Ferric Chloride - Pyridine Test:The ferric chloride test is used to determine the presence or absence of phenols in a given sample. Enols give positive results as well. The bromine test is useful to confirm the result, although modern spectroscopic techniques (e.g. NMR and IR spectroscopy) are far superior in determining the identity of the unknown. The quantity of total phenols may be spectroscopically determined by the Folin-Ciocalteau assay.
TechniqueThe sample is dissolved in water, or a mixture of water and ethanol, and a few drops of dilute ferric chloride solution is added. The formation of a red, blue, green, or purple coloration indicates the presence of phenols. Where the sample is insoluble in water, it may be dissolved in dichloromethane with a small amount of pyridine.
Chemistry:
Phenols form a complex with Fe(III), which is intensely colored. This is the basis for the test.
Ferric Chloride test for Phenols.: Just as enols can form colored complexes with ferric ion, phenolate ions can as well. Therefore, this test is designed to convert the weakly acidic phenols to their conjugate base which can then complex with ferric ion. If the phenol is water soluble, add a few drops of 2.5% aqueous ferric chloride solution to a 3% aqueous solution of the phenol. A deep red, green, or blue color is positive. If the phenol is not water soluble, dissolve 20 mg of the solid (or 1 drop of the liquid) in 1 mL of methylene chloride and add 1 drop of pyridine. Add 3 drops of 1% ferric chloride in methylene chloride. An intense color is a positive test. Use phenol as a known. Not all phenols will give a positive test.
Procedure:In hood: Add 4 or 5 drops or 30 - 50 mg of unknown to 2 mL of pure chloroform in a clean, dry test tube. Stir the solution. If the unknown does not dissolve, even partially, add 2 - 3 mL more chloroform and warm gently. Cool to 25oC and add 2 drops of 1% solution of anhydrous ferric chloride in chlorofrom followed by 3 drops of pyridine. Shake the test tube and note the color produced immediately.
Positive Test:The appearance of blue, violet, purple, green, or red-brown color is a positive test.
Complications:Not all phenols or enols give positive results
Most oximes, hydroxamic acids, and sulfinic acids give a positive
Iron (III) Chloride Test for Water-Soluble Phenol Standard
Phenol
Procedure (for water-soluble phenols)
The iron (III) chloride test for phenols is not completely reliable for acidic phenols, but can be administered by dissolving 15 mg of the unknown compound in 0.5 mL of water or water-alcohol mixture and add 1 to 2 drops of 1% aqueous iron (III) chloride solution.
Positive TestA red, blue, green, or purple color is a positive test.
Cleaning upSince the quantity of material is extremely small, the test solution can be diluted with water and flushed down the drain.
Iron(III) Chloride - Pyridine Test for Water-Insoluble PhenolsStandard
Phenol
Procedure (for water-insoluble phenols or less reactive phenols)
A more sensitive test for phenols consists of dissolving or suspending 15 mg of the unknown in 0.5 mL of methylene chloride and adding 3-5 drops of a 1% solution ferric chloride in methylene chloride. Add a drop of pyridine and stir.
Positive Test (b)Addition of pyridine and stirring will produce a color if phenols or enols are present.
Why phenols give ferric chloride test?We use Ferric Chloride (FeCl3) in the lab to test for the presence (or in some case absence) of phenols, although some enols will also yield positive results. The OH (hydroxy group) which is attached directly to an aromatic nucleus (Benzene, for example) is detected by the Ferric chloride. It is important to note that alcohols do not undergo the reaction. Phenols will typically yield dramatic purple,blue,red or green color as an indication of a positive test. FeCl3 will also indicate the presence of aliphatic acids (that is, non-aromatic organic acids, such as Acetic acid) turning the solution a yellow color. Aromatic acids will test as a beige-tan color. Enols will also show a characteristic yellow color. It is also important to understand that not all phenols will test positively in the presence of the FeCl3 reagent. A good example of this is in highly hindered phenols which do not yield positive tests. However, a negative test is not completely conclusive, so other tests can be preformed to verify the absence of a phenol (such as NMR and IR spectroscopy)
We use Ferric Chloride (FeCl3) in the lab to test for the presence (or in some case absence) of phenols, although some enols will also yield positive results. The OH (hydroxy group) which is attached directly to an aromatic nucleus (Benzene, for example) is detected by the Ferric chloride. It is important to note that alcohols do not undergo the reaction. Phenols will typically yield dramatic purple,blue,red or green color as an indication of a positive test. FeCl3 will also indicate the presence of aliphatic acids (that is, non-aromatic organic acids, such as Acetic acid) turning the solution a yellow color. Aromatic acids will test as a beige-tan color. Enols will also show a characteristic yellow color. It is also important to understand that not all phenols will test positively in the presence of the FeCl3 reagent. A good example of this is in highly hindered phenols which do not yield positive tests. However, a negative test is not completely conclusive, so other tests can be preformed to verify the absence of a phenol (such as NMR and IR spectroscopy)
Material Safety Data SheetFerric Chloride TS MSDSSection 1: Chemical Product and Company Identification
Product Name: Ferric Chloride TS
Catalog Codes: SLF1045
CAS#: Mixture.
RTECS: Not applicable.
TSCA: TSCA 8(b) inventory: Water; Ferric chloride
hexahydrate
CI#: Not available.
Synonym: Ferric Chloride Test Solution
Chemical Name: Not applicable.
Chemical Formula: Not applicable.
Contact Information:
Sciencelab.com, Inc.
14025 Smith Rd.
Houston, Texas 77396
US Sales: 1-800-901-7247
International Sales: 1-281-441-4400
Order Online: ScienceLab.com
CHEMTREC (24HR Emergency Telephone), call:
1-800-424-9300
International CHEMTREC, call: 1-703-527-3887
For non-emergency assistance, call: 1-281-441-4400
Section 2: Composition and Information on Ingredients
Composition:
Name CAS # % by Weight
Water 7732-18-5 91
Ferric chloride hexahydrate 10025-77-1 9
Toxicological Data on Ingredients: Ferric chloride hexahydrate LD50: Not available. LC50: Not available.
Section 3: Hazards Identification
Potential Acute Health Effects:
Very hazardous in case of skin contact (irritant), of eye contact (irritant), of ingestion, . Hazardous in case of skin
contact (corrosive, permeator), of eye contact (corrosive). Slightly hazardous in case of inhalation (lung
sensitizer). Non-corrosive for lungs. Liquid or spray mist may produce tissue damage particularly on mucous
membranes of eyes, mouth and respiratory tract. Skin contact may produce burns. Inhalation of the spray mist
may produce severe irritation of respiratory tract, characterized by coughing, choking, or shortness of breath.
Severe over-exposure can result in death. Inflammation of the eye is characterized by redness, watering, and
itching. Skin inflammation is characterized by itching, scaling, reddening, or, occasionally, blistering.
Potential Chronic Health Effects:
CARCINOGENIC EFFECTS: Not available.
MUTAGENIC EFFECTS: Mutagenic for mammalian somatic cells. [Ferric chloride hexahydrate].
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TERATOGENIC EFFECTS: Not available.
DEVELOPMENTAL TOXICITY: Not available.
The substance may be toxic to kidneys, liver, spleen, cardiovascular system, central nervous system (CNS).
Repeated or prolonged exposure to the substance can produce target organs damage. Repeated or prolonged
contact with spray mist may produce chronic eye irritation and severe skin irritation. Repeated or prolonged
exposure to spray mist may produce respiratory tract irritation leading to frequent attacks of bronchial infection.
Repeated exposure to a highly toxic material may produce general deterioration of health by an accumulation in
one or many human organs.
Section 4: First Aid Measures
Eye Contact:
Check for and remove any contact lenses. In case of contact, immediately flush eyes with plenty of water for at
least 15 minutes. Cold water may be used. Get medical attention immediately.
Skin Contact:
In case of contact, immediately flush skin with plenty of water for at least 15 minutes while removing contaminated
clothing and shoes. Cover the irritated skin with an emollient. Cold water may be used.Wash clothing before
reuse. Thoroughly clean shoes before reuse. Get medical attention immediately.
Serious Skin Contact:
Wash with a disinfectant soap and cover the contaminated skin with an anti-bacterial cream. Seek immediate
medical attention.
Inhalation:
If inhaled, remove to fresh air. If not breathing, give artificial respiration. If breathing is difficult, give oxygen. Get
medical attention immediately.
Serious Inhalation:
Evacuate the victim to a safe area as soon as possible. Loosen tight clothing such as a collar, tie, belt or
waistband. If breathing is difficult, administer oxygen. If the victim is not breathing, perform mouth-to-mouth
resuscitation. Seek medical attention.
Ingestion:
If swallowed, do not induce vomiting unless directed to do so by medical personnel. Never give anything by
mouth to an unconscious person. Loosen tight clothing such as a collar, tie, belt or waistband. Get medical
attention immediately.
Serious Ingestion: Not available.
Section 5: Fire and Explosion Data
Flammability of the Product: Non-flammable.
Auto-Ignition Temperature: Not applicable.
Flash Points: Not applicable.
Flammable Limits: Not applicable.
Products of Combustion: Not available.
Fire Hazards in Presence of Various Substances: Not applicable.
Explosion Hazards in Presence of Various Substances: Non-explosive in presence of open flames and sparks, of shocks.
Fire Fighting Media and Instructions: Not applicable.
Special Remarks on Fire Hazards: Not available.
p. 2
Special Remarks on Explosion Hazards: Not available.
Section 6: Accidental Release Measures
Small Spill:
Dilute with water and mop up, or absorb with an inert dry material and place in an appropriate waste disposal
container.
Large Spill:
Corrosive liquid. Poisonous liquid.
Stop leak if without risk. Absorb with DRY earth, sand or other non-combustible material. Do not get water inside
container. Do not touch spilled material. Use water spray curtain to divert vapor drift. Use water spray to reduce
vapors. Prevent entry into sewers, basements or confined areas; dike if needed. Call for assistance on disposal.
Be careful that the product is not present at a concentration level above TLV. Check TLV on the MSDS and with
local authorities.
Section 7: Handling and Storage
Precautions:
Keep locked up.. Keep container dry. Do not ingest. Do not breathe gas/fumes/ vapor/spray. Never add water
to this product. In case of insufficient ventilation, wear suitable respiratory equipment. If ingested, seek medical
advice immediately and show the container or the label. Avoid contact with skin and eyes.
Storage: Keep container tightly closed. Keep container in a cool, well-ventilated area. Do not store above 24°C (75.2°F).
Section 8: Exposure Controls/Personal Protection
Engineering Controls:
Provide exhaust ventilation or other engineering controls to keep the airborne concentrations of vapors below their
respective threshold limit value.
Personal Protection:
Face shield. Full suit. Vapor respirator. Be sure to use an approved/certified respirator or equivalent. Gloves.
Boots.
Personal Protection in Case of a Large Spill:
Splash goggles. Full suit. Vapor respirator. Boots. Gloves. A self contained breathing apparatus should be
used to avoid inhalation of the product. Suggested protective clothing might not be sufficient; consult a specialist
BEFORE handling this product.
Exposure Limits:
Ferric chloride hexahydrate
TWA: 1 (mg/m3) from ACGIH (TLV) [United States]
TWA: 1 (mg/m3) from NIOSH
Consult local authorities for acceptable exposure limits.
Section 9: Physical and Chemical Properties
Physical state and appearance: Liquid.
Odor: Not available.
Taste: Not available.
Molecular Weight: Not applicable.
Color: Not available.
p. 3
pH (1% soln/water): Neutral.
Boiling Point: The lowest known value is 100°C (212°F) (Water).
Melting Point: Not available.
Critical Temperature: Not available.
Specific Gravity: Weighted average: 1.04 (Water = 1)
Vapor Pressure: The highest known value is 2.3 kPa (@ 20°C) (Water).
Vapor Density: The highest known value is 0.62 (Air = 1) (Water).
Volatility: Not available.
Odor Threshold: Not available.
Water/Oil Dist. Coeff.: Not available.
Ionicity (in Water): Not available.
Dispersion Properties: See solubility in water.
Solubility: Easily soluble in cold water, hot water.
Section 10: Stability and Reactivity Data
Stability: The product is stable.
Instability Temperature: Not available.
Conditions of Instability: Incompatible materials
Incompatibility with various substances: Not available.
Corrosivity: Non-corrosive in presence of glass.
Special Remarks on Reactivity: Hygroscopic (Ferric chloride hexahydrate)
Special Remarks on Corrosivity: Not available.
Polymerization: Will not occur.
Section 11: Toxicological Information
Routes of Entry: Absorbed through skin. Dermal contact. Eye contact.
Toxicity to Animals:
LD50: Not available.
LC50: Not available.
Chronic Effects on Humans:
MUTAGENIC EFFECTS: Mutagenic for mammalian somatic cells. [Ferric chloride hexahydrate].
Contains material which may cause damage to the following organs: kidneys, liver, spleen, cardiovascular system,
, central nervous system (CNS).
Other Toxic Effects on Humans:
Very hazardous in case of skin contact (irritant), of ingestion, .
p. 4
Hazardous in case of skin contact (corrosive, permeator), of eye contact (corrosive).
Slightly hazardous in case of inhalation (lung sensitizer, lung corrosive).
Special Remarks on Toxicity to Animals: LDL [Rat] - Route: Oral; Dose: 900 mg/kg (Ferric chloride hexahydrate)
Special Remarks on Chronic Effects on Humans: May affect genetic material (mutagen) (Ferric chloride hexahydrate)
Special Remarks on other Toxic Effects on Humans:
Acute Potential Health Effects:
Skin: Causes irritation and burns of the skin.
Eyes: Causes eye irritation and burns. Higher exposures may lead to corneal or conjunctival ulceration.
Ingestion: Harmful if swallowed. Causes irritation of the gastrointestinal (digestive) tract with nausea, vomiting,
diarrhea and hemorrage and possible burns. May cause severe and permanent damage to the digestive tract.
Delayed effects may include cardiovascular disturbances, liver/kidney damage, cerebral coma and possible death.
Inhalation: Causes irritation of the respiratory tract with possible burns.
Chronic Potential Health Effects:
May affect genetic material
Ingestion: May affect liver, spleen Kidneys, ureter, bladder), central nervous system, and cardiovascular system.
Section 12: Ecological Information
Ecotoxicity: Not available.
BOD5 and COD: Not available.
Products of Biodegradation:
Possibly hazardous short term degradation products are not likely. However, long term degradation products may
arise.
Toxicity of the Products of Biodegradation: The products of degradation are less toxic than the product itself.
Special Remarks on the Products of Biodegradation: Not available.
Section 13: Disposal Considerations
Waste Disposal:
Waste must be disposed of in accordance with federal, state and local environmental
control regulations.
Section 14: Transport Information
DOT Classification: Class 8: Corrosive material
Identification: : Ferric Chloride Solution (Ferric chloride hexahydrate) UNNA: 2582 PG: III
Special Provisions for Transport: Not available.
Section 15: Other Regulatory Information
Federal and State Regulations:
Pennsylvania RTK: Ferric chloride hexahydrate
Minnesota: Ferric chloride hexahydrate
TSCA 8(b) inventory: Water; Ferric chloride hexahydrate
Other Regulations: OSHA: Hazardous by definition of Hazard Communication Standard (29 CFR 1910.1200).
Other Classifications:
p. 5
WHMIS (Canada):
CLASS D-2B: Material causing other toxic effects (TOXIC).
CLASS E: Corrosive liquid.
DSCL (EEC):
R25- Toxic if swallowed.
R36/38- Irritating to eyes and skin.
S1/2- Keep locked up and out of the reach of
children.
S45- In case of accident or if you feel unwell,
seek medical advice immediately (show the
label where possible).
S46- If swallowed, seek medical advice
immediately and show this container or label.
HMIS (U.S.A.):
Health Hazard: 3
Fire Hazard: 0
Reactivity: 0
Personal Protection:
National Fire Protection Association (U.S.A.):
Health: 2
Flammability: 0
Reactivity: 0
Specific hazard:
Protective Equipment:
Gloves.
Full suit.
Vapor respirator. Be sure to use an
approved/certified respirator or
equivalent. Wear appropriate respirator
when ventilation is inadequate.
Face shield.
Section 16: Other Information
References: Not available.
Other Special Considerations: Not available.
Created: 10/10/2005 10:12 AM
Last Updated: 11/06/2008 12:00 PM
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Safety data for pyridine: GeneralSynonyms: azabenzene, pyridin
Molecular formula: C5H5N
CAS No: 110-86-1
EINECS No: 203-809-9
Annex I Index No: 613-002-00-7
Physical data
Appearance: colourless liquid with a very unpleasant odour
Melting point: -42 C
Boiling point: 115 C
Vapour density: 2.7 (air = 1)
Vapour pressure: 16 mm Hg at 20 C
Density (g cm-3):
Flash point: 17 C (closed cup)
Explosion limits: 1.8 % - 12.4 %
Autoignition temperature:
Water solubility:
StabilityStable. Flammable. Incompatible with strong oxidizing agents, strong acids.
ToxicologyHarmful by ingestion, inhalation and if absorbed through skin. May affect fertility. May cause irreversible effects. Severe eye and skin irritant - may cause burns. Long-term exposure may cause liver, kidney or CNS damage. Typical STEL 10 ppm. Typical PEL 15 ppm.
Toxicity data (The meaning of any toxicological abbreviations which appear in this section is given here.)
ORL-RAT LD50 891 mg kg-1
IPR-RAT LD50 866 mg kg-1
SCU-RAT LD50 1000 mg kg-1
SKN-RBT LD50 1121 mg kg-1
Risk phrases
(The meaning of any risk phrases which appear in this section is given here.)
R11 R20 R21 R22.
Transport information(The meaning of any UN hazard codes which appear in this section is given here.)
UN No 1282. Hazard class 3. Packing group II.
Personal protection
Safety glasses, gloves, good ventilation.
Refrence:
1.www.chemicalinfo.com
2. http://msds.chem.ox.ac.uk
3. http://www.inchem.com.ph
4. http:www.hvchemical.com
5. http://en.wikipedia.org
6. http://www.osha.gov
7. http://chemfinder.cumbridgesoft.com
8. http://www.sciencelab.com
9. www.wellesley.edu/.../phenol_amine_nitro.html
