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Instrumentation
Deals with the theoretical and practical aspects of
different instruments and instrumental techniques
involved in Analytical Chemistry,




Which is a branch of chemistry involving separation,
identification and determination of components of a
sample
Instrumentation 1
Instrumentation 1
Instrumentation 1
Instrumentation 1
1 M = 1 mole/1 liter solution
Instrumentation 1
Instrumentation 1
Instrumentation 1
Classification of analyte

•   Major component 1-100%
•   Minor component 0.01 to <1.00%
•   Trace component 1ppb – 100 ppm
•   Ultra-trace component <1ppb
Analytical method on the basis of sample
                  size
    Method      Weight mg    Volume µl

     Meso           >100       >100

  Semi-micro        10-100    50-100

     Micro          1-<10      <50


Ultra micro    <1
Instrumentation 1
Problems
•   Prepare a solution of 1 Molar HCl
•   Prepare a solution of 1 Molar NaOH
•   Prepare a solution of 1 Molar H2SO4
• Prepare a solution of 1 Molar Oxalic acid
  dihydrate
• Prepare a solution of 1 Normal Oxalic acid
  dihydrate
Instrumentation 1
Problem
• You have a stock solution of NaOH having
  concentration of 1 M, prepare 500 mL solutions of
  0.1N, 0.2N, 0.3N using dilution equation
Instrumentation 1
Problem

• What is pCl and pNa of a 5.00g/L solution
 of NaCl?



  Na     Cl    NaCl   Given   Molar   pNa/pCl

  23    35.5   58.5   5g/L 0.085470 1.068186
Selecting an Analytical Technique
Defining the problem first:
1. What accuracy and precision is required?
2. How much sample is available?
3. What is the concentration range of the
  analyte?
4. What components of the sample cause
  interference?
5. What are the physical and chemical
  properties of the sample matrix or interfering
  species?
6. How many samples are to be analyzed?
Numerical Criteria for Selecting Analytical
                  Technique
1. Precision
2. Bias (A systematic error occurring in a chemical
  measurement that is inherent in the method itself or
  caused by some artifact in the system, such as a
  temperature effect)
3. Sensitivity (LOD and LOQ)
4. Detection Limits
5. Concentration Range
6. Selectivity
Other Characteristics to Be
   Considered in Method of Choice
1. Speed
2. Ease and Convenience
3. Cost and availability of instrument
4. Per-sample cost
Sampling
• Homogeneous materials (grab sample,
  random)
• Heterogeneous materials (Several          samples
  are required) that include
1- Gross sampling
2- Laboratory sample (taken from gross sampling and
  homogenized)
3- Analysis samples (taken from laboratory sample)
4- Biological fluids (sampling time and preservation)
5- Storage of the samples (suitable containers, low
  temp)
6- Urine samples (acidified pH4.5)
Preparation of samples
•   Weighing of the sample
•   Samples are prepared in replicates
•   Solid samples must be dissolved
•   Ashing or digestion for trace metals
•   Preparation of blank
Chemical separation
• Includes precipitation, extraction,
  chromatography, dialysis and distillation,
  and
1- Eliminates interferences (analyte away
  from matrix)
2- Provides suitable selectivity in
  measurement
Classification of Analytical Methods

1-Classical methods
   –   Gravimetric
   –   Titrimetric
2-Instrumental methods
   –   Spectroscopy
   –   Electroanalytical
   –   Chromatography
Data Analysis
• The concentration of analyte in the sample
  solution is used to calculate the concentration of
  analyte in the original sample, and is expressed
  in relative terms

• Precision is expressed by SD of RSD
• Finally
  Critical evaluation of results (To see whether
  results relate to the analytical problem, as stated
  before the experiment

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Instrumentation 1

  • 1. Instrumentation Deals with the theoretical and practical aspects of different instruments and instrumental techniques involved in Analytical Chemistry, Which is a branch of chemistry involving separation, identification and determination of components of a sample
  • 6. 1 M = 1 mole/1 liter solution
  • 10. Classification of analyte • Major component 1-100% • Minor component 0.01 to <1.00% • Trace component 1ppb – 100 ppm • Ultra-trace component <1ppb
  • 11. Analytical method on the basis of sample size Method Weight mg Volume µl Meso >100 >100 Semi-micro 10-100 50-100 Micro 1-<10 <50 Ultra micro <1
  • 13. Problems • Prepare a solution of 1 Molar HCl • Prepare a solution of 1 Molar NaOH • Prepare a solution of 1 Molar H2SO4 • Prepare a solution of 1 Molar Oxalic acid dihydrate • Prepare a solution of 1 Normal Oxalic acid dihydrate
  • 15. Problem • You have a stock solution of NaOH having concentration of 1 M, prepare 500 mL solutions of 0.1N, 0.2N, 0.3N using dilution equation
  • 17. Problem • What is pCl and pNa of a 5.00g/L solution of NaCl? Na Cl NaCl Given Molar pNa/pCl 23 35.5 58.5 5g/L 0.085470 1.068186
  • 18. Selecting an Analytical Technique Defining the problem first: 1. What accuracy and precision is required? 2. How much sample is available? 3. What is the concentration range of the analyte? 4. What components of the sample cause interference? 5. What are the physical and chemical properties of the sample matrix or interfering species? 6. How many samples are to be analyzed?
  • 19. Numerical Criteria for Selecting Analytical Technique 1. Precision 2. Bias (A systematic error occurring in a chemical measurement that is inherent in the method itself or caused by some artifact in the system, such as a temperature effect) 3. Sensitivity (LOD and LOQ) 4. Detection Limits 5. Concentration Range 6. Selectivity
  • 20. Other Characteristics to Be Considered in Method of Choice 1. Speed 2. Ease and Convenience 3. Cost and availability of instrument 4. Per-sample cost
  • 21. Sampling • Homogeneous materials (grab sample, random) • Heterogeneous materials (Several samples are required) that include 1- Gross sampling 2- Laboratory sample (taken from gross sampling and homogenized) 3- Analysis samples (taken from laboratory sample) 4- Biological fluids (sampling time and preservation) 5- Storage of the samples (suitable containers, low temp) 6- Urine samples (acidified pH4.5)
  • 22. Preparation of samples • Weighing of the sample • Samples are prepared in replicates • Solid samples must be dissolved • Ashing or digestion for trace metals • Preparation of blank
  • 23. Chemical separation • Includes precipitation, extraction, chromatography, dialysis and distillation, and 1- Eliminates interferences (analyte away from matrix) 2- Provides suitable selectivity in measurement
  • 24. Classification of Analytical Methods 1-Classical methods – Gravimetric – Titrimetric 2-Instrumental methods – Spectroscopy – Electroanalytical – Chromatography
  • 25. Data Analysis • The concentration of analyte in the sample solution is used to calculate the concentration of analyte in the original sample, and is expressed in relative terms • Precision is expressed by SD of RSD • Finally Critical evaluation of results (To see whether results relate to the analytical problem, as stated before the experiment