UNIVERSIDAD DE JAÉN
Vicerrectorado de Docencia y Profesorado
Secretariado de Innovación Docente y Formación del Profesorado
MEMORIA FINAL DE PROYECTOS DE INNOVACIÓN DOCENTE
CONVOCATORIA CURSO 2011/2013
DATOS DEL/DE LA SOLICITANTE
Nombre
ANTONIO JOSÉ
Apellidos
MARCHAL INGRAIN
D.N.I.
26024590 K
Centro
Facultad
E-mail
de
amarchal@ujaen.es
Ciencias Teléfono 953212751
Experimentales
Departamento
Categoría
Química Inorgánica y Orgánica
Profesor Titular de Universidad
DATOS DEL PROYECTO
Título
“Hacia el bilingüismo en los grados. El caso de la Asignatura
Operaciones Básicas de Laboratorio II”
II
Línea de actuación
Proyectos para Asignaturas
Titulación/Grado implicado
mplicado/s
Química
Departamento/s implicados
1.- Filología Inglesa
2.- Química Inorgánica y Orgánica
Asignatura/s implicada/s
Operaciones Básicas de Laboratorio II
Curso/s implicado/s
Primero
Nº aproximado de alumnos afectados
100 = 50 /curso
1
UNIVERSIDAD DE JAÉN
Vicerrectorado de Docencia y Profesorado
Secretariado de Innovación Docente y Formación del Profesorado
MEMORIA DEL PROYECTO
Justificación
Ante la escasa oferta de materiales multilingües para la enseñanza y el aprendizaje de conceptos
científico-técnicos
técnicos asociados al trabajo en un laboratorio químico, en el curso 2007 un grupo interdisciplinar de
profesores y profesoras de la Universidad de Jaén decidimos participar
participar en la convocatoria 2007-2009
2007
de
Proyectos del Vicerrectorado de Innovación Docente y Formación del Profesorado con el proyecto titulado
“Material Multimedia Multilingüe de Introducción a un Laboratorio de Química” (PID7A).
La concesión del citado proyecto
proy
nos permitió elaborar un material audiovisual en cuatro idiomas,
inédito y en formato CD, que está sirviendo para que los estudiantes universitarios de disciplinas técnicas de la
Universidad de Jaén, hispanohablantes o no, aprendan, afiancen y recuerden múltiples conceptos científicocien
técnicos en el contexto propio de un laboratorio de química.
Desde la edición del material por el Servicio de Publicaciones de la Universidad de Jaén en el año 2009
se está incluyendo como bibliografía específica recomendada en las guías docentes de las asignaturas con
laboratorio de química de las titulaciones científico-técnicas
científico técnicas que oferta la Universidad de Jaén y se está
utilizando en el aula para trabajar otras competencias, como las de “Conocimiento de una lengua extranjera”.
ia adquirida en el aula con el alumnado se deduce la necesidad de dedicarle más tiempo
De la experiencia
a trabajar un segundo idioma, hasta el punto de hacer bilingües las clases. A este respecto se ha empezado por
incluir algunos guiones de las prácticas de laboratorio en inglés para que los estudiantes se familiaricen con el
vocabulario y la traducción. No obstante, queremos dar un paso más y conseguir que el alumnado salga del
laboratorio sabiendo expresarse oralmente en inglés para describir una técnica u operación sencilla
senc
y desarrolle,
al mismo tiempo, competencias comunicativas fundamentales como la habilidad para hablar en público. Este ha
sido el objetivo principal del presente proyecto que, con la implicación de profesorado experimentado de dos
departamentos claves,, Filología Inglesa y Química Inorgánica y Orgánica, hemos perseguido.
perseguido
2
UNIVERSIDAD DE JAÉN
Vicerrectorado de Docencia y Profesorado
Secretariado de Innovación Docente y Formación del Profesorado
Objetivos conseguidos
1. Se han realizado una serie de encuestas que ponen claramente de manifiesto el bajo nivel de inglés
hablado y de comprensión auditiva de los estudiantes de nuevo ingreso en el Grado en Química
Qu
de la
Universidad de Jaén. Ver Anexo 1
2. Se ha hecho ver a los 100 estudiantes de primer curso del Grado en Química (Cursos 2011-2012
2011
y
2012-2013)
2013) la necesidad e importancia de leer, escribir, escuchar y hablar en inglés correctamente con
vistas a mejorar su inserción laboral.
laboral
3. Se ha creado en el alumnado del Grado en Química el hábito de leer, escribir, escuchar y hablar en
inglés.
4. Se ha trabajado con los estudiantes las siguientes competencias básicas o trasversales de Grado en
Química establecidas en el RD 1393/2007: B1. Capacidad de análisis y síntesis, B2. Capacidad de
organización y planificación, B3. Comunicación oral y escrita en la lengua nativa y, especialmente B4.
Conocimiento de una lengua extranjera, inglés.
5. Se han elaborado ejercicios que han permitido evaluar tanto de forma continua como en el examen final
las competencias anteriormente citadas. Ver Anexo 3
6. See ha traducido al inglés la Guía Docente de la asignatura del Grado en Química “Operaciones Básicas
de laboratorio II”. Ver Anexo 4
7. El alumnado del
el Grado en Química ha traducido íntegramente al inglés el cuaderno de laboratorio
lab
de la
asignatura “Operaciones Básicas de laboratorio II”. Ver Anexo 4.
8. Buena parte del alumnado del Grado en Química ha tenido la oportunidad de leer textos en inglés y
corregir su pronunciación con el apoyo del Profesorado del Departamento de Filología
Fil
Inglesa de la
Universidad participante en el proyecto.
9. Con los textos traducidos al inglés y los mejores audios grabados se ha iniciado la elaboración de un
material docente de apoyo al profesorado para favorecer el movimiento hacia el bilingüismo en
e
asignaturas experimentales como es el caso de “Operaciones Básicas de Laboratorio II” del Grado en
Química. Ver Anexo 5.
3
UNIVERSIDAD DE JAÉN
Vicerrectorado de Docencia y Profesorado
Secretariado de Innovación Docente y Formación del Profesorado
Contenidos desarrollados
La asignatura “Operaciones Básicas de Laboratorio II OBL-II”,
OBL II”, en la que se centra el presente proyecto, es una
materia obligatoria que se imparte en el segundo cuatrimestre del primer curso del Grado en Química y que
completa la formación en operaciones básicas
bá
de laboratorio adquirida por el alumnado con la asignatura de
primer cuatrimestre “Operaciones Básicas de Laboratorio I (OBL-I)”.
(OBL
En la asignatura OBL-I el alumnado aprende las normas de seguridad en un laboratorio de química y
operaciones básicas de trabajo como pesar, preparar y valorar disoluciones o separar los componentes de una
mezcla mediante extracción simple o múltiple.
En la asignatura OBL-II
II por otro lado, el estudiante aplica las habilidades experimentales básicas adquiridas en
la Asignatura OBL-II al estudio de casos más complejos como,
como por ejemplo, el estudio de las propiedades físicoquímicas de compuestos inorgánicos o la purificación y caracterización de productos orgánicos obtenidos
mediante procedimientos sintéticos.
En el anexo 5 se detallan las 12 experiencias que el alumnado tiene que desarrollar en el trascurso de la
asignatura y que han sido traducidas al inglés por é mismo durante los dos cursos de ejecución del presente
proyecto.
Metodología empleada
(sesiones de trabajo, actividades, recursos didácticos, cronograma, etc)
Una de las competencias que se trabaja en la asignatura Operaciones Básicas de Laboratorio II OBLII del Grado en
Química según se indica en la Guía Docente [1] es la de “Conocimiento
Conocimiento de una lengua extranjera, preferentemente
inglés”.
Hasta el curso 2010-2011
2011 esta competencia se había trabajado incluyendo en el guión de prácticas:
prácticas
1.- Una experiencia escrita integramente en inglés, (Exp. 10: Synthesis and Purification Through Recrystallization of
Acetylsalicylic Acid (Aspirin).
2.- Cuestiones en inglés que los estudiantes debían responder en inglés y/o en castellano (Ej."Take
(Ej.
a look at the following
pictograms. All of them can be found on the labels of the reagents used in this experiment. Write their meaning in English
and Spanish."
3.- Cuestiones en castellano que los estudiantes debían responder en inglés. (Ej. Escriba en inglés todo el material de
vidrio que necesita para realizar la experiencia).
experiencia
Con el desarrollo del presente Proyecto
royecto de Innovacion
nnovacion Docente hemos pretendido además que,
que el alumnado matriculado
en la asignatura …
4
UNIVERSIDAD DE JAÉN
Vicerrectorado de Docencia y Profesorado
Secretariado de Innovación Docente y Formación del Profesorado
1.- traduzca al inglés un texto sencillo.
2.- lea
ea correctamente el texto traducido.
Para conseguir ambos objetivos, durante el curso 2011-2012
2011
contamos con la colaboración
aboración de tres profesores del
Departamento de Filología Inglesa de la Universidad que han grabado las voces del
del alumnado y le han corregido la
pronunciación en varias sesiones de tutorización durante el transcurso de la asignatura en el 2º cuatrimestre.
cuatrimestre
Antes de asignarle al alumnado unn texto,
texto el primer día de clase se le pasó un breve cuestionario para conocer su nivel
inicial de inglés hablado, escrito, de comprensión lectora y auditiva. Asimismo también se le preguntó sobre los años de
inglés cursados en la escuela, en el instituto y en academias. (Anexo 1)
Con los datos de nivel obtenidos a cada estudiante se le asignó un texto de mayor o menor
meno extensión y se le proporcionó
diferente material bibliográfico y “on
on line”
line para abordar la traducción. [2-5]
Una vez que las traducciones contaron con el visto bueno de los profesores implicados en la asignatura después de varias
sesiones de tutorización y seguimiento, los estudiantes pasaron a entrevistarse con los profesores del Departamento de
Filología Inglesa
esa para leer los textos, corregir su pronunciación y grabar los audios.
La última sesión de la asignatura se dedicó a escuchar los audios y trabajar,
trabajar con
on los estudiantes,
estudiantes su comprensión auditiva
intentando contestar algunas cuestiones relacionadas con los
lo audios.
Finalizado el curso 2011-2012, all alumnado interesado, con mejor nivel, se le ofreció la oportunidad de seguir
practicando y mejorando su nivel de lectura con el apoyo de uno de los profesores del Departamento de Filología Inglesa
durante el curso 2012-2013. Si bien buena parte del alumnado participante se mostró inicialmente interesado, finalmente,
por incompatibilidades horarias con otras asignaturas del grado, solo cinco han podido continuar con la experiencia.
experiencia
Aun así y, con objeto de animar all alumnado a que trabaje, además de las competencias lingüísticas, otras competencias
específicas y transversales también incluidas en el Grado (RD 1393/2007) como:
como “Conocer los tipos de reacción que
experimentan los compuestos químicos en el medio ambiente y su incidencia en el mismo”, “capacidad de adaptarse a
nuevas situaciones y toma de decisiones”, “razonamiento crítico”, “sensibilidad hacia temas medioambientales”
medioambientale o
“compromiso ético”; a todos se les ha hecho entrega del texto de lectura graduada con CD “Chemical Secret” de Tim
Vicary. En este texto se narra el dilema ético y moral al que se enfrenta un científico que trabaja en una fábrica de
pinturas que genera vertidos contaminantes.
Durante el curso 2012-2013
2013 se ha repetido la experiencia con los estudiantes de nuevo ingreso en el Grado en Química
(49) solo que no se ha podido realizar la grabación de los audios por incompatibilidades horarias.
horarias Aun así, sí se ha
conseguido la traducción integra de todas las experiencias de la asignatura del español al inglés. Esto junto con los audios
grabados por los estudiantes (51) que ingresaron en el curso 2011-2012
2011
nos han permitido elaborar una amplia batería de
ejercicios de gran interés (anexo 3) para evaluar la competencia “Conocimiento
Conocimiento de una lengua extranjera,
extranjera
preferentemente inglés” incluida en la asignatura Operaciones Básicas de Laboratorio II de primer curso del grado en
Quimica
[1] http://goo.gl/PMDdp;
[2] Marchal, A et col. (2009) Introducción a un Laboratorio de Química. Guía Audivisual Multilíngüe en CD.
Universidad de Jaén.;
[3] Pavia, D.L.; Lampman, G.M.; Kriz_Jr, G.S.; Engel, R.D. (2005) Introduction to Organic Laboratory Techniques,
Techniques 2nd
ed. Thonson Brooks/cole.;
[4] Woolins, J.D. (2003) Inorganic Experiments,
Experiments Weinheim, Wiley-VCH.
[5]
http://www.pobel.es; http://www.sigmaaldrich.com
/www.sigmaaldrich.com
5
UNIVERSIDAD DE JAÉN
Vicerrectorado de Docencia y Profesorado
Secretariado de Innovación Docente y Formación del Profesorado
Resultados obtenidos
(los materiales o documentos que se hayan producido en la experiencia deben
en presentarse en forma de anexo)
Ver apartado Objetivos conseguidos y ANEXOS
Proyección e Impacto
(transferencia de los resultados y mejoras en el aprendizaje demostrables)
El impacto de la iniciativa en el alumnado ha sido muy importante al no haber hablado muchos de ellos,
ellos nunca,
en inglés en sus institutos según manifiestan,
manifiestan y haber tenido la oportunidad, gracias a la experiencia llevada a
cabo, de que un profesor o profesora les corrigiese la pronunciación.
Puesto que en el marco del EEES a todo el alumnado se le va a exigir que acredite un determinado nivel de
inglés para conseguir
onseguir el título de grado,
grado, la experiencia les ha servido para darse cuenta del bajo nivel que tienen
y la necesidad de hacer cursos que les permitan mejorarlo.
Por otro lado, la edición de un material audiovisual accesible que incorpore los
l s mejores audios del alumnado
servirá para que promociones futuras se beneficien también de la experiencia mejorando indudablemente su
conocimiento de una lengua extranjera, el inglés en el caso que nos ocupa,
ocupa y que interesa mucho a los futuros
profesionales de la Química.
Finalmente, puesto que en el marco del EEES, la formación de los graduados se mide en base a la adquisición
de competencias, el diseño de herramientas que permita evaluarlas objetivamente adquiere un papel
trascendental. A este respecto, el desarrollo del presente proyecto ha permitido elaborar una amplia diversidad
de ejercicios (anexo 3), de utilidad para evaluar, tanto en un proceso de formación
forma
continua como en un
examen final, la competencia “Conocimiento
Conocimiento de una lengua extranjera,
extranjera preferentemente inglés” incluida en la
asignatura Operaciones Básicas de Laboratorio II de primer curso del Grado
rado en Química.
Qu
Esta competencia, si
bien está incluida en las Guías Docentes de otras cinco asignaturas del Grado en Química de la Universidad de
Jaén, no se evalúa en ninguna de ellas siendo por tanto el trabajo realizado un excelente referente para las
mismas.
6
UNIVERSIDAD DE JAÉN
Vicerrectorado de Docencia y Profesorado
Secretariado de Innovación Docente y Formación del Profesorado
Evaluación del proceso y Autoevaluación
(instrumentos y recursos empleados)
Las actividades planteadas y llevadas a cabo en el marco del Proyecto de Innovación Docente han sido muy
bien aceptadas por la mayor parte del alumnado de primer curso del Grado en Química (Anexo 2) al reconocer
éste su bajo nivel en inglés y, asumir la importancia de conocer una lengua extranjera para:
1.- Conseguir el título de grado.
2.- Tener opción a una beca de movilidad internacional.
3.- Ampliar el abanico de posibles salidas profesionales.
Si bien durante los dos cursos 2011-2012
2012 y 2012-2013,
2012
en los que se ha desarrollado el proyecto ha habido
estudiantes que han demostrado especiales dificultades para resolver las actividades propuestas (algunos de
ellos incluso han suspendido
pendido la prueba final escrita),
escrita) la gran mayoría ha respondido con interés llegando incluso
a sugerir la posibilidad de seguir contando con el apoyo del profesorado del Departamento de Filología Inglesa
para seguir mejorando su pronunciación en cursos sucesivos. Esta idea es la que ha permitido que cinco
estudiantes que participaron
ron en el proyecto en el curso 2011-2012
2011 2012 hayan continuado en el curso 2012-2013.
2012
Este apoyo ha sido también fundamental para el profesorado del Departamento de Química Inorgánica y
Orgánica participante en el proyecto dado que, si bien éste era el responsable principal de que los textos que
había que traducir estuvieran a tiempo para una primera corrección por su parte, la revisión definitiva, con los
comentarios oportunos a los errores cometidos,
cometidos ha corrido por cuenta del profesorado del Departamento
Departa
de
Filología Inglesa en su horario de tutorías.
tutorías. Esta doble corrección que podría carecer de importancia en un
principio, ha permitido mejorar considerablemente la calidad de los textos consiguiéndose así un material muy
válido para ser difundido entree el alumnado en cursos futuros.
Finalmente queremos comentar que si bien el proyecto inicial incluía la grabación en video de las
intervenciones del alumnado ésta se ha desestimado al
a ver las dificultades que presentaba para comunicarse en
su lengua no nativa, más aún si iban a ser grabados. Alternativamente se ha considerado más oportuno grabar
algunas escenas breves de los experimentos para incluirlas en el material bilingüe audiovisual que se está
elaborando.
Otras consideraciones
7
UNIVERSIDAD DE JAÉN
Vicerrectorado de Docencia y Profesorado
Secretariado de Innovación Docente y Formación del Profesorado
Gastos generados en el segundo año
Fungibles
Inventariables
Viajes/Actividades
350 €. Inscripción en las VIII Jornadas de Innovación Docente en
Química INDOQUIM 2013.. Alcalá Henares.
Henares Presentación resultados
preliminares.
420 €. Inscripción en 6th International Conference of Education,
Research and Innovation ICERI2013. Sevilla
350 €. Inscripción en European Conference on Research in Chemical
Education. ECRICE 2014. Jyväskylä (Finlandia)
Otros
275 €. Libros y CDs de lectura graduada para el alumnado
alumnado participante en el
proyecto. Chemical Secret de Tim Vicary.
Vicary. Perfeccionamiento capacidad auditiva y
comprensión de textos en lengua inglesa.
175 €. Grabadora de video y accesorios.
accesorios. Grabación de experimentos para
material docente multimedia
Justificación
8
UNIVERSIDAD DE JAÉN
Vicerrectorado de Docencia y Profesorado
Secretariado de Innovación Docente y Formación del Profesorado
DATOS DE LOS MIEMBROS DEL GRUPO
Nombre
CONCEPCIÓN
Apellidos
SOTO PALOMO
D.N.I.
24136280-B
B
Centro
Facultad
de
E-mail
Humanidades
csoto@ujaen.es
y Teléfono 953211830
Ciencias de la Educación
Departamento
Filología Inglesa
Asignatura impartida
Lingüística Contrastiva Inglés-Español
Curso
Optatividad de 2º ciclo
Categoría
Profesora Asociada III
Firma
Concepción Soto Palomo
DATOS DE LOS MIEMBROS DEL GRUPO
Nombre
JOSÉ MARÍA
Apellidos
MESA VILLAR
D.N.I.
26014548-F
F
Centro
Facultad
E-mail
de
Humanidades
jmvillar@ujaen.es
y Teléfono 953213375
Ciencias de la Educación
Departamento
Filología Inglesa
Asignatura impartida Lexicología y lexicografía del Inglés (2ª ciclo de
Filología Inglesa), Cultura de los Países de Habla
Inglesa (2º curso de Estudios Ingleses), Estudio
Selectivo de Literatura Inglesa:
Drama (2ª ciclo de Filología Inglesa). Prácticum
(Magisterio Lengua Extranjera).
Curso
Categoría
2º, Optatividad de 2º ciclo, Prácticum.
Profesor Sustituto Interino Firma
(tiempo completo, larga
duración).
Profesor en el Centro de
Estudios Avanzados de
Lenguas
modernas
José María Mesa Villar
CEALM
9
UNIVERSIDAD DE JAÉN
Vicerrectorado de Docencia y Profesorado
Secretariado de Innovación Docente y Formación del Profesorado
DATOS DE LOS MIEMBROS DEL GRUPO
Nombre
YOLANDA
Apellidos
CABALLERO ACEITUNO
D.N.I.
26036456-L
L
Centro
Facultad
E-mail
de
ycaballe@ujaen.es
Humanidades
y Teléfono 953212608
Ciencias de la Educación
Departamento
Filología Inglesa
Asignatura impartida
Textos Literarios en Lengua Inglesa (Licenciatura en
Filología
Inglesa
y
Diplomatura
en
Turismo);
Literatura Inglesa hasta 1660 (Grado en Estudios
Ingleses)
Curso
4º y 1º
Categoría
Profesora
Ayudante Firma
Doctora
Yolanda
Aceituno
Caballero
DATOS DE LOS MIEMBROS DEL GRUPO
Nombre
NURIA
Apellidos
ILLAN CABEZA
D.N.I.
26.027.019
26.027.019-N
Centro
Facultad
E-mail
de
naillan@ujaen.es
Ciencias Teléfono 953212949
Experimentales
Departamento
Química Inorgánica y orgánica
Asignatura impartida
Curso
11º
Categoría
Profesora
a
Operaciones Básicas de Laboratorio II
Titular
de Firma
Universidad
Nuria Illán Cabeza
(Añadir tantas tablas como participantes en el Proyecto)
10
UNIVERSIDAD DE JAÉN
Vicerrectorado de Docencia y Profesorado
Secretariado de Innovación Docente y Formación del Profesorado
VºBº de Coordinador/a
Fdo.: Antonio Marchal Ingrain
Jaén, a 19 de julio de 2013
VICERRECTOR DE DOCENCIA Y PROFESORADO DE LA UNIVERSIDAD DE JAÉN
11
UNIVERSIDAD DE JAÉN
Vicerrectorado de Docencia y Profesorado
Secretariado de Innovación Docente y Formación del Profesorado
ANEXOS
ANEXO 1
ENCUESTAS EVALUACIÓN INICIAL NIVEL DE INGLÉS
ANEXO 2
ENCUESTAS OPINIÓN ESTUDIANTES SOBRE EL PROYECTO
ANEXO 3
EJERCICIOS DE LISTENING
ANEXO 4
CUARDERNO DE LABORATORIO EN INGLÉS
ANEXO 5
MATERIAL MULTIMEDIA
12
Estimados/as estudiantes,
Como sabréis, si habéis leído la guía Docente de la asignatura OBL 2, una de las competencias a
trabajar en la misma es la de Conocimiento de una lengua extranjera, preferentemente inglés.
A este respecto vais a …
1.- realizar y contestar las cuestiones de una experiencia escrita íntegramente en inglés, (Exp. 10)
2.- contestar en inglés o castellano cuestiones escritas en inglés distribuidas en el resto de las
experiencias.
3.- nombrar en inglés el material de trabajo básico de laboratorio.
4.- escuchar y comprender varios textos sencillos relacionados con las experiencias que vais a
realizar.
5.- traducir al inglés un texto en castellano sencillo relacionado con las experiencias que vais a
realizar.
En relación con este último punto y con objeto de poder asignaros un texto acorde con vuestros
conocimientos de partida necesitaríamos que rellenarais y nos entregaseis el siguiente cuestionario.
THANK YOU SO MUCH.
NAME:
1. Años cursados de inglés en el colegio:
2. Años cursados de inglés en el Instituto:
3. Años cursados de inglés en una Academia:
4. Estancias en el extranjero y duración de las mismas:
5. Nivel acreditado: A1, A2, B1, B2, C1, C2, OTRO:
6. Valórese del 1 al 4 los niveles que cree que tiene de los siguientes aspectos:
• Nivel de comprensión auditiva:
• Nivel de comprensión lectora:
• Nivel de inglés escrito:
• Nivel de inglés hablado:
7. Traduzca al inglés y luego al castellano las siguientes frases:
El agua hierve a 100 grados centígrados
Write in Spanish and English the words that represent the following pictures that you can find on the labels of
the bottles used, as well as their corresponding meaning.
RESULTADOS EVALUACIÓN NIVEL INICIAL DE INGLÉS
Curso 2012-2013
Estudiantes encuestados: 49
1. Años cursados de inglés en colegio: 4
2. Años cursados de inglés en Instituto: 6
3. Estudiantes que han cursado inglés en academia para aprobar o para mejorar: 24
4. Estudiantes que han realizado estancias por estudios en el extranjero: 24
5. Nivel acreditado: A1(1), A2(9), B1(8), B2 (3), C1, C2, OTRO (2), NINGUNO (26):
6. Nivel que dicen los estudiantes que tienen de…:
•
Nivel de comprensión lectora (4 máx.): 2.5
•
Nivel de comprensión auditiva (4 máx.): 1.5
•
Nivel de inglés escrito (4 máx.): 2.4
•
Nivel de inglés hablado (4 máx.): 1.9
7. Traduce las siguientes frases: Errores más comunes
El agua hierve a 100 grados centígrados
No conocen el verbo “hervir” (8)
Opciones. Is boiling; pass gas, Buill, up burn, boild, bois, hierving
No conocen la palabra “grados”
Watter (2) Wather (2)
Write in Spanish and English the words that represent the following pictures that you can find on the labels of
the bottles used, as well as their corresponding meaning.
Todos traducen bien
RESULTADOS EVALUACIÓN NIVEL INICIAL DE INGLÉS
Curso 2011-2012
Estudiantes encuestados: 51
1. Años cursados de inglés en colegio: 4
2. Años cursados de inglés en Instituto: 6
3. Estudiantes que han cursado inglés en academia para aprobar o para mejorar: 15
4. Estudiantes que han realizado estancias por estudios en el extranjero: 7
5. Nivel acreditado: A1(1), A2(2), B1(4), OTRO (3), NINGUNO (41):
6. Nivel que dicen los estudiantes que tienen de…:
•
Nivel de comprensión lectora (4 máx.): 2
•
Nivel de comprensión auditiva (4 máx.): 2
•
Nivel de inglés escrito (4 máx.): 3
•
Nivel de inglés hablado (4 máx.): 1.5
7. Traduce las siguientes frases: Errores más comunes
El agua hierve a 100 grados centígrados
No conocen el verbo “hervir” (19)
Opciones. burn, boild
No conocen la palabra “grados” (23)
Write in Spanish and English the words that represent the following pictures that you can find on the labels of
the bottles used, as well as their corresponding meaning.
No contestan 7
Estimados/as estudiantes:
Como habéis podido comprobar durante el desarrollo de la asignatura una de las competencias que hemos intentado que
trabajéis ha sido la de Conocimiento de una lengua extranjera, concretamente inglés.
Esta competencia se ha trabajado incluyendo en el guión de prácticas:
1.- una experiencia escrita íntegramente en inglés, (Exp. 10: Synthesis of aspirin)
2.- cuestiones en inglés que debían contestarse en castellano o en inglés.
3.- cuestiones en castellano que debían contestarse en inglés (material de laboratorio).
Con esto, además habéis traducido al inglés un texto sencillo, se os ha corregido y se os ha grabado una vez trabajada la
pronunciación, ritmo y entonación del texto.
Puesto que no suele ser habitual trabajar esta competencia en las aulas nos gustaría que, contestando a las siguientes
preguntas, nos dieseis vuestra opinión sobre la experiencia llevada a cabo, aspectos positivos, a mejorar y sugerencias.
Las cuestiones serán puntuadas, con una X, de 1 a 4 según vuestro grado de acuerdo, siendo 1 la expresión de grado
menor y 4 la de grado mayor. ¡¡ GRACIAS !!
ITEMS
Me ha resultado fácil entender las preguntas formuladas en inglés en el guión de prácticas.
Debería haber más preguntas escritas en inglés para conocer expresiones y vocabulario
específico de química en el guión de prácticas
Me ha resultado fácil seguir la experiencia escrita íntegramente en inglés.
Debería haber más experiencias escritas íntegramente en inglés para conocer vocabulario y
nuevas estructuras gramaticales en el guión de prácticas.
Me ha resultado fácil contestar en inglés algunas preguntas.
Deberíamos contestar más cuestiones en inglés para mejorar nuestro vocabulario y
expresiones gramaticales.
Me ha resultado fácil seguir los videos sobre técnicas de laboratorio en inglés.
Deberíamos ver más videos sobre técnicas de laboratorio en inglés.
El texto que se me ha asignado para traducir ha sido fácil.
Valoro positivamente que un profesor/a de inglés corrija mi pronunciación.
Hubiese sido necesario dedicarle más tiempo a corregir mi pronunciación con el profesor/a de
inglés.
Escuchar las grabaciones es bueno para mejorar mi pronunciación.
Al menos una sesión de laboratorio debería ser en inglés para mejorar mi conocimiento de
inglés.
Creo que sería capaz de seguir una sesión de laboratorio íntegramente en inglés.
Al menos una sesión de laboratorio debería ser bilingüe para mejorar mi conocimiento de
inglés.
Creo que sería capaz de seguir una sesión de laboratorio bilingüe.
En su conjunto las actividades realizadas me han ayudado a mejorar mi conocimiento de
inglés.
Sugerencias o mejoras adicionales que introducirías:
1
2
3
4
RESULTADOS DE …
Encuesta de evaluación del proyecto PID17_201113 realizada los días 7 de junio y 8 de junio
por los alumnos/as de la asignatura “Operaciones Básicas de Laboratorio II” participantes en
el mismo.
Alumnos participantes en el proyecto: 55 (A: 15; B: 14; C: 12; D: 14)
Alumnos encuestados: 38 (69%) (A: 13 (87%); B: 5(36%); C: 11(92%); D: 9 (64%)
ITEM
FORMULADOS
CUESTIONES
1
Me ha resultado fácil entender las preguntas formuladas en inglés en el guión de
prácticas.
2
Debería haber más preguntas escritas en inglés para conocer expresiones y vocabulario
específico de química en el guión de prácticas
3
Me ha resultado fácil seguir la experiencia escrita íntegramente en inglés.
4
Debería haber más experiencias escritas íntegramente en inglés para conocer vocabulario
y nuevas estructuras gramaticales en el guión de prácticas.
5
Me ha resultado fácil contestar en inglés algunas preguntas.
6
Deberíamos contestar más cuestiones en inglés para mejorar nuestro vocabulario y
expresiones gramaticales.
7
Me ha resultado fácil seguir los videos sobre técnicas de laboratorio en inglés.
8
Deberíamos ver más videos sobre técnicas de laboratorio en inglés.
9
El texto que se me ha asignado para traducir ha sido fácil.
10
Valoro positivamente que un profesor/a de inglés corrija mi pronunciación.
11
Hubiese sido necesario dedicarle más tiempo a corregir mi pronunciación con el
profesor/a de inglés.
12
Escuchar las grabaciones es bueno para mejorar mi pronunciación.
13
Al menos una sesión de laboratorio debería ser en inglés para mejorar mi conocimiento
de inglés.
14
Creo que sería capaz de seguir una sesión de laboratorio íntegramente en inglés.
15
Al menos una sesión de laboratorio debería ser bilingüe para mejorar mi conocimiento de
inglés.
16
Creo que sería capaz de seguir una sesión de laboratorio bilingüe.
17
En su conjunto las actividades realizadas me han ayudado a mejorar mi conocimiento de
inglés.
IMPORTANCIA QUE LOS ESTUDIANTES DAN A CADA ITEM
¿?
1
GRUPO A y B
18
2
3
4
NC
72
máx
1
GRUPO C y D
20
2
3
4
10
0
0
7
11
0
65
0
1
8
12
0
0
10
8
0
62
1
2
8
0
2
8
8
0
60
1
9
0
1
9
8
0
61
17
0
1
9
7
1
1
0
5
6
7
15
0
3
7
3
0
2
16
1
13
NC
80
máx
11
0
70
9
8
0
64
3
6
10
0
65
1
4
9
6
0
60
57
1
0
9
9
1
64
0
56
0
4
9
7
0
63
8
0
59
0
5
12
3
0
58
9
7
0
59
0
2
10
6
0
58
3
6
7
1
53
0
5
10
5
0
60
0
5
5
8
0
57
0
9
7
4
0
55
5
0
5
9
4
0
53
1
4
13
2
0
56
6
0
4
8
6
0
56
1
10
4
5
0
53
7
2
3
8
5
0
52
2
5
9
4
0
55
2
0
5
9
4
0
53
2
6
9
3
0
53
4
1
6
6
5
0
51
2
7
7
4
0
53
11
4
9
1
4
0
41
3
7
6
4
0
56
14
2
5
8
3
0
48
2
12
5
1
0
45
¿?
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
1
GRUPO A y B
18
2
3
4
NC
0
0
0
1
0
0
2
0
0
0
4
0
0
2
0
1
0
5
5
2
6
5
4
3
2
1
0
9
0
5
5
3
3
1
6
9
9
6
9
8
8
8
9
7
1
10
5
8
7
6
9
7
4
7
5
4
6
5
8
8
11
4
8
8
3
8
7
7
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
1
1
72
máx
56
53
59
51
53
56
52
60
61
65
41
62
57
48
59
53
57
1
0
2
0
2
1
1
2
1
1
0
3
1
0
2
0
0
1
GRUPO C y D
20
2
3
4
4
6
2
7
4
10
5
3
4
1
7
2
9
12
5
5
0
9
9
10
7
13
4
9
6
9
8
6
9
7
5
12
10
9
7
3
6
4
2
5
4
10
6
11
4
8
4
1
3
5
9
NC
80
máx
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
1
63
53
58
53
56
53
55
65
60
70
56
64
55
45
58
60
64
TOTAL
38
2
3
4
1
NC
152máx
135
(8.8)
126
(8.3)
125
(8.2)
121
(7.9)
121
(7.9)
119
(7.8)
117
(7.7)
117
(7.7)
113
(7.4)
112
(7.3)
109
(7.1)
109
(7.1)
107
(7.0)
106
(7.0)
104
(6.8)
97
(6.3)
93
(6.1)
1
TOTAL
38
2
3
4
NC
152
máx
119
106
117
104
109
109
107
125
121
135
97
126
112
93
117
113
121
Student´s name: ________________________________________
Listen the record number 1 and try to complete the gaps.
Put a pinch of manganese dioxide into a clean, dry glass test
tube, and use an ______________(1) to measure its total mass.
The margin of error must be less than 0.01g. Add about 1 gram of
dry _________ (2) chlorate, then weigh again and shake softly to
homogenize the mixture. Clamp the ________ (3) to a stand so as
to keep it at a constant 45 degree angle. Heat it lightly using a
__________(4), making sure you avoid a loss of solids or any
crackling issues. Once the solid melts, raise the heat as much as
possible for a few
(5). Allow some time for the test
tube to cool down and _______ (6) again. Put another pinch
of____________(7) into a clean, dry glass test tube, and use an
analytical balance to ___________(8) its total mass. Again, the
margin of error must be less than 0.01g. The teacher will then
provide a
(9) of potassium chlorate and potassium
chloride in unknown proportions: put about
(10) into the
already weighed test tube that contains the manganese dioxide.
Once added, weigh again and _______ (11) the tube to mix its
contents. Follow the same process explained above to heat the test
tube once more. Finally, allow it to cool down and repeat the
weighing step –this time with the final ________ (12).
Student´s name:________________________________________
Listen the record number 2 and try to complete the gaps
Choose one of the two cola drinks A or B that the teacher will
provide us and find out if they have caffeine or not. For this, pour
about ______ (1) mL of cola drink in a ______ (2), add 2 g of
potassium carbonate and shake it with a ______ (3) to eliminate the
maximum amount of ___________ (4). Next, pour the mixture into a
____________ (5) and add 15 ml of dichloromethane. Shake it to
prevent the _______ (6) to pop out by the effect of pressure and to
avoid emulsions. Organic phase is separated and aqueous phase is
extracted twice, using 20 ml of _____________ (7). Then, organic
phases are put together and treated with anhydrous sodium
__________ (8). The dry organic extract is filtered in a previously
weighed ___________ (9) and then, the solvent is removed in
the____________ (10). If the cola drink has ________ (11); it must
appear on the walls of the flask as a ____________ (12). Finally, the
flask is weighed again and the yield of caffeine extracted is
calculated.
Student´s name:________________________________________
Listen the record number 3 and try to complete the gaps
In a 250 mL round bottom flask resting on a ______ (1), 100
mL of a water-acetone ______ (2) is added. As it was done above, a
_________ (3) is added and then the flask is holded with a
_______(4) to a metallic support. Place the flask on a ________ (5)
and, greasing the standard-taper joints with silicone, attach a
vigreux ______ (6) and then, a _______________ (7) with a
___________ (8). After that, joint the condenser holding it with a
clamp, the bend adapter and a graduated beaker. Heat bath water
and wait to collect the first drop of distillate to record the
_____________ (9). Then, when the distillation is regular, the
distillation temperature is recorded and the collecting beaker is
replaced by a ____________ (10) to measure how much distillate is
obtained. When the temperature starts to drop, the distillation flask
is removed from the ___________ (11), then the graduated cylinder
is removed and finally, all the apparatus is disassembled piece by
piece in reverse.
Student´s name:________________________________________
Listen the record number 4 and try to complete the gaps
Filtration is a technique used to _________ (1) a solid from the
solution where it is initially. If we want the solution, filtration must be
done under gravity through a highly ______________ (2) in a glass
conical funnel. If we want the solid, filtration is most efficiently done
under suction through a flat filter in a porcelain ___________ (3).
Both kinds of filtrations are used in a procedure for purification of
solid substances called ___________ (4). This one consists of:
- Solving the impure solid in the minimum amount of a
___________ (5),
- ________ (6) by gravity the hot solution to remove any
insoluble ________ (7),
- ________ (8),the solution to ambient temperature
- ________ (9), the crystals by ________ (10) filtration.
Student´s name: ________________________________________
Listen the record number 5 and try to complete the gaps.
Weigh 2.0 g of __________ (1) and transfer them to a 100 mL ______________(2).
Add 4.0 mL of acetic anhydride and then add 5 drops of concentrated________ (3).
Shake the flask gently until the salicycilic acid dissolves.
Let the flask cool down to room temperature till the acetylsalicylic acid begins to
crystallize. If it does not, scratch the walls of the flask with a _________ (4) and let
the mixture cool down in an __________ (5) until crystallization takes place.
Once crystal formation is completed, add 50 mL of water and shake the flask gently
in order to liberate the crystals.
By means of __________ (6), collect the product on a ___________ (7). Add a
small amount of cold water to assist the transfer of crystals to the funnel. Rinse the
crystals several times with small portions of ________(8). Keep on with the suction
on the Büchner funnel for some minutes, drawing air through the crystals till they are
free of solvent.
Sometimes the crude product may contain some unreacted salicyclic acid residues,
so purification by ______________ (9) may be necessary.
In order to select the most adequate solvent, transfer a bit of solid to _________
(10) and add to each of them 1 ml of cool water, _________ (11) and ethyl acetate
respectively.
Pay attention to that solvent in which the solid is not dissolved at room temperature
and then, heat the tubes in a ____________ (12).
1
Student´s name: ________________________________________
Listen the record number 6 and try to complete the gaps.
In this ___________ (1), caffeine will be isolated from tea bags and separated from
other accompanying ___________ (2) thanks to their different acid-basic
__________ (3) and their different __________ (4) in both water and organic
_______ (5).
Weigh 1 g of potassium _________ (6), transfer it to a beaker and dissolve it in 100
mL of water. Add a _________ (7), heat the solution on a __________ (8) and when
it is about to boil turn the hotplate off and place ______ (9) tea bags into the hot
solution so that they lie flat on the bottom of the ______ (10) and are fully covered
by water. After 10 minutes, remove the tea bags by gently pushing them against the
walls of the flask with the help of a glass rod or a _____ (11), avoiding breaking it.
Clean the bags with water and finally dispose of them in a solid waste _______ (12).
Cool the brown solution at room temperature and transfer it to a ___________ (13)
through a bed of cotton.
Student´s name: ________________________________________
Listen the record number 7 and try to complete the gaps.
Solvent Extraction is a ____________(1) technique used to ______ (2) a compound
from an _______ (3) solution by shaking with an _______(4) solvent, the extractor
solvent.
To get a most efficient extraction, the extractor solvent must:
-
be _________ (5) with the aqueous solution where the required compound is
initially,
-
dissolve the required compound ________ (6) than water,
-
not ________ (7) with the required compound,
-
be easily ________ (8),
- not to be _________ (9) or _______ (10).
Student´s name: ________________________________________
Listen the record number 8 and try to complete the gaps.
Chromatography is a ________ (1) which can _________ (2) the components
of a ________ (3) due to their different interactions with a _______ (4) phase (solid
or liquid) when they are pulled along by a _______ (5) phase (gaseous or liquid).
Chromatography can be either ______ (6) or in _______ (7) according to the
layout of the stationary phase.
Thin layer chromatography, usually called ______ (8), is the most used type of
plane chromatography.
Here, a solid stationary phase is attached to a _______ (9) and a liquid, which
is called ______ (10), and which rises up by ________ (11) sweeping and
separating the components of the mixture.
This type of chromatography is useful for:
1. ________ (12) the purity of a compound
2. ________ (13) the components of quite complex mixtures
3. ________ (14) and ________ (15) the components of a mixture
4. ________(16) the progress of a reaction
Student´s name: ________________________________________
Academic course: ______________________________________
BACHELOR IN CHEMISTRY
FACULTY: EXPERIMENTAL SCIENCES
ACADEMIC COURSE: 1
COURSE GUIDE
1. BASIC DATA OF THE SUBJECT
NAME: BASIC LABORATORY OPERATIONS II
CODE: 10311004
ECTS credits: 6
course: 1º
CHARACTER: BASIC
semester: 2º
2. BASIC DATA FROM INSTRUCTORS
NAME (coordinator):
DEPARMENT: Inorganic and Organic Chemistry
AREA
Nº OFFICE:
PLACE: B3
TLF:
PREREQUIREMENTS: None
CONTEXT IN THE DEGREE: Compulsory subject which is imparted in the 2nd
semester of the 1st course. This subject will develop and expand on the practical
skills which students acquired in Basic Laboratory Operations I (1st semester)
RECOMMENDATIONS AND CURRICULAR ADAPTATIONS: Possessing a
medium level in English and having passed the subject Basic Laboratory Operations
I
4. COMPETENCES AND LEARNING OUTCOMES
CODE
B4
B11
Q3
P1
P2
P3
C1
SKILLS
Knowledge of a foreign language (preferably English).
Sensibility towards environmental issues
Skills in the evaluation, interpretation and synthesis of chemical
information and data.
Skills in the safe handling of chemical materials, taking into account
their physical and chemical properties, including any specific hazards
associated with their use.
Skills required for the participation in and development of the
standard laboratory procedures required and use of instrumentation
in synthetic and analytical work, in relation to both organic and
inorganic systems.
Skills in the monitoring, through observation and measurement, of
chemical properties, events or changes, and in the systematic and
reliable recording and documentation thereof.
Knowledge of the main aspects of chemical terminology,
nomenclature, conventions and units
Result 1
Result 2
Result 3
Result 4
Result 5
Result 6
Result 7
LEARNING OUTCOMES
S/he knows basic vocabulary in English related to security, reagents
and basic laboratory operations.
S/he is able to minimize the generation of residues and manage
them
S/he has knowledge and skills in the safe handling of chemical
materials, taking into account their hazards and the possible risks
associated with their use
S/he is able to apply the basic practical skills acquired in the subject
Basic Laboratory Operation I to complex situations.
S/he knows the experimental techniques used in the purification of a
chemical compound.
S/he knows the procedures to be followed in the chemical
characterization of a chemical compound.
S/he is able to interpret and communicate in an adequate way the
results of the experiments using a proper scientific terminology.
5. CONTENTS
Part I: Basic Operations applied to the study of physicochemical properties of
inorganic compounds
1.- Determining the atomic mass of magnesium (Mg)
2.- Determining the molecular mass of CO2
3.- Establishing the formula of KClO3
4.- Obtention and acid-base properties of HCl and NH3
5.- Obtention and study of redox properties of H2O2
6.- Obtention and physical properties of [Cu(NH3)4]SO4·H2O
Part II: Isolation of compounds from reaction media, natural and commercial
sources.
7.- Separation and purification of the components of a mixture through distillation
8.- Isolation of essential oils from aromatic plants through steam distillation
9.- Isolation of caffeine from a cola drink and tea leaves.
10.- Isolation and identification of the components of an Analgesic Tablet
11.- Synthesis and purification through recrystallization of acetylsalicylic acid
(Aspirin)
12.- Monitoring the progress of a reaction by means of thin layer chromatography
and isolation of products.
6. METHODS AND ACTIVITIES
AUTONOMOUS
TOTAL
LEARNING
HOURS
HOURS
8
16
ACTIVITIES
CLASSROOM
HOURS
ECTS
CREDITS
COMPETENCES
(Codes)
Introductory seminar
8.0
0.80
B4, B11, C1
Tutorials
2.0
2
4
0.20
Q3
Practice 1
3.5
6
9.5
0.35
Practice 2
3.5
6
9.5
0.35
Practice 3
4.0
7
11
0.40
Practice 4
4.0
7
11
0.40
Practice 5
4.0
7
11
0.40
Practice 6
4.0
7
11
0.40
Practice 7
Practice 8
3.5
4.0
6
7
9.5
11
0.35
0.40
Practice 9
3.5
6
9.5
0.35
Practice 10
4.0
7
11
0.35
Practice 11
4.0
7
11
0.40
Practice 12
4.0
7
11
0.40
4
0.40
150
6
Theorical-practical
exam
TOTAL:
4
60
90
B4, P1, P2, P3,
Q3, C1
B4, P1, P2, P3,
Q3, C1
7. ASSESSMENT METHODS
1. Monitoring the work done by the student in the lab
2. Laboratory reports
3. Theoretical-practical examination
ASPECT
Attendance
and
participation
ASSESMENT
- Punctuality
-Active participation in seminars and
tutorials
INSTRUMENT
Teacher notes and
observation of the
students.
WEIGHT (a)
25 %
-Well-written reports:
· Grammar and neat presentation
Laboratory
· Quality in the use of references
Weekly revision
15 %
· Quality of the texts translated into
reports
English.
· Originality
-Knowledge and mastery of the
60 %
theoretical and practical issues of the
Conceptual
Theorical-practical
subject.
understanding -Mastery of the basic English
examination
terminology needed to work in a
laboratory
(a) The percentages above will exclusively be applied if, and only if, the students get, at least, 3
out of 10 points in the theoretical-practical exam. Once this requirement has been met, the
students will be awarded a passing mark if the final qualification in the subject is of 5 out of 10
points, in accordance with the evaluative system regulated by the RD 1125/2003 (September
5) which, following the European Credit System, specifies the evaluative procedure to be
applied in official university degrees.
8. REFERENCES
SPECIFIC OR BASIC:
1. GARCÉS, A. “Experimentación en Química Inorgánica”, Ed. Dykinson 2009. Experiences 1-6
2. RAMOS, M. M. y VARGAS, C. “LABORATORIO DE QUIMICA ORGANICA”, EDITORIAL
UNIVERSITARIA RAMON ARECES, MADRID: 2006. Experiences 7, 8 y 9
3. MARTINEZ M.A., CSÁKY A.G.“Técnicas Experimentales en Síntesis Orgánica” Ed. Síntesis S.A;
1998. Experiences 1-12
4. MARCHAL, A et col. “Introduction to Laboratory of Chemistry. Multilingual Audivisual Guide” CD.
Universidad de Jaén, 2009 Experiences 7-12
5. PAVÍA D.L., LAMPMAN G.M., KRIZ-Jr G.S, Engel, R.D. "Introduction to Organic Laboratory
Techniques", 2nd ed., Thonson Brooks/cole, 2005 Experiences 7-12.
6. Webs
www.chemspider.com
http://www.ub.edu/oblq/
http://www.liceoagb.es/quimiorg/indice.html
GENERAL AND COMPLEMENTARY:
1. WOOLLINS J.D. (ed.); "Inorganic Experiments", VCH; 2003.
2. HORTA A., ESTEBAN S., NAVARRO R., CORNAGO P., BARTHELEMY C; “Técnicas
experimentales de Química”, UNED, 2001.
3. CONTRERAS A., CASELLES, M. J., MOLERO, M ; “Introducción a la Química Experimental. (I)El
laboratorio de Química. Instalaciones y Material. (II) Productos o Sustancias Químicas. (III) Técnicas
Básicas de Laboratorio”.3 videos y 2 teaching guides. UNED 1992
Semester 2nd
1st:
2nd:
3nd
4th:
5th:
6th:
7th:
8th:
9th:
10th:
11th:
12th:
13th:
14th:
15th:
Total hours:
Exam
Autonomous
learning
Activity n
Experimental
work
Tutorial
WEEK
Seminar
9. SCHEDULE (second semester)
Observations
Lab Safety Rules
http://nobel.scas.bcit.ca/debeck_pt/science/safety.htm#gg
GENERAL GUIDELINES
1. Conduct yourself in a responsible manner at all times in the
laboratory.
2. Follow all written and verbal instructions carefully. If you do
not understand a direction or part of a procedure, ASK YOUR
TEACHER BEFORE PROCEEDING WITH THE ACTIVITY.
3. Never work alone in the laboratory. No student may work in
the science classroom without the presence of the teacher.
4. When first entering a science room, do not touch any
equipment, chemicals, or other materials in the laboratory area
until you are instructed to do so.
5. Perform only those experiments authorized by your teacher.
Carefully follow all instructions, both written and oral.
Unauthorized experiments are not allowed.
6. Do not eat food, drink beverages, or chew gum in the
laboratory. Do not use laboratory glassware as containers for
food or beverages.
1
7. Be prepared for your work in the laboratory. Read all
procedures thoroughly before entering the laboratory. Never
fool around in the laboratory. Horseplay, practical jokes, and
pranks are dangerous and prohibited.
8. Always work in a well-ventilated area.
9. Observe good housekeeping practices. Work areas should
be kept clean and tidy at all times.
10. Be alert and proceed with caution at all times in the
laboratory. Notify the teacher immediately of any unsafe
conditions you observe.
11. Dispose
pose of all chemical waste properly. Never mix
chemicals in sink drains. Sinks are to be used only for water.
Check with your teacher for disposal of chemicals and
solutions.
12. Labels and equipment instructions must be read carefully
before use. Set up and use the equipment as directed by your
teacher.
13. Keep hands away from face, eyes, mouth, and body while
using chemicals or lab equipment. Wash your hands with soap
and water after performing all experiments.
14. Experiments must be personallyy monitored at all times. Do
not wander around the room, distract other students, startle
other students or interfere with the laboratory experiments of
others.
15. Know the locations and operating procedures of all safety
equipment including: first aid kit(s),
it(s), and fire extinguisher. Know
where the fire alarm and the exits are located.
16. Know what to do if there is a fire drill during a laboratory
period; containers must be closed, and any electrical equipment
turned off.
2
CLOTHING
17. Any time chemicals, heat, or glassware are used, students
will wear safety goggles. NO EXCEPTIONS TO THIS RULE!
18. Contact lenses may be not be worn in the laboratory.
19. Dress properly during a laboratory activity. Long hair,
dangling jewelry, and loose or baggy clothing are a hazard in the
laboratory. Long hair must be tied back, and dangling jewelry
and baggy clothing must be secured. Shoes must completely
cover the foot. No sandals allowed on lab days.
20. A lab coat or smock should be worn during laboratory
experiments.
ACCIDENTS AND INJURIES
21. Report any accident (spill, breakage, etc.) or injury (cut,
burn, etc.) to the teacher immediately, no matter how trivial it
seems. Do not panic.
22. If you or your lab partner is hurt, immediately (and loudly)
yell out the teacher's name to get the teacher's attention. Do not
panic.
23. If a chemical should splash in your eye(s) or on your skin,
immediately flush with running water for at least 20 minutes.
Immediately (and loudly) yell out the teacher's name to get the
teacher's attention.
3
HANDLING CHEMICALS
24. All chemicals in the laboratory are to be considered
dangerous. Avoid handling chemicals with fingers. Always use a
tweezer.. When making an observation, keep at least 1 foot
away from the specimen. Do not taste, or smell any chemicals.
25. Check the label on all chemical bottles twice before
removing any of the contents. Take only as much chemical as
you need.
26. Never return unused chemicals to their original container.
27. Never remove chemicals or other materials from the
laboratory area.
HANDLING GLASSWARE AND
EQUIPMENT
28. Never handle broken glass with your bare hands. Use a
brush and dustpan to clean up broken glass. Place broken
glass in the designated glass disposal container.
29. Examine glassware before each use. Never use chipped,
cracked, or dirty glassware.
30. If you do not understand how to use a piece of equipment,
ASK THE TEACHER FOR HELP!
31. Do not immerse hot glassware in cold water. The glassware
may shatter.
HEATING SUBSTANCES
32. Do not operate a hot plate by yourself. Take care that hair,
clothing, and hands are a safe distance from the hot plate at all
times. Use of hot plate is only allowed in the presence of the
teacher.
33. Heated glassware remain very hot for a long time. They
should be set aside in a designated place to cool, and picked up
with caution. Use tongs or heat protective gloves if necessary.
34. Never look into a container that is being heated.
35. Do not place hot apparatus directly on the laboratory desk.
Always use an insulated pad. Allow plenty of time for hot
apparatus to cool before touching it.
4
5
R & S phrases
Indication of Particular Risks
R1:
Explosive when dry
35:
Causes severe burns
2:
Risk of explosion by shock, friction, fire or other sources of ignition
36:
Irritating to the eyes
3:
Extreme risk of explosion by shock, friction, fire or other sources of
ignition
37:
Irritating to the respiratory system
38:
Irritating to the skin
4:
Forms very sensitive explosive metallic compounds
39:
Danger of very serious irreversible effects
5:
Heating may cause an explosion
40:
Limited evidence of a carcinogenic effect
6:
Explosive with or without contact with air
41:
Risk of serious damage to eyes
7:
May cause fire
42:
May cause sensitization by inhalation
8:
Contact with combustible material may cause fire
43:
May cause sensitization by skin contact
9:
Explosive when mixed with combustible material
44:
Risk of explosion if heated under confinement
10:
Flammable
45:
May cause cancer
11:
Highly Flammable
46:
May cause heritable genetic damage
12:
Extremely Flammable
48:
Danger of serious damage to health by prolonged exposure
14:
Reacts violently with water
49:
May cause cancer by inhalation
15:
Contact with water liberates extremely flammable gases
50:
Very Toxic to aquatic organisms
16:
Explosive when mixed with oxidizing substances
51:
Toxic to aquatic organisms
17:
Spontaneously flammable in air
52:
Harmful to aquatic organisms
18:
In use may form flammable/explosive vapor-air mixture
53:
May cause long-term adverse effects in the aquatic environment
19:
May form explosive peroxides
54:
Toxic to flora
20:
Harmful by inhalation
55:
Toxic to fauna
21:
Harmful in contact with skin
56:
Toxic to soil organisms
22:
Harmful if swallowed
57:
Toxic to bees
23:
Toxic by inhalation
58:
May cause long-term adverse effects in the environment
24:
Toxic in contact with skin
59:
Dangerous for the ozone layer
25:
Toxic if swallowed
60:
May impair fertility
26:
Very Toxic by inhalation
61:
May cause harm to the unborn child
27:
Very Toxic in contact with skin
62:
Possible risk of impaired fertility
28:
Very Toxic if swallowed
63:
Possible risk of harm to the unborn child
29:
Contact with water liberates toxic gas
64:
May cause harm to breast-fed babies
30:
Can become highly flammable in use
65:
Harmful: May cause lung damage if swallowed
31:
Contact with acids liberates toxic gas
66:
Repeated exposure may cause skin dryness or cracking
32:
Contact with acids liberates very toxic gas
67:
Vapors may cause drowsiness and dizziness
33:
Danger of cumulative effects
68:
Possible risk of irreversible effects
34:
Causes burns
6
Combination of Risks
14/15:
Reacts violently with water, liberating extremely flammable gases
42/43:
May cause sensitization by inhalation and skin contact
15/29:
Contact with water liberates toxic, extremely flammable gas
48/20:
Harmful: danger of serious damage to health by prolonged exposure
through inhalation
20/21:
Harmful by inhalation and in contact with skin
48/20/21:
Harmful: danger of serious damage to health by prolonged exposure
through inhalation and in contact with skin
48/20/21/22:
Harmful: danger of serious damage to health by prolonged exposure
through inhalation, and in contact with skin and if swallowed
48/20/22:
Harmful: danger of serious damage to health by prolonged exposure
through inhalation and if swallowed
48/21:
Harmful: danger of serious damage to health by prolonged exposure in
contact with skin
48/21/22:
Harmful: danger of serious damage to health by prolonged exposure in
contact with skin and if swallowed
48/22:
Harmful: danger of serious damage to health by prolonged exposure if
swallowed
48/23:
Toxic: danger of serious damage to health by prolonged exposure through
inhalation
48/23/24:
Toxic: danger of serious damage to health by prolonged exposure through
inhalation and in contact with skin
20/21/22:
Harmful by inhalation, in contact with skin and if swallowed
20/22:
Harmful by inhalation and if swallowed
21/22:
Harmful in contact with skin and if swallowed
23/24:
Toxic by inhalation and in contact with skin
23/24/25:
Toxic by inhalation, in contact with skin and if swallowed
23/25:
Toxic by inhalation and if swallowed
24/25:
Toxic in contact with skin and if swallowed
26/27:
Very Toxic by inhalation and in contact with skin
26/27/28:
Very Toxic by inhalation, in contact with skin and if swallowed
26/28:
Very Toxic by inhalation and if swallowed
27/28:
Very Toxic in contact with skin and if swallowed
36/37:
Irritating to eyes and respiratory system
36/37/38:
Irritating to eyes, respiratory system and skin
36/38:
Irritating to eyes and skin
37/38:
Irritating to respiratory system and skin
39/23:
Toxic: danger of very serious irreversible effects through inhalation
39/23/24:
Toxic: danger of very serious irreversible effects through inhalation in
contact with skin
39/23/24/25:
Toxic: danger of very serious irreversible effects through inhalation, in
contact with skin and if swallowed
39/23/25:
Toxic: danger of very serious irreversible effects through inhalation and if
swallowed
39/24:
Toxic: danger of very serious irreversible effects in contact with skin
39/24/25:
Toxic: danger of very serious irreversible effects in contact with skin and if
swallowed
39/25:
Toxic: danger of very serious irreversible effects if swallowed
39/26:
Very Toxic: danger of very serious irreversible effects through inhalation
39/26/27:
Very Toxic: danger of very serious irreversible effects through inhalation
and in contact with skin
48/23/24/25: Toxic: danger of serious damage to health by prolonged exposure through
inhalation, in contact with skin and if swallowed
Very Toxic: danger of very serious irreversible effects through inhalation
and if swallowed
39/27:
Very Toxic: danger of very serious irreversible effects in contact with skin
39/27/28:
Very Toxic: danger of very serious irreversible effects in contact with skin
and if swallowed
39/28:
Very Toxic: danger of very serious irreversible effects if swallowed
Toxic: danger of serious damage to health by prolonged exposure through
inhalation and if swallowed
48/24:
Toxic: danger of serious damage to health by prolonged exposure in
contact with skin
48/24/25:
Toxic: danger of serious damage to health by prolonged exposure in
contact with skin and if swallowed
48/25:
Toxic: danger of serious damage to health by prolonged exposure if
swallowed
50/53:
Very Toxic to aquatic organisms, may cause long-term adverse effects in
the aquatic environment
51/53:
Toxic to aquatic organisms, may cause long-term adverse effects in the
aquatic environment
52/53:
Harmful to aquatic organisms, may cause long-term adverse effects in the
aquatic environment
68/20:
Harmful: possible risk of irreversible effects through inhalation
68/20/21:
Harmful: possible risk of irreversible effects through inhalation and in
contact with skin
68/20/21/22: Harmful: possible risk of irreversible effects through inhalation, in contact
with skin and if swallowed
39/26/27/28: Very Toxic: danger of very serious irreversible effects through inhalation,
in contact with skin and if swallowed
39/26/28:
48/23/25:
7
68/20/22:
Harmful: possible risk of irreversible effects through inhalation and if
swallowed
68/22:
Harmful: possible risk of irreversible effects if swallowed
68/21:
Harmful: possible risk of irreversible effects in contact with skin
68/21/22:
Harmful: possible risk of irreversible effects in contact with skin and if
swallowed
68/22:
Harmful: possible risk of irreversible effects if swallowed
Indication of Safety Precautions
S1: Keep locked up
37: Wear suitable gloves
2: Keep out of the reach of children
38: In case of insufficient ventilation, wear suitable respiratory equipment
3: Keep in a cool place
39: Wear eye/face protection
4: Keep away from living quarters
40: To clean the floor and all objects contaminated by this material use ... (to
be specified by the manufacturer)
5: Keep contents under ... (appropriate liquid to be specified by the
manufacturer)
41: In case of fire and/or explosion do not breathe fumes
6: Keep under ... (inert gas to be specified by the manufacturer)
42: During fumigation/spraying wear suitable respiratory equipment
(appropriate wording to be specified)
7: Keep container tightly closed
43: In case of fire, use ... (indicate in the space the precise type of fire-fighting
equipment. If water increases the risk add - Never use water)
8: Keep container dry
45: In case of accident or if you feel unwell, seek medical advice immediately
(show label where possible)
9: Keep container in a well-ventilated place
12: Do not keep the container sealed
46: If swallowed, seek medical advice immediately and show this container or
label
13: Keep away from food, drink and animal feeding stuffs
47: Keep at temperature not exceeding ... E C (to be specified by the
manufacturer)
14: Keep away from ... (incompatible materials to be indicated by the
manufacturer)
48: Keep wetted with ... (appropriate material to be specified by the
manufacturer)
15: Keep away from heat
49: Keep only in the original container
16: Keep away from sources of ignition - No smoking
50: Do not mix with ... (to be specified by the manufacturer)
17: Keep away from combustible material
51: Use only in well-ventilated areas
18: Handle and open container with care
52: Not recommended for interior use on large surface areas
20: When using, do not eat or drink
53: Avoid exposure - obtain special instruction before use
21: When using, do not smoke
22: Do not breathe dust
56: Dispose of this material and its container to hazardous or special waste
collection point
23: Do not breathe gas/fumes/vapor/spray (appropriate wording to be specified
by the manufacturer)
57: Use appropriate container to avoid environmental contamination
59: Refer to manufacturer/supplier for information on recovery/recycling
24: Avoid contact with skin
60: This material and/or its container must be disposed of as hazardous waste
25: Avoid contact with eyes
61: Avoid release to the environment. Refer to special instructions safety data
sheet
26: In case of contact with eyes, rinse immediately with plenty of water and
seek medical advice
62: If swallowed, do not induce vomiting: seek medical advice immediately and
show this container or label
27: Take off immediately all contaminated clothing
28: After contact with skin, wash immediately with plenty of ... (to be specified
by the manufacturer)
63: In case of accident by inhalation, remove casualty to fresh air and keep at
rest
29: Do not empty into drains
64: If swallowed, rinse mouth with water (only if the person is conscious)
30: Never add water to this product
33: Take precautionary measures against static discharges
35: This material and its container must be disposed of in a safe way
36: Wear suitable protective clothing
8
Code
Hazard statements
Hazard class
Category
Signal
word
Pictogram
P-Codes
H200
Unstable Explosive
Explosives
Unstable Explosive
Danger
P201, P202, P281, P372, P373, P380,
P401, P501
H201
Explosive; mass explosion hazard
Explosives
Div 1.1
Danger
P210, P230, P240, P250, P280,
P370+P380, P372, P373, P401, P501
H202
Explosive; severe projection hazard
Explosives
Div 1.2
Danger
P210, P230, P240, P250, P280,
P370+P380, P372, P373, P401, P501
H203
Explosive; fire, blast or projection hazard
Explosives
Div 1.3
Danger
P210, P230, P240, P250, P280,
P370+P380, P372, P373, P401, P501
H204
Fire or projection hazard
Explosives
Div 1.4
Warning
P210, P240, P250, P280, P370+P380,
P372, P373, P374, P401, P501
H205
May mass explode in fire
Explosives
Div 1.5
Danger
P210, P230, P240, P250, P280,
P370+P380, P372, P373, P401, P501
H220
Extremely flammable gas
Flammable gases
Category 1
Danger
P210, P377, P381, P403
H221
Flammable gas
Flammable gases
Category 2
Warning
P210, P377, P381, P403
H222
Extremely flammable aerosol
Flammable aerosols
Category 1
Danger
P210, P211, P251, P410+P412
H223
Flammable aerosol
Flammable aerosols
Category 2
Warning
H224
Extremely flammable liquid and vapour
Flammable liquids
Category 1
Danger
H225
Highly Flammable liquid and vapour
Flammable liquids
Category 2
Danger
H226
Flammable liquid and vapour
Flammable liquids
Category 3
Warning
Div 1.6
H227
Combustible liquid
Flammable liquids
Category 4
Warning
H228
Flammable solid
Flammable solids
Category 1
Danger
H228
Flammable solid
Flammable solids
Category 2
Warning
P210, P211, P251, P410+P412
P210,P233, P240, P241, P242, P243,
P280, P303+ P361+P353, P370+P378,
P403+P235, P501
P210, P280, P370+P378, P403+P235,
P501
P210, P240,P241, P280, P370+P378
P210, P220, P234, P280, P370+ P378,
P370+ P380+P375, P403+P235, P411,
P420, P501
P210, P220, P234, P280, P370+P378,
P370+ P380+P375, P403+P235, P411,
P420, P501
H240
Heating may cause an explosion
Self-reactive substances and mixtures; and Organic
peroxides
Type A
Danger
H241
Heating may cause a fire or explosion
Self-reactive substances and mixtures; and
Organic peroxides
Type B
Danger
H242
Heating may cause a fire
Self-reactive substances and mixtures; and
Organic peroxides
Type C, D,
Danger
P210, P220, P234, P280, P370+P378,
P403+P235, P411, P420, P501
H242
Heating may cause a fire
Self-reactive substances and mixtures; and
Organic peroxides
Type E, F
Warning
P210, P220, P234, P280, P370+P378,
P403+P235, P411, P420, P501
P210, P222, P280, P302+P334,
P370+P378, P422
Type G
H250
Catches fire spontaneously if exposed to air
Pyrophoric liquids; Pyrorophoric solids
Category 1
Danger
H251
Self-heating; may catch fire
Self-heating in large quantities; may catch fire
Self-heating substances and mixtures
Self-heating substances and mixtures
Category 1
Danger
H260
In contact with water releases flammable gases which may
ignite spontaneously
H261
In contact with water releases flammable gas
Substances And Mixtures Which, In Contact With Water,
Emit Flammable Gases
Substances And Mixtures Which, In Contact With Water,
Emit Flammable Gases
H261
In contact with water releases flammable gas
H270
H252
Category 2
Warning
Category 1
Danger
Category 2
Danger
Substances And Mixtures Which, In Contact With Water,
Emit Flammable Gases
Category 3
Warning
May cause or intensify fire; oxidizer
Oxidising gases
Category 1
Danger
H271
May cause fire or explosion; strong oxidiser
Oxidising liquids;Oxidising solids
Category 1
Danger
H272
May intensify fire; oxidizer
Oxidising liquids;Oxidising solids
Category 2
Danger
H272
May intensify fire; oxidizer
Oxidising liquids;Oxidising solids
Category 3
Warning
Warning
P235+P410, P280, P407, P413, P420
P223, P231+P232, P280, P335+ P334,
P370+P378, P402+P404, P501
P231+P232, P280, P370+P378,
P402+P404, P501
P220, P244, P370+P376, P403
P210, P220, P221, P280, P283,
P306+P360, P371+P380+P375,
P370+P378, P501
P210, P220, P221P280, P370+P378,
P501
H280
Contains gas under pressure; may explode if heated
Gases under pressure
Compressed gas
Liquefied gas
Dissolved gas
H281
Contains refrigerated gas; may cause cryogenic burns or injury
Gases under pressure
Refrigerated liquefied
gas
Warning
H290
May be corrosive to metals
Corrosive to Metals
Category 1
Warning
H300
Fatal if swallowed
Acute toxicity,oral
Category 1, 2
Danger
P264, P270, P301+P310, P321, P330,
P405, P501
H301
Toxic if swalloed
Acute toxicity,oral
Category 3
Danger
P264, P270, P301+P310, P321, P330,
P405, P501
Warning
P410+P403
P282, P336, P315, P403
P234, P390, P404
H302
Harmful if swallowed
Acute toxicity,oral
Category 4
H303
May be harmfulif swallowed
Acute toxicity,oral
Category 5
H304
May be fatal if swallowed and enters airways
Aspiration hazard
Category 1
Danger
H305
May be fatal if swallowed and enters airways
Aspiration hazard
Category 2
Warning
H310
Fatal in contact with skin
Acute toxicity,dermal
Category 1, 2
Danger
H311
Toxic in contact with skin
Acute toxicity,dermal
Category 3
Danger
P280, P302+P352, P312, P322, P361,
P363, P405, P501
Warning
P280,P302+P352, P312, P322, P363,
P501
P312
P260,P264, P280, P301+P330+ P331,
P303+P361+P353, P363, P304+P340,
P310, P321, P305+ P351+P338, P405,
P501
H312
Harmful in contact with skin
Acute toxicity,dermal
Category 4
H313
May be harmful in contact with skin
Acute toxicity,dermal
Category 5
H314
Causes severe skin burns and eye damage
Skin corrosion/irritation
Category 1A, B, C
Danger
H315
Causes skin irritation
Skin corrosion/irritation
Category 2
Warning
H316
Causes mild skin irritation
Skin corrosion/irritation
Category 3
Warning
H317
May cause an allergic skin reaction
Sensitisation, Skin
Category 1
Warning
Page 1 / 2
P264, P270, P301+P312, P330, P501
P312
P301+P310, P331, P405, P501
P262, P264, P270, P280, P302+P350,
P310, P322, P361, P363, P405, P501
P264, P280, P302+P352, P321,
P332+P313, P362
P332+P313
P261, P272, P280, P302+P352,
P333+P313, P321, P363, P501
H318
Causes serious eye damage
Serious eye damage/eye irritation
Category 1
Danger
H319
Causes serious eye irritation
Serious eye damage/eye irritation
Category 2A
Warning
P264, P280, P305+P351+P338,
P337+P313P
H320
Causes eye irritation
Serious eye damage/eye irritation
Category 2B
Warning
P264, P305+P351+P338,
P337+P313
H330
Fatal if inhaled
Acute toxicity,inhalation
Category 1, 2
Danger
H331
Toxic if inhaled
Acute toxicity,inhalation
Category 3
Danger
Warning
P280, P305+P351+P338, P310
H332
Harmful if inhaled
Acute toxicity,inhalation
Category 4
H333
May be harmful if inhaled
Acute toxicity,inhalation
Category 5
H334
May cause allergy or asthma symptoms or breathing
difficulties if inhaled
Sensitisation, respiratory
Category 1
Danger
H335
May cause respiratory irritation
Category 3
Warning
H336
May cause drowsiness or dizziness
Category 3
Warning
Specific target organ toxicity, single exposure;
Respiratory tract irritation
Specific target organ toxicity,single exposure; Narcotic
effects
H340
May cause genetic defects
Germ cell mutagenicity
Category 1A, 1B
Danger
H341
H350
Suspected of causing genetic defects
Germ cell mutagenicity
Category 2
Warning
May cause cancer
Carcinogenicity
Category 1A, 1B
Danger
H351
Suspected of causing cancer
Carcinogenicity
Category 2
Warning
P260, P271, P284, P304+P340, P310,
P320, P403+P233, P405, P501
P261, P271, P304+P340, P311, P321,
P403+P233, P405, P501
P261, P271, P304+P340, P312
P304+P312
P261, P285, P304+P341, P342+P311,
P501
P261, P271, P304+P340, P312,
P403+P233, P405, P501
P201,P202, P281, P308+P313, P405,
P501
P201, P202, P281, P308+P313, P405,
P501
H360
May damage fertility or the unborn child
Reproductive toxicity
Category 1A, 1B
Danger
H361
Suspected of damaging fertility or the unborn child
Reproductive toxicity
Category 2
Warning
P201, P202, P281, P308+P313, P405,
P501
P201, P260, P263, P264, P270,
P308+P313
P260, P264, P270, P307+P311, P321,
P405, P501
P260, P264, P270, P309+P311, P405,
P501
H362
May cause harm to breast-fed children
Reproductive toxicity, effects on or via lactation
Additional category
H370
Causes damage to organs
Specific target organ toxicity, single exposure
Category 1
Danger
H371
H372
H373
H400
May cause damage to organs
Causes damage to organs through prolonged or
repeated exposure
Causes damage to organs through prolonged or
repeated exposure
Very toxic to aquatic life
Specific target organ toxicity, single exposure
Category 2
Warning
Specific target organ toxicity, repeated exposure
Category 1
Danger
P260, P264, P270, P314, P501
Specific target organ toxicity, repeated exposure
Category 2
Warning
P260, P314, P501
Hazardous to the aquatic environment, acute
hazard
Category 1
Warning
P273, P391, P501
Hazardous to the aquatic environment, acute
hazard
Hazardous to the aquatic environment, acute
hazard
Hazardous to the aquatic environment, long-term
hazard
Hazardous to the aquatic environment, long-term
hazard
Hazardous to the aquatic environment, long-term
hazard
H401
Toxic to aquatic life
H402
Harmful to aquatic life
H410
Very toxic to aquatic life with long lasting effects
H411
Toxic to aquatic life with long lasting effects
H412
Harmful to aquatic life with long lasting effects
H413
May cause long lasting harmful effects to aquatic life
Hazardous to the aquatic environment, long-term
hazard
Category 4
H420
Harms public health and the environment by destroying
ozone in the upper atmosphere
Hazardous to the ozone layer
Category 1
Additional Hazard statements - EU Left-overs
EUH001
Explosive when dry
EUH006
Explosive with or without contact with air
EUH014
Reacts violently with water
EUH018 In use may form flammable/explosive vapour-air mixture
EUH019
May form explosive peroxides
EUH029
Contact with water liberates toxic gas
EUH031
Contact with acids liberates toxic gas
EUH032
Contact with acids liberates very toxic gas
EUH044
Risk of explosion if heated under confinement
EUH059
Hazardous to the ozone layer
EUH066 Repeated exposure may cause skin dryness or cracking
EUH070
Toxic by eye contact
Page 2 / 2
Category 2
P273, P501
Category 3
Category 1
Warning
P273, P391, P501
Category 2
Category 3
P273, P501
Warning
P502
Precautionary statements - General
P101
P102
P103
If medical advice is needed,have product container or label at hand.
Keep out of reach of children.
Read label before use
Precautionary statements — Prevention
P201
P202
P210
P211
P220
P221
P222
P223
P230
P231
P232
P233
P234
P235
P240
P241
P242
P243
P244
P250
P251
P260
P261
P262
P263
P264
P264
P270
P271
P272
P273
P280
P281
P282
P283
P284
P285
P231 + P232
P235 + P410
Obtain special instructions before use.
Do not handle until all safety precautions have been read and understood.
Keep away from heat/sparks/open flames/hot surfaces. — No smoking.
Do not spray on an open flame or other ignition source.
Keep/Store away from clothing/…/combustible materials.
Take any precaution to avoid mixing with combustibles/…
Do not allow contact with air.
Keep away from any possible contact with water, because of violent reaction and possible flash fire.
Keep wetted with …
Handle under inert gas.
Protect from moisture.
Keep container tightly closed.
Keep only in original container.
Keep cool.
Ground/bond container and receiving equipment.
Use explosion-proof electrical/ventilating/lighting/…/equipment.
Use only non-sparking tools.
Take precautionary measures against static discharge.
Keep reduction valves free from grease and oil.
Do not subject to grinding/shock/…/friction.
Pressurized container: Do not pierce or burn, even after use.
Do not breathe dust/fume/gas/mist/vapours/spray.
Avoid breathing dust/fume/gas/mist/vapours/spray.
Do not get in eyes, on skin, or on clothing.
Avoid contact during pregnancy/while nursing.
Wash hands thoroughly after handling.
Wash skin thouroughly after handling.
Do not eat, drink or smoke when using this product.
Use only outdoors or in a well-ventilated area.
Contaminated work clothing should not be allowed out of the workplace.
Avoid release to the environment.
Wear protective gloves/protective clothing/eye protection/face protection.
Use personal protective equipment as required.
Wear cold insulating gloves/face shield/eye protection.
Wear fire/flame resistant/retardant clothing.
Wear respiratory protection.
In case of inadequate ventilation wear respiratory protection.
Handle under inert gas. Protect from moisture.
Keep cool. Protect from sunlight.
Precautionary statements — Response
P301
P304
P305
P306
P307
P308
P309
P310
P311
P312
P313
P314
P315
IF SWALLOWED:
IF INHALED:
IF IN EYES:
IF ON CLOTHING:
IF exposed:
IF exposed or concerned:
IF exposed or if you feel unwell:
Immediately call a POISON CENTER or doctor/physician.
Call a POISON CENTER or doctor/physician.
Call a POISON CENTER or doctor/physician if you feel unwell.
Get medical advice/attention.
Get medical advice/attention if you feel unwell.
Get immediate medical advice/attention.
Page 1 / 3
P320
P321
P322
P330
P331
P332
P333
P334
P335
P336
P337
P338
P340
P341
P342
P350
P351
P352
P353
P360
P361
P362
P363
P370
P371
P372
P373
P374
P376
P377
P378
P380
P381
P390
P391
P301 + P310
P301 + P312
P301 + P330 + P331
P302 + P334
P302 + P350
P302 + P352
P303 + P361 + P353
P304 + P312
P304 + P340
P304 + P341
P305 + P351 + P338
P306 + P360
P307 + P311
P308 + P313
P309 + P311
P332 + P313
P333 + P313
P335 + P334
P337 + P313
P342 + P311
P370 + P376
P370 + P378
P370 + P380
P370 + P380 + P375
P371 + P380 + P375
Specific treatment is urgent (see … on this label).
Specific treatment (see … on this label).
Specific measures (see …on this label).
Rinse mouth.
Do NOT induce vomiting.
IF SKIN irritation occurs:
If skin irritation or rash occurs:
Immerse in cool water/wrap n wet bandages.
Brush off loose particles from skin.
Thaw frosted parts with lukewarm water. Do not rub affected area.
If eye irritation persists:
Remove contact lenses, if present and easy to do. Continue rinsing.
Remove victim to fresh air and keep at rest in a position comfortable for breathing.
If breathing is difficult, remove victim to fresh air and keep at rest in a position comfortable for breathing.
If experiencing respiratory symptoms:
Gently wash with plenty of soap and water.
Rinse cautiously with water for several minutes.
Wash with plenty of soap and water.
Rinse skin with water/shower.
Rinse immediately contaminated clothing and skin with plenty of water before removing clothes.
Remove/Take off immediately all contaminated clothing.
Take off contaminated clothing and wash before reuse.
Wash contaminated clothing before reuse.
In case of fire:
In case of major fire and large quantities:
Explosion risk in case of fire.
DO NOT fight fire when fire reaches explosives.
Fight fire with normal precautions from a reasonable distance.
Stop leak if safe to do so. Oxidising gases (section 2.4) 1
Leaking gas fire: Do not extinguish, unless leak can be stopped safely.
Use … for extinction.
Evacuate area.
Eliminate all ignition sources if safe to do so.
Absorb spillage to prevent material damage.
Collect spillage. Hazardous to the aquatic environment
IF SWALLOWED: Immediately call a POISON CENTER or doctor/physician.
IF SWALLOWED: call a POISON CENTER or doctor/physician IF you feel unwell.
IF SWALLOWED: Rinse mouth. Do NOT induce vomiting.
IF ON SKIN: Immerse in cool water/wrap in wet bandages.
IF ON SKIN: Gently wash with plenty of soap and water.
IF ON SKIN: wash with plenty of soap and water.
IF ON SKIN (or hair): Remove/Take off Immediately all contaminated clothing. Rinse SKIN with water/shower.
IF INHALED: Call a POISON CENTER or doctor/physician if you feel unwell.
IF INHALED: Remove victim to fresh air and Keep at rest in a position comfortable for breathing.
IF INHALED: If breathing is difficult, remove victim to fresh air and keep at rest in a position comfortable for breathing.
IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. Continue
rinsing.
IF ON CLOTHING: Rinse Immediately contaminated CLOTHING and SKIN with plenty of water before removing clothes.
IF exposed: call a POISON CENTER or doctor/physician.
IF exposed or concerned: Get medical advice/attention.
IF exposed or if you feel unwell: call a POISON CENTER or doctor/physician.
IF SKIN irritation occurs: Get medical advice/attention.
IF SKIN irritation or rash occurs: Get medical advice/attention.
Brush off loose particles from skin. Immerse in cool water/wrap in wet bandages.
IF eye irritation persists: Get medical advice/attention.
IF experiencing respiratory symptoms: call a POISON CENTER or doctor/physician.
in case of fire: Stop leak if safe to Do so.
In case of fire: Use … for extinction.
in case of fire: Evacuate area.
in case of fire: Evacuate area. Fight fire remotely due to the risk of explosion.
in case of major fire and large quantities: Evacuate area. Fight fire remotely due to the risk of explosion.
Precautionary statements — Storage
P401
P402
P403
P404
Store …
Store in a dry place.
Store in a well-ventilated place.
Store in a closed container.
Page 2 / 3
IA9000 SERIES
Digital Melting Point
Apparatus
Operating and
Safety Instructions
Upon receipt of the instrument proceed consecutively as follows:4.2.1
Power Supply.
The power supply supplied with your new IA 9100 supports all A.C.
Mains supply voltages within the range of 100V to 240V inclusive at
50-60Hz. Do not use the power supply with a D.C. supply voltage or in
conjunction with any type of voltage regulation equipment. Do not use
with a mains supply supplying power at a different frequency other than
that stated.
4.2.2
Set-Up
N.B. DO NOT ATTEMPT TO MOVE ADJUSTMENT ARM BEFORE
RELEASING CLAMP SCREWS. (See Figure 2).
After releasing the clamp screws, adjust the angle and extension of the
arm, and rotate the oven head if required in order to establish the most
comfortable viewing position; re-tighten screws.
Do not over tighten.
10
4.2.3
Connections.
a)
Insert the jack connection Plug from the Power Supply Unit
into the instrument supply socket.
b)
Connect the Power Supply mains cable to the Power Supply
Unit.
c)
Plug the Mains power supply cable into the supply outlet.
4.2.4
Start up.
Switch the power on.
Observe all indicator lights flash momentarily and then the display rolls
from 9999 to 0000 and settles at the oven ambient temperature.
NOTE: In order to attain maximum accuracy from the unit it is
important to allow all components to stabilise at their working
temperature. It is recommended therefore that the unit is switched on
for 30 minutes before use.
Alternatively the unit may be switched on overnight at ambient
temperature. The bulb will supply sufficient heat to maintain stability.
The insulation material of the oven may absorb small amounts of
moisture if left un-powered for any length of time (dependant upon
ambient conditions). It is suggested the oven is heated up to a
temperature of 400"C before use as described in sections 4.2.6 and
4.2.7, with the removed, and then allowed to cool, switching the oven
off as in section 4.12.13 before replacing the lens.
11
4.2.5
Prepare a Sample
Up to three samples may be accommodated in the tube
guide. To prepare a sample proceed as follows:
Break a new capillary tube in half and insert the powdered
sample in the tube. The quantity should be such that the
height dose no exceed 1mm.
Locate the sample in the tube guide. It is recommended
that three tubes are inserted even if each tube dose not
contain a sample.
4.2.6
Enter the ‘set Point’
(This should be 2 to 5"C below the expected melt point).
Proceed as follows (a figure of 107"C is given as an example):Press arrow UP key eleven times (value 10"C per keystroke) to
set a temperature of 110"C.
Press the arrow DOWN key three times (value –1"C per key
stroke) to reduce the ‘set-point’ to 107"C.
If an error is made, press the CLEAR key and recommence
entering the set point.
4.2.7
GOTO ‘Set Point’
Press GOTO key.
The four bar L.E.D’s will illuminate consecutively as the
temperature rises.
To review the ‘Set Point’ Press the UP arrow key and the
‘Set Point’ will be displayed for approximately 1 second.
When the ‘Set Point’ temperature is reached the left hand
L.E.D. on the GOTO key will illuminate and three audible
bleeps will sound to indicate the temperature has
stabilised.
4.2.8
Initiate Ramp.
Press GOTO to initiate the temperature ramp of 1.0"C per
minute. The four bar L.E.D’s and the left hand L.D.D on the
GOTO will go out. The right-hand L.E.D will illuminate.
After a brief delay the oven temperature will commence to rise at
1.0"C per minute.
4.2.8a
Fast Ramp Selection – See Appendix B (Page 27).
12
4.2.9
Analysis and Storage of Melt points.
The four basic stages of melting should be
anticipated as described in Principals of Operation on
Page 6. Proceed as follows:
Adjust the object lens by rotation until a sharp focus
on the sample is obtained.
When the desired stage of melt is observed press the
GOTO key to store that temperature in the memory.
Up to four values can be stored. An additional L.E.D.
above the GOTO key will illuminate as each value is
stored. After the fourth value is stored the oven
temperature will return to the ‘Set Point’.
N.B. If less than four melt points are to be stored,
press the CLEAR key once only after the last
temperature has been stored, the oven temperature
will return to ‘Set Point’.
4.2.10
Recall of Information.
To review the melt points:
The display will show the temperature of each
successive melt point held in the memory with each
subsequent depression of the GOTO key. An L.E.D.
above the GOTO will indicate which of the stored
temperatures is being displayed. If less than four
temperatures have been recorded then unused
memory will be displayed by 0000.
N.B. Temperatures must be recorded on paper at this
point.
4.2.11
To Carry out further melt
a)
Press CLEAR only once. The current ‘Set Point’ will
be displayed. If this is the value desired, press GOTO
keys as in section 4.2.7.
b)
If a new ‘Set Point’ is desired press the UP/DOWN
keys as in section 4.2.6. Press GOTO key as in
section 4.2.7. Do not insert new samples until
temperature has stabilised at the new ‘Set Point’ (as
indicated in section 4.2.7). After insertion allow 2
minutes for tubes and samples to stabilise at the ‘Set
Point’ before initiating ramp as in section 4.2.8.
N.B. Faster cooling where required can be achieved
by the insertion of a Cold Finger (Accessory AZ9001).
13
4.2.12
CLEAR Key.
The CLEAR key may be operated at any time and
will, depending upon the current stage, function as
follows:
1.
If as section 4.2.6 operation of the CLEAR key will
reset display to 0000
2.
If at section 4.2.7 by pressing CLEAR key the display
will show oven temperature and heater will control to
’Set point’.
2a.
Press CLEAR again and display shows 0000. Enter
new ‘Set Point’ as described in section 4.2.6
3.
If at section 4.2.8, pressing CLEAR once will prevent
further entry into the memory of the melt points, and
the oven will revert to ‘Set Point’.
4.
Pressing CLEAR again will display current ‘Set Point’
– proceed at section 4.2.6
4.2.13
Oven off
Pressing CLEAR key three times during any stage
will turn off the heating to the oven.
14
Basic Laboratory Operations II
EXPERIMENT 1
Determining the atomic mass of magnesium (Mg)
Name:
Date:
1.- Introduction
The reaction of magnesium with an acid solution (HCl in this experiment) produces
hydrogen gas. The atomic mass of magnesium –expressed in grams– can be calculated by
measuring the volume of hydrogen gas produced when hydrochloric acid is added to a given
quantity of magnesium whose weight is known.
2.- Main aims of the experiment and learning outcomes
1. Calculating the atomic mass of a metal by measuring the amount of hydrogen
produced.
2. Building an appropriate apparatus for the reaction between a metal and an acid
solution.
3. Learning the general properties of metals and hydrogen.
3.- Pre-laboratory work
1. Learn the English terms and phrases used to refer to the labware tools and
equipment required for this experiment.
2. Focus on and enumerate the physical properties of hydrogen H2, copper Cu and
magnesium Mg.
3. Look for a table that shows the relationship between H2 vapor and temperature.
4. Consider the standard potentials of reduction for Eº(Cu2+/Cu) and Eº(Mg2+/Mg).
5. Calculate how to prepare 1 L of HCl solution (6M) from another solution of HCl (37%)
with a density of 1.19 g/mL.
6. Be aware of the risks embedded in the experiment and adopte all the security
measures needed when deal with reagents such as the ones used in this experiment.
7. References
1
Basic Laboratory Operations II
4.- Laboratory work:
Material
Laboratory stand with clamps
One graduated test tube with a cork
500 mL graduated beaker
Products
A 6 M solution of HCl.
Magnesium ribbon.
A spiral of copper wire
Procedure
Weigh a piece of magnesium ribbon between 2 and 3 centimeters long with a precision
of +/- 0.001g. Wind the magnesium ribbon onto a thick copper wire spiral attached to a cork
stopper. You may need to drill a small hole in the cork yourself –so that it fits snugly.
Separately, add 6 mL of a 6-8 M HCl solution into a test tube graduated in terms of
volume (± 1 mL). Then add enough distilled water to fill it up: this must be done with extreme
care, so as to avoid (as much as possible) mixing water with the acid added previously. As
you carefully drop the liquid into the test tube, make sure to sweep away any remains of acid
left in the mouth of the vial, which must be clean before going on with the experiment.
Should any bubbles stick to its inner walls after the filling process, tap the test tube gently
with your fingers until they come off.
Once the previous step is complete, plug the cork into the test tube, making sure it fits
perfectly. The copper wire spiral plus the piece of magnesium ribbon will be submerged in
the water. Remember that, after plugging the cork, no air bubbles must remain inside the
vial. The possible mixture of the water with the HCl solution must be avoided, too.
Using your finger to cover the hole of the cork stopper, turn the test tube invert the test
tube. Without bringing it back to the original position, put it inside a 500 mL graduated
beaker and clamp it onto the stand –so that it is held in vertical position (check figure 1). The
acid, denser than water, will diffuse at that point and react with the magnesium wound onto
the spiral. At this point, tap the test tube lightly for a few minutes so as to remove any
bubbles from its (inner) sides. Subsequently, read the volume of hydrogen inside the tube.
This experiment must be carried out twice. The average of both results will be taken as the
final atomic mass value obtained in this experiment.
3
Basic Laboratory Operations II
Figure 1
5.- Post-laboratory work
Note down the following data. They will be needed during the calculation process:
a)
Results and calculations
Gas Temperature:
............................................................................................. ºC
Atmospheric pressure: ............................................................................................. atm
Water steam pressure: ............................................................................................. atm
Exper
T
(ºC)
P
(atm)
Pv (H2O)
(atm)
m(Mg)
(g)
1º
2º
4
V(H2)
(mL)
Mat(Mg)
(g)
Error
(%)
Operaciones Básicas de Laboratorio II
b) Discussion and justification of results
1.
Write down the reaction between magnesium and chlorhydric acid.
2.
Why is it important to prevent water and HCl from mixing before inverting the test tube?
3.
Why does HCl react with magnesium but not with copper?
4.
In your opinion, how may the presence of inert impurities in the magnesium ribbon
affect the experimental value of the atomic mass obtained in the experiment? Would
the results be higher or lower than normal?
5.
Hydrogen is soluble in water: at 25ºC, 0.0193 L of hydrogen will dissolve in 1 L of
water. How do you think this will affect the value of the atomic mass obtained in the
experiment? Would the results be higher or lower than normal?
6
Basic Laboratory Operations II
EXPERIMENT 2
Determining the molecular mass of CO2
Name:
Date:
1. Introduction
A well-known fact is that the mole of a substance such as CO2 (carbon dioxide) is the
mass, expressed in grams, of 6,022.1023 of its molecules (Avogadro`s number). This
coincides numerically with its molecular mass –that is, the mass of one of its molecules,
usually expressed in atomic mass units.
One mole of any ideal gas, held at the standard conditions of 1 atm pressure and 0ºC,
occupies a volume of 22.4 L. This is the so-called ‘molar volume’ of an ideal gas. It is used
as a reference to determine the amount of gas in a given volume. The just mentioned
conditions are used whenever comparing the volume of different ideal gases. This explains
why they are known as Standard Temperature and Pressure (often abbreviated STP).
Therefore, if one measures the mass of a given volume of laboratory-obtained gas
(CO2 in our current experiment), a simple rule of proportion may be accordingly applied to
calculate the mass of 22.4 L under standard conditions –plus its molecular mass in amu
(atomic mass units).
The gas whose molecular weight we aim to calculate here can be produced through
the reaction between chlorhydric acid and calcium carbonate. The latter is usually found in
great abundance in commercial marble.
2.- Main aims of the experiment and learning outcomes
1. Becoming familiar with the tools and equipment needed to generate and collect a gas
under standard temperature and pressure conditions.
2. Calculating the molecular mass of a substance (CO2) in gaseous state at room
temperature and pressure.
3. Measuring temperature and atmospheric pressure.
3.- Pre-laboratory work
1. Consider the English words used to refer to the different labware tools and items
required in this experiment.
2. Enumerate the physical properties of CaCO3 (calcium carbonate), CaCl2 (calcium
chloride), CO2 (carbon dioxide) and HCl (hydrochloric acid).
3. Be aware of the risks associated with the reagents used in the experiment and
highlight the corresponding security measures that need to be applied.
4. References
1
Basic Laboratory Operations II
4.- Laboratory work
Material
- Laboratory stand and clamps.
- Dropping funnel
- U-shaped tube (with openings near both ends)
- 250 mL two-neck balloon flask
- 250 mL one-neck balloon flask
- Cork ring
Products
- Commercial marble
- Concentrated hydrochloric acid HCl
- Calcium chloride
Procedure
Put 20 g of commercial marble into flask A (see figure 1) and add a measured amount
of water –just enough to cover it. Make sure flask B, into which carbon dioxide is to be
collected later, is clean and dry (it is advisable to keep it in a drying chamber for as long as
necessary, prior to the experiment). Insert an L-shaped tube into flask B: the end inside must
remain one centimeter far from its bottom.
Before the experiment starts, flask B (filled with air at room pressure and temperature)
needs to be weighed at an accuracy of 0.01 g. From thence onwards, with a view to avoid
any errors when determining the mass of the gas, the flask must not be touched unless
necessary –and, in such a case it may be held only by the neck. During this process, a cork
ring will keep the flask upright –this support must be weighed together with the flask.
Subsequently, a U-shaped drying tube containing a hygroscopic substance (CaCl2) will
be attached to the flask using a rubber septum. Once assembled, the whole apparatus will
look as shown in the following figure.
3
Basic Laboratory Operations II
Figure 1
After completing all these preparations, use a dropping funnel to pour concentrated
hydrochloric acid HCl onto the marble chips in flask A. The reaction between hydrochloric
acid HCl and calcium carbonate CaCO3 will start right at that point: carbon dioxide will come
out in the form of bubbles. Keep the gas flow for 20 minutes –enough for flask B to get filled
with dry carbon dioxide. Disconnect the tube attached to flask B (remember to hold the flask
by the neck) and repeat the weighing process. Subsequently, fill up the flask with (bubbleless) tap water to the brim –then pour this amount of water into a graduated test tube to
measure its volume. Note that it must be equivalent to that of the obtained carbon dioxide
and to the initial amount (volume) of air in the flask. Finally, note down the room temperature
and the atmospheric pressure.
4
Basic Laboratory Operations II
5.- Post-laboratory work
a) Results and calculations
Mass of the flask filled with air .......................................................................... g
Mass of the flask filled with CO2 ....................................................................... g
Volume of the flask ............................................................................................ mL
CO2 temperature ............................................................................................... ºC
Atmospheric pressure ....................................................................................... atm
Empty flask mass (without air) ........................................................................... g
Mass of collected CO2 ....................................................................................... g
Volume of CO2 collected in standard conditions (STP). ..................................... mL
Molecular mass of CO2 obtained in the course of the experiment ...................... g/mol
Molecular mass of CO2 deduced from the formula ............................................ g/mol
Absolute error.................................................................................................... g
Relative error..................................................................................................... %
(*) The density of air at 25ºC is 1.29 g/L
5
Basic Laboratory Operations II
b) Discussion and justification of results
1.
Write down the reaction between HCl and CaCO3, from which the stream of CO2 is
obtained. Indicate what type of reaction it is.
2.
Why is CO2 passed through CaCl2 before being collected in flask B?
3.
How does humidity affect the calculation of the molecular mass of CO2? Would it affect
the experiment in a significant way?
4.
Which other sources of experimental error can be reasonably addressed and avoided
in the context of this experiment?
5.
Given the conditions of the current experiment, would it be correct to write down the
temperature of CO2 as if it were the same as room temperature? Why / why not?
6
Basic Laboratory Operations II
6.
Describe and explain the apparatus employed in this experiment.
EXPERIMENT 2
Additional notes and comments
7
Basic Laboratory Operations II
EXPERIMENT 3
Establishing the formula of KClO3
Name:
Date:
1. Introduction
The term stoichiometry refers to the relations between mass and weight in chemical
formulae and reactions. In this experiment, students are asked to investigate the
stoichiometry of potassium chlorate and to use the results obtained in the analysis of a
sample of potassium chlorate and potassium chloride. The former compound is a mixture of
potassium, chlorine and oxygen. If heated intensely, it decomposes and loses all its oxygen,
leaving a residue of chlorine and potassium (KCl).
When potassium chloride and potassium chlorate are heated together, the mass lost
corresponds to that of the oxygen generated from the decomposition of potassium chlorate.
This allows us to calculate the quantity of chlorate contained in the initial mixture.
This experiment uses manganese dioxide, whose mass remains constant, as a
catalyst to speed up the decomposition process described above.
2.- Main aims of the experiment and learning outcomes
1. Finding out the molecular formula of an inorganic salt (potassium chlorate).
2. Determining the composition of a mixture of inorganic salts.
3.- Pre-laboratory work
1. Focus on the English terms used to refer to the labware tools and equipment
required for this experiment.
2. Enumerate the physical properties of MnO2 (dioxide of manganese), KClO3
(potassium chlorate), KCl (potassium chloride) and O2 (oxygen).
3. Be aware of the risks embedded in this experiment and adopte all the security
measures needed when deal with reagents.
4. References
1
Basic Laboratory Operations II
4.- Laboratory work
Material
Glass test tubes
Wooden clamps
Products
Manganese dioxide
Pure potassium chlorate
Mixture of potassium chloride and potassium chlorate
Procedure
1) Put a pinch of manganese dioxide into a clean, dry glass test tube, and use an analytical
balance to measure its total mass. The margin of error must be less than 0.01g. Add
approximately 1 g of dry potassium chlorate, then weigh again and shake softly to
homogenize the mixture. Clamp the test tube to a stand so as to keep it at a constant 45º
angle. Heat it lightly using a Bunsen heater, making sure you avoid a loss of solids or
any crackling issues. Once the solid melts, raise the heat (of the burner) as much as
possible for a few minutes. Allow some time for the test tube to cool down and weigh
again.
2) Put a pinch of manganese dioxide into a clean, dry glass test tube, and use an analytical
balance to measure its total mass. Again, the margin of error must be less than 0.01g.
The teacher will then provide a mixture of potassium chlorate and potassium chloride in
unknown proportions: put about 1 g of this mixture into the already weighed test tube that
contains the manganese dioxide. Once added, weigh again and shake the tube to mix its
contents. Follow the same process explained above to heat the test tube once more.
Finally, allow it to cool down and repeat the weighing step –this time with the final
product.
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Basic Laboratory Operations II
5.- Post-laboratory work
a) Results
1.Mass of the test tube containing the catalyst ........................................................... g
Mass of the test tube containing the catalyst and potassium chlorate ...................... g
Mass of the test tube containing the catalyst and the residue .................................. g
Mass of oxygen lost................................................................................................. g
Mass of potassium chloride ..................................................................................... g
Grams atoms of oxygen released ........................................................................ at-g
Number of moles of potassium chloride........................................................... moles
Gram atoms of potassium in the initial sample .................................................... at-g
Gram atoms of chloride in the initial sample ........................................................ at-g
Gram atoms of oxygen in the initial sample ......................................................... at-g
Empirical formula of potassium chlorate ....................................................................
2.-
Mass of the test tube containing the catalyst .......................................................... g
Mass of the test tube containing the catalyst plus the mixture of potassium chloride and
potassium chlorate ............................................................................................... g
Mass of the test tube containing the catalyst and the residue ................................. g
Mass of the test sample mixture ............................................................................. g
Mass of oxygen lost ............................................................................................... g
Gram atoms of oxygen lost................................................................................. at-g
Decomposed moles of potassium chlorate ..................................................... moles
Mass of potassium chlorate in the initial sample ..................................................... g
Mass of KCl ........................................................................................................... g
% in weight of potassium chloride in the test sample mixture ................................ %
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Basic Laboratory Operations II
b) Calculations
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Basic Laboratory Operations II
c) Discussion and justification of results
1.
What is a catalyst?
2.
Why are the products under study kept in a drying chamber?
3.
When heated in the correct conditions, barium oxide (BaO) absorbs more oxygen than
usual. If 1.15 grams of oxide transform into 1.27 grams of the new product, what would be
the empirical formula of the latter?
4.
If heated, sodium nitrate releases oxygen, and so decomposes into sodium nitrite. A
mixture of both –with a mass of 0.74 grams– loses 0.064 gram in the heating process. Use
these data to calculate the amount (%) of sodium nitrate in the original mixture.
7
Basic Laboratory Operations II
5.
A common source of error in this experiment stems from not waiting for the
decomposition of potassium chlorate to complete. Imagine this happened during the first
step in this experiment: how would it affect the molecular formula of potassium chlorate?
6.
How would the results obtained in the first stage be affected if the sample of potassium
chlorate were contaminated with moisture? Consider this on the assumption that the sample
should decompose completely.
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Basic Laboratory Operations II
EXPERIMENT 4
Obtention and acid-base properties of HCl and NH3
Name:
Date:
n
dula del KCIO3
1.- Introduction
Hydrides are binary compounds containing hydrogen plus another element. Water and
hydrogen peroxide are examples of this.
Whenever combined with hydrogen, a non-metallic element stands out as the
constituent with the highest level of electronegativity in the resulting compound. While
essentially ‘covalent’ (a term used to label this sort of hydrides), the bond will also bear a
certain polar character.
In a polar solvent (such as water), and providing that the A-H bond is highly polar, a
compound of this kind will dissociate into protons, therefore acting as a Brönsted acid (HCl,
for instance).
If the A-H bond is not highly polar, the hydride will not be acid. Being an element in the
p-block (with free pairs of electrons in its valence layer), A will nonetheless remain a
potential proton acceptor –that is, a potential Brönsted base (as in the case of NH3).
2.- Main aims of the experiment and learning outcomes
1. Obtaining HCl and NH3 (covalent hydrides) and describing them according to their
behaviour as acid bases.
2. Knowing how to use acid-base indicators.
3.- Pre-laboratory work
1. Focus on the English terms used to refer to the labware tools and equipment
required for this experiment.
2. Enumerate the physical properties of HCl, NaCl, CuO, NH3, AgNO3, NH4Cl, methyl
orange and phenolphthalein.
3. Be aware of the risks embedded in this experiment and adopting all the security
measures needed when dealing with reagents.
4. References
1
Basic Laboratory Operations II
A) Obtention and properties of HCl
Material
Wooden clamps
Pyrex test tube (with a stopper)
Four extra test tubes
Hollow glass rod, bent in U-shape
Solid glass rod
An acid base indicator strip
Hot plate
Products
Aqueous solution of methyl orange (0.01%)
Solid sodium chloride NaCl
Concentrated sulfuric acid H2SO4
Solid copper (II) oxide CuO
Concentrated solution of ammonia NH3
Aqueous solution of silver nitrate AgNO3
Procedure
Put a little solid sodium chloride into a test tube and soak it with a concentrated
solution of sulfuric acid. Heat the sample tube gently over a Bunsen burner. Then, moisten a
string of acid-base indicator paper and bring it to the mouth of the test tube (question 2).
Next, dip the end of a glass rod into an aqueous solution of ammonia and bring it to the
mouth of the test tube, as well (question 3).
After all this, use a stopper (with a delivery tube) to seal the test tube. Place the other
end of the delivery tube into another test tube filled with two thirds of water, as shown in the
image. Heat the generating tube gently for a few minutes and let it cool. Some of the HCl
generated will dissolve in the water.
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Basic Laboratory Operations II
Divide the solution obtained here into three different test tubes.
Add the following:
* Tube 1: some drops of methyl orange (question 4).
* Tube 2: some drops of aqueous AgNO3 (question 5).
* Tube 3: a pinch of solid CuO. Heat this tube gently (question 6).
5.- Post-laboratory work
Questions
1. Consider the reaction of obtention of HCl. Write it down and indicate what type it is.
2. How does the indicator paper change when brought to the mouth of the test tube?
What does that mean?
3. What do you notice after bringing the glass rod (previously dipped into an aqueous
solution of ammonia) to the mouth of the test tube? Explain what type of reaction it is
and write it down.
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Basic Laboratory Operations II
4. What happens after adding methyl orange to the HCl solution? Explain it.
5. What happens when AgNO3 is added? Write down the reaction, too.
6. What happens after adding CuO to the third portion? Write the reaction.
7. Additional notes and comments.
5
Basic Laboratory Operations II
B) Obtention and properties of NH3
Material
Wooden clamps
Pyrex test tube (with a stopper)
Four extra test tubes
Hollow glass rod, bent in U-shape
Solid glass rod
An acid base indicator strip
Products
Solid NH4Cl
Solid NaOH
Concentrated HCl
Hydroethanolic solution of phenolphthalein
CuSO4 solution
Procedure
The reaction of ammonium salt with a strong base produces ammonia gas (NH3),
which exhales a peculiar smell. When this gas dissolves in water, it gets partially
transformed, according to NH3 + H2O→NH4+ + OH-. Therefore, aqueous ammonia solutions
can be easily recognized thanks to the particular reactions underwent by NH3 or by
ammonium cation.
Take a test tube with a cork. In it, prepare a 3 mL concentrated solution of NH4Cl. Add
two or three pellets of NaOH. Heat the tube gently and then remove it from the flame.
Identify the liberated compound in that odor. Bring an acid/base indicator strip to the mouth
of the test tube (question 8); then bring a glass rod (previously dipped into a solution of
concentrated HCl) to the mouth of the test tube (question 9). Use a stopper with a delivery
tube to seal the test tube containing NH3. Heat it in the same way as with the one containing
HCl, so as to obtain an aqueous solution. The resulting product is divided into two test tubes.
Add a few drops of phenolphthalein to one; then, drop by drop, add a solution of CuSO4 to
the other one, until obtaining a light blue solid (Cu(OH)2), or an intense blue coloration
(question 12).
7
Laboratorio de aislamiento y caracterización de sustancias químicas
5.- Post-laboratory work
Questions
7. Focus on the reaction of obtention of NH3. Write it down.
8. What happens after bringing the acid/base indicator strip to the mouth of the test tube?
Explain it.
9. Write down the reaction that takes place when a glass rod dipped in a solution of
concentrated HCl is brought to the mouth of the test tube.
10. Observe and note down the reaction between NH3 and H2O that occurs when the
aqueous solution of NH3 is formed.
8
Laboratorio de aislamiento y caracterización de sustancias químicas
11.
12.
What happens when adding phenolphthalein to the NH3 solution? Why?
What happens when adding CuSO4 to the NH3 solution? Write the reaction and explain
the process.
EXPERIMENT 4
Additional comments and notes
9
Basic Laboratory Operations II
EXPERIMENT 5
Obtention and redox properties of H2O2
Name:
Date:
1.- Introduction
Hydrogen peroxide provides the basis for peroxides, peroxy acids and peroxy salts.
These are usually labeled as ‘substitution compounds’ on the basis that one or two hydrogen
atoms can be replaced with metals (peroxides) or more complex radicals (peroxy acids).
Therefore, the –O-O- group (peroxide) is common to them all.
Hence, hydrogen peroxide may be obtained using any peroxide, peroxy acid or peroxy
salt as raw material. The current experiment will use barium peroxide as a starting reagent
for obtaining hydrogen peroxide.
2.- Main aims of the experiment and learning outcomes
1. Highlighting the oxidizing and reducing properties of hydrogen peroxide.
2. Knowing the differences between hydrogen peroxide and “agua oxigenada”.
3. Using KMnO4 (in redox titration) as an indicator to measure the concentration of
hydrogen peroxide.
3.- Prelaboratory work
1. List the terms used in English to mention the labware tools and items required in this
experiment.
2. Enumerate the physical properties of barium peroxide BaO2, hydrogen peroxide
H2O2, phosphoric acid H3PO4, potassium permanganate KMnO4 and potassium
iodide KI.
3. Find out the standard reduction potentials for O2/H2O2, H2O2/H2O, MnO4-/Mn2+, I2/I4. Determine how to prepare 1 L of KMnO4 0.04 M solution.
5. Be aware of the risks embedded in the experiment and adopting all the security
measures needed when dealing with reagents such as the ones used in this
experiment.
6. References
1
Basic Laboratory Operations II
4.- Laboratory work
A) Obtaining hydrogen peroxide
Materials
Erlenmeyer flask
Test tube
Glass funnel
Support ring
Laboratory stand with bosses and clamps
Products
Barium peroxide, BaO2
Phosphoric acid, H3PO4
Procedure
Mix one gram of barium peroxide and 100 mL of water in an Erlenmeyer flask. Stir well.
While stirring, add 7 mL of phosphoric acid with a concentration of 85%. Then, measure the
total volume of the solution obtained. Save the solution for later. Focus on stages B and C.
5.- Post-laboratory work
- Discussion and justification of results
1. Write the reaction of obtaining hydrogen peroxide.
3
Basic Laboratory Operations II
2. What is the difference between "agua oxigenada" and "hydrogen peroxide"?
3. What is the difference between a peroxide and a dioxide?
4. What does ’10 volume hydrogen peroxide’ mean?
4
Basic Laboratory Operations II
B) Hydrogen peroxide titration
Introduction
Hydrogen peroxide may be used as an oxidizer in an acid solution or as a reducing
agent in the presence of another, more concentrated, oxidizer. Due to this, one may find out
the concentration of a solution of hydrogen peroxide by allowing it to react with a reducing
agent or an oxidizer. Potassium permanganate (KMnO4) will be used here to determine the
concentration of hydrogen peroxide (H2O2).
Material
Laboratory stand with bosses and clamps
Beaker
25 mL pipette
Burette
Erlenmeyer flask
Products
0.04M solution of KMnO4
Procedure
Use a pipette to transfer 25 mL of the solution obtained in stage A into an Erlenmeyer
flask. Add H2O2 until reaching a total volume of 100 mL. Then slowly titrate by adding 0,04 M
KMnO4 , drop by drop with a burette. Do not forget to shake well right after every drop is
added. Keep doing this until the solution produces a strong violet color (due to KMnO4). Note
down the volume of KMnO4 used in the titration.
5
Basic Laboratory Operations II
5.- Post-laboratory work
a) Discussion and justification of results
1. How does H2O2 act when mixed with KMnO4? Is it an oxidant or a reducing agent?
Express the reaction that takes place between them.
2. Write the reaction equation between KMnO4 and H2O2. Balance this by the ionelectron method.
3. What substance has been used as an indicator in the titration process?
6
Basic Laboratory Operations II
b) Calculations
Taking as a reference the volume of permanganate used in the titration process,
calculate:
1. The percentage by weight of the hydrogen peroxide solution prepared in this experiment.
2. Reaction yield of the hydrogen peroxide obtained.
7
Basic Laboratory Operations II
C) Assessing the oxidizing properties of hydrogen peroxide
Transfer the solution of hydrogen peroxide obtained in stage A into one 5 mL test tube.
Add a few drops of KI solution and comment what happens. Write the reaction equation
between KI and H2O2. Balance these by the ion-electron method.
EXPERIMENT 5
Additional comments and notes
9
Basic Laboratory Operations II
EXPERIMENT 6
Obtaining [Cu(NH3)4] SO4·H2O
and enumerating its physical properties
Name:
Date:
1.- Introduction
Coordination compounds (i.e. metal complexes) consist of a central metallic ion
(generally a transition metal) to which a set of ligands are attached via covalent bond. In
basic terms, the latter are neutral molecules or negative ions (simple or complex) with pairs
of free electrons in some of their atoms, which are attached to the aforementioned core ion
by means of a dative covalent bond. This process results in a compound which may either
be electrically neutral (left figure) or non-neutral (right figure). In the second case, a
counterion will be needed to neutralize the charge of the complex.
[Mn(SO4)(fen)(H2O)3]
[Mn(fen)(H2O)4]SO4·2H2O
Coordination compounds may have different geometrical structures: their shape
depends on the number and type of ligands. This applies to any metal ion. A two-ligand
complex (coordination number 2) will have a linear structure; if it had four, it would have a
tetrahedral (square planar) structure. A six-ligand complex would have an octahedral one.
Whenever a coordination compound is formed, the energy of the five degenerate d
orbitals in the external layer of the metal is split in a more or less complex manner, according
to the number of electrons they have and the position of ligands. This process is responsible
for the color of these compounds, since the electronic transitions between these split orbitals
correspond to the visible part of the electromagnetic spectrum.
1
Basic Laboratory Operations II
The splitting of the d orbitals in a Cu(II) ion coordinated to four ligands in a square
planar arrangement (as in the case of the [Cu(NH3)4]2+ ion) is relatively simple. The diagram
below displays the different types of splitting that d orbitals are likely to undergo, depending
on the position of ligands around the core Cu2+ ion. Tetraamminecopper(II) ions bear an
intense blue color due to the transition of one d electron from orbital dxy to orbital dx2-y2. The
remaining transitions belong to the infrared region of the electromagnetic spectrum and,
therefore, have no influence in the resulting color.
x2-y2
x2-y2, z2
xy, xz, yz
sp
∆sp
∆oo
∆t t
xy
x2-y2, z2
z2
xy, xz, yz
xz, yz
T
O
PC
Certain coordination compounds play an important role in our lives. Two examples of
this are found in hemoglobin and chlorophyll: the former (basically an iron complex with a
biomolecule) is essential to the transport of oxygen in vertebrates; the latter (a magnesium
complex) is utterly necessary for vegetable life.
2.- Main aims of the experiment and learning outcomes
1.
2.
3.
4.
Obtaining a coordination compound.
Determining the absorption spectrum of a compound (in its visible region).
Calculating the splitting energy of the obtained square planar complex.
Testing the solubility of the obtained compound in H2O and EtOH.
2
Basic Laboratory Operations II
3.- Pre-laboratory work
1. Focus on the English terms used to refer to the labware tools and equipment
required for this experiment.
2. Enumerate the physical properties of the CuSO4·5H2O, ethanol, ethyl eter and NH3.
3. Cite three examples of coordination compounds found in biologic processes.
4. Become aware of the risks embedded in the experiment. Adopting all the security
measures needed when dealing with reagents such as the ones used in this
experiment.
5. References
3
Basic Laboratory Operations II
4.- Laboratory work
Material
-
250 mL beaker
Cylinder
Solid glass rod
Kitasato flask
Büchner funnel
Vacuum pump
Cooling bath vessel
Products
-
Solid CuSO4·5H2O
Concentrated aqueous solution of ammonia
Ethyl alcohol
Diethyl ether
Instruments
- Ultraviolet-visible spectrophotometer
Procedure
A) Obtaining [Cu(NH3)4]SO4·H2O
In a beaker, dissolve one gram of [Cu(NH3)]SO4·H2O in about 7 mL of distilled water by
stirring with a glass rod. Observe the color. Once the solution is ready, slowly add 3 mL of
concentrated NH3 while stirring. At this precise point, you will notice the formation of a light
blue hued solid –i.e. copper hydroxide(II). However, as you keep adding NH3, Cu(OH)2 redissolves to turn into [Cu(NH3)4]2+. Pay attention to how the color has changed.
4
Basic Laboratory Operations II
Subsequently, without stopping stirring, add 10 mL of
ethyl alcohol to this transparent solution. You will then
see a dark blue precipitate –that is, solid
[Cu(NH3)]SO4·H2O.
Before filtering under vacuum, place the beaker in
a cooling bath for 15 minutes (see diagram).
After filtering, wash the resulting (filtered) solid with
two 5 mL portions of ethanol –and then with ethyl ether,
to improve the drying process. Once it has been
thoroughly air-dried, weigh the solid.
B) Solubility tests
Put about 0.1 grams of the dry product just obtained in a test tube. Do the same with
another test tube. Then:
· Fill the former with water to the half and then heat it gently.
· Add ethyl alcohol to the latter test tube.
C) Obtaining UV-VIS absorption spectrum
Using as a sample the aqueous solution of [Cu(NH3)]SO4·H2O from step B, obtain the
absorption spectrum of the compound in its visible region.
5
Basic Laboratory Operations II
5.- Post-laboratory work
a) Calculations
Initial moles of CuSO4 .......................................................................................
Mass of [Cu(NH3)4]SO4·H2O obtained ................................................................
Moles of [Cu(NH3)4]SO4·H2O obtained ...............................................................
Reaction yield (%): ............................................................................................
6
Basic Laboratory Operations II
b) Results of the experiment
Taking as a reference the aforementioned absorption spectrum, calculate:
· The wavelength corresponding to the maximum in the absorption spectrum (nm).
· The frequency of transition between levels dxy and dx2-y2 (s-1).
· Splitting Energy (∆sp) in joules and at cm-1
c) Discussion and justification of results
1.
Formulate the reactions taking place since the dissolution of CuSO4·5H2O (after adding
concentrated ammonia) until the step in which tetraamminecopper(II) sulfate is
obtained. Explain and justify the color changes that you perceive.
7
Basic Laboratory Operations II
2.
What would you add regarding the solubility tests of [Cu(NH3)4]SO4·H2O in water and
ethanol? Justify your answer(s).
3.
Why is ethanol necessary to precipitate the solid complex?
4.
Why is the complex washed with ethanol and ether instead of water?
5.
What is the blue color of the complex due to?
EXPERIMENT 6
Additional comments and notes
8
Basic Laboratory Operations II
EXPERIMENT 7
Separation and purification of the components of a mixture
through distillation
Name:
Date:
1.- Introduction
Distillation is the most important and frequent method of separation of liquid substances
due to their different boiling points.
There are several types of distillation. In all them, we can distinguish three fundamental
steps
1.- Heating and evaporation of substances
2.- Cooling and condensation of the vapor produced.
3.- Separation and collection of substances in a separate container.
We must know that when a liquid substance is put inside a container and this is closed, a
number of molecules in the surface of the liquid pass to the vapor state. At the same time, a
number of molecules on the surface pass from vapor state to the liquid state. When the
condensation rate and the evaporation rate are the same, the equilibrium is achieved.]
To understand the basis of a distillation, we should know that, when at a certain
temperature a liquid is introduced into a vacuum container -and this is closed-, some of the liquid
evaporates exerting molecules -in vapor state- a pressure on the liquid surface. In turn, some
molecules -in a vapor state- condense until balanced. That means that the evaporation rate equals
the rate of condensation.
The pressure that the molecules exert on the surface of the liquid, in the equilibrium state, is
called vapor pressure. This magnitude is constant and depends on the composition of each
compound and temperature such that when the temperature increases, the vapor pressure also
increases regularly. If warmed in an open container at the time when the vapor pressure increases
and to equalize the atmospheric or external pressure, the liquid begins to boil. The temperature at
which this occurs is called the temperature or the boiling point, and depends, apart from the
external pressure, on the molecular mass of the molecules and the intensity of the attractive forces
between them.
1
Basic Laboratory Operations II
Thus, in a series of organic compounds, which share the same functional group and which
differ only in the nature of the hydrocarbon chain (that is, a homologous series of compounds), the
boiling points of each compound increase regularly with the molecular weight. When the number
of atoms in the molecules increases, the van der Waals forces increase between them, too. Polar
liquids, on the other hand, tend to boil at higher temperatures than non polar ones –with the same
molecular mass- , and polar compounds, which are associated with each other via hydrogen
bonding, boil at higher temperatures than those that cannot be associated.
When, instead of a pure compound, we have a mixture, the interactions established
between its molecules determine that either are thoroughly mixed resulting in a homogeneous
solution (eg water-ethanol) or are mixed partly or not mixed at all (eg. water-oil) separating into
two layers.
When a homogenous mixture of liquids is heated (see Figure 1) it happens that:
1. The mixture boiling point depends on the boiling points of its components and their
relative proportions.
2. Its boiling point will be between the boiling points of the pure compounds.
3. When the mixture starts to boil, the vapor –B- will be richer in the volatile components of
the mixture than the liquid in equilibrium –A-
Figure 1. Liquid-vapor diagram for a two component mixture.
2
Basic Laboratory Operations II
According to the above we obtain a pure compound by distillation if:
•
The difference in boiling points of the components of a mixture is very large, greater
than 80 ° C, (eg, water and salt).
•
The amount of impurities contaminating a liquid substance is below 10%
•
Vapors are condensed and redistilled a number of times.
The simplest apparatus that is used to perform a distillation is depicted in the following figure
Figure 2. Simple distillation apparatus
As you can see, the apparatus comprises a spherical flask or distillation flask, a distillation
head equipped with a thermometer, a straight condenser with water circulating through an outer
jacket, a bent adapter and a collecting flask. To heat the flask homogenously, an oil bath or an
electric heating mantle, as that displayed in the figure, is usually employed. In addition, a steam
water bath can be also used when heating over 100 ºC is not necessary.
The distillation mixture is put in a flask and it is heated. When the boiling point is reached, a
great amount of vapor is produced. Firstly the vapor condenses on the wall of the flask, then on
the thermometer and finally is collected on a beaker due to the flow of cool water which circulate
through the outer jacket of the refrigerant
3
Basic Laboratory Operations II
Fractional Distillation
The distillation apparatus displayed in Figure 2 can be adapted to achieve the separation of
mixtures of substances whose boiling points differ by 30-80 ºC.
When we have a mixture of this type, a simple distillation offers a distillate enriched in the
more volatile component.
If this distillate is reloaded in the distillation flask and heated again, we will get a new distillate.
We should repeat this operation a number of times to get the most volatile component in pure
form. To avoid this, between the distillation flask and the distillation head, a fractional distillation
column is placed. This one, through the multiple surfaces that fill inside, enables, in the same
distillation equipment, a continuous series of numerous partial evaporations and condensations,
providing a vapor becoming richer in the most volatile component.
Vigreux column are the type of fractionating columns most frequently used in the laboratory.
The separation power of a column of this type is greatest when this is adiabatic, that is, when
no heat is exchanged with the outside; and this only takes place between the ascending vapor -the
vapor goes up through the column-, and the descending liquid -the liquid goes down.
Fractional distillation plays a fundamental role in petrochemical industry to be an early stage to
which the petrol is subjected to perform the separation of its main components.
Figure 3
Fractional distillation apparatus
Figure 4
Different fractions obtained
petroleum distillation
4
from
the
process
of
Basic Laboratory Operations II
Reduced-pressure distillation
Many substances cannot be purified by means of distillation at normal pressure either
because they get decomposed below their respective boiling points or because they have such
high boiling points that the energy expenditure required does not compensate for its purification by
means of distillation. However, these liquids can be distilled by means of reduced-pressure
distillation, i.e., by means of a pressure lower than the atmospheric.
As it has already been mentioned, a liquid starts to boil at the temperature at which its
vapor pressure becomes equal to the external pressure.
If, someway, we manage to reduce the external pressure we will also be able to reduce the
boiling point of the liquid, since the value of its vapor pressure will be closer to the new external
pressure.
In order to achieve this reduction of pressure, the simple or fractional distillation equipment
must be connected to a special device, a vacuum pump capable of reducing atmospheric pressure
up to pressures of approximately 10 mm of mercury.
In subsequent experiences, we will carry out distillation under reduced pressure to
concentrate solutions or remove large amounts of volatile solvents from solutions composed of
that solvent and any other little volatile compound that we might want to isolate.
To this end, instead of using the above mentioned simple or fractional distillation
equipments, we will use the rotary evaporator, which is a device which incorporates one engine
that allows rotation of the distillation flask and, therefore, favours the continuous distillation of its
contents.
Figure 5. Rotary evaporator used to concentrate solutions from volatile solvents under reduced pressure.
5
Basic Laboratory Operations II
2.- Main aims of the experiment and learning outcomes
1. Knowing the main characteristics of simple, fractional and vacuum distillation and the
factors influencing them.
2. Knowing how to choose the most suitable distillation, depending on the nature of the liquids
to be separated.
3. Obtaining acetone from a mixture of solvents by means of fractional distillation.
4. Representing simple organic compounds and identifying organic functional groups.
5. Knowing the name, both in Spanish and English, of the material needed to carry out every
type of distillation.
3.- Pre-Laboratory work
Analyze the following issues, answer the questions and comment them with your teacher –in
tutorials- before the next laboratory session.
1.- Draw the following compounds and justify the increase of the boiling point observed in each
series:
a) Methanol (65ºC); Ethanol (78ºC); Propyl alcohol (97ºC); Butyl alcohol (118ºC)
b) Butane (-0,5ºC); Ethyl methyl ether (7,6ºC); Acetone (56ºC); Propyl alcohol (97ºC)
c) Pentane (36ºC); 2,2- Dimethyl-propane(9,5ºC); 2-Methylbutane (27,5ºC); 2,3-Dimetyl-butane (58ºC)
2.- Search for the boiling points of the compounds below and indicate what type of distillation will
be the most suitable to separate them.
a)
b)
c)
d)
e)
f)
Water and Ethanol
Water and Acetone
Water and Sodium chloride
Acetonitrile and Methanol
Toluene and Dichloromethane
Diethyl ether and benzaldehyde
3.- What an azeotrope is? Find out whether any of the pairs of compounds of the previous
exercise could form an azeotrope and indicate its boiling point and composition.
4.- Why is it advisable to add a piece of boiling or anti-bumping stone into the distillation flask?
7
Basic Laboratory Operations II
5.- What is the main function of the Liebig’s condenser? Explain what the direction of flow of
cooling water in the Liebig’s condenser should be. Justify your answer.
6.- In the experiment, a steam bath is used to heat the distillation flask and distillate acetone.
Could we have used a steam bath as a heating source to distillate toluene? Justify the answer.
7.- Identify the risks and the security measures (R/S sentences) to be taken with acetone obtained
after distillation.
8.- What DNFH or Brady´s reagent is?. Find out what reaction takes place between Brady’s
reagent and acetone.
9.- Will acetaldehyde react with Brady’s reagent? And ethanol?
5.- Write in English the name of all the material you will need in order to carry out the experiment.
6.- References
8
Basic Laboratory Operations II
4.- Laboratory work
a) Experimental Procedure
With the help of a graduated cylinder, measure 100 mL of the water-acetone mixture to be
distilled; and, by using a conical funnel, transfer it to a 250 mL round bottom flask resting on a cork
ring. Then add a boiling stone and hold the flask to a metallic support with a clamp. Place the flask
on a steam bath and, greasing the standard-taper joints with silicone, attach it to a fractionating
column and to a distillation head with a thermometer. Now, connect to the condenser a water input
hose at the furthest end from the heated flask and a water outflow hose near the heated flask.
Check both that the condenser is not broken and the refrigeration is efficient. After that, hold
the condenser with a clamp and joint it to the distillation head. Finally, after having greased the
standard-taper joints with silicone, attach to the condenser a bend adapter and, at the end of it,
place a 100 ml beaker or Erlenmeyer flask.
When the distillation equipment is ready, put on the steam bath and wait to collect the first drop
of distillate. Then, once the distillation temperature becomes regular, record its value and replace
the collecting beaker by a graduated cylinder. When the temperature starts to drop, put the
heating source off and again replace the graduated cylinder by a beaker. Annotate the volume of
the distillate obtained.
Once the heating source has cooled down, disassemble the equipment piece by piece in
reverse. Finally, wash all parts with water and acetone and let them be dried in a hot air oven.
Acetone, a solvent widely used as nail polish remover for example, can be distinguished from
water by its boiling point, its smell and, furthermore, by the formation of an orange solid when it
reacts with Brady´s reagent. To check this, transfer a few drops of acetone to a test tube and add
two drops of Brady´s reagent. What happens? To contrast the results, repeat the same test with a
few drops of water instead of acetone.
9
Basic Laboratory Operations II
b) Results
•
Initial volume of mixture:
•
Laboratory pressure:
•
Temperature at which distillate is collected:
•
Temperature at which distillate is expected to be collected:
•
Volume of distillate collected:
•
Concentration of the acetone solution in the mixture expressed through a percentage
volume/volume:
C) Discussion
1. Was coincident the theoretical boiling point of acetone with the distillation temperature? If
no, explain the reason.
2. Comment the result of the Brady´s test
10
Basic Operations Laboratory II
EXPERIMENT 8
Isolation of essential oils from aromatic plants through steam
distillation
Name:
Date:
1.- Introduction
Steam distillation is a valuable technique for the separation of thermally labile, high-boiling and
water immiscible (water) substances from miscible and relatively nonvolatile materials.
Steam distillation is preferable to ordinary distillation because the volatile components distill at
temperatures below their normal boiling points, reducing or preventing decomposition due to overheating.
To understand how steam distillation works we have to take into account that, in a mixture with two
immiscible liquids, A (water) and B (oil), every liquid has a characteristic vapour pressure, independently
of the other. That means that the vapour pressure of the mixture is the addition of the vapour pressures of
every individual liquid
PT = PA + PB (PA and PB are the individual vapour pressures of A and B)
The melting point of a mixture with compounds A and B is the temperature achieved when the total
pressure PT and the external or atmospheric pressure are the same. So, if PA or PB are not zero, the
temperarure of the mixture will be lower than A or B boiling points separately.
Taking this into account and the fact that the temperature during a steam distillation is never above
100 ºC, this kind of distillation is especially useful to separate thermo labile substances with high boiling
points. These substances are co-distilled with water, and then isolated from the mixture collected. Some
examples of these substances are a lot organic compounds of high boiling points which are part of the
essential oils in aromatic plants.
In this experiment steam distillation will be used to extract the essential oils e.g. the volatile
components that exhibit the odor and other characteristics of plants such as cinnamon, glove, spearmint,
peppermint, etc…
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Basic Operations Laboratory II
2.- Main aims of the experiment and learning outcomes
1. Applying the steam distillation technique to the isolation of thermally labile and immiscible
water compounds obtained from a natural source.
2. Applying the liquid-liquid extraction technique to the isolation of an organic compound
knowing its solubility properties.
3. Learning to handle a rotary evaporator to remove, at low pressure, volatile solvents
4. Identifying organic functional groups through colorimetric tests.
5. Analyzing and justifying the experimental results obtained.
3.- Pre-laboratory work:
Analyze the following issues, answer the questions and comment them with your teacher –in
tutorials- before the next laboratory session.
1. What is a functional group?
2. Investigate the substances found in the essential oil of the plant under study and
complete the following table
Compound
Molecular
(name)
Formula
Structural Formula
A
Name of the
Plant:
B
C
2
Boiling/Melting
Functional
Point ºC
groups
Basic Operations Laboratory II
3. Indicate which functional groups can be identified by the following colorimetric tests.
In which tests would the three main components, of the essential oil extracted, give
positive?
Results (+)
Test
Functional groups
A
B
C
Lucas test
Brady test
Tollens test
Iodoform test
Hidroxamic acid test
Nitroso acid test
Iron III test
Baeyer test
Friedel-Crafts test
4. Mark with a circle and name the functional groups that you can find in the followings
molecules a, b and c. Then, indicate what colorimetric tests can be carried out to
distinguish them. Include, in the table, the result of the test: positive or negative.
O
CH3
O
H
O
OH
OH
a
b
Test
+ or - test
3
OH
c
Basic Operations Laboratory II
5. Look at the apparatus in Figure 1 and explain what is the role of the straight glass rod
introduced into the Erlenmeyer flask.
6. After distillation, essential oils are separated from water through liquid-liquid extraction.
Look for information about this separation technique and answer the following questions:
a. How do you know what the organic phase and the aqueous phase are? List four
methods to distinguish them
b. The aqueous solution is treated three times with 15 mL of solvent extractor. Do you
think you would you have obtained the same result by treating the solution once with
45 mL? Why?
c.
After shaking the separatory funnel, it is always advisable to open the key? why?
d. After the extraction, why anhydrous sodium sulfate is added to the organic extract?
e. List the risks and safety measures (R / S sentences) you must observe, when you
work with dichloromethane.
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Basic Operations Laboratory II
7. Complete the gaps indicating the action students are doing
She is ____________ a __________ from a
He´s ______________ a separatory funnel
Erlenmeyer flask to a ________________
She is ________ the ___________________
She is ________ a ___________________
She´s _____________________ a solid
He´s ______________ a reaction mixture
and _________ temperature
8. References
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Basic Operations Laboratory II
4.- Laboratory work
a) Experimental procedure
Add a piece of boiling stone, together with 500mL of water, to a 1000mL Erlenmeyer flask with a
29/32 ground-glass joint. Hold the flask to a supporting stand with a metallic clamp and place it on a
hotplate, avoiding direct contact with it. Now, attach to it a side-arm adapter and a leaky cork. Introduce
through it a straight hollow glass rod, which will act as a safety valve.
On the other hand, weigh 25 g of plant in a 250mL beaker and transfer it through a powder funnel to a
1000mL round-bottom flask with a 29/32 ground-glass joint resting on a cork ring. Then, add a piece of
boiling stone and 250 mL of water. Next, hold the flask to a supporting stand with the help of a metallic
clamp and attach it to the Erlenmeyer flask through a bent hollow glass rod. Finally, attach a condenser to
the round-bottom flask through a leaky cork with a bent hollow glass rod and a collecting flask.
Figure 1
Once the equipment has been assembled (see Figure 1), turn on the heat and refrigeration source
and wait to collect approximately 200 mL of the oil-water immiscible mixture in a 250 mL beaker by paying
attention to the possible overpressures that might take place. Once collected the aforementioned 200mL of
distillate, turn the hot plate off, replace the collecting beaker by an empty one and transfer the distillate to a
graduated cylinder to measure the volume. Next, pour the mixture into a separatory funnel and add 15 ml of
dichloromethane. Shake it smoothly to prevent the stopper from popping out due to pressure and to avoid
forming emulsions. Collect the organic phase into an Erlenmeyer flask and work on the aqueous phase
twice by using 20 ml of dichloromethane. Then, put both phases together and treat them with anhydrous
sodium sulfate. Filter the dry organic extract in a previously weighed spherical flask and then, remove the
solvent with the help of a rotary evaporator.
After a few minutes, an odorous, oily residue should appear on the wall of the flask. Weigh the flask
again and calculate the yield of the oil extracted. Finally, carry out a test with the oil extracted to identify
functional groups.
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Basic Operations Laboratory II
b) Results
•
Plant analyzed:
•
Weight of plant analyzed:
•
Volume of distillate collected: (b):
•
Weight of round-bottom flask (empty) (c):
•
Weight of round-bottom flask (with oil) (d):
•
Amount of essential oil extracted (e):
•
Extraction efficiency (e)/(a) x 100:
•
Result of colorimetric test: (+/-):
c) Discussion
•
How did the distillate obtained look like? And the resulting oil?
•
What is your opinion about the amount of oil extracted?
•
Indicate same way to increase the amount of oil extractedAccording with the colorimetric test carried
out, what functional groups are present in the final extract? Is the result consistent with what
expected?
•
During steam distillation, take two test tubes labeled as 1, 2 and 3 containing a sample of unknown
compounds a, b or c. Perform two colorimetric tests, write the results herein and discover in which
test tube is every compound.
Test
Tube 1
Tube 2
Tube 3
Result
+ or -
Molecule (a, b, c)
7
Basic Operations Laboratory II
EXPERIMENT 9
Isolation of caffeine from commercial sources
NAME:
DATE:
1.- Introduction
A) Isolation of caffeine from tea bags
Tea and coffee drinks have been popular drinks for centuries, mainly because they contain caffeine, a
chemical stimulant which active the central nervous system and speeds up breathing and heartbeat.
Caffeine is also diuretic, causes nervousness and insomnia and, as many drugs may cause addiction. This
compound is also found in cocoa and added to cola beverages.
A cup of coffee contains 60 to 100 mg of caffeine, a cup of tea contains 30 to 50 mg, a chocolate
bar contains 10 mg, and a can of cola 43 mg.
Caffeine belongs to a kind of compounds called alkaloids. These are compounds present regularly
in plants. They are composed by atoms of carbon and nitrogen and therefore, infusions have a bitter taste
and basic and physiological properties.
O
H3C
OR
CH3
O
N
N
RO
RO
O
OR
O
N
OR
N
CH3
O
O
R=
HO
Caffeine
OH
O
OH
OH
O
Flavone
OH
Tannins
Figure 1. Main components of tea leaves
The main component of tea leaves is cellulose, which is the principal structural material of all plant
cells. Cellulose is a polymer of glucose. Because cellulose is virtually insoluble in water, it presents no
problems in the isolation procedure. Caffeine is mixed with other compounds in tea leaves. Some of these
compounds are called tannins and have acid properties (see figure). In addition there are also pigments as
chlorophylls or flavones. Typical brown color of infusions (tea solutions) is due to (flavonoid pigments)
flavones and their respective oxidation products.
Different solubility of caffeine in water and organic solvents is key to get an efficient separation from
the other compounds.
Chlorophylls are insoluble in water; however, caffeine, tannins and flavone derivatives are soluble
enough in hot water. So, a first separation can be achieved heating tea leaves in hot water and filtering.
Next, the aqueous solution is done alkaline. In this way, solubility in water of tannins and flavones is
increased due to its acid properties, and caffeine can be easily extracted with an organic solvent,
methylene chloride, for example.
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Basic Operations Laboratory II
B) Isolation of caffeine from cola drinks
Caffeine can be easily isolated from a cola drink through a liquid-liquid extraction since all the
ingredients are more soluble in water than in organic solvents.
Concentration of caffeine in cola drink is 0.1 mg/mL, e.g. six times lower than coffee.
Cola is a drink composed by an aqueous extract of cola nuts. This extract can be got as a syrup. If
this syrup is combined with phosphoric acid, caramel, water, carbon dioxide and some unknown ingredient,
the very famous coca-cola drink is obtained
Caffeine limit in cola drinks, established by the Food and Drugs Administration in U.S., is 17 mg per
100 mL. To regulate its level, firstly caffeine is completely extracted from syrup by producers and then the
legally allowed amount is added.
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Basic Operations Laboratory II
2.- Main aims of the experiment and learning outcomes
1. Applying the liquid-liquid extraction technique to the isolation of an organic compound from a natural
or commercial source, given its acid-base and solubility properties.
2. Learning how to handle a rotary evaporator to remove volatile solvents at low pressure.
3. Checking the identity of a compound through tlc.
4. Analyzing and justifying the experimental results obtained.
3.- Pre-laboratory work
Before starting the next laboratory practice, read the introduction to this experience and answer the
following questions.
1.
What substances do you ingest when you drink tea? Draw the structural formula of caffeine and
indicate: its molecular formula, molecular weight, melting point and toxicity characteristics
2.
What substances do we take when we drink a cola drink? Read the label and write their names.
3.
During the extraction of caffeine, emulsions can be formed. Answer: a) What an emulsion is?; How
can emulsions be avoided?, c) If any emulsion is formed, what can we do to break it?
4.
Make a complete list, both in English and Spanish, of the glassware and appliances needed in this
experience.
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Basic Operations Laboratory II
5. Read the experimental procedure and fill the gaps in the following schematic overview:
6. References
4
Basic Operations Laboratory II
4.- Laboratory work
a) Isolation of caffeine from tea bags. Experimental procedure
Weigh 1 g of potassium carbonate, transfer it to a beaker and dissolve it in 100 mL of water. Add a
boiling stone, heat the solution on a hotplate and when it is about to boil turn the hotplate off and place five
tea bags into the hot solution so that they lie flat on the bottom of the beaker and are fully covered by water.
After 10 minutes, remove the tea bags by gently pushing them against the walls of the flask with the
help of a glass rod or a test tube, avoiding breaking it. Clean the bags with water and finally dispose of
them in a solid waste container.
Cool the brown solution at room temperature and transfer it to a separatory funnel through a bed of
cotton. Add 15 ml of dichloromethane and shake the funnel smoothly to prevent the stopper from popping
out due to pressure and to avoid forming emulsions. Separate the organic phase and collect it into an
Erlenmeyer flask. Work on the aqueous phase twice by using 20 ml of dichloromethane. Then, put the
organic phases together and treat them with anhydrous sodium sulfate. Filter the dry organic extract in a
previously weighed spherical flask and then, remove the solvent with the help of a rotary evaporator. Once
the solvent is removed; caffeine will appear as a white solid on the walls of the flask. Finally, weigh the flask
and calculate the yield of the caffeine extracted. The purity of the caffeine obtained can be known by its
color, its melting point and through thin layer chromatography –tlc-, comparing it with commercial caffeine.
To learn how perform a TLC see part c).
b) Isolation of caffeine from cola drinks. Experimental procedure
Weigh 2 g of potassium carbonate and transfer them into a beaker. Now, pour slowly about 200 mL of
cola drink into the beaker and shake them with a glass rod to eliminate the maximum amount of carbon
dioxide possible. Next, pour the mixture into a separatory funnel and add 15 ml of dichloromethane. Shake
it smoothly to prevent the stopper from popping out due to pressure and to avoid forming emulsions. Collect
the organic phase into an Erlenmeyer flask and work on the aqueous phase twice by using 20 ml of
dichloromethane. Then, put the organic phases together and treat them with anhydrous sodium sulfate.
Filter the dry organic extract in a previously weighed spherical flask and then, remove the solvent with the
help of a rotary evaporator. If the cola drink contains caffeine it will appear as a white solid on the walls of
the flask. Finally, weigh the flask again and calculate the yield of the caffeine extracted.
The purity of the caffeine obtained can be known by its color, its melting point or through thin layer
chromatography –tlc-, comparing it with commercial caffeine. To learn how perform a TLC see part c).
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Basic Operations Laboratory II
c) Identification of compounds by thin layer chromatography TLC
1. Add 5 mL of eluent in an elution tank or development chamber. Close it well and wait for the
saturation of the vapor inside before the introduction of the chromatographic plate. In order to
know when saturation is achieved, insert a rectangular piece of filter paper and wait until it
soaks.
2. Now, cut or ask the teacher for a 2.5 x 6 cm chromatographic plate and draw with a blunt pencil
a horizontal line at 1 cm from the short side of the plate.
3. On the horizontal line, draw crosses with the pencil, according to the number of samples to
analyze and identify the crosses. For example, the test sample can be identified with a letter M,
and the reference we use to compare with a letter R.
4. Dissolve a small amount of the reference sample into a volatile solvent (acetone or
dichromethane) and, using a thin glass capillary tube, deposit a small amount repeatedly tapping
on the corresponding signals carried on the plate. Repeat the same operation with a small
amount of the test sample.
5. Place the plate inside the elution tank, close it and wait until the eluent rise by capillarity. When
the elution front is about 0.5 cm from the end of the plate, take it out and mark the front with a
horizontal line.
6. Reveal the plate to know where the products are. Draw a circle on the signals that appear.
7. Calculate the Rf of each displayed signal, i.e the ratio of the distance covered by the signal and
the distance covered by the eluent.
6
Basic Operations Laboratory II
a) Results
• Caffeine source:
( ) Tea, Brand:______
( ) Cola drink, Brand:________
• Amount of tea or cola drink studied:
• Weight of the round-bottom flask (empty):
• Weight of the round-bottom flask with extract:
• Amount of extract obtained:
b) Comments to results
• What does the final residue obtained look like, after distillation in the rotary evaporator?
• According to the thin layer chromatography –tlc- performed to the final extract, was there
caffeine in it?, was the extract pure? Draw here the result and calculate the Rf of the
products visualized.
• What system has been used to visualize the signals?
• If a tea bag contains about 30-50 mg of caffeine, what can you say about the efficiency of
the extraction?
• If a can of coke of 330 ml contains about 43 mg of caffeine, what can you say about the
efficiency of the extraction?
7
Basic Operations Laboratory II
EXPERIMENT 10
Isolation and identification of the Components of an Analgesic
Tablet
Name:
Date:
1.- Introduction
Aspirin or acetylsalicylic acid is a derivative of salicylic acid that is used as a mild and non-narcotic
analgesic useful in the relief of headache and muscle and joint aches. Nowadays, aspirin is the most
popular and sold painkiller in the world. The history of aspirin starts when Hippocrates, the father of modern
medicine, who lived between 460 B.C and 377 B.C., describes the use of a powder made from the bark
and leaves of the willow tree to help heal headaches, pains and fevers. Several centuries later, in 1828,
Johann Buchner, professor of pharmacy at the University of Munich, isolated the active ingredient in willow
bark; a tiny amount of bitter tasting yellow, needle-like crystals, which he called salicin. Ten years later, an
Italian chemist named Raffaele Piria split salicin into a sugar and salicylaldehyde and then converted the
latter, by hydrolysis and oxidation, to an acid of crystallised colourless needles, which he named salicylic
acid. The use of salicylic acid as a painkiller was soon limited by its acidic properties, as it produced
irritation of the mucous membranes of the mouth, esophagus and stomach. The problem was solved when
a French chemist named Charles Frederic Gerhardt, in 1853, neutralized salicylic acid by buffering it with
sodium (sodium salicylate) and acetyl chloride, creating acetylsalicylic acid. Gerhardt's product worked very
well but he had no desire to market it and abandoned his discovery. In 1899, a German chemist named
Felix Hoffmann, who worked for a German company called Bayer rediscovered Gerhardt's formula and
convinced Bayer to market the new wonder drug. Aspirin was patented on February 27, 1900. The
commercial name of aspirin comes from: the 'A" in acetyl, the "spir" in spiraea ulmaria (the plant the
salicylic acid comes from) and the 'in' was then a familiar name ending for medicines.
In this experiment, you will carry out the isolation and identification of the components of an
Analgesic Tablet. Analgesic tablets may contain a mixture of aspirin, acetominophen and caffeine along
with a binder. The binder, a neutral substance usually made of silica gel, starch or microcrystalline cellulose
is used to hold the tablet together after packaging, shipping and while it is being swallowed. The binder is
not soluble in water or common organic solvents so it can be easily separated by suspension and filtration.
On the other hand, the solubilities of the three components are different in different solvents. For
example, aspirin and caffeine are soluble in dichloromethane while acetaminophen is not. Hence we can
separate acetaminophen (and the binder) from aspirin and caffeine by dissolving the tablet in
dichloromethane followed by filtration. Acetominophen is found to be soluble in ethanol. Therefore,
acetominophen can be separated from the binder with the same technique. Inspection of the structures of
aspirin and caffeine reveals that they are an organic acid and an organic base, respectively. The
1
Basic Operations Laboratory II
corresponding conjugated base and conjugated acid are soluble in water but not in dichloromethane.
Furthermore, water and dichloromethane are immiscible. Therefore, the aspirin and caffeine in the filtrate
can be separated by extraction either with acid, which remove the caffeine as a water-soluble salt, or by
extraction with base, which will remove the aspirin as a water-soluble salt. The latter procedure will be used
in this experiment. The products obtained are then identified by melting-point determination and thin-layer
chromatography tlc.
2.- Main aims of the experiment and learning outcomes
1. Applying the technique of liquid-liquid extraction to the isolation and separation of several organic
compounds contained in a commercial tablet in accordance with their physical and chemical
properties
2. Analyzing and justifying the experimental results obtained.
2
Basic Operations Laboratory II
3.- Pre-laboratory work
Read the introduction to this experience and answer the following questions before the next laboratory
practice.
1. Analgesic tablets may contain a mixture of aspirin, acetominophen and caffeine along with a binder.
Read the experimental procedure and, with the following solubility data, complete the gaps in the
flowchart.
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Basic Operations Laboratory II
2.- Taking into account that both acetylsalicylic acid and caffeine are better soluble in dichloromethane than
in water, how can you manage to separate them?
3.- If instead of dichloromethane in the initial extraction stage, diethyl ether has been used, how could the
compounds have been separated? Draw a flowchart similar to this one on page three.
4.- In general, analgesic tablets contain only one active component along with a binder. According with the
solubility data displayed on page 3, how could we separate them?
5.- Draw the structural formula of acetaminophen, acetyl salicylic acid and caffeine. Furthermore, write out
the molecular formula, the molecular weight, melting point and toxicological properties of everyone.
6.- Write in Spanish and English the words that represent the following pictograms that you can find on the
labels of the reagents used, as well as their corresponding meaning,
4
Basic Operations Laboratory II
4.- Laboratory work
a)
Experimental procedure
Select an analgesic to analyze A, B or C and, in a mortar, grind four pills/tablets to very fine powder.
Place this powder in a conical flask previously weighed, and take note of the amount of powder transferred.
Next, add about 50 mL of dichloromethane and stir the mixture with a magnetic stirrer for about ten
minutes. The solid in suspension in the dichloromethane mixture is filtered by gravity into a separatory
funnel. Then, the solid and the filter paper are put into a beaker labelled ‘S1’. All this is stored, for later use,
inside a hot air oven.
Now, check by tlc (adsorbent: Silica gel; eluent: Ethyl acetate) the filtrate L1 and, if the tlc plate reveals
that caffeine or acetylsalicylic acid are not present, collect the filtrate in a pre weighed round bottom flask
and remove the solvent on vacuum to obtain one of the components. On the other hand, if both caffeine
and acetylsalicylic acid are present, add 50 mL of 1 M sodium bicarbonate solution and shake the mixture
thoroughly. Collect the aqueous layer into a 250 mL beaker and extract the organic solution again with 50
mL of 1 M sodium bicarbonate solution. Collect the aqueous layer and combine it with the previously
collected aqueous extract. Store this solution in the fridge. Finally, wash the organic phase with 50 mL of
water and collect it in a 100 mL conical flask labelled “L2”.
Add anhydrous Na2SO4 powder into the dichloromethane extract until the drying agent no longer
clumps together. Swirl the mixture for about 30 minutes to complete the drying process and filter the
mixture by gravity into a pre weighed round bottom flask labelled “S2”. Remove the solvent from the
solution completely by rotary vacuum distillation and finally, weigh the solid obtained. Compare the result
with the expected amount and confirm the identity and purity of the solid determining the melting point.
Take the aqueous alkaline extract from the fridge and add 10 mL of 1 M hydrochloric acid drop by drop
and test the acidity of the extract with pH paper from time to time until the pH of the extract is ca 3. If
necessary, add more acid solution. When a suspension is formed, cool the mixture with an ice-bath, filter it
and wash the solid with iced water. Then dry the solid completely to the air. Weigh the solid obtained,
compare the result with the expected amount and confirm its identity and purity determining the melting
point.
Finally, transfer the solid (S1) previously kept in a hot air oven into a conical flask, add 15 mL of ethanol
and heat the mixture until boiling. Filter the solid particles in suspension and collect the filtrate into a
previously weighed spherical flask labelled ‘S3’. Remove completely the solvent from the solution by rotary
vacuum distillation and finally, weigh the solid obtained. Compare the result with the expected amount and
confirm the identity and purity of the solid determining the melting point.
5
Basic Operations Laboratory II
b) Experimental results
•
Analgesic tablet analyzed (A, B or C):
•
Amount of analgesic tablet analyzed:
•
According to the tlc performed to the filtrated –L1-, what compounds were present?
•
Draw herein the chromatography plates made to L1 and calculate the Rf of the products that you
Weight of one pill:
get to visualize.
•
Amount of caffeine extracted (a1)
•
Experimental melting point:___________ Theoretical melting poin
•
Amount of acetylsalicylic isolated (b1)
•
Experimental melting point: ________________ Theoretical melting point: __________
•
According to the tlc performed to the filtrated –L3-, what compounds were expected to be
isolated?
•
Draw herein the chromatography plates made to L3 and calculate the Rf of the products that you
get to visualize.
•
Amount of acetaminophen isolated (c1)
•
Experimental melting point: ________________ Theoretical melting point: __________
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Basic Operations Laboratory II
Once the experiment has concluded, ask the teacher for the labels of the tablets analyzed and indicate
which of them they belong to. Read on the label the amount of active ingredients contained in every tablet
and calculate the yield required to extract each of them. Comment the result.
Caffeine
According to the label, how much caffeine should contain the sample? (a2) _______ g
Extraction Yield/efficiency (a1/a2 x100): _________ %
Acetylsalicilic acid / aspirin
According to the label, how much of acetylsalicylic should contain the sample? (b2): ________ g
Extraction Yield/Efficiency (b1/b2 x100): _________ %
Acetaminophen
According to the label, what amount of acetaminophen should contain the sample? (c2): _______g
Extraction yield(c1/c2 x100): _________ %
c) Discussion of results
Considering the tests performed (melting point and thin layer chromatography), what can you say about
the identity and purity of the products obtained
What is your opinion about the extraction efficiency?
7
Basic Laboratory Operations II
EXPERIMENT 11
Synthesis and Purification Through Recrystallization of
Acetylsalicylic Acid (Aspirin)
Date: _________
Name:
1.- Introduction
In this experiment you will carry out the synthesis of one of the most famous medicaments
synthesized by human beings: the aspirin. Acetylsalicylic Acid (Aspirin) can be easily prepared by means of
the reaction between salicylic acid and acetic anhydride through a reaction catalyzed by an acid called
esterification.
2.- Main aims of the experiment and learning outcomes
1. Reading and understanding an experimental procedure written in the English language.
2. Learning vocabulary related to a chemistry laboratory in English.
3. Learning how to separate a solid from a reaction mixture using the technique known as vacuum
filtration
4. Knowing the usefulness of crystallization techniques to purify solid compounds and the glassware
and appliances necessary to make it.
5. Analyzing and justifying the experimental results.
3.- Pre-laboratory work
Answer the following questions and comment them with your teacher before the next laboratory practice
1.- Translate the experimental procedure into Spanish.
1
Basic Laboratory Operations II
2.- Have a look at the following images of labware used in this experience: write their name, and
explain for what purpose they are used:
It is a/an ________________________________________ and
it is used for ______________________ a reaction mixture
It is a/an _________________________ and
it is used for ______________ the solid in a suction filtration
It is a/an _________________________ and
it is used for __________ the liquid in a suction filtration
It is a/an _________________________ and
It is used to _________ liquids from one container into another
It is a/an _________________________ and
it is used for ______________ a conical or separatoy funnel
It is a/an _________________________ and
it is used to _______________ a melting point
2
Basic Laboratory Operations II
3.- Draw the reaction scheme including the structural formula of reagents and products.
4.- Why is concentrated sulfuric acid used in the synthesis of aspirin?
5.- Complete the following data table in English.
Compound
Risk and Security
Molecular
Molecular
Boiling/Melting
Formula
Weight
Point ºC
6.- Why are 50 mL of water added into the flask containing the first mass of aspirin crystals?
7.- Why is it advisable to wash crystals several times, instead of just once, with small portions of
water but with so much solvent?
3
Basic Laboratory Operations II
8.- What test can you apply to determine whether there is any salicylic acid remaining in the
aspirin? Explain it
9.- Read about recrystallization as a purification technique for solid compounds and answer the
following questions in Spanish:
a) Why must active carbon be added in the recrystallization process?
b) What physical and chemical properties must a liquid have so as to be used as a solvent in the
recrystallization process?
c) Why are not ethyl acetate or ethanol suitable solvents for the crystallization of aspirin?
10.- References
4
Basic Laboratory Operations II
4.- Laboratory work
a) Experimental procedure
Weigh 2.0 g of salicylic acid and transfer them to a 100 mL Erlenmeyer flask. Add 4.0 mL of acetic
anhydride and then add 5 drops of concentrated sulfuric acid. Shake the flask gently until the salicycilic acid
dissolves. Let the flask cool down to room temperature till the acetylsalicylic acid begins to crystallize. If it
does not, scratch the walls of the flask with a glass rod and let the mixture cool down in an ice bath until
crystallization takes place. Once crystal formation is completed, add 50 mL of water and shake the flask
gently in order to liberate the crystals. By means of vacuum filtration, collect the product on a Büchner
funnel. Add a small amount of cold water to assist the transfer of crystals to the funnel. Rinse the crystals
several times with small portions of cold water. Keep on with the suction on the Büchner funnel for some
minutes, drawing air through the crystals till they are free of solvent.
Sometimes the crude product may contain some unreacted salicyclic acid residues, so purification by
recrystallization may be necessary. In order to select the most adequate solvent, transfer a bit of solid to
three test tubes and add to each of them 1 ml of cool water, ethanol and ethyl acetate respectively. Pay
attention to that solvent in which the solid is not dissolved at room temperature and then, heat the tubes in
a steam bath. Select the solvent that dissolves the solid in the hot and not on the cold solvent.
Weigh and transfer the wet solid to a 100 mL Erlenmeyer flask. Then, add a few grains of activated
carbon. Besides, in another flask boil a small amount of the chosen solvent and pour it in small fractions
into the flask until the solid dissolves. Then, filter the hot solution by gravity into an Erlenmeyer flask
through a folded filter paper. Let the filtered solution cool down at room temperature until crystals appear. If
crystallization does not take place, scratch the walls of the flask with a glass rod and slightly cool down the
mixture in an ice bath until crystallization takes place. Collect the product through vacuum filtration using a
Büchner funnel and remove the crystals for air drying. Check contamination with salicyclic acid by means of
the ferric chloride test. Finally, weigh the crude product, calculate the percentage yield and measure its
melting point.
5
Basic Laboratory Operations II
b) Stoichiometric calculations and yield
Limitant reagent (mol)
Expected weight of Aspirin –aExperimental weight of Aspirin –c- (wet)
Experimental weight of Aspirin –d- (dry)
Yield %
d/a x 100
Recrystallization efficiency
d/c x 100
Experimental melting point (ºC)
c) Results: Discussion and Justification
What can you say about the purity of the product obtained according to the tests performed? And about the
yield?
6
Basic Operations Laboratory II
EXPERIMENT 12
Monitoring the progress of a reaction by means of thin layer
chromatography
NAME:
DATE:
1.- Introduction
Chromatography is a technique which can separate the components of a mixture due to their
different interactions with a stationary phase (solid or liquid) when they are pulled along by a mobile phase
(gaseous or liquid).
Chromatography can be either plane or in column according to the layout of the stationary phase.
Thin layer chromatography, usually called TLC, is the most used type of plane chromatography.
Here, a solid stationary phase is attached to a flat plate and a liquid, which is called eluant, and which rises
up by capillarity sweeping and separating the components of the mixture. This type of chromatography is
useful for:
1. Testing the purity of a compound.
2. Identifying the components of quite complex mixtures.
3. Separating and purifying the components of a mixture.
4. Monitoring the progress of a reaction.
In this experiment we are going to control the progress of an oxidation reaction through tlc.
2.- Main aims of the experiment and learning outcomes
1. Learning the equipment you need to heat refluxing a mixture.
2. Monitoring the progress of a reaction through tlc.
3. Applying the liquid-liquid extraction technique to the isolation of an organic compound from a
reaction mixture knowing its solubility properties.
4. Analyzing and justifying the experimental results obtained.
1
Basic Operations Laboratory II
3.- Pre-laboratory work
Answer the following questions and comment them with your teacher before the next laboratory practice.
1. Complete the following data table in English.
Compound
Risk and Security
(name)
Molecular
Molecular
Boiling/Melting
Formula
Weight
Point ºC
2. Why are sodium hypochlorite, acetic acid and acetone used in this reaction?
3. Draw the reaction scheme that takes place between 9-fluorenol and sodium hypochlorite,
including the structural formula of reagents and products.
4. The Rf of a compound is 0.6 when a mixture hexane:acetone 7:3 v/v is used as eluent. if a
mixture hexane:acetone 5:5 v/v is used as eluent, how will the new value of Rf be, greater or
lower?
5. Sort by order of increasing polarity the following mixtures of eluents. Justify your answer
a) n-Butanol, Acetic acid 4:1 v/v.
b) n-Butanol, Acetic acid, Ethanol 3:1:1 v/v/v.
c) n-Butanol, Acetic acid, Water 3:1:1 v/v/v.
d) n-Butanol, Ethanol, Water 3:1:1 v/v/v.
6. When a mixture is refluxed, a tube filled with calcium chloride (drying tube) is placed on the
condenser. However, in the experiment to be carried out this tube won’t be necessary. Why?
7. Why were 5 mL of NaHCO3 (1 M) added to the reaction mixture once the reaction had
finished?.
2
Basic Operations Laboratory II
4.- Laboratory work
a) Experimental procedure
Weigh 50 mg of 9-hidroxifluorene and transfer them to a dry 50 mL round bottom flask holding to a
supporting stand with the help of a metallic clamp and place it on a stirrer plate. Then, add 3.0 mL of
acetone, 1.0 mL of sodium hypochlorite, 0.2 mL of acetic acid and finally a magnetic stirrer. Now, attach a
condenser to the round-bottom flask and start stirring at room temperature.
After ten minutes, check the reaction media through tlc (Adsorbent: Silica gel; Eluent A: hexane:acetone
7:3 v/v; Eluent B: hexane:acetone 5:5, v/v). The reaction is concluded if starting material is not visualized.
Besides, if starting material is even present in the reaction media we can:
a) Way for ten minute more and check again by tlc.
b) Add 1.0 mL of sodium hypochlorite and after 15 minutes, check again by tlc.
c) Reflux the mixture and after 15 minutes, check again by tlc.
Follow stirring and slowly, add 20 mL of NaHCO3 (1M) on the mixture. Next, pour the mixture into a
separatory funnel and add 20 ml of diethyl ether. Shake it smoothly to prevent the stopper from popping out
due to pressure. Remove the aqueous phase and wash the organic phase twice by using 10 ml of water.
Then, treat organic extract with anhydrous sodium sulfate. Filter the dry organic extract in a previously
weighed petri dish and then, remove the solvent with the help of a vent.
After a few minutes, a yellow residue should appear. Weigh the petri dish again and calculate the yield
of the compound obtained, 9-fluorenone. Finally, carry out Brady´s test to verify that carbonyl group is
present in the residue.
3
Basic Operations Laboratory II
b) Results: Discussion and Justification
1. When an extra amount of sodium hypochlorite was added on the reaction medium, what
happened? And what happened when the reaction was refluxed?.
2.
When do you think that addition of an extra amount of sodium hypochlorite or an increase in
temperature can have a negative effect on reaction?
3. Draw the results of all the thin layer chromatography performed using as eluents both 5.5 v/v as
7.3 v/v hexane:acetone mixtures and calculate the Rf of the products visualized with Ultraviolet
lamp.
4. After evaporation, what does the final residue obtained look like?
5. What test can you make to know the purity of the final product?
6. What information have you obtained by applying Brady´s test?
4
Basic Operations Laboratory II
c) Stoichiometric calculations and yield
Limitant reagent (mol)
Expected weight of product
Experimental weight of product
Yield %
EXPERIMENT 12
Additional notes and comments
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UNIVERSIDAD DE JAÉN
UNIVERSITY OF JAEN
Guía Audiovisual de Operaciones Básicas de Laboratorio II
Audiovisual Guide of Basic Laboratory Operations II
ELIJA IDIOMA
CHOOSE LANGUAGE
Yolanda Caballero Aceituno
Jose Maria Mesa Villar
Concepción Soto Palomo
Departamento de Filología Inglesa-UJA
Nuria Illán Cabeza
Antonio Marchal Ingrain (coord.)
Departamento de Química Inorgánica y Orgánica-UJA
Guía Audiovisual de Operaciones Básicas de
Laboratorio II
1.
2.
3.
4.
5.
6.
7.
Presentación
Introducción a la Asignatura Operaciones Básicas de Laboratorio II OBL-II
Competencias y Resultados de Aprendizaje
Recursos Bibliográficos y on-line
Evaluación
Bloques temáticos
– Normas de Seguridad en el Laboratorio
– Experiencias con Operaciones Básicas aplicadas al estudio de las
propiedades físico-química de compuestos inorgánicos
– Experiencias con Operaciones Básicas aplicadas a la separación y
purificación de los componentes de una mezcla de naturaleza orgánica
Ejercicios
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1. Presentación
La presente Guía Bilingüe de la asignatura “Operaciones Básicas de Laboratorio II
<OBL-II>”, del Grado en Química surge en primer lugar con el ánimo de facilitar al alumnado
no hispano-hablante matriculado en la asignatura, el acceso a los contenidos de la misma
en inglés y en segundo lugar para que todo el alumnado se familiarice con la terminología
científico-técnica propia de un laboratorio de química en castellano y en inglés. Para
conseguirlo, los diferentes contenidos se presentan mediante documentos descargables,
audios activos y videos de las experiencias que se realizan durante el desarrollo de la
asignatura.
Agradecimientos:
Este material se ha elaborado gracias a la concesión del proyecto PID17-201113 por
parte del Vicerrectorado de Profesorado e Innovación Docente de la Universidad de
Jaén en la Convocatoria 2011-2013 y a la participación de los estudiantes del Grado en
Química matriculados en la asignatura en los cursos 2011-2012 y 2012-2013.
2. Introducción a la Asignatura
Operaciones Básicas de Laboratorio II
La asignatura “Operaciones Básicas de Laboratorio II OBL-II”, se imparte en el
segundo cuatrimestre del primer curso del Grado en Química y completa la formación
en operaciones básicas de laboratorio adquirida por el alumnado con la asignatura de
primer cuatrimestre “Operaciones Básicas de Laboratorio I (OBL-I)”.
En la asignatura OBL-I el alumnado aprende las normas de seguridad en un
laboratorio de química y operaciones básicas de trabajo como pesar, preparar y
valorar disoluciones o separar los componentes de una mezcla mediante extracción
simple o múltiple.
En la asignatura OBL-II por otro lado, el alumnado aplica las habilidades
experimentales básicas adquiridas en la Asignatura OBL-I al estudio de casos más
complejos como por ejemplo, el estudio de las propiedades físico-químicas de
compuestos inorgánicos o la purificación y caracterización de productos orgánicos
obtenidos mediante procedimientos sintéticos.
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3. Competencias y Recursos de
Aprendizaje
Al finalizar el estudio de la asignatura, el alumnado…:
•Conoce vocabulario básico en inglés relacionado con la seguridad, reactivos y operaciones básicas de
laboratorio.
•Conoce la necesidad de minimizar la generación de residuos y su gestión.
•Dispone de conocimientos y habilidades suficientes para utilizar correctamente y con seguridad los
productos y el material más habitual en un laboratorio químico siendo consciente de sus características
más importantes incluyendo peligrosidad y posibles riesgos.
•Aplica las habilidades experimentales básicas adquiridas en la Asignatura OBL-I al estudio de casos más
complejos.
•Conoce las técnicas más sencillas para la purificación de un compuesto químico.
•Conoce procedimientos sencillos para caracterizar un producto químico.
•Interpreta y comunica adecuadamente los resultados de un experimento utilizando la terminología
científico-técnica propia de la química de forma correcta.
4. Recursos Bibliográficos y on line
•
•
•
•
•
•
•
•
CONTRERAS, A., CASELLES, M. J., MOLERO, M ; “Introducción a la Química Experimental. (I)El laboratorio
de Química. Instalaciones y Material. (II) Productos o Sustancias Químicas. (III) Técnicas Básicas de
Laboratorio”.3 vídeos y 2 guías didácticas. UNED 1992.
GARCÉS, A. “Experimentación en Química Inorgánica”, Ed. Dykinson 2009.
HORTA A., ESTEBAN S., NAVARRO R., CORNAGO P., BARTHELEMY C; “Técnicas experimentales de Química”,
UNED, 2001.
MARCHAL, A et col. “Introducción a un Laboratorio de Química. Guía Audivisual Multilíngüe” CD.
Universidad de Jaén, 2009
MARTINEZ M.A., CSÁKY A.G.“Técnicas Experimentales en Síntesis Orgánica” Ed. Síntesis S.A; 1998.
PAVÍA D.L., LAMPMAN G.M., KRIZ-Jr G.S, Engel, R.D. "Introduction to Organic Laboratory Techniques", 2nd
ed., Thomson Brooks/cole, 2005
RAMOS, M. M. y VARGAS, C. “LABORATORIO DE QUIMICA ORGANICA”, EDITORIAL UNIVERSITARIA RAMON
ARECES, MADRID: 2006.
WOOLLINS J.D. (ed.); "Inorganic Experiments", VCH; 2003.
– www.panreac.es
– www.pobel.es
– www.sigmaaldrich.com/labware.html
– www.ub.edu/oblq/
– www.ugr.es/~quiored/
– www.chemspider.com
– www.liceoagb.es/quimiorg/indice.html
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5. Evaluación
Al tratarse de una asignatura experimental, se ha establecido un sistema de evaluación
que valora en gran medida la asistencia y participación del alumnado en las actividades
propuestas tanto en el laboratorio como en tutorías. Así la calificación final vendrá dada por:
EXAMEN TEÓRICO-PRÁCTICO (60% NOTA FINAL) en el que el alumnado deberá demostrar su
dominio de los conocimientos teóricos y operativos desarrollados en la asignatura y de la
terminología básica de laboratorio, en castellano e inglés.
REVISIÓN SEMANAL DEL CUADERNO DE LABORATORIO (15 % NOTA FINAL) en el que se
valorará:
- Ortografía y presentación.
- Calidad de las fuentes de consulta utilizadas.
- Calidad de la traducción de textos en inglés.
- Capacidad de observación y extracción de conclusiones.
- Resolución de cuestiones.
TRABAJO DE LABORATORIO (25 % NOTA FINAL) en el que se valorará:
-Orden, limpieza y aplicación adecuada de las normas de seguridad y manejo de sustancias
químicas.
-Finalización de cada experiencia en el tiempo adecuado.
-Destreza en la realización de las operaciones propias de cada experiencia .
-Capacidad de resolución de imprevistos.
6. Bloques Temáticos
A. Normas de Seguridad en el Laboratorio.
B. Experiencias con Operaciones Básicas aplicadas al
estudio de las propiedades físico-química de
compuestos inorgánicos. 1-6
C. Experiencias con Operaciones Básicas aplicadas a la
separación y purificación de los componentes de
una mezcla de naturaleza orgánica. 7-12
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A. Normas de seguridad
1.- Trabaje seguro en el laboratorio
2.- Normas de seguridad en los laboratorios de la UJA
3.- Frases de riesgo y seguridad
4.- Material de laboratorio
5.- Instrucciones de uso del Medidor Punto de Fusión
Trabaje seguro en el laboratorio
P
I
C
T
O
G
R
A
M
A
S
Tóxico
Corrosivo
Peligroso para el
medio ambiente
Inflamable
Peligroso para
las personas
Antes de iniciar una
experiencia lea la
etiqueta de los reactivos
Explosivo
Oxidante
Nocivo e
Irritante
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Trabaje seguro en el laboratorio
Lleve bata de mangas largas
No use sandalias. Los zapatos
deben cubrir el pie entero
No use lentes de contacto. Use gafas de
seguridad cerradas
El pelo debe recogerse o cubrirse
Elija los guantes adecuados pare el manejo
seguro de sustancias peligrosas
Trabaje seguro en el laboratorio
Use la DUCHA DE SEGURIDAD
en caso de incendio
Compruebe el BOTIQUÍN
regularmente
El trabajo con reactivos tóxicos debe
realizarse en la CAMPANA
EXTRACTORA
Use el LAVAOJOS con abundante agua
cuando algún reactivo le salpique a la cara
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Trabaje seguro en el laboratorio
Manta ignífuga
Salida de
Emergencia
Manguera
Extintor
Alarma
B. Experiencias 1-3
1.- Determinación de la masa atómica del magnesio
Procedimiento experimental
2.- Determinación de la masa molecular del CO2
Procedimiento experimental
3.- Determinación de la fórmula del KClO3
Procedimiento experimental
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B. Experiencias 4-6
4.- Obtención y propiedades ácido-base del HCl y del NH3
Procedimiento experimental
5.- Obtención y estudio de las propiedades rédox del H2O2
Procedimiento experimental
6.- Obtención y propiedades físicas del [Cu(NH3)4]SO4·H2O
Procedimiento experimental
B. Experiencias 7-9
7.- Separación de los componentes de una mezcla mediante
destilación. Procedimiento experimental.
8.- Aislamiento de aceites esenciales de plantas aromáticas
mediante Arrastre de vapor. Procedimiento experimental.
9.- Aislamiento de cafeína de hojas te y refresco de cola.
Procedimiento experimental.
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B. Experiencias 10-12
10.- Aislamiento e identificación de los componentes de un
Analgésico. Procedimiento experimental.
11.- Síntesis y purificación mediante recristalización de
ácido acetilsalicílico. Procedimiento experimental.
12.- Seguimiento del progreso de una reacción mediante
cromatografía en capa fina ccf.
Procedimiento experimental
Ejercicios de inglés
Escuche los siguientes audios en inglés relacionados con los procedimientos
experimentales e intente contestar a las cuestiones incluidas en los
documentos pdf rellenables.
Audio # 1.
Ejercicio 1
Audio # 5.
Ejercicio 5
Audio # 2.
Ejercicio 2
Audio # 6.
Ejercicio 6
Audio # 3.
Ejercicio 3
Audio # 7.
Ejercicio 7
Audio # 4.
Ejercicio 4
Audio # 8.
Ejercicio 8
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15/07/2013
UNIVERSITY OF JAEN
UNIVERSIDAD DE JAÉN
Audiovisual Guide of Basic Laboratory Operations II
Guía Audiovisual de Operaciones Básicas de Laboratorio II
ELIJA IDIOMA
CHOOSE LANGUAGE
Yolanda Caballero Aceituno
Jose Maria Mesa Villar
Concepción Soto Palomo
Departamento de Filología Inglesa-UJA
Nuria Illán Cabeza
Antonio Marchal Ingrain (coord.)
Departamento de Química Inorgánica y Orgánica-UJA
Audiovisual Guide of Basic Laboratory
Operations II
1.
2.
3.
4.
5.
6.
7.
Presentation of this Guide
Introduction to the subject “Basic Laboratory Operations II BLO-II”
Competences and Learning Outcomes
Literature and internet sources
Assessment methods
Contents
– Lab Safety rules
– Basic Laboratory Operations applied to the study of physical and
chemical properties of inorganic compounds
– Basic Laboratory Operations applied to the isolation of compounds from
reaction media, natural or commercial sources
Listening exercises
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1. Presentation
This Bilingual Guide of the subject “Basic Laboratory Operations II” has been
designed by a group of professors at the University of Jaén (Spain) aiming to firstly,
facilitate to foreign students the contents of the subject in English and then, to get
Spanish students are familiar with the typical scientific-technical vocabulary used in a
laboratory of chemistry both in English as in Spanish language. Contents are presented
as downloadable documents, audios and video about all the experiments performed
during the course.
Acknowledgements
Authors are grateful to students enrolled in the subject “Basic Laboratory Operations II” (Bachelor in
Chemistry) in the 2011-2012 and 2012-2013 courses for your participation and to the Vicerrectorado de
Profesorado e Innovación Docente of the University of Jaén for supporting this initiative through the
project PID17-201113
2. Introduction to the subject
Basic Laboratory Operations II
The subject “Basic Laboratory Operations II” is taught in the second semester of the
first year of Bachelor in Chemistry and complete the learning acquired by the students in the
subject “Basic Laboratory Operations I” coursed in the first semester.
In the subject “Basic Laboratory Operations I BLO-I”, security rules in a laboratory and
basic operations such as weighing, preparing a solution or separating the components of a
mixture through simple or multiple extraction are learned.
On the other hand, in the subject “Basic Laboratory Operations II BLO-II”, the
experimental skills acquired in BLO-I by students are applied to more complex situations, e.g.
studying the physical and chemical properties of inorganic compounds or the purification and
characterization of organic compounds isolated both from natural as artificial sources.
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3. Competences and Learning
outcomes
Upon completetion of the study of this subject, students acquire ... :
•
Knowledge of the main aspects of chemical terminology, nomenclature, conventions and units.
•
Knowledge of a foreign language (preferably English).
•
Sensibility towards environmental topics.
•
Skills in the evaluation, interpretation and synthesis of chemical information and data.
•
Skills in the safe handling of chemical materials, taking into account their physical and chemical
properties, including any specific hazards associated with their use.
•
Skills required for the conduct of standard laboratory procedures involved and use of
instrumentation in synthetic and analytical work, in relation to both organic and inorganic systems.
•
Skills in the monitoring, by observation and measurement, of chemical properties, events or
changes, and the systematic and reliable recording and documentation thereof.
4. Literature and internet sources
•
•
•
•
•
•
•
•
CONTRERAS, A., CASELLES, M. J., MOLERO, M ; “Introducción a la Química Experimental. (I)El laboratorio
de Química. Instalaciones y Material. (II) Productos o Sustancias Químicas. (III) Técnicas Básicas de
Laboratorio”.3 vídeos y 2 guías didácticas. UNED 1992.
GARCÉS, A. “Experimentación en Química Inorgánica”, Ed. Dykinson 2009.
HORTA A., ESTEBAN S., NAVARRO R., CORNAGO P., BARTHELEMY C; “Técnicas experimentales de Química”,
UNED, 2001.
MARCHAL, A et col. “Introduction to a Laboratory of Chemistry. Multilingual audiovisual guide” CD.
Universidad de Jaén, 2009
MARTINEZ M.A., CSÁKY A.G.“Técnicas Experimentales en Síntesis Orgánica” Ed. Síntesis S.A; 1998.
PAVÍA D.L., LAMPMAN G.M., KRIZ-Jr G.S, Engel, R.D. "Introduction to Organic Laboratory Techniques", 2nd
ed., Thomson Brooks/cole, 2005
RAMOS, M. M. y VARGAS, C. “LABORATORIO DE QUIMICA ORGANICA”, EDITORIAL UNIVERSITARIA RAMON
ARECES, MADRID: 2006.
WOOLLINS J.D. (ed.); "Inorganic Experiments", VCH; 2003.
– www.panreac.es
– www.pobel.es
– www.sigmaaldrich.com/labware.html
– www.ub.edu/oblq/
– www.ugr.es/~quiored/
– www.chemspider.com
– www.liceoagb.es/quimiorg/indice.html
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5. Assessment methods
Basic Laboratory Operations II BLO-II, is an experimental subject therefore,
to evaluate the learning outcomes, a special attention will be payed in the
attendance and the active participation in seminars and tutorials. So, the final
qualification will be given by:
Theorical-practical examination (60% FINAL QUALIFICATION). Students have to demonstrate …
Theorical- Knowledge and mastery of the theoretical and practical issues of the subject.
- Mastery of the basic English terminology needed to work in a laboratory.
Weekly revision of Laboratory reports (15 % FINAL QUALIFICATION). Special attention will be
payed in… :
- Well-written reports.
- Grammar and neat presentation.
- Quality in the use of references.
- Quality of the texts translated into English.
- Originality.
Attendance and active participation in seminars and tutorials (25 % FINAL QUALIFICATION).
Special attention will be payed in.. . :
- Tidy work, cleaning and proper application of the safety rules and handling of chemicals.
- Completion of each experience at the right time.
- Skill in the implementation of operations of each experience .
- Ability to solve unforeseen.
6. Contents
A. Lab Safety Rules.
B. Laboratory Operations applied to the study of
physical and chemical properties of inorganic
compounds.
C. Basic Laboratory Operations applied to the isolation
of compounds from reaction media, natural or
commercial sources.
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A. Lab Safety Rules
1.- Work safety in the lab!!
2.- Precautionary and Hazards statements
3.- Glassware
4.- Digital Melting Point Apparatus. Operating and Safety
Instructions
Work safety in the lab!!
P
I
C
T
O
G
R
A
M
S
Toxic
Corrosive
Dangerous for the
environment
Explosive
Flammable
Dangerous for
people
Oxidising
Before starting an
experiment read the
reagents label
Harmful
or Irritant
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Work safety in the lab!!
No sandals
sandals.. Shoes should
cover entire foot
Wear fullfull-length lab coat
No contact lenses.
lenses.
Use safety close
close--fitting googles
Loose hair should be
covered or tied
Choose adequate gloves for the safe
handling of hazardous substances
Work safety in the lab!!
Use SAFETY SHOWER in
case of fire
Check FIRST
FIRST--AID
AID-- KIT
regularly
Work with toxic chemicals should be
carried out in a FUME HOOD
Use EYEWASH with water enough
when a reagent splash on you face
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Work safety in the lab!!
Fire blanket
Emergency exit
Hosepipe
Fire extinguisher
Fire alarm
B. Experiments 1-3
1.- Determining the atomic mass of magnesium.
Experimental Procedure.
2.- Determining the molecular mass of carbon dioxide.
Experimental Procedure.
3.- Establishing the formula of KClO3
Experimental Procedure.
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B. Experiments 4-6
4.- Obtention and acid-base properties of HCl and NH3
Experimental Procedure.
5.- Obtention and study of redox properties of H2O2
Experimental Procedure.
6.- Isolation and and study of physical properties of
[Cu(NH3)4]SO4·H2O
Experimental Procedure.
B. Experiments 7-9
7.- Separation and purification of the components
of a mixture through distillation. Experimental Procedure.
8.- Isolation of essential oils from aromatic plants through
steam distillation. Experimental Procedure.
9.- Isolation of caffeine from a cola drink and tea bags.
Experimental Procedures.
Part A (tea bags)
Part B (cola drink)
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B. Experiments 10-12
10.- Isolation and identification of the components
of an Analgesic Tablet. Experimental Procedure.
11.- Synthesis and purification through recrystallization of
acetylsalicylic acid (Aspirin). Experimental Procedure.
12.- Monitoring the progress of a reaction by means of
thin layer chromatography and isolation of products.
Experimental Procedure.
Listening Exercises
Listen the followings records related to the experimental procedures and try
to answer the guestions included in the pdf documents.
Record # 1.
Exercise 1
Record # 5.
Exercise 5
Record # 2.
Exercise 2
Record # 6.
Exercise 6
Record # 3.
Exercise 3
Record # 7.
Exercise 7
Record # 4.
Exercise 4
Record # 8.
Exercise 8
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