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CURSO DE CALIFICACION
NIVEL I Y II
LIQUIDOS PENETRANTES
2013
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INDICE
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LECCION 1
CALIFICACION
DE
PERSONAL EN NDE
CALIFICACION
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CALIFICACION
CALIFICACION
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CALIFICACION
CALIFICACION
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CALIFICACION
CALIFICACION
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CALIFICACION
El SNT-TC- 1 A describe:
- Los requisitos de conocimiento
- Las capacidades
Para estar calificado en cada uno de los
niveles establecidos.
9
NIVELES DE CALIFICACION
10
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APRENDICES
11
NIVEL I
12
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NIVEL II
NIVEL II
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NIVEL III
NIVEL III
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NIVEL III
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CALIFICACION
VERSUS
CERTIFICACION
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PROCESO DE CALIFICACION
PROCESO DE CALIFICACION
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PROCESO DE CALIFICACION
CERTIFICACION
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CERTIFICACION
CERTIFICACION
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CERTIFICACION
PORQUE ES IMPORTANTE
QUE YO ESTE CERTIFICADO?
25
CERTIFICACION
26
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RETOS
RETOS
28
PAGINA16 DE 200
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LECCION 2
INTRODUCCION A LOS LIQUIDOS PENETRANTES (PT)
Historia
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HISTORIA
HISTORIA
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HISTORIA
HISTORIA
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HISTORIA
HISTORIA
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INTRODUCCION
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PROPOSITO DE LOS PT
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PROPOSITO DE LOS PT
Los líquidos penetrantes permiten
detectar discontinuidades abiertas a la
superficie en materiales que no sean
porosos.
Es un método de NDE muy barato teniendo
en cuenta el poco entrenamiento
requerido por el personal, los materiales,
y la facilidad para aplicar el NDE.
PROPOSITO DE LOS PT
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PROPOSITO DE LOS PT
PROPOSITO DE LOS PT
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PROPOSITO DE LOS PT
PROPOSITO DE LOS PT
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PROPOSITO DE LOS PT
PRINCIPIOS BASICOS
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PRIMER PASO
SEGUNDO PASO
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TERCER PASO
CUARTO PASO
Aplicación del revelador. El revelador
ayuda a extraer cualquier liquido penetrante
atrapado en las discontinuidades, para luego
dispersarlo sobre la superficie, mejorando la
visibilidad de las indicaciones.
El revelador también provee un fondo de
contraste en la superficie de la parte,
especialmente en los no fluorescentes
PAGINA28 DE 200
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QUINTO PASO
SEXTO PASO
PAGINA29 DE 200
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PORQUE UTILIZAR PT
PORQUE UTILIZAR PT
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PORQUE UTILIZAR PT
PORQUE UTILIZAR PT
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TIPOS DE PENETRANTES
TIPOS DE PENETRANTES
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TIPOS DE PENETRANTE
METODO DE REMOCION
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SENSITIVIDAD (FLUORESCENTES)
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CLASES DE SOLVENTES
PRECAUCIONES DE SEGURIDAD
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PRECAUCIONES DE SEGURIDAD
FUEGO
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IRRITACION DE LA PIEL
POLUCION
Los polvos y vapores de los materiales de
líquidos penetrantes no son tóxicos pero
inhalarlos en exceso pueden ser un peligro
para la salud. En las áreas confinadas deberá
colocarse un ventilador de extracción. Otros
ventiladores pueden ser necesarios para
remover los vapores.
PAGINA37 DE 200
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RADIACION ULTRAVIOLETA
PAGINA38 DE 200
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LECCION 3
PROCESADO DE LOS LIQUIDOS PENETRANTES
PROCEDIMIENTOS Y TECNICAS
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PAGINA42 DE 200
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PRELIMPIEZA
PRELIMPIEZA
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METODOS DE LIMPIEZA
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LIMPIEZA ULTRASONICA
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REMOVEDORES DE PINTURA
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ATACADO
ATACADO
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PAGINA50 DE 200
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SECADO
SECADO
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SECADO
TIEMPO DE PERMANENCIA
(DWELL TIME)
• PENETRANTE
El tiempo de permanencia del penetrante, es la longitud de
tiempo en la cual este humedece la superficie y se introduce en
las discontinuidades
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TIEMPO DE PERMANENCIA
(DWELL TIME)
• REVELADOR
El tiempo de permanencia del revelador es la longitud de
tiempo, en la cual el penetrante empapa el revelador antes que
la indicación sea evaluada.
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PAGINA55 DE 200
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ILUMINACION ADECUADA
100 lx de luz blanca es la iluminación adecuada en la
estación de enjuague para los líquidos penetrantes
fluorescentes, y debe ser mayor de 100 mW/cm2 de
radiación ultravioleta, para poder monitorear la
remoción del exceso de penetrante fluorescente, y
poder limitar un enjuague excesivo o deficiente. Si se
desea la estación del enjuague puede tener una
radiación UVA de 1000 mW/cm2 y menos de 20 Lux de luz
blanca
ILUMINACION ADECUADA
PAGINA56 DE 200
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LUXOMETRO
Este es un medidor
típico que permite
evaluar la iluminación
visible o la luz negra
requerida para el
examen con líquidos
fluorescentes
ILUMINACION ADECUADA
PAGINA57 DE 200
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Lámpara de luz
negra para los
líquidos
penetrantes
fluorescentes
OTROS MODELOS
DE FUENTE DE
RADIACION UVA
Estos son otros
modelos modernos de
lámparas de luz negra
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PAGINA59 DE 200
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ESTACION DE ENJUAGUE
PAGINA60 DE 200
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PAGINA61 DE 200
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APLICACION DEL
REVELADOR Y SECADO
APLICACION DEL
REVELADOR Y SECADO
PAGINA62 DE 200
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1. Suspendidos en el aire.
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SUSPENDIDOS EN AGUA
(FORMA C)
1. Son suministrados como un concentrado seco que
tiene que mezclarse y conservarse en la relación
apropiada de revelador y agua.
2. Los reveladores acuosos suspendidos no se
disuelven en el agua, luego es necesario agitarlos
antes de su aplicación para que las partículas estén
suspendidas.
SUSPENDIDOS EN AGUA
(FORMA C)
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SUSPENDIDOS EN AGUA
(FORMA C)
SUSPENDIDOS EN AGUA
(FORMA C)
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DEFINICIONES
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Conjunto de
liquidos
penetrantes
visibles y
fluorescentes
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TIEMPO DE REVELADO
TIEMPO DE REVELADO
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TIEMPO DE REVELADO
INTERPRETACION Y EVALUACION
DEFINICIONES
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TIPOS DE INDICACIONES
Las indicaciones se forman en la superficie de los
objetos examinados simplemente porque son
discontinuidades abiertas a la superficie, y ellas
pueden categorizarse como sigue:
1. Indicaciones falsas.
2. Indicaciones no relevantes.
3. Indicaciones relevantes
TIPOS DE INDICACIONES
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DISCONTINUIDADES
INDICACIONES FALSAS
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INDICACIONES FALSAS
INDICACIONES FALSAS
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INDICACIONES FALSAS
INDICACIONES FALSAS
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INDICACIONES NO RELEVANTES
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INDICACIONES NO RELEVANTES
2. Conexiones remachadas.
INDICACIONES RELEVANTES
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INDICACIONES RELEVANTES
a. Grietas.
b. Costuras (Seams).
c. Rechupes (Cold shuts).
d. Traslapos forjados (Forging
laps).
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INDICACIONES REDONDEADAS
O PUNTUALES
INDICACIONES REDONDEADAS
O PUNTUALES
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POST-LIMPIEZA
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EQUIPOS PARA EL
EXAMEN
LECCION 4
UNIDADES EXAMINADORAS
1. Las unidades examinadoras de líquidos penetrantes
pueden ser diseñadas de tal manera que los objetos a
examinar se puedan mover de la siguiente manera:
a. Manualmente
b. Mecánicamente asistida.
c. Semiautomático.
d. Completamente automático.
PAGINA83 DE 200
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UNIDADES EXAMINADORAS
2. Laescogencia depende del presupuesto, tiempo, y
desempeño del sistema a largo plazo
3. El tamaño de la unidad examinadora es fuertemente
dependiente del tamaño y tipo de objeto a examinar. La
configuración del sistema puede tomar varios diseños
dependiendo de las facilidades disponibles, velocidad de
producción deseada, y la manipulación fácil de los objetos
a examinar.
UNIDADES EXAMINADORAS
Los requisitos para las dependen de los
siguientes factores:
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EQUIPOS AUXILIARES
1. Se requieren equipos auxiliares localizados en las estaciones
de examen con penetrantes (diferente a las estaciones de
limpieza) para poder realizar el examen con líquidos penetrantes
2. Los equipos auxiliares pueden construirse en una o mas
estaciones de examen.
EQUIPOS AUXILIARES
Lámpara
Estación de ultravioleta
secado
Lámpara
Estación
ultravioleta
de drenado
Estación de
emulsificado Estación de
Estación examen
de Estación de
penetración revelado
Estación de
enjuague
Panel de
control
PAGINA85 DE 200
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Estacion
Secadoor
de
Lampara Estacion Estacion de examen
ultravioleta de reposoi
revelado
Estacion de
enjuague
Rociador
Estacion de
drenaje
Estacion
de
penetracion
Estacion Estacion
de Secador de
Estacion de revelado Luz examen
enjuague blanca
Lamparas
Estacion de ultravioleta
Estacion drenaje
de
penetracion
Manguera alimentacion
Manguera agua
Manguera Lampara
alimentacion ultravioleta
PAGINA86 DE 200
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UNIDADES MODULARES
Las estaciones son suministradas en unidades
modulares para permitir muchas configuraciones
tales como en linea recta en L , o en U.
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ESTACION DE LAVADO
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HORNO DE SECADO
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SISTEMA DE COMPONENTES
MULTIPLES EN LINEA
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SISTEMA DE COMPONENTES
MULTIPLES EN LINEA
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ESTACION DE BOMBAS
Varias bombas se instalan en las estaciones del
penetrante, emulsificador, enjuague y revelador como
se necesite para los siguientes procedimientos::
1. Agitación de las soluciones.
2. Bombear hacia afuera el material dentro de los
tanques adecuados para la re-utilizacion o
filtración para desecho.
ESTACION DE BOMBAS
3. El uso de mangueras a presión y aplicadores.
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ROCIADORES Y APLICADORES
1. Los rociadores y aplicadores se usan frecuentemente en las
estaciones de penetración, emulsificacion, enjuague, y revelado.
2. Estos reducen el tiempo de examinación pues permiten la
aplicación rápida y homogénea de los materiales para los
líquidos penetrantes.
ROCIADORES Y APLICADORES
3. Los rociadores convencionales y los electrostáticos son
utilizados para los penetrantes secos y los reveladores
suspendidos.
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TERMOSTATOS Y TERMOMETROS
Los termostatos y termometros se utilizan
para monitorear y controlar las temperaturas
de lo siguiente:
1. Materiales penetrantes.
2. Hornos de secado.
4. Atmosfera.
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REFRACTOMETRO
Se utiliza para medir
la concentración del
emulsificador
hidrofilico en el agua.
HIDROMETRO
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HIDROMETRO
Balasto Tallo
Escala
Cuerpo
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LUXOMETROS
1. Los sensores de luz blanca miden en pies-candela o lux.
MATERIALES PARA
LIQUIDOS PENETRANTES
Los materiales utilizados en el examen con líquidos
penetrantes incluyen:
1. Penetrantes.
2. Emulsificadores.
3. Removedores.
4. Limpiadores.
5. Reveladores.
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PRELIMPIEZA Y POSTLIMPIEZA
PENETRANTES LAVABLES
CON AGUA
1. Son líquidos aceitosos altamente penetrantes que contienen un
agente emulsificante que hace el medio aceitoso lavable con
agua.
2. Son muy simples de usar, son penetrantes visibles o por
contraste de colores, y no se requiere iluminación fluorescentes
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PENETRANTES LAVABLES
CON AGUA
3. Se obtiene una mayor visibilidad si se utilizan penetrantes
fluorescentes y son observados bajo radiación ultravioleta.
PENETRANTES POSTEMULSIFICABLES
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EMULSIFICADORES
1. Cuando se aplican los emulsificadores a un
penetrante post-emulsificado, estos se combinan
con el penetrante para que la mezcla resultante
sea lavable con agua.
2. El emulsificador, usualmente tiene un color
naranja para que tenga contraste con el
penetrante, puede ser lipofilico (en base aceite)
o hidrofilico (detergente con base agua).
EMULSIFICADORES
Tanque de inmersion
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EMULSIFICADORES
LIPOFILICOS
1. Ellos comienzan la emulsificacion en contacto con el penetrante.
2. Los emulsificadores nunca deben aplicarse con brocha.
3. La mezcla del penetrante y el emulsificador puede removerse
con un enjuague de agua estandar.
4. Este hace que el penetrante sea lavable con agua.
EMULSIFICADORES
HIDROFILICOS
1. Funcionan por el desplazamiento del exceso de penetrante
de la superficie a través de una acción detergente.
2. La fuerza del chorro de agua o la agitación con aire /
mecánica en un tanque suministra la acción de frotado
mientras el detergente desplaza la película de penetrante.
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EMULSIFICADORES
HIDROFILICOS
3. El tiempo de emulsificacion variara dependiendo de
su concentración la cual puede ser monitoreada
utilizando el refractometro.
4. Los emulsificadores (removedores) hidrofilicos
pueden también utilizarse como emulsificadores de
contacto.
EMULSIFICADORES
HIDROFILICOS
5. Estos penetrantes tienen la ventaja de eliminar en parte el
peligro del sobre enjuague.
6. Requieren agitación para permitir que el emulsificador fresco
entre en contacto con el penetrante en la superficie.
7. Hacen el penetrante lavable con agua.
PAGINA115 DE 200
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REVELADORES
1. El revelado de las indicaciones de penetrante es el
proceso de extraer el penetrante de las
discontinuidades abiertas a la superficie por medio
de la acción secante del revelador aplicado.
2. Estos incrementan la visibilidad de las indicaciones
bajo una luz visible o fluorescente adecuada.
PAGINA116 DE 200
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REVELADOR SECO
1. Polvo suave el cual es aplicado a las superficies a
examinar secas.
2. La mayoría se adaptan a superficies rugosas y el
procesado automático.
3. Fáciles de remover.
REVELADOR SECO
4. Un gran cuidado debe tomarse para no contaminar el
revelador con penetrante fluorescente.
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REVELADOR HUMEDO
NO ACUOSO
1. Son partículas de revelador suspendidas en un
solvente de secado rápido
2. Son usados con el proceso de remoción con
solvente.
3. Se aplican solo sobre las superficies secas.
4. Este tipo de revelador debe aplicarse por
rociado únicamente.
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PRECAUCIONES
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LECCION 5
SELECCION DEL METODO DE
EXAMEN
INTRODUCCION
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INTRODUCCION
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VENTAJAS
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DESVENTAJAS
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PT COMO METODO
COMPLEMENTARIO
1. El método de los penetrantes puede usarse
como un método preliminar para detectar
las discontinuidades superficiales.
2.El método de los penetrantes es efectivo
como un medio de verificar las indicaciones
superficiales detectadas con los otros
métodos.
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4.Tipo de discontinuidades.
5.Condiciona superficial de los objetos a
examinar.
6.Uso final de los objetos a examinar.
7.Selección del revelador.
8.Criterio de aceptación y rechazo.
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PORTABILIDAD
PORTABILIDAD
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Postemulsification
POSTEMULSIFICABLES
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POSTEMULSIFICADO
REVELADOR
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REVELADOR SECO
REVELADOR SECO
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REVELADOR SECO
REVELADORES HUMEDOS
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REVELADORES HUMEDOS
Wet Developers
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REVELADORES HUMEDOS
6. El
revelador suspendido en agua requiere la
agitación, y ambos tipos requieren
chequeos de mantenimiento diario cuando
se utilicen tanques.
7. Cuando un revelador húmedo no acuoso
se utilice, el objeto a examinar tiene que
estar completamente seco antes de
aplicar el revelador.
REVELADORES HUMEDOS
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REVELADORES HUMEDOS
REVELADORES ESPECIALES
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INTERPRETACION Y EVALUACION
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1. Tipos de material.
2. Circunstancias de exposición.
3. Tipo de equipo.
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GRIETA GRIETA
GRANDE FINA
TRASLAPO POROS
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2. La temperatura.
3. El tiempo de permanencia
4. La aplicación del revelador.
5. Condiciones de examen.
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7. La temperatura.
a. La viscosidad de la mayoría de los
líquidos se incrementa a bajas
temperaturas
b. La volatilidad de los componentes puede
ocasionar que se evaporen si están muy
calientes
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a. Grietas.
b. Rechupes.
d. Costuras.
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5. Indicaciones difusas.
a. porosidad esparcida.
b. revelado excesivo.
c. Vacíos o contracciones que salen a la superficie.
d. grietas anchas.
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4. Contaminantes.
a. Las manos del examinador untadas de penetrante.
b. Contaminación del revelador húmedo o seco.
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LECCION 7
CONTROL DE PROCESO
INTRODUCION
1. La confiabilidad de cualquier examen con líquidos penetrantes es
determinado en gran parte por la condición del material utilizado.
2. Los chequeos en servicio son efectuados con materiales almacenados
en los tanques abiertos y sujetos a contaminación o evaporación.
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6. Punto de inflamación.
7. Toxicidad.
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MUESTREO DE CONTROL
1. Los muestreos de control se toman al momento de la
recepción de los materiales provenientes del
suministrador, incluyendo los reveladores.
2. Las muestras son conservadas en contenedores sellados y
almacenados donde no se deterioren por el calor, la luz o la
evaporación.
3. Las muestras deberían ser suficientes para la vida de los
materiales.
BLOQUES DE REFERENCIA
1. Los bloques, laminas, paneles de referencia son especificados por
los procedimientos para el control de calidad de los materiales para
los líquidos penetrantes.
2. Estos estándares son comúnmente llamados especímenes de prueba
con defectos conocidos (KDTS).
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BLOQUES DE REFERENCIA
3. Los materiales utilizados en la fabricación de los bloques de
referencia incluyen aluminio, acero, níquel, vidrio, y
cerámicas.
4. Algunos de los bloques son diseñados principalmente para las
siguientes funciones:
BLOQUES DE REFERENCIA
a. Verificar la sensitividad del sistema de líquidos penetrantes.
b. Realizar pruebas de comparación
c. Verificar la lavabilidad del penetrante o el emulsificador.
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PANELES DE PRUEBA
1. Son paneles de níquel cromo plateados y agrietados.
2. El panel sirve para monitorear los sistemas de líquidos penetrantes
(PSM).
3. Puede ser un bloque de aluminio agrietado por el templado.
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BLOQUES DE REFERENCIA DE
ALUMINIO
1. Los bloques de referencia de miden cerca de 5 por 7.5 cm. , y se
cortan a partir de una placa de 8 mm de espesor de material
aluminio 2024 – T3
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BLOQUES DE REFERENCIA DE
ALUMINIO
2. Los bloques son calentados y enfriados en agua para producir
grietas térmicas. Esto se logra soportando el bloque en un marco y
calentando este no uniformemente con una llama en el centro y por
la parte inferior del bloque.
BLOQUES DE REFERENCIA DE
ALUMINIO
3. Se corta una ranura de 1.5 mm X 1.5 mm de profundidad en la
dirección de 5 cm a través del centro de la zona afectada .
4. Lo anterior forma dos áreas de prueba y permite la aplicación en
cada lado y comparar los dos penetrantes sin contaminación.
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BLOQUES DE REFERENCIA DE
ALUMINIO
5. Este tipo de bloque es ampliamente utilizado para comparar el
desempeño de los penetrantes en condiciones de campo.
BLOQUES DE REFERENCIA DE
ALUMINIO
6. El bloque se calienta lentamente hasta 425°C , la temperatura se debe
medir con una crayola o termómetro y luego se enfría en agua.
Luego se calienta a 70°C por 30 minutos para permitir que toda la
humedad salga de las grietas y posteriormente se enfría a temperatura
ambiente.
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BLOQUES DE REFERENCIA DE
ALUMINIO
7. Después que un bloque de referencia ha sido utilizado, este debe
limpiarse antes de reutilizar.
BLOQUES DE REFERENCIA DE
ALUMINIO
Bloque de aluminio de
referencia típico en 2024 –
T3 después de calentarlo y
templarlo y realizarle el
corte de la ranura, note la
ZAC en el centro.
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4. Lavabilidad
5. Decoloración de las tintas penetrantes ( chequeado
por una prueba de comparación sencilla).
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PRUEBAS EN LOS
REVELADORES SECOS
1. Los reveladores secos usan contenedores abiertos o cámaras y son
probados normalmente mediante la observación.
2. Los reveladores secos no son higroscópicos ellos no absorben la
humedad del aire y son relativamente libres de problemas, mientras
ellos no entren en contacto con el agua.
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PRUEBAS EN LOS
REVELADORES SECOS
3. Cualquier revelador seco que se encuentre grumoso o apelmazado
en vez de ligero y suave , o que muestre otros signos de haberse
humedecido se descarta.
PRUEBAS EN LOS
REVELADORES SECOS
4. El revelador seco se chequea diariamente para lo siguiente:
a. Agrietamiento.
b. Suciedad.
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HIDROMETRO TIPICO
Balasto Tallo
Escala
Cuerpo
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LECCION 8
ARTICULO 6 SECCION V
INFORMACION GENERAL
(T-620)
Los líquidos penetrantes son un método efectivo
para detectar discontinuidades que estén
abiertas a la superficie de metales no porosos
Las discontinuidades típicamente detectadas
son : grietas, costuras, traslapos, rechupes,
laminaciones, y porosidad
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PROCEDIMIENTO
(T-621)
Se requiere de un procedimiento escrito que
incluya todas las variables indicadas en la Tabla
T-621
Si el código de construcción así lo especifica el
procedimiento debe ser calificado.
Si se cambia una variable esencial el
procedimiento debe recalificarse
CONTROL DE CONTAMINANTES
(T-641)
Se deben obtener certificaciones de los
materiales para líquidos penetrantes si se
van a examinar aceros inoxidables
austeniticos o dúplex, aleaciones de
níquel, o titanio
Las certificaciones deben incluir el
numero de lote
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T-651 TÉCNICAS
LAVABLES
VISIBLE
CON AGUA
POST-
EMULSIFICABLES
FLUORESCENTES
REMOVIBLES CON
SOLVENTE
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T-653 TÉCNICAS NO
ESTANDAR
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T-660 CALIBRACIÓN
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T-675 REVELADO
El método de aplicación del revelador es variable esencial
elrevelador seco se puede aplicar con brocha, o soplado
del polvo.
elrevelador húmedo si es acuoso se puede aplicar por
inmersión, spray, o brocha, para el secado no exceder de
125°f en la parte
elrevelador húmedo no acuoso se debe aplicar con
brocha, spray, o inmersión pero la parte debe estar seca
antes del revelado
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T-676 - ILUMINACIÓN
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T-676 - ILUMINACIÓN
T-676- INTERPRETACIÓN
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T-680 EVALUACIÓN
CRITERIO DE ACEPTACION
SECCION I, VIII DIV. 1/2
Indicaciones relevantes > 1/16” (1.5 mm)
No se acepta ninguna indicación lineal relevante
No se aceptan indicaciones redondeadas > 3/16” (5 mm)
No se aceptan cuatro o mas indicaciones relevantes
redondeadas alineadas separadas 1/16” (1.5 mm) o menos
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CRITERIO DE ACEPTACION
ASME B-31.1
Indicaciones relevantes > 1/16” (1.5 mm)
No se acepta ninguna indicación lineal relevante o grieta
No se aceptan indicaciones redondeadas > 3/16” (5 mm)
No se aceptan cuatro o mas indicaciones relevantes
redondeadas alineadas separadas 1/16” (1.5 mm) o menos
Diez o mas indicaciones redondeadas en 6 pulgadas
cuadradas, (3870 mm2), si la dimensión mayor del área no
excede 6 pulgadas (150 mm)
T-677 POST-LIMPIEZA
si
lo requiere el procedimiento este
debe realizarse lo mas pronto posible
una vez terminado el examen.
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T-690 DOCUMENTOS
la siguiente información debe ser reportada:
identificación del procedimiento
tipo de liquido penetrante
designación de cada uno de los componentes
identificación de los examinadores
mapa o registro de las indicaciones
material y espesor
equipo de iluminación
fecha del examen
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ARTICLE 6 2011a SECTION V
ARTICLE 6
LIQUID PENETRANT EXAMINATION
T-620 GENERAL
The liquid penetrant examination method is an effective T-640 MISCELLANEOUS REQUIREMENTS
means for detecting discontinuities which are open to the T-641 Control of Contaminants
surface of nonporous metals and other materials. Typical
discontinuities detectable by this method are cracks, seams, The user of this Article shall obtain certification of con-
laps, cold shuts, laminations, and porosity. taminant content for all liquid penetrant materials used on
In principle, a liquid penetrant is applied to the surface nickel base alloys, austenitic or duplex stainless steels, and
to be examined and allowed to enter discontinuities. All titanium. These certifications shall include the penetrant
excess penetrant is then removed, the part is dried, and a manufacturers’ batch numbers and the test results obtained
developer is applied. The developer functions both as a in accordance with Mandatory Appendix II of this Article.
blotter to absorb penetrant that has been trapped in disconti- These records shall be maintained as required by the refer-
nuities, and as a contrasting background to enhance the encing Code Section.
visibility of penetrant indications. The dyes in penetrants
are either color contrast (visible under white light) or fluo- T-642 Surface Preparation
rescent (visible under ultraviolet light).
(a) In general, satisfactory results may be obtained when
the surface of the part is in the as-welded, as-rolled, as-cast,
T-621 Written Procedure Requirements
or as-forged condition. Surface preparation by grinding,
T-621.1 Requirements. Liquid penetrant examination machining, or other methods may be necessary where sur-
shall be performed in accordance with a written procedure face irregularities could mask indications.
which shall as a minimum, contain the requirements listed
(b) Prior to each liquid penetrant examination, the sur-
in Table T-621. The written procedure shall establish a
face to be examined and all adjacent areas within at least
single value, or range of values, for each requirement.
1 in. (25 mm) shall be dry and free of all dirt, grease,
T-621.2 Procedure Qualification. When procedure lint, scale, welding flux, weld spatter, paint, oil, and other
qualification is specified by the referencing Code Section, extraneous matter that could obscure surface openings or
a change of a requirement in Table T-621 identified as an otherwise interfere with the examination.
essential variable shall require requalification of the written (c) Typical cleaning agents which may be used are
procedure by demonstration. A change of a requirement detergents, organic solvents, descaling solutions, and paint
128
2011a SECTION V ARTICLE 6
TABLE T-621
REQUIREMENTS OF A LIQUID PENETRANT EXAMINATION PROCEDURE
Essential Nonessential
Requirement Variable Variable
removers. Degreasing and ultrasonic cleaning methods T-652 Techniques for Standard Temperatures
may also be used.
As a standard technique, the temperature of the penetrant
(d) Cleaning solvents shall meet the requirements of
and the surface of the part to be processed shall not be
T-641. The cleaning method employed is an important part
below 40°F (5°C) nor above 125°F (52°C) throughout the
of the examination process.
examination period. Local heating or cooling is permitted
NOTE: Conditioning of surfaces prior to examination as required in provided the part temperature remains in the range of 40°F
T-642(a) may affect the results. See SE-165, Annex A1. to 125°F (5°C to 52°C) during the examination. Where it is
not practical to comply with these temperature limitations,
other temperatures and times may be used, provided the
T-643 Drying After Preparation procedures are qualified as specified in T-653.
After cleaning, drying of the surfaces to be examined
shall be accomplished by normal evaporation or with
T-653 Techniques for Nonstandard
forced hot or cold air. A minimum period of time shall
Temperatures
be established to ensure that the cleaning solution has
evaporated prior to application of the penetrant. When it is not practical to conduct a liquid penetrant
examination within the temperature range of 40°F to 125°F
(5°C to 52°C), the examination procedure at the proposed
T-650 TECHNIQUE lower or higher temperature range requires qualification
of the penetrant materials and processing in accordance
T-651 Techniques
with Mandatory Appendix III of this Article.
Either a color contrast (visible) penetrant or a fluorescent
penetrant shall be used with one of the following three
penetrant processes: T-654 Technique Restrictions
(a) water washable Fluorescent penetrant examination shall not follow a
(b) post-emulsifying color contrast penetrant examination. Intermixing of pene-
(c) solvent removable trant materials from different families or different manufac-
The visible and fluorescent penetrants used in combina- turers is not permitted. A retest with water washable
tion with these three penetrant processes result in six liquid penetrants may cause loss of marginal indications due to
penetrant techniques. contamination.
129
ARTICLE 6 2011a SECTION V
Aluminum, magnesium, steel, brass Castings and welds Cold shuts, porosity, lack of fusion, 5
and bronze, titanium and high- cracks (all forms)
temperature alloys
Wrought materials — extrusions, Laps, cracks 10
forgings, plate
Carbide-tipped tools Brazed or welded Lack of fusion, porosity, cracks 5
Plastic All forms Cracks 5
Glass All forms Cracks 5
Ceramic All forms Cracks 5
NOTE:
(1) For temperature range from 50°F to 125°F (10°C to 52°C). For temperatures from 40°F (5°C) up to 50°F (10°C), minimum penetrant dwell
time shall be 2 times the value listed.
130
2011a SECTION V ARTICLE 6
T-674 Drying After Excess Penetrant Removal not alter the examination results, longer periods are permit-
ted. If the surface to be examined is large enough to pre-
(a) For the water washable or post-emulsifying tech-
clude complete examination within the prescribed or
nique, the surfaces may be dried by blotting with clean
established time, the examination shall be performed in
materials or by using circulating air, provided the tempera-
increments.
ture of the surface is not raised above 125°F (52°C).
(b) For the solvent removable technique, the surfaces T-676.2 Characterizing Indication(s). The type of dis-
may be dried by normal evaporation, blotting,wiping, or continuities are difficult to evaluate if the penetrant diffuses
forced air. excessively into the developer. If this condition occurs,
close observation of the formation of indication(s) during
T-675 Developing application of the developer may assist in characterizing
and determining the extent of the indication(s).
The developer shall be applied as soon as possible after
penetrant removal; the time interval shall not exceed that T-676.3 Color Contrast Penetrants. With a color con-
established in the procedure. Insufficient coating thickness trast penetrant, the developer forms a reasonably uniform
may not draw the penetrant out of discontinuities; con- white coating. Surface discontinuities are indicated by
versely, excessive coating thickness may mask indications. bleed-out of the penetrant which is normally a deep red
With color contrast penetrants, only a wet developer color that stains the developer. Indications with a light
shall be used. With fluorescent penetrants, a wet or dry pink color may indicate excessive cleaning. Inadequate
developer may be used. cleaning may leave an excessive background making inter-
pretation difficult. A minimum light intensity of 100 fc
T-675.1 Dry Developer Application. Dry developer
(1000 lx) is required on the surface to be examined to
shall be applied only to a dry surface by a soft brush, hand
ensure adequate sensitivity during the examination and
powder bulb, powder gun, or other means, provided the
evaluation of indications. The light source, technique used,
powder is dusted evenly over the entire surface being
and light level verification is required to be demonstrated
examined.
one time, documented, and maintained on file.
T-675.2 Wet Developer Application. Prior to applying
suspension type wet developer to the surface, the developer T-676.4 Fluorescent Penetrants. With fluorescent
must be thoroughly agitated to ensure adequate dispersion penetrants, the process is essentially the same as in T-676.3,
of suspended particles. with the exception that the examination is performed using
(a) Aqueous Developer Application. Aqueous developer an ultraviolet light, called black light. The examination
may be applied to either a wet or dry surface. It shall be shall be performed as follows:
applied by dipping, brushing, spraying, or other means, (a) It shall be performed in a darkened area.
provided a thin coating is obtained over the entire surface (b) Examiners shall be in a darkened area for at least
being examined. Drying time may be decreased by using 5 min prior to performing examinations to enable their
warm air, provided the surface temperature of the part is eyes to adapt to dark viewing. Glasses or lenses worn by
not raised above 125°F (52°C). Blotting is not permitted. examiners shall not be photosensitive.
(b) Nonaqueous Developer Application. Nonaqueous (c) Black lights shall achieve a minimum of 1000
developers shall be applied by spraying, except where W/cm2 on the surface of the part being examined through-
safety or restricted access preclude it. Under such condi- out the examination.
tions, developer may be applied by brushing. For (d) Reflectors and filters should be checked and, if nec-
water-washable or post-emulsifiable penetrants, the devel- essary, cleaned prior to use. Cracked or broken filters shall
oper shall be applied to a dry surface. For solvent remov- be replaced immediately.
able penetrants, the developer may be applied as soon as (e) The black light intensity shall be measured with a
practical after excess penetrant removal. Drying shall be black light meter prior to use, whenever the light’s power
by normal evaporation. source is interrupted or changed, and at the completion of
(10) T-675.3 Developing Time. Developing time for final the examination or series of examinations.
interpretation begins immediately after the application of
a dry developer or as soon as a wet developer coating is dry.
T-677 Post-Examination Cleaning
T-676 Interpretation When post-examination cleaning is required by the pro-
(10) T-676.1 Final Interpretation. Final interpretation shall cedure, it should be conducted as soon as practical after
be made not less than 10 min nor more than 60 min after Evaluation and Documentation using a process that does
the requirements of T-675.3 are satisfied. If bleed-out does not adversely affect the part.
131
ARTICLE 6 2011a SECTION V
132
2011a SECTION V ARTICLE 6
ARTICLE 6
MANDATORY APPENDICES
133
ARTICLE 6 2011a SECTION V
the test results obtained in accordance with II-640. These FIG. III-630 LIQUID PENETRANT COMPARATOR
records shall be maintained as required by the referencing (NOTE: Dimensions given are for guidance only and are not
Code Section. critical.)
Scribe
(39 mm)
line
11/2 in.
APPENDIX III — QUALIFICATION
(39 mm)
III-610 SCOPE
11/2 in.
When a liquid penetrant examination cannot be con-
ducted within the standard temperature range of 40°F to
125°F (5°C to 52°C), the temperature of the examination 2 in. 3/ in.
8
shall be qualified in accordance with this Appendix. (50 mm)
(10 mm)
III-630 MATERIALS
B
A liquid penetrant comparator block shall be made as
follows. The liquid penetrant comparator blocks shall be
made of aluminum, ASTM B 209, Type 2024, 3⁄8 in. A
(9.5 mm) thick, and should have approximate face dimen-
sions of 2 in. ⴛ 3 in. (50 mm ⴛ 75 mm). At the center
of each face, an area approximately 1 in. (25 mm) in
diameter shall be marked with a 950°F (510°C) tempera-
ture-indicating crayon or paint. The marked area shall be
heated with a blowtorch, a Bunsen burner, or similar device
to a temperature between 950°F (510°C) and 975°F “A” in the 40°F to 125°F (5°C to 52°C) temperature range.
(524°C). The specimen shall then be immediately quenched The indications of cracks shall be compared between blocks
in cold water, which produces a network of fine cracks on “A” and “B.” If the indications obtained under the proposed
each face. conditions on block “B” are essentially the same as
The block shall then be dried by heating to approxi- obtained on block “A” during examination at 40°F to 125°F
mately 300°F (149°C). After cooling, the block shall be (5°C to 52°C), the proposed procedure shall be considered
cut in half. One-half of the specimen shall be designated qualified for use. A procedure qualified at a temperature
block “A” and the other block “B” for identification in lower than 40°F (5°C) shall be qualified from that tempera-
subsequent processing. Figure III-630 illustrates the com- ture to 40°F (5°C).
parator blocks “A” and “B.” As an alternate to cutting the
block in half to make blocks “A” and “B,” separate blocks III-641.2 Temperature Greater Than 125°F (52°C).
2 in. ⴛ 3 in. (50 mm ⴛ 75 mm) can be made using the If the proposed temperature for the examination is above
heating and quenching technique as described above. Two 125°F (52°C), block “B” shall be held at this temperature
comparator blocks with closely matched crack patterns throughout the examination. The indications of cracks shall
may be used. The blocks shall be marked “A” and “B.” be compared as described in III-641.1 while block “B” is
at the proposed temperature and block “A” is at the 40°F
to 125°F (5°C to 52°C) temperature range.
III-640 REQUIREMENTS To qualify a procedure for temperatures above 125°F
(52°C), the upper and lower temperature limits shall be
III-641 Comparator Application
established and the procedure qualified at these tempera-
III-641.1 Temperature Less Than 40°F (5°C). If it is tures. [As an example, to qualify a procedure for the tem-
desired to qualify a liquid penetrant examination procedure perature range 126°F (52°C) to 200°F (93°C), the
at a temperature of less than 40°F (5°C), the proposed capability of a penetrant to reveal indications on the compa-
procedure shall be applied to block “B” after the block rator shall be demonstrated at both temperatures.]
and all materials have been cooled and held at the proposed
examination temperature until the comparison is com- III-641.3 Alternate Techniques for Color Contrast
pleted. A standard procedure which has previously been Penetrants. As an alternate to the requirements of III-641.1
demonstrated as suitable for use shall be applied to block and III-641.2, when using color contrast penetrants, it is
134
2011a SECTION V ARTICLE 6
permissible to use a single comparator block for the stan- Photographs shall be taken after processing at the nonstan-
dard and nonstandard temperatures and to make the com- dard temperature and then after processing at the standard
parison by photography. temperature. The indication of cracks shall be compared
(a) When the single comparator block and photographic between the two photographs. The same criteria for quali-
technique is used, the processing details (as applicable) fication as III-641.1 shall apply.
described in III-641.1 and III-641.2 apply. The block shall (b) Identical photographic techniques shall be used to
be thoroughly cleaned between the two processing steps. make the comparison photographs.
135
ARTICLE 24, SE-165 2011a SECTION V
certified in accordance with a written procedure conform- 10.3 Nondestructive Testing Agency Qualification — If
ing to the applicable edition of recommended Practice a nondestructive testing agency as described in Practice
SNT-TC-1A, ANSI/ASNT CP-189, NAS-410, or E 543 is used to perform the examination, the agency
MIL-STD-410. should meet the requirements of Practice E 543.
10.2 Procedure Qualification — Qualification of proce-
dures using times, conditions, or materials differing from 10.4 Requalification may be required when a change or
those specified in this general practice or for new materials substitution is made in the type of penetrant materials or
may be performed by any of several methods and should in the procedure (see 10.2).
be agreed upon by the contracting parties. A test piece
containing one or more discontinuities of the smallest rele-
vant size is used. When agreed upon by the contracting 11. Keywords
parties, the test piece may contain real or simulated discon-
tinuities, providing it displays the characteristics of the 11.1 fluorescent liquid penetrant testing; hydrophilic
discontinuities encountered in product examination. emulsification; lipophilic emulsification; liquid penetrant
10.2.1 Requalification of the procedure to be used testing; nondestructive testing; solvent removable; visible
may be required when a change is made to the procedure liquid penetrant testing; water-washable; post-emulsified;
or when material substitution is made. black light; ultraviolet light; visible light
494
2011a SECTION V ARTICLE 24, SE-165
ANNEXES
(Mandatory Information)
495
ARTICLE 24, SE-165 2011a SECTION V
buffing, scraping, mechanical milling, drilling, reaming, A2. Methods for Measuring Total Chlorine Content
grinding, liquid honing, sanding, lathe cutting, tumble or in Combustible Liquid Penetrant Materials
vibratory deburring, and abrasive blasting, including abra- A2.1 Scope and Application
sives such as glass beads, sand, aluminum oxide, ligno-
cellulose pellets, metallic shot, etc., are often used to A2.1.1 These methods cover the determination of
remove such soils as carbon, rust and scale, and foundry chlorine in combustible liquid penetrant materials, liquid
or solid. Its range of applicability is 0.001 to 5% using
adhering sands, as well as to deburr or produce a desired
either of the alternative titrimetric procedures. The proce-
cosmetic effect on the part. These processes may decrease
dures assume that bromine or iodine will not be present.
the effectiveness of the penetrant testing by smearing or
If these elements are present, they will be detected and
peening over metal surfaces and filling discontinuities open
reported as chlorine. The full amount of these elements will
to the surface, especially for soft metals such as aluminum,
not be reported. Chromate interferes with the procedures,
titanium, magnesium, and beryllium alloy.
causing low or nonexistent end points. The method is appli-
A1.1.1.8 Acid Etching — Inhibited acid solutions cable only to materials that are totally combustible.
(pickling solutions) are routinely used for descaling part
A2.2 Summary of Methods
surfaces. Descaling is necessary to remove oxide scale,
which can mask surface discontinuities and prevent pene- A2.2.1 The sample is oxidized by combustion in a
trant from entering. Acid solutions/etchants are also used bomb containing oxygen under pressure (see A2.2.1.1).
routinely to remove smeared metal that peens over surface The chlorine compounds thus liberated are absorbed in a
discontinuities. Such etchants should be used in accordance sodium carbonate solution and the amount of chloride pres-
with the manufacturers’ recommendations. ent is determined titrimetrically either against silver nitrate
with the end point detected potentiometrically (Method A)
NOTE A1.1: Etched parts and materials should be rinsed completely free or coulometrically with the end point detected by current
of etchants, the surface neutralized and thoroughly dried by heat prior flow increase (Method B).
to application of penetrants. Acids and chromates can adversely affect
the fluorescence of fluorescent materials. A2.2.1.1 Safety — Strict adherence to all of the
provisions prescribed hereinafter ensures against explosive
NOTE A1.2 Whenever there is a possibility of hydrogen embrittlement rupture of the bomb, or a blow-out, provided the bomb is
as a result of acid solution/etching, the part should be baked at a suitable of proper design and construction and in good mechanical
temperature for an appropriate time to remove the hydrogen before further condition. It is desirable, however, that the bomb be
processing. After baking, the part shall be cooled to a temperature below
125°F (52°C) before applying penetrants.
enclosed in a shield of steel plate at least 1⁄2 in. (12.7 mm)
thick, or equivalent protection be provided against unfore-
A1.1.1.9 Air Firing of Ceramics — Heating of a seeable contingencies.
ceramic part in a clean, oxidizing atmosphere is an effective
way of removing moisture or light organic soil or both. A2.3 Apparatus
The maximum temperature that will not cause degradation A2.3.1 Bomb, having a capacity of not less than
of the properties of the ceramic should be used. 300 mL, so constructed that it will not leak during the test,
and that quantitative recovery of the liquids from the bomb
A1.2 Post Cleaning may be readily achieved. The inner surface of the bomb
A1.2.1 Removal of Developer — Dry powder devel- may be made of stainless steel or any other material that
oper can be effectively removed with an air blow-off (free will not be affected by the combustion process or products.
of oil) or it can be removed with water rinsing. Wet devel- Materials used in the bomb assembly, such as the head
oper coatings can be removed effectively by water rinsing gasket and leadwire insulation, shall be resistant to heat
or water rinsing with detergent either by hand or with a and chemical action, and shall not undergo any reaction
mechanical assist (scrub brushing, washing machine, etc.). that will affect the chlorine content of the liquid in the
The soluble developer coatings simply dissolve off of the bomb.
part with a water rinse. A2.3.2 Sample Cup, platinum, 24 mm in outside
A1.2.2 Residual penetrant may be removed through diameter at the bottom, 27 mm in outside diameter at the
solvent action. Solvent soaking (15 min minimum) and top, 12 mm in height outside and weighing 10 to 11 g,
ultrasonic solvent cleaning (3 min minimum) techniques opaque fused silica, wide-form with an outside diameter
of 29 mm at the top, a height of 19 mm, and a 5-mL
are recommended. In some cases, it is desirable to vapor
capacity (Note A2.1), or nickel (Kawin capsule form), top
degrease, then follow with a solvent soak. The actual time
diameter of 28 mm, 15 mm in height, and 5-mL capacity.
required in the vapor degreaser and solvent soak will
depend on the nature of the part and should be determined NOTE A2.1: Fused silica crucibles are much more economical and longer-
experimentally. lasting than platinum. After each use, they should be scrubbed out with
496
2011a SECTION V ARTICLE 24, SE-165
fine, wet emery cloth, heated to dull red heat over a burner, soaked in TABLE A2.1
hot water for 1 h, then dried and stored in a desiccator before reuse. GAGE PRESSURES
A2.3.3 Firing Wire, platinum, approximately No. 26 Gage Pressure, atm (MPa)
B & S gage. Capacity of Bomb, mL minA max
A2.3.4 Ignition Circuit (Note A2.2), capable of sup-
300 to 350 38 (3.85) 40 (4.05)
plying sufficient current to ignite the nylon thread or cotton 350 to 400 35 (3.55) 37 (3.75)
wicking without melting the wire. 400 to 450 30 (3.04) 32 (3.24)
450 to 500 27 (2.74) 29 (2.94)
NOTE A2.2: The switch in the ignition circuit shall be of a type that
A
remains open, except when held in closed position by the operator. The minimum pressures are specified to provide sufficient oxygen
for complete combustion and the maximum pressures present a
A2.3.5 Nylon Sewing Thread, or Cotton Wicking, safety requirement.
white.
A2.4 Purity of Reagents add it to the sample cup by means of a dropper at this time
A2.4.1 Reagent grade chemicals shall be used in all (see Note A2.5 and Note A2.6).
tests. Unless otherwise indicated, it is intended that all
NOTE A2.3: After repeated use of the bomb for chlorine determination,
reagents shall conform to the specifications of the Commit- a film may be noticed on the inner surface. This dullness should be
tee on Analytical Reagents of the American Chemical Soci- removed by periodic polishing of the bomb. A satisfactory method for
ety, where such specifications are available. Other grades doing this is to rotate the bomb in a lathe at about 300 rpm and polish
may be used provided it is first ascertained that the reagent the inside surface with Grit No. 2/0 or equivalent paper coated with a
is of sufficiently high purity to permit its use without less- light machine oil to prevent cutting, and then with a paste of grit-free
chromic oxide and water. This procedure will remove all but very deep
ening the accuracy of the determination. pits and put a high polish on the surface. Before using the bomb, it should
A2.4.2 Unless otherwise indicated, references to be washed with soap and water to remove oil or paste left from the
water shall be understood to mean referee grade reagent polishing operation. Bombs with porous or pitted surfaces should never
be used because of the tendency to retain chlorine from sample to sample.
water conforming to Specification D 1193. It is recommended to not use more than 1 g total of sample and white
A2.5 Decomposition oil or other chlorine-free combustible material.
A2.5.1 Reagents and Materials: NOTE A2.4: If the sample is not readily miscible with white oil, some
other nonvolatile, chlorine-free combustible diluent may be employed in
A2.5.1.1 Oxygen, free of combustible material and
place of white oil. However, the combined weight of sample and nonvola-
halogen compounds, available at a pressure of 40 atm tile diluent shall not exceed 1 g. Some solid additives are relatively
(4.05 MPa). insoluble, but may be satisfactorily burned when covered with a layer
of white oil.
A2.5.1.2 Sodium Carbonate Solution (50 g
Na2CO3/L) — Dissolve 50 g of anhydrous Na2CO3 or 58.5 g NOTE A2.5: The practice of running alternately samples high and low
of Na2CO3 · H2O) or 135 g of Na2CO3 · 10H2O in water in chlorine content should be avoided whenever possible. It is difficult
and dilute to 1 L. to rinse the last traces of chlorine from the walls of the bomb and the
tendency for residual chlorine to carry over from sample to sample has
A2.5.1.3 White Oil, refined. been observed in a number of laboratories. When a sample high in chlorine
has preceded one low in chlorine content, the test on the low-chlorine
A2.5.2 Procedure:
sample should be repeated and one or both of the low values thus obtained
A2.5.2.1 Preparation of Bomb and Sample — Cut should be considered suspect if they do not agree within the limits of
a piece of firing wire approximately 100 mm in length. repeatability of this method.
Coil the middle section (about 20 mm) and attach the free A2.5.2.2 Addition of Oxygen — Place the sample
ends to the terminals. Arrange the coil so that it will be cup in position and arrange the nylon thread, or wisp of
above and to one side of the sample cup. Place 5 mL of cotton so that the end dips into the sample. Assemble the
Na2CO3 solution in the bomb (Note A2.3), place the cover bomb and tighten the cover securely. Admit oxygen (see
on the bomb and vigorously shake for 15 s to distribute Note A2.6) slowly (to avoid blowing the sample from the
the solution over the inside of the bomb. Open the bomb, cup) until a pressure is reached as indicated in Table A2.1.
place the sample-filled sample cup in the terminal holder,
and insert a short length of thread between the firing wire Note A2.6: It is recommended to not add oxygen or ignite the sample if
and the sample. Use of a sample weight containing over the bomb has been jarred, dropped, or tilted.
20 mg of chlorine may cause corrosion of the bomb. The A2.5.2.3 Combustion — Immerse the bomb in a
sample weight should not exceed 0.4 g if the expected cold-water bath. Connect the terminals to the open electri-
chlorine content is 2.5% or above. If the sample is solid, cal circuit. Close the circuit to ignite the sample. Remove
not more than 0.2 g should be used. Use 0.8 g of white the bomb from the bath after immersion for at least ten
oil with solid samples. If white oil will be used (Note A2.4), minutes. Release the pressure at a slow, uniform rate such
497
ARTICLE 24, SE-165 2011a SECTION V
that the operation requires not less than 1 min. Open the amount of difference between the present reading and the
bomb and examine the contents. If traces of unburned oil last reading. Continue adding 0.1-mL increments, making
or sooty deposits are found, discard the determination, and readings and determining differences between readings
thoroughly clean the bomb before again putting it in use until a maximum difference between readings is obtained.
(Note A2.3). The total amount of AgNO3 solution required to produce
this maximum differential is the end point. Automatic titra-
A2.6 Analysis, Method A, Potentiometric Titration
tors continuously stir the sample, add titrant, measure the
Procedure
potential difference, calculate the differential, and plot the
A2.6.1 Apparatus:
differential on a chart. The maximum differential is taken
A2.6.1.1 Silver Billet Electrode. at the end point.
A2.6.1.2 Glass Electrode, pH measurement type.
NOTE A2.8: For maximum sensitivity, 0.00282 N AgNO3 solution may
A2.6.1.3 Buret, 25-mL capacity, 0.05-mL gradua- be used with the automatic titrator. This dilute reagent should not be
tions. used with large samples or where chlorine content may be over 0.1%
since these tests will cause end points of 10 mL or higher. The large
A2.6.1.4 Millivolt Meter, or expanded scale pH amount of water used in such titrations reduces the differential between
meter capable of measuring 0 to 220 mV. readings, making the end point very difficult to detect. For chlorine
contents over 1% in samples of 0.8 g or larger, 0.282 N AgNO3 solution
NOTE A2.7: An automatic titrator is highly recommended in place of will be required to avoid exceeding the 10-mL water dilution limit.
items A2.6.1.3 through A2.6.1.4. Repeatability and sensitivity of the
method are much enhanced by the automatic equipment while much A2.6.5 Blank — Make blank determinations with the
tedious effort is avoided. amount of white oil used but omitting the sample. (Liquid
A2.6.2 Reagents and Materials: samples normally require only 0.15 to 0.25 g of white oil
A2.6.2.1 Acetone, chlorine-free. while solids require 0.7 to 0.8 g.) Follow normal procedure,
making two or three test runs to be sure the results are
A2.6.2.2 Methanol, chlorine-free. within the limits of repeatability for the test. Repeat this
A2.6.2.3 Silver Nitrate Solution (0.0282 N) — Dis- blank procedure whenever new batches of reagents or white
solve 4.7910 ± 0.0005 g of silver nitrate (AgNO3) in water oil are used. The purpose of the blank run is to measure
and dilute to 1 L. the chlorine in the white oil, the reagents, and that intro-
A2.6.2.4 Sodium Chloride Solution (0.0282 N) — duced by contamination.
Dry a few grams of sodium chloride (NaCl) for 2 h at A2.6.6 Standardization — Silver nitrate solutions are
130°C to 150°C, weigh out 1.6480 ± 0.0005 g of the dried not permanently stable, so the true activity should be
NaCl, dissolve in water, and dilute to 1 L. checked when the solution is first made up and then periodi-
A2.6.2.5 Sulfuric Acid (1 + 2) — Mix 1 volume cally during the life of the solution. This is done by titration
of concentrated sulfuric acid (H2SO4, sp. gr 1.84) with 2 of a known NaCl solution as follows: Prepare a mixture
volumes of water. of the amounts of the chemicals (Na2CO3 solution, H2SO4
solution, acetone, and methanol) specified for the test. Pipet
A2.6.3 Collection of Chlorine Solution — Remove
in 5.0 mL of 0.0282-N NaCl solution and titrate to the
the sample cup with clean forceps and place in a 400-mL
end point. Prepare and titrate a similar mixture of all the
beaker. Wash down the walls of the bomb shell with a
chemicals except the NaCl solution, thus obtaining a
fine stream of methanol from a wash bottle, and pour the
reagent blank reading. Calculate the normality of the
washings into the beaker. Rinse any residue into the beaker.
AgNO3 solution as follows:
Next, rinse the bomb cover and terminals into the beaker.
Finally, rinse both inside and outside of the sample crucible 5.0 ⴛ NNaCl
NAgNO3 p (A2.1)
into the beaker. Washings should equal but not exceed VA − VB
100 mL. Add methanol to make 100 mL. where:
A2.6.4 Determination of Chlorine — Add 5 mL of NAgNO3 p normality of the AgNO3 solution,
H2SO4 (1:2) to acidify the solution (solution should be NNaCl p normality of the NaCl solution,
acid to litmus and clear of white Na2CO3 precipitate). Add VA p millilitres of AgNO3 solution used for the titra-
100 mL of acetone. Place the electrodes in the solution, tion including the NaCl solution, and
start the stirrer (if mechanical stirrer is to be used), and VB p millilitres of AgNO3 solution used for the titra-
begin titration. If titration is manual, set the pH meter on tion of the reagents only.
the expanded millivolt scale and note the reading. Add
A2.6.7 Calculation — Calculate the chlorine content
exactly 0.1 mL of AgNO3 solution from the buret. Allow a
of the sample as follows:
few seconds stirring; then record the new millivolt reading.
Subtract the second reading from the first. Continue the (VS − VB) ⴛ N ⴛ 3.545
Chlorine, weight % p (A2.2)
titration, noting each amount of AgNO3 solution and the W
498
2011a SECTION V ARTICLE 24, SE-165
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ARTICLE 24, SE-165 2011a SECTION V
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2011a SECTION V ARTICLE 24, SE-165
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ARTICLE 24, SE-165 2011a SECTION V
A3.8 Calculation are separated on the basis of their relative affinities for a
A3.8.1 Calculate the fluorine content of the sample low capacity, strongly basic anion exchanger (guard and
as follows: separator column). The separated anions are directed onto
a strongly acidic cation exchanger (suppressor column)
2 ⴛ 10−4 2 ⴛ 10−4 where they are converted to their highly conductive acid
Fluorine, ppm p
冤10⌬E /S − 1 − 10⌬E /S − 1冥 ⴛ 10
1 2 6
(A3.1) form and the carbonate-bicarbonate eluant is converted to
W weakly conductive carbonic acid. The separated anions in
their acid form are measured by conductivity. They are
where: identified on the basis of retention time as compared to
⌬E1 p millivolt change in sample solution on addition standards. Quantitation is by measurement of peak area or
of 100 L of stock fluoride solution, peak height. Blanks are prepared and analyzed in a similar
⌬E2 p millivolt change in blank solution on addition of fashion.
100 L of the stock fluoride solution, A4.2.2 Interferences — Any substance that has a
S p slope of fluoride electrode as determined in retention time coinciding with that of any anion to be
A3.7.1, and determined will interfere. For example, relatively high con-
W p grams of sample. centrations of low-molecular-weight organic acids interfere
A3.9 Precision and Bias with the determination of chloride and fluoride. A high
A3.9.1 Repeatability — The results of two determina- concentration of any one ion also interferes with the resolu-
tions by the same analyst should not be considered suspect tion of others. Sample dilution overcomes many interfer-
unless they differ by more than 1.1 ppm (0.00011%) or ences. To resolve uncertainties of identification or
8.0% of the amount detected, whichever is greater. quantitation use the method of known additions. Spurious
peaks may result from contaminants in reagent water, glass-
A3.9.2 Reproducibility — The results of two determi-
ware, or sample processing apparatus. Because small sam-
nations by different laboratories should not be considered
ple volumes are used, scrupulously avoid contamination.
suspect unless they differ by 6.7 ppm or 129.0% of the
amount detected, whichever is greater. A4.2.3 Minimum Detectable Concentration — The
minimum detectable concentration of an anion is a function
A3.9.3 Bias — The average recovery of the method
of sample size and conductivity scale used. Generally,
is 62% to 64% of the amount actually present although 83%
to 85% recoveries can be expected with proper technique. minimum detectable concentrations are in the range of
0.05 mg/L for F− and 0.1 mg/L for Br−, Cl−, NO3−, NO2−,
PO43−, and SO42− with a 100-L sample loop and a 10-
A4. Determination of Anions by Ion mho full-scale setting on the conductivity detector. Simi-
Chromatography With Conductivity lar values may be achieved by using a higher scale setting
Measurement and an electronic integrator.
A4.1 Scope and Application
A4.3 Apparatus
A4.1.1 This method is condensed from ASTM proce-
A4.3.1 Bomb, having a capacity of not less than
dures and APHA Method 429 and optimized for the analy-
300 mL, so constructed that it will not leak during the test,
sis of detrimental substances in organic based materials.
and that quantitative recovery of the liquids from the bomb
It provides a single instrumental technique for rapid,
may be readily achieved. The inner surface of the bomb
sequential measurement of common anions such as bro-
may be made of stainless steel or any other material that
mide, chloride, fluoride, nitrate, nitrite, phosphate, and
will not be affected by the combustion process or products.
sulfate.
Materials used in the bomb assembly, such as the head
A4.2 Summary of Method gasket and leadwire insulation, shall be resistant to heat
A4.2.1 The material must be put in the form of an and chemical action, and shall not undergo any reaction
aqueous solution before analysis can be attempted. The that will affect the chlorine content of the liquid in the
sample is oxidized by combustion in a bomb containing bomb.
oxygen under pressure. The products liberated are absorbed A4.3.2 Sample Cup, platinum, 24 mm in outside
in the eluant present in the bomb at the time of ignition. diameter at the bottom, 27 mm in outside diameter at the
This solution is washed from the bomb, filtered, and diluted top, 12 mm in height outside, and weighing 10 to 11 g;
to a known volume. opaque fused silica, wide-form with an outside diameter
A4.2.1.1 A filtered aliquot of sample is injected of 29 mm at the top, a height of 19 mm, and a 5-mL
into a stream of carbonate-bicarbonate eluant and passed capacity (Note A4.1), or nickel (Kawin capsule form), top
through a series of ion exchangers. The anions of interest diameter of 28 mm, 15 mm in height, and 5-mL capacity.
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2011a SECTION V ARTICLE 24, SE-165
NOTE A4.1: Fused silica crucibles are much more economical and longer A4.4.4 Regenerant Solution 1, H2SO4, 1 N, use this
lasting than platinum. After each use, they should be scrubbed out with regenerant when suppressor is not a continuously regener-
fine, wet emery cloth, heated to dull red heat over a burner, soaked in
hot water for 1 h then dried and stored in a desiccator before reuse.
ated one.
A4.3.3 Firing Wire, platinum, approximately No. 26 A4.4.5 Regenerant Solution 2, H2SO4, 0.025 N, dilute
B and S gage. 2.8 mL conc H2SO4 to 4 L or 100 mL regenerant solution
1 to 4 L. Use this regenerant with continuous regeneration
A4.3.4 Ignition Circuit (Note A4.2), capable of sup- fiber suppressor system.
plying sufficient current to ignite the nylon thread or cotton
A4.4.6 Standard Anion Solutions, 100 mg/L, prepare
wicking without melting the wire.
a series of standard anion solutions by weighing the indi-
NOTE A4.2: The switch in the ignition circuit shall be of a type that cated amount of salt, dried to a constant weight at 105°C,
remains open, except when held in closed position by the operator. to 1000 mL. Store in plastic bottles in a refrigerator; these
A4.3.5 Nylon Sewing Thread, or Cotton Wicking, solutions are stable for at least one month.
white. Amount,
Anion Salt g/L
A4.3.6 Ion Chromatograph, including an injection
valve, a sample loop, guard, separator, and suppressor col- Cl− NaCl 1.6485
F− NaF 2.2100
umns, a temperature-compensated small-volume conduc- Br− NaBr 1.2876
tivity cell (6 L or less), and a strip chart recorder capable NO3− NaNO3 1.3707
of full-scale response of 2 s or less. An electronic peak NO2− NaNO2 1.4998
integrator is optional. The ion chromatograph shall be capa- PO43− KH2PO4 1.4330
ble of delivering 2 to 5 mL eluant/min at a pressure of SO42− K2SO4 1.8141
1400 to 6900 kPa. A4.4.7 Combined Working Standard Solution, High
A4.3.7 Anion Separator Column, with styrene Range — Combine 10 mL of the Cl−, F−, NO3−, NO2−, and
divinyl-benzene-based low-capacity pellicular PO43− standard anion solutions, 1 mL of the Br−, and 100
anion-exchange resin capable of resolving Br−, Cl−, F−, mL of the SO42− standard solutions, dilute to 1000 mL,
NO3−, NO2−, PO43−, and SO42−; 4 ⴛ 250 mm. and store in a plastic bottle protected from light; contains
A4.3.8 Guard Column, identical to separator column 10 mg/L each of Cl−, F−, NO3−, NO2−, and PO43−, 1 mg
except 4 ⴛ 50 mm, to protect separator column from Br−/L, and 100 mg SO42−/L. Prepare fresh daily.
fouling by particulates or organics. A4.4.8 Combined Working Standard Solution, Low
A4.3.9 Suppressor Column, high-capacity cation- Range — Dilute 100 mL combined working standard solu-
exchange resin capable of converting eluant and separated tion, high range, to 1000 mL and store in a plastic bottle
anions to their acid forms. protected from light; contains 1.0 mg/L each Cl−, F−, NO3−,
NO2−, and PO43−, 0.1 mg Br−/L, and 10 mg SO42−/L. Pre-
A4.3.10 Syringe, minimum capacity of 2 mL and pare fresh daily.
equipped with a male pressure fitting.
A4.4.9 Alternative Combined Working Standard
A4.4 Reagents Solutions — Prepare appropriate combinations according
A4.4.1 Purity of Reagents — Reagent grade chemi- to anion concentration to be determined. If NO2− and PO43−
cals shall be used in all tests. Unless otherwise indicated, are not included, the combined working standard is stable
it is intended that all reagents shall conform to the specifi- for one month.
cations of the Committee on Analytical Reagents of the
A4.5 Decomposition Procedure
American Chemical Society, where such specifications are
available. Other grades may be used provided it is first A4.5.1 Preparation of Bomb and Sample — Cut a
ascertained that the reagent has sufficiently high purity piece of firing wire approximately 100 mm in length. Coil
to permit its use without lessening the accuracy of the the middle section (about 20 mm) and attach the free ends
determination. to the terminals. Arrange the coil so that it will be above
and to one side of the sample cup. Place 5 mL of Na2CO3/
A4.4.2 Deionized or Distilled Water, free from inter- NaHCO3 solution in the bomb, place the cover on the bomb,
ferences at the minimum detection limit of each constituent and vigorously shake for 15 s to distribute the solution over
and filtered through a 0.2-m membrane filter to avoid the inside of the bomb. Open the bomb, place the sample-
plugging columns. filled sample cup in the terminal holder, and insert a short
A4.4.3 Eluant Solution, sodium bicarbonate-sodium length of thread between the firing wire and the sample.
carbonate, 0.003M NaHCO3− 0.0024M Na2CO3: dissolve The sample weight used should not exceed 1 g. If the
1.008 g NaHCO3 and 1.0176 g Na2CO3 in water and dilute sample is a solid, add a few drops of white oil at this time
to 4 L. to ensure ignition of the sample.
503
ARTICLE 24, SE-165 2011a SECTION V
300 to 350 38 40
350 to 400 35 37
400 to 450 30 32
450 to 500 27 29
A
The minimum pressures are specified to provide sufficient oxygen
for complete combustion and the maximum pressures present a
safety requirement.
Chlorine Sample
Content, Weight, White Oil
% g Weight, g A4.6 Procedure
2 to 5 0.4 0.4 A4.6.1 System Equilibration — Turn on ion chroma-
5 to 10 0.2 0.6 tograph and adjust eluant flow rate to approximate the
10 to 20 0.1 0.7 separation achieved in Fig. A4.1 (2 to 3 mL/min). Adjust
20 to 50 0.05 0.7 detector to desired setting (usually 10 mho) and let system
CAUTION: Do not use more than 1 g total of sample and white oil come to equilibrium (15 to 20 min). A stable base line
or other fluorine-free combustible material. indicates equilibrium conditions. Adjust detector offset to
zero-out eluant conductivity; with the fiber suppressor
A4.5.2 Addition of Oxygen — Place the sample cup adjust the regeneration flow rate to maintain stability, usu-
in position and arrange the nylon thread, or wisp of cotton ally 2.5 to 3 mL/min.
so that the end dips into the sample. Assemble the bomb and
tighten the cover securely. Admit oxygen (see Note A4.4) A4.6.1.1 Set up the ion chromatograph in accor-
slowly (to avoid blowing the sample from the cup) until dance with the manufacturer’s instructions.
a pressure is reached as indicated in Table A4.1. A4.6.2 Calibration — Inject standards containing a
single anion or a mixture and determine approximate reten-
NOTE A4.4: It is recommended to not add oxygen or ignite the sample
if the bomb has been jarred, dropped, or tilted. tion times. Observed times vary with conditions but if
standard eluant and anion separator column are used, reten-
A4.5.3 Combustion — Immerse the bomb in a cold- tion always in the order F−, Cl−, NO2−, PO43−, Br−, NO3−,
water bath. Connect the terminals to the open electrical and SO42−. Inject at least three different concentrations for
circuit. Close the circuit to ignite the sample. Remove the each anion to be measured and construct a calibration curve
bomb from the bath after immersion for at least 10 min. by plotting peak height or area against concentration on
Release the pressure at a slow, uniform rate such that the linear graph paper. Recalibrate whenever the detector set-
operation requires not less than 1 min. Open the bomb and ting is changed. With a system requiring suppressor regen-
examine the contents. If traces of unburned oil or sooty eration, NO2− interaction with the suppressor may lead to
deposits are found, discard the determination, and thor- erroneous NO2− results; make this determination only when
oughly clean the bomb before again putting it in use. the suppressor is at the same stage of exhaustion as during
A4.5.4 Collection of Solution — Remove the sample standardization or recalibrate frequently. In this type of
cup with clean forceps and rinse with deionized water and system the water dip (see Note A4.4) may shift slightly
filter the washings into a 100-mL volumetric flask. Rinse during suppressor exhaustion and with a fast run column
the walls of the bomb shell with a fine stream of deionized this may lead to slight interference for F− or Cl−. To elimi-
water from a wash bottle, and add the washings through nate this interference, analyze standards that bracket the
the filter paper to the flask. Next, rinse the bomb cover expected result or eliminate the water dip by diluting the
and terminals and add the washings through the filter into sample with eluant or by adding concentrated eluant to the
the volumetric flask. Finally, add deionized water to bring sample to give the same HCO3−/CO32− concentration as in
the contents of the flask to the line. Use aliquots of this the eluant. If sample adjustments are made, adjust standards
solution for the ion chromatography (IC) analysis. and blanks identically.
504
2011a SECTION V ARTICLE 24, SE-165
NOTE A4.5: Water dip occurs because water conductivity in sample is TABLE A4.2
less than eluant conductivity (eluant is diluted by water). PRECISION AND ACCURACY OBSERVED FOR ANIONS
A4.6.2.1 If linearity is established for a given AT VARIOUS CONCENTRATION LEVELS IN REAGENT
detector setting, it is acceptable to calibrate with a single WATER
standard. Record the peak height or area and retention time Single-
to permit calculation of the calibration factor, F. Amount Amount Overall Operator Significant
Added, Found, Precision, Precision, Bias 95%
A4.6.3 Sample Analysis — Remove sample particu- Anion mg/L mg/L mg/L mg/L Level
lates, if necessary, by filtering through a prewashed
0.2-m-pore-diam membrane filter. Using a prewashed F− 0.48 0.49 0.05 0.03 No
syringe of 1 to 10 mL capacity equipped with a male luer F− 4.84 4.64 0.52 0.46 No
Cl 0.76 0.86 0.38 0.11 No
fitting inject sample or standard. Inject enough sample to Cl− 17 17.2 0.82 0.43 No
flush sample loop several times: for 0.1 mL sample loop Cl 455 471 46 13 No
inject at least 1 mL. Switch ion chromatograph from load NO2 0.45 0.09 0.09 0.04 Yes, neg
to inject mode and record peak heights and retention times NO2 21.8 19.4 1.9 1.3 Yes, neg
on strip chart recorder. After the last peak (SO42−) has Br− 0.25 0.25 0.04 0.02 No
Br− 13.7 12.9 1.0 0.6 No
appeared and the conductivity signal has returned to base PO43− 0.18 0.10 0.06 0.03 Yes, neg
line, another sample can be injected. PO43− 0.49 0.34 0.15 0.17 Yes, neg
A4.6.4 Regeneration — For systems without fiber NO3− 0.50 0.33 0.16 0.03 No
NO3− 15.1 14.8 1.15 0.9 No
suppressor regenerate with 1 N H2SO4 in accordance with SO42− 0.51 0.52 0.07 0.03 No
the manufacturer’s instructions when the conductivity base SO42− 43.7 43.5 2.5 2.2 No
line exceeds 300 mho when the suppressor column is
on line.
A4.7 Calculation H p peak height or area,
A4.7.1 Calculate concentration of each anion, in F p response factor − concentration of standard/
mg/L, by referring to the appropriate calibration curve. height (or area) of standard, and
Alternatively, when the response is shown to be linear, use D p dilution factor for those samples requiring
the following equation: dilution.
505