ANALYTICAL CHEMISTRY (SSCK 1203)

Analytical Chemistry and Instrumentation Panel Department of Chemistry Faculty of Science UTM Skudai

INTRODUCTION TO ANALYTICAL CHEMISTRY

(PART 1)
ANALYTICAL CHEMISTRY - A branch of chemistry that deals with the separation, identification & determination of analytes (components) in a sample

-It involves the application of a range of techniques and methodologies to obtain and assess qualitative, quantitative and structural information on the nature of matter.

AREAS OF ANALYTICAL CHEMISTRY

Environmental analysis Monitoring of pollutants, soil and water analysis, pesticides, etc (environment quality) Forensic analysis Analysis related to criminology, DNA finger printing, finger print detection, blood analysis (crime detection and court testimonies) Industrial quality control Requirements of companies for product quality . Bioanalytical chemistry and analysis Detection and/or analysis of biological components (eg proteins, DNA, RNA, carbohydrates, etc) Clinical analysis Analysis of blood, urine, feces, cellular fluids, etc (for use in medical diagnosis) Pharmaceutical analysis Establishment of physical properties, toxicity, metabolites, quality control, etc (medicine/drugs)

ANALYTICAL CHEMISTS IN INDUSTRY - INTERFACES

Other Colleges Lawyers chemists Universities Health Peers, & Supervisors Safety Technical reps In field Production plants

Life scientists

Analytical chemist

Contract labs

Sales & Marketing

Suppliers Engineers

Management

Professional organizations Statisticians Government agencies

Attributes of a good Analytical Chemist

Knows and has skill in the methods and instruments used for analysis Understands the principles of analysis (able to apply and modify analytical methods to solve a particular problem) Able to evaluate and interpret results of an analysis Able to develop, validate, verify and apply new methods of analysis Validate: Prove that the method works and define its limitations (ie. sample type, detection limits, interferences, concentration, sensitivity, etc) Verify: Ensure that analysts are able to obtain correct results using the method (in the laboratory)

CHEMICAL ANALYSIS
What? How much?

Qualitative Analysis
An analysis to identify the material(s) present in a sample

Quantitative Analysis
An analysis to determine the amount of a material is present in a sample

Instrumental & Chemical methods

Classical (Wet) Methods

Instrumental Methods

No obvious dividing line

Analyte: the substance to be identified, detected, or separated in some manner Sample : representative of the population or gross sample Matrix: all other constituents in a sample except for the analyte

Quantitative Analysis
Complete Analysis - amount of each constituent of

the sample is determined Ultimate Analysis - amount of each element in a sample is determined regardless of the actual compounds present Partial Analysis - amount of a certain selected constituent in a sample is determined

Classification of constituents in a sample Major (> 1%) Minor (0.11%) Trace (< 0.1%) Ultra trace (A few ppm or less)
What do these statements mean? ? As in urine (0.1 ppm) ? Caffiene in coffee (10 %v/v) ? H2SO4 in rain (0.0001 M) ? Ca in mineral water (42 mg/L) ? Vitamin C in supplementary tablets (12 mg/tablet)

Classification of Analytical Methods Classical Methods

(1) Gravimetric Methods Measure the mass of the analyte or a compound chemically related to the analyte

Instrumental Methods
(1) Separation/Chromatographic Methods Measure the peak areas of the separated components of a sample (2) Spectroscopic Methods Measure the interaction between the analyte and electromagnetic radiation or the production of radiation by an analyte

(2) Volumetric Methods Measure the volume of a solution containing sufficient reagent to react (3) Electroanalytical Methods with the analyte (eg. Measure an electrical property (eg titration, gas analysis) potential, current, etc) which is chemically related to the amount of analyte

Classification of Techniques
Classical Separation of Analytes - Extraction, filtration, distillation, Precipitation, etc (Simple physical procedures) Quantitative Analysis - Titration - Gravimetric analysis Qualitative Analysis - Boiling & Melting pt, color, odor, density, reactivity, refractive index, etc Instrumental Separation of Analytes - Chromatography, Electrophoresis - Spectroscopic separation Quantitative Analysis - UV-Vis spectrometry - Atomic absorption spectro. - Atomic emission spectro. - Conductivity (pH, ISE) Qualitative Analysis X-ray spectrometry Infrared spectroscopy (IR) Mass Spectrometry (MS) Nuclear magnetic resonance

EXPRESSIONS OF CONCENTRATION Concentration is the amount of solute in a known amount of solution Concentration = Amount of solute Amount of solution Molarity (M) Formality (F) Normality (N) Molality (m) Part per thousand (ppt) Parts per million (ppm) Parts per billion (ppb) Percent concentration (%w/w, %w/v, %v/v)

 Molarity (M) = # moles solute # liters of solution

This unit describes what exists at equilibrium

Molality (m) = #moles of solute #kilograms of solvent Formality (F) = # moles solute # liters of solution

This unit describes how to make a solution, not what exists at equilibrium (aka analytical molarity)

 Normality (N) = # equivalents solute # liters of solution Equivalents = Weight equivalent weight Equivalent weight = formula weight n where, n is the number of e or H+ ions or OH- ions N = (Formality) x (#electrons transferred) or = (Formality) x (#H+ neutralized) or = (Formality) x (#OH- neutralized) Eg. 0.100 N Na2CO3 solution The solution contains 0.100 equivalents Na2CO3 Rxn with H+ : CO32- + 2H+ H2O + CO2 1 L solution contains 0.1 equivalents Na2CO3 0.10 equivalent Na2CO3 0.050 mol Na2CO3

 Parts per thousand (ppt ) = g solute 103 g solution Parts per million (ppm) = (mg mL-1) = g solute 106 g solution mg solute Liter solution

For dilute aqueous solutions, 1 ppm = 1 g solute 106 mL solution = 1 g solute mL solution = 1 mg/L Parts per billion (ppb) = g solute 109 g solution For dilute aqueous solutions, 1 ppb = 1 g solute 109 mL solution = 1 ng solute mL solution = 1 ng/L

 Weight percent =

(%w/w)

Weight of solute x 100% Weight of solution

Volume percent = Volume of solute x 100% (%v/v) Volume of solution

Weight-volume = Weight of solute x 100% (%w/v) Volume of solution

Commercial aqueous reagents are usually sold in (%w/w) Example: 37% is labeled on a HCl reagent bottle. This means that it contains 37 g HCl per 100 g solution

 Density

mass of substance volume of substance

(g mL-1 is the most usual unit for density)

Specific Gravity = Mass of substance Mass of equal volume of water = Density of substance Density of water

Specific gravity is more often used in commercial reagents than density (The temperature must be specified)

PREPARATION OF SOLUTION Example: Describe the preparation of 250 mL of 0.100 M Na from reagent grade NaOH [Known MW: NaOH = 40, Na= 23.00] 1. Calculate the weight (g) of NaOH that is equivalent to the required moles of Na in solution

Calculations ???

2. Weigh ??? g of solid (generally 0.1 mg, ie up to 4 decimal places in grams) 3. Dissolve in water, transfer (quantitatively with rinsings) to a 250 mL volumetric flask, and dilute to the mark

DILUTION OF SOLUTION The moles solute in concentrated (1) solution equals the moles in dilute (2) solution

M1 V1 = M2 V2
Example: Describe the preparation of 50 mL of 0.100 M NaOH solution from a 0.5 molar solution Calculations How to ??? Glassware requirement: ?? mL pipet and ?? mL volumetric flask