020 305.36 256.89 228.51 15.87 11.05 25.17
05_8020 315.46 265.23 234.89 15.92 11.44 25.54
1130_5020 324.26 306.87 284.36 5.36 7.34 12.30
1230_5020 316.25 302.14 274.26 4.46 9.23 13.28
1330_5020 305.87 294.24 277.23 3.80 5.78 9.36 10.32
1430_5020 318.25 287.86 287.17 9.55 0.24 9.77
1530_5020 307.56 296.68 286.32 3.54 3.49 6.91
2125_6015 296.34 278.38 242.24 6.06 12.98 18.26
2225_6015 284.27 268.53 248.21 5.54 7.57 12.69
2325_6015 298.62 274.45 265.46 8.09 3.28 11.10 15.53
2425_6015 281.88 245.38 232.45 12.95 5.27 17.54
2525_6015 298.43 264.87 244.54 11.25 7.68 18.06
3110_8010 291.55 261.83 232.2 10.19 11.32 20.36
3210_8010 289.41 258.45 237.2 10.70 8.22 18.04
3310_8010 294.64 260.67 238.24 11.53 8.60 19.14 18.62
3410_8010 295.79 263.03 235.42 11.08 10.50 20.41
3510_8010 284.69 267.24 241.62 6.13 9.59 15.13
4128_5517 302.56 288.75 262.67 4.56 9.03 13.18
4228_5517 310.21 279.36 258.71 9.94 7.39 16.60
4328_5517 299.56 274.56 254.53 8.35 7.30 15.03 13.58
4428_5517 297.89 279.45 263.47 6.19 5.72 11.55
4528_5517 298.79 287.69 264.31 3.71 8.13 11.54
5120_6515 294.54 259.82 244.73 11.79 5.81 16.91
5220-6515 297.23 260.46 250.19 12.37 3.94 15.83
5320_6515 290.59 261.28 240.36 10.09 8.01 17.29 15.92
5420_6515 294.45 256.86 246.28 12.77 4.12 16.36
5520_6515 295.47 273.21 256.37 7.53 6.16 13.23
6129_5219 306.59 288.61 259.67 5.86 10.03 15.30
6229_5219 294.89 272.38 261.13 7.63 4.13 11.45
6329_5219 305.82 281.24 268.23 8.04 4.63 12.29 12.19
6429_5219 304.31 280.57 274.46 7.80 2.18 9.81
6529_5219 297.34 278.49 261.37 6.34 6.15 12.10
Fuente: Elaboracin Propia
146
Tabla A.7 Resultados del porcentaje de humedad seca (Hs), de coccin (Hc) y total (Hs)
Hs H c H t Promedio
Muestras Wh Ws Wc
(%) (%) (%) H t (%)
7118_7012 295.57 269.22 257.17 8.91 4.48 12.99
7218_7012 291.86 261.89 242.56 10.27 7.38 16.89
7318_7012 292.34 260.76 245.23 10.80 5.96 16.11 16.39
7418_7012 297.48 266.47 239.36 10.42 10.17 19.54
7518_7012 285.36 259.64 238.47 9.01 8.15 16.43
8126_5713 289.49 266.45 244.75 7.96 8.14 15.45
8226_5713 290.77 277.56 252.4 4.54 9.06 13.20
8326_5713 294.69 281.63 263.59 4.43 6.41 10.55 12.90
8426_5713 287.37 272.36 254.14 5.22 6.69 11.56
8526_5713 291.54 281.36 251.56 3.49 10.59 13.71
9119_6714 282.54 264.12 243.57 6.52 7.78 13.79
9219_6714 288.24 267.32 245.51 7.26 8.16 14.82
9319_6714 285.22 275.28 241.73 3.49 12.19 15.25 14.86
6419_6714 284.28 269.34 246.79 5.26 8.37 13.19
6419_6714 292.91 268.51 242.34 8.33 9.75 17.26
10122_6315 302.54 283.74 266.31 6.21 6.14 11.98
10222_6315 315.42 290.32 265.48 7.96 8.56 15.83
10322_6315 298.23 282.43 269.61 5.30 4.54 9.60 12.72
10422_6315 303.73 284.61 261.67 6.30 8.06 13.85
10522_6315 301.67 294.56 264.37 2.36 10.25 12.36
11121_6514 287.34 262.55 249.83 8.63 4.84 13.05
11221_6514 289.81 263.47 250.24 9.09 5.02 13.65
11321_6514 288.97 260.81 252.46 9.74 3.20 12.63 15.47
11421_6514 287.57 262.45 234.73 8.74 10.56 18.37
11521_6514 295.46 266.45 237.49 9.82 10.87 19.62
12123_6114 290.46 264.73 249.55 8.86 5.73 14.08
12223_6114 282.74 256.58 242.23 9.25 5.59 14.33
12323_6114 288.61 260.61 244.38 9.70 6.23 15.33 14.20
12423_6114 299.53 269.46 252.46 10.04 6.31 15.71
12523_6114 295.46 277.34 261.34 6.13 5.77 11.55
Fuente: Elaboracin Propia
147
Tabla A.8 Resultados del porcentaje de porosidad
Promedio
Densidad
Muestras M4 -3 Dr (gcm-
real (gcm ) 3
)
01_8020 170.09 2.04
02_8020 168.67 1.58 1.87
03_8020 169.97 1.99
1130_5020 170.06 2.02
1230_5020 171.22 2.65 2.27
1330_5020 170.35 2.15
2125_6015 170.09 2.04
2225_6015 170.02 2.01 2.02
2325_6015 170.05 2.02
3110_8010 169.97 1.99
3210_8010 169.72 1.89 1.96
3310_8010 170.01 2.00
4128_5517 170.37 2.16
4228_5517 170.15 2.06 2.10
4328_5517 170.21 2.09
5120_6515 170.05 2.02
5220-6515 170.56 2.25 2.08
5320_6515 169.88 1.95
6129_5219 170.38 2.16
6229_5219 170.27 2.11 2.14
6329_5219 170.31 2.13
7118_7012 170.11 2.04
7218_7012 170.05 2.02 2.03
7318_7012 170.07 2.03
8126_5713 170.06 2.02
8226_5713 170.01 2.00 2.01
8326_5713 170.03 2.01
9119_6714 170.15 2.06
9219_6714 170.21 2.09 2.05
9319_6714 170.03 2.01
Fuente: Elaboracin Propia
148
Tabla A.9 Resultados del porcentaje de porosidad
Densidad
Promedio
Muestras M4 real (gcm-
3 Dr (gcm-3)
)
10122_6315 170.23 2.10
10222_6315 170.16 2.07 2.07
10322_6315 170.13 2.05
11121_6514 170.11 2.04
11221_6514 170.16 2.07 2.06
11321_6514 170.18 2.07
12123_6114 170.09 2.04
12223_6114 170.05 2.02 2.04
12323_6114 170.12 2.05
Fuente: Elaboracin Propia
149
Tabla A.11 Resultado de la densidad aparente
Densidad Promedio
Muestras G Ga Gs
aparente Da
7118_7012 269.22 355.76 199.65 1.72
7218_7012 261.89 358.59 202.97 1.68 1.75
7318_7012 260.76 338.47 197.36 1.85
8126_5713 266.45 325.77 196.54 2.06
8226_5713 277.56 386.54 214.56 1.61 1.75
8326_5713 281.63 379.65 201.75 1.58
9119_6714 264.12 365.76 199.65 1.59
9219_6714 267.32 357.69 202.97 1.73 1.71
9319_6714 275.28 368.45 217.36 1.82
10122_6315 283.74 355.76 198.65 1.81
10222_6315 290.32 366.78 197.56 1.72 1.78
10322_6315 282.43 354.44 198.63 1.81
11121_6514 262.55 376.58 204.59 1.53
11221_6514 263.47 358.59 199.65 1.66 1.73
11321_6514 260.81 338.47 208.36 2.00
12123_6114 264.73 348.26 199.85 1.78
12223_6114 256.58 341.25 201.53 1.84 1.72
12323_6114 260.61 366.84 197.17 1.54
Fuente: Elaboracin Propia
150
Tabla A.13 Resultados de Absorcin Mxima.
Absorcin
Muestras Pi Pf Promedios
Max. (%)
4128_5517 288.75 339.45 17.56
4228_5517 279.36 349.38 25.06 21.52
4328_5517 274.56 334.83 21.95
5120_6515 259.82 330.97 27.38
5220-6515 260.46 342.75 31.59 27.42
5320_6515 261.28 322.15 23.30
6129_5219 308.63 358.31 16.10
6229_5219 315.14 368.56 16.95 14.54
6329_5219 320.79 354.71 10.57
7118_7012 269.22 341.12 26.71
7218_7012 261.89 344.05 31.37 27.47
7318_7012 260.76 324.22 24.34
8126_5713 266.45 311.77 17.01
8226_5713 277.56 372.46 34.19 26.94
8326_5713 281.63 365.07 29.63
9119_6714 264.12 351.13 32.94
9219_6714 267.32 343.39 28.46 29.94
9319_6714 275.28 353.51 28.42
10122_6315 283.74 341.44 20.34
10222_6315 290.32 352.30 21.35 20.72
10322_6315 282.43 340.25 20.47
11121_6514 262.55 361.78 37.79
11221_6514 263.47 343.94 30.54 30.85
11321_6514 260.81 323.93 24.20
12123_6114 264.73 333.33 25.91
12223_6114 256.58 326.66 27.31 29.51
12323_6114 260.61 352.62 35.31
Fuente: Elaboracin Propia
151
Tabla A.14 Resultado de Resistencia a la Compresin
PROMEDIO DE CARGA DE
RESISTENCIA RESISTENCIA
Muestras AREAS ROTURA
cm2 pulg2 lb Lb pulg-2 Kgf cm-2 MPa Promedio
03_8020 26.68 10.50 23000.00 2189.91 153.97 15.10
04_8020 26.32 10.36 24000.00 2316.47 162.86 15.97 14.87
05_8020 26.88 10.58 20800.00 1965.17 138.17 13.55
1330_5020 27.30 10.75 40600.00 3777.44 265.58 26.04
1430_5020 27.30 10.75 46300.00 4307.68 302.86 29.70 28.39
1530_5020 27.19 10.71 45700.00 4268.49 300.10 29.43
2325_6015 27.35 10.77 35500.00 3296.66 231.78 22.73
2425_6015 27.67 10.89 30400.00 2791.01 196.23 19.24 21.69
2525_6015 27.67 10.89 36500.00 3350.91 235.59 23.10
3310_8010 27.61 10.87 37900.00 3486.16 245.10 24.04
3410_8010 26.88 10.58 21500.00 2031.63 142.84 14.01 18.01
3510_8010 26.83 10.56 24500.00 2319.29 163.06 15.99
4328_5517 27.56 10.85 31700.00 2921.56 205.41 20.14
4428_5517 27.55 10.85 34600.00 3189.70 224.26 21.99 20.66
4528_5517 27.20 10.71 30800.00 2876.58 202.24 19.83
5320_6515 27.55 10.85 25300.00 2332.35 163.98 16.08
5420-6515 27.56 10.85 29100.00 2681.94 188.56 18.49 18.44
5520_6515 27.35 10.77 32400.00 3008.73 211.53 20.74
6329_5219 27.25 10.73 38900.00 3626.18 254.95 25.00
6429_5219 27.30 10.75 34300.00 3191.22 224.36 22.00 24.51
6529_5219 27.19 10.71 41200.00 3848.18 270.55 26.53
7318_7012 26.99 10.62 27700.00 2607.07 183.30 17.98
7418_7012 27.30 10.75 26500.00 2465.57 173.35 17.00 18.42
7518_7012 27.35 10.77 31700.00 2943.72 206.96 20.30
8326_5713 27.61 10.87 30600.00 2814.77 197.90 19.41
8426_5713 27.77 10.93 33000.00 3018.10 212.19 20.81 20.27
8526_5713 27.20 10.71 32000.00 2988.66 210.12 20.61
9319_6714 27.14 10.69 33700.00 3153.48 221.71 21.74
9419_6714 27.20 10.71 32100.00 2998.13 210.79 20.67 20.64
9519_6714 27.30 10.75 30400.00 2828.37 198.85 19.50
10322_6315 27.51 10.83 26400.00 2437.62 171.38 16.81
10422_6315 27.67 10.89 28400.00 2607.25 183.31 17.98 17.31
10522_6315 27.46 10.81 26900.00 2488.46 174.96 17.16
Fuente: Elaboracin Propia
152
Tabla A.15 Resultado de Resistencia a la Compresin
PROMEDIO DE CARGA DE
RESISTENCIA RESISTENCIA
Muestras AREAS ROTURA
cm2 pulg2 lb Lb pulg-2 Kgf cm-2 MPa Promedio
11321_6514 27.83 10.95 34900.00 3185.85 223.99 21.97
11421_6514 27.72 10.91 30100.00 2758.07 193.91 19.02 20.32
11521_6514 27.77 10.93 31700.00 2899.33 203.84 19.99
12323_6114 26.83 10.56 35200.00 3332.21 234.28 22.97
12423_6114 27.62 10.87 32300.00 2970.93 208.88 20.48 21.73
12523_6114 27.35 10.77 32800.00 3045.84 214.14 21.00
Fuente: Elaboracin Propia
153
Tabla A.17 Resultados Estimados para Resistencia Compresin
Observado
Ajustados Inferior 95.0% Superior 95.0%
s
Fila Valores Valores para Media para Media
25 19.41 20.8869 18.869 22.9048
26 20.81 20.8869 18.869 22.9048
27 20.61 20.8869 18.869 22.9048
28 20.14 20.3386 17.7422 22.935
29 21.99 20.3386 17.7422 22.935
30 19.83 20.3386 17.7422 22.935
31 25.0 24.4094 21.6843 27.1345
32 22.0 24.4094 21.6843 27.1345
33 26.53 24.4094 21.6843 27.1345
34 26.04 28.4988 25.7387 31.2588
35 29.7 28.4988 25.7387 31.2588
36 29.43 28.4988 25.7387 31.2588
Fuente: Elaboracin Propia
154
Resultado de Anlisis de Fluorescencia de Rayos X
155
II. Espectros de cada muestra individual y una en conjunto
156
157
ANEXO B
Normas Utilizadas
158
Designation: D 422 63 (Reapproved 2002)
Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
159
1
D 422 63 (2002)
Metric Equivalents
in. 0.001 0.049 0.203 12 34
NOTE 6A set of sieves giving uniform spacing of points for the graph,
as required in Section 17, may be used if desired. This set consists of the
following sieves:
3-in. (75-mm) No. 16 (1.18-mm)
112-in. (37.5-mm) No. 30 (600-m)
34-in. (19.0-mm) No. 50 (300-m)
38-in. (9.5-mm) No. 100 (150-m)
No. 4 (4.75-mm) No. 200 (75-m)
No. 8 (2.36-mm)
3.7 Water Bath or Constant-Temperature RoomA water
bath or constant-temperature room for maintaining the soil
suspension at a constant temperature during the hydrometer
analysis. A satisfactory water tank is an insulated tank that
maintains the temperature of the suspension at a convenient
constant temperature at or near 68F (20C). Such a device is
illustrated in Fig. 4. In cases where the work is performed in a
room at an automatically controlled constant temperature, the
water bath is not necessary.
3.8 BeakerA beaker of 250-mL capacity.
3.9 Timing DeviceA watch or clock with a second hand.
4. Dispersing Agent
Metric Equivalents
in. 1.3 2.6 3.75
4.1 A solution of sodium hexametaphosphate (sometimes
mm 33 66 95.2 called sodium metaphosphate) shall be used in distilled or
FIG. 2 Dispersion Cups of Apparatus
demineralized water, at the rate of 40 g of sodium
hexametaphosphate/litre of solution (Note 7).
NOTE 7Solutions of this salt, if acidic, slowly revert or hydrolyze
marked for a volume of 1000 mL. The inside diameter shall be back to the orthophosphate form with a resultant decrease in dispersive
such that the 1000-mL mark is 36 6 2 cm from the bottom on action. Solutions should be prepared frequently (at least once a month) or
adjusted to pH of 8 or 9 by means of sodium carbonate. Bottles containing
the inside. solutions should have the date of preparation marked on them.
3.5 ThermometerA thermometer accurate to 1F (0.5C).
3.6 SievesA series of sieves, of square-mesh woven-wire 4.2 All water used shall be either distilled or demineralized
cloth, conforming to the requirements of Specification E 11. A water. The water for a hydrometer test shall be brought to the
full set of sieves includes the following (Note 6): temperature that is expected to prevail during the hydrometer
3-in. (75-mm) No. 10 (2.00-mm) test. For example, if the sedimentation cylinder is to be placed
2-in. (50-mm) No. 20 (850-m) in the water bath, the distilled or demineralized water to be
112-in. (37.5-mm) No. 40 (425-m) used shall be brought to the temperature of the controlled water
1-in. (25.0-mm) No. 60 (250-m)
34-in. (19.0-mm) No. 140 (106-m) bath; or, if the sedimentation cylinder is used in a room with
38-in. (9.5-mm) No. 200 (75-m) controlled temperature, the water for the test shall be at the
No. 4 (4.75-mm) temperature of the room. The basic temperature for the
160
2
D 422 63 (2002)
Metric Equivalents
in.
78 1 3 614 14 37
mm 22.2 25.4 76.2 158.2 356 940
hydrometer test is 68F (20C). Small variations of tempera- Nominal Diameter of Approximate Minimum
ture do not introduce differences that are of practical signifi- Largest Particles, Mass of Portion, g
in. (mm)
cance and do not prevent the use of corrections derived as 38 (9.5) 500
prescribed. 34 (19.0) 1000
1 (25.4) 2000
5. Test Sample 112 (38.1) 3000
2 (50.8) 4000
5.1 Prepare the test sample for mechanical analysis as 3 (76.2) 5000
outlined in Practice D 421. During the preparation procedure
the sample is divided into two portions. One portion contains 5.1.2 The size of the portion passing the No. 10 sieve shall
only particles retained on the No. 10 (2.00-mm) sieve while the be approximately 115 g for sandy soils and approximately 65
other portion contains only particles passing the No. 10 sieve. g for silt and clay soils.
The mass of air-dried soil selected for purpose of tests, as 5.2 Provision is made in Section 5 of Practice D 421 for
prescribed in Practice D 421, shall be sufficient to yield weighing of the air-dry soil selected for purpose of tests, the
quantities for mechanical analysis as follows: separation of the soil on the No. 10 sieve by dry-sieving and
5.1.1 The size of the portion retained on the No. 10 sieve washing, and the weighing of the washed and dried fraction
shall depend on the maximum size of particle, according to the retained on the No. 10 sieve. From these two masses the
following schedule:
161
3
D 422 63 (2002)
percentages retained and passing the No. 10 sieve can be needed. Measurement of the composite corrections may be
calculated in accordance with 12.1. made at two temperatures spanning the range of expected test
temperatures, and corrections for the intermediate temperatures
NOTE 8A check on the mass values and the thoroughness of pulveri-
zation of the clods may be secured by weighing the portion passing the calculated assuming a straight-line relationship between the
No. 10 sieve and adding this value to the mass of the washed and two observed values.
oven-dried portion retained on the No. 10 sieve. 7.3 Prepare 1000 mL of liquid composed of distilled or
demineralized water and dispersing agent in the same propor-
SIEVE ANALYSIS OF PORTION RETAINED ON NO. tion as will prevail in the sedimentation (hydrometer) test.
10 Place the liquid in a sedimentation cylinder and the cylinder in
(2.00-mm) SIEVE the constant-temperature water bath, set for one of the two
temperatures to be used. When the temperature of the liquid
6. Procedure
becomes constant, insert the hydrometer, and, after a short
6.1 Separate the portion retained on the No. 10 (2.00-mm) interval to permit the hydrometer to come to the temperature of
sieve into a series of fractions using the 3-in. (75-mm), 2-in. the liquid, read the hydrometer at the top of the meniscus
(50-mm), 112-in. (37.5-mm), 1-in. (25.0-mm), 34-in. (19.0- formed on the stem. For hydrometer 151H the composite
mm), 38-in. (9.5-mm), No. 4 (4.75-mm), and No. 10 sieves, or correction is the difference between this reading and one; for
as many as may be needed depending on the sample, or upon hydrometer 152H it is the difference between the reading and
the specifications for the material under test. zero. Bring the liquid and the hydrometer to the other tempera-
6.2 Conduct the sieving operation by means of a lateral and ture to be used, and secure the composite correction as before.
vertical motion of the sieve, accompanied by a jarring action in
order to keep the sample moving continuously over the surface 8. Hygroscopic Moisture
of the sieve. In no case turn or manipulate fragments in the 8.1 When the sample is weighed for the hydrometer test,
sample through the sieve by hand. Continue sieving until not weigh out an auxiliary portion of from 10 to 15 g in a small
more than 1 mass % of the residue on a sieve passes that sieve metal or glass container, dry the sample to a constant mass in
during 1 min of sieving. When mechanical sieving is used, test an oven at 230 6 9F (110 6 5C), and weigh again. Record
the thoroughness of sieving by using the hand method of the masses.
sieving as described above.
6.3 Determine the mass of each fraction on a balance 9. Dispersion of Soil Sample
conforming to the requirements of 3.1. At the end of weighing, 9.1 When the soil is mostly of the clay and silt sizes, weigh
the sum of the masses retained on all the sieves used should out a sample of air-dry soil of approximately 50 g. When the
equal closely the original mass of the quantity sieved. soil is mostly sand the sample should be approximately 100 g.
9.2 Place the sample in the 250-mL beaker and cover with
HYDROMETER AND SIEVE ANALYSIS OF PORTION
125 mL of sodium hexametaphosphate solution (40 g/L). Stir
PASSING THE NO. 10 (2.00-mm) SIEVE
until the soil is thoroughly wetted. Allow to soak for at least 16
7. Determination of Composite Correction for h.
Hydrometer Reading 9.3 At the end of the soaking period, disperse the sample
further, using either stirring apparatus A or B. If stirring
7.1 Equations for percentages of soil remaining in suspen- apparatus A is used, transfer the soil-water slurry from the
sion, as given in 14.3, are based on the use of distilled or beaker into the special dispersion cup shown in Fig. 2, washing
demineralized water. A dispersing agent is used in the water, any residue from the beaker into the cup with distilled or
however, and the specific gravity of the resulting liquid is demineralized water (Note 9). Add distilled or demineralized
appreciably greater than that of distilled or demineralized water, if necessary, so that the cup is more than half full. Stir
water. for a period of 1 min.
7.1.1 Both soil hydrometers are calibrated at 68F (20C),
and variations in temperature from this standard temperature NOTE 9A large size syringe is a convenient device for handling the
produce inaccuracies in the actual hydrometer readings. The water in the washing operation. Other devices include the wash-water
bottle and a hose with nozzle connected to a pressurized distilled water
amount of the inaccuracy increases as the variation from the tank.
standard temperature increases.
7.1.2 Hydrometers are graduated by the manufacturer to be 9.4 If stirring apparatus B (Fig. 3) is used, remove the cover
read at the bottom of the meniscus formed by the liquid on the cap and connect the cup to a compressed air supply by means
stem. Since it is not possible to secure readings of soil of a rubber hose. A air gage must be on the line between the
suspensions at the bottom of the meniscus, readings must be cup and the control valve. Open the control valve so that the
taken at the top and a correction applied. gage indicates 1 psi (7 kPa) pressure (Note 10). Transfer the
7.1.3 The net amount of the corrections for the three items soil-water slurry from the beaker to the air-jet dispersion cup
enumerated is designated as the composite correction, and may by washing with distilled or demineralized water. Add distilled
be determined experimentally. or demineralized water, if necessary, so that the total volume in
7.2 For convenience, a graph or table of composite correc- the cup is 250 mL, but no more.
tions for a series of 1 temperature differences for the range of NOTE 10The initial air pressure of 1 psi is required to prevent the
expected test temperatures may be prepared and used as soil-water mixture from entering the air-jet chamber when the mixture is
162
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D 422 63 (2002)
transferred to the dispersion cup. CALCULATIONS AND REPORT
9.5 Place the cover cap on the cup and open the air control 12. Sieve Analysis Values for the Portion Coarser than
valve until the gage pressure is 20 psi (140 kPa). Disperse the the No. 10 (2.00-mm) Sieve
soil according to the following schedule:
12.1 Calculate the percentage passing the No. 10 sieve by
Dispersion Period,
Plasticity Index
min dividing the mass passing the No. 10 sieve by the mass of soil
originally split on the No. 10 sieve, and multiplying the result
Under 5 5 by 100. To obtain the mass passing the No. 10 sieve, subtract
6 to 20 10
Over 20 15 the mass retained on the No. 10 sieve from the original mass.
12.2 To secure the total mass of soil passing the No. 4
Soils containing large percentages of mica need be dispersed (4.75-mm) sieve, add to the mass of the material passing the
for only 1 min. After the dispersion period, reduce the gage No. 10 sieve the mass of the fraction passing the No. 4 sieve
pressure to 1 psi preparatory to transfer of soil-water slurry to and retained on the No. 10 sieve. To secure the total mass of
the sedimentation cylinder. soil passing the 38-in. (9.5-mm) sieve, add to the total mass of
soil passing the No. 4 sieve, the mass of the fraction passing the
10. Hydrometer Test 38-in. sieve and retained on the No. 4 sieve. For the remaining
10.1 Immediately after dispersion, transfer the soil-water sieves, continue the calculations in the same manner.
slurry to the glass sedimentation cylinder, and add distilled or 12.3 To determine the total percentage passing for each
sieve, divide the total mass passing (see 12.2) by the total mass
demineralized water until the total volume is 1000 mL.
of sample and multiply the result by 100.
10.2 Using the palm of the hand over the open end of the
cylinder (or a rubber stopper in the open end), turn the cylinder 13. Hygroscopic Moisture Correction Factor
upside down and back for a period of 1 min to complete the 13.1 The hydroscopic moisture correction factor is the ratio
agitation of the slurry (Note 11). At the end of 1 min set the between the mass of the oven-dried sample and the air-dry
cylinder in a convenient location and take hydrometer readings mass before drying. It is a number less than one, except when
at the following intervals of time (measured from the beginning there is no hygroscopic moisture.
of sedimentation), or as many as may be needed, depending on
the sample or the specification for the material under test: 2, 5, 14. Percentages of Soil in Suspension
15, 30, 60, 250, and 1440 min. If the controlled water bath is 14.1 Calculate the oven-dry mass of soil used in the
used, the sedimentation cylinder should be placed in the bath hydrometer analysis by multiplying the air-dry mass by the
between the 2- and 5-min readings. hygroscopic moisture correction factor.
14.2 Calculate the mass of a total sample represented by the
NOTE 11The number of turns during this minute should be approxi-
mately 60, counting the turn upside down and back as two turns. Any soil mass of soil used in the hydrometer test, by dividing the
remaining in the bottom of the cylinder during the first few turns should oven-dry mass used by the percentage passing the No. 10
be loosened by vigorous shaking of the cylinder while it is in the inverted (2.00-mm) sieve, and multiplying the result by 100. This value
position. is the weight W in the equation for percentage remaining in
suspension.
10.3 When it is desired to take a hydrometer reading,
14.3 The percentage of soil remaining in suspension at the
carefully insert the hydrometer about 20 to 25 s before the
level at which the hydrometer is measuring the density of the
reading is due to approximately the depth it will have when the
suspension may be calculated as follows (Note 13): For
reading is taken. As soon as the reading is taken, carefully hydrometer 151H:
remove the hydrometer and place it with a spinning motion in
a graduate of clean distilled or demineralized water. P 5 @~100 000/W! 3 G/~G 2 G 1!#~R 2 G1! (1)
NOTE 13The bracketed portion of the equation for hydrometer 151H
NOTE 12It is important to remove the hydrometer immediately after is constant for a series of readings and may be calculated first and then
each reading. Readings shall be taken at the top of the meniscus formed multiplied by the portion in the parentheses.
by the suspension around the stem, since it is not possible to secure
readings at the bottom of the meniscus. For hydrometer 152H:
10.4 After each reading, take the temperature of the suspen- P 5 ~Ra/W! 3 100 (2)
sion by inserting the thermometer into the suspension. where:
a = correction faction to be applied to the reading of
11. Sieve Analysis hydrometer 152H. (Values shown on the scale are
11.1 After taking the final hydrometer reading, transfer the computed using a specific gravity of 2.65. Correction
suspension to a No. 200 (75-m) sieve and wash with tap water factors are given in Table 1),
until the wash water is clear. Transfer the material on the No. P = percentage of soil remaining in suspension at the level
200 sieve to a suitable container, dry in an oven at 230 6 9F at which the hydrometer measures the density of the
(110 6 5C) and make a sieve analysis of the portion retained, suspension,
using as many sieves as desired, or required for the material, or R = hydrometer reading with composite correction ap-
plied (Section 7),
upon the specification of the material under test.
163
5
D 422 63 (2002)
W = oven-dry mass of soil in a total test sample repre- TABLE 2 Values of Effective Depth Based on Hydrometer and
Sedimentation Cylinder of Specified SizesA
sented by mass of soil dispersed (see 14.2), g,
G = specific gravity of the soil particles, and Hydrometer 151H Hydrometer 152H
G1 = specific gravity of the liquid in which soil particles Actual
Effective
Actual
Effective
Actual Effective
Hydrometer Hydrometer Hydrometer Depth, L,
are suspended. Use numerical value of one in both Reading
Depth, L, cm
Reading
Depth, L, cm
Reading cm
instances in the equation. In the first instance any
1.000 16.3 0 16.3 31 11.2
possible variation produces no significant effect, and 1.001 16.0 1 16.1 32 11.1
in the second instance, the composite correction for R 1.002 15.8 2 16.0 33 10.9
is based on a value of one for G1. 1.003 15.5 3 15.8 34 10.7
1.004 15.2 4 15.6 35 10.6
1.005 15.0 5 15.5
1.006 14.7 6 15.3 36 10.4
15. Diameter of Soil Particles 1.007 14.4 7 15.2 37 10.2
1.008 14.2 8 15.0 38 10.1
15.1 The diameter of a particle corresponding to the per-
1.009 13.9 9 14.8 39 9.9
centage indicated by a given hydrometer reading shall be 1.010 13.7 10 14.7 40 9.7
calculated according to Stokes law (Note 14), on the basis that 1.011 13.4 11 14.5 41 9.6
1.012 13.1 12 14.3 42 9.4
a particle of this diameter was at the surface of the suspension 1.013 12.9 13 14.2 43 9.2
at the beginning of sedimentation and had settled to the level at 1.014 12.6 14 14.0 44 9.1
which the hydrometer is measuring the density of the suspen- 1.015 12.3 15 13.8 45 8.9
1.016 12.1 16 13.7 46 8.8
sion. According to Stokes law: see Table 2 1.017 11.8 17 13.5 47 8.6
D 5 =@30n/980~G 2 G 1!# 3 L/T (3) 1.018 11.5 18 13.3 48 8.4
1.019 11.3 19 13.2 49 8.3
1.020 11.0 20 13.0 50 8.1
where: 1.021 10.7 21 12.9 51 7.9
D = diameter of particle, mm, 1.022 10.5 22 12.7 52 7.8
n = coefficient of viscosity of the suspending medium (in 1.023 10.2 23 12.5 53 7.6
1.024 10.0 24 12.4 54 7.4
this case water) in poises (varies with changes in 1.025 9.7 25 12.2 55 7.3
temperature of the suspending medium), 1.026 9.4 26 12.0 56 7.1
L = distance from the surface of the suspension to the 1.027 9.2 27 11.9 57 7.0
level at which the density of the suspension is being 1.028 8.9 28 11.7 58 6.8
1.029 8.6 29 11.5 59 6.6
measured, cm. (For a given hydrometer and sedimen- 1.030 8.4 30 11.4 60 6.5
tation cylinder, values vary according to the hydrom- 1.031 8.1
eter readings. This distance is known as effective 1.032 7.8
1.033 7.6
depth (see Table 2)), 1.034 7.3
T = interval of time from beginning of sedimentation to 1.035 7.0
the taking of the reading, min, 1.036 6.8
1.037 6.5
G = specific gravity of soil particles, and 1.038 6.2
G1 = specific gravity (relative density) of suspending me- A
Values of effective depth are calculated from the equation:
dium (value may be used as 1.000 for all practical L 5 L1 1 1 / 2 @L2 2 ~VB/A!# (5)
purposes).
where:
NOTE 14Since Stokes law considers the terminal velocity of a single L = effective depth, cm,
sphere falling in an infinity of liquid, the sizes calculated represent the L1 = distance along the stem of the hydrometer from the top of the bulb to
diameter of spheres that would fall at the same rate as the soil particles. the mark for a hydrometer reading, cm,
L 2 = overall length of the hydrometer bulb, cm,
15.2 For convenience in calculations the above equation VB = volume of hydrometer bulb, cm3, and
may be written as follows: see Table 3 A = cross-sectional area of sedimentation cylinder, cm2
164
6
D 422 63 (2002)
TABLE 3 Values of K for Use in Equation for Computing Diameter of Particle in Hydrometer Analysis
Temperature, Specific Gravity of Soil Particles
C 2.45 2.50 2.55 2.60 2.65 2.70 2.75 2.80 2.85
16 0.01510 0.01505 0.01481 0.01457 0.01435 0.01414 0.01394 0.01374 0.01356
17 0.01511 0.01486 0.01462 0.01439 0.01417 0.01396 0.01376 0.01356 0.01338
18 0.01492 0.01467 0.01443 0.01421 0.01399 0.01378 0.01359 0.01339 0.01321
19 0.01474 0.01449 0.01425 0.01403 0.01382 0.01361 0.01342 0.1323 0.01305
20 0.01456 0.01431 0.01408 0.01386 0.01365 0.01344 0.01325 0.01307 0.01289
21 0.01438 0.01414 0.01391 0.01369 0.01348 0.01328 0.01309 0.01291 0.01273
22 0.01421 0.01397 0.01374 0.01353 0.01332 0.01312 0.01294 0.01276 0.01258
23 0.01404 0.01381 0.01358 0.01337 0.01317 0.01297 0.01279 0.01261 0.01243
24 0.01388 0.01365 0.01342 0.01321 0.01301 0.01282 0.01264 0.01246 0.01229
25 0.01372 0.01349 0.01327 0.01306 0.01286 0.01267 0.01249 0.01232 0.01215
26 0.01357 0.01334 0.01312 0.01291 0.01272 0.01253 0.01235 0.01218 0.01201
27 0.01342 0.01319 0.01297 0.01277 0.01258 0.01239 0.01221 0.01204 0.01188
28 0.01327 0.01304 0.01283 0.01264 0.01244 0.01255 0.01208 0.01191 0.01175
29 0.01312 0.01290 0.01269 0.01249 0.01230 0.01212 0.01195 0.01178 0.01162
30 0.01298 0.01276 0.01256 0.01236 0.01217 0.01199 0.01182 0.01165 0.01149
where: is not made on a portion of the soil, the preparation of the graph
K = constant depending on the temperature of the suspen- is optional, since values may be secured directly from tabulated
sion and the specific gravity of the soil particles. data.
Values of K for a range of temperatures and specific
gravities are given in Table 3. The value of K does not 18. Report
change for a series of readings constituting a test, 18.1 The report shall include the following:
while values of L and T do vary.
18.1.1 Maximum size of particles,
15.3 Values of D may be computed with sufficient accuracy,
18.1.2 Percentage passing (or retained on) each sieve, which
using an ordinary 10-in. slide rule.
may be tabulated or presented by plotting on a graph (Note 16),
NOTE 15The value of L is divided by T using the A- and B-scales, the 18.1.3 Description of sand and gravel particles:
square root being indicated on the D-scale. Without ascertaining the value
of the square root it may be multiplied by K, using either the C- or 18.1.3.1 Shaperounded or angular,
CI-scale. 18.1.3.2 Hardnesshard and durable, soft, or weathered
and friable,
16. Sieve Analysis Values for Portion Finer than No. 10 18.1.4 Specific gravity, if unusually high or low,
(2.00-mm) Sieve
18.1.5 Any difficulty in dispersing the fraction passing the
16.1 Calculation of percentages passing the various sieves No. 10 (2.00-mm) sieve, indicating any change in type and
used in sieving the portion of the sample from the hydrometer amount of dispersing agent, and
test involves several steps. The first step is to calculate the mass 18.1.6 The dispersion device used and the length of the
of the fraction that would have been retained on the No. 10 dispersion period.
sieve had it not been removed. This mass is equal to the total
percentage retained on the No. 10 sieve (100 minus total NOTE 16This tabulation of graph represents the gradation of the
percentage passing) times the mass of the total sample repre- sample tested. If particles larger than those contained in the sample were
sented by the mass of soil used (as calculated in 14.2), and the removed before testing, the report shall so state giving the amount and
maximum size.
result divided by 100.
16.2 Calculate next the total mass passing the No. 200 sieve. 18.2 For materials tested for compliance with definite speci-
Add together the fractional masses retained on all the sieves, fications, the fractions called for in such specifications shall be
including the No. 10 sieve, and subtract this sum from the mass reported. The fractions smaller than the No. 10 sieve shall be
of the total sample (as calculated in 14.2). read from the graph.
16.3 Calculate next the total masses passing each of the 18.3 For materials for which compliance with definite
other sieves, in a manner similar to that given in 12.2. specifications is not indicated and when the soil is composed
16.4 Calculate last the total percentages passing by dividing almost entirely of particles passing the No. 4 (4.75-mm) sieve,
the total mass passing (as calculated in 16.3) by the total mass the results read from the graph may be reported as follows:
of sample (as calculated in 14.2), and multiply the result by (1) Gravel, passing 3-in. and retained on No. 4 sieve ..... %
100. (2) Sand, passing No. 4 sieve and retained on No. 200 sieve ..... %
(a) Coarse sand, passing No. 4 sieve and retained on No. 10 sieve ..... %
17. Graph (b) Medium sand, passing No. 10 sieve and retained on No. 40 sieve ..... %
(c) Fine sand, passing No. 40 sieve and retained on No. 200 sieve ..... %
17.1 When the hydrometer analysis is performed, a graph of (3) Silt size, 0.074 to 0.005 mm ..... %
the test results shall be made, plotting the diameters of the (4) Clay size, smaller than 0.005 mm ..... %
Colloids, smaller than 0.001 mm ..... %
particles on a logarithmic scale as the abscissa and the
percentages smaller than the corresponding diameters to an 18.4 For materials for which compliance with definite
arithmetic scale as the ordinate. When the hydrometer analysis specifications is not indicated and when the soil contains
165
7
D 422 63 (2002)
material retained on the No. 4 sieve sufficient to require a sieve No. 10 (2.00-mm) .........
analysis on that portion, the results may be reported as follows No. 40 (425-m) .........
No. 200 (75-m) .........
(Note 17): HYDROMETER ANALYSIS
SIEVE ANALYSIS
0.074 mm .........
Percentage 0.005 mm .........
Sieve Size
Passing 0.001 mm .........
3-in. ......... NOTE 17No. 8 (2.36-mm) and No. 50 (300-m) sieves may be
2-in. ......... substituted for No. 10 and No. 40 sieves.
112-in. .........
1-in. ......... 19. Keywords
34-in. .........
38-in. ......... 19.1 grain-size; hydrometer analysis; hygroscopic moisture;
No. 4 (4.75-mm) ......... particle-size; sieve analysis
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166
8
Designation: D 2216 98
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
1. Scope * when tested by this method will give a mass of solids which
1.1 This test method covers the laboratory determination of includes the previously soluble solids. These materials require
the water (moisture) content by mass of soil, rock, and similar special treatment to remove or account for the presence of
materials where the reduction in mass by drying is due to loss precipitated solids in the dry mass of the specimen, or a
of water except as noted in 1.4, 1.5, and 1.7. For simplicity, the qualified definition of water content must be used. For ex-
word material hereinafter also refers to either soil or rock, ample, see Noorany2 regarding information on marine soils.
whichever is most applicable. 1.6 This test method requires several hours for proper
1.2 Some disciplines, such as soil science, need to deter- drying of the water content specimen. Test Method D 4643
mine water content on the basis of volume. Such determina- provides for drying of the test specimen in a microwave oven
tions are beyond the scope of this test method. which is a shorter process. Also see Gilbert3 for details on the
1.3 The water content of a material is defined in 3.2.1. background of this test method.
1.4 The term solid material as used in geotechnical 1.7 This standard requires the drying of material in an oven
engineering is typically assumed to mean naturally occurring at high temperatures. If the material being dried is contami-
mineral particles of soil and rock that are not readily soluble in nated with certain chemicals, health and safety hazards can
water. Therefore, the water content of materials containing exist. Therefore, this standard should not be used in determin-
extraneous matter (such as cement, and the like) may require ing the water content of contaminated soils unless adequate
special treatment or a qualified definition of water content. In health and safety precautions are taken.
addition, some organic materials may be decomposed by oven 1.8 This standard does not purport to address all of the
drying at the standard drying temperature for this method safety concerns, if any, associated with its use. It is the
(110C). Materials containing gypsum (calcium sulfate dihy- responsibility of the user of this standard to establish appro-
drate or other compounds having significant amounts of priate safety and health practices and determine the applica-
hydrated water) may present a special problem as this material bility of regulatory limitations prior to use.
slowly dehydrates at the standard drying temperature (110C) 2. Referenced Documents
and at very low relative humidities, forming a compound
(calcium sulfate hemihydrate) which is not normally present in 2.1 ASTM Standards:
natural materials except in some desert soils. In order to reduce D 653 Terminology Relating to Soil, Rock, and Contained
the degree of dehydration of gypsum in those materials Fluids4
containing gypsum, or to reduce decomposition in highly D 2974 Test Methods for Moisture, Ash, and Organic Mat-
organic soils, it may be desirable to dry these materials at 60C ter of Peat and Other Organic Soils4
or in a desiccator at room temperature. Thus, when a drying D 4220 Practice for Preserving and Transporting Soil
temperature is used which is different from the standard drying Samples4
temperature as defined by this test method, the resulting water D 4318 Test Method for Liquid Limit, Plastic Limit, and
content may be different from standard water content deter- Plasticity Index of Soils4
mined at the standard drying temperature. D 4643 Test Method for Determination of Water (Moisture)
Content of Soil by the Microwave Oven Method4
NOTE 1Test Methods D 2974 provides an alternate procedure for D 4753 Specification for Evaluating, Selecting, and Speci-
determining water content of peat materials.
fying Balances and Scales for Use in Soil and Rock
1.5 Materials containing water with substantial amounts of Testing4
soluble solids (such as salt in the case of marine sediments)
2
Noorany, I., Phase Relations in Marine Soils, Journal of Geotechnical
1
This test method is under the jurisdiction of ASTM Committee D-18 on Soil Engineering, ASCE, Vol. 110, No. 4, April 1984, pp. 539543.
3
and Rock and is the direct responsibility of Subcommittee D18.03 on Texture, Gilbert, P.A., Computer Controlled Microwave Oven System for Rapid Water
Plasticity and Density Characteristics of Soils. Content Determination, Tech. Report GL-8821, Department of the Army, Water-
Current edition approved Feb. 10, 1998. Published January 1999. Originally ways Experiment Station, Corps of Engineers, Vicksburg, MS, November 1988.
4
published as D 2216 63 T. Last previous edition D 2216 92. Annual Book of ASTM Standards, Vol 04.08.
1 167
D 2216
D 6026 Guide for Using Significant Digits in Calculating NOTE 2The purpose of close-fitting lids is to prevent loss of moisture
and Reporting Geotechnical Test Data5 from specimens before initial mass determination and to prevent absorp-
E 145 Specification for Gravity-Convection And Forced- tion of moisture from the atmosphere following drying and before final
mass determination.
Ventilation Ovens6
6.4 DesiccatorA desiccator cabinet or large desiccator jar
3. Terminology of suitable size containing silica gel or anhydrous calcium
3.1 Refer to Terminology D 653 for standard definitions of sulfate. It is preferable to use a desiccant which changes color
terms. to indicate it needs reconstitution. See 10.5.
3.2 Definitions of Terms Specific to This Standard: NOTE 3Anhydrous calcium sulfate is sold under the trade name
3.2.1 water content (of a material)the ratio expressed as a Drierite.
percent of the mass of pore or free water in a given mass 6.5 Container Handling Apparatus, gloves, tongs, or suit-
of material to the mass of the solid material. A standard able holder for moving and handling hot containers after
temperature of 110 6 5C is used to determine these masses. drying.
4. Summary of Test Method 6.6 Miscellaneous, knives, spatulas, scoops, quartering
cloth, sample splitters, etc, as required.
4.1 A test specimen is dried in an oven at a temperature of
110 6 5C to a constant mass. The loss of mass due to drying 7. Samples
is considered to be water. The water content is calculated using 7.1 Samples shall be preserved and transported in accor-
the mass of water and the mass of the dry specimen. dance with Practice 4220 Groups B, C, or D soils. Keep the
samples that are stored prior to testing in noncorrodible airtight
5. Significance and Use containers at a temperature between approximately 3 and 30C
5.1 For many materials, the water content is one of the most and in an area that prevents direct contact with sunlight.
significant index properties used in establishing a correlation Disturbed samples in jars or other containers shall be stored in
between soil behavior and its index properties. such a way as to prevent or minimize moisture condensation on
5.2 The water content of a material is used in expressing the the insides of the containers.
phase relationships of air, water, and solids in a given volume 7.2 The water content determination should be done as soon
of material. as practicable after sampling, especially if potentially corrod-
5.3 In fine-grained (cohesive) soils, the consistency of a ible containers (such as thin-walled steel tubes, paint cans, etc.)
given soil type depends on its water content. The water content or plastic sample bags are used.
of a soil, along with its liquid and plastic limits as determined
by Test Method D 4318, is used to express its relative consis- 8. Test Specimen
tency or liquidity index. 8.1 For water contents being determined in conjunction with
another ASTM method, the specimen mass requirement stated
6. Apparatus in that method shall be used if one is provided. If no minimum
6.1 Drying Oven, thermostatically-controlled, preferably of specimen mass is provided in that method then the values given
the forced-draft type, meeting the requirements of Specifica- below shall apply. See Howard7 for background data for the
tion E 145 and capable of maintaining a uniform temperature values listed.
of 110 6 5C throughout the drying chamber. 8.2 The minimum mass of moist material selected to be
6.2 BalancesAll balances must meet the requirements of representative of the total sample shall be in accordance with
Specification D 4753 and this section. A Class GP1 balance of the following:
0.01g readability is required for specimens having a mass of up Recommended Recommended
to 200 g (excluding mass of specimen container) and a Class minimum mass of minimum mass of
Maximum particle
Standard Sieve moist test spec- moist test spec-
GP2 balance of 0.1g readability is required for specimens size (100 %
Size imen for water imen for water
passing)
having a mass over 200 g. However, the balance used may be content reported content reported
to 60.1 % to 61 %
controlled by the number of significant digits needed (see 8.2.1
and 12.1.2). 2 mm or less No. 10 20 g 20 gA
6.3 Specimen ContainersSuitable containers made of ma- 4.75 mm No. 4 100 g 20 gA
9.5 mm 38-in. 500 g 50 g
terial resistant to corrosion and change in mass upon repeated 19.0 mm 34-in. 2.5 kg 250 g
heating, cooling, exposure to materials of varying pH, and 37.5 mm 112 in. 10 kg 1 kg
cleaning. Unless a dessicator is used, containers with close- 75.0 mm 3-in. 50 kg 5 kg
A
fitting lids shall be used for testing specimens having a mass of To be representative not less than 20 g shall be used.
less than about 200 g; while for specimens having a mass 8.2.1 The minimum mass used may have to be increased to
greater than about 200 g, containers without lids may be used obtain the needed significant digits for the mass of water when
(see Note 7). One container is needed for each water content reporting water contents to the nearest 0.1 % or as indicated in
determination. 12.1.2.
7
Howard, A. K., Minimum Test Specimen Mass for Moisture Content Deter-
5
Annual Book of ASTM Standards, Vol 04.09. mination, Geotechnical Testing Journal, A.S.T.M., Vol. 12, No. 1, March 1989, pp.
6
Annual Book of ASTM Standards, Vol 14.02. 39-44.
2 168
D 2216
8.3 Using a test specimen smaller than the minimum indi- tative slice from the interval being tested; or (3) trimming the
cated in 8.2 requires discretion, though it may be adequate for exposed surface of one-half or from the interval being tested.
the purposes of the test. Any specimen used not meeting these
NOTE 4Migration of moisture in some cohesionless soils may require
requirements shall be noted on the test data forms or test data that the full section be sampled.
sheets.
8.4 When working with a small (less than 200g) specimen 9.3.3 If a layered material (or more than one material type is
containing a relatively large gravel particle, it is appropriate encountered), select an average specimen, or individual speci-
not to include this particle in the test specimen. However, any mens, or both. Specimens must be properly identified as to
discarded material shall be described and noted on the test data location, or what they represent, and appropriate remarks
forms or test data sheets. entered on the test data forms or test data sheets.
8.5 For those samples consisting entirely of intact rock, the 10. Procedure
minimum specimen mass shall be 500 g. Representative 10.1 Determine and record the mass of the clean and dry
portions of the sample may be broken into smaller particles, specimen container (and its lid, if used).
depending on the samples size, the container and balance 10.2 Select representative test specimens in accordance with
being used and to facilitate drying to constant mass, see 10.4. Section 9.
Specimen sizes as small as 200 g may be tested if water 10.3 Place the moist test specimen in the container and, if
contents of only two significant digits are acceptable. used, set the lid securely in position. Determine the mass of the
9. Test Specimen Selection container and moist material using a balance (see 6.2) selected
on the basis of the specimen mass. Record this value.
9.1 When the test specimen is a portion of a larger amount
of material, the specimen must be selected to be representative NOTE 5To prevent mixing of specimens and yielding of incorrect
of the water condition of the entire amount of material. The results, all containers, and lids if used, should be numbered and the
container numbers shall be recorded on the laboratory data sheets. The lid
manner in which the test specimen is selected depends on the
numbers should match the container numbers to eliminate confusion.
purpose and application of the test, type of material being NOTE 6To assist in the oven-drying of large test specimens, they
tested, the water condition, and the type of sample (from should be placed in containers having a large surface area (such as pans)
another test, bag, block, and the likes.) and the material broken up into smaller aggregations.
9.2 For disturbed samples such as trimmings, bag samples, 10.4 Remove the lid (if used) and place the container with
and the like, obtain the test specimen by one of the following moist material in the drying oven. Dry the material to a
methods (listed in order of preference): constant mass. Maintain the drying oven at 110 6 5C unless
9.2.1 If the material is such that it can be manipulated and otherwise specified (see 1.4). The time required to obtain
handled without significant moisture loss and segregation, the constant mass will vary depending on the type of material, size
material should be mixed thoroughly and then select a repre- of specimen, oven type and capacity, and other factors. The
sentative portion using a scoop of a size that no more than a influence of these factors generally can be established by good
few scoopfuls are required to obtain the proper size of judgment, and experience with the materials being tested and
specimen defined in 8.2. the apparatus being used.
9.2.2 If the material is such that it cannot be thoroughly
mixed or mixed and sampled by a scoop, form a stockpile of NOTE 7In most cases, drying a test specimen overnight (about 12 to
the material, mixing as much as possible. Take at least five 16 h) is sufficient. In cases where there is doubt concerning the adequacy
of drying, drying should be continued until the change in mass after two
portions of material at random locations using a sampling tube,
successive periods (greater than 1 h) of drying is an insignificant amount
shovel, scoop, trowel, or similar device appropriate to the (less than about 0.1 %). Specimens of sand may often be dried to constant
maximum particle size present in the material. Combine all the mass in a period of about 4 h, when a forced-draft oven is used.
portions for the test specimen. NOTE 8Since some dry materials may absorb moisture from moist
9.2.3 If the material or conditions are such that a stockpile specimens, dried specimens should be removed before placing moist
cannot be formed, take as many portions of the material as specimens in the same oven. However, this would not be applicable if the
practical, using random locations that will best represent the previously dried specimens will remain in the drying oven for an
additional time period of about 16 h.
moisture condition. Combine all the portions for the test
specimen. 10.5 After the material has dried to constant mass remove
9.3 Intact samples such as block, tube, split barrel, and the the container from the oven (and replace the lid if used). Allow
like, obtain the test specimen by one of the following methods the material and container to cool to room temperature or until
depending on the purpose and potential use of the sample. the container can be handled comfortably with bare hands and
9.3.1 Using a knife, wire saw, or other sharp cutting device, the operation of the balance will not be affected by convection
trim the outside portion of the sample a sufficient distance to currents and/or its being heated. Determine the mass of the
see if the material is layered and to remove material that container and oven-dried material using the same type/capacity
appears more dry or more wet than the main portion of the balance used in 10.3. Record this value. Tight fitting lids shall
sample. If the existence of layering is questionable, slice the be used if it appears that the specimen is absorbing moisture
sample in half. If the material is layered, see 9.3.3. from the air prior to determination of its dry mass.
9.3.2 If the material is not layered, obtain the specimen NOTE 9Cooling in a desiccator is acceptable in place of tight fitting
meeting the mass requirements in 8.2 by: (1) taking all or lids since it greatly reduces absorption of moisture from the atmosphere
one-half of the interval being tested; (2) trimming a represen- during cooling especially for containers without tight fitting lids.
3 169
D 2216
11. Calculation 12.1.4 Indicate if test specimen contained more than one
11.1 Calculate the water content of the material as follows: material type (layered, etc.).
12.1.5 Indicate the temperature of drying if different from
Mw
w 5 @~Mcws 2 Mcs!/~Mcs 2 M c!# 3 100 5 M 3 100 (1) 110 6 5C.
s
12.1.6 Indicate if any material (size and amount) was
where: excluded from the test specimen.
w 5 water content, %, 12.2 When reporting water content in tables, figures, etc.,
Mcws 5 mass of container and wet specimen, g, any data not meeting the requirements of this test method shall
Mcs 5 mass of container and oven dry specimen, g, be noted, such as not meeting the mass, balance, or temperature
Mc 5 mass of container, g, requirements or a portion of the material is excluded from the
Mw 5 mass of water (M w 5 Mcws Mcds), g, and test specimen.
Ms 5 mass of solid particles (Ms 5 Mcds Mc), g.
13. Precision and Bias
12. Report 13.1 Statement on BiasThere is no accepted reference
12.1 Test data forms or test data sheets shall include the value for this test method; therefore, bias cannot be deter-
following: mined.
12.1.1 Identification of the sample (material) being tested, 13.2 Statements on Precision:
such as boring number, sample number, test number, container 13.2.1 Single-Operator Precision (Repeatability)The
number etc. single-operator coefficient of variation has been found to be 2.7
12.1.2 Water content of the specimen to the nearest 1 % or percent. Therefore, results of two properly conducted tests by
0.1 %, as appropriate based on the minimum sample used. If the same operator with the same equipment should not be
this method is used in concert with another method, the water considered suspect unless they differ by more than 7.8 percent
content of the specimen should be reported to the value of their mean.8
required by the test method for which the water content is 13.2.2 Multilaboratory Precision (Reproducibility)9The
being determined. Refer to Guide D 6026 for guidance con- multilaboratory coefficient of variation has been found to be
cerning significant digits, especially if the value obtained from 5.0 percent. Therefore, results of two properly conducted tests
this test method is to be used to calculate other relationships by different operators using different equipment should not be
such as unit weight or density. For instance, if it is desired to considered suspect unless they differ by more than 14.0 percent
express dry unit weight to the nearest 0.1 lbf/f3(0.02 kN/m3), it of their mean.
may be necessary to use a balance with a greater readability or 14. Keywords
use a larger specimen mass to obtain the required significant 14.1 consistency; index property; laboratory; moisture
digits the mass of water so that the water content can be analysis; moisture content; soil aggregate; water content
determined to the required significant digits. Also, the signifi-
cant digits in Guide D 6026 may need to be increased when
8
calculating phase relationships requiring four significant digits. These numbers represent the (1s) and (d2s) limits as described in Practice C
670.
12.1.3 Indicate if test specimen had a mass less than the 9
These numbers represent the (1s %) and (d2s %) limits as described in Practice
minimum indicated in 8.2. C 670.
SUMMARY OF CHANGES
Committee D-18 has identified the location of selected changes to this standard since the last issue.
(D 2216-92) that may impact the use of this standard.
(1) Title was changed to emphasize that mass is the basis for (10) In 6.4, anhydrous calcium phosphate was changed to
the standard. anyhydrous calcium sulfate to correct an error and to agree
(2) Section 1.1 was revised to clarify similar materials. with Note 3.
(3) New 1.2 was added to explain a limitation in scope. The (11) A typo in 8.1 was corrected from before to below and
other sections were renumbered as appropriate. a footnoted reference was added for information.
(4) An information reference was included in 1.5. (12) A portion of 8.2 was deleted for clarity.
(5) An information reference was included in 1.6 (13) A new 8.2.1 was added to clarify minimum mass require-
(6) A new ASTM referenced document was included in 2.1. ments.
(7) New Footnotes 2, 3, and 5 were added and identified.
(14) Sections 8.3, 8.4, 9.3.3, and 12.1 were changed to
Other footnotes were renumbered where necessary for sequen-
substitute test data form/sheet for report.
tial identification.
(8) Information concerning balances was added in 6.2 (15) Footnote seven was identified.
(9) Section 6.3 was revised to clarify the use of close-fitting (16) Section 9.2.1 was revised to improve clarity and intent.
lids, and a reference to Note 8 was added. (17) The word possible was changed to practical in 9.2.3.
4 170
D 2216
(18) Section 9.3.1 and 9.3.2 were revised to improve clarity version. These explanations provide clarity and information to
and for practicality. the user.
(19) A reference to Guide D 6026 was added in 12.1.2. (21) A Summary of Changes was added to reflect D-18s
(20) Footnotes 8 and 9 were added to 13.2.1 and 13.2.2, policy.
respectively. These were inadvertently omitted from the 1992
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your
views known to the ASTM Committee on Standards, 100 Barr Harbor Drive, West Conshohocken, PA 19428.
5 171
Designation: D 4318 00
174
3
D 4318
6.3 GageA metal gage block for adjusting the height-of- GP1 (readability of 0.01 g).
drop of the cup, having the dimensions shown in Fig. 4. The 6.6 Mixing and Storage ContainerA container to mix the
design of the tool may vary provided the gage will rest securely soil specimen (material) and store the prepared material.
on the base without being susceptible to rocking, and the edge During mixing and storage, the container shall not contaminate
which contacts the cup during adjustment is straight, at least 10 the material in any way, and prevent moisture loss during
mm (38 in.) wide, and without bevel or radius. storage. A porcelain, glass, or plastic dish about 11.4 cm
6.4 Water Content ContainersSmall corrosion-resistant (412 in.) in diameter and a plastic bag large enough to enclose
containers with snug-fitting lids for water content specimens.
the dish and be folded over is adequate.
Aluminum or stainless steel cans 2.5 cm (1 in.) high by 5 cm
(2 in.) in diameter are appropriate. 6.7 Plastic Limit:
6.5 Balance, conforming to Specification D 4753, Class 6.7.1 Ground Glass PlateA ground glass plate at least 30
175
4
D 4318
having a rim at least 5 cm (2 in.) above the mesh. A 2.00-mm
(No. 10) sieve meeting the same requirements may also be
needed.
6.10 Wash Bottle, or similar container for adding controlled
amounts of water to soil and washing fines from coarse
particles.
6.11 Drying Oven, thermostatically controlled, preferably of
the forced-draft type, capable of continuously maintaining a
temperature of 110 6 5C (230 6 9F) throughout the drying
chamber.
6.12 Washing Pan, round, flat-bottomed, at least 7.6 cm (3
FIG. 4 Height-of-Drop Gage
in.) deep, and slightly larger at the bottom than a 20.3-cm
(8-in.) diameter sieve.
cm (12 in.) square by 1 cm (38 in.) thick for rolling plastic limit
7. Reagents and Materials
threads.
6.7.2 Plastic Limit-Rolling Device (optional)A device 7.1 Purity of WaterWhere distilled water is referred to in
made of acrylic conforming to the dimensions shown in Fig. this test method, either distilled or demineralized water may be
5.7,8 The type of unglazed paper attached to the top and bottom used. See Note 7 covering the use of tap water.
plate (see 16.2.2) shall be such that it does not add foreign 8. Sampling and Specimen
matter (fibers, paper fragments, etc.) to the soil during the
rolling process. 8.1 Samples may be taken from any location that satisfies
6.8 SpatulaA spatula or pill knife having a blade about 2 testing needs. However, Practices C 702, D 75, and D 420
cm (34 in.) wide, and about 10 to 13 cm (3 to 4 in.) long. should be used as guides for selecting and preserving samples
6.9 Sieve(s)A 200-mm (8-in.) diameter, 425-m (No. 40) from various types of sampling operations. Samples in which
sieve conforming to the requirements of Specification E 11 and specimens will be prepared using the wet-preparation method
(10.1) must be kept at their assampled water content prior to
preparation.
8.1.1 Where sampling operations have preserved the natural
7
The plastic limit-rolling device is covered by a patent (U.S. Patent No. stratification of a sample, the various strata must be kept
5,027,660).7 Interested parties are invited to submit information regarding the separated and tests performed on the particular stratum of
identification of an alternative(s) to this patented item to ASTM Headquarters. Your
comments will receive careful consideration at a meeting of the responsible interest with as little contamination as possible from other
subcommittee, which you may attend. strata. Where a mixture of materials will be used in construc-
8
Bobrowski, L. J., Jr. and Griekspoor, D. M., Determination of the Plastic Limit tion, combine the various components in such proportions that
of a Soil by Means of a Rolling Device, Geotechnical Testing Journal, GTJODJ,
the resultant sample represents the actual construction case.
Vol 15, No. 3, September 1992, pp. 284287.
176
5
D 4318
8.1.2 Where data from these test methods are to be used for maximum height. Slide the height gage under the cup from the front, and
correlation with other laboratory or field test data, use the same observe whether the gage contacts the cup or the tape. (See Fig. 2.) If the
material as used for those tests where possible. tape and cup are both simultaneously contacted, the height-of-drop is
ready to be checked. If not, adjust the cup until simultaneous contact is
8.2 SpecimenObtain a representative portion from the made. Check adjustment by turning the crank at 2 revolutions per second
total sample sufficient to provide 150 to 200 g of material while holding the gage in position against the tape and cup. If a faint
passing the 425-m (No. 40) sieve. Free flowing samples ringing or clicking sound is heard without the cup rising from the gage, the
(materials) may be reduced by the methods of quartering or adjustment is correct. If no ringing is heard or if the cup rises from the
splitting. Non-free flowing or cohesive materials shall be gage, readjust the height-of-drop. If the cup rocks on the gage during this
mixed thoroughly in a pan with a spatula or scoop and a checking operation, the cam follower pivot is excessively worn and the
worn parts should be replaced. Always remove tape after completion of
representative portion scooped from the total mass by making
adjustment operation.
one or more sweeps with a scoop through the mixed mass.
10. Preparation of Test Specimen
9. Calibration of Apparatus
10.1 Wet Preparation MethodExcept where the dry
9.1 Inspection of Wear: method of specimen preparation is specified (10.2), prepare the
9.1.1 Liquid Limit DeviceDetermine that the liquid limit specimen for testing as described in the following sections.
device is clean and in good working order. Check the following 10.1.1 Material Passes the 425-m (No. 40) Sieve:
specific points. 10.1.1.1 Determine by visual and manual methods that the
9.1.1.1 Wear of BaseThe spot on the base where the cup specimen from 8.2 has little or no material retained on a
makes contact should be worn no greater than 10 mm (38 in.) 425-m (No. 40) sieve. If this is the case, prepare 150 to 200
in diameter. If the wear spot is greater than this, the base can g of material by mixing thoroughly with distilled or deminer-
be machined to remove the worn spot provided the resurfacing alized water on the glass plate or mixing dish using the spatula.
does not make the base thinner than specified in 6.1 and the If desired, soak the material in a mixing/storage dish with a
other dimensional relationships are maintained. small amount of water to soften the material before the start of
9.1.1.2 Wear of CupReplace the cup when the grooving mixing. If using Method A, adjust the water content of the
tool has worn a depression in the cup 0.1 mm (0.004 in.) deep material to bring it to a consistency that would require about 25
or when the rim of the cup has been reduced to half its original to 35 blows of the liquid limit device to close the groove (Note
thickness. Verify that the cup is firmly attached to the cup 6). For Method B, the number of blows should be between
hanger. about 20 and 30 blows.
9.1.1.3 Wear of Cup HangerVerify that the cup hanger 10.1.1.2 If, during mixing, a small percentage of material is
pivot does not bind and is not worn to an extent that allows encountered that would be retained on a 425-m (No. 40)
more than 3 mm (18 in.) side-to-side movement of the lowest sieve, remove these particles by hand (if possible). If it is
point on the rim. impractical to remove the coarser material by hand, remove
9.1.1.4 Wear of CamThe cam shall not be worn to an small percentages (less than about 15 %) of coarser material by
extent that the cup drops before the cup hanger (cam follower) working the material (having the above consistency) through a
loses contact with the cam. 425-m sieve. During this procedure, use a piece of rubber
9.1.2 Grooving ToolsInspect grooving tools for wear on a sheeting, rubber stopper, or other convenient device provided
frequent and regular basis. The rapidity of wear depends on the the procedure does not distort the sieve or degrade material that
material from which the tool is made, and the types of soils would be retained if the washing method described in 10.1.2
being tested. Soils containing a large proportion of fine sand were used. If larger percentages of coarse material are encoun-
particles may cause rapid wear of grooving tools; therefore, tered during mixing, or it is considered impractical to remove
when testing these materials, tools should be inspected more the coarser material by the procedures just described, wash the
frequently than for other soils. sample as described in 10.1.2. When the coarse particles found
NOTE 4The width of the tip of grooving tools is conveniently checked during mixing are concretions, shells, or other fragile particles,
using a pocket-sized measuring magnifier equipped with a millimeter do not crush these particles to make them pass a 425-m sieve,
scale. Magnifiers of this type are available from most laboratory supply but remove by hand or by washing.
companies. The depth of the tip of grooving tools can be checked using the 10.1.1.3 Place the prepared material in the mixing/storage
depth-measuring feature of vernier calipers.
dish, check its consistency (adjust if required), cover to prevent
9.2 Adjustment of Height-of-DropAdjust the height-of- loss of moisture, and allow to stand (cure) for at least 16 h
drop of the cup so that the point on the cup that comes in (overnight). After the standing period and immediately before
contact with the base rises to a height of 10 6 0.2 mm. See Fig. starting the test, thoroughly remix the soil.
2 for proper location of the gage relative to the cup during
NOTE 6The time taken to adequately mix a soil will vary greatly,
adjustment.
depending on the plasticity and initial water content. Initial mixing times
NOTE 5A convenient procedure for adjusting the height-of-drop is as of more than 30 min may be needed for stiff, fat clays.
follows: place a piece of masking tape across the outside bottom of the cup 10.1.2 Material Containing Particles Retained on a 425-m
parallel with the axis of the cup hanger pivot. The edge of the tape away
from the cup hanger should bisect the spot on the cup that contacts the
(No. 40) Sieve:
base. For new cups, placing a piece of carbon paper on the base and 10.1.2.1 Place the specimen (see 8.2) in a pan or dish and
allowing the cup to drop several times will mark the contact spot. Attach add sufficient water to cover the material. Allow the material to
the cup to the device and turn the crank until the cup is raised to its soak until all lumps have softened and the fines no longer
177
6
D 4318
adhere to the surfaces of the coarse particles (Note 7). number of blows should be between about 20 and 30. Put, if
necessary, the mixed material in the storage dish, cover to
NOTE 7In some cases, the cations of salts present in tap water will
exchange with the natural cations in the soil and significantly alter the test prevent loss of moisture, and allow to stand (cure) for at least
results if tap water is used in the soaking and washing operations. Unless 16 h. After the standing period and immediately before starting
it is known that such cations are not present in the tap water, distilled or the test, thoroughly remix the specimen.
demineralized water should be used. As a general rule, water containing 10.2 Dry Preparation Method:
more than 100 mg/L of dissolved solids should not be used for either the 10.2.1 Dry the specimen from 8.2 at room temperature or in
soaking or washing operations. an oven at a temperature not exceeding 60C until the soil
10.1.2.2 When the material contains a large percentage of clods will pulverize readily. Disaggregation is expedited if the
particles retained on the 425-m (No. 40) sieve, perform the material is not allowed to completely dry. However, the
following washing operation in increments, washing no more material should have a dry appearance when pulverized.
than 0.5 kg (1 lb) of material at one time. Place the 425-m 10.2.2 Pulverize the material in a mortar with a rubber-
sieve in the bottom of the clean pan. Transfer, without any loss tipped pestle or in some other way that does not cause
of material, the soil-water mixture onto the sieve. If gravel or breakdown of individual particles. When the coarse particles
coarse sand particles are present, rinse as many of these as found during pulverization are concretions, shells, or other
possible with small quantities of water from a wash bottle, and fragile particles, do not crush these particles to make them pass
discard. Alternatively, transfer the soil-water mixture over a a 425-m (No. 40) sieve, but remove by hand or other suitable
2.00-mm (No. 10) sieve nested atop the 425-m sieve, rinse the means, such as washing. If a washing procedure is used, follow
fine material through and remove the 2.00-mm sieve. After 10.1.2.1-10.1.2.4.
washing and removing as much of the coarser material as 10.2.3 Separate the material on a 425-m (No. 40) sieve,
possible, add sufficient water to the pan to bring the level to shaking the sieve by hand to assure thorough separation of the
about 13 mm (12 in.) above the surface of the 425-m sieve. finer fraction. Return the material retained on the 425-m sieve
Agitate the slurry by stirring with the fingers while raising and to the pulverizing apparatus and repeat the pulverizing and
lowering the sieve in the pan and swirling the suspension so sieving operations. Stop this procedure when most of the fine
that fine material is washed from the coarser particles. Disag- material has been disaggregated and material retained on the
gregate fine soil lumps that have not slaked by gently rubbing 425-m sieve consists of individual particles.
them over the sieve with the fingertips. Complete the washing 10.2.4 Place material retained on the 425-m (No. 40) sieve
operation by raising the sieve above the water surface and after the final pulverizing operations in a dish and soak in a
rinsing the material retained with a small amount of clean small amount of water. Stir this mixture and transfer it to a
water. Discard material retained on the 425-m sieve. 425-m sieve, catching the water and any suspended fines in
10.1.2.3 Reduce the water content of the material passing the washing pan. Pour this suspension into a dish containing
the 425m (No. 40) sieve until it approaches the liquid limit. the dry soil previously sieved through the 425-m sieve.
Reduction of water content may be accomplished by one or a Discard material retained on the 425-m sieve.
combination of the following methods: (a) exposing to air 10.2.5 Proceed as described in 10.1.2.3 and 10.1.2.4.
currents at room temperature, (b) exposing to warm air currents
from a source such as an electric hair dryer, (c) decanting clear MULTIPOINT LIQUID LIMITMETHOD A
water from surface of the suspension, (d) filtering in a Bchner
funnel or using filter candles, or (e) draining in a colander or 11. Procedure
plaster of Paris dish lined with high retentivity,9 high wet- 11.1 Thoroughly remix the specimen (soil) in its mixing
strength filter paper. If a plaster of Paris dish is used, take care cup, and, if necessary, adjust its water content until the
that the dish never becomes sufficiently saturated that it fails to constancy requires about 25 to 35 blows of the liquid limit
absorb water into its surface. Thoroughly dry dish between device to close the groove. Using a spatula, place a portion(s)
uses. During evaporation and cooling, stir the material often of the prepared soil in the cup of the liquid limit device at the
enough to prevent over-drying of the fringes and soil pinnacles point where the cup rests on the base, squeeze it down, and
on the surface of the mixture. For materials containing soluble spread it into the cup to a depth of about 10 mm at its deepest
salts, use a method of water reduction (a or b) that will not point, tapering to form an approximately horizontal surface.
eliminate the soluble salts from the test specimen. Take care to eliminate air bubbles from the soil pat, but form
10.1.2.4 If applicable, remove the material retained on the the pat with as few strokes as possible. Keep the unused soil in
filter paper. Thoroughly mix this material or the above material the mixing/storage dish. Cover the dish with a wet towel (or
on the glass plate or in the mixing dish using the spatula. use other means) to retain the moisture in the soil.
Adjust the water content of the mixture, if necessary, by adding 11.2 Form a groove in the soil pat by drawing the tool,
small increments of distilled or demineralized water or by beveled edge forward, through the soil on a line joining the
allowing the mixture to dry at room temperature while mixing highest point to the lowest point on the rim of the cup. When
on the glass plate. If using Method A, the material should be at cutting the groove, hold the grooving tool against the surface of
a water content that would require about 25 to 35 blows of the the cup and draw in an arc, maintaining the tool perpendicular
liquid limit device to close the groove. For Method B, the to the surface of the cup throughout its movement. See Fig. 6.
In soils where a groove cannot be made in one stroke without
tearing the soil, cut the groove with several strokes of the
9
S and S 595 filter paper available in 320-mm circles has proven satisfactory. grooving tool. Alternatively, cut the groove to slightly less than
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D 4318
required dimensions with a spatula and use the grooving tool to 11.4 Verify that an air bubble has not caused premature
bring the groove to final dimensions. Exercise extreme care to closing of the groove by observing that both sides of the groove
prevent sliding the soil pat relative to the surface of the cup. have flowed together with approximately the same shape. If a
11.3 Verify that no crumbs of soil are present on the base or bubble has caused premature closing of the groove, reform the
the underside of the cup. Lift and drop the cup by turning the soil in the cup, adding a small amount of soil to make up for
crank at a rate of 1.9 to 2.1 drops per second until the two that lost in the grooving operation and repeat 11.1-11.3. If the
halves of the soil pat come in contact at the bottom of the soil slides on the surface of the cup, repeat 11.1-11.3 at a higher
groove along a distance of 13 mm (12 in.). See Fig. 7. water content. If, after several trials at successively higher
NOTE 8Use of a scale is recommended to verify that the groove has water contents, the soil pat continues to slide in the cup or if the
closed 13 mm (12 in.). number of blows required to close the groove is always less
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than 25, record that the liquid limit could not be determined, 13.3 Determine water contents of specimens in accordance
and report the soil as nonplastic without performing the plastic with 11.8.
limit test.
11.5 Record the number of drops, N, required to close the 14. Calculation
groove. Remove a slice of soil approximately the width of the 14.1 Determine the liquid limit for each water content
spatula, extending from edge to edge of the soil cake at right specimen using one of the following equations:
S D
angles to the groove and including that portion of the groove in N 0.121
which the soil flowed together, place in a container of known LLn 5 Wn 25
mass, and cover.
or
11.6 Return the soil remaining in the cup to the dish. Wash
and dry the cup and grooving tool and reattach the cup to the LLn 5 k Wn
carriage in preparation for the next trial.
11.7 Remix the entire soil specimen in the dish adding where:
LLn = one point liquid limit for given trial, %,
distilled water to increase the water content of the soil and
N = number of blows causing closure of the groove for
decrease the number of blows required to close the groove.
given trial,
Repeat 11.1-11.6 for at least two additional trials producing Wn = water content for given trial, %, and
successively lower numbers of blows to close the groove. One k = factor given in Table 1.
of the trials shall be for a closure requiring 25 to 35 blows, one 14.1.1 The liquid limit, LL, is the average of the two trial
for closure between 20 and 30 blows, and one trial for a closure liquid-limit values, to the nearest whole number (without the
requiring 15 to 25 blows. percent designation).
11.8 Determine the water content, Wn, of the soil specimen 14.2 If the difference between the two trial liquid-limit
from each trial in accordance with Test Method D 2216. values is greater than one percentage point, repeat the test as
11.8.1 Determination of initial masses (container plus moist described in 13.1 through 14.1.1.
soil) should be performed immediately after completion of the
test. If the test is to be interrupted for more than about 15 PLASTIC LIMIT
minutes, determine the mass of the water content specimens
already obtained at the time of the interruption. 15. Preparation of Test Specimen
15.1 Select a 20-g or more portion of soil from the material
12. Calculation prepared for the liquid limit test; either, after the second mixing
12.1 Plot the relationship between the water content, Wn, before the test, or from the soil remaining after completion of
and the corresponding number of drops, N, of the cup on a the liquid limit test. Reduce the water content of the soil to a
semilogarithmic graph with the water content as ordinates on consistency at which it can be rolled without sticking to the
the arithmetical scale, and the number of drops as abscissas on hands by spreading or mixing continuously on the glass plate
a logarithmic scale. Draw the best straight line through the or in the mixing/storage dish. The drying process may be
three or more plotted points. accelerated by exposing the soil to the air current from an
12.2 Take the water content corresponding to the intersec- electric fan, or by blotting with paper, that does not add any
tion of the line with the 25-drop abscissa as the liquid limit of fiber to the soil. Paper such as hard surface paper toweling or
the soil and round to the nearest whole number. Computational high wet-strength filter paper is adequate.
methods may be substituted for the graphical method for fitting
a straight line to the data and determining the liquid limit. 16. Procedure
16.1 From this plastic-limit specimen, select a 1.5 to 2.0 g
ONE-POINT LIQUID LIMITMETHOD B portion. Form the selected portion into an ellipsoidal mass.
16.2 Roll the soil mass by one of the following methods
13. Procedure (hand or rolling device):
13.1 Proceed as described in 11.1-11.5 except that the
number of blows required to close the groove shall be 20 to 30. TABLE 1 Factors for Obtaining Liquid Limit from Water Content
If less than 20 or more than 30 blows are required, adjust the and Number of Drops Causing Closure of Groove
water content of the soil and repeat the procedure. N k
13.2 Immediately after removing a water content specimen (Number of Drops) (Factor for Liquid Limit)
as described in 11.5, reform the soil in the cup, adding a small 20 0.973
amount of soil to make up for that lost in the grooving and 21 0.979
22 0.985
water content sampling orientations. Repeat 11.2-11.5, and, if 23 0.990
the second closing of the groove requires the same number of 24 0.995
drops or no more than two drops difference, secure another 25 1.000
26 1.005
water content specimen. Otherwise, remix the entire specimen 27 1.009
and repeat. 28 1.014
29 1.018
NOTE 9Excessive drying or inadequate mixing will cause the number 30 1.022
of blows to vary.
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D 4318
16.2.1 Hand MethodRoll the mass between the palm or together, knead between the thumb and first finger of each
fingers and the ground-glass plate with just sufficient pressure hand, reform into an ellipsoidal mass, and re-roll. Continue this
to roll the mass into a thread of uniform diameter throughout its alternate rolling to a thread 3.2 mm in diameter, gathering
length (see Note 10). The thread shall be further deformed on together, kneading and re-rolling, until the thread crumbles
each stroke so that its diameter reaches 3.2 mm (18 in.), taking under the pressure required for rolling and the soil can no
no more than 2 min (see Note 11). The amount of hand or longer be rolled into a 3.2-mm diameter thread (see Fig. 8). It
finger pressure required will vary greatly according to the soil has no significance if the thread breaks into threads of shorter
being tested, that is, the required pressure typically increases length. Roll each of these shorter threads to 3.2 mm in
with increasing plasticity. Fragile soils of low plasticity are diameter. The only requirement for continuing the test is that
best rolled under the outer edge of the palm or at the base of the
these threads can be reformed into an ellipsoidal mass and
thumb.
rolled out again. The operator shall at no time attempt to
NOTE 10A normal rate of rolling for most soils should be 80 to 90 produce failure at exactly 3.2-mm diameter by allowing the
strokes per minute, counting a stroke as one complete motion of the hand thread to reach 3.2 mm, then reducing the rate of rolling or the
forward and back to the starting position. This rate of rolling may have to
be decreased for very fragile soils.
hand pressure, or both, while continuing the rolling without
NOTE 11A 3.2-mm (18-in.) diameter rod or tube is useful for frequent further deformation until the thread falls apart. It is permis-
comparison with the soil thread to ascertain when the thread has reached sible, however, to reduce the total amount of deformation for
the proper diameter. feebly plastic soils by making the initial diameter of the
16.2.2 Rolling Device MethodAttach smooth unglazed ellipsoidal mass nearer to the required 3.2-mm final diameter.
paper to both the top and bottom plates of the plastic If crumbling occurs when the thread has a diameter greater
limit-rolling device. Place the soil mass on the bottom plate at than 3.2 mm, this shall be considered a satisfactory end point,
the midpoint between the slide rails. Place the top plate in provided the soil has been previously rolled into a thread 3.2
contact with the soil mass(es). Simultaneously apply a slight mm in diameter. Crumbling of the thread will manifest itself
downward force and back and forth motion to the top plate so differently with the various types of soil. Some soils fall apart
that the top plate comes into contact with the side rails within in numerous small aggregations of particles, others may form
2 min (see Notes 10 and 12). During this rolling process, the an outside tubular layer that starts splitting at both ends. The
end(s) the soil thread(s) shall not contact the side rail(s). If this splitting progresses toward the middle, and finally, the thread
occurs, roll a smaller mass of soil (even if it is less than that falls apart in many small platy particles. Fat clay soils require
mentioned in Section 16.1). much pressure to deform the thread, particularly as they
NOTE 12In most cases, two soil masses (threads) can be rolled approach the plastic limit. With these soils, the thread breaks
simultaneously in the plastic limit-rolling device. into a series of barrel-shaped segments about 3.2 to 9.5 mm (18
16.3 When the diameter of the thread becomes 3.2 mm, to 38 in.) in length.
break the thread into several pieces. Squeeze the pieces 16.4 Gather the portions of the crumbled thread together
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D 4318
and place in a container of known mass. Immediately cover the liquid limit or plastic limit tests could not be performed, or if
container. the plastic limit is equal to or greater than the liquid limit,
16.5 Select another 1.5 to 2.0-g portion of soil from the report the soil as nonplastic, NP,
plasticlimit specimen and repeat the operations described in 19.1.5 Estimate of the percentage of sample retained on the
16.1 and 16.2 until the container has at least 6 g of soil. 425-m (No. 40) sieve, and
16.6 Repeat 16.1-16.5 to make another container holding at 19.1.6 Procedure by which liquid limit was performed, if it
least 6 g of soil. Determine the water content of the soil differs from the multipoint method.
contained in the containers in accordance with Test Method
D 2216. See 11.8.1. 20. Precision and Bias
20.1 PrecisionCriteria for judging the acceptability of test
17. Calculation
results obtained by these test methods on a range of soil types
17.1 Compute the average of the two water contents (trial are given in Tables 2 and 3. In performing these test methods,
plastic limits) and round to the nearest whole number. This Method A and the Wet Preparation Method (except soil was
value is the plastic limit, PL. Repeat the test if the difference air-dried) were used.
between the two trial plastic limits is greater than the accept- 20.1.1 These estimates of precision are based on the results
able range for two results listed in Table 2 for single-operator of the interlaboratory program conducted by the ASTM Ref-
precision, that is, 1.4 percentage points; i.e., (2.8 3 0.5). erence Soils and Testing Program.10 In this program, some
PLASTICITY INDEX laboratories performed three replicate tests per soil type
(triplicate test laboratory), while other laboratories performed a
18. Calculation single test per soil type (single-test laboratory). A description
18.1 Calculate the plasticity index as follows: of the soils tested is given in 20.1.5. The precision estimates
vary with soil type and method(s) used. Judgment is required
PI 5 LL 2 PL
when applying these estimates to another soil and method used
where: (Method A or B, or Wet or Dry Preparation Method).
LL = liquid limit (whole number), and 20.1.2 The data in Table 2 are based on three replicate tests
PL = plastic limit (whole number). performed by each triplicate test laboratory on each soil type.
18.1.1 Both LL and PL are whole numbers. If either the The single operator and multilaboratory standard deviation
liquid limit or plastic limit could not be determined, or if the shown in Table 2, Column 4, were obtained in accordance with
plastic limit is equal to or greater than the liquid limit, report Practice E 691, which recommends each testing laboratory
the soil as nonplastic, NP. perform a minimum of three replicate tests. Results of two
properly conducted tests performed by the same operator on
19. Report the same material, using the same equipment, and in the
19.1 Report the following information: shortest practical period of time should not differ by more than
19.1.1 Sample identifying information, the single-operator d2s limits shown in Table 2, Column 5. For
19.1.2 Any special specimen selection process used, such as definition of d2s see Footnote C in Table 2. Results of two
removal of sand lenses from undisturbed sample, properly conducted tests performed by different operators and
19.1.3 Report sample as air-dried if the sample was air-dried
before or during preparation,
19.1.4 Liquid limit, plastic limit, and plasticity index to the 10
Supporting data are available from ASTM Headquarters. Request RR: D18-
nearest whole number, omitting the percent designation. If the 1013.
TABLE 2 Summary of Test Results from Triplicate Test Laboratories (Atterberg Limits)
(1) (2) (3) (4) (5)
Number of Triplicate Test Average ValueA (Percentage Standard DeviationB Acceptable Range of Two
C
Soil Type Laboratories Points) (Percentage Points) Results (Percentage Points)
Type Test
LL PL PI LL PL PI LL PL PI LL PL PI
Single-Operator Results (Within-Laboratory Repeatability)
CH 13 13 13 59.8 20.6 39.2 0.7 0.5 0.8 2 1 2
CL 14 13 13 33.4 19.9 13.6 0.3 0.4 0.5 1 1 1
D D
ML 12 11 11 27.4 23.4 4.1 0.5 0.3 0.6 2 1 2
Multilaboratory Results (Between-Laboratory Reproducibility)
CH 13 13 13 59.8 20.6 39.2 1.3 2.0 2.5 4 6 7
CL 14 13 13 33.4 19.9 13.6 1.0 1.2 1.7 3 3 5
ML 12 11 11 27.4 23.4D 4.1D 1.3 0.9 1.9 4 3 5
A
The number of significant digits and decimal places presented are representative of the input data. In accordance with Practice D 6026, the standard deviation and
acceptable range of results can not have more decimal places than the input data.
B
Standard deviation is calculated in accordance with Practice E 691 and is referred to as the 1s limit.
C
Acceptable range of two results is referred to as the d2s limit. It is calculated as 2 1.960 =2 1s, as defined by Practice E 177. The difference between two properly
conducted tests should not exceed this limit. The number of significant digits/decimal places presented is equal to that prescribed by this test method or Practice D 6026.
In addition, the value presented can have the same number of decimal places as the standard deviation, even if that result has more significant digits than the standard
deviation.
D
For the ML soil, 2 out of 14 triplicate test laboratories reported the soil as nonplastic.
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11
D 4318
TABLE 3 Summary of Single-Test Result from Each Laboratory laboratories with different operators using different equipment
(Atterberg Limits)A and on different days should not vary by more than the d2s
(1) (2) (3) (4) (5) limits shown in Table 3, Column 5. The results in Table 2 and
Acceptable
Standard Range of Two
Table 3 are dissimilar because the data sets are different.
Average Value Deviation Results 20.1.4 Table 2 presents a rigorous interpretation of triplicate
Number of Test (Percentage (Percentage (Percentage test data in accordance with Practice E 691 from pre-qualified
Soil Type Laboratories Points) Points) Points)
laboratories. Table 3 is derived from test data that represents
Type Test
LL PL PI LL PL PI LL PL PI
common practice.
20.1.5 Soil TypesBased on the multilaboratory test re-
CH 24 59.9 20.4 39.5 2.1 2.7 3.1 6 7 9
CL 24 33.3 19.9 13.4 0.8 1.3 1.6 2 4 4 sults, the soils used in the program are described below in
ML 18 27.1 23.2B 3.9B 1.3 1.2 1.8 4 3 5 accordance with Practice D 2487. In addition, the local names
A
For column footnotes, see Table 3. of the soils are given.
B
For the ML soil, 6 out of 24 laboratories reported the soil as nonplastic. CHFat clay, CH, 99 % fines, LL=60, PI=39, grayish brown, soil had been
air dried and pulverized. Local nameVicksburg Buckshot Clay
CLLean clay, CL, 89 % fines, LL=33, PI=13, gray, soil had been air dried
on different days should not differ by more than the multilabo- and pulverized. Local nameAnnapolis Clay
ratory d2s limits shown in Table 2, Column 5. MLSilt, ML, 99 % fines, LL=27, PI=4, light brown, soil had been air dried
20.1.3 In the ASTM Reference Soils and Testing Program, and pulverized. Local nameVicksburg Silt
many of the laboratories performed only a single test on each 20.2 BiasThere is no acceptable reference value for these
soil type. This is common practice in the design and construc- test methods; therefore, bias cannot be determined.
tion industry. The data for each soil type in Table 3 are based
upon the first test results from the triplicate test laboratories 21. Keywords
and the single test results from the other laboratories. Results 21.1 activity; Atterberg limits; liquid limit; plasticity index;
of two properly conducted tests performed by two different plastic limit
ANNEX
(Mandatory Information)
A1.1 A device for measuring the resilience of liquid limit tested. Holding the tube lightly against the liquid limit device
device bases is shown in Fig. A1.1. The device consists of a base with one hand, release the ball by pulling the magnet out
clear acrylic plastic tube and cap, a 516-in. diameter steel ball, of the cap. Use the scale markings on the outside of the
and a small bar magnet. The cylinder may be cemented to the cylinder to determine the highest point reached by the bottom
cap or threaded as shown. The small bar magnet is held in the of the ball. Repeat the drop at least three times, placing the
recess of the cap and the steel ball is fixed into the recess in the tester in a different location for each drop. Tests should be
underside of the cap with the bar magnet. The cylinder is then conducted at room temperature.
turned upright and placed on the top surface of the base to be
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D 4318
SUMMARY OF CHANGES
Committee D18 has identified the location of selected changes to this standard since the last issue (1998) that
may impact the use of this standard.
(1) Replaced procedure with method, when the topic (7) Under Preparation of Test Specimen: The subsections
covers how one is to perform a task. covering the wet and dry preparation methods were reworded
(2) In Scope covering units, clarified that the standard units to include the required number of blows for Method A and B.
for resilience tester are in inch-pound, not metric. In addition, used the term material instead of soil or sample,
(3) Where applicable, replaced weight with mass or whenever applicable, and replaced grains with particle..
reworded to remove such terms as weight, weighing, or (8) Under One-Point Liquid Limit, Method B, Section 13 on
weigh. Preparation of Test Specimen was removed since the informa-
(4) Where applicable, replaced natural as an adjective to tion given in that section was moved to 10.1.2.4.
water content with such terms as its or as-sampled. (9) In the calculation sections, defined that the calculated test
(5) In Apparatus, under 6.6, storage container was changed result is rounded to the nearest whole number.
to mixing and storage container and subsection reworded to (10) References to Practice C 670 were deleted in text, and
indicate this container/dish may be used to mix the soil. references to Practices D 3740, D 6026, E 177, and E 691 were
Remaining sections in the standard, where applicable, were incorporated.
reworded to indicate storage dish may also be the mixing (11) At the end of the Significance and Use section, a new Note
dish. 1 was added referencing Practice D 3740 in accordance with
(6) In Section 8, changed title to include Specimen, and D18 policy, and all subsequent notes were renumbered.
where applicable reworded to distinguish between the sample (12) Section 20.1 on Precision was revised completely.
and the specimen before processing using the wet or dry (13) In Table 1, corrected the factor for 20 number of drops.
preparation method. (14) Appendix X1 was changed to Annex A1, and the scribe
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D 4318
line at 8.0 in Fig. A1.1 was changed to 7.7.
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185
14
Designation: D 854 02
pycnometer using a wash/spray squirt bottle. entrapped air should only be removed by use of an aspirator. Kerosene is
9.2.4 Proceed as described in 9.4. a flammable liquid that must be used with extreme caution.
9.3 Method BProcedure for Oven-Dried Specimens: 9.5 Deairing the Soil SlurryEntrapped air in the soil
9.3.1 Dry the specimen to a constant mass in an oven slurry can be removed using either heat (boiling), vacuum or
maintained at 110 6 5C. Break up any clods of soil using a combining heat and vacuum.
mortar and pestle. If the soil will not easily disperse after 9.5.1 When using the heat-only method (boiling), use a
drying or has changed composition, use Test Method A. Refer duration of at least 2 h after the soil-water mixture comes to a
to 1.2.1 for soils that require use of Test Method A. full boil. Use only enough heat to keep the slurry boiling.
9.3.2 Place the funnel into the pycnometer. The stem of the Agitate the slurry as necessary to prevent any soil from sticking
funnel must extend past the calibration mark or stopper seal. to or drying onto the glass above the slurry surface.
Spoon the soil solids directly into the funnel. Rinse any soil 9.5.2 If only a vacuum is used, the pycnometer must be
particles remaining on the funnel into the pycnometer using a continually agitated under vacuum for at least 2 h. Continually
wash/spray squirt bottle. agitated means the silt/clay soil solids will remain in suspen-
9.4 Preparing the Soil SlurryAdd water until the water sion, and the slurry is in constant motion. The vacuum must
level is between 13 and 12 of the depth of the main body of the remain relatively constant and be sufficient to cause bubbling at
pycnometer. Agitate the water until slurry is formed. Rinse any the beginning of the deairing process.
soil adhering to the pycnometer into the slurry. 9.5.3 If a combination of heat and vacuum are used, the
9.4.1 If slurry is not formed, but a viscous paste, use a pycnometers can be placed in a warm water bath (not more
pycnometer having a larger volume. See 7.1.1. than 40C) while applying the vacuum. The water level in the
NOTE 5For some soils containing a significant fraction of organic bath should be slightly below the water level in the pycnom-
matter, kerosene is a better wetting agent than water and may be used in eter, if the pycnometer glass becomes hot, the soil will
place of distilled water for oven-dried specimens. If kerosene is used, the typically stick to or dry onto the glass. The duration of vacuum
189
4
D 854 02
and heat must be at least 1 h after the initiation of boiling. soil solids plus tare to the nearest 0.01 g using the designated
During the process, the slurry should be agitated as necessary balance. Calculate and record the mass of dry soil solids to the
to maintain boiling and prevent soil from drying onto the nearest 0.01 g.
pycnometer.
NOTE 6This method has been proven to provide more consistent,
9.6 Filling the Pycnometer with WaterFill the pycnometer repeatable results than determining the dry mass prior to testing. This is
with deaired water (see 8.2.2) by introducing the water through most probably due to the loss of soil solids during the de-airing phase of
a piece of small-diameter flexible tubing with its outlet end testing.
kept just below the surface of the slurry in the pycnometer or
by using the pycnometer filling tube. If the pycnometer filling 10. Calculation
tube is used, fill the tube with water, and close the valve. Place 10.1 Calculate the mass of the pycnometer and water at the
the tube such that the drainage holes are just at the surface of test temperature as follows:
the slurry. Open the valve slightly to allow the water to flow Mpw,t 5 Mp 1 ~Vp rw,t! (2)
over the top of the slurry. As the clear water layer develops,
raise the tube and increase the flow rate. If the added water where:
becomes cloudy, do not add water above the calibration mark Mrw,t = mass of the pycnometer and water at the test
or into the stopper seal area. Add the remaining water the next temperature (Tt), g,
day. Mp = the average calibrated mass of the dry
9.6.1 If using the stoppered iodine flask, fill the flask, such pycnometer, g,
that the base of the stopper will be submerged in water. Then Vp = the average calibrated volume of the pycnometer,
rest the stopper at an angle on the flared neck to prevent air mL, and
entrapment under the stopper. If using a volumetric or stop- rw,t = the density of water at the test temperature (Tt),
pered flask, fill the flask to above or below the calibration mark g/mL from Table 2.
depending on preference. 10.2 Calculate the specific gravity at soil solids the test
9.7 If heat has been used, allow the specimen to cool to temperature, Gt as follows:
approximately room temperature. rs Ms
Gt 5 r 5 (3)
9.8 Thermal EquilibriumPut the pycnometer(s) into the w,t ~Mrw,t 2 ~Mrws,t Ms!!
insulated container. The thermometer, a beaker of water, and
some deaired water in a bottle along with either an eyedropper where:
or pipette should also be placed in the insulated container. rs = the density of the soil solids Mg/m3 or g/cm3,
Keep these items in the closed container overnight to achieve rw,t = the density of water at the test temperature (Tt),
thermal equilibrium. from Table 2, g/mL or g/cm3.
Ms = the mass of the oven dry soil solids (g), and
9.9 Pycnometer Mass DeterminationIf the insulated con- Mrws,t = the mass of pycnometer, water, and soil solids at
tainer is not positioned near a balance, move the insulated the test temperature, (Tt), g.
container near the balance or vice versa. Open the container
10.3 Calculate the specific gravity of soil solids at 20C as
and remove the pycnometer. Only touch the rim of the
follows:
pycnometer because the heat from hands can change the
thermal equilibrium. Place the pycnometer on an insulated G20C 5 K Gt (4)
block (Styrofoam or equivalent). where:
9.9.1 If using a volumetric flask, adjust the water to the K = the temperature coefficient given in Table 2.
calibration mark following the procedure in 8.4.1. 10.4 For soil solids containing particles greater than the
9.9.2 If a stoppered flask is used, place the stopper in the 4.75-mm (No. 4) sieve for which Test Method C 127 was used
bottle while removing the excess water using an eyedropper. to determine the specific gravity of these particles, calculate an
Dry the rim using a paper towel. Be sure the entire exterior of average specific gravity. Test Method C 127 requires the test be
the flask is dry. performed at 23 6 1.7C and does not require the specific
9.10 Measure and record the mass of pycnometer, soil, and gravity data to be corrected to 20C. Use 10.3 to correct this
water to the nearest 0.01 g using the same balance used for measurement to 20C. Use the following equation to calculate
pycnometer calibration. the average specific gravity:
9.11 Pycnometer Temperature DeterminationMeasure 1
and record the temperature of the slurry/soil-water mixture to Gavg@20C 5 R P (5)
the nearest 0.1C using the thermometer and method used 100 G 1@20C 1 100 G2@20C
during calibration in 8.5. This is the test temperature, Tt.
9.12 Mass of Dry SoilDetermine the mass of a tare or pan where:
to the nearest 0.01 g. Transfer the soil slurry to the tare or pan. R = the percent of soil retained on the 4.75-mm
It is imperative that all of the soil be transferred. Water can be sieve,
added. Dry the specimen to a constant mass in an oven P = the percent of soil passing the 4.75-mm sieve,
maintained at 110 6 5C and cool it in a desiccator. If the tare G1@20C = the apparent specific gravity of soils retained
can be sealed so that the soil can not absorb moisture during on the 4.75-mm sieve as determined by Test
cooling, a desiccator is not required. Measure the dry mass of Method C 127, corrected to 20C
190
5
D 854 02
G2@20C = the specific gravity of soil solids passing the TABLE 3 Summary of Test Results from Triplicate Test
Laboratories (Specific Gravity)
4.75-mm sieve as determined by these test
(1) (2) (3) (4) (5)
methods (Equation 4). Number of Acceptable
Triplicate Test Average Standard Range of Two
11. Report: Test Data Sheets(s)/Form(s) Soil Type Labs ValueA DeviationB ResultsC
11.1 The method used to specify how data are recorded on Single-Operator Results (Within- Laboratory Repeatability):
the test data sheets or forms, as given below, is the industry CH 14 2.717 0.009 0.03
CL 13 2.670 0.006 0.02
standard, and are representative of the significant digits that ML 14 2.725 0.006 0.02
should be retained. These requirements do not consider in situ SP 14 2.658 0.006 0.02
material variation, use of the data, special purpose studies, or Multilaboratory Results (Between- Laboratory Reproducibility):
CH 14 2.717 0.028 0.08
any considerations for the users objectives. It is common CL 13 2.670 0.022 0.06
practice to increase or reduce significant digits of reported data ML 14 2.725 0.022 0.06
commensurate with these considerations. It is beyond the scope SP 14 2.658 0.008 0.02
A
of the standard to consider significant digits used in analysis The number of significant digits and decimal places presented are represen-
tative of the input data. In accordance with Practice D 6026, the standard deviation
methods for engineering design. and acceptable range of results cannot have more decimal places than the input
11.2 Record as a minimum the following information (data): data.
B
11.2.1 Identification of the soil (material) being tested, such Standard deviation is calculated in accordance with Practice E 691 and is
referred to as the 1s limit.
as boring number, sample number, depth, and test number. C
Acceptable range of two results is referred to as the d2s limit. It is calculated as
11.2.2 Visual classification of the soil being tested (group 1.960=2 1s, as defined by Practice E 177. The difference between two properly
name and symbol in accordance with Practice D 2487). conducted tests should not exceed this limit. The number of significant digits/
decimal places presented is equal to that prescribed by these test methods or
11.2.3 Percent of soil particles passing the No. 4 (4.75-mm) Practice D 6026. In addition, the value presented can have the same number of
sieve. decimal places as the standard deviation, even if that result has more significant
digits than the standard deviation.
11.2.4 If any soil or material was excluded from the test
specimen, describe the excluded material.
11.2.5 Method used (Method A or Method B). TABLE 4 Summary of Single Test Result from Each Laboratory
(Specific Gravity)A
11.2.6 All mass measurements (to the nearest 0.01 g).
(1) (2) (3) (4) (5)
11.2.7 Test temperature (to the nearest 0.1C). Acceptable
11.2.8 Specific gravity at 20C (G, Gs, G20C) to the nearest Number of Test Average Standard Range of Two
0.01. If desired, values to the nearest 0.001 may be recorded. Soil Type Laboratories Value Deviation Results
11.2.9 Average specific gravity at 20C (Gave or Gavg@20C) Multilaboratory Results (Single-Test Performed by Each Laboratory):
to the nearest 0.01, if applicable. CH 18 2.715 0.027 0.08
CL 18 2.673 0.018 0.05
ML 18 2.726 0.022 0.06
12. Precision and Bias SP 18 2.660 0.007 0.02
12.1 PrecisionCriteria for judging the acceptability of test A
See footnotes in Table 3.
results obtained by these test methods on a range of soil types
using Method A (except the soil was air dried) is given in the single-operator d2s limits shown in Table 3, Column 5. For
Tables 3 and 4. These estimates of precision are based on the definition of d2s see Footnote C in Table 3. Results of two
results of the interlaboratory program conducted by the ASTM properly conducted tests performed by different operators and
Reference Soils and Testing Program.7 In this program, some on different days should not differ by more than the multilabo-
laboratories performed three replicate tests per soil type ratory d2s limits shown in Table 3, Column 5.
(triplicate test laboratory), while other laboratories performed a 12.1.2 In the ASTM Reference Soils and Testing Program,
single test per soil type (single test laboratory). A description of many of the laboratories performed only a single test. This is
the soils tested is given in 12.1.4. The precision estimates may common practice in the design and construction industry. The
vary with soil type and method used (Method A or B). data in Table 4 are based upon the first test result from the
Judgement is required when applying these estimates to triplicate test laboratories and the single test results from the
another soil or method. other laboratories. Results of two properly conducted tests
12.1.1 The data in Table 3 are based on three replicate tests performed by two different laboratories with different operators
performed by each triplicate test laboratory on each soil type. using different equipment and on different days should not vary
The single operator and multilaboratory standard deviation by more than the d2s limits shown in Table 4, Column 5. The
shown in Table 3, Column 4 were obtained in accordance with results in Tables 3 and 4 are dissimilar because the data sets are
Practice E 691, which recommends each testing laboratory different.
perform a minimum of three replicate tests. Results of two 12.1.3 Table 3 presents a rigorous interpretation of triplicate
properly conducted tests performed by the same operator on test data in accordance with Practice E 691 from prequalified
the same material, using the same equipment, and in the laboratories. Table 4 is derived from test data that represents
shortest practical period of time should not differ by more than common practice.
12.1.4 Soil TypeBased on the multilaboratory test results,
the soil used in the program is described below in accordance
7
Supporting data is available from ASTM Headquarters. Request RR: D18- with Practice D 2487. In addition, the local name of the soil is
1009. given.
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D 854 02
CHFat clay, CH, 99 % fines, LL=60, PI=39, grayish brown, soil had been SPPoorly graded sand; SP, 20 % coarse sand, 48 % medium sand, 30 %
air dried and pulverized. Local nameVicksburg Buckshot Clay fine sand, 2 % fines, yellowish brown. Local nameFrederick sand
CLLean clay, CL, 89 % fines, LL=33, PI=13, gray, soil had been air dried
and pulverized. Local nameAnnapolis Clay 12.2 BiasThere is no acceptable reference value for this
MLSilt, ML, 99 % fines, LL=27, PI=4, light brown, soil had been air dried
and pulverized. Local nameVicksburg Silt
test method, therefore, bias cannot be determined.
SUMMARY OF CHANGES
In accordance with Committee D18 policy, this section identifies the location of changes to this standard since
the last edition (00e1) that may impact the use of this standard.
(1) The balance capacity was reduced from 2000 g to either the beaker during thermal equilibrium.
500 g or 1000 g depending on pycnometer size. (3) 9.2 The dispersion technique is better defined.
(2) 8.3 and 9.8. The thermometer no longer is required to be in
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.
This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org).
192
7
Designation: C 170 90 (Reapproved 1999)
This standard has been approved for use by agencies of the Department of Defense.
1. Scope 6. Sampling
1.1 This test method covers the sampling, preparation of 6.1 The sample shall be selected to represent a true average
specimens, and determination of the compressive strength of of the type or grade of stone under consideration and shall be
dimension stone. of the quality supplied to the market in finished form under the
1.2 This standard does not purport to address all of the type designation to be tested. The sample may be selected by
safety concerns, if any, associated with its use. It is the the purchaser or his authorized representative from quarried
responsibility of the user of this standard to establish appro- stone or taken from the natural ledge and shall be of adequate
priate safety and health practices and determine the applica- size to permit the preparation of the desired number of test
bility of regulatory limitations prior to use. specimens. When perceptible variations occur, the purchaser
may select as many samples as are necessary for determining
2. Referenced Documents the variation in compressive strength.
2.1 ASTM Standards:
C 119 Terminology Relating to Dimension Stone2 7. Test Specimens
E 4 Practices for Force Verification of Testing Machines3 7.1 The test specimens may be cubes, square prisms, or
cylinders and shall be cut from the sample with saws or core
3. Terminology drills. The diameter or lateral dimension (distance between
3.1 DefinitionsAll definitions are in accordance with Ter- opposite vertical faces) shall be not less than 2 in. (50.8 mm)
minology C 119. (Explanatory Note 1), and the ratio of height (Explanatory
Note 2) to diameter or lateral dimension should be not less than
4. Significance and Use 1:1. At least five specimens shall be prepared for each
4.1 This test method is useful in indicating the differences in condition of the test; that is, when the compressive strength is
compressive strength between the various dimension stones. desired for the wet and dry conditions but in only one direction,
This test method also provides one element in comparing such as perpendicular to the bed (or rift) (see Fig. 1( a)), ten
stones of the same type. specimens will be required. For wet and dry strength tests both
perpendicular and parallel to the bed (or rift) (see Fig. 1(a) and
5. Apparatus (b)), twenty specimens are required (Explanatory Note 3). The
5.1 Any testing machine conforming to Practices E 4 and to load-bearing faces shall be finished by grinding to as nearly
the speed of testing requirements prescribed in Section 9 of this true and parallel planes (Explanatory Note 4) as practicable.
test method may be used. 7.2 The load-bearing surfaces and the direction of bedding
5.2 In vertical testing machines, the spherical bearing block (or rift) shall be marked on each specimen after finishing.
shall be suspended from the upper head of the machine in such 7.3 The load-bearing areas of the specimen shall be calcu-
a manner that the contact plate remains in a central position lated from measurements taken midway between the load-
(spherical surfaces in full contact) when not loaded. The bearing surfaces. The dimensions of the specimens shall be
spherical surfaces shall be well lubricated, and the center of measured to the nearest 0.02 in. (0.5 mm) and the load-bearing
curvature shall lie in the surface of contact with the specimen. areas calculated to the nearest 0.04 in. 2 (0.26 cm2).
8. Conditioning
1
This test method is under the jurisdiction of ASTM Committee C-18 on 8.1 Before testing the specimens in a dry condition, dry
Dimension Stone and is the direct responsibility of Subcommittee C18.01 on Test
Methods. them for 48 h at 60 6 2C (140 6 4F). At the 46th, 47th, and
Current edition approved Sept. 28, 1990. Published November 1990. Originally 48th h, weigh the specimens to ensure that the weight is the
published as C 170 41 T. Last previous edition C 170 87e1. same. If the weight continues to drop, continue to dry the
2
Annual Book of ASTM Standards, Vol 04.07.
3 specimens until there are 3 successive hourly readings with the
Annual Book of ASTM Standards, Vol 03.01.
Copyright ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
193
1
C 170
NOTE 1Dashed lines indicate direction of bedding or rift. Arrows indicate direction of loading.
(a) Loading Perpendicular to Bedding or Rift (b) Loading Parallel to Bedding or Rift
FIG. 1 Methods of Applying Load with Reference to Bedding or Rift
same weight. After removing the specimens from the oven, rift) as shown in Fig. 1(a) in a dry condition as the compressive
cool them to room temperature in a desiccator before testing strength perpendicular to the rift in a dry condition. Similarly
them. report the values perpendicular/wet, parallel/dry as shown in
8.2 Before testing the specimens in a wet condition, im- Fig. 1(b) and parallel/wet. All determinations shall be reported
merse them in water for 48 h at 22 6 2C (72 6 4F). Test as information.
them immediately upon removal from the bath, wiping the 11.2 The following additional information shall be reported:
specimens free of surface water. 11.2.1 Identification of the sample, including name and
location of the quarry, name or position of the ledge, date when
9. Procedure sample was taken and trade name or grade of stone,
9.1 Center the specimens in the testing machine and apply 11.2.2 Size and shape of specimens used in the tests, and
the initial load at a rate that will permit hand adjustment of the 11.2.3 A description of the way in which the specimens
contact plate on the specimen. Rotate the plate back and forth were prepared.
through an angle of about 30 under a small load to properly
seat the spherical block, but take care not to move the specimen 12. Precision and Bias
out of the central position. Preferably, the rate of loading 12.1 Individual variations in a natural product may result in
should not exceed 100 psi (690 kPa)/s, but this requirement deviation from accepted values. A precision section will be
may be considered as being met if the speed of the loading added when sufficient data are available to indicate acceptable
head is not more than 0.05 in. (1.3 mm)/min. tolerances in repeatability and reproducibility.
10. Calculation
EXPLANATORY NOTES
10.1 Calculate the compressive strength of each specimen
as follows: NOTE 1For very coarse-grain materials like some of the granites, the
diameter of the specimen should not be less than 2.5 in. (63.5 mm).
C 5 W/A (1) NOTE 2The height of the specimen is considered as the distance
between the load-bearing faces.
where: NOTE 3In some materials, such as granite, three directions with
C 5 compressive strength of the specimen, psi (MPa) respect to fissility are recognized, as follows: rift (the plane of easiest
W 5 total load, lbf (N), on the specimen at failure, and splitting), grain (the plane of next easiest splitting), and head-grain
A 5 calculated area of the bearing surface in in.2 (mm2). (the plane of hardest splitting). Occasionally, tests are required for
Round each individual result to the nearest 100 psi (1 MPa). determining the strength perpendicular to each of these directions. In such
10.2 When the ratio of height to diameter (or lateral cases, the sample shall be marked at the quarry to show which faces are
dimension) differs from unity by 25 % or more, calculate the grain, rift, and head-grain, and the required number of specimens shall be
prepared with load-bearing faces parallel to each of these planes and
result to that of the corresponding cube, as follows: properly labeled for the various tests.
Cc 5 Cp/@0.778 1 0.222~b4 h!# (2) NOTE 4Accuracy of test results depends largely on uniform distribu-
tion of the load over the bearing faces. In order to grind the surfaces to
where: reasonably true planes, considerable care is necessary. The following
Cc 5 compressive strength of an equivalent cubical speci- procedure is suggested: Assuming that the specimen is a rectangular prism
men, and the load is to be applied to the ends, mark two adjacent sides for
Cp 5 compressive strength of the specimen having a height reference, then grind the ends on a grinding wheel or lap until they are
greater than the diameter or lateral dimension, perpendicular to these reference sides as gaged by a try square. Complete
the grinding by rubbing the ends on a smooth machine-planed surface of
b 5 diameter or lateral dimension, and
a cast iron plate with No. 80 emery and water. The specimen should be
h 5 height. grasped as near the surface of the plate as possible to prevent rocking of
11. Report the specimen. A suitable way to determine when the surfaces are
reasonably plane is to dip the specimen in water and press the ends on a
11.1 Report the average of all values of compressive smooth machine-planed and polished surface of a 10-lb (4.5-kg) weight.
strength of specimens loaded perpendicular to the bedding (or If the weight can be lifted by raising the specimen, the surfaces may be
194
2
C 170
considered to be sufficiently accurate. A satisfactory mechanical means of metal between the specimen and one chuck point. This causes the
finishing the bearing surfaces of the specimens is to place them in a chuck specimen to be placed somewhat off-center but does not interfere with the
in a lathe and surface the ends with a tool post grinder. This grinder surfacing process. The surface can be tested for planeness by holding a
consists of a small motor and arbor carrying an abrasive wheel which turns straightedge on the surface and viewing it before a strong light. Specimens
at about 5000 rpm. A three-point chuck is used to permit the surfacing of finished in this way commonly give considerably higher test results than
cylindrical, square prism, or cubical specimens. When the square-type specimens prepared by hand.
specimen is used it will be necessary to place a small piece of notched
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your
views known to the ASTM Committee on Standards, at the address shown below.
This standard is copyrighted by ASTM, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above address or at
610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website (www.astm.org).
195
3