Importance of instrumental Analysis

Presented By

Mr N P Badgujar

Obtaining information in diverse areas of science andtechnology

A modern well-educated scientist is one who is capableof solving problems with an analytical approach and whocan apply modern instrumentation to problems

1) Fundamental principles of instrumental measurements

2)Applications of these principles to specific types ofchemical measurements (types of samples analyzedfigures of merit strengths and limitations)

3) Examples of modern instrumentation

4) Use of instruments to solve real analytical problem

Importance of instrumental methods in conjunctions with conventional analytical methods

What is the the difference between an analytical technique and an analytical method

------------------------------------------------------------------------------------------

Analytical technique is considered to be a fundamental scientificphenomenon that has been found to be useful to provide informationabout the composition of a substance

An analytical method involves the use of an analytical techniqueoperated within specific and appropriate measurement parameters

--------------------------------------------------------------------------------------------------

Differentiate the terms procedure and protocol

PROCEDURE represents a set of written instructions for carrying outthe steps of an analytical method Organizations such as the AmericanSociety for Testing Materials (ASTM)

PROTOCOL contains a much more rigidly defined description of the steps of the analytical method Generally a protocol is used to meet the demands of a government regulatory agency or to provide information for legal purposes

Terms instrument and machine are important to clarify

INSTRUMENT A measuring device for determining the presentvalue of a quantity under observation

MACHINE should be reserved for use in describing a device usedto perform work or change the direction of motion of an object

Instruments may often contain components that are machines butultimately the instrument has the purpose of making a chemicalmeasurement and should be recognized accordingly

Methods of Chemical Analysis

The objective of a chemical analysis whether the measurement isperformed using classical (wet chemical) or instrumental methodsis to provide information in order to solve a problem or to make adecision

Instruments are important but solid scientific proceduresthroughout a method of analysis are necessary in order toproduce valid

A scientistrsquos role in a method of analysis is more thanunderstanding and making measurements

Designing a method of analysis appropriate to the problemrequires experience broad knowledge and the problem solvingskills

The analyst must deal with the nature and origin of the samplethe desired accuracy and precision limitations in costs and timefor the analysis and the selection of appropriate techniques

Significant interactions with collaborating investigators aretypically required not only for the analyst to acquire thenecessary information to solve the problem

To communicate the information that can realistically beprovided given the nature of the sample and measurementtechniques available

When the concepts of quality are applied to a chemicalmeasurement the term quality assurance is more commonlyused

Quality assurance in a chemical measurement involves theactions within the method of analysis that provide satisfactorymeasurements with appropriate confidence high dependabilityand in a cost-effective manner

Define the Problem

The intent of the measurement

The necessary considerations in sampling and sample preparation

The best technique for making the measurement

Evaluation of the data

Reporting the results

The resources needed to accomplish the analysis

The method chosen may provide either qualitative or quantitativeinformation

Qualitative method data may include the composition oxidationstates structural information or the isotopic distributions ofelements contained in a sample

An understanding of the instrumentation used to make thequalitative measurement also leads one to a rough approximation ofthe concentration of the species being measured

Whether the substance is a major (gt1) minor (001-1) trace (10-2 ndash 10-6) or ultra-trace (10-6- 10-9) component

Quantitative methods the analyst needs to plan tasks associatedwith sampling sample preparation and calibration moremeticulously than a qualitative analysis

Often preliminary measurements will be required to develop aquantitative method

bull A careful consideration of the analyte sample andinstrumentation are critical in the development of a validinstrumental method

Properties of the sample

Analyte properties

Anticipated concentration range of the analyte

Sample preparation

Desired precision

Desired accuracy

ConcomitantsInterferents

Existing methods

Method Modeling and Plan

The model is an idealized representation of the complex steps ofthe analytical method

It includes a specific statement of the problem information aboutthe sample and analyte (concentration levels of concern potentialinterferences location of the analyte in the sample phaserelationships particle size distributionhellip)

bull The development of a model may require experiments to obtainmore information about the sample or to validate assumptions

It necessary to perform measurements on the sample todetermine its homogeneity

Development of a sampling plan to accurately address the goalsof the method

The results of these preliminary experiments are used to helprefine the original model

bull After establishment of the model a plan must be created toprovide specific directions for each step in the method

bull The plan translates the model into standard operating procedureswhich provide the actions and reviews necessary to complete theanalysis with the necessary precision and accuracy

EXProposed Research Work i Project Title ii Introduction bull Origin of the research problem bull Interdisciplinary relevance bull Review of Research and Development in the Subject

1048708 International status 1048708 National Status 1048708 Significance of the study

(iii) Objectives (iv) Methodology (v) Year-wise Plan of work and targets to be achieve

Obtain and Store the Sample Expert knowledge in the mechanics of instrumental measurements is a critical

aspect in the role of an analyst however it is insufficient in gaining accurateand precise results

Proper consideration of the sampling and sample handling are equallyimportant

Even with the best quality instrumental measurement a poorly selected orimproperly handled sample will give erroneous or inappropriate results

Sample Preparation

The samples must also be treated to make them compatible withthe instrumental technique

Transformation of the sample into a form that can be measuredusing the selected technique is termed sample preparation

Sample selection and preparation usually represent the largestinvestment of time in the implementation of an analytical method

It is important to realize that the majority of instrumentaltechniques require the sample to be in a liquid phase

For solid samples several techniques are taken to transfer theanalyte into the liquid phase

Care must be taken in these steps to preserve the integrity of theanalyte by considering the possibility of contamination loss orchemical and physical changes to the analyte

Perform Measurements

Once the sample has been prepared it is necessary to measurereplicate samples to establish the precision of the method

The measurement depends upon the interaction of the techniquewith a unique chemical or physical property of the analyte

Consider the example involving the use of IR spectrophotometryto measure the residual styrene and acrylonitrile monomersremaining in a copolymer sample

The measurement relies on the fact that the aromatic carbon-carbon bonds in the styrene monomer absorb infrared radiation atapproximately 1600 cm-1 while the cyano group of theacrylonitrile monomer absorbs at 2275 cm-1

An accurate analysis will assure minimal or no absorbance of thestyrene monomer at the frequency of the acrylonitrile monomer

Compare Results with Standards

Reliable and convincing analytical results must involve a propercareful comparison of the analytersquos signal to that of appropriatestandards of known analyte concentration as well as a calibrationblank solution This is known as calibration or standardization

Calibration establishes the mathematical relationship between theanalytical signal and the concentration of analyte in the calibrationstandards The most common approach is to develop a ldquoworkingrdquocurve

Obtaining information in diverse areas of science andtechnology

A modern well-educated scientist is one who is capableof solving problems with an analytical approach and whocan apply modern instrumentation to problems

1) Fundamental principles of instrumental measurements

2)Applications of these principles to specific types ofchemical measurements (types of samples analyzedfigures of merit strengths and limitations)

3) Examples of modern instrumentation

4) Use of instruments to solve real analytical problem

Importance of instrumental methods in conjunctions with conventional analytical methods

What is the the difference between an analytical technique and an analytical method

------------------------------------------------------------------------------------------

Analytical technique is considered to be a fundamental scientificphenomenon that has been found to be useful to provide informationabout the composition of a substance

An analytical method involves the use of an analytical techniqueoperated within specific and appropriate measurement parameters

--------------------------------------------------------------------------------------------------

Differentiate the terms procedure and protocol

PROCEDURE represents a set of written instructions for carrying outthe steps of an analytical method Organizations such as the AmericanSociety for Testing Materials (ASTM)

PROTOCOL contains a much more rigidly defined description of the steps of the analytical method Generally a protocol is used to meet the demands of a government regulatory agency or to provide information for legal purposes

Terms instrument and machine are important to clarify

INSTRUMENT A measuring device for determining the presentvalue of a quantity under observation

MACHINE should be reserved for use in describing a device usedto perform work or change the direction of motion of an object

Instruments may often contain components that are machines butultimately the instrument has the purpose of making a chemicalmeasurement and should be recognized accordingly

Methods of Chemical Analysis

The objective of a chemical analysis whether the measurement isperformed using classical (wet chemical) or instrumental methodsis to provide information in order to solve a problem or to make adecision

Instruments are important but solid scientific proceduresthroughout a method of analysis are necessary in order toproduce valid

A scientistrsquos role in a method of analysis is more thanunderstanding and making measurements

Designing a method of analysis appropriate to the problemrequires experience broad knowledge and the problem solvingskills

The analyst must deal with the nature and origin of the samplethe desired accuracy and precision limitations in costs and timefor the analysis and the selection of appropriate techniques

Significant interactions with collaborating investigators aretypically required not only for the analyst to acquire thenecessary information to solve the problem

To communicate the information that can realistically beprovided given the nature of the sample and measurementtechniques available

When the concepts of quality are applied to a chemicalmeasurement the term quality assurance is more commonlyused

Quality assurance in a chemical measurement involves theactions within the method of analysis that provide satisfactorymeasurements with appropriate confidence high dependabilityand in a cost-effective manner

Define the Problem

The intent of the measurement

The necessary considerations in sampling and sample preparation

The best technique for making the measurement

Evaluation of the data

Reporting the results

The resources needed to accomplish the analysis

The method chosen may provide either qualitative or quantitativeinformation

Qualitative method data may include the composition oxidationstates structural information or the isotopic distributions ofelements contained in a sample

An understanding of the instrumentation used to make thequalitative measurement also leads one to a rough approximation ofthe concentration of the species being measured

Whether the substance is a major (gt1) minor (001-1) trace (10-2 ndash 10-6) or ultra-trace (10-6- 10-9) component

Quantitative methods the analyst needs to plan tasks associatedwith sampling sample preparation and calibration moremeticulously than a qualitative analysis

Often preliminary measurements will be required to develop aquantitative method

bull A careful consideration of the analyte sample andinstrumentation are critical in the development of a validinstrumental method

Properties of the sample

Analyte properties

Anticipated concentration range of the analyte

Sample preparation

Desired precision

Desired accuracy

ConcomitantsInterferents

Existing methods

Method Modeling and Plan

The model is an idealized representation of the complex steps ofthe analytical method

It includes a specific statement of the problem information aboutthe sample and analyte (concentration levels of concern potentialinterferences location of the analyte in the sample phaserelationships particle size distributionhellip)

bull The development of a model may require experiments to obtainmore information about the sample or to validate assumptions

It necessary to perform measurements on the sample todetermine its homogeneity

Development of a sampling plan to accurately address the goalsof the method

The results of these preliminary experiments are used to helprefine the original model

bull After establishment of the model a plan must be created toprovide specific directions for each step in the method

bull The plan translates the model into standard operating procedureswhich provide the actions and reviews necessary to complete theanalysis with the necessary precision and accuracy

EXProposed Research Work i Project Title ii Introduction bull Origin of the research problem bull Interdisciplinary relevance bull Review of Research and Development in the Subject

1048708 International status 1048708 National Status 1048708 Significance of the study

(iii) Objectives (iv) Methodology (v) Year-wise Plan of work and targets to be achieve

Obtain and Store the Sample Expert knowledge in the mechanics of instrumental measurements is a critical

aspect in the role of an analyst however it is insufficient in gaining accurateand precise results

Proper consideration of the sampling and sample handling are equallyimportant

Even with the best quality instrumental measurement a poorly selected orimproperly handled sample will give erroneous or inappropriate results

Sample Preparation

The samples must also be treated to make them compatible withthe instrumental technique

Transformation of the sample into a form that can be measuredusing the selected technique is termed sample preparation

Sample selection and preparation usually represent the largestinvestment of time in the implementation of an analytical method

It is important to realize that the majority of instrumentaltechniques require the sample to be in a liquid phase

For solid samples several techniques are taken to transfer theanalyte into the liquid phase

Care must be taken in these steps to preserve the integrity of theanalyte by considering the possibility of contamination loss orchemical and physical changes to the analyte

Perform Measurements

Once the sample has been prepared it is necessary to measurereplicate samples to establish the precision of the method

The measurement depends upon the interaction of the techniquewith a unique chemical or physical property of the analyte

Consider the example involving the use of IR spectrophotometryto measure the residual styrene and acrylonitrile monomersremaining in a copolymer sample

The measurement relies on the fact that the aromatic carbon-carbon bonds in the styrene monomer absorb infrared radiation atapproximately 1600 cm-1 while the cyano group of theacrylonitrile monomer absorbs at 2275 cm-1

An accurate analysis will assure minimal or no absorbance of thestyrene monomer at the frequency of the acrylonitrile monomer

Compare Results with Standards

Reliable and convincing analytical results must involve a propercareful comparison of the analytersquos signal to that of appropriatestandards of known analyte concentration as well as a calibrationblank solution This is known as calibration or standardization

Calibration establishes the mathematical relationship between theanalytical signal and the concentration of analyte in the calibrationstandards The most common approach is to develop a ldquoworkingrdquocurve

What is the the difference between an analytical technique and an analytical method

------------------------------------------------------------------------------------------

Analytical technique is considered to be a fundamental scientificphenomenon that has been found to be useful to provide informationabout the composition of a substance

An analytical method involves the use of an analytical techniqueoperated within specific and appropriate measurement parameters

--------------------------------------------------------------------------------------------------

Differentiate the terms procedure and protocol

PROCEDURE represents a set of written instructions for carrying outthe steps of an analytical method Organizations such as the AmericanSociety for Testing Materials (ASTM)

PROTOCOL contains a much more rigidly defined description of the steps of the analytical method Generally a protocol is used to meet the demands of a government regulatory agency or to provide information for legal purposes

Terms instrument and machine are important to clarify

INSTRUMENT A measuring device for determining the presentvalue of a quantity under observation

MACHINE should be reserved for use in describing a device usedto perform work or change the direction of motion of an object

Instruments may often contain components that are machines butultimately the instrument has the purpose of making a chemicalmeasurement and should be recognized accordingly

Methods of Chemical Analysis

The objective of a chemical analysis whether the measurement isperformed using classical (wet chemical) or instrumental methodsis to provide information in order to solve a problem or to make adecision

Instruments are important but solid scientific proceduresthroughout a method of analysis are necessary in order toproduce valid

A scientistrsquos role in a method of analysis is more thanunderstanding and making measurements

Designing a method of analysis appropriate to the problemrequires experience broad knowledge and the problem solvingskills

The analyst must deal with the nature and origin of the samplethe desired accuracy and precision limitations in costs and timefor the analysis and the selection of appropriate techniques

Significant interactions with collaborating investigators aretypically required not only for the analyst to acquire thenecessary information to solve the problem

To communicate the information that can realistically beprovided given the nature of the sample and measurementtechniques available

When the concepts of quality are applied to a chemicalmeasurement the term quality assurance is more commonlyused

Quality assurance in a chemical measurement involves theactions within the method of analysis that provide satisfactorymeasurements with appropriate confidence high dependabilityand in a cost-effective manner

Define the Problem

The intent of the measurement

The necessary considerations in sampling and sample preparation

The best technique for making the measurement

Evaluation of the data

Reporting the results

The resources needed to accomplish the analysis

The method chosen may provide either qualitative or quantitativeinformation

Qualitative method data may include the composition oxidationstates structural information or the isotopic distributions ofelements contained in a sample

An understanding of the instrumentation used to make thequalitative measurement also leads one to a rough approximation ofthe concentration of the species being measured

Whether the substance is a major (gt1) minor (001-1) trace (10-2 ndash 10-6) or ultra-trace (10-6- 10-9) component

Quantitative methods the analyst needs to plan tasks associatedwith sampling sample preparation and calibration moremeticulously than a qualitative analysis

Often preliminary measurements will be required to develop aquantitative method

bull A careful consideration of the analyte sample andinstrumentation are critical in the development of a validinstrumental method

Properties of the sample

Analyte properties

Anticipated concentration range of the analyte

Sample preparation

Desired precision

Desired accuracy

ConcomitantsInterferents

Existing methods

Method Modeling and Plan

The model is an idealized representation of the complex steps ofthe analytical method

It includes a specific statement of the problem information aboutthe sample and analyte (concentration levels of concern potentialinterferences location of the analyte in the sample phaserelationships particle size distributionhellip)

bull The development of a model may require experiments to obtainmore information about the sample or to validate assumptions

It necessary to perform measurements on the sample todetermine its homogeneity

Development of a sampling plan to accurately address the goalsof the method

The results of these preliminary experiments are used to helprefine the original model

bull After establishment of the model a plan must be created toprovide specific directions for each step in the method

bull The plan translates the model into standard operating procedureswhich provide the actions and reviews necessary to complete theanalysis with the necessary precision and accuracy

EXProposed Research Work i Project Title ii Introduction bull Origin of the research problem bull Interdisciplinary relevance bull Review of Research and Development in the Subject

1048708 International status 1048708 National Status 1048708 Significance of the study

(iii) Objectives (iv) Methodology (v) Year-wise Plan of work and targets to be achieve

Obtain and Store the Sample Expert knowledge in the mechanics of instrumental measurements is a critical

aspect in the role of an analyst however it is insufficient in gaining accurateand precise results

Proper consideration of the sampling and sample handling are equallyimportant

Even with the best quality instrumental measurement a poorly selected orimproperly handled sample will give erroneous or inappropriate results

Sample Preparation

The samples must also be treated to make them compatible withthe instrumental technique

Transformation of the sample into a form that can be measuredusing the selected technique is termed sample preparation

Sample selection and preparation usually represent the largestinvestment of time in the implementation of an analytical method

It is important to realize that the majority of instrumentaltechniques require the sample to be in a liquid phase

For solid samples several techniques are taken to transfer theanalyte into the liquid phase

Care must be taken in these steps to preserve the integrity of theanalyte by considering the possibility of contamination loss orchemical and physical changes to the analyte

Perform Measurements

Once the sample has been prepared it is necessary to measurereplicate samples to establish the precision of the method

The measurement depends upon the interaction of the techniquewith a unique chemical or physical property of the analyte

Consider the example involving the use of IR spectrophotometryto measure the residual styrene and acrylonitrile monomersremaining in a copolymer sample

The measurement relies on the fact that the aromatic carbon-carbon bonds in the styrene monomer absorb infrared radiation atapproximately 1600 cm-1 while the cyano group of theacrylonitrile monomer absorbs at 2275 cm-1

An accurate analysis will assure minimal or no absorbance of thestyrene monomer at the frequency of the acrylonitrile monomer

Compare Results with Standards

Reliable and convincing analytical results must involve a propercareful comparison of the analytersquos signal to that of appropriatestandards of known analyte concentration as well as a calibrationblank solution This is known as calibration or standardization

Calibration establishes the mathematical relationship between theanalytical signal and the concentration of analyte in the calibrationstandards The most common approach is to develop a ldquoworkingrdquocurve

Terms instrument and machine are important to clarify

INSTRUMENT A measuring device for determining the presentvalue of a quantity under observation

MACHINE should be reserved for use in describing a device usedto perform work or change the direction of motion of an object

Instruments may often contain components that are machines butultimately the instrument has the purpose of making a chemicalmeasurement and should be recognized accordingly

Methods of Chemical Analysis

The objective of a chemical analysis whether the measurement isperformed using classical (wet chemical) or instrumental methodsis to provide information in order to solve a problem or to make adecision

Instruments are important but solid scientific proceduresthroughout a method of analysis are necessary in order toproduce valid

A scientistrsquos role in a method of analysis is more thanunderstanding and making measurements

Designing a method of analysis appropriate to the problemrequires experience broad knowledge and the problem solvingskills

The analyst must deal with the nature and origin of the samplethe desired accuracy and precision limitations in costs and timefor the analysis and the selection of appropriate techniques

Significant interactions with collaborating investigators aretypically required not only for the analyst to acquire thenecessary information to solve the problem

To communicate the information that can realistically beprovided given the nature of the sample and measurementtechniques available

When the concepts of quality are applied to a chemicalmeasurement the term quality assurance is more commonlyused

Quality assurance in a chemical measurement involves theactions within the method of analysis that provide satisfactorymeasurements with appropriate confidence high dependabilityand in a cost-effective manner

Define the Problem

The intent of the measurement

The necessary considerations in sampling and sample preparation

The best technique for making the measurement

Evaluation of the data

Reporting the results

The resources needed to accomplish the analysis

The method chosen may provide either qualitative or quantitativeinformation

Qualitative method data may include the composition oxidationstates structural information or the isotopic distributions ofelements contained in a sample

An understanding of the instrumentation used to make thequalitative measurement also leads one to a rough approximation ofthe concentration of the species being measured

Whether the substance is a major (gt1) minor (001-1) trace (10-2 ndash 10-6) or ultra-trace (10-6- 10-9) component

Quantitative methods the analyst needs to plan tasks associatedwith sampling sample preparation and calibration moremeticulously than a qualitative analysis

Often preliminary measurements will be required to develop aquantitative method

bull A careful consideration of the analyte sample andinstrumentation are critical in the development of a validinstrumental method

Properties of the sample

Analyte properties

Anticipated concentration range of the analyte

Sample preparation

Desired precision

Desired accuracy

ConcomitantsInterferents

Existing methods

Method Modeling and Plan

The model is an idealized representation of the complex steps ofthe analytical method

It includes a specific statement of the problem information aboutthe sample and analyte (concentration levels of concern potentialinterferences location of the analyte in the sample phaserelationships particle size distributionhellip)

bull The development of a model may require experiments to obtainmore information about the sample or to validate assumptions

It necessary to perform measurements on the sample todetermine its homogeneity

Development of a sampling plan to accurately address the goalsof the method

The results of these preliminary experiments are used to helprefine the original model

bull After establishment of the model a plan must be created toprovide specific directions for each step in the method

bull The plan translates the model into standard operating procedureswhich provide the actions and reviews necessary to complete theanalysis with the necessary precision and accuracy

EXProposed Research Work i Project Title ii Introduction bull Origin of the research problem bull Interdisciplinary relevance bull Review of Research and Development in the Subject

1048708 International status 1048708 National Status 1048708 Significance of the study

(iii) Objectives (iv) Methodology (v) Year-wise Plan of work and targets to be achieve

Obtain and Store the Sample Expert knowledge in the mechanics of instrumental measurements is a critical

aspect in the role of an analyst however it is insufficient in gaining accurateand precise results

Proper consideration of the sampling and sample handling are equallyimportant

Even with the best quality instrumental measurement a poorly selected orimproperly handled sample will give erroneous or inappropriate results

Sample Preparation

The samples must also be treated to make them compatible withthe instrumental technique

Transformation of the sample into a form that can be measuredusing the selected technique is termed sample preparation

Sample selection and preparation usually represent the largestinvestment of time in the implementation of an analytical method

It is important to realize that the majority of instrumentaltechniques require the sample to be in a liquid phase

For solid samples several techniques are taken to transfer theanalyte into the liquid phase

Care must be taken in these steps to preserve the integrity of theanalyte by considering the possibility of contamination loss orchemical and physical changes to the analyte

Perform Measurements

Once the sample has been prepared it is necessary to measurereplicate samples to establish the precision of the method

The measurement depends upon the interaction of the techniquewith a unique chemical or physical property of the analyte

Consider the example involving the use of IR spectrophotometryto measure the residual styrene and acrylonitrile monomersremaining in a copolymer sample

The measurement relies on the fact that the aromatic carbon-carbon bonds in the styrene monomer absorb infrared radiation atapproximately 1600 cm-1 while the cyano group of theacrylonitrile monomer absorbs at 2275 cm-1

An accurate analysis will assure minimal or no absorbance of thestyrene monomer at the frequency of the acrylonitrile monomer

Compare Results with Standards

Reliable and convincing analytical results must involve a propercareful comparison of the analytersquos signal to that of appropriatestandards of known analyte concentration as well as a calibrationblank solution This is known as calibration or standardization

Calibration establishes the mathematical relationship between theanalytical signal and the concentration of analyte in the calibrationstandards The most common approach is to develop a ldquoworkingrdquocurve

Methods of Chemical Analysis

The objective of a chemical analysis whether the measurement isperformed using classical (wet chemical) or instrumental methodsis to provide information in order to solve a problem or to make adecision

Instruments are important but solid scientific proceduresthroughout a method of analysis are necessary in order toproduce valid

A scientistrsquos role in a method of analysis is more thanunderstanding and making measurements

Designing a method of analysis appropriate to the problemrequires experience broad knowledge and the problem solvingskills

The analyst must deal with the nature and origin of the samplethe desired accuracy and precision limitations in costs and timefor the analysis and the selection of appropriate techniques

Significant interactions with collaborating investigators aretypically required not only for the analyst to acquire thenecessary information to solve the problem

To communicate the information that can realistically beprovided given the nature of the sample and measurementtechniques available

When the concepts of quality are applied to a chemicalmeasurement the term quality assurance is more commonlyused

Quality assurance in a chemical measurement involves theactions within the method of analysis that provide satisfactorymeasurements with appropriate confidence high dependabilityand in a cost-effective manner

Define the Problem

The intent of the measurement

The necessary considerations in sampling and sample preparation

The best technique for making the measurement

Evaluation of the data

Reporting the results

The resources needed to accomplish the analysis

The method chosen may provide either qualitative or quantitativeinformation

Qualitative method data may include the composition oxidationstates structural information or the isotopic distributions ofelements contained in a sample

An understanding of the instrumentation used to make thequalitative measurement also leads one to a rough approximation ofthe concentration of the species being measured

Whether the substance is a major (gt1) minor (001-1) trace (10-2 ndash 10-6) or ultra-trace (10-6- 10-9) component

Quantitative methods the analyst needs to plan tasks associatedwith sampling sample preparation and calibration moremeticulously than a qualitative analysis

Often preliminary measurements will be required to develop aquantitative method

bull A careful consideration of the analyte sample andinstrumentation are critical in the development of a validinstrumental method

Properties of the sample

Analyte properties

Anticipated concentration range of the analyte

Sample preparation

Desired precision

Desired accuracy

ConcomitantsInterferents

Existing methods

Method Modeling and Plan

The model is an idealized representation of the complex steps ofthe analytical method

It includes a specific statement of the problem information aboutthe sample and analyte (concentration levels of concern potentialinterferences location of the analyte in the sample phaserelationships particle size distributionhellip)

bull The development of a model may require experiments to obtainmore information about the sample or to validate assumptions

It necessary to perform measurements on the sample todetermine its homogeneity

Development of a sampling plan to accurately address the goalsof the method

The results of these preliminary experiments are used to helprefine the original model

bull After establishment of the model a plan must be created toprovide specific directions for each step in the method

bull The plan translates the model into standard operating procedureswhich provide the actions and reviews necessary to complete theanalysis with the necessary precision and accuracy

EXProposed Research Work i Project Title ii Introduction bull Origin of the research problem bull Interdisciplinary relevance bull Review of Research and Development in the Subject

1048708 International status 1048708 National Status 1048708 Significance of the study

(iii) Objectives (iv) Methodology (v) Year-wise Plan of work and targets to be achieve

Obtain and Store the Sample Expert knowledge in the mechanics of instrumental measurements is a critical

aspect in the role of an analyst however it is insufficient in gaining accurateand precise results

Proper consideration of the sampling and sample handling are equallyimportant

Even with the best quality instrumental measurement a poorly selected orimproperly handled sample will give erroneous or inappropriate results

Sample Preparation

The samples must also be treated to make them compatible withthe instrumental technique

Transformation of the sample into a form that can be measuredusing the selected technique is termed sample preparation

Sample selection and preparation usually represent the largestinvestment of time in the implementation of an analytical method

It is important to realize that the majority of instrumentaltechniques require the sample to be in a liquid phase

For solid samples several techniques are taken to transfer theanalyte into the liquid phase

Care must be taken in these steps to preserve the integrity of theanalyte by considering the possibility of contamination loss orchemical and physical changes to the analyte

Perform Measurements

Once the sample has been prepared it is necessary to measurereplicate samples to establish the precision of the method

The measurement depends upon the interaction of the techniquewith a unique chemical or physical property of the analyte

Consider the example involving the use of IR spectrophotometryto measure the residual styrene and acrylonitrile monomersremaining in a copolymer sample

The measurement relies on the fact that the aromatic carbon-carbon bonds in the styrene monomer absorb infrared radiation atapproximately 1600 cm-1 while the cyano group of theacrylonitrile monomer absorbs at 2275 cm-1

An accurate analysis will assure minimal or no absorbance of thestyrene monomer at the frequency of the acrylonitrile monomer

Compare Results with Standards

Reliable and convincing analytical results must involve a propercareful comparison of the analytersquos signal to that of appropriatestandards of known analyte concentration as well as a calibrationblank solution This is known as calibration or standardization

Calibration establishes the mathematical relationship between theanalytical signal and the concentration of analyte in the calibrationstandards The most common approach is to develop a ldquoworkingrdquocurve

Significant interactions with collaborating investigators aretypically required not only for the analyst to acquire thenecessary information to solve the problem

To communicate the information that can realistically beprovided given the nature of the sample and measurementtechniques available

When the concepts of quality are applied to a chemicalmeasurement the term quality assurance is more commonlyused

Quality assurance in a chemical measurement involves theactions within the method of analysis that provide satisfactorymeasurements with appropriate confidence high dependabilityand in a cost-effective manner

Define the Problem

The intent of the measurement

The necessary considerations in sampling and sample preparation

The best technique for making the measurement

Evaluation of the data

Reporting the results

The resources needed to accomplish the analysis

The method chosen may provide either qualitative or quantitativeinformation

Qualitative method data may include the composition oxidationstates structural information or the isotopic distributions ofelements contained in a sample

An understanding of the instrumentation used to make thequalitative measurement also leads one to a rough approximation ofthe concentration of the species being measured

Whether the substance is a major (gt1) minor (001-1) trace (10-2 ndash 10-6) or ultra-trace (10-6- 10-9) component

Quantitative methods the analyst needs to plan tasks associatedwith sampling sample preparation and calibration moremeticulously than a qualitative analysis

Often preliminary measurements will be required to develop aquantitative method

bull A careful consideration of the analyte sample andinstrumentation are critical in the development of a validinstrumental method

Properties of the sample

Analyte properties

Anticipated concentration range of the analyte

Sample preparation

Desired precision

Desired accuracy

ConcomitantsInterferents

Existing methods

Method Modeling and Plan

The model is an idealized representation of the complex steps ofthe analytical method

It includes a specific statement of the problem information aboutthe sample and analyte (concentration levels of concern potentialinterferences location of the analyte in the sample phaserelationships particle size distributionhellip)

bull The development of a model may require experiments to obtainmore information about the sample or to validate assumptions

It necessary to perform measurements on the sample todetermine its homogeneity

Development of a sampling plan to accurately address the goalsof the method

The results of these preliminary experiments are used to helprefine the original model

bull After establishment of the model a plan must be created toprovide specific directions for each step in the method

bull The plan translates the model into standard operating procedureswhich provide the actions and reviews necessary to complete theanalysis with the necessary precision and accuracy

EXProposed Research Work i Project Title ii Introduction bull Origin of the research problem bull Interdisciplinary relevance bull Review of Research and Development in the Subject

1048708 International status 1048708 National Status 1048708 Significance of the study

(iii) Objectives (iv) Methodology (v) Year-wise Plan of work and targets to be achieve

Obtain and Store the Sample Expert knowledge in the mechanics of instrumental measurements is a critical

aspect in the role of an analyst however it is insufficient in gaining accurateand precise results

Proper consideration of the sampling and sample handling are equallyimportant

Even with the best quality instrumental measurement a poorly selected orimproperly handled sample will give erroneous or inappropriate results

Sample Preparation

The samples must also be treated to make them compatible withthe instrumental technique

Transformation of the sample into a form that can be measuredusing the selected technique is termed sample preparation

Sample selection and preparation usually represent the largestinvestment of time in the implementation of an analytical method

It is important to realize that the majority of instrumentaltechniques require the sample to be in a liquid phase

For solid samples several techniques are taken to transfer theanalyte into the liquid phase

Care must be taken in these steps to preserve the integrity of theanalyte by considering the possibility of contamination loss orchemical and physical changes to the analyte

Perform Measurements

Once the sample has been prepared it is necessary to measurereplicate samples to establish the precision of the method

The measurement depends upon the interaction of the techniquewith a unique chemical or physical property of the analyte

Consider the example involving the use of IR spectrophotometryto measure the residual styrene and acrylonitrile monomersremaining in a copolymer sample

The measurement relies on the fact that the aromatic carbon-carbon bonds in the styrene monomer absorb infrared radiation atapproximately 1600 cm-1 while the cyano group of theacrylonitrile monomer absorbs at 2275 cm-1

An accurate analysis will assure minimal or no absorbance of thestyrene monomer at the frequency of the acrylonitrile monomer

Compare Results with Standards

Reliable and convincing analytical results must involve a propercareful comparison of the analytersquos signal to that of appropriatestandards of known analyte concentration as well as a calibrationblank solution This is known as calibration or standardization

Calibration establishes the mathematical relationship between theanalytical signal and the concentration of analyte in the calibrationstandards The most common approach is to develop a ldquoworkingrdquocurve

Define the Problem

The intent of the measurement

The necessary considerations in sampling and sample preparation

The best technique for making the measurement

Evaluation of the data

Reporting the results

The resources needed to accomplish the analysis

The method chosen may provide either qualitative or quantitativeinformation

Qualitative method data may include the composition oxidationstates structural information or the isotopic distributions ofelements contained in a sample

An understanding of the instrumentation used to make thequalitative measurement also leads one to a rough approximation ofthe concentration of the species being measured

Whether the substance is a major (gt1) minor (001-1) trace (10-2 ndash 10-6) or ultra-trace (10-6- 10-9) component

Quantitative methods the analyst needs to plan tasks associatedwith sampling sample preparation and calibration moremeticulously than a qualitative analysis

Often preliminary measurements will be required to develop aquantitative method

bull A careful consideration of the analyte sample andinstrumentation are critical in the development of a validinstrumental method

Properties of the sample

Analyte properties

Anticipated concentration range of the analyte

Sample preparation

Desired precision

Desired accuracy

ConcomitantsInterferents

Existing methods

Method Modeling and Plan

The model is an idealized representation of the complex steps ofthe analytical method

It includes a specific statement of the problem information aboutthe sample and analyte (concentration levels of concern potentialinterferences location of the analyte in the sample phaserelationships particle size distributionhellip)

bull The development of a model may require experiments to obtainmore information about the sample or to validate assumptions

It necessary to perform measurements on the sample todetermine its homogeneity

Development of a sampling plan to accurately address the goalsof the method

The results of these preliminary experiments are used to helprefine the original model

bull After establishment of the model a plan must be created toprovide specific directions for each step in the method

bull The plan translates the model into standard operating procedureswhich provide the actions and reviews necessary to complete theanalysis with the necessary precision and accuracy

EXProposed Research Work i Project Title ii Introduction bull Origin of the research problem bull Interdisciplinary relevance bull Review of Research and Development in the Subject

1048708 International status 1048708 National Status 1048708 Significance of the study

(iii) Objectives (iv) Methodology (v) Year-wise Plan of work and targets to be achieve

Obtain and Store the Sample Expert knowledge in the mechanics of instrumental measurements is a critical

aspect in the role of an analyst however it is insufficient in gaining accurateand precise results

Proper consideration of the sampling and sample handling are equallyimportant

Even with the best quality instrumental measurement a poorly selected orimproperly handled sample will give erroneous or inappropriate results

Sample Preparation

The samples must also be treated to make them compatible withthe instrumental technique

Transformation of the sample into a form that can be measuredusing the selected technique is termed sample preparation

Sample selection and preparation usually represent the largestinvestment of time in the implementation of an analytical method

It is important to realize that the majority of instrumentaltechniques require the sample to be in a liquid phase

For solid samples several techniques are taken to transfer theanalyte into the liquid phase

Care must be taken in these steps to preserve the integrity of theanalyte by considering the possibility of contamination loss orchemical and physical changes to the analyte

Perform Measurements

Once the sample has been prepared it is necessary to measurereplicate samples to establish the precision of the method

The measurement depends upon the interaction of the techniquewith a unique chemical or physical property of the analyte

Consider the example involving the use of IR spectrophotometryto measure the residual styrene and acrylonitrile monomersremaining in a copolymer sample

The measurement relies on the fact that the aromatic carbon-carbon bonds in the styrene monomer absorb infrared radiation atapproximately 1600 cm-1 while the cyano group of theacrylonitrile monomer absorbs at 2275 cm-1

An accurate analysis will assure minimal or no absorbance of thestyrene monomer at the frequency of the acrylonitrile monomer

Compare Results with Standards

Reliable and convincing analytical results must involve a propercareful comparison of the analytersquos signal to that of appropriatestandards of known analyte concentration as well as a calibrationblank solution This is known as calibration or standardization

Calibration establishes the mathematical relationship between theanalytical signal and the concentration of analyte in the calibrationstandards The most common approach is to develop a ldquoworkingrdquocurve

The method chosen may provide either qualitative or quantitativeinformation

Qualitative method data may include the composition oxidationstates structural information or the isotopic distributions ofelements contained in a sample

An understanding of the instrumentation used to make thequalitative measurement also leads one to a rough approximation ofthe concentration of the species being measured

Whether the substance is a major (gt1) minor (001-1) trace (10-2 ndash 10-6) or ultra-trace (10-6- 10-9) component

Quantitative methods the analyst needs to plan tasks associatedwith sampling sample preparation and calibration moremeticulously than a qualitative analysis

Often preliminary measurements will be required to develop aquantitative method

bull A careful consideration of the analyte sample andinstrumentation are critical in the development of a validinstrumental method

Properties of the sample

Analyte properties

Anticipated concentration range of the analyte

Sample preparation

Desired precision

Desired accuracy

ConcomitantsInterferents

Existing methods

Method Modeling and Plan

The model is an idealized representation of the complex steps ofthe analytical method

It includes a specific statement of the problem information aboutthe sample and analyte (concentration levels of concern potentialinterferences location of the analyte in the sample phaserelationships particle size distributionhellip)

bull The development of a model may require experiments to obtainmore information about the sample or to validate assumptions

It necessary to perform measurements on the sample todetermine its homogeneity

Development of a sampling plan to accurately address the goalsof the method

The results of these preliminary experiments are used to helprefine the original model

bull After establishment of the model a plan must be created toprovide specific directions for each step in the method

bull The plan translates the model into standard operating procedureswhich provide the actions and reviews necessary to complete theanalysis with the necessary precision and accuracy

EXProposed Research Work i Project Title ii Introduction bull Origin of the research problem bull Interdisciplinary relevance bull Review of Research and Development in the Subject

1048708 International status 1048708 National Status 1048708 Significance of the study

(iii) Objectives (iv) Methodology (v) Year-wise Plan of work and targets to be achieve

Obtain and Store the Sample Expert knowledge in the mechanics of instrumental measurements is a critical

aspect in the role of an analyst however it is insufficient in gaining accurateand precise results

Proper consideration of the sampling and sample handling are equallyimportant

Even with the best quality instrumental measurement a poorly selected orimproperly handled sample will give erroneous or inappropriate results

Sample Preparation

The samples must also be treated to make them compatible withthe instrumental technique

Transformation of the sample into a form that can be measuredusing the selected technique is termed sample preparation

Sample selection and preparation usually represent the largestinvestment of time in the implementation of an analytical method

It is important to realize that the majority of instrumentaltechniques require the sample to be in a liquid phase

For solid samples several techniques are taken to transfer theanalyte into the liquid phase

Care must be taken in these steps to preserve the integrity of theanalyte by considering the possibility of contamination loss orchemical and physical changes to the analyte

Perform Measurements

Once the sample has been prepared it is necessary to measurereplicate samples to establish the precision of the method

The measurement depends upon the interaction of the techniquewith a unique chemical or physical property of the analyte

Consider the example involving the use of IR spectrophotometryto measure the residual styrene and acrylonitrile monomersremaining in a copolymer sample

The measurement relies on the fact that the aromatic carbon-carbon bonds in the styrene monomer absorb infrared radiation atapproximately 1600 cm-1 while the cyano group of theacrylonitrile monomer absorbs at 2275 cm-1

An accurate analysis will assure minimal or no absorbance of thestyrene monomer at the frequency of the acrylonitrile monomer

Compare Results with Standards

Reliable and convincing analytical results must involve a propercareful comparison of the analytersquos signal to that of appropriatestandards of known analyte concentration as well as a calibrationblank solution This is known as calibration or standardization

Calibration establishes the mathematical relationship between theanalytical signal and the concentration of analyte in the calibrationstandards The most common approach is to develop a ldquoworkingrdquocurve

bull A careful consideration of the analyte sample andinstrumentation are critical in the development of a validinstrumental method

Properties of the sample

Analyte properties

Anticipated concentration range of the analyte

Sample preparation

Desired precision

Desired accuracy

ConcomitantsInterferents

Existing methods

Method Modeling and Plan

The model is an idealized representation of the complex steps ofthe analytical method

It includes a specific statement of the problem information aboutthe sample and analyte (concentration levels of concern potentialinterferences location of the analyte in the sample phaserelationships particle size distributionhellip)

bull The development of a model may require experiments to obtainmore information about the sample or to validate assumptions

It necessary to perform measurements on the sample todetermine its homogeneity

Development of a sampling plan to accurately address the goalsof the method

The results of these preliminary experiments are used to helprefine the original model

bull After establishment of the model a plan must be created toprovide specific directions for each step in the method

bull The plan translates the model into standard operating procedureswhich provide the actions and reviews necessary to complete theanalysis with the necessary precision and accuracy

EXProposed Research Work i Project Title ii Introduction bull Origin of the research problem bull Interdisciplinary relevance bull Review of Research and Development in the Subject

1048708 International status 1048708 National Status 1048708 Significance of the study

(iii) Objectives (iv) Methodology (v) Year-wise Plan of work and targets to be achieve

Obtain and Store the Sample Expert knowledge in the mechanics of instrumental measurements is a critical

aspect in the role of an analyst however it is insufficient in gaining accurateand precise results

Proper consideration of the sampling and sample handling are equallyimportant

Even with the best quality instrumental measurement a poorly selected orimproperly handled sample will give erroneous or inappropriate results

Sample Preparation

The samples must also be treated to make them compatible withthe instrumental technique

Transformation of the sample into a form that can be measuredusing the selected technique is termed sample preparation

Sample selection and preparation usually represent the largestinvestment of time in the implementation of an analytical method

It is important to realize that the majority of instrumentaltechniques require the sample to be in a liquid phase

For solid samples several techniques are taken to transfer theanalyte into the liquid phase

Care must be taken in these steps to preserve the integrity of theanalyte by considering the possibility of contamination loss orchemical and physical changes to the analyte

Perform Measurements

Once the sample has been prepared it is necessary to measurereplicate samples to establish the precision of the method

The measurement depends upon the interaction of the techniquewith a unique chemical or physical property of the analyte

Consider the example involving the use of IR spectrophotometryto measure the residual styrene and acrylonitrile monomersremaining in a copolymer sample

The measurement relies on the fact that the aromatic carbon-carbon bonds in the styrene monomer absorb infrared radiation atapproximately 1600 cm-1 while the cyano group of theacrylonitrile monomer absorbs at 2275 cm-1

An accurate analysis will assure minimal or no absorbance of thestyrene monomer at the frequency of the acrylonitrile monomer

Compare Results with Standards

Reliable and convincing analytical results must involve a propercareful comparison of the analytersquos signal to that of appropriatestandards of known analyte concentration as well as a calibrationblank solution This is known as calibration or standardization

Calibration establishes the mathematical relationship between theanalytical signal and the concentration of analyte in the calibrationstandards The most common approach is to develop a ldquoworkingrdquocurve

Method Modeling and Plan

The model is an idealized representation of the complex steps ofthe analytical method

It includes a specific statement of the problem information aboutthe sample and analyte (concentration levels of concern potentialinterferences location of the analyte in the sample phaserelationships particle size distributionhellip)

bull The development of a model may require experiments to obtainmore information about the sample or to validate assumptions

It necessary to perform measurements on the sample todetermine its homogeneity

Development of a sampling plan to accurately address the goalsof the method

The results of these preliminary experiments are used to helprefine the original model

bull After establishment of the model a plan must be created toprovide specific directions for each step in the method

bull The plan translates the model into standard operating procedureswhich provide the actions and reviews necessary to complete theanalysis with the necessary precision and accuracy

EXProposed Research Work i Project Title ii Introduction bull Origin of the research problem bull Interdisciplinary relevance bull Review of Research and Development in the Subject

1048708 International status 1048708 National Status 1048708 Significance of the study

(iii) Objectives (iv) Methodology (v) Year-wise Plan of work and targets to be achieve

Obtain and Store the Sample Expert knowledge in the mechanics of instrumental measurements is a critical

aspect in the role of an analyst however it is insufficient in gaining accurateand precise results

Proper consideration of the sampling and sample handling are equallyimportant

Even with the best quality instrumental measurement a poorly selected orimproperly handled sample will give erroneous or inappropriate results

Sample Preparation

The samples must also be treated to make them compatible withthe instrumental technique

Transformation of the sample into a form that can be measuredusing the selected technique is termed sample preparation

Sample selection and preparation usually represent the largestinvestment of time in the implementation of an analytical method

It is important to realize that the majority of instrumentaltechniques require the sample to be in a liquid phase

For solid samples several techniques are taken to transfer theanalyte into the liquid phase

Care must be taken in these steps to preserve the integrity of theanalyte by considering the possibility of contamination loss orchemical and physical changes to the analyte

Perform Measurements

Once the sample has been prepared it is necessary to measurereplicate samples to establish the precision of the method

The measurement depends upon the interaction of the techniquewith a unique chemical or physical property of the analyte

Consider the example involving the use of IR spectrophotometryto measure the residual styrene and acrylonitrile monomersremaining in a copolymer sample

The measurement relies on the fact that the aromatic carbon-carbon bonds in the styrene monomer absorb infrared radiation atapproximately 1600 cm-1 while the cyano group of theacrylonitrile monomer absorbs at 2275 cm-1

An accurate analysis will assure minimal or no absorbance of thestyrene monomer at the frequency of the acrylonitrile monomer

Compare Results with Standards

Reliable and convincing analytical results must involve a propercareful comparison of the analytersquos signal to that of appropriatestandards of known analyte concentration as well as a calibrationblank solution This is known as calibration or standardization

Calibration establishes the mathematical relationship between theanalytical signal and the concentration of analyte in the calibrationstandards The most common approach is to develop a ldquoworkingrdquocurve

bull After establishment of the model a plan must be created toprovide specific directions for each step in the method

bull The plan translates the model into standard operating procedureswhich provide the actions and reviews necessary to complete theanalysis with the necessary precision and accuracy

EXProposed Research Work i Project Title ii Introduction bull Origin of the research problem bull Interdisciplinary relevance bull Review of Research and Development in the Subject

1048708 International status 1048708 National Status 1048708 Significance of the study

(iii) Objectives (iv) Methodology (v) Year-wise Plan of work and targets to be achieve

Obtain and Store the Sample Expert knowledge in the mechanics of instrumental measurements is a critical

aspect in the role of an analyst however it is insufficient in gaining accurateand precise results

Proper consideration of the sampling and sample handling are equallyimportant

Even with the best quality instrumental measurement a poorly selected orimproperly handled sample will give erroneous or inappropriate results

Sample Preparation

The samples must also be treated to make them compatible withthe instrumental technique

Transformation of the sample into a form that can be measuredusing the selected technique is termed sample preparation

Sample selection and preparation usually represent the largestinvestment of time in the implementation of an analytical method

It is important to realize that the majority of instrumentaltechniques require the sample to be in a liquid phase

For solid samples several techniques are taken to transfer theanalyte into the liquid phase

Care must be taken in these steps to preserve the integrity of theanalyte by considering the possibility of contamination loss orchemical and physical changes to the analyte

Perform Measurements

Once the sample has been prepared it is necessary to measurereplicate samples to establish the precision of the method

The measurement depends upon the interaction of the techniquewith a unique chemical or physical property of the analyte

Consider the example involving the use of IR spectrophotometryto measure the residual styrene and acrylonitrile monomersremaining in a copolymer sample

The measurement relies on the fact that the aromatic carbon-carbon bonds in the styrene monomer absorb infrared radiation atapproximately 1600 cm-1 while the cyano group of theacrylonitrile monomer absorbs at 2275 cm-1

An accurate analysis will assure minimal or no absorbance of thestyrene monomer at the frequency of the acrylonitrile monomer

Compare Results with Standards

Reliable and convincing analytical results must involve a propercareful comparison of the analytersquos signal to that of appropriatestandards of known analyte concentration as well as a calibrationblank solution This is known as calibration or standardization

Calibration establishes the mathematical relationship between theanalytical signal and the concentration of analyte in the calibrationstandards The most common approach is to develop a ldquoworkingrdquocurve

Obtain and Store the Sample Expert knowledge in the mechanics of instrumental measurements is a critical

aspect in the role of an analyst however it is insufficient in gaining accurateand precise results

Proper consideration of the sampling and sample handling are equallyimportant

Even with the best quality instrumental measurement a poorly selected orimproperly handled sample will give erroneous or inappropriate results

Sample Preparation

The samples must also be treated to make them compatible withthe instrumental technique

Transformation of the sample into a form that can be measuredusing the selected technique is termed sample preparation

Sample selection and preparation usually represent the largestinvestment of time in the implementation of an analytical method

It is important to realize that the majority of instrumentaltechniques require the sample to be in a liquid phase

For solid samples several techniques are taken to transfer theanalyte into the liquid phase

Care must be taken in these steps to preserve the integrity of theanalyte by considering the possibility of contamination loss orchemical and physical changes to the analyte

Perform Measurements

Once the sample has been prepared it is necessary to measurereplicate samples to establish the precision of the method

The measurement depends upon the interaction of the techniquewith a unique chemical or physical property of the analyte

Consider the example involving the use of IR spectrophotometryto measure the residual styrene and acrylonitrile monomersremaining in a copolymer sample

The measurement relies on the fact that the aromatic carbon-carbon bonds in the styrene monomer absorb infrared radiation atapproximately 1600 cm-1 while the cyano group of theacrylonitrile monomer absorbs at 2275 cm-1

An accurate analysis will assure minimal or no absorbance of thestyrene monomer at the frequency of the acrylonitrile monomer

Compare Results with Standards

Reliable and convincing analytical results must involve a propercareful comparison of the analytersquos signal to that of appropriatestandards of known analyte concentration as well as a calibrationblank solution This is known as calibration or standardization

Calibration establishes the mathematical relationship between theanalytical signal and the concentration of analyte in the calibrationstandards The most common approach is to develop a ldquoworkingrdquocurve

Sample Preparation

The samples must also be treated to make them compatible withthe instrumental technique

Transformation of the sample into a form that can be measuredusing the selected technique is termed sample preparation

Sample selection and preparation usually represent the largestinvestment of time in the implementation of an analytical method

It is important to realize that the majority of instrumentaltechniques require the sample to be in a liquid phase

For solid samples several techniques are taken to transfer theanalyte into the liquid phase

Care must be taken in these steps to preserve the integrity of theanalyte by considering the possibility of contamination loss orchemical and physical changes to the analyte

Perform Measurements

Once the sample has been prepared it is necessary to measurereplicate samples to establish the precision of the method

The measurement depends upon the interaction of the techniquewith a unique chemical or physical property of the analyte

Consider the example involving the use of IR spectrophotometryto measure the residual styrene and acrylonitrile monomersremaining in a copolymer sample

The measurement relies on the fact that the aromatic carbon-carbon bonds in the styrene monomer absorb infrared radiation atapproximately 1600 cm-1 while the cyano group of theacrylonitrile monomer absorbs at 2275 cm-1

An accurate analysis will assure minimal or no absorbance of thestyrene monomer at the frequency of the acrylonitrile monomer

Compare Results with Standards

Reliable and convincing analytical results must involve a propercareful comparison of the analytersquos signal to that of appropriatestandards of known analyte concentration as well as a calibrationblank solution This is known as calibration or standardization

Calibration establishes the mathematical relationship between theanalytical signal and the concentration of analyte in the calibrationstandards The most common approach is to develop a ldquoworkingrdquocurve

Perform Measurements

Once the sample has been prepared it is necessary to measurereplicate samples to establish the precision of the method

The measurement depends upon the interaction of the techniquewith a unique chemical or physical property of the analyte

Consider the example involving the use of IR spectrophotometryto measure the residual styrene and acrylonitrile monomersremaining in a copolymer sample

The measurement relies on the fact that the aromatic carbon-carbon bonds in the styrene monomer absorb infrared radiation atapproximately 1600 cm-1 while the cyano group of theacrylonitrile monomer absorbs at 2275 cm-1

An accurate analysis will assure minimal or no absorbance of thestyrene monomer at the frequency of the acrylonitrile monomer

Compare Results with Standards

Reliable and convincing analytical results must involve a propercareful comparison of the analytersquos signal to that of appropriatestandards of known analyte concentration as well as a calibrationblank solution This is known as calibration or standardization

Calibration establishes the mathematical relationship between theanalytical signal and the concentration of analyte in the calibrationstandards The most common approach is to develop a ldquoworkingrdquocurve

Compare Results with Standards

Reliable and convincing analytical results must involve a propercareful comparison of the analytersquos signal to that of appropriatestandards of known analyte concentration as well as a calibrationblank solution This is known as calibration or standardization

Calibration establishes the mathematical relationship between theanalytical signal and the concentration of analyte in the calibrationstandards The most common approach is to develop a ldquoworkingrdquocurve