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Limit Test For Arsenic

The Limit Test for Arsenic is a qualitative analysis method used to detect arsenic impurities in pharmaceuticals, following guidelines from major pharmacopoeias. It involves converting arsenic into arsine gas, which reacts with mercuric chloride paper to produce a color stain that is compared to a standard. The test ensures drug safety by limiting arsenic contamination to permissible levels of 1 ppm for IP and BP, and 2 ppm for USP.

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340 views2 pages

Limit Test For Arsenic

The Limit Test for Arsenic is a qualitative analysis method used to detect arsenic impurities in pharmaceuticals, following guidelines from major pharmacopoeias. It involves converting arsenic into arsine gas, which reacts with mercuric chloride paper to produce a color stain that is compared to a standard. The test ensures drug safety by limiting arsenic contamination to permissible levels of 1 ppm for IP and BP, and 2 ppm for USP.

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liveinsure108
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Limit Test for Arsenic – Study Material

1. Introduction

 The Limit Test for Arsenic is a qualitative test used in pharmaceutical analysis to
detect and limit the presence of arsenic impurities in drugs and raw materials.
 It follows the guidelines of the Indian Pharmacopoeia (IP), British Pharmacopoeia
(BP), and United States Pharmacopoeia (USP).

2. Principle of the Test

 The test is based on the Gutzeit method, where arsenic, if present, is converted into
arsine gas (AsH₃) using zinc (Zn) and acid (H₂SO₄ or HCl).
 The arsine gas reacts with mercuric chloride (HgCl₂) paper, forming a yellow-brown
stain, the intensity of which is compared to a standard stain.

3. Chemical Reactions Involved

1. Reduction of Arsenic Compound:

As₂O₃ + 6Zn + 12HCl → 2AsH₃ + 6ZnCl₂ + 3H₂O

(Arsenious oxide reacts with zinc and hydrochloric acid to form arsine gas.)

2. Reaction with Mercuric Chloride Paper:

AsH₃ + HgCl₂ → As(HgCl)₃ (yellow-brown stain)

(Arsine reacts with mercuric chloride, forming a yellow to brown stain.)

4. Apparatus Required

 Gutzeit Apparatus (consists of a wide-mouthed bottle with a perforated stopper and a


mercuric chloride paper)
 Nessler Cylinders
 Standard Arsenic Solution
 Comparative Scale for Color Intensity Measurement

5. Reagents Used

1. Arsenic-Free Zinc (Zn) – Reducing agent


2. Hydrochloric Acid (HCl) or Sulfuric Acid (H₂SO₄) – Acid medium for reduction
3. Stannous Chloride (SnCl₂) – Enhances reaction efficiency
4. Lead Acetate Cotton Plug – Absorbs interfering sulfides
5. Mercuric Chloride (HgCl₂) Paper – Detects arsine gas by color change
6. Procedure

1. Preparation of the Sample Solution


o Dissolve the sample in acidic medium (HCl or H₂SO₄).
o Add zinc granules and stannous chloride.
o The reaction produces arsine gas (AsH₃).
2. Collection of Arsine Gas
o The gas passes through lead acetate cotton (removes interfering sulfur
compounds).
o It then reacts with mercuric chloride paper.
3. Observation & Comparison
o Compare the color intensity of the stain on the paper with a standard arsenic
stain.
o If the sample stain is lighter than the standard, it passes the test.
o If the sample stain is darker, it fails the test (arsenic content exceeds the limit).

7. Interpretation of Results

 Pass: If the sample stain is not darker than the standard stain.
 Fail: If the sample stain is darker than the standard, indicating excess arsenic.

8. Permissible Limits of Arsenic

Pharmacopoeia Permissible Limit


Indian Pharmacopoeia (IP) 1 ppm (0.0001%)
British Pharmacopoeia (BP) 1 ppm
United States Pharmacopoeia (USP) 2 ppm

9. Applications

 Ensures drug safety by limiting arsenic contamination.


 Used in the quality control of pharmaceutical raw materials and finished products.
 Prevents toxicity due to arsenic, which can cause carcinogenic and neurological
disorders.

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