Royal Military College of Canada

Research Groups at RMC

Analytical Sciences Group

Undergraduate Teaching, Research and Training

The ASG is taking an active role in the development of analytical skills for students at the undergraduate level. The ASG conducts a fourth year undergraduate laboratory, taught by David Kelly, using selected techniques and laboratory equipment. The course, entitled CCE 441 Instrumental Analysis, provides officer cadets with an introduction to some of analytical techniques and laboratory practices that an officer may need to interpret during a career in the Canadian Forces. Students are supervised by selected ASG staff members and carry out exercises simulating real world equipment validation, experimental design, error analysis and decision-making based on environmental land use guidelines.

Specific exercises include:

The Analysis of Polyaromatic Hydrocarbons (PAHS) in Soil by Gas Chromatography - Mass Spectrometry (GC-MS)
The Analysis of Trace Elements in Water by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
The Analysis of Cyanide by Ion Chromatography (IC)
Atomic Absorption Analysis of Manganese in Steel
Polymer Analysis using Neutron Activation

Experiment 1: The Analysis of Polyaromatic Hydrocarbons (PAHS) in Soil by Gas Chromatography - Mass Spectrometry (GC-MS)

Experiment objectives:

To provide direct experience of the operation of extraction and analysis instrumentation.
To use analytical data as decision-making tool. In this instance, in an environmental context.

Before commencing the experiment cadets, are instructed to watch a PowerPoint written and narrated by David Kelly. The presentation provides information regarding the following points:

Details of PAH structure, formation, occurrence, and toxicity.
A discussion of the principles of extraction and the use of surrogates.
A brief review of gas chromatography and mass spectrometry.
An overview of the important of laboratory QA/QC

Two soils and one sediment sample is extracted, along with appropriate QA/QC samples. The samples are analyzed for the presence of polyaromatic hydrocarbons (PAHs). Pressurized solvent extraction is used to demonstrate the speed and efficiency of this method. Although up to sixteen PAHs are commonly analyzed in soil and water, the experiment focuses on the four PAHs shown below:


naphthalene [C₁₀H₈]	phenanthrene [C₁₄H₁₀]

anthracene [C₁₄H₁₀]	benzo(a)anthracene [C₁₈H₁₂]

The efficiency of extraction is assessed for each of the PAHs by comparison with its deuterated analogue. In addition to the extraction and analysis of samples, students are expected to develop a programme of QA/QC analyses. This is a student-based design activity.

Gas chromatography – mass spectrometry (GC-MS) is used to separate and quantify the PAHs of interest. The analytical data produced is compared with calibration standards and converted to PAH in soil and sediment concentrations. These concentrations are then compared to appropriate environmental regulations.

On completion of the experiment students become:

Experienced in the implementation of standard test methods.
Familiar with the operation of automated extraction equipment and GC-MS instrumentation.
Able to discuss the use of surrogate standards and their use for the correction of variations in extraction efficiency and system fluctuations.
Aware of the importance of QA/QC, such as duplicate, blank and control data in the acceptance of sample data.
Aware of provincial regulations regarding soil quality, land use and remediation and the role of the Canadian Council of Ministers of the Environment (CCME). Capable of assessing analytical data in the text of such regulations.
Capable of reporting data in a range of scientifically valid formats.

Experiment 2: The Analysis of Trace Elements in Water by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

Experiment objectives:

To provide direct experience of the operation of analytical instrumentation.
To use analytical data as decision-making tool, in this instance in an environmental context.

Before commencing the experiment, cadets are instructed to watch a PowerPoint written and narrated by David Kelly. The presentation provides information regarding the following points:

The principles of method validation
The use of internal standards
A brief review of inductively coupled plasma generation and mass spectrometry

ICP-MS is capable of quantifying the concentration of almost every element in the periodic table from lithium to uranium in aqueous solution. In this experiment an ICP-MS instrument is tuned and calibrated. Replicate data are then obtained from standard solutions. Instrument responses are converted to aqueous concentrations by the use of calibration solutions, and the results obtained are used to validate the instrument. Accuracy, precision and detection limit are determined and reported in a manner similar to that used by instrument manufacturers. The concentrations of 16 elements (rather than ions or compounds) are regulated for Canadian Drinking Water Quality. A slightly different list, of 13 elements, is regulated for freshwater. In this experiment, six elements arsenic, cadmium, lead, manganese, selenium and uranium are studied. Instrument performance is monitored using indium as an internal standard.

The quality of freshwater and drinking water in Canada is regulated. Validation results generated by students are assessed against the current Drinking Water Guidelines. Three components are required for reporting, an application note, a sample calculation and responses to questions. The application note format is similar to that used for a scientific journal communication, but follows the same basic format of a formal report.

On completion of the experiment students become:

Experienced in the implementation of standard test methods.
Familiar with the operation of automated ICP-MS equipment and aware of operational limitations such as isobaric interference.
Able to discuss the use of internal standards and their use for the correction of variations in instrument performance, sample evaporation and other typical system fluctuations.
Able to use replicate analytical data to obtain instrument validation parameters such as precision, accuracy and detection limit.
Aware of the importance of QA/QC, such as duplicate, blank and control data in the acceptance of sample data.
Aware of federal, provincial and local regulations regarding water quality and capable of assessing analytical data in the text of such regulations.
Capable of reporting data in a range of scientifically valid formats.

Experiment 3: The Analysis of Cyanide by Ion Chromatography (IC)

This experiment is based on a fictional scenario in which analysis of the cyanide anion is required. The scenario has been constructed such that individuals might suffer severe dehydration or exposure to lethal levels of cyanide. Decision-making requires the determination of cyanide and a scientifically valid estimate of the reliability of this result, i.e. a determination of error. In the interest of student safety, cyanide is replaced in this experiment by a significantly less toxic anion. The health risks associated with this substitute are similar to those of other laboratory chemicals. Experimental design and data interpretation are not affected by this substitution.

Experiment objectives:

To become familiar with the concept of experimental design, i.e. the use of instrumentation to meet a specific requirement.
To develop further experience in the determination and interpretation of error.
To interpret results in the context of regulations.

Before commencing the experiment cadets are instructed to watch a PowerPoint written and narrated by David Kelly. The presentation provides information regarding the following points:

The chemistry and toxicity of cyanide.
The theory and practice of ion chromatography.
A brief review of error analysis.
A description of the format required for reporting

The experiment is a design exercise. Standard reference solids and solutions are provided, along with appropriate glassware. An experiment demonstrator and laboratory technician are present to offer guidance with respect to potential experimental approaches and the operation of ion chromatography (IC) instrumentation. Design and implementation is student-lead.

On completion of the experiment students become:

Experienced in the design of experimental parameters to meet specific requirements.
Familiar with the operation of ion chromatography equipment.
Able to discuss the determination of error based on replicate analyses and on the examination of error in individual experimental steps.
Aware of the importance of quality control data.
Aware of drinking water quality regulations and guidelines, and of the health-based factors upon which such guidelines and regulations are based.

Experiment 4: Atomic Absorption Analysis of Manganese in Steel

Experiment objectives:

To provide experience of the widely used technique of acid digestion.
To develop skills in the use of error and formal reporting.

Before commencing the experiment cadets are instructed to watch a PowerPoint written and narrated by David Kelly. The presentation provides information regarding the following points:

The scope and principles of acid digestion.
The theory of atomic absorbance analysis.
Error, quality control and reporting

In this experiment a steel sample is digested in duplicate in an acidic solution, along with a control and blank sample. The digests are analysed by atomic absorption spectroscopy (AA) relative to a set of calibration standards. Three components are required for reporting, are a formal report, sample calculation and Question Responses.

On completion of the experiment students become:

Familiar with the principle of acid digestion.
Able to discuss the theory and practical of atomic absorption spectroscopy.
Aware of the importance of QA/QC, such as duplicate, blank and control data in the acceptance of sample data.
Able to determine error based in replicate data and estimation methods.

Experiment 5: Polymer Analysis using Neutron Activation

Experiment Objectives

To become familiar with neutron activation analysis, the use of multi-channel analysers (MCA) and gamma-ray spectroscopy.
To gain experience of NAA as a non-destructive technique and be able to compare this form of analysis with those requiring sample digestion or extraction.

Before commencing the experiment cadets, are instructed to watch a PowerPoint written and narrated David Kelly. The presentation provides information regarding the following points:

The principles of non-destructive testing
The neutron activation process and the decay of activated nuclei.
The theory and practice of gamma-ray spectroscopy.

In this experiment the copper and titanium content of an organic polymer material is measurement. Metal content can compromise the long-term stability of polymers and analyses must be performed to confirm that particular samples are of appropriate quality for their final application. The metal content of polymers can be assessed by a combination of ashing and/or acid digestion, followed by an appropriate analysis using atomic absorption (AA), inductively coupled plasma – mass spectrometry (ICP-MS) or inductively coupled plasma – optical emission spectroscopy (ICP-OES). Such analyses are time consuming and may under estimate the true metal content. NAA offers a rapid and efficient method of analysis, and preserves the sample studied for further testing.

Activation: Na-23 + à Na-24

Decay: Na-24 à Mg-24 + 2 b + 2 g

A calibration standard containing copper and titanium is activated using the SLOWPOKE-2 reactor facility. The sample is then transferred to a shielded gamma ray spectrometer to determine the extent of activation by measuring decays occur with a specific gamma energy. This analysis determines the efficiency of both activation and decay detection. Similar activation and measurement occurs for the polymer sample. QA/QC is also performed, which includes a control sample and duplicate analysis.

On completion of the experiment students become:

Experienced in the use of neutron activation and gamma ray spectroscopy.
Familiar with the principles of non-destructive testing.
Aware of the importance of QA/QC, such as duplicate and control data in the acceptance of sample data.
Familiar with the use of background noise in the determination of error.

Undergraduate Teaching

Undergraduate and graduate students conducting research in other areas of the department are permitted to use equipment within the ASG facility. Students are able to carry out their own analyses from sample preparation to instrumental analysis to data interpretation under the supervision of experienced ASG staff.

Some recent experiments include:

Digestion and analysis of Lead/Tin/Bismuth alloys using microwave digestion and ICP-MS.
Zirconium and Hafnium analysis by NAA.
ICP-MS analysis of dysprosium solutions.
Evaluation of hydrocarbon contamination in aircraft wiring.
Hydrocarbon bioremediation studies.

The ASG is also actively participating co-operative education programs with the University of Waterloo and St. Lawrence College.

Co-op students are exposed to: