Welcome to CH 315 Analytical Instrumentation

Course Description
This course allows students to apply their skills and knowledge of analytical chemistry and instrumentation to the theory and practice of chemical sampling and analysis used by the MOE (Ministry of the Environment). The problems presented in the course will emphasis the chemical analysis of environmental samples utilizing MOE procedures and equipment available at the college.

Course Learning Outcomes

Upon successful completion students will be able to: Identify and follow appropriate procedures for sample collection, preparation and analysis. Solve mathematical problems related to concentration and dilution. Describe, explain and solve problems related to redox titration. Operate AAS, GC, HPLC, Ion Selective Electrodes and Spectrophotometers. Collect, record, analyze, interpret and present data obtained from experiments with the above instruments according to MOE procedures.

Dr. Andrew Baer

Office Hours Monday: 12:30 pm 2:00 pm (HPSTC 428) Wednesday: 10:30 am 12:00 pm (HPSTC 428) Friday: 12:30 pm 2:00 pm (HPSTC 428) or by appointment Email: abaer@centennialcollege.ca Lecture: Thursday: 10:30 am 12:20 pm (Sec 061-062) (HPSTC 422) Textbooks: Harris, Daniel C., Exploring Chemical Analysis, 5th Ed., W. H. Freeman and Company, 2012. Harvey, David, Analytical Chemistry 2.0 Available Online at:
http://www.asdlib.org/onlineArticles/ecourseware/Analytical%20Chemistry%202.0/Text_Files_files/AnalChem2.0.pdf.

Course Overview
Week Jan. 7th Jan. 14th Jan. 21st Jan. 28th Feb. 4th Feb. 11th Feb. 18th Feb. 25th March 4th March 11th March 18th March 25th April 1st April 8th April 15th April 22nd Topic Concentration, Dilution and Statistics Spectrophotometry/AAS Quality Assurance Sampling and Sample preparation Introduction to Chromatography Midterm 1 Introduction to Chromatography GC Reading Week HPLC Redox and Redox titrations Midterm 2 Redox and Redox titrations Ion Selective Electrodes Review Final Exam (Exam Week) Tentative Date Tentative Date Notes

Course Evaluation
Evaluation Assignments/Quizzes = 5.0 % Midterm test 1 = 12.5 % Midterm test 2 = 12.5 % Final Exam = 25.0 % Laboratory = 45.0 % Course Materials Course lectures will be available on the course eCentennial site. I would like everyone to print out a copy of the notes and bring them to the lecture. You will really struggle if you dont have the notes. You will need to scribble and add things to the notes during class.

Laboratory
Labs: Friday: 2:30 pm 5:20 pm (Sec 061) (HPSTC 440) Friday: 5:30 pm 8:20 pm (Sec 062) (HPSTC 440)

Laboratory Requirements: Lab Manual: CH315 Analytical Instrumentation (available for download from eCentennial) Lab Coat, Safety Glasses, Long Pants, Closed Shoes A notebook and pen Locker (contact Enrolment Services for rental)

Laboratory Overview
Date Jan. 11th Jan. 18th Jan. 25th Feb. 1st Feb. 8th Feb. 15th Feb. 22nd March 1st March 8th March 15th March 22nd March 29th April 5th April 12th April 19th April 22nd Topic Introduction / Safety Lab 1 (all students) Lab 2 (all students) Lab 2 (all students) Begin Lab Rotation (Lab 3 8) Lab Rotation (Lab 3 8) Lab Rotation (Lab 3 8) Lab Rotation (Lab 3 8) Reading week Lab Rotation (Lab 3 8) Lab Rotation (Lab 3 8) Good Friday Lab Rotation (Lab 3 8) End Lab Rotation (Lab 3 8) Makeup Lab Exam Week (No Labs) Lab 2 due Labs due as appropriate. Labs due as appropriate. Labs due as appropriate. No labs due Labs due as appropriate. Labs due as appropriate. No labs due Labs due as appropriate. Labs due as appropriate. Final Lab due. Lab 1 due Notes

Ways of Expressing Concentrations of Solutions

Concentration expressions
The concentration of a solution is the amount of solute present in a given quantity of solvent or solution.
Molarity Normality Parts per million Parts per billion Parts per trillion

Concentration Expressions
High to Mid-range Concentrations: Molarity (mol/L) or Normality (mol/L) Very Low Concentrations: ppm or mg/L ppb or g/L ppt or ng/L

Molarity
You should be able to calculate molarity:

M = molarity =

mol solute L solution

Calculating Molarity
What is the molarity of a solution made by dissolving 2.355g of sulfuric acid (H2SO4) in water and diluting to a final volume of 50.0 mL?

Concentration Units (Molarity)

What mass of KCl would you need to prepare 250.0 mL of a 0.340 M solution of KCl (MW = 74.55 g/mol) in water:

Concentration Units (Molarity)

Calculate the molarity of a solution containing 34.2 g of NaCl(s) (MW = 58.5 g/mol) in 250.0 mL of solution.

Concentration Units (Normality)

The Normality of a solution is defined as the number of equivalents of solute per liter of solution.

# of equivalent N = normality = L solution

What is an equivalent?

Concentration Units (Normality)

An equivalent of a substance is the amount of that substance in moles which supplies or consumes one mol of reactive species. The equivalent weight is the mass of a substance which supplies or consumes one mol of reactive species.
# of equivalent = mass equivalent weight
molecular weight reaction capacity

equivalent weight =

Concentration Units (Normality)

In acid-base chemistry: For an acid: Reaction capacity = # of H+ produced by the acid. The equivalent weight of acid is equal to its molecular weight divided by the number of hydrogen atoms produced by the acid. For a base: Reaction capacity = # of H+ that the base would react with. The equivalent weight of a base is equal to its molecular weight divided by the number of H+ the base would react with.

Concentration Units (Normality)

Determine the reaction capacity of the following: HCl H2SO4 H3PO4 CH3OOH NaOH Ba(OH)2 Na2CO3

Concentration Units (Normality)

What is the Molarity and Normality of a solution made by dissolving 17.5 grams of NaOH in 200 ml of water?

Concentration Units (Normality)

What is the Molarity and Normality of a solution made by dissolving 49.0 grams of Na2CO3 in 1 L of water?

Dilutions
The ability to prepare a solution of a specific concentration from a stock is very important in analytical chemistry:

C1 V1 = C2 V2

Calculating dilutions
How would you prepare 500.0 mL of 0.2500 M NaOH solution starting from a concentration of 1.000 M?

Solution Stoichiometry
Molarity is useful in performing stoichiometry calculations on substances in solutions.
Balanced equation: aA + bB 1. 2. 3. 4. c C + dD Find the number of moles of the first reactant (A). Use the coefficients of the balanced equation to find the mole ratio of the first reactant (A) to the second reactant (B). Calculate the number of moles of the second reactant (B). Use this to find the amount of the second reactant.

Solution Stoichiometry
Stomach acid, a dilute solution of HCl in water, can be neutralized by reaction with NaHCO3, according to the equation: HCl(aq) + NaHCO3(aq) NaCl(aq) + H2O(l) + CO2(g)

How many milliliters of 0.125 M NaHCO3 solution are needed to neutralize 18.0 mL of 0.100 M HCl?

Solution Stoichiometry
1. Find the number of moles of HCl in 18.0 mL of a 0.100 M solution:
Moles of HCl = 18.0 mL 1L 0.100 mol = 1.80 x 10 -3 mol 1000 mL 1L

2. Check the coefficients of the balanced equation: 1 mol HCl reacts with 1 mol NaHCO3 3. Calculate the volume of the 0.125 M NaHCO3 solution needed:
1 mol NaHCO 3 1L solution 1.80 x 10 mol HCl = 0.0144 L 1 mol HCl 0.125 mol NaHCO 3
-3

4. 14.4 mL of 0.125 M NaHCO3 solution is needed to neutralize 18.0 mL of the 0.100 M HCl solution.

Calculating Dilutions
If 15.0 mL of a 12.0 M HCl solution were diluted to a volume of 100.0 mL, what would the concentration of the new solution be?

Calculating Dilutions
How would you prepare 60.0 mL of 0.20 M HNO3 from a stock solution of 4.00 M HNO3?

Concentration Units (ppm, ppb, ppt)

In chemistry sometimes substances are at very low concentrations. They are often expressed as parts per million (ppm), parts per billion (ppb) or parts per trillion (ppt).

mass of substance ppm = 10 6 mass of sample mass of substance ppb = 10 9 mass of sample mass of substance ppt = 1012 mass of sample

How much is a part per million (ppm)?

1 ppm = 1 piece in 1,000,000 pieces In an aqueous solution 1 ppm = 1 mg/L (assuming 1 kg water = 1 L water). It is the equivalent of 30 seconds out of a year.

mass of substance ppm = 10 6 mass of sample

How much is a part per billion (ppb)?

1 ppb = 1 piece in 1,000,000,000 pieces In an aqueous solution 1 ppb = 1 g/L (assuming 1 kg water = 1 L water). It is the equivalent of 3 seconds out of a century.

mass of substance ppb = 10 9 mass of sample

How much is a part per trillion (ppt)?

1 ppt = 1 piece in 1,000,000,000,000 pieces. In an aqueous solution 1 ppt = 1 ng/L (assuming 1 kg water = 1 L water). It is the equivalent of 3 seconds out of one hundred thousand years.

mass of substance ppt = 1012 mass of sample

Using ppm in a calculation

An 11.0 kg sample of soil was extracted and produced 2.732 g of oil. How many ppm of oil were in the soil? Mass of total sample = 11.0 kg = 1.10 x 104 g Mass oil = 2.732 g ppm = (2.732 g / 1.10 x 104 g) x 106 = 248.4 ppm = 248. ppm

Using ppm in a calculation

Calculate the ppm concentration of 2.7 x 10-3 mg of gold (Au) in 450 mL of aqueous solution: The density of a dilute water sample is 1.00 g/mL.

Mass of gold in g = 2.7 x 10-3 mg / 1000 = 2.7 x 10-6 g Mass of water = 450 mL (1.00 g/mL) = 450. g ppm = (2.7 x 10-6 g / 450. g) x 106 = 0.006 ppm

Using ppm in a calculation

Calculate the concentration in ppm of K present in a solution prepared by dissolving 2.0 g of pure KNO3 and diluting to a volume of 1L MW(KNO3) = 101.11 g/mol, MW (K) = 39.1 g/mol

Using ppm in a calculation

Calculate the concentration of Na+ in ppm, present in a solution prepared by dissolving 1.002 g of pure NaBr and diluting to a volume of one liter. Calculate the molarity of Na+ as well. NaBr = 23.0 g/mol + 79.9 g/mol = 102.9 g/mol

Using ppm in a calculation

Calculate the mass of KCl required to make 1 L of a 1000 ppm K+ stock solution. K = 39.1g/mol KCl = 74.6g/mol

Using ppb in a calculation

Calculate the mass of CaCl2 needed to prepare 1000mL of a solution that is 100 ppb in Ca.

Statistics

Evaluation of Analytical Data

Mean ( x ): Also known as the average. Obtained by dividing the sum of replicate measurements by the number of measurements in the set. Given mathematically as:
N

x
x=
i =1

where xi represents the individual values of x making up the set of N replicate measurements.

Evaluation of Analytical Data

Formula for sample and population means:
N

x
x=
i =1

N i

x
=
i =1

N For an infinite set of data the mean is called the population mean () and is calculated in the same manner as the sample mean.

Since an infinite set of data cannot exist, the population mean can never actually be measured. However as the number of measurements in a set of data increases x approaches .

Evaluation of Analytical Data

Standard deviation: Standard deviation is a measure of how closely data is clustered around the mean. A small standard deviation means the data is clustered close to the mean. A large standard deviation means the data can deviate significantly from the mean. The standard deviation is a measure of the precision of the data.

Evaluation of Analytical Data

The population standard deviation () is the standard deviation of an infinite set of data. It can never be measured but is approached as the number of measurements increases.
N

(x )
i

i =1

Evaluation of Analytical Data

The sample standard deviation (s) should be used in place of the population standard deviation () when analyzing small sample sets:
N 2 ( ) x x i

s=

i =1

N 1

In the sample standard deviation N (population size) is replaced in the denominator of the standard deviation equation with (N-1), which is known as the number of degrees of freedom. As a rule of thumb, the sample set is considered small when N < 30.

Calculating Standard Deviations

5 samples of copper ore were analyzed to determine their copper content yielding values of 16.54%, 16.64%, 16.61%, 16.67% and 16.70%.

Calculating Standard Deviations

5 samples of aspirin were analyzed to determine their aspirin content yielding values of 75.54%, 75.34%, 75.61%, 74.67% and 74.70%.

Evaluation of Analytical Data

Confidence Intervals:
It is impossible to determine the population mean () or population standard deviation () from a small data set. A confidence interval (CI) is a range around a measured mean in which there is a specific probability of finding the population mean.

Confidence Intervals

ts =x n
s = measured standard deviation n = number of observations t = Value of Students t

Confidence Intervals
Values of Students t:

Calculating Confidence Intervals

5 samples of aspirin were analyzed to determine their aspirin content yielding values of 75.54%, 75.34%, 75.61%, 74.67% and 74.70%. Find the 50% and 90% confidence intervals for the aspirin content: