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CURSO
NIVEL II
LIQUIDOS PENETRANTES
HERNAN FERRER
ASNT – NDT LEVEL III
INDICE
LECCION 1 CALIFICACION DE PERSONAL
LECCION 2 METALURGIA & PROCESOS
LECCION 3 DISCONTINUIDADES
LECCION 4 INTRODUCCION A LOS NDT
LECCION 5 HISTORIA DE LOS LIQUIDOS PENETRANTES
LECCION 6 PRINCIPIOS BASICOS
LECCION 7 PENETRANTES & REVELADORES
LECCION 8 PREPARACION DE LAS PARTES
LECCION 9 METODOS
LECCION 10 EQUIPOS PARA PRUEBA
LECCION 11 SELECCIÓN DEL METODO
LECCION 12 INTERPRETACION & EVALUACION
LECCION 13 CONTROL DE PROCESO
LECCION 14 ARTICULO 6, SECCION V
ANEXO 1 ASME SECTION V, EDITION 2013, ARTICLE 6
ANEXO 2 ASME SECTION V, EDITION 2013, SE-165
16/10/2014
LECCION 1
CALIFICACION DEL
PERSONAL
RESPUESTA
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RESPUESTA
SNT-TC-1A
La Asociación Americana de
Pruebas No Destructivas (ASNT)
desde 1966 publica una guía para el
entrenamiento y calificación del
personal involucrado en los
exámenes no destructivos
SNT-TC-1A
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SNT-TC-1A
SNT-TC-1A
CONTENIDO DE LA NORMA
SNT-TC-1A
El SNT-TC- 1 A describe:
- Los requisitos de conocimiento
- Las capacidades
Para estar calificado en cada uno de
los niveles establecidos.
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NIVELES DE CALIFICACION
APRENDICES
NIVEL I
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NIVEL II
NIVEL II
NIVEL III
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NIVEL III
NIVEL III
EXPERIENCIA
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ENTRENAMIENTO
CALIFICACION
VERSUS
CERTIFICACION
PROCESO DE CALIFICACION
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PROCESO DE CALIFICACION
PROCESO DE CALIFICACION
CERTIFICACION
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CERTIFICACION
CERTIFICACION
CERTIFICACION
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LECCION 2
METALURGIA
&
PROCESOS
QUE ES EL ACERO
□ El acero es una aleación de hierro
carbón, donde el contenido de
carbón no supera el 2%
□ El acero es producido a partir del
mineral de hierro o la chatarra y
fundido en un horno eléctrico
OTROS ELEMENTOS
□ El acero no solo contiene hierro y
carbono, sino otros elementos como:
Manganeso
Silicio
Fosforo
Azufre
(Estos últimos son considerados
impurezas)
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ALEANTES
□ Además de los elementos antes
descritos, a los aceros se les adicionan
otros elementos llamados aleantes
con la finalidad de mejorar sus
propiedades mecánicas.
□ Elementos como el Cromo, el Níquel y
el Molibdeno, tienen un efecto
importante en las propiedades del
acero
SOLIDIFICACION
□ Durante la solidificación del metal
liquido en particular los aceros
pueden tener dos arreglos cristalinos,
estos arreglos cristalinos pueden
cambiar dependiendo de la
temperatura
BCC
□ Un arreglo se llama Cubico de cuerpo
centrado y es el que exhibe el hierro
en temperaturas por debajo de los 910
grados C.
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FCC
□ Otro arreglo se llama Cubico de cara
centrado y es el que exhibe el hierro
en temperaturas por encima de los
910 grados C.
GRANOS
□ Estos granos solo pueden observarse
en el microscopio, y de su tamaño
dependen las propiedades del
material
MICROESTRUCTURA
□ La distribución de estos granos se
llama la microestructura, de esta
dependen básicamente las
propiedades mecánicas del material
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TRATAMIENTOS TERMICOS
□ El proceso de solidificación, las
impurezas en el material, y los
procesos de conformado que
veremos a continuación producen
esfuerzos residuales que afectan las
propiedades mecánicas de los
materiales
TRATAMIENTOS TERMICOS
□ El proceso de solidificación, las
impurezas en el material, y los
procesos de conformado que
veremos a continuación producen
esfuerzos residuales que afectan las
propiedades mecánicas de los
materiales
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TRATAMIENTOS TERMICOS
□ Los tratamientos térmicos mas
comunes son:
□ Recocido (annealing)
□ Normalizado (normilizing)
□ Templado & Revenido (Quenched
&tempered)
□ Relevo de esfuerzos (stress relieving)
□ Recocido de disolución (solution
annealing)
RECOCIDO
NORMALIZADO
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RELEVO DE ESFUERZOS
RECOCIDO DE DISOLUCION
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CONFORMADO
CONFORMADO
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CONFORMADO
DISCONTINUIDADES
SOLDADURA
□ Otro de los procesos importantes es el
proceso de soldadura, el proceso mas
común utilizado en la industria es la
soldadura de arco.
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SOLDADURA
□ Los procesos utilizados comúnmente
son:
□ SMAW (Soldadura de arco con electrodo
recubierto)
□ SAW (Soldadura de arco sumergido)
□ GTAW (TIG)
□ GMAW (MIG o MAG)
□ FCAW (Soldadura con alambre con
núcleo de fundente)
JUNTAS
□ Dos tipos de juntas son utilizadas en la
fabricación de las uniones soldadas:
1. Juntas en Ranura
2. Juntas de filete
SOLDADURA DE RANURA
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SOLDADURA DE FILETE
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DISCONTINUIDADES
DEFINICION DE DISCONTINUIDAD
DEFINICION DE DISCONTINUIDAD
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CATEGORIAS DE LAS
DISCONTINUIDADES
DISCONTINUIDADES INHERENTES
En los metales, las discontinuidades inherentes son aquellas
que se relacionan con la fundición y la solidificación original del
metal fundido, el lingote, o la fundición.
DSICONTINUIDADES DE PROCESO
Las discontinuidades de proceso están relacionadas con los
procesos de manufactura tales como forjado, mecanizado,
conformado, extruido, enrollado, soldadura. Tratamiento térmico, y
plateado.
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DSICONTINUIDADES DE SERVICIO
Las discontinuidades de servicio están
relacionadas con las condiciones en servicio de los
objetos a examinar.
DISCONTINUIDADES INHERENTES
Las discontinuidades inherentes en los
lingotes se forman durante el proceso y la
solidificación, e incluye las siguientes:
1. Inclusiones (escoria, impurezas etc.).
2. Porosidad (gases atrapados).
3. Tubería contracción).
4. Grietas.
DISCONTINUIDADES
INHERENTES
Las discontinuidades inherentes en la
fundición son aquellas relacionadas con el
proceso de fundición, y la solidificación del
objeto a examinar e incluyen las siguientes:
1. Porosidad (gases atrapados).
2. Contracción
3. Desgarramientos en caliente.
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DISCONTINUIDADE
INHERENTES
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DISCONTINUIDADES DE LAS
FUNDICIONES
Aunque la fundición es un proceso primario las
discontinuidades son inherentes e incluyen lo siguiente:
1. Inclusiones.
2. Desgarramientos en caliente.
3. Porosidad.
4. Enfriadores no fundidos.
5. Capillas no fundidas.
6. Rechupes.
DISCONTINUIDADES DE LA SOLDADURA
a) Agrietamiento en frio
DISCONTINUIDADES DE LA SOLDADURA
b) Agrietamiento en caliente
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DISCONTINUIDADES DE LA SOLDADURA
c) Desgarramiento laminar
DISCONTINUIDADES DE LA SOLDADURA
d) Falta de fusión
DISCONTINUIDADES DE LA SOLDADURA
e) Falta de penetración
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DISCONTINUIDADES DE LA SOLDADURA
f) Porosidad
DISCONTINUIDADES DE LA SOLDADURA
g) Inclusiones de escoria
DISCONTINUIDADES DE LA SOLDADURA
h) Mordedura (undercut)
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DISCONTINUIDADES DE LA SOLDADURA
DISCONTINUIDADES DE LA SOLDADURA
i) Concavidad en la raíz
DISCONTINUIDADES DE LA SOLDADURA
i) Penetración excesiva
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DISCONTINUIDADES DE LA SOLDADURA
j) Excesivo refuerzo
DISCONTINUIDADES DE LA SOLDADURA
k) Traslapo
DISCONTINUIDADES EN SERVICIO
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AGRIETAMIENTO
AGRIETAMIENTO
DISCONTINUIDADES DE SERVICIO
1. GRIETAS DE FATIGA
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DISCONTINUIDADES DE SERVICIO
DISCONTINUIDADES DE SERVICIO
DISCONTINUIDADES DE SERVICIO
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LECCION 4
INTRODUCCION
A LOS NDT
QUE ES UN NDT
□ Un NDT es una prueba física (MT/RT/UT)
o fisicoquímica (PT, que permite
encontrar las discontinuidades en una
pieza, sin destruir su utilidad.
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LIQUIDOS PENETRANTES
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LIQUIDOS PENETRANTES
El método de líquidos penetrantes esta
basado en los siguientes factores:
La posibilidad de detectar las zonas en la
superficie de la parte donde los líquidos
han penetrado.
LIQUIDOS PENETRANTES
LIQUIDOS PENETRANTES
El Procedimiento de ensayo es como
sigue a continuación:
El exceso de penetrante enseguida se
remueve por medio de la limpieza de la
superficie y una substancia (llamada
revelador) absorbe el penetrante que
se ha introducido en la discontinuidad,
de tal manera que evidencia el hecho
de la presencia de una discontinuidad
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LIQUIDOS PENETRANTES
Los líquidos penetrantes requieren de la
utilización de:
Un liquido penetrante que sea capaz de
penetrar dentro de las discontinuidades,
emergiendo a la superficie por medio de
la acción de capilaridad
LIQUIDOS PENETRANTES
Los líquidos penetrantes requieren de
la utilización de:
Un revelador el cual se aplica una vez el
exceso del penetrante ha sido
removido, y permite que el penetrante
acumulado en la discontinuidad salga
de esta y permita su detección.
VENTAJAS
LIQUIDOS PENETRANTES
1. Pueden aplicarse en materiales
ferromagnéticos y no
ferromagnéticos
2. Se pueden realizar fácilmente sobre
las superficies que sean accesibles
3. El procedimiento de aplicación e
interpretación es relativamente
sencillo
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VENTAJAS
LIQUIDOS PENETRANTES
4. El equipo en comparación con los
otros métodos de ensayo es mucho
mas económico.
LIMITACIONES
LIQUIDOS PENETRANTES
Las limitaciones mas importantes son:
1. Solo puede detectar
discontinuidades abiertas a la
superficie
2. Las discontinuidades que se
encuentren llenas de algún material
extraño no pueden ser detectables.
LIMITACIONES
LIQUIDOS PENETRANTES
Las limitaciones mas importantes son:
3. El acondicionado de la superficie
tiene que ser mas seguro que para
los otros métodos de ensayo.
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LIMITACIONES
LIQUIDOS PENETRANTES
Las limitaciones mas importantes son:
3. El acondicionado de la superficie
tiene que ser mas seguro que para
los otros métodos de ensayo.
PARTICULAS MAGNETICAS
PARTICULAS MAGNETICAS
□ La magnitud del flujo dispersado se
utiliza para la visualización de las
discontinuidades en la forma de una
indicación visible utilizando un medio
especifico para el ensayo.
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PARTICULAS MAGNETICAS
□ Este método permite que aquellas
discontinuidades que estén
demasiado cerca una de otra o
aquellas que estén contacto y que
sean difíciles de observar con el ojo sin
ayuda, sean visualizadas utilizando un
medio especifico de ensayo, el cual
se va acumular en la discontinuidad.
PARTICULAS MAGNETICAS
El método de partículas magnéticas
solo se puede utilizar en piezas que se
puedan magnetizar y esta basado en
los siguientes factores:
1. Que exista la posibilidad de
magnetizar la pieza
PARTICULAS MAGNETICAS
El método de partículas magnéticas
solo se puede utilizar en piezas que se
puedan magnetizar y esta basado en
los siguientes factores:
2. Que existan variaciones en el campo
magnético generadas por la
discontinuidad en la pieza.
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PARTICULAS MAGNETICAS
El método de partículas magnéticas
solo se puede utilizar en piezas que se
puedan magnetizar y esta basado en
los siguientes factores:
3. La posibilidad de detectar las
variaciones en la superficie y cerca
de la superficie en el campo
magnético en la pieza.
PARTICULAS MAGNETICAS
El ensayo requiere de un sistema que
comprende los siguientes elementos:
1. Un equipo para producir la
magnetización de la pieza
2. Los polvos magnéticos
(partículas)que deben ser
dispersados sobre la pieza para
poder revelar las variaciones en el
campo magnético
PARTICULAS MAGNETICAS
VENTAJAS
1. Permite detectar discontinuidades
superficiales & sub-superficiales
2. No requiere de un
acondicionamiento especial de la
superficie
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PARTICULAS MAGNETICAS
LIMITACIONES
1. Solo se puede utilizar en materiales
ferromagnéticos
2. Se requiere de un equipo que pueda
producir el campo magnético de la
potencia adecuada.
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LIMITACIONES
1. La pieza que se desee examinar
debe ser fácilmente accesible
2. No es un ensayo muy preciso para
evaluar la altura de la discontinuidad
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ENSAYO RADIOGRAFICO
Este ensayo se ejecuta mediante la
utilización de la radiación y esta basado
en los siguientes factores:
1. La capacidad de la radiación de
pasar a través de la material
2. La absorción diferencial de la
radiación en la pieza examinada
3. La posibilidad de medir las diferencias
de absorción
ENSAYO RADIOGRAFICO
El ensayo radiográfico requiere de la
utilización de:
1. Una fuente de radiación
2. Un detector de radiación (película o
una pantalla)
ENSAYO RADIOGRAFICO
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ENSAYO RADIOGRAFICO
VENTAJAS:
1. Produce una imagen verdadera de
la sección de la pieza.
2. Permite examinar una gran variedad
de materiales
3. Permite examinar el volumen de
materiales muy gruesos.
ENSAYO RADIOGRAFICO
LIMITACIONES:
1. El acceso a la pieza debe ser por
ambos lados
2. No es ideal para medir la altura o
profundidad de las discontinuidades
o para identificar las dimensiones de
discontinuidades oblicuas al eje del
rayo.
CONFIABILIDAD
El siguiente es un resumen de la
confiabilidad de los ensayos no
destructivos para detector las
discontinuidades y su evaluación en
cuanto al tamaño y profundidad tanto
para las superficiales o sub-superficiales
14
DISCONTINUIDAD
SUPERFICIAL SUB-SUPERFICIAL
METODO EVALUACION EVALUACION EVALUACION EVALUACION
DETECCION DETECCION PROFUNDIDAD
LONGITUD ALTURA LONGITUD ALTURA
PT ADECUADA ADECUADA INAPLICABLE INAPLICABLE INAPLICABLE INAPLICABLE INAPLICABLE
MT ADECUADA ADECUADA LIMITADO BAJA EFICIENCIA BAJA EFICIENCIA INAPLICABLE INAPLICABLE
UT LIMITADO BAJA EFICIENCIA BAJA EFICIENCIA ADECUADA BUENA BAJA EFICIENCIA ADECUADA
RT ADECUADA ADECUADA INAPLICABLE ADECUADA BUENA BAJA EFICIENCIA APLICABLE *
* SE REQUIEREN TECNICAS ESPECIALES CON CALCULOS Y AL MENOS DOS EXPOSICIONES
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PROCESO DE EVALUACION
PROCESO DE EVALUACION
PROCESO DE EVALUACION
ENSAYO
INDICACION
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PROCESO DE EVALUACION
INTERPRETACION FALSA
DE LA INDICACION
DISCONTINUIDAD
PROCESO DE EVALUACION
EVALUACION DE NO
LA INDICACION RELEVANTE
RELEVANTE
(FALLA)
PROCESO DE EVALUACION
APLICACION DEL ACEPTABLE
(CRITERIO)
RECHAZADO
(DEFECTO)
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PROCESO
□ Como se pudo ver en el diagrama
anterior el proceso de evaluación de
los ensayos no destructivos es
complejo y requiere de un
conocimiento adecuado
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Historia de los
líquidos penetrantes
LECCION 5
Historia
Los líquidos penetrantes es uno de los
métodos mas antiguo de examen no
destructivo, su origen se remonta a la
inspección de los ejes de locomotora
en los años 1890.
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PARTICULAS MAGNETICAS
Una vez se introdujo la técnica de las
partículas magnéticas en 1930 en la
industria, la prueba de cal y aceite
se convirtió en obsoleta, aunque en
nuestro medio aun se utiliza para
examinar soldaduras de sello
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UTILIZACION DE NO FERROSOS
MAGNAFLUX
En 1941 Magnaflux patento el primer
producto para realizar los líquidos
penetrantes, en los materiales para
detectar defectos superficiales.
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Líquidos penetrantes
fluorescentes post-emulsificables
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PRINCIPIOS BASICOS
LECCION 6
PRINCIPIOS BASICOS
PRIMER PASO
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PRIMER PASO
PRIMER PASO
SEGUNDO PASO
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SEGUNDO PASO
TERCER PASO
TERCER PASO
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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.
CUARTO PASO
CUARTO PASO
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QUINTO PASO
Examen visual de las superficies a
examinar, interpretación y
evaluación de las indicaciones.
QUINTO PASO
Examen visual de las superficies a
examinar, interpretación y evaluación
de las indicaciones.
SEXTO PASO
Post-limpieza de la parte.
El propósito de este paso es eliminar
los residuos del proceso, si estos
pueden demeritar las operaciones
posteriores, o la función de la parte.
En algunos casos se puede requerir de
un tratamiento especial para evitar la
corrosión.
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PORQUE UTILIZAR PT
PORQUE UTILIZAR PT
PORQUE UTILIZAR PT
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PORQUE UTILIZAR PT
- Los técnicos pueden detectar visualmente
las indicaciones
- Los líquidos penetrantes pueden usarse en
la detección temprana de problemas de
producción o en las verificaciones en
servicio
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CARACTERISTICAS QUIMICAS
Los líquidos penetrantes en su mayoría son
orgánicos, y tienen un muy bajo peso especifico
tales como los alcoholes, aceites minerales o
vegetales y substancias sintéticas derivadas del
petróleo, lo anterior mezclado.
CARACTERISTICAS QUIMICAS
Estas substancias (penetrantes, solventes,
emulsificadores y reveladores) tienen que ser
químicamente inerte para los materiales
ensayados, y en especial no ser corrosivos.
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PROPIEDADES FISICAS
Los líquidos penetrantes tienen que tener ciertas
características que aseguren la penetración en las
discontinuidades, aunque estas sean muy
angostas.
PROPIEDADES FISICAS
La habilidad de penetrar de un liquido depende de una
propiedad llamada capilaridad, la cual depende de:
1. Tensión superficial
2. La acción humedecedora
3. Viscosidad
TENSION SUPERFICIAL
La tensión superficial es la fuerza cohesiva ejercida por
las moléculas superficiales de un liquido, haciendo que la
superficie se comporte como una membrana elástica.
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ACCION HUMEDECEDORA
La habilidad de humedecer y el ángulo de contacto
entre un liquido y un gas y un solido y un liquido
son inversamente proporcionales. Luego entre el
ángulo de contacto sea mas pequeño se obtiene
una mayor habilidad de humedecer
ANGULO DE CONTACTO
El ángulo de contacto determina la habilidad de
humedecer. El ángulo de contacto también variara
con la substancia que es humedecida. La siguiente
figura muestra la relación entre el ángulo de
contacto y la habilidad de humedecer.
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VISCOSIDAD
VISCOSIDAD
Los penetrantes con alta viscosidad requieren un
tiempo de permanencia mayor, lo cual incrementa el
tiempo del ensayo, contrariamente un penetrante de
baja viscosidad puede fluir muy rápidamente en la
superficie, no permitiendo el tiempo de permanencia en
superficies inclinadas
ACCION DE CAPILARIDAD
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ACCION DE CAPILARIDAD
ACCION DE CAPILARIDAD
El ángulo de contacto bajo ocasiona que el borde
del liquido se curve hacia arriba de la pared del
tubo. La tensión superficial del liquido ocasiona que
el liquido se adhiera a la pared del tubo atrayendo
liquido adicional para humedecer el área
ocasionando que el liquido se eleve en el tubo
ACCION DE CAPILARIDAD
Cuando el ángulo de contacto se acerca a 90°, el
liquido no se derrama y el nivel del liquido en el tubo
permanece en el mismo nivel que fuera del tubo. Lo
contrario ocurre cuando el ángulo es mayor de 90°, los
ángulos de contacto grandes curvan el borde del
liquido hacia abajo y el nivel se deprime
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ACCION DE CAPILARIDAD
La siguiente figura ilustra el efecto de capilaridad
EFECTO DE LA TEMPERATURA
EFECTO DE LA TEMPERATURA
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EFECTO DE LA TEMPERATURA
OTRAS PROPIEDADES
PUNTO DE INFLAMACION
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TOXICIDAD E IRRITABILIDAD
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EMULSIFICACION
La mezcla entre el aceite y el agua se llama emulsión,
ciertos químicos tienen la habilidad de mezclarse con
el aceite y formar mezclas fácilmente emulsificables,
este es el caso de los penetrantes y los
emulsificadores, cuando los penetrantes basados en
el petróleo se combina con el emulsificador , esta
mezcla puede removerse con un enjuague de agua
EMULSIFICACION
Hay dos tipos de emulsificadores en el proceso de
remoción del exceso de penetrante, estos son:
Lipofilicos
Hidrofiilicos
CURSO ANDRITZ
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EMULSIFICACION
El mecanismo de acción de los emulsificadores es
diferente, las siguientes figuras ilustran los
mecanismos de acción de los emulsificadores
lipofilicos e hidrofilicos.
CURSO ANDRITZ
CURSO ANDRITZ
CURSO ANDRITZ
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ACCION REVELADORA
La función básica de todos los reveladores es
mejorar la visibilidad de las indicaciones del
penetrante. La mejora en la visibilidad se logra a
través de un numero de mecanismos incluyendo:
ACCION REVELADORA
ACCION REVELADORA
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ACCION REVELADORA
ACCION REVELADORA
ABSORCION
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ADSORCION
TIPO DE REVELADOR
2. Reveladores acuosos
3. Reveladores no acuosos
TIPO DE REVELADOR
2. Reveladores acuosos
3. Reveladores no acuosos
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REVELADORES SECOS
REVELADORES ACUOSOS
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1. Fácil de aplicar
2. Se puede dispersar fácilmente en la superficie
formando una capa uniforme
3. Altamente absorbente
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TIPOS DE PENETRANTE
METODO DE REMOCION
SENSITIVIDAD (FLUORESCENTES)
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CLASES DE SOLVENTES
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PREPARACION SUPERFICIAL
PREPARACION SUPERFICIAL
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PREPARACION SUPERFICIAL
De todas maneras el objeto que se vaya
a examinar debe estar libre de cualquier
material extraño que pueda interferir
con el examen y completamente seco
PREPARACION SUPERFICIAL
OPERACIONES
CONTRAINDICADAS
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OPERACIONES
CONTRAINDICADAS
Las especificaciones generalmente prohíben las
operaciones que puedan producir entrapado del
material, o que enmascaren las discontinuidades
abiertas a la superficie antes de los líquidos
penetrantes.
Algunas especificaciones exigen algún método de
preparación para remover el metal entrapado, tales
como el atacado con acido.
ACABADO SUPERFICIAL
Un acabado superficial liso es preferible, pero se
puede realizar los líquidos penetrantes en las
soldaduras o fundiciones con una variedad de
superficies siempre y cuando se utilicen los
materiales para los líquidos penetrantes
apropiados, y los métodos de remoción del
exceso de penetrante adecuados
PRE-LIMPIEZA
Existen muchos métodos de pre-limpieza, la
selección del método depende del material a
ser examinado y la condición de la superficie .
Todos los métodos de limpieza que se
deseen utilizar tienen que cumplir con los
requisitos ambientales, de seguridad y salud
locales.
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PRE-LIMPIEZA
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METODOS DE LIMPIEZA
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NIVEL I PT
LIMPIEZA
CON DETERGENTE
Para la limpieza con detergentes se utilizan
tanques de inmersión con soluciones
detergentes.
Los detergentes húmedos, penetran,
emulsifican, y saponifican los solidos.
El único equipo especial que se necesita es la
necesidad de un enjuague y secado.
DESENGRASADO
CON VAPOR
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DESENGRASADO
CON VAPOR
DESENGRASADO
CON VAPOR
LIMPIEZA CON
VAPOR Y DETERGENTE
Esta limpieza se realiza en piezas complicadas y
muy grandes donde no se puede utilizar la limpieza
por inmersión
Se utiliza una mezcla de vapor con un detergente
alcalino el cual emulsifica, ablanda y disuelve los
contaminantes orgánicos.
El vapor produce la acción mecánica de remoción
del objeto del detergente y los contaminantes.
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LIMPIEZA ULTRASONICA
LIMPIEZA ULTRASONICA
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REMOVEDORES DE PINTURA
Los separadores o solventes que permiten
remover la pintura del sustrato pueden usarse
para la pre-limpieza
El equipo requerido y las direcciones deben
cumplir con las recomendaciones del fabricante
ATACADO
Los objetos a examinar que hayan sufrido
operaciones que puedan entrapar el metal, tales
como limpieza con cepillo eléctrico, neumático, o
chorro de arena, usualmente requieren del atacado
para poder realizar los líquidos penetrantes.
Este proceso utiliza una substancia acida o alcalina
la cual abre las discontinuidades y remueve el metal
entrapado.
ATACADO
Todos los residuos de acido o alcalinos
tienen que ser neutralizados y removidos
antes de la prueba con líquidos penetrantes
El proceso de atacado se realiza en
tanques o en equipos manuales
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PROCESOS DE PRE-LIMPIEZA
QUE DEBEN SER EVITADOS
Los siguientes procesos no deberían ser utilizados
antes de los líquidos penetrantes:
Limpieza con chorro (arena, perdigones u otro
medio solido con presión) “sandblasting or
shotblasting”
Limpieza con agua a alta presión
Tela de esmeril
Cepillos de alambre eléctricos o neumáticos
Raspadores de metal
PROCESOS DE PRE-LIMPIEZA
QUE DEBEN SER EVITADOS
El problema con los procesos anteriores es que
tienden a cerrar las discontinuidades mediante el
entrapado del metal, el martillado, o el trabajo en
frio de la superficie.
El cepillo de alambre manual puede ser
suficiente para remover el herrumbre, sarro, o la
pintura de la superficie.
SECADO
Un paso muy importante en el proceso de los
líquidos penetrantes es asegurar que todas las
superficies y todas las discontinuidades potenciales
están completamente secas, la razón es sencilla si
alguno de los líquidos utilizados en la pre-limpieza
permanece en la discontinuidad va a evitar que el
penetrante entre haciendo ineficiente el examen.
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SECADO
Lo anterior es muy critico ya que el examinador
puede no estar prevenido en cuanto que el
penetrante no haya entrado en la discontinuidad.
Algunos procedimientos requieren que después de
alguna limpieza con agua, reciban una limpieza final
con un solvente tal como la acetona o el alcohol
isopropilico para promover la evaporación del agua
de las discontinuidades.
SECADO
Algunos procedimientos de examen requieren
que los objetos a examinar sean secados en un
horno a temperaturas de hasta 71°C.
Como mínimo todas las superficies deberían ser
secadas por evaporación normal por un mínimo
de cinco minutos.
LECCION 9
APLICACIÓN DEL
PENETRANTE
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APLICACIÓN DEL
PENETRANTE
La aplicación del penetrante se lleva a cabo
después que la superficie a examinar este
completamente limpia y seca.
APLICACIÓN DEL
PENETRANTE
Los métodos de aplicación del penetrante
pueden ser:
Rociado (spray)
Con pincel o brocha
Vertido
Inmersión
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APLICACIÓN DEL
PENETRANTE
APLICACIÓN EN LAS
SOLDADURAS
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APLICACIÓN DE LOS
PENETRANTES FLUORESCENTES
Nótese que en este
proceso es necesario
suspender la pieza a
examinar durante todo el
tiempo de permanencia
del penetrante requerido
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
ILUMINACION ADECUADA
LECCION 10
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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
La evaluación de las indicaciones con líquidos
penetrantes requiere de una iluminación apropiada del
área a examinar, la cantidad de iluminación se
encuentra en los procedimientos , pero para los
líquidos penetrantes visibles 1000 Lx son adecuados.
LUXOMETRO
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ILUMINACION ADECUADA
Para los líquidos penetrantes fluorescentes la
superficie debe iluminarse con 1000 mW/cm2,
de radiación ultravioleta (UV-A) medida en la
superficie a examinar, y la luz blanca en la
zona no debe exceder de 20 Lx.
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ESTACION DE ENJUAGUE
Los objetos que se
están examinando
son expuestos a una
luz fluorescente para
asegurarla completa
limpieza total
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APLICACIÓN DEL
REVELADOR
LECCION 12
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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)
3. Las indicaciones reveladas no se inician hasta
tanto la humedad del revelador no se evapore
completamente.
4. El espesor del recubrimiento y su color blanco
ayudan a ver las tintas visibles.
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SUSPENDIDOS EN AGUA
(FORMA C)
5. Los objetos a examinar deberían ser
chequeados para asegurar que se haya aplicado
un cubrimiento uniforme del revelador.
6. El revelador debería ser chequeado
regularmente para detectar contaminación y
evaporación del agua según las especificaciones
con un hidrómetro.
SUSPENDIDOS EN AGUA
(FORMA C)
7. La remoción de los reveladores suspendibles
secos puede ser mas dificultosa pues ellos no
son solubles en el agua.
8. Todos los reveladores acuosos necesariamente
deben contener biosidas, inhibidores de
corrosión y agentes humectantes.
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Conjunto de
líquidos
penetrantes
visibles y
fluorescentes
TIEMPO DE REVELADO
1. El revelado de las indicaciones solamente se
inicia cuando la humedad del revelador se
evapora completamente.
2. El objeto a examinar tiene que ser monitoreado
muy cercanamente durante el tiempo de
permanencia del revelador para poder evaluar
las indicaciones cuando ellas se forman
TIEMPO DE REVELADO
3. Típicamente el tiempo de permanencia del
revelador es como mínimo 10 minutos, aunque
siempre se deberá consultar las especificaciones.
4. El punto en el cual se inicia el tiempo de
permanencia del revelador depende del tipo de
revelador utilizado.
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TIEMPO DE REVELADO
5. Para los reveladores húmedos, el tiempo de
permanencia se inicia tan pronto como el
revelador se seca.
6. Para los reveladores secos y los no acuosos, el
tiempo de permanencia se inicia al momento de la
aplicación
DEFINICIONES
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DEFINICIONES
Evaluación. Una revisión después de la
interpretación de las indicaciones detectadas
para determinar cuando ellas cumplen con el
criterio de aceptación.
DEFINICIONES
DEFINICIONES
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DEFINICIONES
POST-LIMPIEZA
La post-limpieza puede envolver uno o varios de los
siguientes métodos:
1. Desengrasado con vapor.
2. Empapado con solvente.
3. Limpieza ultrasónica.
Otros métodos de limpieza posterior al examen
pueden ser especificados en los procedimientos
particulares.
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METODOS DE ENSAYO
Click here to add text
LECCION 9
ClickA
METODO here
/ to add text. Click here to add
REVELADOR SECOtext.
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METODO A
PREPARACION DE LA SUPERFICIE
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APLICACIÓN PENETRANTE
TIEMPO DE PERMANENCIA
ENJUAGE
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SECADO
APLICACIÓN REVELADOR
TIEMPO DE REVELADO
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INSPECCION
METODOClick
A here
/ REVELADOR ACUOSO
to add text. Click here to add text.
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METODO A
PREPARACION DE LA SUPERFICIE
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APLICACIÓN PENETRANTE
TIEMPO DE PERMANENCIA
ENJUAGE
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APLICACIÓN REVELADOR
SECADO
TIEMPO DE REVELADO
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INSPECCION
METODOClick
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/ REVELADOR SECO
to add text. Click here to add text.
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METODO B
PREPARACION DE LA SUPERFICIE
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APLICACIÓN PENETRANTE
TIEMPO DE PERMANENCIA
APLICACIÓN DEL
EMULSIFICADOR
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ENJUAGE
SECADO
APLICACIÓN REVELADOR
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TIEMPO DE REVELADO
INSPECCION
METODOClick
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/ REVELADOR ACUOSO
to add text. Click here to add text.
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METODO B
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PREPARACION DE LA SUPERFICIE
APLICACIÓN PENETRANTE
TIEMPO DE PERMANENCIA
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APLICACIÓN DEL
EMULSIFICADOR
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ENJUAGE
APLICACIÓN REVELADOR
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SECADO
TIEMPO DE REVELADO
INSPECCION
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METODOClick
C here to add text. Click here to add text.
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METODO C
PREPARACION DE LA SUPERFICIE
APLICACIÓN PENETRANTE
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TIEMPO DE PERMANENCIA
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TIEMPO DE REVELADO
INSPECCION
METODOClick
D here
/ REVELADOR SECO
to add text. Click here to add text.
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METODO D
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PREPARACION DE LA SUPERFICIE
APLICACIÓN PENETRANTE
TIEMPO DE PERMANENCIA
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PRE-ENJUAGE
APLICACIÓN DEL
EMULSIFICADOR
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ENJUAGE
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SECADO
APLICACIÓN REVELADOR
TIEMPO DE REVELADO
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INSPECCION
METODOClick
D here
/ REVELADOR ACUOSO
to add text. Click here to add text.
Click here to add text. Click here to add text.
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METODO D
PREPARACION DE LA SUPERFICIE
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APLICACIÓN PENETRANTE
TIEMPO DE PERMANENCIA
PRE-ENJUAGE
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APLICACIÓN DEL
EMULSIFICADOR
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ENJUAGE
APLICACIÓN REVELADOR
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SECADO
TIEMPO DE REVELADO
INSPECCION
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EQUIPOS PARA
PRUEBA
LECCION 10
UNIDADES DE PRUEBA
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.
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UNIDADES EXAMINADORAS
2. La escogencia 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:
1. Tipo de penetrante utilizado
2. Requisitos del procesado.
3. Tamaño de los objetos a examinar.
4. Cantidad / velocidad de producción deseada.
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.
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EQUIPOS DE ESTACIONES
EQUIPOS DE ESTACIONES
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UNIDADES DE ESTACIONES
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ESTACION DE LAVADO
HORNO DE SECADO
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ESTACION DE BOMBAS
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ESTACION DE BOMBAS
3. El uso de mangueras a presión y aplicadores.
4. Requieren mantenimiento rutinario para asegurar su
confiabilidad.
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
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TERMOSTATOS Y TERMOMETROS
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REFRACTOMETRO
Se utiliza para
medir la
concentración del
emulsificador
hidrofilico en el
agua.
HIDROMETRO
Un hidrómetro se utiliza
para medir la gravedad
especifica de los
reveladores con base agua.
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HIDROMETRO
Balasto Tallo
Escala
Cuerpo
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Conjunto
típico portátil
de líquidos
penetrantes
visibles.
CONJUNTO DE PENETRANTES
FLUORESCENTES
El conjunto de penetrante fluorescente combina la
portabilidad con la alta visibilidad y normalmente contiene:
1. Lámpara ultravioleta portátil.
2. Limpiador solvente.
3. Removedor del penetrante.
4. Penetrante fluorescente.
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CONJUNTO DE PENETRANTES
FLUORESCENTES
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NIVEL I
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LUXOMETROS
1. Los sensores de luz blanca miden en pies-candela o lux.
2. Los sensores de radiación ultravioleta miden en micro vatios
por centímetro cuadrado (mW/cm2).
NIVEL I
MATERIALES
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MATERIALES PARA
LIQUIDOS PENETRANTES
PRELIMPIEZA Y POSTLIMPIEZA
1. Los materiales tienen que ser compatibles con el
penetrante.
2. Los fabricantes recomiendan un limpiador aprobado
para sus productos.
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.
NIVEL I
PENETRANTES POSTEMULSIFICABLES
1. Los penetrantes postemulsificables están disponibles en el
tipo fluorescente.
2. Estos penetrantes tienen la ventaja de eliminar en parte el
sobre enjuague.
EMULSIFICADORES
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EMULSIFICADORES
Tanque de inmersion
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 estándar.
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
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.
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REVELADORES
REVELADOR SECO
REVELADOR SECO
4. Un gran cuidado debe tomarse para no contaminar el
revelador con penetrante fluorescente.
5. La contaminación con penetrante puede causar motas
que aparecen como indicaciones.
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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
1. Asegúrese que el objeto a examinar no se dañe o se
sobrecaliente durante el examen
2. El examinador tiene que asegurarse que el solvente no es
peligroso para el objeto a examinar .
3. Revise las MSDS frecuentemente.
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INTRODUCCION
INTRODUCCION
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VENTAJAS
1. Las ventajas de utilizar penetrantes fluorescentes es
que las indicaciones con fluorescente son mas
fáciles de ver.
2. La ventaja de los penetrantes removibles con agua
es que son mas rápidos, seguros, ecológicos, y
baratos.
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DESVENTAJAS
La desventaja de los penetrantes removibles con agua es
el peligro de sobre lavarlos, si el examinador no utiliza las
técnicas apropiadas. El sobre lavado puede ocurrir con
cualquier tipo, método, o nivel de sensitividad, si los
examinadores fallan en seguir las practicas de trabajo
apropiadas.
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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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PORTABILIDAD
1. Los exámenes con líquidos penetrantes en el campo
pueden realizarse efectivamente y eficientemente
utilizando conjuntos de penetrante Tipo I
(fluorescente) o tipo II (visible) ya sea limpiados con
agua o con solvente.
2. Los conjuntos de líquidos penetrantes aerosol son
portátiles, y si son Tipo II removibles con solvente, no
se necesita electricidad ni agua.
PORTABILIDAD
3. La ventaja de los conjuntos de aerosol es su portabilidad , y
se requieren tiempos muy cortos de ajuste.
4. La desventaja de la limpieza manual es que el método es
lento
Postemulsification
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POSTEMULSIFICABLES
POSTEMULSIFICADO
5. La desventaja del método de los postemulsificados es el costo
del emulsificador y el equipo, el tiempo adicional para el paso
de la emulsificacion y los chequeos de mantenimiento para el
emulsificador.
6. El Método B no se permite en algunas especificaciones
industriales.
REVELADOR
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REVELADOR SECO
1. El revelador seco es mejor para las superficies rugosas, tales
como las fundiciones, o objetos a examinar con roscas finas y
esquinas, tales como chaveteros
2. El revelador seco es también mas fácil de manejar y aplicar.
REVELADOR SECO
REVELADOR SECO
5. El revelador seco es el tipo de revelador menos sensitivo y no
debería utilizarse para los penetrantes visibles.
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REVELADORES HUMEDOS
1. Los reveladores acuosos pueden aplicarse inmediatamente
después del enjugado con agua y antes del secado.
2. Ambos los reveladores suspendidos en agua y los solubles en
agua pueden aplicarse por inmersión rociado, o derramando
REVELADORES HUMEDOS
REVELADORES HUMEDOS
5. Ambos tipos de revelador húmedo dejan un deposito de
revelador en las superficies rugosas tales como las fundiciones
u objetos a examinar con roscas finas o esquinas tales como
chaveteros.
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REVELADORES HUMEDOS
REVELADORES HUMEDOS
8. Los reveladores húmedos no acuosos son los mas sensitivos
puesto que ellos son rociados en una capa delgada muy
controlada
REVELADORES HUMEDOS
9. El solvente se disuelve en el penetrante, ligeramente
reduciendo su viscosidad incrementando el volumen del
penetrante en la discontinuidad arrastrando las indicaciones a
la superficie cuando el liquido volátil se evapora.
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REVELADORES ESPECIALES
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Interpretación &
evaluación
Lección 12
TIPOS DE INDICACIONES
TIPOS DE INDICACIONES
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INDICACIONES TIPICAS
DE LOS LIQUIDOS PENETRANTES
GRIETA GRIETA
GRANDE FINA
INDICACIONES TIPICAS
DE LOS LIQUIDOS PENETRANTES
TRASLAPOS POROS
COSTURAS
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3
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EFECTOS DE LA TEMPERATURA
EFECTOS DE LA TEMPERATURA
4
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ILUMINACION
ILUMINACION
5
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SEQUENCIA
6
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7
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2. La temperatura.
3. El tiempo de permanencia
4. La aplicación del revelador.
5. Condiciones de examen.
8
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Durante el PROCESO
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
Durante el PROCESO
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Durante el PROCESO
Durante el PROCESO
Durante el PROCESO
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INDICACIONES DE GRIETAS
INDICACIONES ESPECIFICAS
EN LOS MATERIALES
INDICACIONES ESPECIFICAS
EN LOS MATERIALES
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INDICACIONES DE
LAS DISCONTINUIDADES
a. Grietas.
b. Rechupes.
d. Costuras.
INDICACIONES DE
LAS DISCONTINUIDADES
INDICACIONES DE
LAS DISCONTINUIDADES
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INDICACIONES DE
LAS DISCONTINUIDADES
5. Indicaciones difusas.
a. porosidad esparcida.
b. revelado excesivo.
c. Vacíos o contracciones que salen a la superficie.
d. grietas anchas.
INDICACIONES DE
LAS DISCONTINUIDADES
INDICACIONES FALSAS
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INDICACIONES FALSAS
INDICACIONES FALSAS
INDICACIONES FALSAS
14
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INDICACIONES FALSAS
INDICACIONES NO RELEVANTES
15
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INDICACIONES NO RELEVANTES
2. Conexiones remachadas.
INDICACIONES RELEVANTES
INDICACIONES RELEVANTES
16
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17
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CONTROL DE
PROCESO
LECCION 13
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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5. Viscosidad.
6. Punto de inflamación.
7. Toxicidad.
NIVEL II
MUESTREO DE CONTROL
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
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.
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
NIVEL II
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BLOQUES DE REFERENCIA DE
ALUMINIO
BLOQUES DE REFERENCIA DE
ALUMINIO
BLOQUES DE REFERENCIA DE
ALUMINIO
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BLOQUES DE REFERENCIA DE
ALUMINIO
BLOQUES DE REFERENCIA DE
ALUMINIO
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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PANELES DE PRUEBA
ANODIZADOS Y PLATEADOS
UTILIZACION DE LOS
PANELES PLATEADOS
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4. Lavabilidad
5. Decoloración de las tintas penetrantes
( chequeado por una prueba de
comparación sencilla).
a. La prueba de luminosidad de
los fluorescentes es una
comparación entre una muestra
de control y el penetrante de
los tanques.
b. Las muestras son
alternativamente leídas en el
fluorometro y los resultados
comparados.
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PRUEBAS A LOS
EMULSIFICADORES
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PRUEBAS EN LOS
REVELADORES SECOS
PRUEBAS EN LOS
REVELADORES SECOS
PRUEBAS EN LOS
REVELADORES SECOS
a. Agrietamiento.
b. Suciedad.
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PRUEBA REVELADORES
HUMEDOS
PRUEBA REVELADORES
HUMEDOS
3. Si las lecturas del hidrometro difieren de los
requisitos del fabricante, se deberá adicionar polvo
o agua en las cantidades suficientes para obtener la
concentración dentro de los limites aceptables.
PRUEBA REVELADORES
HUMEDOS
4. Una pequeña placa de prueba lisa sin indicaciones
es sumergida en el tanque de revelado y examinada
visualmente para detectar la suciedad.
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PRUEBA REVELADORES
HUMEDOS
5. El tanque y la placa son chequeados para ver la
fluorescencia o la contaminación con penetrante
bajo la radiación ultravioleta. Si cualquier condición
es evidente se descarta el revelador.
HIDROMETRO TIPICO
Balasto
Tallo
Escala
Cuerpo
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ARTICULO 6
SECCION V
LECCION 14
INFORMACION GENERAL
(T-620)
Los líquidos penetrantes son un método efectivo para
detectar discontinuidades que estén abiertas a la
superficie de metales no porosos
PROCEDIMIENTO
(T-621)
Se requiere de un procedimiento escrito que incluya todas
las variables indicadas en la Tabla T-621
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CONTROL DE CONTAMINANTES
(T-641)
T-642 LIMPIEZA DE LA
SUPERFICIE
Antes de efectuar los líquidos penetrantes, la
superficie a examinar mas 1 pulg. (25 mm) a
cada lado debe estar libre de polvo, grasa,
oxido, fundente, salpicaduras, pintura, aceite y
cualquier otro material extraño que pueda
interferir con el examen
T-642 LIMPIEZA DE LA
SUPERFICIE
la preparación de la superficie es una variable esencial,
se puede usar cualquier tipo de limpiador , solvente,
removedor de pintura, los solventes deben cumplir con
los requisitos de control de contaminantes
El desengrasado con vapor o la limpieza ultrasónica
pueden utilizarse
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T-651 TÉCNICAS
LAVABLES
VISIBLE
CON AGUA
POST-
EMULSIFICABLES
FLUORESCENT
ES
REMOVIBLES CON
SOLVENTE
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T-653 TÉCNICAS NO
ESTANDAR
T-654 RESTRICCIONES
TÉCNICAS
el examen con líquidos penetrantes fluorescentes no
debe seguir después del examen con líquidos
penetrantes visibles
mezcla de los materiales de diferente familia o de
diferente fabricante no esta permitida
una re-prueba con penetrantes lavables con agua puede
causar la perdida de indicaciones marginales debido a la
contaminación
T-660 CALIBRACIÓN
los medidores de luz ya sean visibles o fluorescentes (luz negra)
deben calibrase cada año o cuando el medidor sea reparado.
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T-672 TIEMPO DE
PENETRACIÓN
El tiempo de penetración es critico y por lo tanto es una
variable esencial ver la tabla T-672
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T-675 REVELADO
El método de aplicación del revelador es variable esencial
• el revelador seco se puede aplicar con brocha, o soplado del polvo.
• el revelador húmedo si es acuoso se puede aplicar por inmersión,
spray, o brocha, para el secado no exceder de 125°f en la parte
• el revelador 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-675.3 TIEMPO DE
REVELADO
el tiempo de revelado inicia desde que se aplica el
revelador para los reveladores secos, y cuando la
capa de revelador se ha secado para los reveladores
húmedos
la interpretación final solo debe realizarse en el rango
de tiempo indicado en T-676.1
T-676 - ILUMINACIÓN
La intensidad de luz mínima es variable
esencial
T-676 - ILUMINACIÓN
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T-676- INTERPRETACIÓN
T-680 EVALUACIÓN
CRITERIO DE ACEPTACION
SECCION I &VIII DIV. 1
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CRITERIO DE ACEPTACION
ASME B-31.1
T-677 POST-LIMPIEZA
T-690 DOCUMENTOS
9
2013 SECTION V ARTICLE 1
SUBSECTION A
NONDESTRUCTIVE METHODS OF
EXAMINATION
ARTICLE 1
GENERAL REQUIREMENTS
T-110 SCOPE (e) For those documents that directly reference this Ar-
ticle for the qualification of NDE personnel, the qualifica-
(a) This Section of the Code contains requirements and tion shall be in accordance with their employer’s written
methods for nondestructive examination (NDE), which are practice which must be in accordance with one of the fol-
Code requirements to the extent they are specifically re- lowing documents:
ferenced and required by other Code Sections or referen-
(1) SNT-TC-1A,3 Personnel Qualification and Certifi-
cing document. These NDE methods are intended to detect
cation in Nondestructive Testing; or
surface and internal imperfections in materials, welds,
fabricated parts, and components. They include radio- (2) ANSI/ASNT CP-189,3 ASNT Standard for Qualifi-
graphic examination, ultrasonic examination, liquid pene- cation and Certification of Nondestructive Testing
trant examination, magnetic particle examination, Personnel
eddy current examination, visual examination, leak (f) National or international central certification pro-
testing, and acoustic emission examinatio n. See grams, such as the ASNT Central Certification Program
Nonmandatory Appendix A of this Article for a listing of (ACCP) or ISO 9712:2012-based programs, may be alter-
common imperfections and damage mechanisms, and natively used to fulfill the training, experience, and exam-
the NDE methods that are generally capable of detecting ination requirements of the documents listed in (e) as
them. specified in the employer’s written practice.
(b) For general terms such as Inspection, Flaw, Disconti- (g) When the referencing Code Section does not specify
nuity, Evaluation, etc., refer to Mandatory Appendix I. qualifications or does not reference directly Article 1 of
this Section, qualification may simply involve a personnel
demonstration to show that the personnel performing the
ð13Þ T-120 GENERAL nondestructive examinations are competent to do so in ac-
(a) Subsection A describes the methods of nondestruc- cordance with the Manufacturer’s established procedures.
tive examination to be used if referenced by other Code (h) The user of this Article is responsible for the qualifi-
Sections or referencing documents. cation and certification of NDE Personnel in accordance
(b) Subsection B lists Standards covering nondestruc- with the requirements of this Article. The Code User’s 4
tive examination methods which have been accepted as Quality Program shall stipulate how this is to be accom-
standards. These standards are nonmandatory unless spe- plished. Qualifications in accordance with a prior edition
cifically referenced in whole or in part in Subsection A or of SNT-TC-1A, or CP-189 are valid until recertification. Re-
as indicated in other Code Sections or referencing certification or new certification shall be in accordance
document. with the edition of SNT-TC-1A or CP-189 specified in Foot-
(c) Any reference to a paragraph of any Article in note. 3
Subsection A of this Section includes all of the applicable (i) Limited certification of nondestructive examination
rules in the paragraph.1 In every case, reference to a para- personnel who do not perform all of the operations of a
graph includes all the subparagraphs and subdivisions un- nondestructive method that consists of more than one op-
der that paragraph. eration, or who perform nondestructive examinations of
(d) Reference to a standard contained in Subsection B is limited scope, may be based on fewer hours of training
mandatory only to the extent specified.2 and experience than recommended in SNT-TC-1A or
1
ARTICLE 1 2013 SECTION V
CP-189. Any limitations or restrictions placed upon a per- is capable of detecting discontinuities under the special
son’s certification shall be described in the written prac- conditions equal to the capabilities of the method when
tice and on the certification. used under more general conditions. These special proce-
(j) Either U.S. Customary Units or SI Units may be used dures shall be submitted to the Inspector for acceptance
for compliance with all requirements of this edition, but when required by the referencing Code Section, and shall
one system shall be used consistently throughout for all be adopted as part of the Manufacturer’s quality control
phases of construction. program.
(1) Either the U.S. Customary Units or SI Units that (c) When a referencing Code Section requires an exam-
are listed in Mandatory Appendix II are identified in the ination to be performed in accordance with the require-
text, or are identified in the nomenclature for equations ments of this Section, it shall be the responsibility of the
shall be used consistently for all phases of construction Manufacturer, fabricator, or installer to establish nondes-
(e.g., materials, design, fabrication, and reports). Since va- tructive examination procedures and personnel qualifica-
lues in the two systems are not exact equivalents, each tion and certification procedures conforming to the
system shall be used independently of the other without referenced requirements.
mixing U.S. Customary Units and SI Units. (d) When qualification of the written examination pro-
(2) When SI Units are selected, U.S. Customary values cedure is required by the referencing Code Section, it shall
in referenced specifications that do not contain SI Units be qualified by performing a demonstration examination
shall be converted to SI values to at least three significant which shall be performed
figures for use in calculations and other aspects of (1) under the control and supervision of a Level III
construction. Examiner who is qualified and certified for performing
the examination method and technique specified by the
procedure, and shall be witnessed by the Inspector. The
T-130 EQUIPMENT supervising Level III may be an employee of the qualifying
organization or a subcontractor organization.
It is the responsibility of the Code User to ensure that (2) on a minimum of one test specimen having flaws
the examination equipment being used conforms to the re- whose size, location, orientation, quantity, and characteri-
quirements of this Code Section. zation have been determined prior to the demonstration
and are known only by the supervising Level III Examiner.
(-a) The maximum acceptable flaw size, required
ð13Þ T-150 PROCEDURE flaw orientation, and minimum number of flaws shall be
(a) When required by the referencing Code Section, all as specified by the referencing Code Section.
nondestructive examinations performed under this Code (-b) Natural flaws are preferred over artificial
Section shall be performed following a written procedure. flaws whenever possible.
A procedure demonstration shall be performed to the sa- (3) by a Level II or Level III Examiner (other than the
tisfaction of the Inspector. When required by the referen- supervising Level III) who is qualified and certified to per-
cing Code Section, a personnel demonstration may be used form the examination method and technique specified by
to verify the ability of the examiner to apply the examina- the written procedure.
tion procedure. The examination procedure shall comply The procedure shall be considered qualified when the
with the applicable requirements of this Section for the supervising Level III and the Inspector are satisfied that
particular examination method. Written procedures shall indications produced by the demonstrated procedure ef-
be made available to the Inspector on request. At least fectively reveal the size, location, orientation, quantity,
one copy of each procedure shall be readily available to and characterization of the flaws known to be present in
the Nondestructive Examination Personnel for their refer- the examined test specimen.
ence and use. The qualification demonstration shall be documented
(b) The nondestructive examination methods and tech- as required by the referencing Code Section and by this
niques included in this Section are applicable to most geo- Section, as set forth in the applicable Article for the exam-
metric configurations and materials encountered in ination method and the applicable Appendix for the speci-
fabrication under normal conditions. Whenever special fied examination technique. The qualification document
configurations or materials require modified methods shall be annotated to indicate qualification of the written
and techniques, the Manufacturer shall develop special procedure, and identify the examined test specimen. The
procedures which are equivalent or superior to the meth- name and/or identity and signature of the supervising Le-
ods and techniques described in this Code Section, and vel III and the witnessing Inspector shall be added to indi-
which are capable of producing interpretable examination cate their acceptance of the procedure qualification.
results under the special conditions. Such special proce-
dures may be modifications or combinations of methods
described or referenced in this Code Section. A procedure
demonstration shall be performed to verify the technique
2
2013 SECTION V ARTICLE 1
3
ARTICLE 1 2013 SECTION V
MANDATORY APPENDIX I
GLOSSARY OF TERMS FOR NONDESTRUCTIVE EXAMINATION
4
2013 SECTION V ARTICLE 1
NONMANDATORY APPENDIX A
IMPERFECTION VS TYPE OF NDE METHOD
A-110 SCOPE differences from the degree of effectiveness implied in the table.
For service-induced imperfections, accessibility and other condi-
Table A-110 lists common imperfections and the NDE tions at the examination location are also significant factors that
methods that are generally capable of detecting them. must be considered in selecting a particular NDE method. In ad-
dition, Table A-110 must not be considered to be all inclusive;
CAUTION: Table A-110 should be regarded for general guidance there are several NDE methods/techniques and imperfections
only and not as a basis for requiring or prohibiting a particular not listed in the table. The user must consider all applicable con-
type of NDE method for a specific application. For example, ma- ditions when selecting NDE methods for a specific application.
terial and product form are factors that could result in
Table A-110
Imperfection vs Type of NDE Method
Sub-surf. [Note
Surface [Note (1)] (2)] Volumetric [Note (3)]
VT PT MT ET RT UTA UTS AE UTT
Service-Induced Imperfections
Abrasive Wear (Localized) ⦿ ⊛ ⊛ ... ⦿ ⊛ ⊛ ... ⊛
Baffle Wear (Heat Exchangers) ⦿ ... ... ⊛ ... ... ... ... ...
Corrosion-Assisted Fatigue Cracks ⦾ ⊛ ⦿ ... ⦾ ⦿ ... ⦿ ...
Corrosion
-Crevice ⦿ ... ... ... ... ... ... ... ⦾
-General / Uniform ... ... ... ⦾ ⊛ ... ⊛ ... ⦿
-Pitting ⦿ ⦿ ⦾ ... ⦿ ⦾ ⦾ ⊛ ⦾
-Selective ⦿ ⦿ ⦾ ... ... ... ... ... ⦾
Creep (Primary)[Note (4)] ... ... ... ... ... ... ... ... ...
Erosion ⦿ ... ... ... ⦿ ⦾ ⊛ ... ⊛
Fatigue Cracks ⦾ ⦿ ⦿ ⊛ ⊛ ⦿ ... ⦿ ...
Fretting (Heat Exchanger Tubing) ⊛ ... ... ⊛ ... ... ... ... ⊛
Hot Cracking ... ⊛ ⊛ ... ⊛ ⦾ ... ⊛
Hydrogen-Induced Cracking ... ⊛ ⊛ ... ⦾ ⊛ ... ⊛ ...
Intergranular Stress-Corrosion Cracks ... ... ... ... ... ⦾ ... ... ...
Stress-Corrosion Cracks (Transgranular) ⦾ ⊛ ⦿ ⦾ ⊛ ⊛ ... ⊛ ...
Welding Imperfections
Burn Through ⦿ ... ... ... ⦿ ⊛ ... ... ⦾
Cracks ⦾ ⦿ ⦿ ⊛ ⊛ ⦿ ⦾ ⦿ ...
Excessive/Inadequate Reinforcement ⦿ ... ... ... ⦿ ⊛ ⦾ ... ⦾
Inclusions (Slag/Tungsten) ... ... ⊛ ⊛ ⦿ ⊛ ⦾ ⦾ ...
Incomplete Fusion ⊛ ... ⊛ ⊛ ⊛ ⦿ ⊛ ⊛ ...
Incomplete Penetration ⊛ ⦿ ⦿ ⊛ ⦿ ⦿ ⊛ ⊛ ...
Misalignment ⦿ ... ... ... ⦿ ⊛ ... ... ...
Overlap ⊛ ⦿ ⦿ ⦾ ... ⦾ ... ... ...
Porosity ⦿ ⦿ ⦾ ... ⦿ ⊛ ⦾ ⦾ ...
Root Concavity ⦿ ... ... ... ⦿ ⊛ ⦾ ⦾ ⦾
Undercut ⦿ ⊛ ⊛ ⦾ ⦿ ⊛ ⦾ ⦾ ...
Product Form Imperfections
Bursts (Forgings) ⦾ ⦿ ⦿ ⊛ ⊛ ⊛ ⊛ ⦿ ...
Cold Shuts (Castings) ⦾ ⦿ ⦿ ⦾ ⦿ ⊛ ⊛ ⦾ ...
Cracks (All Product Forms) ⦾ ⦿ ⦿ ⊛ ⊛ ⊛ ⦾ ⦿
Hot Tear (Castings) ⦾ ⦿ ⦿ ⊛ ⊛ ⊛ ⦾ ⦾ ...
Inclusions (All Product Forms) ... ... ⊛ ⊛ ⦿ ⊛ ⦾ ⦾ ...
5
ARTICLE 1 2013 SECTION V
Table A-110
Imperfection vs Type of NDE Method (Cont'd)
Sub-surf. [Note
Surface [Note (1)] (2)] Volumetric [Note (3)]
VT PT MT ET RT UTA UTS AE UTT
Lamination (Plate, Pipe) ⦾ ⊛ ⊛ ... ... ⦾ ⦿ ⦾ ⦿
Laps (Forgings) ⦾ ⦿ ⦿ ⦾ ⊛ ... ⦾ ⦾
Porosity (Castings) ⦿ ⦿ ⦾ ... ⦿ ⦾ ⦾ ⦾ ...
Seams (Bar, Pipe) ⦾ ⦿ ⦿ ⊛ ⦾ ⊛ ⊛ ⦾ ...
Legend:
AE — Acoustic Emission UTA — Ultrasonic Angle
⦿ — All or most standard techniques will detect this
Beam
imperfection under all or most conditions.
ET — Electromagnetic UTS — Ultrasonic Straight
⊛ — One or more standard technique(s) will detect this
(Eddy Current) Beam
imperfection under certain conditions.
MT — Magnetic Particle UTT — Ultrasonic
⦾ — Special techniques, conditions, and/or personnel
Thickness Measurements
qualifications are required to detect this imperfection.
PT — Liquid Penetrant VT — Visual
RT — Radiography
GENERAL NOTE: Table A-110 lists imperfections and NDE methods that are capable of detecting them. It must be kept in mind that this
table is very general in nature. Many factors influence the detectability of imperfections. This table assumes that only qualified personnel
are performing nondestructive examinations and good conditions exist to permit examination (good access, surface conditions, cleanli-
ness, etc.).
NOTES:
(1) Methods capable of detecting imperfections that are open to the surface only.
(2) Methods capable of detecting imperfections that are either open to the surface or slightly subsurface.
(3) Methods capable of detecting imperfections that may be located anywhere within the examined volume.
(4) Various NDE methods are capable of detecting tertiary (3rd stage) creep and some, particularly using special techniques, are capable
of detecting secondary (2nd stage) creep. There are various descriptions/definitions for the stages of creep and a particular descrip-
tion/definition will not be applicable to all materials and product forms.
6
2013 SECTION V ARTICLE 6
ARTICLE 6
LIQUID PENETRANT EXAMINATION
163
ARTICLE 6 2013 SECTION V
Table T-621
Requirements of a Liquid Penetrant Examination Procedure
Nonessential
Requirement Essential Variable Variable
Identification of and any change in type or family group of penetrant materials including X ...
developers, emulsifiers, etc.
Surface preparation (finishing and cleaning, including type of cleaning solvent) X . . .
Method of applying penetrant X . . .
Method of removing excess surface penetrant X . . .
Hydrophilic or lipophilic emulsifier concentration and dwell time in dip tanks and agitation time X . . .
for hydrophilic emulsifiers
Hydrophilic emulsifier concentration in spray applications X . ..
Method of applying developer X . ..
Minimum and maximum time periods between steps and drying aids X . ..
Decrease in penetrant dwell time X . ..
Increase in developer dwell time (Interpretation Time) X . ..
Minimum light intensity X . ..
Surface temperature outside 40°F to 125°F (5°C to 52°C) or as previously qualified X . ..
Performance demonstration, when required X . ..
Personnel qualification requirements ... X
Materials, shapes, or sizes to be examined and the extent of examination ... X
Post-examination cleaning technique ... X
164
2013 SECTION V ARTICLE 6
air inlet to preclude contamination of the penetrant by oil, the mixture shall be removed by immersing in or rinsing
water, dirt, or sediment that may have collected in the with water. The temperature and pressure of the water
lines. shall be as recommended by the manufacturer.
NOTE: Additional information may be obtained from SE-165.
T-672 PENETRATION (DWELL) TIME
T-673.3 Solvent Removable Penetrants. Excess sol-
Penetration (dwell) time is critical. The minimum pene- vent removable penetrants shall be removed by wiping
tration time shall be as required in Table T-672 or as qua- with a cloth or absorbent paper, repeating the operation
lified by demonstration for specific applications. until most traces of penetrant have been removed. The re-
maining traces shall be removed by lightly wiping the sur-
T-673 EXCESS PENETRANT REMOVAL face with cloth or absorbent paper moistened with
After the specified penetration (dwell) time has elapsed, solvent. To minimize removal of penetrant from disconti-
any penetrant remaining on the surface shall be removed, nuities, care shall be taken to avoid the use of excess sol-
taking care to minimize removal of penetrant from vent. Flushing the surface with solvent, following the
discontinuities. application of the penetrant and prior to developing,
is prohibited.
T-673.1 Water-Washable Penetrants. Excess water-
washable penetrant shall be removed with a water spray. T-674 DRYING AFTER EXCESS PENETRANT
The water pressure shall not exceed 50 psi (350 kPa), and REMOVAL
the water temperature shall not exceed 110°F (43°C). (a) For the water washable or post-emulsifying techni-
T-673.2 Post-Emulsification Penetrants. que, the surfaces may be dried by blotting with clean ma-
(a) Lipophilic Emulsification. After the required pene- terials o r by using circulating air, provided the
trant dwell time, the excess surface penetrant shall be temperature of the surface is not raised above 125°F
emulsified by immersing or flooding the part with the (52°C).
emulsifier. Emulsification time is dependent on the type (b) For the solvent removable technique, the surfaces
of emulsifier and surface condition. The actual emulsifica- may be dried by normal evaporation, blotting, wiping, or
tion time shall be determined experimentally. After emul- forced air.
sification, the mixture shall be removed by immersing in
or rinsing with water. The temperature and pressure of T-675 DEVELOPING
the water shall be as recommended by the manufacturer. The developer shall be applied as soon as possible after
(b) Hydrophilic Emulsification. After the required pene- penetrant removal; the time interval shall not exceed that
trant dwell time and prior to emulsification, the parts shall established in the procedure. Insufficient coating thick-
be pre-rinsed with water spray using the same process as ness may not draw the penetrant out of discontinuities;
for water-washable penetrants. Pre-rinsing time shall not conversely, excessive coating thickness may mask
exceed 1 min. After pre-rinsing, the excess surface pene- indications.
trant shall be emulsified by immersing in or spraying with With color contrast penetrants, only a wet developer
hydrophilic emulsifier. Bath concentration shall be as re- shall be used. With fluorescent penetrants, a wet or dry
commended by the manufacturer. After emulsification, developer may be used.
Table T-672
Minimum Dwell Times
Dwell Times [Note (1)]
(minutes)
Material Form Type of Discontinuity Penetrant
Aluminum, magnesium, steel, brass and bronze, Castings and welds Cold shuts, porosity, lack of fusion, 5
titanium and high- temperature alloys cracks (all forms)
Wrought materials — Laps, cracks 10
extrusions, 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.
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ARTICLE 6 2013 SECTION V
T-675.1 Dry Developer Application. Dry developer ensure adequate sensitivity during the examination and
shall be applied only to a dry surface by a soft brush, hand evaluation of indications. The light source, technique used,
powder bulb, powder gun, or other means, provided the and light level verification is required to be demonstrated
powder is dusted evenly over the entire surface being one time, documented, and maintained on file.
examined.
T-676.4 Fluorescent Penetrants. With fluorescent
T-675.2 Wet Developer Application. Prior to apply- penetrants, the process is essentially the same as in
ing suspension type wet developer to the surface, the de- T-676.3, with the exception that the examination is per-
veloper must be thoroughly agitated to ensure adequate formed using an ultraviolet light, called black light. The ex-
dispersion of suspended particles. amination shall be performed as follows:
(a) Aqueous Developer Application. Aqueous developer (a) It shall be performed in a darkened area.
may be applied to either a wet or dry surface. It shall be (b) Examiners shall be in a darkened area for at least
applied by dipping, brushing, spraying, or other means, 5 min prior to performing examinations to enable their
provided a thin coating is obtained over the entire surface eyes to adapt to dark viewing. Glasses or lenses worn by
being examined. Drying time may be decreased by using examiners shall not be photosensitive.
warm air, provided the surface temperature of the part (c) B l a c k l i g h t s s h a l l a c h i e v e a m i n i m u m o f
is not raised above 125°F (52°C). Blotting is not 1000 μW/cm2 on the surface of the part being examined
permitted. throughout the examination.
(b) Nonaqueous Developer Application. Nonaqueous de- (d) Reflectors and filters should be checked and, if ne-
velopers shall be applied by spraying, except where safety cessary, cleaned prior to use. Cracked or broken filters
or restricted access preclude it. Under such conditions, de- shall be replaced immediately.
veloper may be applied by brushing. For water-washable
(e) The black light intensity shall be measured with a
or post-emulsifiable penetrants, the developer shall be ap-
black light meter prior to use, whenever the light’s power
plied to a dry surface. For solvent removable penetrants,
source is interrupted or changed, and at the completion of
the developer may be applied as soon as practical after ex-
the examination or series of examinations.
cess penetrant removal. Drying shall be by normal
evaporation.
T-677 POST-EXAMINATION CLEANING
T-675.3 Developing Time. Developing time for final
interpretation begins immediately after the application When post-examination cleaning is required by the pro-
of a dry developer or as soon as a wet developer coating cedure, it should be conducted as soon as practical after
is dry. Evaluation and Documentation using a process that does
not adversely affect the part.
T-676 INTERPRETATION
T-676.1 Final Interpretation. Final interpretation
shall be made not less than 10 min nor more than
T-680 EVALUATION
60 min after the requirements of T-675.3 are satisfied. If (a) All indications shall be evaluated in terms of the ac-
bleed-out does not alter the examination results, longer ceptance standards of the referencing Code Section.
periods are permitted. If the surface to be examined is (b) Discontinuities at the surface will be indicated by
large enough to preclude complete examination within bleed-out of penetrant; however, localized surface irregu-
the prescribed or established time, the examination shall larities due to machining marks or other surface condi-
be performed in increments. tions may produce false indications.
T-676.2 Characterizing Indication(s). The type of (c) Broad areas of fluorescence or pigmentation which
discontinuities are difficult to evaluate if the penetrant dif- could mask indications of discontinuities are unaccepta-
fuses excessively into the developer. If this condition oc- ble, and such areas shall be cleaned and reexamined.
curs, close observation of the formation of indication(s)
during application of the developer may assist in charac-
terizing and determining the extent of the indication(s). T-690 DOCUMENTATION
T-676.3 Color Contrast Penetrants. With a color con- T-691 RECORDING OF INDICATIONS
trast penetrant, the developer forms a reasonably uniform
T-691.1 Nonrejectable Indications. Nonrejectable in-
white coating. Surface discontinuities are indicated by
dications shall be recorded as specified by the referencing
bleed-out of the penetrant which is normally a deep red
Code Section.
color that stains the developer. Indications with a light
pink color may indicate excessive cleaning. Inadequate T-691.2 Rejectable Indications. Rejectable indica-
cleaning may leave an excessive background making inter- tions shall be recorded. As a minimum, the type of indica-
pretation difficult. A minimum light intensity of 100 fc tions (linear or rounded), location and extent (length or
(1000 lx) is required on the surface to be examined to diameter or aligned) shall be recorded.
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2013 SECTION V ARTICLE 6
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ARTICLE 6 2013 SECTION V
MANDATORY APPENDIX I
GLOSSARY OF TERMS FOR LIQUID PENETRANT EXAMINATION
(a) The following SE-1316 terms are used in conjunc- solvent removable penetrant: a type of penetrant used
tion with this Article: black light; bleedout; blotting; clean; where the excess penetrant is removed from the surface
contaminant; contrast; developer; developer, aqueous; of the part by wiping using a nonaqueous liquid.
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2013 SECTION V ARTICLE 6
MANDATORY APPENDIX II
CONTROL OF CONTAMINANTS FOR LIQUID PENETRANT
EXAMINATION
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ARTICLE 6 2013 SECTION V
block “A” and the other block “B” for identification in sub-
3 in. (75 mm)
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2013 SECTION V ARTICLE 6
To qualify a procedure for temperatures above 125°F (a) When the single comparator block and photographic
(52°C), the upper and lower temperature limits shall be technique is used, the processing details (as applicable)
established and the procedure qualified at these tempera- described in III-641.1 and III-641.2 apply. The block shall
tures. [As an example, to qualify a procedure for the tem- be thoroughly cleaned between the two processing steps.
perature range 126°F (52°C) to 200°F (93°C), the Photographs shall be taken after processing at the non-
capability of a penetrant to reveal indications on the com- standard temperature and then after processing at the
parator shall be demonstrated at both temperatures.] standard temperature. The indication of cracks shall be
III-641.3 Alternate Techniques for Color Contrast compared between the two photographs. The same criter-
Penetrants. As an alternate to the requirements of ia for qualification as III-641.1 shall apply.
III-641.1 and III-641.2, when using color contrast pene- (b) Identical photographic techniques shall be used to
trants, it is permissible to use a single comparator block make the comparison photographs.
for the standard and nonstandard temperatures and to
make the comparison by photography.
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2.2 ASNT Documents: NOTE 2: Fluorescent penetrant examination shall not follow a visible
penetrant examination unless the procedure has been qualified in accor-
SNT-TC-1A Recommended Practice for Nondestructive dance with 10.2, because visible dyes may cause deterioration or quench-
Testing Personnel Qualification and Certification ing of fluorescent dyes.
ANSI/ASNT CP-189 Standard for Qualification and Certi- 4.2 Processing parameters, such as surface precleaning,
fication of Nondestructive Testing Personnel penetration dwell time and excess penetrant removal meth-
2.3 Military Standard: ods, are dependent on the specific materials used, the nature
of the part under examination (that is, size, shape, surface
MIL-STD-410 Nondestructive Testing Personnel Qualifi- condition, alloy), and type of discontinuities expected.
cation and Certification
2.4 APHA Standard: 5. Significance and Use
429 Method for the Examination of Water and Wastewater 5.1 Liquid penetrant examination methods indicate the
presence, location and, to a limited extent, the nature and
2.5 AIA Standard: magnitude of the detected discontinuities. Each of the vari-
NAS-410 Certification and Qualification of Nondestructive ous methods has been designed for specific uses such as
Test Personnel critical service items, volume of parts, portability or local-
2.6 SAE Standards: ized areas of examination. The method selected will depend
accordingly on the design and service requirements of the
AMS 2644 Inspection Material, Penetrant parts or materials being tested.
QPL-AMS-2644 Qualified Products of Inspection Materi-
als, Penetrant 6. Classification of Penetrant Materials and
Methods
3. Terminology 6.1 Liquid penetrant examination methods and types
3.1 The definitions relating to liquid penetrant examina- are classified in accordance with MIL-I-25135 and
tion, which appear in Terminology E 1316, shall apply to AMS 2644 and listed in Table 1.
the terms used in this standard. 6.2 Fluorescent Penetrant Testing (Type 1) — Fluores-
cent penetrant testing utilizes penetrants that fluoresce bril-
4. Summary of Test Method liantly when excited by black light (UVA). The sensitivity
of fluorescent penetrants depends on their ability to be
4.1 Liquid penetrant may consist of visible or fluores-
retained in the various size discontinuities during pro-
cent material. The liquid penetrant is applied evenly over
cessing, then to bleed out into the developer coating and
the surface being examined and allowed to enter open
produce indications that will fluoresce. Fluorescent indica-
discontinuities. After a suitable dwell time, the excess sur-
tions are many times brighter than their surroundings when
face penetrant is removed. A developer is applied to draw
viewed under black light illumination.
the entrapped penetrant out of the discontinuity and stain
the developer. The test surface is then examined to deter- 6.3 Visible Penetrant Testing (Type 2) — Visible pene-
mine the presence or absence of indications. trant testing uses a penetrant that can be seen in visible
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ARTICLE 24, SE-165 2013 SECTION V
light. The penetrant is usually red, so that the indications 7.3 Emulsifiers:
produce a definite contrast with the white background of 7.3.1 Lipophilic Emulsifiers are oil-miscible liquids
the developer. Visible penetrant indications must be viewed used to emulsify the post-emulsified penetrant on the sur-
under adequate white light. face of the part, rendering it water-washable. The individ-
ual characteristics of the emulsifier and penetrant, and the
7. Types of Materials geometry/surface roughness of the part material contribute
to determining the emulsification time.
7.1 Liquid penetrant examination materials consist of
fluorescent and visible penetrants, emulsifiers (oil-base and 7.3.2 Hydrophilic Emulsifiers are water-miscible liq-
water-base), removers (water and solvent) and developers uids used to emulsify the excess post-emulsified penetrant
(dry powder, aqueous and nonaqueous). A family of liquid on the surface of the part, rendering it water-washable.
penetrant examination materials consists of the applicable These water-base emulsifiers (detergent-type removers) are
penetrant and emulsifier, as recommended by the manufac- supplied as concentrates to be diluted with water and used
turer. Any liquid penetrant, remover, and developer listed as a dip or spray. The concentration, use, and maintenance
in QPL-25135/QPL-AMS2644 can be used, regardless of shall be in accordance with manufacturer’s recommenda-
the manufacturer. Intermixing of penetrants and emulsifiers tions.
from different manufacturers is prohibited. 7.3.2.1 Hydrophilic emulsifiers function by dis-
placing the excess penetrant film from the surface of the
NOTE 3: Refer to 9.1 for special requirements for sulfur, halogen and
alkali metal content. part through detergent action. The force of the water spray
or air/mechanical agitation in an open dip tank provides
NOTE 4: While approved penetrant materials will not adversely affect the scrubbing action while the detergent displaces the film
common metallic materials, some plastics or rubbers may be swollen or of penetrant from the part surface. The individual charac-
stained by certain penetrants.
terisitics of the emulsifier and penetrant, and the geometry
7.2 Penetrants: and surface roughness of the part material contribute to
7.2.1 Post-Emulsifiable Penetrants are insoluble in determining the emulsification time. Emulsification con-
water and cannot be removed with water rinsing alone. centration shall be monitored weekly using a suitable
They are formulated to be selectively removed from the refractometer.
surface using a separate emulsifier. Properly applied and 7.4 Solvent Removers. Solvent removers function by
given a proper emulsification time, the emulsifier combines dissolving the penetrant, making it possible to wipe the
with the excess surface penetrant to form a water-washable surface clean and free of excess penetrant.
mixture, which can be rinsed from the surface, leaving the
surface free of excessive fluorescent background. Proper 7.5 Developers. Developers form a translucent or white
emulsification time must be experimentally established and absorptive coating that aids in bringing the penetrant out
maintained to ensure that over-emulsification does not of the surface discontinuities through blotting action, thus
occur, resulting in loss of indications. increasing the visibility of the indications.
7.2.2 Water-Washable Penetrants are formulated to 7.5.1 Dry Powder Developers. Dry powder devel-
be directly water-washable from the surface of the test opers are used as supplied, that is, free-flowing, non-caking
part, after a suitable penetrant dwell time. Because the powder (see 8.8.2). Care should be taken not to contaminate
emulsifier is “built-in,” water-washable penetrants can be the developer with fluorescent penetrant, as the contami-
washed out of discontinuities if the rinsing step is too long nant developer specks can appear as penetrant indications.
or too vigorous. It is therefore extremely important to 7.5.2 Aqueous Developers. Aqueous developers are
exercise proper control in the removal of excess surface normally supplied as dry powder particles to be either
penetrant to ensure against overwashing. Some penetrants suspended (water suspendable) or dissolved (water soluble)
are less resistant to overwashing than others, so caution in water. The concentration, use, and maintenance shall
should be exercised. be in accordance with manufacturer’s recommendations.
Water soluble developers shall not be used with Type 2
7.2.3 Solvent-Removable Penetrants are formulated
penetrants or Type 1, Method A penetrants.
so that excess surface penetrant can be removed by wiping
until most of the penetrant has been removed. The NOTE 5: Aqueous developers may cause stripping of indications if not
remaining traces should be removed with the solvent properly applied and controlled. The procedure should be qualified in
remover (see 8.6.4). To prevent removal of penetrant from accordance with 10.2.
discontinuities, care should be taken to avoid the use of 7.5.3 Nonaqueous Wet Developers. Nonaqueous wet
excess solvent. Flushing the surface with solvent to remove developers are supplied as suspensions of developer parti-
the excess penetrant is prohibited as the penetrant indica- cles in a nonaqueous solvent carrier ready for use as sup-
tors could easily be washed away. plied. Nonaqueous, wet developers are sprayed on to form
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2013 SECTION V ARTICLE 24, SE-165
a thin coating on the surface of the part when dried. The be clean and dry before the penetrant is applied. If only a
thin coating serves as the developing medium. section of a part, such as a weld, including the heat affected
zone is to be examined, all contaminants shall be removed
NOTE 6: This type of developer is intended for application by spray only.
from the area being examined as defined by the contracting
7.5.4 Liquid Film Developers are solutions or colloi- parties. “Clean” is intended to mean that the surface must
dal suspensions of resins/polymer in a suitable carrier. be free of rust, scale, welding flux, weld spatter, grease,
These developers will form a transparent or translucent paint, oily films, dirt, and so forth, that might interfere
coating on the surface of the part. Certain types of film with the penetrant process. All of these contaminants can
developer may be stripped from the part and retained for prevent the penetrant from entering discontinuities (see
record purposes (see 8.8.4). Annex or Cleaning of Parts and Materials).
8.4.1 Drying After Cleaning — It is essential that the
8. Procedure surface of parts be thoroughly dry after cleaning, since any
8.1 The following processing parameters apply to both liquid residue will hinder the entrance of the penetrant.
fluorescent and visible penetrant testing methods. Drying may be accomplished by warming the parts in
drying ovens, with infrared lamps, forced hot air, or expo-
8.2 Temperature Limits — The temperature of the pene- sure to ambient temperature.
trant materials and the surface of the part to be processed
shall be between 40°F and 125°F (4°C and 52°C) or the NOTE 9: Residues from cleaning processes such as strong alkalies, pick-
ling solutions and chromates, in particular, may adversely react with the
procedure must be qualified at the temperature used as
penetrant and reduce its sensitivity and performance.
described in 10.2.
8.5 Penetrant Application — After the part has been
8.3 Examination Sequence — Final penetrant examina-
cleaned, dried, and is within the specified temperature
tion shall be performed after the completion of all opera-
range, the penetrant is applied to the surface to be examined
tions that could cause surface-connected discontinuities or
so that the entire part or area under examination is com-
operations that could expose discontinuities not previously
pletely covered with penetrant. Application methods
open to the surface. Such operations include, but are not
include dipping, brushing, flooding, or spraying. Small
limited to, grinding, welding, straightening, machining, and
parts are quite often placed in suitable baskets and dipped
heat treating. Satisfactory inspection results can usually be
into a tank of penetrant. On larger parts, and those with
obtained on surfaces in the as-welded, as-rolled, as-cast,
complex geometries, penetrant can be applied effectively
as-forged, or ceramics in the densified condition.
by brushing or spraying. Both conventional and electro-
8.3.1 Surface Treatment — Final penetrant examina- static spray guns are effective means of applying liquid
tion may be performed prior to treatments that can smear penetrants to the part surfaces. Not all penetrant materials
the surface but not by themselves cause surface discontinu- are suitable for electrostatic spray applications, so tests
ities. Such treatments include, but are not limited to, vapor should be conducted prior to use. Electrostatic spray appli-
blasting, deburring, sanding, buffing, sandblasting, or lap- cation can eliminate excess liquid build-up of penetrant on
ping. Performance of final penetrant examination after such the part, minimize overspray, and minimize the amount
surface treatments necessitates that the part(s) be etched of penetrant entering hollow-cored passages which might
to remove smeared metal from the surface prior to testing serve as penetrant reservoirs, causing severe bleedout prob-
unless otherwise agreed by the contracting parties. Note lems during examination. Aerosol sprays are conveniently
that final penetrant examination shall always precede sur- portable and suitable for local application.
face peening.
NOTE 10: With spray applications, it is important that there be proper
NOTE 7: Sand or shot blasting can close discontinuities so extreme ventilation. This is generally accomplished through the use of a properly
care should be taken to avoid masking discontinuities. under certain designed spray booth and exhaust system.
circumstances, however, grit blasting with certain air pressures and/or
8.5.1 Penetrant Dwell Time — After application,
mediums may be acceptable without subsequent etching when agreed by
the contracting parties. allow excess penetrant to drain from the part (care should
be taken to prevent pools of penetrant from forming on
NOTE 8: Surface preparation of structural or electronic ceramics for the part), while allowing for proper penetrant dwell time
penetrant testing by grinding, sand blasting, and etching is not recom- (see Table 2). The length of time the penetrant must remain
mended because of the potential for damage.
on the part to allow proper penetration should be as recom-
8.4 Precleaning — The success of any penetrant exami- mended by the penetrant manufacturer. Table 2, however,
nation procedure is greatly dependent upon the surrounding provides a guide for selection of penetrant dwell times for
surface and discontinuity being free of any contaminant a variety of materials, forms, and types of discontinuity.
(solid or liquid) that might interfere with the penetrant Unless otherwise specified, the dwell time shall not exceed
process. All parts or areas of parts to be examined must the maximum recommended by the manufacturer.
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ARTICLE 24, SE-165 2013 SECTION V
TABLE 2
RECOMMENDED MINIMUM DWELL TIMES
Aluminum, magnesium, steel, brass castings and welds cold shuts, porosity, lack of fusion, 5 10
and bronze, titanium and high- cracks (all forms)
temperature alloys
wrought materials — extrusions, laps, cracks (all forms) 10 10
forgings, plate
Carbide-tipped tools lack of fusion, porosity, cracks 5 10
Plastic all forms cracks 5 10
Glass all forms cracks 5 10
Ceramic all forms cracks, porosity 5 10
A
For temperature range from 50 to 100°F (10 to 38°C) for fluorescent penetrants and 50 to 125°F (10 to 52°C) for visible penetrant.
B
Maximum penetrant dwell time in accordance with 8.5.2.
C
Development time begins as soon as wet developer coating has dried on surface of parts (recommended minimum). Maximum development
time in accordance with 8.8.6.
8.6 Penetrant Removal emulsifier shall not be agitated while being immersed. After
8.6.1 Water Washable (Method A): application of the emulsifier, the parts shall be drained and
positioned in a manner that prevents the emulsifier from
8.6.1.1 Removal of Excess Penetrants — After the
pooling on the part(s).
required penetrant dwell time, the excess penetrant on the
surface being examined must be removed with water. It 8.6.2.2 Emulsification Time — The emulsification
can be removed manually by a coarse spray or wiping the time begins as soon as the emulsifier is applied. The length
aprt surface with a dampened rag, automatic or of time that the emulsifier is allowed to remain on a part
semi-automatic water-spray equipment, or by water immer- and in contact with the penetrant is dependent on the type
sion. For immersion rinsing, parts are completely immersed of emulsifier employed and the surface roughness. Nominal
in the water bath with air or mechanical agitation. emulsification time should be as recommended by the man-
(a) The temperature of the water shall be maintained ufacturer. The actual emulsification time must be deter-
within the range of 50°F to 100°F (10°C to 38°C). mined experimentally for each specific application. The
(b) Spray-rinse water pressure should not exceed 40 psi surface finish (roughness) of the part is a significant factor
(275 kPa). When hydro-air pressure spray guns are used, in the selection of and in the emulsification time of an
the air pressure should not exceed 25 psi (172 kPa). emulsifier. Contact time shall be kept to the minimum time
to obtain an acceptable background and shall not exceed
NOTE 11: Overwashing should be avoided. Excessive washing can cause three minutes.
penetrant to be washed out of discontinuities. With fluorescent penetrant
methods perform the rinsing operation under black light so that it can 8.6.2.3 Post Rinsing — Effective post rinsing of the
be determined when the surface penetrant has been adequately removed. emulsified penetrant from the surface can be accomplished
8.6.1.2 Removal by Wiping (Method C) — After using either manual, semi-automated, or automated water
the required penetrant dwell time, the excess penetrant is immersion or spray equipment or combinations thereof.
removed by wiping with a dry, clean, lint-free cloth/towel. 8.6.2.4 Immersion — For immersion post rinsing,
Then use a clean lint-free cloth/towel lightly moistened parts are completely immersed in the water bath with air
with water or solvent to remove the remaining traces of or mechanical agitation. The amount of time the part is in
surface penetrant as determined by examination under the bath should be the minimum required to remove the
black light for fluorescent methods and visible light for emulsified penetrant. In addition, the temperature range of
visible methods. the water should be 50°F to 100°F (10°C to 38°C). Any
8.6.2 Lipophilic Emulsification (Method B): necessary touch-up rinse after an immersion rinse shall
8.6.2.1 Application of Lipophilic Emulsifier — meet the requirements of 8.6.2.5.
After the required penetration dwell time, the excess pene- 8.6.2.5 Spray Post Rinsing — Effective post rins-
trant on the part must be emulsified by immersing or flood- ing following emulsification can also be accomplished by
ing the parts with the required emulsifier (the emulsifier either manual or automatic water spray rinsing. The water
combines with the excess surface penetrant and makes the temperature shall be between 50°F and 100°F (10°C and
mixture removable by water rinsing). Lipophililc emulsifier 38°C). The water spray pressure shall not exceed 40 psi
shall not be applied by spray or brush and the part or (275 kPa) when manual spray guns are used. When
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2013 SECTION V ARTICLE 24, SE-165
hydro-air pressure spray guns are used, the air pressure emulsify the residual penetrant on part surfaces to render
should not exceed 25 psi (172 kPa). it water-washable. The concentration of the emulsifier for
8.6.2.6 Rinse Effectiveness — If the emulsification spray application should be in accordance with the manu-
and final rinse step is not effective, as evidenced by exces- facturer’s recommendations, but it shall not exceed 5%.
sive residual surface penetrant after emulsification and rins- The water spray pressure should be less than 40 psi
ing, thoroughly reclean and completely reprocess the part. (275 kPa). Contact with the emulsifier shall be kept to the
minimum time to obtain an acceptable background and
8.6.3 Hydrophilic Emulsification (Method D): shall not exceed two minutes. The water temperature shall
8.6.3.1 Application of Hydrophilic Remover — be maintained between 50°F and 100°F (10°C and 38°C).
Following the required penetration dwell time, the parts 8.6.3.6 Post-Rinsing of Hydrophilic Emulsified
may be be prerinsed with water prior to application of the Parts — Effective post-rinsing of emulsified penetrant from
hydrophilic emulsifier. This prerinse allows for the removal the surface can be accomplished using either manual or
of excess surface penetrant from the parts prior to emulsifi- automated water spray, water immersion, or combinations
cation so as to minimize penetrant contamination in the thereof. The total rinse time shall not exceed two minutes
hydrophilic emulsifier bath, thereby extending its life. It regardless of the number of rinse methods used.
is not necessary to prerinse a part if a spray application of
8.6.3.7 Immersion Post-Rinsing — If an agitated
emulsifier is used.
immersion rinse is used, the amount of time the part(s) is
8.6.3.2 Prerinsing Controls — Effective prerinsing (are) in the bath shall be the minimum required to remove
is accomplished by manual, semi-automated, or automated the emulsified penetrant and shall not exceed two minutes.
water spray rinsing of the part(s). The water spray pressure In addition, the temperature range of the water shall be
shall not exceed 40 psi (275 kPa) when manual or hydro within 50°F and 100°F (10°C and 38°C). Be aware that a
air spray guns are used. When hydro-air pressure spray touch-up rinse may be necessary after immersion rinse,
guns are used, the air pressure shall not exceed 25 psi but the total wash time still shall not exceed two minutes.
(172 kPa). Water free of contaminants that could clog spray 8.6.3.8 Spray Post-Rinsing — Effective post-rins-
nozzles or leave a residue on the part(s) is recommended. ing following emulsification can also be accomplished by
8.6.3.3 Application of Emulsifier — The residual manual, semi-automatic, or automatic water spray. The
surface penetrant on part(s) must be emulsified by immers- water spray pressure shall not exceed 40 psi (275kPa) when
ing the part(s) in an agitated hydrophilic emulsifier bath manual or hydro air spray guns are used. When hydro-air
or by spraying the part(s) with water/emulsifier solutions pressure spray guns are used, the air pressure shall not
thereby rendering the remaining residual surface penetrant exceed 25 psi (172 kPa). The water temperature shall be
water-washable for the final rinse station. The emulsifica- between 50°F and 100°F (10°C and 38°C). The spray rinse
tion time begins as soon as the emulsifier is applied. The time shall be less than two minutes, unless otherwise spec-
length of time that the emulsifier is allowed to remain on ified.
a part and in contact with the penetrant is dependent on 8.6.3.9 Rinse Effectiveness — If the emulsification
the type of emulsifier employed and the surface roughness. and final rinse steps are not effective, as evidenced by
The emulsification time should be determined experimen- excessive residual surface penetrant after emulsification
tally for each specific application. The surface finish and rinsing, thoroughly reclean, and completely reprocess
(roughness of the part is a significant factor in determining the part.
the emulsification time necessary for an emulsifier. Contact 8.6.4 Removal of Solvent-Removable Penetrant
emulsification time should be kept to the least possible (Method C) — After the required penetrant dwell time, the
time consistent with an acceptable background and shall
excess penetrant is removed by wiping with a dry, clean,
not exceed two minutes. lint-free cloth/towel. Then use a clean, lint-free cloth/towel
8.6.3.4 Immersion — For immersion application, lightly moistened with solvent remover to remove the
parts shall be completely immersed in the emulsifier bath. remaining traces of surface penetrant. Gently wiping must
The hydrophilic emulsifier concentration shall be as recom- be used to avoid removing penetrant from any discontinu-
mended by the manufacturer and the bath or part shall be ity. On smooth surfaces, an alternate method of removal
gently agitated by air or mechanically throughout the cycle. can be done by wiping with a clean, dry cloth. Flushing
The minimum time to obtain an acceptable background the surface with solvent following the application of the
shall be used, but the dwell time shall not be more than penetrant and prior to developing is prohibited.
two minutes unless approved by the contracting parties. 8.7 Drying — Regardless of the type and method of
8.6.3.5 Spray Application — For spray applica- penetrant used, drying the surface of the part(s) is necessary
tions, all part surfaces should be evenly and uniformly prior to applying dry or nonaqueous developers or follow-
sprayed with a water/emulsifier solution to effectively ing the application of the aqueous developer. Drying time
569
ARTICLE 24, SE-165 2013 SECTION V
will vary with the size, nature, and number of parts being surface has been dried, apply nonaqueous wet developer
processed. by spraying in such a manner as to ensure complete part
8.7.1 Drying Parameters — Components shall be air coverage with a thin, even film of developer. The developer
dried at room temperature or in a drying oven. Oven tem- shall be applied in a manner appropriate to the type of
peratures shall not exceed 160°F (71°C). Drying time shall penetrant being used. For visible dye, the developer must
only be that necessary to adequately dry the part. Compo- be applied thickly enough to provide a contrasting back-
nents shall be removed from the oven after drying. Compo- ground. For fluorescent dye, the developer must be applied
nents should not be placed in the oven with pooled water thinly to produce a translucent covering. Dipping or flood-
or pooled aqueous solutions/suspensions. ing parts with nonaqueous developers is prohibited,
because the solvent action of these types of developers can
8.8 Developer Application — There are various modes flush or dissolve the penetrant from within the discontinu-
of effective application of the various types of developers ities.
such as dusting, immersing, flooding or spraying. The
developer form, the part size, configuration, and surface NOTE 12: The vapors from the volatile solvent carrier in the developer
may be hazardous. Proper ventilation should be provided at all times,
roughness will influence the choice of developer appli-
but especially when the developer is applied inside a closed area.
cation.
8.8.4 Liquid Film Developers — Apply by spraying
8.8.1 Dry Powder Developer (Form A) — Dry pow- as recommended by the manufacturer. Spray parts in such
der developers should be applied immediately after the a manner as to ensure complete part coverage of the area
part is dry in such a manner as to ensure complete coverage being examined with a thin, even film of developer.
of the area of interest. Parts can be immersed in a container
8.8.5 Developing Time — The length of time the
of dry developer or in a fluid bed of dry developer. They
developer is to remain on the part prior to inspection shall
can also be dusted with the powder developer through a
be not less than ten minutes. Developing time begins imme-
hand powder bulb or a conventional or electrostatic powder
diately after the application of dry powder developer or as
gun. It is common and effective to apply dry powder in
soon as the wet (aqueous and nonaqueous) developer coat-
an enclosed dust chamber, which creates an effective and
ing is dry (that is, the water or solvent carrier has evaporated
controlled dust cloud. Other means suited to the size and
to dryness). The maximum permitted developing times
geometry of the specimen may be used, provided the pow-
shall be four hours for dry powder developer (Form A),
der is applied evenly over the entire surface being exam-
two hours for aqueous developer (Forms B and C), and
ined. Excess developer powder may be removed by shaking
one hour for nonaqueous developer (Forms D and E).
or tapping the part, or by blowing with low-pressure dry,
clean, compressed air not exceeding 5 psi (34 kPa). Dry 8.9 Inspection — After the applicable development
developers shall not be used with Type II penetrant. time, perform inspection of the parts under visible or ultra-
8.8.2 Aqueous Developers (Forms B and C) — Water violet light as appropriate. It may be helpful to observe
soluble developers (Form B) are prohibited for use with the bleed out during the development time as an aid in
Type 2 penetrants or Type 1, Method A penetrants. Water interpreting indications.
suspendable developers (Form C) can be used with noth 8.9.1 Ultraviolet Light Examination — Examine parts
Type 1 and Type 2 penetrants. Aqueous developers shall tested with Type 1 fluorescent penetrant under black light
be applied to the part immediately after the excess penetrant in a darkened area. Ambient light shall not exceed 2 fc
has been removed and prior to drying. Aqueous developers (21.5 lx). The measurement shall be made with a suitable
shall be prepared and maintained in accordance with the visible light sensor at the inspection surface.
manufacturer’s instructions and applied in such a manner
NOTE 13: Because the fluorescent constituents in the penetrant will
as to ensure complete, even, part coverage. Aqueous devel- eventually fade with direct exposure to ultraviolet light, direct exposure
opers may be applied by spraying, flowing, or immersing of the part under test to ultraviolet light should be minimized when not
the part in a prepared developer bath. Immerse the parts removing excess penetrant or evaluating indications.
only long enough to coat all of the part surfaces with the 8.9.1.1 Black Light Level Control — Black lights
developer since indications may leach out if the parts are shall produce a minimum light intensity of 1000 W/cm2,
left in the bath too long. After the parts are removed from at a distance of 15 in. (38.1 cm). The intensity should be
the developer bath, allow the parts to drain. Drain all excess checked daily to ensure the required output. Reflectors and
developer from recesses and trapped sections to eliminate filters should also be checked daily for cleanliness and
pooling of developer, which can obscure discontinuities. integrity. Cracked or broken ultraviolet filters shall be
Dry the parts in accordance with 8.7. The dried developer replaced immediately. Since a drop in line voltage can
coating appears as a translucent or white coating on the part. cause decreased black light output with consequent incon-
8.8.3 Nonaqueous Wet Developers (Forms D and sistent performance, a constant-voltage transformer should
E) — After the excess penetrant has been removed and the be used when there is evidence of voltage fluctuation.
570
2013 SECTION V ARTICLE 24, SE-165
NOTE 14: Certain high-intensity black lights may emit unacceptable 9. Special Requirements
amounts of visible light, which can cause fluorescent indications to disap-
pear. Care should be taken to use only bulbs suitable for fluorescent
9.1 Impurities:
penetrant testing purposes. 9.1.1 When using penetrant materials on austenitic
8.9.1.2 Black Light Warm-Up — Unless otherwise stainless steels, titanium, nickel-base or other high-temper-
ature alloys, the need to restrict certain impurities such as
specified by the manufacturer, allow the black light to
sulfur, halogens and alkali metals must be considered.
warm up for a minimum of five minutes prior to use or
These impurities may cause embrittlement or corrosion,
measurement of its intensity.
particularly at elevated temperatures. Any such evaluation
8.9.1.3 Visual Adaptation — Personnel examining should also include consideration of the form in which the
parts after penetrant processing shall be in the darkened impurities are present. Some penetrant materials contain
area for at least one minute before examining parts. Longer significant amounts of these impurities in the form of vola-
times may be necessary under some circumstances. Photo- tile organic solvent that normally evaporate quickly and
chromic or tinted lenses shall not be worn during the pro- usually do not cause problems. Other materials may contain
cessing and examination of parts. impurities, which are not volatile and may react with the
part, particularly in the presence of moisture or elevated
8.9.2 Visible Light Examination— Inspect parts tested
temperatures.
with Type 2 visible penetrant under either natural or artifi-
cial visible light. Proper illumination is required to ensure 9.1.2 Because volatile solvents leave the surface
adequate sensitivity of the examination. A minimum light quickly without reaction under normal examination proce-
intensity at the examination surface of 100 fc (1076 lx) is dures, penetrant materials are normally subjected to an
required. evaporation procedure to remove the solvents before the
materials are analyzed for impurities. The residue from
8.9.3 Housekeeping — Keep the examination area this procedure is then analyzed in accordance with Test
free of interfering debris, including fluorescent residues Method D 1552 or Test Method D 129 decomposition
and objects. followed by Test Method D 516, Method B (Turbidimetric
8.9.4 Indication Verification — For Type 1 inspec- Method) for sulfur. The residue may also be analyzed by
tions only, it is common practice to verify indications by Test Method D 808 or Annex A2 on Methods for Measur-
wiping the indication with a solvent-dampened swab or ing Total Chlorine Content in Combustible Liquid Pene-
brush, allowing the area to dry, and redeveloping the area. trant Materials (for halogens other than fluorine) and Annex
Redevelopment time shall be a minimum of ten minutes, A3 on Method for Measuring Total Fluorine Content in
except nonaqueous redevelopment time should be a mini- Combustible Liquid Penetration Materials (for fluorine).
mum of three minutes. If the indication does not reappear, An alternative procedure, Annex A4 on Determination of
the original indication may be considered false. This proce- Anions by Ion Chromatography, provides a single instru-
dure may be performed up to two times for any given mental technique for rapid sequential measurement of com-
original indication. mon anions such as chloride, fluoride, and sulfate. Alkali
metals in the residue are determined by flame photometry,
8.9.5 Evaluation — All indications found during atomic absorption spectrophotometry, or ion chromatogra-
inspection shall be evaluated in accordance with acceptance phy (see ASTM D 4327).
criteria as specified. Referenced Photographs of indications
NOTE 15: Some current standards require impurity levels of sulfur and
are noted in E 433.
halogens to not exceed 1% of any one suspect element. This level,
however, may be unacceptable for some applications, so the actual maxi-
8.10 Post Cleaning — Post cleaning is necessary when
mum acceptable impurity level must be decided between supplier and
residual penetrant or developer could interfere with subse- user on a case by case basis.
quent processing or with service requirements. It is particu-
larly important where residual penetrant testing materials 9.2 Elevated-Temperature Testing — Where penetrant
might combine with other factors in service to produce testing is performed on parts that must be maintained at
corrosion and prior to vapor degreasing or heat treating elevated temperature during examination, special penetrant
the part as these processes can bake the developer onto materials and processing techniques may be required. Such
the part. A suitable technique, such as a simple water rinse, examination requires qualification in accordance with 10.2
water spray, machine wash, solvent soak, or ultrasonic and the manufacturer’s recommendations shall be
cleaning may be employed (see Annex A1 for further infor- observed.
mation on post cleaning). It is recommended that if devel-
oper removal is necessary, it should be carried out as 10. Qualification and Requalification
promptly as possible after examination so that the devel- 10.1 Personal Qualification — When required by cus-
oper does not adhere to the part. tomer, all penetrant testing personnel shall be qualified/
571
ARTICLE 24, SE-165 2013 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
572
2013 SECTION V ARTICLE 24, SE-165
ANNEXES
(Mandatory Information)
573
ARTICLE 24, SE-165 2013 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
enclosed in a shield of steel plate at least 1⁄2 in. (12.7 mm)
125°F (52°C) before applying penetrants.
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
574
2013 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
575
ARTICLE 24, SE-165 2013 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
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2013 SECTION V ARTICLE 24, SE-165
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ARTICLE 24, SE-165 2013 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
1
−
2
ⴛ 10 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%
minimum detectable concentrations are in the range of
to 85% recoveries can be expected with proper technique.
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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2013 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
wicking without melting the wire. A4.4.6 Standard Anion Solutions, 100 mg/L, prepare
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.
581
ARTICLE 24, SE-165 2013 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.
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2013 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.
583