Toxicology Practicum: Detailed Guide to Chemical Reactions


Toxicology Practicum: Detailed Guide to Chemical Reactions

Toxicology Practicum: Detailed Guide to Chemical Reactions

I. Formaldehyde (HCHO)

1. Isolation of HCHO:

  • Method: Steam distillation.
  • Role of H3PO4: Converts HCHO from its bound form to its free form, making the distillation process more efficient.

2. Qualitative Analysis of HCHO:

  • Reaction with chromotropic acid:
  • Detection limit: 0.5mg/kg solid sample.
  • Color: Violet.
  • Reaction with 1% Phloroglucinol/alkali:
  • Color: Red.
  • Reaction with phenol/acid:
  • Phenomenon: Pink color appears at the interface.

3. Semi-quantitative Analysis of HCHO:

  • Reagent: Chromotropic acid.
  • Difference between test tubes: Concentration of HCHO.

II. Hydrogen Cyanide (HCN)

1. Qualitative Analysis of HCN:

  • Guignard’s reaction:
  • Reagent: Picric acid/alkali.
  • Product: Isopurpurin, orange-yellow color.
  • Grignard’s reaction:
  • Components of test paper: Picric acid, Na2CO3.
  • Phenomenon: Picric acid-soaked paper changes from yellow => orange-yellow => brown.
  • Role of HCl: Added to allow HCN to evaporate, avoiding the alkaline environment from affecting the paper.
  • Prussian blue reaction:
  • Precipitate: Fe II and Fe III sulfate/alkali.
  • Prussian blue: The precipitate turns blue when acidified.
  • Alkalizing the sample solution: NaOH 50% – Converts cyanide to ionized form (CN-).
  • Maximum duration for determination: 48 hours.

2. Quantitative Analysis of HCN:

  • Method: Argentometry.

III. Phenol

1. Isolation of Phenol:

  • Method: Steam distillation.
  • Detection of phenol in distillate: p-nitroaniline diazotization/alkali. Measure the absorbance of the formed product and compare it to the standard solution.

2. Phenol in urine:

  • Form of existence: Phenyl sulfonic acid.
  • Treatment: Hydrolyze with H2SO4 => free phenol.

3. Quantitative Analysis of Phenol:

  • Method: Iodometry (determining the amount of excess bromine after reaction with phenol).
  • Role of chloroform: Dissolves the tribromophenol precipitate.
  • Form of bromine: Bromide-bromate solution.

IV. Ethanol (C2H5OH)

1. Qualitative Analysis of Ethanol:

  • Reaction with Sulphomolybdic Acid:
  • Color: Deep blue.
  • Reaction to form iodoform:
  • Sensitivity: 0.04mg/mL.
  • Environment: Alkali (NaOH or K2CO3 10%).
  • Temperature: Not exceeding 50 degrees Celsius.
  • I2: 1% iodine solution.
  • Reaction to form ethyl acetate:
  • Sensitivity: 15-20 mg/mL.
  • Identification: Characteristic smell of the reaction between ethanol and acetic acid catalyzed by H2SO4 acid.

2. Quantitative Analysis of Ethanol:

  • Nicloux’s method:
  • Oxidizing agent: Potassium bichromate/concentrated sulfuric acid.
  • Color change: Blue (excess ethanol) => green (excess potassium bichromate).
  • Role of picric acid: Precipitates protein.
  • Maximum amount of potassium bichromate: 1.1mL.
  • Applicable sample: Fresh samples: blood, brain… not yet decomposed. Add NaF to preserve decomposed blood.

V. Methanol (CH3OH)

1. Qualitative Analysis of Methanol:

  • Schiff’s reagent: Based on the oxidation product, Formaldehyde.
  • Reaction with 1% resorcin:
  • Environment: Alkali.
  • Color: Pink or crimson.
  • Reaction with Schiff’s reagent:
  • Environment: Acid.
  • Color: Blue or blue-violet.
  • Esterification reaction: Add the test solution + 0.03g salicylic acid and 2-3 drops of concentrated H2SO4, heat. If methanol is present, there will be a hot oil smell.

VI. Arsenic (As)

1. Isolation of Arsenic:

  • Inorganicization:
  • Wet inorganicization: sulfo-nitric + H2O2/HClO4.
  • Dry inorganicization: MgO-MgNO3.

2. Qualitative Analysis of Arsenic:

  • Bougault’s reaction:
  • Reagent: H3PO2/HCl.
  • Catalyst: High temperature, an iodine spot.
  • Sensitivity: 10 mcg.
  • Phenomenon: Brown precipitate – As metal.

VII. Bismuth (Bi)

1. Qualitative Analysis of Bismuth:

  • Leger’s reaction:
  • Environment: Weak acid.
  • Phenomenon: Red-orange precipitate of iodobismuthite quinine soluble in organic solvents.

VIII. Chromium (Cr)

1. Qualitative Analysis of Chromium:

  • Cazeneuve’s reaction:
  • Reagent: 1% Diphenylcarbazide/alcohol.
  • Phenomenon: Pink-purple solution, unstable.

IX. Manganese (Mn)

1. Qualitative Analysis of Manganese:

  • Marshall’s reaction:
  • Phenomenon: The solution appears pink-purple.

X. Lead (Pb)

1. Qualitative Analysis of Lead:

  • Reaction with Dithizone:
  • Phenomenon: The solution turns purple-pink.
  • Reaction with KI:
  • Phenomenon: PbI2, a yellow precipitate, is formed.
  • Reaction with K2Cr2O7:
  • Phenomenon: PbCrO4 precipitate is formed, which has a yellow color.

XI. Mercury (Hg)

1. Isolation of Mercury:

  • Method: Inorganicization with sulfo-nitric.

2. Quantitative Analysis of Mercury:

  • Method: Formation of the Cu2I2 complex. Compare to the standard solution with a known concentration.

XII. General Notes:

  • Sensitivity of the reaction: Note the sensitivity of each reaction to determine the minimum amount of toxic substance that can be detected.
  • Environmental conditions: Chemical reactions are often dependent on the environment (acid, alkali, temperature…). Follow the instructions carefully so that the reaction takes place effectively.
  • Chemical safety: Always use safe protective measures when working with hazardous chemicals.
  • Practical techniques: The practical operations need to be accurate and careful to avoid errors.

Note: This document provides basic information on chemical reactions in toxicology practicum. To understand more about each reaction, please refer to other professional documents.



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