General introduction of limit test and limit test for chloride.
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Limit test of chloride is based on the reaction of soluble chloride with silver nitrate in presence of dilute nitric acid to form silver chloride, which appears as solid particles (Opalescence) in the solution.
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Limit test of Arsenic
Arsenic is well known under desirable hand harmful due to its toxic nature, it poses the serious health hazard, which is present in medical substance, many qualitative and quantitative test for arsenic known, however Pharmacopoeia method is based on ‘Gutzeit Method’.
Concentration of arsenic beyond 0.01 mg/L in pollutant by the World Health Organization (WHO).
Reasons:
• Stannous chloride is used for complete evolution of arsine.
• Zinc, potassium iodide and stannous chloride is used as a reducing agent.
• Hydrochloride acid is used to make the solution acidic.
• Lead acetate pledger or papers are used to trap any hydrogen sulphide, which may be evolved along with arsine.
Limit test for iron
The limit test for iron involves comparing the color produced by reacting a sample containing iron with thioglycollic acid in an alkaline solution to the color produced by a standard iron solution. Citric acid is added to the sample and standard, followed by thioglycollic acid and ammonia. A purple color will develop if iron is present. The intensity of the color in the sample is compared to the standard, and if the sample's color is less than or equal to the standard, it passes the limit test for iron.
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This document discusses precipitation titration, which involves the formation of an insoluble precipitate during titration. It describes the Mohr, Volhard, and Fajans methods for detecting the endpoint of precipitation titrations using different indicators like chromate, iron, and fluorescein. The Volhard method, which detects the endpoint potentiometrically by titrating excess silver with thiocyanate, is highlighted as being widely used. Limitations and ways to overcome problems of precipitation titration are also outlined.
Non aqueous titration
This document discusses non-aqueous titrations, which are used to analyze organic acids and bases that are insoluble or weakly reactive in water. It describes the principles, reasons for using non-aqueous titrations, common solvents like acetic acid, and provides examples of procedures to titrate drugs like ephedrine hydrochloride and sodium benzoate. The key steps involve dissolving the analyte in a non-aqueous solvent, titrating with an acid or base, and determining the endpoint using an indicator reaction.
Limit test for heavy metals
This document describes 4 methods for performing a limit test for heavy metals according to the Indian Pharmacopoeia. Method A uses hydrogen sulfide to form metal sulfides from heavy metals in an acidic solution. Method B also uses hydrogen sulfide but first chars and digests the sample. Method C uses sodium sulfide to form metal sulfides in an alkaline solution. Method D uses thioacetamide to react with heavy metals in an acidic buffer solution. For each method, the color produced by the test solution is compared to a standard solution and must not be more intense to pass the limit test.
7.limit test for arsenic
This document describes the Gutzeit test for detecting arsenic. The test works by first converting any arsenic in a sample into arsenious acid, then reducing it to arsine gas. Mercuric chloride paper placed in the apparatus will turn yellow if arsine gas is present, indicating the presence of arsenic in the original sample. The document provides details of the test apparatus, reagents used, procedure, and precautions to get accurate results and avoid contamination.
3.limit test for sulphate
This document describes the procedure for performing a limit test for sulphate according to the Indian Pharmacopoeia. A barium sulphate reagent is prepared containing barium chloride, potassium sulphate, alcohol and water. Standard sulphate solutions are also prepared. The test involves adding nitric acid and the reagent to samples and standards, observing any turbidity formed, and comparing the sample to the standard. If the sample turbidity is less than the standard, it passes the limit test, and if greater, it fails the test.
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Limit Test For Sulphates
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Arsenic is well known under desirable hand harmful due to its toxic nature, it poses the serious health hazard, which is present in medical substance, many qualitative and quantitative test for arsenic known, however Pharmacopoeia method is based on ‘Gutzeit Method’.
Concentration of arsenic beyond 0.01 mg/L in pollutant by the World Health Organization (WHO).
Reasons:
• Stannous chloride is used for complete evolution of arsine.
• Zinc, potassium iodide and stannous chloride is used as a reducing agent.
• Hydrochloride acid is used to make the solution acidic.
• Lead acetate pledger or papers are used to trap any hydrogen sulphide, which may be evolved along with arsine.
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The limit test for iron involves comparing the color produced by reacting a sample containing iron with thioglycollic acid in an alkaline solution to the color produced by a standard iron solution. Citric acid is added to the sample and standard, followed by thioglycollic acid and ammonia. A purple color will develop if iron is present. The intensity of the color in the sample is compared to the standard, and if the sample's color is less than or equal to the standard, it passes the limit test for iron.
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This document discusses precipitation titration, which involves the formation of an insoluble precipitate during titration. It describes the Mohr, Volhard, and Fajans methods for detecting the endpoint of precipitation titrations using different indicators like chromate, iron, and fluorescein. The Volhard method, which detects the endpoint potentiometrically by titrating excess silver with thiocyanate, is highlighted as being widely used. Limitations and ways to overcome problems of precipitation titration are also outlined.
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This document discusses non-aqueous titrations, which are used to analyze organic acids and bases that are insoluble or weakly reactive in water. It describes the principles, reasons for using non-aqueous titrations, common solvents like acetic acid, and provides examples of procedures to titrate drugs like ephedrine hydrochloride and sodium benzoate. The key steps involve dissolving the analyte in a non-aqueous solvent, titrating with an acid or base, and determining the endpoint using an indicator reaction.
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This document describes 4 methods for performing a limit test for heavy metals according to the Indian Pharmacopoeia. Method A uses hydrogen sulfide to form metal sulfides from heavy metals in an acidic solution. Method B also uses hydrogen sulfide but first chars and digests the sample. Method C uses sodium sulfide to form metal sulfides in an alkaline solution. Method D uses thioacetamide to react with heavy metals in an acidic buffer solution. For each method, the color produced by the test solution is compared to a standard solution and must not be more intense to pass the limit test.
7.limit test for arsenic
This document describes the Gutzeit test for detecting arsenic. The test works by first converting any arsenic in a sample into arsenious acid, then reducing it to arsine gas. Mercuric chloride paper placed in the apparatus will turn yellow if arsine gas is present, indicating the presence of arsenic in the original sample. The document provides details of the test apparatus, reagents used, procedure, and precautions to get accurate results and avoid contamination.
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This document describes the procedure for performing a limit test for sulphate according to the Indian Pharmacopoeia. A barium sulphate reagent is prepared containing barium chloride, potassium sulphate, alcohol and water. Standard sulphate solutions are also prepared. The test involves adding nitric acid and the reagent to samples and standards, observing any turbidity formed, and comparing the sample to the standard. If the sample turbidity is less than the standard, it passes the limit test, and if greater, it fails the test.
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The document discusses the limit test for chloride. It defines a limit test as a quantitative or semi-quantitative test to identify and control small amounts of impurities likely to be present in a substance. The limit test for chloride determines the allowable limit of chloride in a sample. It involves dissolving the sample and standard sodium chloride solution, adding nitric acid and silver nitrate, and observing any opalescence or turbidity after 3 minutes. The sample passes the limit test for chloride if the opalescence is less than or equal to the standard solution.
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This document discusses pharmaceutical impurities. It defines impurity as unwanted foreign particles other than the active drug. Impurities can come from raw materials, reagents, manufacturing processes, storage conditions, or deliberate adulteration. The types and amounts of impurities depend on factors like purity of starting materials and purification methods. Limit tests are used to detect and limit specific impurities like chlorides, sulphates, and iron according to pharmacopeia limits. The tests use reactions like precipitation or color changes to compare a sample to a standard of a known impurity level. Maintaining low impurity levels is important for safety, efficacy, and stability of pharmaceutical products.
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Learning Objectives
Introduction
Determination of end point
Mohr’s Method
Volhard’s Method
Fajan’s Method
Application
Conclusion
Reference
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more chemistry contents are available
1. pdf file on Termmate: https://www.termmate.com/rabia.aziz
2. YouTube: https://www.youtube.com/channel/UCKxWnNdskGHnZFS0h1QRTEA
3. Facebook: https://web.facebook.com/Chemist.Rabia.Aziz/
4. Blogger: https://chemistry-academy.blogspot.com/
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4) Neutralization curves for different types of acid-base titrations and the pH at equivalence points.
5) Choice of indicators for different titrations and mixed indicators.
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it will be having the limit test for chloride procedure as per Indian pharmacopoeia and practical hints
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The document discusses several limit tests used to check for impurities in samples according to the Indian Pharmacopoeia, including tests for chloride, sulphate, iron, arsenic, heavy metals, and lead. The limit tests involve comparing the visible reaction of the sample to a standard solution to determine if the level of impurity exceeds the limit. The reactions form precipitates or complexes that can be observed and compared between the sample and standard.
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Sources of impurities
This document discusses pharmaceutical impurities. It defines impurity as unwanted foreign particles other than the active drug. Impurities can come from raw materials, reagents, manufacturing processes, storage conditions, or deliberate adulteration. The types and amounts of impurities depend on factors like purity of starting materials and purification methods. Limit tests are used to detect and limit specific impurities like chlorides, sulphates, and iron according to pharmacopeia limits. The tests use reactions like precipitation or color changes to compare a sample to a standard of a known impurity level. Maintaining low impurity levels is important for safety, efficacy, and stability of pharmaceutical products.
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The document provides information about diazotization titrations. It discusses the principle, theory, procedure, end point detection, factors affecting, applications, and advantages/disadvantages of diazotization titrations. The key points are:
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- The end point is detected using an external indicator like starch iodide paper or electrochemically.
- Factors like acid concentration, temperature, and reaction time must be controlled.
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This document describes the limit test for sulfate. The test is based on the reaction between barium chloride and soluble sulfates in the presence of hydrochloric acid. This results in the precipitation of barium sulfate. The turbidity produced by the test solution is compared to that of a standard sulfate solution. If the turbidity of the test solution is less than the standard, then the sample passes the limit test for sulfate.
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Learning Objectives
Introduction
Determination of end point
Mohr’s Method
Volhard’s Method
Fajan’s Method
Application
Conclusion
Reference
Complexometric Titration
more chemistry contents are available
1. pdf file on Termmate: https://www.termmate.com/rabia.aziz
2. YouTube: https://www.youtube.com/channel/UCKxWnNdskGHnZFS0h1QRTEA
3. Facebook: https://web.facebook.com/Chemist.Rabia.Aziz/
4. Blogger: https://chemistry-academy.blogspot.com/
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This document describes the limit test for iron according to the Indian Pharmacopoeia. The test involves comparing the color produced by reacting a sample with thioglycolic acid in an ammonical citrate buffer to the color produced by a standard iron solution under the same conditions. If the color produced by the sample is less than the standard, it passes the limit test for iron. If the color is greater than the standard, it fails the limit test. The test is sensitive and uses citric acid to eliminate interference from other metal cations.
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This document discusses the theory of acid-base indicators used in titration reactions. It explains that indicators change color within a certain pH range, allowing determination of the endpoint. Two theories are presented: Ostwald's theory states that color change is due to ionization of the indicator, while quinonoid theory proposes the indicator exists in two tautomeric forms in equilibrium, with different colors. Common indicators like phenolphthalein and methyl orange are discussed in the context of the two theories.
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This document provides an overview of acid-base titration and volumetric analysis. It defines key terms like titration, indicator, equivalence point, and standardization. It describes different types of titrations including direct, indirect, and back titration. Acid-base concepts are explained based on Arrhenius, Bronsted-Lowry, and Lewis theories. The document also discusses the ionic product of water, common ion effect, classification of indicators, and theories of indicators including Ostwald and chromophore theories.
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This document discusses acid-base theories and titration. It covers:
1) Arrhenius, Bronsted-Lowry, and Lewis acid-base theories.
2) Types of acids and bases as strong or weak.
3) The law of mass action and dissociation constants.
4) Neutralization curves for different types of acid-base titrations and the pH at equivalence points.
5) Choice of indicators for different titrations and mixed indicators.
Non aqueous titrations
This document discusses non-aqueous titrations, including the types of solvents used, endpoint detection methods, and applications. It covers protogenic solvents like acetic acid that can act as both acids and bases, protophilic solvents with high proton affinity, and aprotic solvents like benzene that are inert. Common indicators and titrants used include crystal violet, perchloric acid, and sodium acetate. The document provides examples of using non-aqueous titrations to assay substances like sodium acetate and norfloxacin tablets that are insoluble or reactive in water.
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This document discusses limit tests, which are used to identify and quantify small amounts of impurities in substances. It focuses on the chloride limit test, which uses a reaction between silver nitrate and chlorides to form an insoluble precipitate of silver chloride. The test involves dissolving the sample and adding silver nitrate and nitric acid, then comparing the level of opalescence to that of a standard solution containing a known amount of chloride. The level of opalescence depends on the amount of chloride present, allowing the test to quantify chloride impurities in inorganic substances.
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Limit tests are quantitative or semi-quantitative tests designed to identify and control small quantities of impurity, which are likely to be present in the substance. The quantity of any one impurity in an official substance is often small, and consequently the visible reaction response to any test for that impurity is also small. The design of individual tests is therefore important if errors are to be avoided in the hands of different operators.
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Limit test (B.Pharm, PCI Syllabus)
Introduction to limit tests, the limit test is a semiquantitative test, limit test for chlorides, limit test for sulfates, limit test for iron, limit test for heavy metals, limit test for arsenic, Gutzeit apparatus
Limit test sulphate
Limit test of sulphate is based on the reaction of soluble sulphate with barium chloride in presence of dilute hydrochloric acid to form barium sulphate which appears as solid particles (turbidity) in the solution.
Limit test sudip modh
Form a red-violet complex
The intensity of the color produced is compared with that obtained by treating a known quantity of iron under the same conditions.
Reagents:
Ammonium thioglycolate solution: Dissolve 20 g of thioglycolic acid and 20 g of ammonium chloride in water and dilute to 100 ml.
Standard iron solution: Dissolve 0.1 g of iron wire in dilute hydrochloric acid, add 5 ml of hydrochloric acid and dilute to 1000 ml with water. 1 ml contains 10 μg of iron.
Procedure:
Pip
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General introduction of limit test and limit test for chloride.
- 1. LIMIT TEST Presented by MahimaDubey(Assistant Professor) Sagar Institute of Pharmaceutical sciences
- 2. TEST FOR PURITY Pharmacopoeia prescribes the “Test for purity” for pharmaceutical substances to check their freedom from undesirable impurities. Pharmacopoeia will decide and fix the limit of tolerance for these impurities. For certain common impurities for which pharmacopoeia prescribes the test of purity are: Colour, odour, taste Physicochemical constants (Iodine value, saponification value, melting point, refractive index etc.) Acidity, alkalinity, pH Humidity (Estimation of moisture) Cations and anions Ash Arsenic or lead Loss on drying Loss on ignition
- 3. LIMIT TESTS: Tests being used to identify the impurity. Tests being used to control the impurity. Definition: Limit tests are quantitative or semi quantitative test designed to identify and control small quantities of impurities which are likely to be present in the substances.
- 4. LIMIT TEST FOR CHLORIDE Principle: Limit test of chloride is based on the reaction of soluble chloride with silver nitrate in presence of dilute nitric acid to form silver chloride, which appears as solid particles (Opalescence) in the solution. Cl- + Soluble chloride present as impurity The silver chloride produced in the presence of dilute Nitric acid makes the test solution turbid, the extent of turbidity depending upon the amount of Chloride present in the substance is compared with the standard opalescence produced by the addition of Silver nitrate to a standard solution having a known amount of chloride and the same volume of dilute nitric acid as used in the test solution. AgNO3 -------------------------- AgCl + NO3 - silver chloride
- 6. Test sample Standard compound Specific weight of compound is dissolved in water or solution is prepared as directed in the pharmacopoeia and transferred in Nessler cylinder Take 1 ml of 0.05845 % W/V solution of sodium chloride in Nessler cylinder Add 1 ml of nitric acid Add 1 ml of nitric acid Dilute to 50 ml in Nessler cylinder Dilute to 50 ml in Nessler cylinder Add 1 ml of AgNO3 solution Add 1 ml of AgNO3 solution Keep aside for 5 min Keep aside for 5 min Observe the Opalescence/Turbidity Observe the Opalescence/Turbidity
- 7. Observation: THE OPALESCENCE PRODUCE IN SAMPLE SOLUTION SHOULD NOT BE GREATER THAN STANDARD SOLUTION. IF OPALESCENCE PRODUCES IN SAMPLE SOLUTION IS LESS THAN THE STANDARD SOLUTION, THE SAMPLE WILL PASS THE LIMIT TEST OF CHLORIDE AND VISAVERSA. Reasons: Nitric acid is added in the limit test of chloride to make solution acidic and helps silver chloride precipitate to make solution turbid at the end of process as Dilute HNO3 is insoluble inAgCl.