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.
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 tests, Introduction, Definition,
Limit Test For Chlorides
Limit Test For Sulphates
Limit Test For Iron
Limit Test For Lead
Limit Test For Arsenic
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.
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 tests, Introduction, Definition,
Limit Test For Chlorides
Limit Test For Sulphates
Limit Test For Iron
Limit Test For Lead
Limit Test For Arsenic
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 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.
Introduction of Inorganic Chemistry, History of Pharmacopoeia.pptxMs. Pooja Bhandare
Introduction of Inorganic Chemistry, History of Pharmacopoeia, Pharmaceutical Chemistry, Inorganic Chemistry:
IMPORTANTS OF INORGANIC CHEMISTRY, Introduction of Pharmacopoeia, Types of Pharmacopoeia, History of pharmacopoeia, HISTROY OF INDIAN PHARMACOPOEIA
Content of pharmacopoeia Introduction including general Notices
Monographs of the official drugs
Appendices
Types and Sources of impurities.pptx Pharmaceutical Inorganic chemistry UNIT-...Ms. Pooja Bhandare
Types and Sources of impurities. Pharmaceutical Inorganic chemistry UNIT-I (Part-II) Impurities:
Impure Chemical Compound
Pure Chemical Compound.
Types of impurities: Organic Impurity, Inorganic impurity, Residual solvent, Sources of Impurities in Pharmaceuticals
The different sources of impurities in pharmaceuticals are listed below:
Raw material used in manufacture
Reagents used in manufacturing process
Method/ process used in manufacture or method of manufacturing
Chemical processes used in the manufacture
Atmospheric contamination during the manufacturing process
Intermediate products in the manufacturing process
Defects in the manufacturing process
Manufacturing hazards
Inadequate Storage conditions
Decomposition of the product during storage
Accidental substitution or deliberate adulteration with spurious or useless materials.
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
Insoluble Constituent or Residue.
Ash, Water insoluble ash
Arsenic or lead
Loss on drying
Loss on ignition.
Effect of Impurities
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.
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
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.
Introduction of Inorganic Chemistry, History of Pharmacopoeia.pptxMs. Pooja Bhandare
Introduction of Inorganic Chemistry, History of Pharmacopoeia, Pharmaceutical Chemistry, Inorganic Chemistry:
IMPORTANTS OF INORGANIC CHEMISTRY, Introduction of Pharmacopoeia, Types of Pharmacopoeia, History of pharmacopoeia, HISTROY OF INDIAN PHARMACOPOEIA
Content of pharmacopoeia Introduction including general Notices
Monographs of the official drugs
Appendices
Types and Sources of impurities.pptx Pharmaceutical Inorganic chemistry UNIT-...Ms. Pooja Bhandare
Types and Sources of impurities. Pharmaceutical Inorganic chemistry UNIT-I (Part-II) Impurities:
Impure Chemical Compound
Pure Chemical Compound.
Types of impurities: Organic Impurity, Inorganic impurity, Residual solvent, Sources of Impurities in Pharmaceuticals
The different sources of impurities in pharmaceuticals are listed below:
Raw material used in manufacture
Reagents used in manufacturing process
Method/ process used in manufacture or method of manufacturing
Chemical processes used in the manufacture
Atmospheric contamination during the manufacturing process
Intermediate products in the manufacturing process
Defects in the manufacturing process
Manufacturing hazards
Inadequate Storage conditions
Decomposition of the product during storage
Accidental substitution or deliberate adulteration with spurious or useless materials.
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
Insoluble Constituent or Residue.
Ash, Water insoluble ash
Arsenic or lead
Loss on drying
Loss on ignition.
Effect of Impurities
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.
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
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.
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
INTRODUCTION TO PHARMACEUTICAL CHEMISTRY AND LIMIT TESTSUJATA WANKHEDE
INTRODUCTION TO PHARMACEUTICAL CHEMISTRY, INTRODUCTION TO LIMIT TESTS, LIMIT TEST OF IRON, CHLORIDE, SULPHATE, ARSENIC AND THERE DIAGRAMS WITHTHE PRINCIPAL AND PROCEDURE OF ALL THE LIMIT TEST WITH THEIR RESULTS
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.
Non aqueous titration refers to a type of titration in which the analyte substance is dissolved in a solvent which does not contain water. This procedure is a very important one in pharmacopoeial assays.
Similar to Limt test Pharmaceutical Inorganic chemistry UNIT-I (Part-III) Limit Test (20)
Pharmaceutical Inorganic chemistry UNIT-V Radiopharmaceutical.pptx
Isotopes Types of decay
Alpha rays, which could barely penetrate a piece of paper
Beta rays, which could penetrate 3 mm of aluminium
Gamma rays, which could penetrate several centimetres of lead
Units of Radioactivity:
Measurement of Radioactivity
The measurement of nuclear radiation and detection is an important aspect in the identification of type of radiations (, , ) and to assay the radionuclide emitting the radiation, suitable detectors are required. The radiations are identified on the basis of their properties.
e.g. Ionization effect is measured in Ionization Chamber, Proportional Counter and Geiger Muller Counter.
The scintillation effect of radiation is measured using scintillation detector and the photographic effect is measured by Autoradiography.
Gas Filled Detectors:
Ionization Chamber:
Proportional Counters:
Geiger-Muller Counter
Properties of α, β, γ radiations
Half –life of Radioelement
Sodium Iodide (I131)
Handling and Storage of Radioactive Material:
Storage of Radioactive Substances –
Precautions For Handling Radioactive Substances
Labelling of Radioactive Substances
Pharmaceutical Application Of Radioactive Substances
Major extra and intracellular electrolytes. Pharmaceutical Inorganic chemistr...Ms. Pooja Bhandare
Major extra and intracellular electrolytes. Pharmaceutical Inorganic chemistry UNIT-II (Part-II)
Electrolyte: Intracellular fluid
Interstitial fluid
Plasma (Vascular fluid)
Anionic electrolytes- HCO₃⁻, Cl⁻, SO₄²⁻, HPO₄²⁻
Cationic electrolytes- Na⁺, K⁺, Ca²⁺, Mg²⁺
Concentration of important Electrolytes:
Electrolytes used in the replacement therapy: Sodium
chloride*, Potassium chloride, Calcium gluconate* and Oral Rehydration Salt
(ORS), Physiological acid base balance.
Acids, Bases And Buffers Pharmaceutical Inorganic chemistry UNIT-II (Part-I)
Acids, Bases are defined by Four main theories,
1.Traditional theory / concept
2.Arrhenius theory
3.Bronsted and Lowry theory
4.Lewis theory
Importance of acids and bases in pharmacy
Buffers: Buffer action
Buffer capacity Buffers system
Types of Buffers : Generally buffers are of two types:
1. Acidic buffers
2. Basic buffers
There are some other buffer system:
3. Two salts acts as acid-base pair. Ex- Potassium hydrogen phosphate and potassium dihydrogen phosphate.
4. Amphoteric electrolyte. Ex- Solution of glycine.
5. Solution of strong acid and solution of strong base. Ex- Strong HCl with KCl Mechanism of Buffer action: Mechanism of Action of acidic buffers: Buffer equation-Henderson-Hasselbalch equation:
Standard Buffer Solutions Preparation of Buffer Solutions: Buffers in pharmaceutical systems or Application of buffer: Stability of buffers Buffered isotonic solution Types of Buffer Isotonic solution
1. Isotonic Solutions:
2. Hypertonic Solutions:
3. Hypotonic Solution:
Measurement of Tonicity: 1. Hemolytic method: 2. Cryoscopic method or depression of freezing point:
Methods of adjusting the tonicity:
Class I methods:
In this type, sodium chloride or other substances are added to the solution in sufficient quantity to make it isotonic. Then the preparation is brought to its final volume withan isotonic or a buffered isotonic diluting solution.
These methods are of two types:
Cryoscopic method
Sodium chloride equivalent method.
Class II methods:
In this type, water is added in sufficient quantity make the preparation isotonic. Then the preparation is brought to its volume with an isotonic or a buffered isotonic diluting solution.
These methods are of two types:
White-Vincent method
Sprowls method.
Polyploidy, mutation and hybridization with reference to medicinal plants. PH...Ms. Pooja Bhandare
Polyploidy, mutation and hybridization with reference to medicinal plants. PHARMACOGNOSY & Phytochemistry-I (BP405T)Unit-IIPart-4
Polyploidy reference to medicinal plants.
Types Of Polyploidy
A. Euploidy
a.Autopolyploidy
b. Allopolyploidy
B. Aneuploidy
1. Causes Of Polyploidy
2. Non-disjunction in mitosis
3. Non-reduction in meiosis
4. Polyspermy
5. Endo-replication or Endo- reduplication.
Factors Promoting Polyploidy
1. Physical factor
2. Chemical factor
3. Biological factor
Physical factor:-
Temperature :- heat temperature & cold temperature
Centrifugation
X-rays
Gamma rays
Cosmic rays
Ionizing & non-ionizing radiations
UV-radiations
Chemical factor:-
Alkylating agents:- nitrogen & sulphur mustard
Acridines
Proflavins
Nitrous acid
Colchicines[6]
Colchicines (Poisonous alkaloids):-
Biological factor
Mode of reproduction
Mode of fertilization
Breeding system present (Hybridization)
Growth habit of the plant
Size of chromosomes
Application Of Polyploidy
Mutation breeding
Seedless fruits production
Bridge crossing
Ornamental & forage breeding
Disease resistance through aneuploidy
Industrial application of polyploidy
mutation reference to medicinal plants
Type of mutations:
1. Spontaneous and induced mutations.
2. Recessive and dominant mutations.
3. Somatic and germinal mutations.
4. Forward, back and suppressor mutation.
5. Chromosomal, genomic and point mutations
Application Of Mutation:
Hybridization reference to medicinal plants
The following steps are involved in hybridization of plant:
Choice Of Parents:.
Selfing Of Parents
Emasculation:.
Bagging:
Crossing Or Cross Pollination
Labelling
Collection Of Hybrid Seeds
Significance of Hybridization
PHARMACOGNOSY & Phytochemistry-I (BP405T)Unit-IIPart-2.FACTORS AFFECTING CULTIVATION
1. Altitude
2.Temperature
3. Rainfall
4. Day Length and Day Light
5. Soil
6. Soil Fertility
7. Fertilizers and Manures
a) Chemical fertilizers
(b) Manures
(c) Biofertilizers
8. Pests and Pests Control
a. Microbes
b) Insects
C) Non insect pests
d) Weeds
9. Other Factors that Affect the Cultivated Plants
a. Air Pollution
b. Herbicide
Cultivation and collections of drugs of natural origin..pptxMs. Pooja Bhandare
PHARMACOGNOSY & Phytochemistry-I (BP405T)Unit-IIPart-1Cultivation and collections of drugs of natural origin.
Advantages of cultivation
Methods of Plant Propagation
1.Sexual method (seed propagation)
2. Asexual method
Methods of sowing the seeds
Broadcasting Dibbling Miscellaneous
Special treatment to seeds
Asexual method.
Asexual method of vegetative propagation consists of three types:
a) Natural methods of vegetative propagation.
b) Artificial methods of vegetative propagation.
c) Aseptic method of micropropagation (tissue-culture).
COLLECTION OF CRUDE DRUGS
HARVESTING OF CRUDE DRUGS
DRYING OF CRUDE DRUGS
(1) natural (sun drying) and (2) artificial
Artificial Drying
Drying by artificial means includes drying the drugs in
(a) an oven; i.e. tray-dryers;
(b) vacuum dryers and
(c) spray dryers.
GARBLING (DRESSING)
PACKING OF CRUDE DRUGS
STORAGE & PRESEVATION OF CRUDE DRUGS
Quality control of Drugs of Natural Origin. PHARMACognosy & Phytochemistry-I ...Ms. Pooja Bhandare
Quality control of Drugs of Natural Origin PHARMACognosy & Phytochemistry-I (BP405T)Unit-I Part-3.
CONTENTS
Adulteration
Evaluation of adulteration
Morphological / Organoleptic evaluation
Microscopic evaluation
Quantitative evaluation
Physical evaluation
Chemical evaluation
Biological evaluation
Adulteration is of two types:
Indirect or Unintentional adulteration
Direct or Intentional adulteration
Intentional adulteration may be due to the following reasons
adulteration using manufactured substances
substitution using inferior commercial varieties
substitution using exhausted drugs
substitution of superficially similar inferior natural substance
adulteration using the vegetative part of the same plant
addition of toxic materials
adulteration of powders
addition of synthetic principles
Evaluation of Crude Drugs
1. ORGANOLEPTIC EVALUATION
2. MICROSCOPICAL EVALUATION
Stomatal index Vein-islet number
Veinlet termination number
Palisade ratio
Quantitative Microscopy (Lycopodium Spore Method)
3.CHEMICAL EVALUATION
4. Physical Evaluation
I. Solubility
II. Optical Rotation
III. Refractive Index
III. Specific Gravity
IV Viscosity
V. Melting Point
VI. Moisture Content
VII. Ultraviolet Light
VIII. Ash Values
Total ash
Acid-insoluble ash
The water-soluble ash
IX. Extractive Values
X. Foreign Organic Matters
5. BIOLOGICAL EVALUATION
Toxicity
Oxytocic activity
Microbiological assays
Classification of Crude Drugs. HARMACognosy & Phytochemistry-I (BP405T)Unit-I...Ms. Pooja Bhandare
Classification of Crude Drugs.PHARMACognosy & Phytochemistry-I (BP405T)Unit-I Part-2.
A method of classification should be:
a) simple,
b) easy to use, and
c) free from confusion and ambiguities.
TYPES OF CLASSIFICATION.
1.Alphabetical classification
2.Taxonomical classification
3.Morphological classification
4.Pharmacological classification
5.Chemical classification
6.Chemotaxonomical classification
7. Serotaxanomical Classification
Animal Cell Culture: Growth of animal cells in culture. PHARMACEUTICAL MICROB...Ms. Pooja Bhandare
PHARMACEUTICAL MICROBIOLOGY (BP303T)Unit-VPart-4
Animal Cell Culture: Growth of animal cells in culture.
Introduction: Histroy, The culture media used for animal cell culture are classified as,
Natural, Artificial, Synthesized
Natural Culture Media:
a. Blood Plasma:
b. Blood Serum:
c. Tissue Extracts:
Artificial Media
Some common examples of artificial media are,
Minimal Essential Medium (MEM),
CMRL 1066,
RPMI 1640.
Synthetic media re classified as,
Serum Containing Media.
Serum Free Media.
a. Serum Containing Media:
b. Serum Free Media:
Physicochemical Parameters needed for growth animal cell culture:
General procedure for cell Culture.
Isolation of the tissue:
Disaggregation of the Tissue:
Mechanical disaggregation
b. Enzymatic Disaggregation
. Trypsin based disaggregation or trypsinization:
Warm trypsinization:
Cold trypsinization:
Drawbacks of trypsin disaggregation:
B. Collagenase based disaggregation:
C. Chelating Agents:
3. Seeding of Culture:
Preservation of pharmaceutical products using antimicrobial agents. PHARMACEU...Ms. Pooja Bhandare
PHARMACEUTICAL MICROBIOLOGY (BP303T)Unit-VPart-3
Preservation of pharmaceutical products using antimicrobial agents.
Introduction. Ideal Properties of Preservatives:
Antimicrobial Chemical Preservatives
Development of a Preservative System.
Factors affecting efficacy of a preservative: 1. Interaction With components of the formulation
2. Properties of the Preservatives:
3) Effect of Containers.
4) Type of microbes:
5) Influence of pH:
Challenge Test: Efficacy Test of Preservative : Medium used, Choice of test organism:
Preparation of the inoculum:
Procedure:
Interpretation of Results:
Assessment of microbial contamination and spoilage. PHARMACEUTICAL MICROBIOLO...Ms. Pooja Bhandare
PHARMACEUTICAL MICROBIOLOGY (BP303T)Unit-VPart-2
Assessment of microbial contamination and spoilage.
Assessment of microbial contamination and spoilage
1. Physical and chemical changes:
2. Assessment of viable microorganisms in non-sterile products:
3. Sterility test:
4. Estimation of pyrogens:
Microbial Limit Tests:
Total Aerobic Microbial Count:
Membrane Filtration.
Plate Count Methods.
Pour Plate Method.
Surface spread Method.
Most Probable Number(MPN)
Types of spoilage, factors affecting the microbial spoilage of pharmaceutical...Ms. Pooja Bhandare
PHARMACEUTICAL MICROBIOLOGY (BP303T)Unit-V Part-1
Types of spoilage, factors affecting the microbial spoilage of pharmaceutical products, source and type of contaminants. Introduction: Defintion Types of Microbial Spoilage:
1. Infection induced due to contaminated pharmaceutical products: Table no. 1.1 Common pathogens spoiling pharmaceutical products:
2. Physicochemical spoilage –
i) Viable growth ii) Gas production
iii) Colouration / Decolouration
iv) Odour formation
v) Taste change
3. Physical Spoilage:
Cracking of emulsion:
Odor changes
4. Biological spoilage:
Microbial Toxins
Microbial Metabolites
5. Chemical spoilage: Table 1.2 Susceptibility of pharmaceutical ingredients to microbial contamination
Factors affecting microbial spoilage
Size of contaminant inoculum
Nutritional factors
Moisture content
pH
Storage temperature
Redox potential
Packaging design
Sources and Types Of Contamination:
Personnel,
Poor facility design,
Incoming ventilation air,
Machinery and other equipment for production,
Raw material and semi-finished material,
Packaging material,
Utilities,
Different media used in the production process as well as for cleaning and Cleanroom clothing.
Microbiological Assay of Vitamin & Amino acid Assessment of a New Antibiotic...Ms. Pooja Bhandare
PHARMACEUTICAL MICROBIOLOGY (BP303T) Unit-IV Part-3
Microbiological Assay of Vitamin & Amino acid Assessment of a New Antibiotic: Introduction:
Principle
Microbiological Assay of Cynocobalamin (Vitamin B12):
Tritrimetric Method.
Turbidimetric Method.
Preparation of Standard Cynocobalmine stock solution:
Preparation of Basal Medium Stock Solution:
Test Solution of the material to be assayed Preparation of inoculum: Procedure of Titrimetric method: Turbidimetric Method: Microbiological assay of Amino acids. Assessment of a New Antibiotic.
Introduction:
MIC of an antibiotic is tested either by one of the following ways,
Liquid Dilution Method.
Solid Dilution Method
Principles and methods of different microbiological assay, methods for standa...Ms. Pooja Bhandare
PHARMACEUTICAL MICROBIOLOGY (BP303T)Unit-IV Part-2 Principles and methods of different microbiological assay, methods for standardization of antibiotics.
Introduction: Principles Advantages of Microbial Assay: Disadvantages of Microbial Assay: MICROBIOLOGICAL ASSAY OF ANIBIOTICS PRINCIPLE Media used for antibiotics assay Standard Preparation. Buffer Solutions Preparation of the Sample Solution: Test Organisms Preparation of inoculum: Methods of preparation of test organism suspension: Assay Methods: Method A: Cup-plate or Cylinder Plate Method.
Method B: Turbidimetric or Tube assay Method
Designing of aseptic area, laminar flow equipment: Study of different source ...Ms. Pooja Bhandare
Designing of aseptic area, laminar flow equipment: Study of different source of contamination in aseptic area and methods of prevention, clean area classification. PHARMACEUTICALMICROBIOLOGY (BP303T)Unit-IVPart-1
Introduction: Designing of Aseptic Area . i) The clean-up area,
ii) The compounding area,
iii) The aseptic area,
iv) The quarantine area and
v) The packaging/labelling area.
Flow diagram of aseptic area. Floors, walls and ceilings, Doors, windows and services Personnel and protective clothing Cleaning and disinfection. Air Supply. Laminar flow equipment. Vertical laminar air flow bench
Horizontal laminar air flow bench
High Efficiency Particulate Air (HEPA) Filter. Operating Instructions Uses of Laminar Air Flow.Advantages of Laminar Air Flow.Limitations of Laminar Air Flow. Air flow pattern Unidirectional airflow
Non-unidirectional airflow
Combined airflow
Different Sources of Contamination in an Aseptic Area
1) Personnel:
2) Buildings and Facilities
3) Equipment and Utensils:
4) Raw Materials
5) Manufacturing Process:
Methods of Prevention of Contamination Clean Area Classification
Honest Reviews of Tim Han LMA Course Program.pptxtimhan337
Personal development courses are widely available today, with each one promising life-changing outcomes. Tim Han’s Life Mastery Achievers (LMA) Course has drawn a lot of interest. In addition to offering my frank assessment of Success Insider’s LMA Course, this piece examines the course’s effects via a variety of Tim Han LMA course reviews and Success Insider comments.
Read| The latest issue of The Challenger is here! We are thrilled to announce that our school paper has qualified for the NATIONAL SCHOOLS PRESS CONFERENCE (NSPC) 2024. Thank you for your unwavering support and trust. Dive into the stories that made us stand out!
Synthetic Fiber Construction in lab .pptxPavel ( NSTU)
Synthetic fiber production is a fascinating and complex field that blends chemistry, engineering, and environmental science. By understanding these aspects, students can gain a comprehensive view of synthetic fiber production, its impact on society and the environment, and the potential for future innovations. Synthetic fibers play a crucial role in modern society, impacting various aspects of daily life, industry, and the environment. ynthetic fibers are integral to modern life, offering a range of benefits from cost-effectiveness and versatility to innovative applications and performance characteristics. While they pose environmental challenges, ongoing research and development aim to create more sustainable and eco-friendly alternatives. Understanding the importance of synthetic fibers helps in appreciating their role in the economy, industry, and daily life, while also emphasizing the need for sustainable practices and innovation.
Embracing GenAI - A Strategic ImperativePeter Windle
Artificial Intelligence (AI) technologies such as Generative AI, Image Generators and Large Language Models have had a dramatic impact on teaching, learning and assessment over the past 18 months. The most immediate threat AI posed was to Academic Integrity with Higher Education Institutes (HEIs) focusing their efforts on combating the use of GenAI in assessment. Guidelines were developed for staff and students, policies put in place too. Innovative educators have forged paths in the use of Generative AI for teaching, learning and assessments leading to pockets of transformation springing up across HEIs, often with little or no top-down guidance, support or direction.
This Gasta posits a strategic approach to integrating AI into HEIs to prepare staff, students and the curriculum for an evolving world and workplace. We will highlight the advantages of working with these technologies beyond the realm of teaching, learning and assessment by considering prompt engineering skills, industry impact, curriculum changes, and the need for staff upskilling. In contrast, not engaging strategically with Generative AI poses risks, including falling behind peers, missed opportunities and failing to ensure our graduates remain employable. The rapid evolution of AI technologies necessitates a proactive and strategic approach if we are to remain relevant.
The Roman Empire A Historical Colossus.pdfkaushalkr1407
The Roman Empire, a vast and enduring power, stands as one of history's most remarkable civilizations, leaving an indelible imprint on the world. It emerged from the Roman Republic, transitioning into an imperial powerhouse under the leadership of Augustus Caesar in 27 BCE. This transformation marked the beginning of an era defined by unprecedented territorial expansion, architectural marvels, and profound cultural influence.
The empire's roots lie in the city of Rome, founded, according to legend, by Romulus in 753 BCE. Over centuries, Rome evolved from a small settlement to a formidable republic, characterized by a complex political system with elected officials and checks on power. However, internal strife, class conflicts, and military ambitions paved the way for the end of the Republic. Julius Caesar’s dictatorship and subsequent assassination in 44 BCE created a power vacuum, leading to a civil war. Octavian, later Augustus, emerged victorious, heralding the Roman Empire’s birth.
Under Augustus, the empire experienced the Pax Romana, a 200-year period of relative peace and stability. Augustus reformed the military, established efficient administrative systems, and initiated grand construction projects. The empire's borders expanded, encompassing territories from Britain to Egypt and from Spain to the Euphrates. Roman legions, renowned for their discipline and engineering prowess, secured and maintained these vast territories, building roads, fortifications, and cities that facilitated control and integration.
The Roman Empire’s society was hierarchical, with a rigid class system. At the top were the patricians, wealthy elites who held significant political power. Below them were the plebeians, free citizens with limited political influence, and the vast numbers of slaves who formed the backbone of the economy. The family unit was central, governed by the paterfamilias, the male head who held absolute authority.
Culturally, the Romans were eclectic, absorbing and adapting elements from the civilizations they encountered, particularly the Greeks. Roman art, literature, and philosophy reflected this synthesis, creating a rich cultural tapestry. Latin, the Roman language, became the lingua franca of the Western world, influencing numerous modern languages.
Roman architecture and engineering achievements were monumental. They perfected the arch, vault, and dome, constructing enduring structures like the Colosseum, Pantheon, and aqueducts. These engineering marvels not only showcased Roman ingenuity but also served practical purposes, from public entertainment to water supply.
Instructions for Submissions thorugh G- Classroom.pptxJheel Barad
This presentation provides a briefing on how to upload submissions and documents in Google Classroom. It was prepared as part of an orientation for new Sainik School in-service teacher trainees. As a training officer, my goal is to ensure that you are comfortable and proficient with this essential tool for managing assignments and fostering student engagement.
The French Revolution, which began in 1789, was a period of radical social and political upheaval in France. It marked the decline of absolute monarchies, the rise of secular and democratic republics, and the eventual rise of Napoleon Bonaparte. This revolutionary period is crucial in understanding the transition from feudalism to modernity in Europe.
For more information, visit-www.vavaclasses.com
Model Attribute Check Company Auto PropertyCeline George
In Odoo, the multi-company feature allows you to manage multiple companies within a single Odoo database instance. Each company can have its own configurations while still sharing common resources such as products, customers, and suppliers.
Palestine last event orientationfvgnh .pptxRaedMohamed3
An EFL lesson about the current events in Palestine. It is intended to be for intermediate students who wish to increase their listening skills through a short lesson in power point.
2024.06.01 Introducing a competency framework for languag learning materials ...Sandy Millin
http://sandymillin.wordpress.com/iateflwebinar2024
Published classroom materials form the basis of syllabuses, drive teacher professional development, and have a potentially huge influence on learners, teachers and education systems. All teachers also create their own materials, whether a few sentences on a blackboard, a highly-structured fully-realised online course, or anything in between. Despite this, the knowledge and skills needed to create effective language learning materials are rarely part of teacher training, and are mostly learnt by trial and error.
Knowledge and skills frameworks, generally called competency frameworks, for ELT teachers, trainers and managers have existed for a few years now. However, until I created one for my MA dissertation, there wasn’t one drawing together what we need to know and do to be able to effectively produce language learning materials.
This webinar will introduce you to my framework, highlighting the key competencies I identified from my research. It will also show how anybody involved in language teaching (any language, not just English!), teacher training, managing schools or developing language learning materials can benefit from using the framework.
Limt test Pharmaceutical Inorganic chemistry UNIT-I (Part-III) Limit Test
1. Pharmaceutical Inorganic chemistry
UNIT-I (Part-III)
Limit Test
Presented By
Ms. Pooja D. Bhandare
(Assistant Professor)
DADASAHEB BALPANDE COLLEGE OF PHARMACY BESA NAGPUR
2. Limit tests:-
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.
• Tests being used to identify the impurity.
• Tests being used to control the impurity.
3. Factors affecting limit tests:
• Specificity of the tests
• Sensitivity
• Control of personal errors (Analyst errors)
a) Test in which there is no visible reaction
b) Comparison methods
c) Quantitative determination
4. Limit test for Chloride:
• The test is used to limit the amount of Chloride as an impurity in inorganic
substances.
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- + AgNO3 --------------------------AgCl + NO3-
Soluble chloride
present as impurity
5. • 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.
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 10 ml of nitric acid Add 10 ml of nitric acid
Dilute to 50 ml with Distilled water in Nessler
cylinder with
Dilute to 50 ml with Distilled water in Nessler
cylinder with
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.
8. • 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 visa versa.
• 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 in AgCl.
9. • Pharmacopoeia does not prescribe any numerical value of limit test for chlorides,
sulphate and iron because limit test is based on the simple comparison of
opalescence or colour between the test and standard solution prescribed according
to pharmacopoeia.
• In this type of limit test, the extent of turbidity or opalescence or colour produced
in influenced by the presence of other impurities present in the substance and also
by variation in time and method of performance of test.
• Thus the pharmacopoeia does not prescribe any numerical value of the limit test.
10. • The limit test involve simple comparisons of opalescence, turbidity, or colour
with standard.
• These are semi-qualitative reactions in which extent of impurities present can
be estimated by comparing visible reaction response of the test and standard.
• By this way, extent of reaction is readily determined by direct comparison of
test solution with standard. So pharmacopoeia prefers comparison methods.
11. Limit test for sulphate:
• The Sulfate Limit Test is designed to determine the allowable limit of sulfate contained in a sample.
Principle:
• 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.
• Then comparison of turbidity is done with a standard turbidity obtained from a known amount of Sulphate
and same volume of dilute Hydrochloric acid have been added to both solutions.
• The barium chloride test solution in the IP has been replaced by Barium sulphate reagent which is having
barium chloride, sulphate free alcohol (Avoid supersaturation) and a solution of potassium sulphate.
Potassium sulphate has been added to increase the sensitivity of the test.
12. 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 0.1089 % W/V solution of potassium
sulphate in Nessler cylinder
Add 2 ml of dilute hydrochloric acid Add 2 ml of dilute hydrochloric acid
Dilute to 45 ml with Distilled water in Nessler
cylinder.
Dilute to 50 ml with Distilled water in Nessler
cylinder.
Add 5 ml of barium sulphate reagent Add 5 ml of barium sulphate reagent
Keep aside for 5 min Keep aside for 5 min
Observe the Opalescence/Turbidity Observe the Opalescence/Turbidity
13. • Barium sulphate reagent contains barium chloride, sulphate free alcohol and small amount of
potassium sulphate.
• Observation:
• The turbidity produce in sample solution should not be greater than standard solution. If turbidity
produces in sample solution is less than the standard solution, the sample will pass the limit test of
sulphate and vice versa.
• Reasons:
• Hydrochloric acid helps to make solution acidic.
• Potassium sulphate is used to increase the sensitivity of the test by giving ionic
• concentration in the reagent.
• Alcohol helps to prevent super saturation and so produces a more uniform opalescence.
14. Limit test for Arsenic:
• Arsenic is a well known undesirable and harmful impurity which is
present in medicinal substances.
• All pharmacopoeias prescribe a limit test for it.
• Pharmacopoeial method is based on the Gutzeit test.
• All the special reagents used in the limit test for Arsenic are marked and
distinguished by letter ‘As T’, which means that they all should be
Arsenic free and should themselves conform to the test for Arsenic.
15. Principle:
• Limit test of Arsenic is based on the reaction of arsenic gas with hydrogen ion to
form yellow stain on mercuric chloride paper in presence of reducing agents like
potassium iodide. It is also called as Gutzeit test and requires special apparatus.
• Arsenic, prese3nt as arsenic acid (H3AsO4) in the sample is reduced to arsenious
acid (H3AsO3) by reducing agents like potassium iodide, stannous acid, zinc,
hydrochloric acid, etc. Arsenious acid is further reduced to arsine (gas) (AsH3) by
hydrogen and reacts with mercuric chloride paper to give a yellow stain.
Substance + dil HCl -------------------------H3AsO4
(contains Arsenic impurity) Arsenic acid
• H3AsO4 + H2SnO2 -------------------→ H3AsO3 + H2SnO3
Arsenic acid Stannous acid Arsenious acid
H3AsO3 + 6[H] ---------------------→ AsH + 3H2O
Arsenious acid nascent hydrogen Arsine gas
The depth of yellow stain on mercuric chloride paper will depend upon the quantity of
arsenic present in the sample.
16. • When the sample is dissolved in acid, the Arsenic present in the sample gets
converted to Arsenic acid.
• By action of reducing agents like Potassium iodide, stannous acid etc.,
Arsenic acid gets reduced to arsenious acid.
• The nascent hydrogen formed during the reaction, further reduces
Arsenious acid to Arsine gas, which reacts with mercuric chloride paper,
giving a yellow stain.
17.
18. • Apparatus:
• It is having a wide mouthed glass bottle of 120 mL capacity having mouth of about 2.5 cm in
diameter. This bottle is fitted with a rubber bung through which passes a glass tube, 20 cm long.
• External diameter=0.8 cm
• Internal diameter=0.65 cm
• The tube is constricted at its lower end extremity to about 1 mm diameter and there is blown a hole,
not less than 2 mm in diameter, in the side of the tube near the constricted part.
• The upper end of the glass tube is fitted with two rubber bungs(25 mm x 25 mm), each having a
hole bored centrally and exactly 6.5 mm in diameter.
• One of the bungs has been fitted to the upper end of the tube, while the second bung has to be fitted
upon the first bung in such a way that the mercuric chloride paper gets exactly sandwiched between
the central perforation of the two.
• The bungs are kept in close contact by using rubber band or spring clip in such a manner that the
gas evolved from the bottle must have to pass through the 0.65 mm internal circle of mercuric
chloride paper.
• During the test, the evolved gases have been passing through the side hole, the lower hole serving as
an exit for water which condenses in the constricted part of the tube.
• An important feature has been the standardization of the area of Mercuric chloride paper which is
exposed to the reaction of arsine gas.
19. Test sample Standard compound
The test solution is prepared by dissolving specific
amount in water and stannated HCl (arsenic free) and
kept in a wide mouthed bottle.
A known quantity of dilute arsenic solution in water
and stannated HCl (arsenic free) is kept in wide
mouthed bottle.
1 g of KI 1 g of KI
5 ml of stannous chloride acid solution 5 ml of stannous chloride acid solution
10 g of granulated zinc is added (all this reagents
must be arsenic free). Close the cork immediately
than place bottle in water bath at 40 C for 40 min
10 g of granulated zinc is added (all this reagents
must be arsenic free). Close the cork immediately
than place bottle in water bath at 40 C for 40 min
Compare the yellow stain on MgCl2 paper Compare the yellow stain on MgCl2 paper
20. • Stain obtained on mercuric chloride paper is compared with standard solution.
Standard stain must be freshly prepared as it fades on keeping.
• Inference: If the stain produced by the test is not deeper than the standard stain,
then sample complies with the limit test for Arsenic.
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 paper are used to trap any hydrogen sulphide which may be evolved
along with arsine.
21. • Use of stannated Hydrochloric acid:
• If pure zinc and HCl are used, the steady evolution of gas does not occur. This
produces improper stain (e.g slow evolution produces short but intense stain
while rapid evolution of gas produces long but diffused stain.)
• So, to get steady evolution of gas, stannated hydrochloric acid is used.
• Use of Lead Acetate solution:
• H2S gas may be formed during the experiment as zinc contains sulphides as
impurities. It gives black stain to HgCl2 paper and so will interfere the test.
• Hence, gases evolved are passed through cotton wool plug moistened with
lead acetate, where H2S gas is trapped as PbS.
• Use of Potassium iodide:
• KI is converted to HI which brings about reduction of unreacted pentavalent
arsenic to trivalent Arsenic. Thus, reproducible results can be obtained. If it is
not used then some pentavalent Arsenic may remain unreacted.
22. Limit test for IRON:
• Limit test of Iron is based on the reaction of iron in ammonical solution with
thioglycollic acid in presence of citric acid to form iron thioglycolate (Ferrous
thioglycolate complex) which produces pale pink to deep reddish purple color
in alkaline media.
• Thioglycolic acid is used as reducing agent.
23. • The color of the Ferrous thioglycolate complex fades in the presence of air
due to oxidation.
• Also, the color is destroyed in presence of oxidizing agents and strong
alkalis.
• The purple color is developed only in alkaline media. So ammonia
solution is used.
• But ammonia reacts with iron, forms precipitate of ferrous hydroxide.
• Thus citric acid is used which prevents the precipitate of iron with
Ammonia by forming a complex with iron as iron citrate.
24. Procedure:
Test sample Standard compound
Sample is dissolved in specific amount
of water and then volume is made up to 40 ml
2 ml of standard solution of iron diluted (0.173
with water upto 40 ml (0.173gm ferric ammonium
sulphate +1.5 ml HCl Volume make upto 1000ml
with distelled water)
Add 2 ml of 20 % w/v of citric acid
(iron free)
Add 2 ml of 20 % w/v of citric acid
(iron free)
Add 2 drops of thioglycollic acid Add 2 drops of thioglycollic acid
Add ammonia to make the solution
alkaline and adjust the volume upto 50 ml with
distilled water.
Add ammonia to make the solution
alkaline and adjust the volume upto 50 ml with
distilled water.
Keep aside for 5 min Keep aside for 5 min
Color developed is viewed vertically
and compared with standard solution
Color developed is viewed vertically
and compared with standard solution
Note: All the reagents used in the limit test for Iron should themselves be iron free.
25. • Observation:
• The purple color produce in sample solution should not be greater than standard solution. If
purple color produces in sample solution is less than the standard solution, the sample will
pass the limit test of iron and vice versa.
Reasons:
• Citric acid forms complex with metal cation and helps precipitation of iron by ammonia by
forming a complex with it.
• Thioglycolic acid helps to oxidize iron (II) to iron (III).
• Ammonia is added to make solution alkaline. The pale pink color is visible only in the
alkaline media. The color is not visible in acidic media as ferrous thioglycolate complex
decomposes in high acidic media.
26. 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
should not exceed the heavy metal limits given under the individual monograph.
• 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
• In substances the proportion of any such impurity (Heavy metals) has been expressed as
the quantity of lead required to produce a color of equal depth as in a standard comparison
solution having a definite quantity of lead nitrate.
27. • Principle: It based upon the reaction between metallic impurities with
hydrogen sulphide in acidic medium it formed the brownish coloured
solution.
• Metal that response the limit test lead, mercury, bismuth, silver, copper etc
2 M + H2S---------------------M2S + H
Metal impurity
• Example:
Copper 2 Cu + H2S --------------- Cu2S + H
Acidic media +
+
Acidic media
+ +
28. • The quantity is stated as the heavy metal limit and is expressed as parts of
lead (by weight) per million parts of the test substance.
• The limit test for heavy metals has been based upon the reaction of the
metal ion with hydrogen sulphide, under the prescribed conditions of the
test causing the formation of metal sulphides.
• These remain distributed in colloidal state, and give rise to a brownish
coloration.
• 2 M + H2S---------------------M2S + H
Metal Hydrogen sulphide
impurity
Acidic media
+ +
29. • I.P limit for heavy metals in 20 ppm.
• The test solution is compared with a standard prepared using a lead solution (as the heavy
metal).The metallic impurities in substance are expressed as parts of lead per million parts
of substance.
• IP has adopted 3 methods for this:
• Method I: The method is applicable for the samples which give clear colourless solutions
under specified conditions of test.
• Method II: The method is applicable for the samples which DO NOT give clear colourless
solutions under specified conditions of test.
• Method III: Used for substances which give clear colourless solutions in sodium hydroxide
medium.
30. Test solution Standard solution
Specified amount of sample with
25 ml water dissolve.
2ml standard lead solution (20ppm)
25 ml water dissolve
Adjust the pH 3 to 4 Adjust the pH 3 to 4
Dilute up to 35 ml water and mix Dilute up to 35 ml water and mix
10 ml H2S solution add again
dilute upto 50 ml
10 ml H2S solution add again
dilute upto 50 ml
Mix the solution darkness observed
white background
Mix the solution darkness observed
white background
31. Limit test for lead:
• Lead is a most undesirable impurity in medical compounds and comes
through use of sulphuric acid, lead lined apparatus and glass bottles use for
storage of chemicals.
• Principle:
• Limit test of lead is based on the reaction of lead and diphenyl thiocabazone
(dithizone) in alkaline solution to form lead dithizone complex which is red in
color.
32. • Dithizone in chloroform, is able to extract lead from alkaline aqueous
solutions as a lead complex (Red in colour)
• The original dithizone is having a green colour in chloroform while the
lead-dithizone is having a violet color. So, resulting color at the end of the
process is red.
33. • The intensity of the color of complex is dependant upon the amount of lead in
• the solution.
• The color of the lead-dithizone complex in chloroform has been compared with a
• standard volume of lead solution, treated in the same manner.
• In this method, the lead present as an impurity in the substances, gets separated by
• extracting an alkaline solution with a dithizone extraction solution.
• The interference and influence of the other metal ions has been eliminated by
adjusting the optimum pH for the extraction by employing Ammonium citrate/
potassium cyanide.
34. Method:
• Sample solution is transferred to a separating funnel.
• To it 6 ml of ammonium citrate, 2 ml potassium cyanide and 2 ml of hydroxalamine HCl are
added.
• 2 drops of phenol red
• Solution is made alkaline by adding ammonia solution.
• This is then extracted with 5 ml portions of dithizone solution until it becomes green.
• The combined dithizone extracts are shaken for 30 min with 30 ml of nitric acid and chloroform
layer is discarded.
• To the acid solution 5 ml of standard dithizone solution is added and 4 ml ammonium cyanide
and solution is shaken for 30 sec.
• Similarly prepare standard.
35. Observation:
• The intensity of the color of complex, is depends on the amount of lead in
the solution. The color produced in sample solution should not be greater
than standard solution. If color produces in sample solution is less than the
standard solution, the sample will pass the limit test of lead and vice versa.
Reasons:
• Ammonium citrate, potassium cyanide, hydroxylamine hydrochloride is
used to make pH optimum so interference and influence of other impurities
have been eliminated.
• Phenol red is used as indicator to develop the color at the end of process
Lead present as an impurities in the substance, gets separated by extracting
an alkaline solution with a dithizone extraction solution.
36. TEST SOLUTION STANDARD SOLUTION
A known quantity of sample solution is
transferred in a separating funnel
A standard lead solution is prepared equivalent to
the amount of lead permitted in the sample under
examination
Add 6ml of ammonium citrate Add 6ml of ammonium citrate
Add 2 ml of potassium cyanide and 2 ml of
hydroxylamine hydrochloride
Add 2 ml of potassium cyanide and 2 ml of
hydroxylamine hydrochloride
Add 2 drops of phenol red Add 2 drops of phenol red
Make solution alkaline by adding ammonia solution. Make solution alkaline by adding ammonia solution.
Extract with 5 ml of dithizone until it becomes green Extract with 5 ml of dithizone until it becomes green
Combine dithizone extracts are shaken for 30 mins
with 30 ml of nitric acid and the chloroform layer is
discarded
Combine dithizone extracts are shaken for 30 mins
with 30 ml of nitric acid and the chloroform layer is
discarded
To the acid solution add 5 ml of standard dithizone
solution
To the acid solution add 5 ml of standard dithizone
solution
Add 4 ml of ammonium cyanide Add 4 ml of ammonium cyanide
Shake for 30 mins Shake for 30 mins
Observe the colour Observe the colour
37. • Aq. Ammonia is added in limit test of lead:
• Pb+ S ------------ PbS
• In limit test of lead, PbS is produced by addition of standard H2S , to the
solution containing lead.
• pH 3-4 is necessary for the precipitation of PbS. So aq. Ammonia /acetic acid
is added to maintain that pH.
38. Modified limit test for Chlorides
• Depending upon the nature of the substance, some modifications have to be
adopted for the preparation of the solution.
Principle:
The limit test for chloride based on the reaction between soluble chloride
impurities present in the substance and silver nitrate solution to give white
precipitates of silver chloride.
These white precipitates are insoluble in dilute nitric acid and hence give
turbidity or opalescence to the test solution.
39. The extent of the turbidity produced depends upon the amount of the chloride
present in the substance which is compared with a standard opalescence produce
by addition of silver nitrate to a standard solution having known amount of
chloride and the same volume of the dilute nitric acid as the use in the test
solution.
If the turbidity developed in the sample is less than the standard turbidity, the
sample passes the limit test for chloride and vice-versa.
As potassium permanganate gives purple color aqueous solution that interferes in
the comparison of opalescence or turbidity, therefore the aqueous solution must
first be decolorized. Potassium permanganate is oxidizing agent while ethanol is
reducing agent.
40. • When potassium permanganate solution is treated with ethanol in presence of
heat the redox reaction will take place, i.e. potassium permanganate gets
reduced to manganese dioxide (precipitates). The filtrate of the reaction is
colorless that is subjected to proceed for limit test for chloride.
Chemical Reaction:
2 KMnO4 + 3 C2H5OH-----------------2MnO2 + 2 KOH + 2 CH3CHO + 2 H2O
Coloured compound------------------- Colourless compound
Basic Reaction
Cl- + AgNO3 --------------------------AgCl + NO3-
Redox reaction
41. • Preparation of Test solution (KMnO4) : Dissolve 1.5 gm KMnO4 in 50 ml distilled water
(purple colour) heat on water bath slowly added 6ml of (95%) ethanol and cool the solution
then dilute with 60 ml distilled water and filter it------ gives ( colourless solution)
• Compare the turbidity or opalescence produced in test solution with respect to
standard solution and report the result and conclusion.
TEST SOLUTION STANDARD SOLUTION
Specified amount Transfer the prepared test
solution in Nessler’s cylinder
Take 10 ml chloride standard solution (25
ppm chloride) and add 5 ml water in a
Nessler’s cylinder.
Add 10 ml of dilute nitric acid and dilute to
50 ml with distilled water
Add 10 ml of dilute nitric acid and dilute to
50 ml with distilled water
Add 1ml of 0.1 M silver nitrate solution and
stir immediately with glass rod and allow
standing for 5 minutes protected from light.
Add 1ml of 0.1 M silver nitrate solution and
stir immediately with glass rod and allow
standing for 5 minutes protected from light.
42. • Observation and conclusion will be of two types:
• If the intensity of turbidity or opalescence appears to be more in test solution
than the standard solution then conclusion is impurities of chloride in given
sample is over the limit as per IP’96. Hence, sample do not passes the limit
test for chlorides.
• If the intensity turbidity or opalescence appears to be less or equal in test
solution than the standard solution then conclusion is impurities of chloride
in given sample is under the limit as per IP’96. Hence, sample passes the
limit test for chloride
43. Principle:
• 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.
• Then comparison of turbidity is done with a standard turbidity obtained from a known amount of
Sulphate and same volume of dilute Hydrochloric acid have been added to both solutions.
• The barium chloride test solution in the IP has been replaced by Barium sulphate reagent which is
having barium chloride, sulphate free alcohol and a solution of potassium sulphate. Potassium
sulphate has been added to increase the sensitivity of the test.
Modified limit test for Sulphate
44. • As potassium permanganate gives purple color aqueous solution that interferes
in the comparison of opalescence or turbidity, therefore the aqueous solution
must first be decolorized. Potassium permanganate is oxidizing agent while
ethanol is reducing agent.
• When potassium permanganate solution is treated with ethanol in presence of
heat the redox reaction will take place, i.e. potassium permanganate gets
reduced to manganese dioxide (precipitates). The filtrate of the reaction is
colorless that is subjected to proceed for limit test for chloride.
Chemical Reaction:
2 KMnO4 + 3 C2H5OH-----------------2MnO2 + 2 KOH + 2 CH3CHO + 2 H2O
Coloured compound------------------- Colourless compound
45. • Preparation of Test solution (KMnO4) : Dissolve 1.5 gm KMnO4 in 50 ml distilled water
(purple colour) heat on water bath slowly added 6ml of (95%) ethanol and cool the
solution then dilute up to 60 ml with distilled water and filter it------ gives ( colourless
solution)
• Compare the turbidity or opalescence produced in test solution with respect to
standard solution and report the result and conclusion.
TEST SOLUTION STANDARD SOLUTION
Specified amount Transfer the prepared test
solution (40ml) in Nessler’s cylinder
Take 1ml of 0.1089% w/v K2SO4.
Add 2ml of dilute HCl/ acetic acid and
dilute to 50 ml with distilled water
Add 2ml of dilute HCl/ acetic acid and
dilute to 50 ml with distilled water.
Add 5ml of BaSO4 reagent and stir
immediately with glass rod and allow
standing for 5 minutes protected from light.
Add 5ml of BaSO4 reagent and stir
immediately with glass rod and allow
standing for 5 minutes protected from light.
46. • Observation and conclusion will be of two types:
• If the intensity of turbidity or opalescence appears to be more in test
solution than the standard solution then conclusion is impurities of sulphate
in given sample is over the limit as per IP’96. Hence, sample do not passes
the limit test for sulphate.
• If the intensity turbidity or opalescence appears to be less or equal in test
solution than the standard solution then conclusion is impurities of sulphate
in given sample is under the limit as per IP’96. Hence, sample passes the
limit test for sulphate.