The document describes three methods (A, B, and C) for performing a limit test for heavy metals according to the Indian Pharmacopoeia. The test involves reacting heavy metal ions in the sample with hydrogen sulfide or sodium sulfide to form colored heavy metal sulfides. The color produced is compared to that of a standard lead solution to determine whether the sample meets the limit of 20 parts per million for heavy metals. Method A is for clear, colorless solutions, Method B is for solutions that are not clear or colorless, and Method C uses sodium hydroxide for solutions that give a clear colorless solution in sodium hydroxide.
Limit tests, Introduction, Definition,
Limit Test For Chlorides
Limit Test For Sulphates
Limit Test For Iron
Limit Test For Lead
Limit Test For Arsenic
Limit tests, Introduction, Definition,
Limit Test For Chlorides
Limit Test For Sulphates
Limit Test For Iron
Limit Test For Lead
Limit Test For 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.
Neutralization curves in acid base analytical titrations, indicators.nehla313
Neutralization curves in acid base analytical titrations, indicators,
strong acid strong base
weak acid strong bse
strong acid weak base
weak acid and weak base
this presentation on limit test for sulphates is very helpful for the diploma and bachelor pharmacy students. this includes principle procedure reaction and observation of limit test.
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.
General introduction of limit test and limit test for chloride.Mahima Dubey
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.
The general principle of Agulhon's test is to convert butyric
acid into its copper salt and to extract this with ether. The
copper butyrate imparts a blue color to the ether layer. The
degree of color varies with the concentration of butyrate, the
acidity of the solution and the quantity of copper salt used.
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.
Neutralization curves in acid base analytical titrations, indicators.nehla313
Neutralization curves in acid base analytical titrations, indicators,
strong acid strong base
weak acid strong bse
strong acid weak base
weak acid and weak base
this presentation on limit test for sulphates is very helpful for the diploma and bachelor pharmacy students. this includes principle procedure reaction and observation of limit test.
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.
General introduction of limit test and limit test for chloride.Mahima Dubey
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.
The general principle of Agulhon's test is to convert butyric
acid into its copper salt and to extract this with ether. The
copper butyrate imparts a blue color to the ether layer. The
degree of color varies with the concentration of butyrate, the
acidity of the solution and the quantity of copper salt used.
Introduction
Limit Test for Chlorides
Limit Test for sulphates
Limit Test for Heavy metals
Limit Test for Iron
Limit Test for Arsenic
Limit Test for Lead
Reference
Limt test Pharmaceutical Inorganic chemistry UNIT-I (Part-III) Limit Test.
Limit tests:- Factors affecting limit tests:
Specificity of the tests
Sensitivity
Control of personal errors (Analyst errors)
Test in which there is no visible reaction
Comparison methods
Quantitative determination
Limit test for Chloride: Principle, Procedure, observation and result.
Limit test for Sulphate: Principle, Procedure, observation and result
Limit test for Iron: Principle, Procedure, observation and result.
Limit test for Heavy metal: Principle, Procedure, observation and result.
Limit test for Lead: Principle, Procedure, observation and result.
Limit test for Arsenic: Principle, Gutzet test Procedure, detail in Gutzet Apparatus. observation and result.
Modifies Limit test for Chloride: Principle, Procedure, observation and result.
Modified Limit test for sulphate: Principle, Procedure, observation and result.
Non Aqueous Titration
Types of solvents used in non aqueous Titration
Compounds used for non aqueous Titration
Titration done for weak acid and weak base,
The need for non aqueous titration arises because water can behave as a weak base and a weak acid as well, and can hence compete in proton acceptance or proton donation with other weak acids and bases dissolved in it.
In this ppt the viewer will able to know about different methods for the protein analysis. Proteins are long chain of amino acids and there are specific test also required depends on the nature and structure of proteins. As the name suggest amino acids are organic compounds that contain amino and carboxyl groups. The R- in the formulas stands for different chemical groups (may be aliphatic, aromatic or heterocycylic) and this determines the characteristics of the amino acids. The colour tests have frequently been used for qualitative detection of amino acids. Not all amino acids contain the same reactive groups. For this reason the various colour tests yield reactions varying in intensity and type of colour according to the nature of groups contained in the particular amino acid under examination.
• Portion explained:
• Detection of Proteins
1. Millon’s reaction
2. Millon-Nasse reaction
3. Xanthoproteic reaction
4. Hopkins-Cole reaction
5. Biuret test
6. Ninhydrin reaction
7. Folin test
8. Sakaguchi test
9. Nitroprusside test
10. Spectrophometric method
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New drug discovery and drug development process
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New drug discovery and drug development process
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2. LIMIT TEST FOR HEAVY METALS
• The limit test for heavy metals is designed to determine the content of
metallic impurities that are coloured by hydrogen sulphide or sodium
sulphide under the condition of the test.
• The heavy metals (metallic impurities) may be iron, copper, lead, nickel,
cobalt, bismuth, antimony etc.
• The limit for heavy metals is indicated in the individual monograph in
term of ppm of lead i.e. the parts of lead per million parts of the
substance being examined.
• The Indian pharmacopoeia had adopted three methods (methods A, B,
and C) for the limit test for heavy metals.
3. PRINCIPLE
• Method A, B and C are based upon the reaction of the heavy metal ion
with hydrogen sulphide (in method A and B) or sodium sulphide (in
method C) leading to the formation of heavy metal sulphides. The metal
sulphides remain distributed in a colloidal state and give rise to a
brownish colouration. The colour produced in the test solution is
compared with that of standard solution containing a definite amount
of the lead.
4. PRINCIPLE
• The colour is compared by keeping the two Nessler cylinders
side by side and viewing vertically downwards against a white
background. The usual limit for heavy metals as per I.P. is 20
ppm.
5. METHOD
• Method A: It is applicable for the substance, which give clear colourless solution
under specified conditions of test.
• Standard solution: Pipette 1.0 ml of standard lead solution (20 ppm Pb) into a
Nessler cylinder labeled as “Standard” and dilute to 25 ml with water. Adjust the
pH between 3.0 and 4.0 with dilute acetic acid or dilute ammonia solutions, dilute
to 35 ml with water and mix.
• Test solution: Take 25 ml of the solution prepared as directed in the individual
monograph into a Nessler cylinder labeled as “Test” or dissolve the specified
quantity of the substance in water to produce 25 ml. Adjust the pH between 3.0
and 4.0 with dilute acetic acid or dilute ammonia solution, dilute to 35 ml with
water and mix.
• Procedure: Add 10 ml of freshly prepared hydrogen sulphide to each of the
Nessler cylinder containing test solution and standard solution respectively. Mix,
dilute to 50 ml with water and allow to stand for 5 minutes. Compare the colour
by viewing vertically downwards over a white surface. The colour produced with
the test solution in not more intense than that produced with the standard
solution.
• Preparation of standard lead solution (20 ppm Pb): Dilute 1 volume of standard
lead solution (0.1% Pb) to 50 volumes with water.
6. METHOD
• Method B: It is applicable for those substances, which do not give a clear
colourless solution under the specified conditions.
• Standard solution: Same as for Method A
• Test solution: In a suitable crucible the quantity of the substane is weighed,
sufficient sulphuric acid added to wet the sample, and ignited at low temperature
until throughly charred. To the charred mass 2ml nitric acid and five drops of
sulphuric acid are added, heated cautiously until white fumes are no longer
evolved, ignited preferably in a muffle furnace, at 500oC to 600oC, until the carbon
is completely burnt off. It is cool, 4ml of hydrochloric acid are added, covered,
digested on a water-bath for 15 minutes, uncovered and slowly evaporated to
dryness on a water-bath.
• The residue is moistened with one drop of HCl and 10ml of hot water are added
and digested for two minutes. Ammonia solution is added drop wise until the
solution is just alkaline to litmus paper, diluted with water to 25ml and adjust pH
between 3.0 to 4.0 with dilute acetic acid. It is filtered and filtrate transfer into
50ml Nesseler cylinder, diluted with water to about 35ml and mixed.
• Procedure: Same as for Method A.
7. METHOD
• Method C: It is applicable to those substances that give clear
colourless solution in sodium hydroxide.
• Standard solution: Pipette 1.0 ml of standard lead solution (20 ppm
Pb) into a Nessler cylinder labeled as “Standard”, add 5 ml of dilute
sodium hydroxide solution, dilute to 50 ml with water and mix.
• Test solution: Place 25 ml of the solution prepared as directed in the
individual monograph into a Nessler cylinder labeled as ‘Test’ or
dissolve the specified quantity of the substance in 20 ml of water and
5 ml of dilute sodium hydroxide solution. Dilute to 50 ml with water
and mix.
• Procedure: Add 5 drops of sodium sulphide solution to each the
Nessler cylinder containing the standard solution and the test solution
respectively. Mix and allows to stands for 5 minutes and compare the
colour by viewing vertically down words over a white surface. The
colour produced with the test solution is not more intense than that
produced with the standard solution.