STUDENT NAME: Manda Baboolal

COURSE CODE: Core Chemistry Laboratory II

LAB DAY: Tuesday

DATE: 21/01/2019

EXPERIMENT #2: Synthesis and Spectroscopic Analysis of Cobalt (III) and Chromium
(III) Complexes
Objectives:

 To synthesize the chromium complex, chromium (III) acetylacetonate, Cr(acac)3.

 To synthesize two cobalt complexes, nitropentaaminecobalt(III), [Co(NH3)5(ONO)]Cl2,
[Co(NH3)5(NO2)]Cl2 .
 Analyze the UV-Vis, IR and NMR spectral data for the chromium and cobalt complexes.
 To identify features of electronic, vibrational and NMR spectra.

Introduction:

This experiment involves the investigation of chromium (iii) and cobalt (iii) complexes through
synthesis and spectroscopic analysis. The synthesis of the cobalt complex,
pentaaminechlorocobalt (iii) gives rise to two linkage isomers, the nitro and nitrito complexes.

The nitrito isomer is less stable and can easily be converted to the nitro isomer by heating with
HCl.

The nitrite ion can coordinate to transition metals through the nitrogen or oxygen atom. This can
happen in the following ways:

1. If donation occurs from the nitrogen atom to the metal center, a nitro- complex is formed
which is blue violet in color.
2. If donation is from one oxygen atom to a metal center, it is known as a nitrito complex
with a red violet color.
3. Donation can also occur from both oxygen atoms, forming a chelate complex.
4. An unsymmetrical bridge is formed from the nitrite ion, between the two metal centers, in
which donation occurs from the nitrogen to the metal atom and from oxygen to the metal
atom.
5. Two metal atoms can bridge from a single oxygen atom.

Nitropentaaminecobalt(iii) chloride is an orange soluble inorganic compound.

[Co(NH3)5(NO2)]2+ and [Co(NH3)5(ONO)]2+ is an example of linkage isomerism. This
nitritopentaamminecobalt(III) isomer converts to the more stable nitro form at room temperature.
The two isomers can be distinguished by UV-Vis spectroscopy. Absorbance maxima for the nitro
isomer occur at 457.5, 325, and 239 nm. The nitrito has maxima at 486, 330, and 220 nm.

Their IR spectra can also be used to distinguish between the two isomers. Their wavelengths are
different. The nitrito isomer absorbs at 1460 and 1065 cm−1. The nitro isomer absorbs at 1430
and 825 cm−1.

[(NH3)5Co(Cl)]Cl2 reacts with sodium nitrite NaNO2 such that the nitrite ion NO2 replaces the
chloride ion Cl- to form [(NH3)5Co(nitrite)]Cl2. The ionic equation for the reaction is given
below.

[(NH3)5Co(Cl)]2+ + NO2-  [(NH3)5 Co(nitrite)]2+ + Cl-

The pH of these two complexes must be kept at 7 because at this pH, the lone pairs do not
protonate, and they are able to coordinate with the central metal atom.a

Acetylacetone is a bidentate ligand that has two tautomeric forms: keto and enol. The preparation
of tris(acetylacetonato) chromium (iii) will then be analyzed by IR and NMR spectra.

Synthesis of Cr(acac)3 is done by chromium (iii) hexahydrate, acetylacetone and urea. The
equation for the synthesis is shown below:

CrCl3·6 H2O + 2 (NH2)2CO + 3 C5H8O2 → Cr(C5H7O 2 )3 + 2CO 2 +4 NH4+ + OH- + 3 Cl- +

3H2O.

These complexes are then analyzed using UV VIS spectrometry. This is process by which light
in the visible and adjacent ranges are used. In UV VIS, a beam with a wavelength that varies
between 180 and 1100nm will pass through a solution placed in a cuvette. The sample will
absorb UV radiation. The light that has passed through is then focused onto the entrance slit of
the monochromator. This separates light by wavelength using a dispersing element which is then
focused onto a CCD dectector. It is then read off to a computer and the spectrum is displayed.
The following diagram shows the structure of the spectrometer.
MSDS of Reagents

CoCl2.6H2O

First Aid Measures

First-aid measures general: Check the vital functions. Unconscious: maintain adequate airway
and respiration. Respiratory arrest: artificial respiration or oxygen. Cardiac arrest: perform
resuscitation. Victim conscious with labored breathing: half-seated. Victim in shock: on his back
with legs slightly raised. Vomiting: prevent asphyxia/aspiration pneumonia. Prevent cooling by
covering the victim (no warming up). Keep watching the victim. Give psychological aid. Keep
the victim calm, avoid physical strain. Depending on the victim's condition: doctor/hospital.

First-aid measures after inhalation: Remove the victim into fresh air.

First-aid measures after skin contact: Wash immediately with lots of water. Soap may be used.
Do not apply (chemical) neutralizing agents. Take victim to a doctor if irritation persists.

First-aid measures after eye contact: Rinse with water. Do not apply neutralizing agents. Take
victim to an ophthalmologist if irritation persists.

First-aid measures after ingestion: Rinse mouth with water. Immediately after ingestion: give lots
of water to drink.

Handling and storage

Precautions for safe handling: Comply with the legal requirements. Remove contaminated
clothing immediately. Clean contaminated clothing. Thoroughly clean/dry the installation before
use. Do not discharge the waste into the drain. Avoid raising dust. Keep away from naked
flames/heat. Observe very strict hygiene - avoid contact. Keep container tightly closed. Measure
the concentration in the air regularly. Carry operations in the open/under local
exhaust/ventilation or with respiratory protection.

Hygiene measures: Wash hands and other exposed areas with mild soap and water before eating,
drinking or smoking and when leaving work.

Physical and Chemical Properties:

Solid Appearance: Crystalline solid. Crystalline powder.

Color: Rose to red

Odor: Mild odour Irritating/pungent odour

pH: 3 - 5.5 (5.0 %)

pH solution: 5 %

Melting point: 86 °C

95% Ethanol

First Aid Measures

First-aid measures general: Check the vital functions. Unconscious: maintain adequate airway
and respiration. Respiratory arrest: artificial respiration or oxygen. Cardiac arrest: perform
resuscitation. Victim conscious with labored breathing: half-seated. Victim in shock: on his back
with legs slightly raised. Vomiting: prevent asphyxia/aspiration pneumonia. Prevent cooling by
covering the victim (no warming up). Keep watching the victim. Give psychological aid. Keep
the victim calm, avoid physical strain. Depending on the victim's condition: doctor/hospital.
Never give alcohol to drink.

First-aid measures after inhalation: Remove the victim into fresh air. Respiratory problems:
consult a doctor/medical service.

First-aid measures after skin contact: Rinse with water. Take victim to a doctor if irritation
persists.

First-aid measures after eye contact: Rinse immediately with plenty of water. Do not apply
neutralizing agents. Take victim to an ophthalmologist if irritation persists.

First-aid measures after ingestion: Rinse mouth with water. Do not induce vomiting.

Handling and storage

Precautions for safe handling: Comply with the legal requirements. Remove contaminated
clothing immediately. Clean contaminated clothing. Handle uncleaned empty containers as full
ones. Thoroughly clean/dry the installation before use. Do not discharge the waste into the drain.
Do not use compressed air for pumping over. Use spark-/explosionproof appliances and lighting
system. Take precautions against electrostatic charges. Keep away from naked flames/heat. Keep
away from ignition sources/sparks. Observe normal hygiene standards. Keep container tightly
closed. Measure the concentration in the air regularly. Work under local exhaust/ventilation.

Hygiene measures: Wash exposed skin thoroughly after handling.

Physical and Chemical Properties:

Physical state: Liquid

Appearance: Liquid.

Molecular mass: 46.07 g/mol

Color: Colourless.

Odor: Alcohol odour. Pleasant odour.

Odor threshold: 100 ppm 188 mg/m³

Relative evaporation rate (butyl acetate=1): 2.4

Relative evaporation rate (ether=1): 8.3

Melting point: -115 °C

Freezing point: No data available

Boiling point: 78 °C

Sodium Nitrite

First Aid Measures

General advice Consult a physician. Show this safety data sheet to the doctor in attendance.

If inhaled If breathed in, move person into fresh air. If not breathing, give artificial respiration.
Consult a physician.

In case of skin contact Wash off with soap and plenty of water. Take victim immediately to
hospital. Consult a physician.

In case of eye contact Rinse thoroughly with plenty of water for at least 15 minutes and consult
a physician.

If swallowed Never give anything by mouth to an unconscious person. Rinse mouth with water.
Consult a physician.

Handling and storage

Precautions for safe handling Avoid contact with skin and eyes. Avoid formation of dust and
aerosols. Provide appropriate exhaust ventilation at places where dust is formed. Keep away
from sources of ignition - No smoking. Keep away from heat and sources of ignition. For
precautions see section 2.2. 7.2
Conditions for safe storage, including any incompatibilities: Store in cool place. Keep container
tightly closed in a dry and well-ventilated place. hygroscopic Storage class (TRGS 510):
Oxidizing hazardous materials

Physical and Chemical Properties:

Appearance Form: solid

Odour: odourless

pH: 9

Melting point/freezing Melting point/range: 271 °C - lit. point

Initial boiling point and 320 °C boiling range

Pentaaminechlorocobalt (III) chloride

First Aid Measures

After inhalation: Supply fresh air and be sure to call for a doctor.

Supply fresh air. If required, provide artificial respiration. Keep patient warm.

Seek immediate medical advice.

After skin contact: Immediately wash with water and soap and rinse thoroughly.

Seek medical advice.

After eye contact: Rinse opened eye for several minutes under running water. Then consult a
doctor.

After swallowing: Seek immediate medical advice.

Handling and Storage

Handling- information for safe handling:

Keep container tightly sealed. Store in a cool dry place in tightly closed containers. Ensure good
ventilation at the workplace.

Storage- Store away from oxidizing agents. Keep container tightly sealed. Store in a cool, dry
conditions in well-sealed containers.

HCl (4M and 6M)

First Aid Measures

First-aid measures general: Never give anything by mouth to an unconscious person. If you feel
unwell, seek medical advice (show the label where possible). First-aid measures after inhalation :
Remove victim to fresh air and keep at rest in a position comfortable for breathing. Immediately
call a poison center or doctor/physician.

First-aid measures after skin contact: Remove/Take off immediately all contaminated clothing.
Rinse skin with water/shower. Immediately call a poison center or doctor/physician.

First-aid measures after eye contact: Rinse cautiously with water for several minutes. Remove
contact lenses, if present and easy to do. Continue rinsing. Immediately call a poison center or
doctor/physician.

First-aid measures after ingestion: Rinse mouth. Do NOT induce vomiting. Immediately call a
poison center or doctor/physician.

Handling and Storage:

Precautions for safe handling: Wash hands and other exposed areas with mild soap and water
before eating, drinking or smoking and when leaving work. Provide good ventilation in process
area to prevent formation of vapor. Do not breathe mist, vapors, spray.

Hygiene measures: Wash exposed skin thoroughly after handling. Wash contaminated clothing
before reuse.

Technical measures: Comply with applicable regulations.

Storage conditions: Keep only in the original container in a cool, well ventilated place away
from: incompatible materials. Keep container closed when not in use.

Incompatible products: metals. cyanides. Strong bases. Strong acids.

Incompatible materials: Direct sunlight.

Packaging materials: Do not store in corrodible metal.

Physical and Chemical Properties:

Physical state: Liquid

Color: Colorless

Odor: Odorless

pH: ≤ 0.5
Urea

First Aid Measures

Eyes: Immediately flush eyes with plenty of water for at least 15 minutes, occasionally lifting the
upper and lower eyelids. Get medical aid.
Skin: Get medical aid. Immediately flush skin with plenty of water for at least 15 minutes while
removing contaminated clothing and shoes.
Ingestion: Get medical aid. Do NOT induce vomiting. If conscious and alert, rinse mouth and
drink 2-4 cupsful of milk or water.
Inhalation: Remove from exposure and move to fresh air immediately. If not breathing, give
artificial respiration. If breathing is difficult, give oxygen. Get medical aid.

Handling and Storage:

Handling: Use with adequate ventilation. Minimize dust generation and accumulation. Avoid
breathing dust, mist, or vapor. Avoid contact with eyes, skin, and clothing. Avoid ingestion and
inhalation.
Storage: Store in a cool, dry place. Store in a tightly closed container.

Physical and Chemical Properties:

Physical State: Solid
Appearance: white
Odor: ammonia-like
pH: 7.5-9.5 (10% aq. solution)
Vapor Pressure: 1.25 mm Hg @ 25 deg C
Boiling Point: decomposes
Freezing/Melting Point:131-135 deg C

Acetylacetone

First Aid Measures

Eyes: Flush eyes with plenty of water for at least 15 minutes, occasionally lifting the upper and
lower eyelids. Get medical aid.
Skin: Get medical aid. Flush skin with plenty of water for at least 15 minutes while removing
contaminated clothing and shoes.
Ingestion: Call a poison control center. If swallowed, do not induce vomiting unless directed to
do so by medical personnel. Never give anything by mouth to an unconscious person. Get
medical aid.
Inhalation: Remove from exposure and move to fresh air immediately. If not breathing, give
artificial respiration. If breathing is difficult, give oxygen. Get medical aid.
Notes to Physician: Treat symptomatically and supportively.
Handling and Storage

Handling: Use only in a well-ventilated area. Ground and bond containers when transferring
material. Use spark-proof tools and explosion proof equipment. Do not get in eyes, on skin, or on
clothing. Empty containers retain product residue, (liquid and/or vapor), and can be dangerous.
Keep container tightly closed. Keep away from heat, sparks and flame. Do not ingest or inhale.
Do not pressurize, cut, weld, braze, solder, drill, grind, or expose empty containers to heat,
sparks or open flames.
Storage: Keep away from heat, sparks, and flame. Keep away from sources of ignition. Store in a
tightly closed container. Store in a cool, dry, well-ventilated area away from incompatible
substances. Flammables-area.

Physical and Chemical Properties

Physical State: Liquid
Appearance: colorless or slight yellow
Odor: putrid odor
pH: Not available.
Vapor Pressure: 6 mm Hg @ 20 deg C
Evaporation Rate:0.75 (n-butyl acetate=1)
Boiling Point: 139 - 141 deg C
Freezing/Melting Point:-23 deg C

Ammonia (2M)

First Aid Measures

Eyes: Immediately flush eyes with plenty of water for at least 15 minutes, occasionally lifting the
upper and lower eyelids. Get medical aid immediately.
Skin: Get medical aid immediately. Immediately flush skin with plenty of water for at least 15
minutes while removing contaminated clothing and shoes.
Ingestion: Do not induce vomiting. Get medical aid immediately. Call a poison control center.
Inhalation: Remove from exposure and move to fresh air immediately. If breathing is difficult,
give oxygen. SPEED IS ESSENTIAL, OBTAIN MEDICAL AID IMMEDIATELY. Do not use
mouth-to-mouth resuscitation if victim ingested or inhaled the substance; induce artificial
respiration with the aid of a pocket mask equipped with a one-way valve or other proper
respiratory medical device.

Handling and Storage

Handling: Do not get in eyes, on skin, or on clothing. Do not ingest or inhale. Use only in a
chemical fume hood.
Storage: Store in a cool, dry place. Do not store in direct sunlight. Store in a tightly closed
container. Corrosives area.

Physical and Chemical Properties

Physical State: Liquid
Appearance: clear, colorless
Odor: strong odor - ammonia-like
pH: 13.6
Vapor Pressure: 557 mm Hg @ 21 deg C
Vapor Density: 0.59 (air=1)
Boiling Point: 27 deg C
Freezing/Melting Point:-69 deg C
Solubility: Soluble.
Specific Gravity/Density:0.89
Molecular Formula:NH4OH
Molecular Weight:35.04

CrCl2.6H2O (Cobalt (II) Chloride Hexahydrate)

First Aid Measures

Eyes: Immediately flush eyes with plenty of water for at least 15 minutes, occasionally lifting the
upper and lower eyelids. Get medical aid.
Skin: Get medical aid. Flush skin with plenty of water for at least 15 minutes while removing
contaminated clothing and shoes. Wash clothing before reuse.
Ingestion: Do not induce vomiting. If victim is conscious and alert, give 2-4 cupsful of milk or
water. Never give anything by mouth to an unconscious person. Get medical aid.
Inhalation: Remove from exposure and move to fresh air immediately. If breathing is difficult,
give oxygen. Get medical aid. Do NOT use mouth-to-mouth resuscitation.
Notes to Physician: Treat symptomatically and supportively.

Handling and Storage

Handling: Use with adequate ventilation. Minimize dust generation and accumulation. Avoid
contact with skin and eyes. Keep container tightly closed. Avoid ingestion and inhalation.
Storage: Store in a cool, dry, well-ventilated area away from incompatible substances.

Physical and Chemical Properties

Physical State: Solid
Appearance: purple
Odor: none reported
pH: 4.6 @ M solution.
Boiling Point: 1048.9 deg C
Freezing/Melting Point:87 deg C
Decomposition Temperature:110 deg C
Solubility: 77 g/100ml (0 C)
Specific Gravity/Density:1.924
Molecular Formula:CoCl2.6H2O
Molecular Weight:237.9196
RESULTS:

Part A

Part 1

Mass of pentaaminechlorocobalt(III)chloride

Mass of beaker 18.7g

Mass of beaker + complex 18.9532g
Mass of penntaaminechlorocobalt(III)chloride 0.2532g

Mass of NaNO2

Mass of watch glass 9.2190g

Mass of watch glass + NaNO2 9.4724g
Mass of NaNO2 0.2534g

Mass of nitrito complex

Mass of vial 12.4195g

Mass of vial + nitrito 12.4226g
Mass of nitrito 0.0031g

Part II

Mass of pentaaminechlorocobalt(III)chloride

Mass of beaker 18.4343g

Mass of beaker + complex 18.6984g
Mass of penntaaminechlorocobalt(III)chloride 0.2641g

Mass of NaNO2

Mass of watch glass 5.2081g

Mass of watch glass + NaNO2 5.5600g
Mass of NaNO2 5.2081g
Mass of nitro complex

Mass of vial 10.0506g

Mass of vial + nitro 10.3160g
Mass of nitro 0.2654g

Part B

Mass of urea used: 2.0102g

Mass of CrCl3.6H2O: 0.2505g

Mass of Cr(acac)3

Mass of vial 7.8958g

Mass of vial + Cr(acac)3 7.9355g
Mass of Cr(acac)3 0.0397g
DISCUSSION:

From the experiment performed, the precautions that were taken is to reduce parallax error when
measuring the distilled water by reding the meniscus of the measuring cylinder and the burette
containing acetyl acetone.

In Part A of the experiment for the formation of nitro and nitrito complexes, resulted in the
formation of a small amount of product for nitrito which was 0.0031g. This was way less than
the expected mass to be formed. The possible sources of error can be due to impurities of the
pentaaminechlorocobalt (iii) chloride and sodium nitrite. Another error can be environmental
factors such as wind that can affect heating and reduce temperatures causing less product to be
formed. During the filtering process, using the wrong sized filter paper and folding technique can
absorb too much liquid. Adjusting the pH can also give rise to errors. Not washing the sensor
with DI water after each measure can cause inaccurate pH readings.

Sources of error that can occur in Part B of the experiment can be accumulation of precipitate in
the beaker and sides of the Buchner funnel when filtering the Cr(acac)3 complex.

The improvements that can be made to this experiment is having more functional equipment
such as analytical balances and more equipment such as Ph meters to reduce time spent on doing
the experiment.

CONCLUSION: