Manual de Laboratorio RQII O23

Laboratorio de Reactores Químicos II
Manual de Prácticas de Laboratorio

Licenciatura en Ingeniería Química Industrial
Otoño 2023
Ingeniería
Química Industrial
Chemical Reactors Lab II
Contenido
Normas de seguridad..........................................................................................................................5
Ubicación de dispositivos de seguridad...........................................................................................5
Uso y manipulación de sustancias químicas....................................................................................5
Calentamiento de sustancias químicas.............................................................................................5
Derrame de sustancias químicas.......................................................................................................6
Llaves de paso..................................................................................................................................6
Actuación en caso de accidente o siniestro......................................................................................6
Identificación de riesgos químicos...................................................................................................6
Medidas específicas de seguridad....................................................................................................7
En caso de duda, consulta al profesor..............................................................................................7
Equipo de protección personal y vestimenta....................................................................................8
Reglamento del Laboratorio..............................................................................................................9
Responsabilidad................................................................................................................................9
Experiment 01. Effect of temperature on the reaction rate.........................................................11
Objectives.......................................................................................................................................11
Introduction....................................................................................................................................11
Reagents.........................................................................................................................................13
Lab materials & equipment............................................................................................................13
| Ingeniería Química Industrial

Procedure........................................................................................................................................14
Results analysis and report.............................................................................................................14
Waste disposal................................................................................................................................16
References......................................................................................................................................16
Experiment 02. Saponification of Ethyl Acetate with NaOH in CSTR a under Pseudo-Steady
State Sonditions................................................................................................................................17
Objectives.......................................................................................................................................17
Introduction....................................................................................................................................17
Reagents.........................................................................................................................................19
Procedure........................................................................................................................................19
Waste disposal................................................................................................................................21
References......................................................................................................................................21
Experiment 03. Reaction of crystal violet with NaOH in an isothermal semi-continuous

reactor................................................................................................................................................22
Objectives.......................................................................................................................................22
Introduction....................................................................................................................................22
Reagents.........................................................................................................................................23

Procedure........................................................................................................................................23
Waste disposal................................................................................................................................25
References......................................................................................................................................25

Normas de seguridad.
Ubicación de dispositivos de seguridad.
 Estos dispositivos son elementos tales como extintores, lavaojos, ducha de seguridad,
salidas de emergencia.
Uso y manipulación de sustancias químicas.
 Revisa los pictogramas de seguridad presentes en la etiqueta de los envases de las

sustancias químicas que manipules en la práctica para determinar el equipo de seguridad
necesario para su manipulación.
 Por tu seguridad evita oler directamente cualquier sustancia química que utilices en el
laboratorio, ya que la sustancia podría llegar a ser tóxica. Si la sustancia es volátil y el
envase tiene pictogramas de riesgo por inhalación debes utilizar mascarilla apropiada.
 La manipulación de las sustancias químicas debes hacerla utilizando guantes apropiados.
 Utilizar perillas o propipetas para el pipeteo de cualquier líquido.
 Proceder siempre con precaución en el trasvase de las sustancias.
 No cambiar las pipetas colocadas en los frascos de reactivos de uno a otro, pues puede
ocurrir contaminación de éstos o reacción química violenta.
 Al preparar ácidos diluidos debe agregarse siempre el ácido concentrado, en pequeñas
cantidades, sobre el agua y agitar permanentemente.
Calentamiento de sustancias químicas.
 Debido al uso de sustancias volátiles, no debes utilizar dispositivos que generen flama o
chispa durante las prácticas, el calentamiento de las sustancias debe hacerse mediante
parrillas de calentamiento o sistemas de intercambio convectivo (baño maría,
intercambiadores, serpentines, resistencias).
 Antes de conectar dichos dispositivos (o cualquier otro que requiere corriente eléctrica),
asegura la integridad y el buen estado físico de las conexiones y cableado.
 Utiliza guantes apropiados para la manipulación de recipientes que contengan fluidos
calientes, así como superficies a alta temperatura.
Derrame de sustancias químicas.
 Evita el derrame de las sustancias a utilizar en las prácticas sobre la mesa de trabajo. Si algo
se derramara notifica al profesor, de manera que puedan aplicarse los procedimientos de
limpieza adecuados.

Llaves de paso.
 Comprobar que las llaves de gas, aire comprimido y agua estén cerradas en cualquier
instante que no sea necesario su uso.
Actuación en caso de accidente o siniestro.
 En caso de cualquier accidente, debes notificar de inmediato al profesor para tomar las
medidas de actuación pertinentes.
 Si hay salpicadura en los ojos o piel con un ácido, una base o cualquier sustancia química,
lávalos abundantemente con agua por lo menos durante 5 minutos. Si es necesario el
profesor te canalizará al servicio médico disponible.
 En caso de cortadas o quemaduras, dependiendo de la gravedad de las mismas, el profesor
te dará los primeros auxilios con ayuda del botiquín del laboratorio. Si la cortadura o
quemadura es grave serás canalizado inmediatamente al servicio médico disponible.
 Ubica donde se encuentra el extintor, si se presenta riesgo por incendio, úsalo en caso de ser
necesario y sólo sí estás capacitado para ello. Si no te es posible utilizarlo o te encuentras
muy lejos del mismo, da la voz de alarma (diciendo en voz alta FUEGO) para salir del
laboratorio y que el profesor tome las medidas pertinentes al respecto.
 En caso de sismo, abandona el laboratorio con precaución hacia el punto de reunión más
cercano y sigue las indicaciones del profesor. Recuerda verificar que no queden equipos
conectados a la corriente eléctrica, llaves de gas abiertas o reacciones en evolución.
Identificación de riesgos químicos.
 Los frascos y contenedores de reactivos contienen pictogramas y frases que informan sobre
los riesgos químicos asociados a su manipulación y almacenamiento, uso correcto y las
medidas a tomar en caso de ingestión, inhalación o contacto con el cuerpo, antes de
manipular cualquier sustancia revisa está información.

Fig. A. Pictogramas de Riesgo Químico para etiquetado de sustancias.
 Algunos aparatos pueden contener información del mismo tipo. Lee detenidamente esta
información y ten en cuenta las especificaciones que se señalan en ella.
 Al destapar cualquier frasco de sustancias, tápese de inmediato después de utilizarlo y evita
cambiar los tapones.
Medidas específicas de seguridad.
 Las operaciones que se realizan en algunas prácticas requieren información específica de

seguridad. Estas instrucciones son dadas por el profesor y/o recogidas en el protocolo de
prácticas de laboratorio y debes de prestarles una especial atención.
En caso de duda, consulta al profesor.
 Cualquier duda que tengas, consúltala con tu profesor. Recuerda que no está permitido
realizar ninguna experiencia no autorizada por tu profesor.
Equipo de protección personal y vestimenta.
 Es obligatorio usar gafas de seguridad o careta siempre que trabajes en el laboratorio para
evitar que tus ojos puedan resultar dañados. No se permite el uso de lentes de contacto en el
laboratorio.

 El uso de bata es obligatorio en el laboratorio. La bata debe ser de algodón acorde a tu

complexión física y deberás portarla abotonada.
 No está permitido acudir al laboratorio con minifaldas, pantalones cortos o medias.
 Debes presentarte con zapatos cerrados, no está permitido acudir con sandalias o zapatos
con tacón.
 Las personas con cabello largo deberán mantenerlo recogido, preferentemente mediante el
uso de una malla.

Reglamento del Laboratorio.

Responsabilidad.
El presente Reglamento, es de observancia general para todos los usuarios del laboratorio, es
responsabilidad del profesor y de los alumnos, dar cumplimiento al mismo.
1. Presentarse puntualmente al laboratorio, la asistencia se registrará hasta 10 minutos después

de la hora de inicio marcada en el horario de clase.
2. Asistir con bata de algodón abotonada, lentes de seguridad, zapato cerrado, cabello
recogido. No se admitirán alumnos o alumnas con falda, short, sandalias, zapatillas, ni el
uso de gorras deportivas dentro del laboratorio.
3. Previo a cada práctica de laboratorio, es obligación del alumno revisar las Hojas de
Seguridad de las sustancias a utilizar, para conocer las propiedades físicas, químicas y
toxicológicas de las sustancias que se utilizarán, así como tener conocimiento de su uso,
manejo y almacenamiento. Igualmente se debe consultar la metodología a desarrollar en el
experimento, plasmada en el presente Manual de Laboratorio.
4. Durante el desarrollo de la práctica las pertenencias y mochilas de los asistentes deben
permanecer en el estante destinado para tal fin.
5. Los alumnos no podrán iniciar su trabajo práctico si no está presente el profesor. Ningún
alumno debe trabajar solo en el laboratorio.
6. Queda prohibida la utilización de teléfonos celulares y dispositivos electrónicos dentro del
laboratorio, a menos que sea solicitado por el profesor como parte de la actividad.
7. Queda prohibido fumar, comer o beber dentro del laboratorio.
8. No se debe encender cerrillos o dispositivos con flama dentro del laboratorio.
9. Está prohibido hacer cualquier tipo de bromas o jugar en el laboratorio.
10. Todo el personal, profesores y alumnos, nunca deben presentarse a trabajar en el laboratorio
bajo la influencia de bebida alcohólicas, narcóticos o drogas enervantes. La presencia del
alumno en cualquiera de estas circunstancias será motivo de suspensión temporal. Esta
suspensión será autorizada por el Director Académico, quien será avisado de inmediato.
11. La mesa de trabajo, el material y los instrumentos utilizados durante la práctica deberán
dejarse limpios y secos al terminar la práctica. El material utilizado debe entregarse
completo y en buen estado.
12. Durante el desarrollo de la práctica, deberán identificarse correctamente todas las sustancias
químicas.
13. Las soluciones o muestras utilizadas deberán desecharse según instrucciones del profesor
de acuerdo a la toxicidad y riesgo químico de las mismas.
14. Los desechos sólidos como papel, aluminio y plásticos serán colocados en los depósitos que
correspondan.

15. Los reactivos utilizados y proporcionados en su envase, deberán devolverse en buen estado
y cerrados.
16. La entrega de material se efectuará exclusivamente durante los primeros 10 minutos de
cada sesión de laboratorio.
17. Verificar que las llaves de servicios (agua, gas, aire comprimido, vapor) permanezcan
cerradas si no están en uso y queden cerradas al finalizar la práctica.
18. En caso de romper material de vidrio y/o descomponer un equipo, éste deberá ser repuesto
por el alumno, quién deberá llenar correctamente y firmar el vale correspondiente de
adeudo de material, haciendo entrega del mismo a la persona encargada del Laboratorio de
Operaciones Unitarias; el material deberá reponerse en un lapso de 15 días naturales, en
caso de no hacerlo se le impedirá el acceso al laboratorio.
19. El material roto en forma irreparable, deberá colocarse en una bolsa adecuada y en los
depósitos destinados a ese efecto. Nunca desechar materiales contaminados con residuos
tóxicos o corrosivos sin enjuagar, ello representa un riesgo para los usuarios y las personas
que nos dan el servicio de limpieza de los laboratorios.
20. Observar en todo momento las normas y recomendaciones de seguridad en el laboratorio.
21. Al finalizar la práctica, deben lavarse las manos con agua y jabón antes de salir del
laboratorio.
10

Experiment 01. Effect of temperature on the reaction

rate.
Objectives.
1. To analyze the effect of temperature on the value of the specific reaction rate constant.
2. To use the Arrhenius theory to explain the effect of temperature on the reaction rate.
3. To calculate the activation energy in the liquid phase esterification of acetic acid using
experimental data.
4. To determine the thermodynamic parameters of the transition state in the esterification of
acetic acid, according to Eyring equation.
Introduction.
In their experimental studies, Arrhenius and van't Hoff observed that the value of the specific
reaction rate constant increases exponentially when increasing temperature (Fig. 7.1).
Fig. 1.1. Effect of temperature on k value.
Arrhenius obtained an empirical equation that correlates temperature with the value of the
specific reaction rate constant, known as Arrhenius' Law:
Eq. (1)
Where k is the specific reaction rate constant, E a is the activation energy, A is the frequency
factor, R is the universal ideal gas constant and T is the absolute temperature. This exponential
11

equation can be linearized to determine the values of the activation energy and the frequency factor:
Eq. (2)
The theoretical explanation of this phenomenon is given from the collision theory, which
considers chemical reactions occurs because of the collision between the reactant molecules. In this
sense, the activation energy is understood as the minimum energy that the reactant molecules must
possess to collide and form the products, so the exponential term measures the fraction of molecules
that have such as energy. The frequency factor is a reference to the "periodicity" with which the
molecules of the reagents collide and the degree of orientation they have to favor the chemical
reaction.
Fig. 1.2. Collision theory (recovered from de https://theory.labster.com/collision_theory-es/).
Eyring alternatively proposed the transition state theory to explain the effect of temperature
on the reaction rate, which is based on the formation of an intermediate chemical species between
reactants and products whose energy is maximum and with short lifetime, called activated complex.
This proposition is established mathematically through the Eyring Equation:
Eq. (3)
Where k is the specific reaction rate constant, k B is Boltzmann's constant (1.38065 x 10 -23
J/K), h is Planck's constant (6.626 x 10 -34 J ۰ s), G* is the free energy of Gibbs for the activated
complex, T is the absolute temperature and R is the universal ideal gas constant. This expression,
like the Arrhenius one, can be linearized in order to estimate the thermodynamic parameters of the
activated complex:
12

Eq. (4)
Fig. 1.3. Transition state theory (recovered from

https://www.britannica.com/science/transition-state-theory).
Reagents.
 Acetic acid.
 Distilled water.  Ice.

 Ethanol.
Lab materials & equipment.
 2 volumetric flasks (500 mL).  Clamp.

 3 beakers (100 mL).  Stand.
 3 beakers (250 mL).  Spatula.
 2 graduated cylinders (50 mL).  Watch glass.
 10 mL-graduated pippete.  Chronometer.
 Pipette bulb.  Thermometer.
13

 pH meter.  Magnetic and heating plate.

 Temperature sensor.  Science Workshop 759 Interface
 Analytic balance. Pasco ®.
 Magnetic stirring bars.  2 bowls.
Procedure.
1. Put water in a bowl and heat up to 50-60 °C. Place the bath on the stir plate. In another
bowl, place crushed ice and reserve in a cool space.
2. Pour 75 mL of ethanol into each of three 250 beakers and place one of the beakers in the
hot water bath and other in the ice bath. Let the solutions warm for 5 minutes. The third
must remain at room temperature.
3. Place the room-temperature sample over the plate and stir. Put inside the pH meter and the
thermometer and begin the measure.
4. Measure 60 mL of acetic acid and pour it into the beaker from the previous beaker.
5. Add 1.5 mL of sulfuric acid and begin to measure the reaction time (20 minutes).
6. Repeat steps 3 to 5 with the samples from the hot water bath and the ice bath.
Results analysis and report.
1. Use the compiled pH data to determine the concentration of acetic acid for the three
experiments.
t Acetic acid
T
Sample pH concentration
[min]
[°C]
[M]
5
1
(Room 10
temperature)
15
20
2 0
(High
5
temperature)
10
14

15
20
5
3
(Low 10
temperature)
15
20
2. The esterification of acetic acid is an elementary (second order) reaction, then use
concentration data and statistical analysis to determine the value of the specific reaction
rate at each temperature.
T (°C) T (K) k
3. Perform linear regression over the data to calculate the parameters of Arrhenius equation.
Report the activation energy and the frequency factor values. Make a plot of 1/T versus
ln(k) to verify the linearity of the results.
4. Use the linearized form of Eyring equation (Eq. 4) to determine the value of the Gibbs
free energy for the activated complex of the reaction.
5. Look for reported values for the calculated parameters (in bibliography) and compare
them with the values obtained experimentally.
Use the following guide questions to write your conclusions:
1. Do the values of the specific reaction rate constant show an specific behavior with
respect to temperature?
2. What does the activation energy affect this behavior?
3. Are the experimental and reported values of parameters related? Are they similar?
15

4. Is there a trend in the Gibbs free energy of the activated complex as function of
temperature?
Waste disposal.
Waste solutions must be collected in a labeled bottle (Type A: non-halogenated organic

compounds) and kept safe until its final disposal by the personnel of the Engineering Laboratories.
References.
 Ávila-Jiménez, M., Corral-López, E., Fernández-Sánchez, L. y Solís-Correa, H.E. (2005).

Manual de Prácticas de Cinética y Catálisis. México: Universidad Autónoma
Metropololitana.
 Fogler, H.S. (2008). Elementos de Ingeniería de las Reacciones Químicas, 4ª. Edición.
México: Pearson Education.
 Hill, C.G. y Root, T.W. (2014). Introduction to Chemical Engineering Kinetics and
Reactor Design, 2nd Ed. New York: Wiley.
 Obaya, A. y Vargas-Rodríguez, Y. M. (2011). La Enseñanza Experimental de la Química
desde una Perspectiva Interdisciplinaria y Ecológica en Química Verde Experimental.
México: Universidad Nacional Autónoma de México.
 Shakhashiri, B. Z. (1992). Chemical Demonstrations, A Handbook for teachers of
Chemistry Vol 4. The University of Wisconsin Press: Madison, WI.
 Smith, J.M. (1981). Chemical Engineering Kinetics, 3rd Edition. New York: McGraw-Hill.
 Vargas Rodríguez, M. y Obaya, A. (2005). Cálculo de parámetros de rapidez en cinética
química y enzimática. México: Universidad Nacional Autónoma de México.
16

Experiment 02. Saponification of Ethyl Acetate with

NaOH in CSTR a under Pseudo-Steady State Sonditions.
Objectives.
1. To apply experimentally reactor design methodology for CSTR reactors in the

saponification reaction of ethyl acetate with NaOH.
2. To use a chemical analytical technique to follow the progress of a chemical reaction.
Introduction.
A chemical reactor is a process equipment in which one or more chemical reactions are
carried out. Such equipment is designed to maximize the conversion and selectivity of the reaction
towards the products of greatest commercial value while minimizing costs.
According to their mode of operation, these can be classified as:
 Batch reactors: those that work in batches, that is, the reactants are fed and remain
inside the reactor for the time necessary to achieve the desired conversion, according
to the kinetics of the reaction.
 Continuous reactors: those in which the feeding of the reactants and the discharge of
the products are done continuously.
Depending on the phases they contain, we can speak of homogeneous reactors, when the
reactants and products are in a single phase, and heterogeneous reactors, when different phases
coexist (gas-solid, liquid-solid, gas-liquid, liquid-liquid, gas-liquid-solid).
If the flow pattern of the reactants and products within the reactor can be considered ideal
(without backmixing or stagnation effects), they are referred to as ideal reactors, otherwise they are
non-ideal reactors and the effects of the flow pattern must be considered in design.
In chemical processes, three basic types of ideal homogeneous reactors are considered:
Batch reactors: they work at non-steady state and the simplest would be a stirred tank reactor.
Continuous stirred tank reactors (CSTR): they work at steady state, that is, their properties do
not vary over time. This requires the assumption that the reaction reaches maximum conversion
when the feed enters the tank, this involves that outlet stream properties are equal to those at any
point inside the reactor.
17

Plug flow reactors (PFR): these reactors also operate at steady state, in this model, an ideal
plug flow is assumed and the conversion is a function of the position or length of the reactor.
Fig. 2.1. Tipos de reactores ideales homogéneos (Tomada de Levenspiel, O. (1999), Chemical Reaction
Engineering, 3rd Ed. New York: Wiley).
For most industrial reactions, these models are valid, otherwise the appropriate material,
energy and momentum balances must be considered to model deviation from ideality.
In this experiment, the saponification reaction of ethyl acetate with sodium hydroxide will be
carried out, whose thermodynamic and kinetic parameters have already been determined in the
previous course. Reaction will be carried out in a continuous stirred tank reactor on a laboratory
scale and under pseudo-steady state conditions. For this type of reactors, the conversion achieved
depends on the reaction volume, the reaction kinetics and the feed flow, according to the following
design equation:
Eq. (1)
Reagents.
 Ethyl acetate.  Sodium hydroxide (NaOH).

 Distilled water.
18

 5 L Glass tank reactor.  Watch glass.

 Chiller system FC-20P.  10 mL pipette.
 1 L volumetric flasks (2 pieces).  Pipette bulb.
 250 mL bakers (2 pieces).  Thermometer.
 1 L bakers (2 pieces).  pH meter probe.
 1 L dosing bottles (2 pieces).  Temperature meter probe.
 50 mL graduated cylinder.  Analytical balance.
 100 mL graduated cylinder.  Magnetic stirrers.
 1L graduated cylinder.  Magnetic and heating plate.
 Chronometer.  Science Workshop 759 Interface
 Spatula. Pasco ®.
 2 m latex hoses (3 pieces).
Procedure.
A. Part I. Solutions preparation and reactor calibration.

1. Prepare 5 liter (0.06 M) standard solutions of NaOH and ethyl acetate
2. Connect the hoses from the chiller to the corresponding flanges on the bioreactor. Turn
on the chiller and set the set point to 30°C. Start water circulation to the reactor.
3. Put the latex hoses through peristaltic pumps and fill a container with distilled water.
Rinse feed vessels with distilled water.
4. Pour NaOH and ethyl acetate solutions in feed vessels (dosing bottles).
5. Adjust peristaltic pumps (1 and 2) to deliver 50 mL/min flowrate for each reagent and
100 mL/min of outlet stream (pump 3).
6. Note down the pH of the NaOH in feed vessel.
7. Turn on stirrer and adjust to 500 rpm.
8. Place the temperature meter probe inside the well and check that it works correctly.
B. Parte II. Pseudo-steady state reaction in CSTR.

1. Start dosing the two solutions from the feed vessels and recirculate the output flow back to
the reactor. Start the chronometer.
2. Keep monitoring the pH and temperature of the reaction mixture after every 5 minutes.
Take readings until (pseudo) steady state is achieved i.e. nearly 45 minutes.
19

3. When pseudo-steady state conditions are reached, turn off the peristaltic pumps. Drain the
reactor content into a measuring flask (graduated cylinder) and note down the volume of
reaction mixture in CSTR.
4. Wash reactor with distilled water and drain any residual water. Turn off electrical
connections.
1. Saponification of ethyl acetate is a 2nd order elementary reaction. Record the results of
the experiment in the following table, use pH values measure to determine the NAOH
concentration.
t T Conc. NaOH
Sample. pH
[min] [°C] [M]
1 0 0.06 M
2 5
3 10
4 15
5 20
6 25
7 30
8 35
9 40
10 45
2. Plot NaOH concentration versus time and determine the reaction rate law for the
saponification of ethyl acetate.
3. Make a mole balance for NaOH and calculate the conversion achieved at steady state
conditions.
20

4. Use the CSTR design equation to determine the reactor volume at pseudo-steady state
conditions, compare this values with that measured in the experiment.
Use the following questions to conclude about the experiment.
1. What was the behavior of pH (and NaOH concentration) along the experiment? Can this
be descript as a batch reactor?
2. Are the experimental and theoretical values obtained for the reactor volume related?
Waste disposal.
Waste solutions must be collected in a labeled bottle (Type A: non-halogenated

organic compounds) and kept safe until its final disposal by the personnel of the
Engineering Laboratories.
References.
 Fogler, H.S. (2022). Elements of Chemical Reaction engineering, 6ª. Edition. México:
Pearson Education.
 Levenspiel, O. (1999). Chemical Reaction Engineering, 3rd Edition. New York: Wiley.
Experiment 03. Reaction of crystal violet with NaOH in

an isothermal semi-continuous reactor.
Objectives.
1. To analyze the operation of a semi-continuous homogeneous reactor on a laboratory scale

and compare it with the theoretical model.
2. To use a spectroscopic analytical technique to follow the progress of a chemical reaction.
21

Introduction.
Reactors are classified by their flow regime, whether fed in a single step it is called a
batch reactor, while in the other extreme continuous reactors are characterized by the
continuous inlet and outlet of material streams. In the middle of both are the semi-batch or
semi-continuous reactors, their operation consists of feeding some chemical species with a
continuous flow, while others were previously fed and do not allow output.
Possible configurations for semi-batch reactors are:
 Variable volume: one or more reagents are loaded at the beginning of operation and
the others are fed continuously, without allowing the exit of any species.
 Constant volume: a reagent is fed continuously, it passes through the system and the
unconsumed fraction is removed with the products.
Semi-batch reactors offers offer advantages in the control of temperature for

reactions in which a large amount of heat must be transferred or when a high selectivity is
desired. They help to solve the problem of the limited solubility of some gases in liquids
and increase the reaction rate in reversible reactions when some product is gaseous and is
evacuated from the system. They present a lot of flexibility, since that multiple types of
reactions can be carried out in it.
In this experiment, the reaction between crystal violet and sodium hydroxide will be
carried out, the progress of which can be followed using spectrophotometric methods given
the change in color experienced by the reaction medium:
Reagents.
 Crystal violet.  Sodium hydroxide (NaOH).

 Distilled water.  Ethanol.
 250 mL volumetric flasks.  1L graduated cylinder.

 500 mL volumetric flasks.  Chronometer.
 250 mL bakers (2 pieces)  Spatula.
 1 L bakers (2 pieces).  Watch glass (2 pieces).
 50 mL graduated cylinder.  10 mL pipette.
22

 Pipette bulb.  Colorimeter.

 Thermometer.  Spectrophotometric cuvettes (4
 Analytical balance. pieces).
 Magnetic stirrers.  Science Workshop 759 Interface
 Magnetic and heating plate. Pasco ®.
 Peristaltic pump.  1 m latex hoses (2 pieces).
Procedure.
A. Part I. Solutions preparation and colorimeter calibration.

1. Prepare 250 mL of crystal violet standard solution (1.5×10 -5 M), in order to improve
solubility add 10 drops of ethanol.
2. Prepare 500 mL of NaOH standard solution (6×10-3 M).
3. Put the latex hoses through peristaltic pump and pour the NaOH solution in a 1 L baker
(this will be the feed vessel).
4. Adjust peristaltic pump to deliver 5 mL/min flowrate for NaOH solution.
5. Turn on the colorimeter. Calibrate it at 460 nm using a cuvette with distilled water,
absorbance for this must zero.
6. Place the reactor (1 L baker) on the stirring plate and place the thermometer inside it.
B. Parte II. Reaction in semi-batch vessel.

5. Pour the crystal violet solution in the reactor and start to stir it.
6. Start to feed the NaOH solution to the reactor and the measure of time reaction.
7. Keep monitoring the absorbance of the reaction media and temperature every 3 minutes,
during a 45-minute span. For concentration measure take a sample of the reaction media
with a clean pipette and pour quickly in a spectrometric cuvette, place it in the colorimeter
and note the first measured value (for calculation the time of reaction must be done by the
instant in which measure is done). Return the sample to the reactor.
8. When the time span finished stop NaOH feeding and take the last sample. After measure
drain the reactor content into a measuring flask (graduated cylinder) and note down the
volume of reaction mixture.
1. Reaction of crystal violet with NaOH is a 2nd order elementary reaction. Record the results of
the experiment in the following table and use the following equation to calculate the crystal
violet concentration dependent on absorbance:
23

t T Ccv
Sample. A
[min] [°C] [M]
1 1.5×10-6 M
10
2. Plot crystal violet concentration versus time and determine the reaction rate law for the
reaction.
3. Use the initial and final concentration values to calculate the conversion achieved in the
reactor:
4. Complete your results table by calculating the change in volume during the reaction:
5. State the molar balance for the reactor in terms of the conversion and solve it using an
appropriate numerical method or software in order to obtain the theoretical conversion,
compare this value with that achieved in the experiment.
1. What was the behavior of concentration along the experiment? Can this be descript as a
batch reactor or a continuous one?
2. Are the experimental and theoretical values obtained for the conversion similar?
24

Waste disposal.
Waste solutions must be collected in a labeled bottle (Type A: non-halogenated

organic compounds) and kept safe until its final disposal by the personnel of the
Engineering Laboratories.
References.
Pearson Education.
Experiment 04. Kinetics of adsorption on solids.

Objectives.
1. To study the adsorption phenomenon in solids as the foundations of heterogeneous

catalysis.
2. To use experimental data to evaluate the parameters of the Langmuir, Freundlich and BET
models.
3. To correlate the models that describe adsorption isotherms to the physicochemical and
structural properties of solid catalysts (such as surface area, diameter and pore volume).
Introduction.
Adsorption is a surface phenomenon that occurs when two phases are in contact,
there is a region called interface where the composition is different from that of the rest of
the phases. Adsorption is particularly referred to the interaction between a fluid and solid
interfaces; the solid is called an adsorbent or sorbent and the adsorbed fluid particles
sorbate or adsorbate. The increase in the concentration of a substance at the interface,
compared to the bulk concentration is consequence of molecular forces between specific
molecules in the fluid phase and surface solid species.
Even the most carefully polished surfaces, viewed microscopically, present

irregularities throughout the area. These surfaces are particularly susceptible to presence of
25

residual force fields. In these places (also called active sites), atoms on the surface of the
solid can attract other atoms or molecules from the surrounding fluid phase (see Figure 4.1).
Thus, the surface activity of solids is responsible for the adsorption mechanism.
Adsorption of a solute on a surface can be physical or chemical. In physical

adsorption, called physisorption, the adsorbate binds to the adsorbent with relatively weak
forces (Van der Waals type), it is reversible, the activation energy of the process is very
small or negligible and more than one layer of adsorbed solute can be formed.
In chemical adsorption, called chemisorption, there is sharing of electrons between

the adsorbate and the surface of the adsorbent, so a chemical reaction occurs. The bond
formed between the adsorbent and the adsorbate is essentially chemical and therefore
stronger than physical adsorption. The chemisorption sometimes requires energy, activation
energy and heat of chemisorption are high, usually greater than in physical adsorption, the
consequence of that is the formation of a monolayer (a layer of monomolecular thickness)
and it is irreversible.
Fig. 4.1. Adsorption phenomena in solid surfaces.

(https://www.shutterstock.com/es/image-vector/surface-catalyst-carbon-monoxide-dioxide-catalysis-
1971129149).
The relationship between the amount of sorbate over a given amount of mass of
adsorbent and the concentration of the fluid phase in an experiment carried out at
temperature constant, when represented graphically, is called adsorption isotherm. The
shape of this isotherm varies when either of the two components changes (adsorbent or
adsorbate) and it can be correlated with the physicochemical and structural properties of the
solid as like to the nature of the interaction forces between the surface and the bulk fluid.
IUPAC recognizes five types of adsorption isotherms based on their graphic behavior. All
of them can be described based on specific theoretical models:
26

Langmuir Isotherm
… Eq. (1)
Freundlich Isotherm
… Eq. (2)
Brunauer-Emmett-Teller (BET) Isotherm

… Eq. (3)
Temkin Isotherm
… Eq. (4)
Reagents.
 Activated carbon (powder).  Ice.

 Distilled water.  Phenolphthalein.
 Ethanol.  Sodium hydroxide (NaOH).
 Glacial acetic acid.
 100 mL volumetric flasks (6 pieces).  Watch glass (2 pieces).

 1 L volumetric flasks (2 pieces).  10 mL pipette.
 50 mL burette (2 pieces).  Pipette bulb.
 Büchner funnel.  Stand.
 150 mL Kitasato flask.  Clamp.
 Whatman No. 5 filter paper.  Thermometer.
 150 mL Erlenmeyer flasks (6 pieces).  Rubber stoppers.
 250 mL Erlenmeyer flasks (6 pieces).  Analytical balance.
 250 mL bakers (2 pieces).  Magnetic stirrers.
 50 mL graduated cylinder.  Magnetic and heating plate.
 Chronometer.  Vacuum pump.
 Spatula.  1 m latex hoses (2 pieces).
27

Procedure.
1. Prepare a 0.4 M standard acetic acid in a 1 L volumetric flask.

2. Prepare a 0.1 M standard NaOH solution in a 1L volumetric flask.
3. Weight 1 g of activated carbon in each of the 125 mL Erlenmeyer flasks.
4. Fill a 50 mL burette with the 0.4 M acetic acid solution. Number each of the 100 mL
volumetric flasks and add to each the volume indicated below and complete the necessary
volume to prepare the samples.
Sample Acetic acid volume [mL]
1 5
2 10
3 20
4 30
5 40
6 50
5. Pour the samples into each of the flasks with the activated carbon and cover, stir the mixtures
continuously for 15 minutes.
6. Vacuum filter the solutions and reserve each one in a 250 mL beaker.
7. Take 10 mL of each sample and empty it into a clean Erlenmeyer flask. Add two drops of
phenolphthalein and titrate with 0.1 M sodium hydroxide. Record the volume of NaOH
solution used for titration.
1. Record the results of the experiment in the following table, calculate the initial an equilibrium
concentration by using the following equations:
28

Vaa T C0 Ceq nads

Sample. VNaOH [mL]
[mL] [°C] [M] [M] [mol/g]
1 5
2 10
3 20
4 30
5 40
6 50
2. Calculate the amount of acetic acid adsorbed per adsorbent gram and record the values in the
table:
3. Plot the equilibrium concentration versus the amount of adsorbed acid and determine the
isotherm type.
4. Determine the parameters for the Langmuir Equation using the following linear model; N m
parameter must be read from the graph in previous point:
5. Establish the parameters for the Freundlich isotherm by adjusting the experimental data to the
following linear model:
29

6. Calculate the parameters for the BET isotherm by the following linear model:
7. Calculate the specific area of the activated carbon, considering that the area (σ) of the acetic
acid is equal to 21 Å 2, by the following equation.
8. Determine the heat of adsorption by the BET equation and the % of covered surface:
1. What was the behavior of equilibrium concentration versus adsorbed amount of acid?
What type of isotherm it correspond to? What kind of adsorption did you study
experimentally?
2. Are the experimental values obtained for the adsorption equilibrium constant?
3. What can you conclude about the properties of the activated carbon as adsorbent?
Waste disposal.
Waste solutions must be collected in a labeled bottle (Type E: partially neutralized acidic
solutions) and kept safe until its final disposal by the personnel of the Engineering Laboratories.
References.
Pearson Education.
30


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Laboratorio de Reactores Químicos II

Manual de Prácticas de Laboratorio

Ubicación de dispositivos de seguridad...........................................................................................5

Uso y manipulación de sustancias químicas....................................................................................5

Calentamiento de sustancias químicas.............................................................................................5

Derrame de sustancias químicas.......................................................................................................6

Actuación en caso de accidente o siniestro......................................................................................6

Identificación de riesgos químicos...................................................................................................6

Medidas específicas de seguridad....................................................................................................7

En caso de duda, consulta al profesor..............................................................................................7

Equipo de protección personal y vestimenta....................................................................................8

Reglamento del Laboratorio..............................................................................................................9

Experiment 01. Effect of temperature on the reaction rate.........................................................11

Lab materials & equipment............................................................................................................13

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Results analysis and report.............................................................................................................14

Lab materials & equipment............................................................................................................19

Results analysis and report.............................................................................................................20

Experiment 03. Reaction of crystal violet with NaOH in an isothermal semi-continuous

Lab materials & equipment............................................................................................................23

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Results analysis and report.............................................................................................................24

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Uso y manipulación de sustancias químicas.

 Revisa los pictogramas de seguridad presentes en la etiqueta de los envases de las

Calentamiento de sustancias químicas.

Derrame de sustancias químicas.

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Actuación en caso de accidente o siniestro.

Identificación de riesgos químicos.

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Fig. A. Pictogramas de Riesgo Químico para etiquetado de sustancias.

Medidas específicas de seguridad.

 Las operaciones que se realizan en algunas prácticas requieren información específica de

En caso de duda, consulta al profesor.

Equipo de protección personal y vestimenta.

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 El uso de bata es obligatorio en el laboratorio. La bata debe ser de algodón acorde a tu

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Reglamento del Laboratorio.

1. Presentarse puntualmente al laboratorio, la asistencia se registrará hasta 10 minutos después

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Experiment 01. Effect of temperature on the reaction

Fig. 1.1. Effect of temperature on k value.

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Fig. 1.2. Collision theory (recovered from de https://theory.labster.com/collision_theory-es/).

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Fig. 1.3. Transition state theory (recovered from

 Distilled water.  Ice.

Lab materials & equipment.

 2 volumetric flasks (500 mL).  Clamp.

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 pH meter.  Magnetic and heating plate.

Results analysis and report.

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Use the following guide questions to write your conclusions:

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Waste solutions must be collected in a labeled bottle (Type A: non-halogenated organic

 Ávila-Jiménez, M., Corral-López, E., Fernández-Sánchez, L. y Solís-Correa, H.E. (2005).

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Experiment 02. Saponification of Ethyl Acetate with

1. To apply experimentally reactor design methodology for CSTR reactors in the

According to their mode of operation, these can be classified as: