Instrumental methods in analytical chemistry I

chemical sciences

intermediate

Prerequisites.

Basic knowledge obtained during the first-degree studies in the field of mathematical analysis, physics, general chemistry, physical chemistry, organic chemistry, and analytical chemistry.

Level: intermediate.

Lectures and auditorium exercises are the first part of the compulsory classes.

They are designed to familiarize the students with the most important methods and techniques of instrumental analytical chemistry in the analysis of the composition of solutions under stagnant conditions so that students in their future professional activity could independently solve problems arising in the determination of selected analytes in real samples and, in particular, deliberately choose the appropriate analytical method and propose the most appropriate determination procedure.

Lecture and auditorium exercise classes.

1. D. A. Skoog, F. J. Holler, S. R. Crouch, "Principles of Instrumental Analysis", 7th edition, Cengage Learning, 2017.

2. Z. Galus, "Fundamentals of Electrochemical Analysis", Second (revised) edition, E. Horwood, New York1, 1994.

3. A. J. Bard, L. R. Faulkner, "Electrochemical Methods: Fundamentals and Applications", Wiley, 2nd edition, New York, NY, 2001.

Subject learning outcomes for practice.

Knowledge.

EK1. The student lists the types of noise in the analytical determination, predicts their origin and proposes hardware and software methods of their elimination.

EK2. The student explains the concept of accuracy, precision, and reliability of analytical determinations.

EK3. The student discusses the concept of limit of detection and the linear dynamic concentration range of an analytical assay.

EK4. The student handles the parameters of analytical assays, including selectivity, specificity, repeatability, reproducibility, resolution and recovery.

EK5. The student predicts interference of the analytical signal by interfering substances.

EC6. The student proposes methods of instrumental chemical analysis that are best suited to solve the given problem of analyte determination.

EK7. Participates in solving analytical chemistry problems during classes.

ECTS description for the lecture class

1. Class attendance: 30 h.

2. Preparation for classes: 10 h.

3. Preparation for verification: 20 h.

4. Consultation with the instructor: 15 h.

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Total: 75 h, i.e., 3 ECTS points.

Subject learning outcomes for the exercise class.

EK1. The student t lists the types of noises in the analytical determination, predicts their origin and proposes hardware and software methods of their elimination.

EK2. The student discusses the accuracy, precision and reliability of analytical determination.

EK3. The student explains the concept of limit of detection and the linear dynamic concentration range of an analytical assay.

EK4. The student uses concepts of analytical assays' parameters, including selectivity, specificity, repeatability, reproducibility, resolution, and recovery.

EK5. The student predicts interference of the analytical signal by interfering substances.

EC6. The student participates in solving analytical chemistry problems during classes.

ECTS description for the auditorium exercise class.

1. Class attendance: 15 h.

2. Preparation for classes: 10 h.

3. Preparation for verification: 15 h.

4. Consultation with the instructor: 10 h.

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Total: 50 h, i.e., 2 ECTS points.

Methods of evaluating learning outcomes:

Lecture.

For EK1-EK5: written exam

Criteria for evaluating learning outcomes for lectures:

EK1. Written exam.

Rating 5. Verification shows that the student describes and explains the physicochemical phenomena underlying various instrumental methods of chemical analysis without noticeable shortcomings.

Rating 4.5. The verification shows that the student almost fully correctly describes and explains the physicochemical phenomena underlying the instrumental methods of chemical analysis, but does not meet the criteria for a higher grade.

Rating 4. Verification shows that the student describes and explains physicochemical phenomena underlying various instrumental methods of chemical analysis to a large extent, but does not meet the criteria for a higher evaluation.

Rating 3.5. The verification shows that the student describes and explains the physicochemical phenomena underlying various instrumental methods of chemical analysis to a large extent correctly but inconsistently, but does not meet the criteria for a higher grade.

Rating 3. Verification shows that in most test cases the student describes and explains the physicochemical phenomena underlying various instrumental methods of chemical analysis, but does not meet the criteria for a higher grade.

Rating 2. Verification does not show that the student describes and explains the physicochemical phenomena underlying the various instrumental methods of chemical analysis, nor that he or she meets the criteria for a higher assessment.

EK2. Written exam.

Rating 5. The verification shows that the student shows the most characteristic applications of each instrumental method of chemical analysis without noticeable shortcomings.

Rating 4.5. The verification shows that the student almost fully correctly indicates the most characteristic applications of individual instrumental methods of chemical analysis, but does not meet the criteria for a higher grade.

Rating 4. The verification shows that the student largely correctly identifies the most characteristic applications of the different instrumental methods of chemical analysis, but does not meet the criteria for a higher mark.

Rating 3.5. The verification shows that the student to a large extent correctly but inconsistently indicates the most characteristic applications of individual instrumental methods of chemical analysis, but does not meet the criteria for a higher grade.

Rating 3. Verification shows that in most test cases the student shows the most typical applications individual instrumental methods of chemical analysis, but does not meet the criteria for a higher grade.

Rating 2. Verification does not show that the student indicates the most appropriate applications of particular instrumental methods of chemical analysis, nor that he or she meets the criteria for a higher grade.

EK3. Written exam.

Rating 5. Verification shows that the student proposes instrumental methods of chemical analysis most suitable for the determination of selected analytes in gas mixtures and solutions without noticeable shortcomings.

Rating 4.5. Verification shows that the student proposes the most appropriate instrumental methods of chemical analysis for the determination of selected analytes in gas mixtures and solutions, but does not meet the criteria for a higher grade.

Rating 4. Verification shows that the student largely correctly proposes the instrumental methods of chemical analysis most suitable for the determination of selected analytes in gas mixtures and solutions, but does not meet the criteria for a higher assessment.

Rating 3.5. Verification shows that the student proposes, to a large extent correctly but inconsistently, the instrumental methods of chemical analysis most suitable for the determination of selected analytes in gas mixtures and solutions, but does not meet the criteria for a higher grade.

Rating 3. Verification shows that in most test cases the student proposes instrumental methods of chemical analysis most suitable for the determination of selected analytes in gas mixtures and solutions, but does not meet the criteria for a higher assessment.

Rating 2. Verification does not demonstrate that the student proposes the most suitable instrumental methods of chemical analysis for the determination of selected analytes in gas mixtures and solutions, nor that he or she meets the criteria for a higher grade.

EK4. Written exam.

Rating 5. Verification shows that without noticeable shortcomings, the student develops the conditions for the determination of analytes in gas mixtures and solutions using the selected instrumental method of chemical analysis.

Rating 4.5. The verification shows that the student almost fully correctly develops the conditions for the determination of analytes in gas mixtures and solutions using the selected instrumental method of chemical analysis, but does not meet the criteria for a higher grade.

Rating 4. Verification shows that to a large extent the student correctly develops the conditions for the determination of analytes in gas mixtures and solutions using the selected instrumental method of chemical analysis, but does not meet the criteria for a higher grade.

Rating 3.5. The verification shows that to a large extent the student correctly but inconsistently develops the conditions for the determination of analytes in gas mixtures and solutions using the selected instrumental method of chemical analysis, but does not meet the criteria for a higher grade.

Rating 3. Verification shows that in most test cases the student develops the conditions for the determination of analytes in gas mixtures and solutions using the selected instrumental method of chemical analysis, but does not meet the criteria for a higher assessment.

Rating 2. Verification does not show that the student develops the conditions for the determination of analytes in gas mixtures and solutions using the selected instrumental method of chemical analysis, or that he or she meets the criteria for a higher grade.

EK5. Written exam.

Rating 5. Verification shows that, without noticeable shortcomings, the student is able to make independent decisions regarding the selection of instrumental methods of analytical chemistry most appropriate to solve a particular analytical problem.

Rating 4.5. Verification shows that the student is almost fully capable of making independent decisions regarding the selection of instrumental methods of analytical chemistry most appropriate to solve a specific analytical problem, but does not meet the criteria for a higher grade.

Rating 4. Verification shows that to a large extent the student is able to independently make decisions regarding the selection of instrumental methods of analytical chemistry most appropriate to solve a specific analytical problem, but does not meet the criteria for a higher assessment.

Rating 3.5. Verification shows that to a large extent, correctly but inconsistently, the student is capable of making decisions on his own

decision regarding the selection of instrumental methods of analytical chemistry most appropriate to solve a specific analytical problem, but does not meet the criteria for a higher grade.

Rating 3. Verification shows that in most test cases the student is able to independently make decisions regarding the selection of instrumental methods of analytical chemistry most appropriate to solve a specific analytical problem, but does not meet the criteria for a higher assessment.

Rating 2. Verification does not show that the student is capable of making his or her own decisions regarding the choice of instrumental methods

of analytical chemistry most suitable for solving a specific analytical problem, or that he or she meets the criteria for a higher grade.

The final grade x is determined based on the value:

st(w)= 5 if 4.5 < w; st(w)= 4.5 if 4.25 < w ≤ 4.5; st(w)= 4 if 3.75 < w ≤ 4.25; st(w)= 3.5 if 3.25 < w ≤ 3.75; st(w)= 3 if 2.75 < w ≤ 3.25; st(w)= 2 if w ≤ 2.75

and based on the following rule:

● if each of the final grades for the related classes is positive and their average is y, then x is determined from the formula x=st((y+z)/2), where z is the weighted average of grades from the verifications carried out, in which grade weights from exams are 2, and the weights of grades from other forms of verification are equal to 1

● if at least one final grade in related activities is 2 or failure, then x=2.

The written examination covers the elaboration of 10 problems.

To facilitate the evaluation, the following approximation is applied.

The maximum rating for the exam is 100 points.

Rating 2 (failure): result < 40 points

Rating 3 (satisfactory): 40 ≤ result < 50 points

Rating 3.5 (satisfactory plus): 50 ≤ result < 60 points

Score 4 (good): 60 ≤ result < 70 points

Rating 4.5 (good plus): 70 ≤ result of < 80 points

Rating 5 (very good): 80 ≤ result ≤ 100 points

Methods of evaluating learning outcomes:

Auditorium exercises.

For EK1-EK5: written test, continuous method. EK6: continuous method.

Criteria for evaluating learning outcomes for exercises:

EK1 Written test.

Rating 5. Verification demonstrates that the student lists the types of noise in the analytical assay, predicts their origin, and proposes hardware and software solutions for their elimination without any discernible shortcomings.

Rating 4.5. The verification shows that the student lists the types of noise in the analytical determination almost correctly, predicts their origin and proposes hardware and software methods of their elimination, but does not meet the criteria for a higher grade.

Rating 4. Verification shows that the student largely correctly lists the types of noise in the analytical assay, predicts their origin and proposes hardware and software methods of removing them, but does not meet the criteria for a higher rating.

Rating 3.5. The verification shows that the student largely correctly but inconsistently lists the types of noise in the analytical assay, predicts their origin and proposes hardware and software methods of removing them, but does not meet the criteria for a higher rating.

Rating 3. Verification shows that in most test cases the student lists the types of noise in the analytical assay, predicts their origin and suggests hardware and software solutions to remove them, but does not meet the criteria for a higher rating.

Rating 2. Verification does not show that the student does not list the types of noise in the analytical assay, does not predict their origin and does not propose hardware and software methods of their removal, or does not meet the criteria for a higher grade.

EK2 Written test.

Rating 5. Verification demonstrates that the student clarifies the concept of accuracy, precision and reliability of an analytical determination without noticeable shortcomings.

Rating 4.5. Verification shows that the student almost fully explains the concept of accuracy, precision and reliability of analytical determination, but does not meet the criteria for a higher rating.

Rating 4. Verification shows that the student largely correctly explains the concept of accuracy, precision and reliability of the analytical determination, but does not meet the criteria for a higher mark.

Rating 3.5. Verification shows that the student largely correctly but inconsistently explains the concept of accuracy, precision and reliability of the analytical determination, but does not meet the criteria for a higher rating

Rating 3. Verification shows that the student clarifies the concept of accuracy, precision, and reliability of an analytical determination in most test cases, but does not meet the criteria for a higher rating.

Rating 2. The verification does not show that the student neither clarifies the concept of accuracy, precision and reliability of the analytical determination, nor does he or she meet the criteria for a higher grade.

EK3 Written test

Rating 5. Verification shows that the student covers the concept of limit of detection and the linear dynamic concentration range of the analytical assay without noticeable shortcomings.

Rating 4.5. Verification shows that the student discusses the concept of the limit of detection and the linear dynamic concentration range of the analytical assay almost fully correctly, but does not meet the criteria for a higher grade.

Rating 4. Verification shows that the concept of limit of detection and the linear dynamic concentration range of the analytical assay the student largely correctly covers, but does not meet the criteria for a higher mark.

Rating 3.5. Verification shows that the student largely correctly but inconsistently discusses the concept of the limit of detection and the linear dynamic concentration range of the analytical assay, but does not meet the criteria for a higher grade.

Rating 3. The review shows that the student covers the concept of limit of detection and the linear dynamic concentration range of the analytical assay in most test cases, but does not meet the criteria for a higher score.

Rating 2. The verification shows that the student neither addresses the concept of the limit of detection and the linear dynamic concentration range of the analytical assay nor does he or she meets the criteria for a higher grade.

EK4 Written test

Rating 5. Verification demonstrates that the student handles analytical assay parameters, including selectivity, specificity, repeatability, reproducibility, resolution, and recovery, with no discernible deficiencies.

Rating 4.5. Verification shows that the student handles the parameters of analytical assays almost completely correctly, including selectivity, specificity, repeatability, reproducibility, resolution and recovery, but does not meet the criteria for a higher rating.

Rating 4. Verification demonstrates the student largely correctly uses analytical assay parameters, including selectivity, specificity, repeatability, reproducibility, resolution, and recovery, but does not meet the criteria for a higher grade.

Rating 3.5. Verification shows that the student extensively but inconsistently handles analytical assay parameters, including selectivity, specificity, repeatability, reproducibility, resolution, and recovery, but does not meet the criteria for a higher grade.

Rating 3. Verification shows that the student uses analytical assay parameters in most test cases, including selectivity, specificity, repeatability, reproducibility, resolution, and recovery, but does not meet the criteria for a higher rating.

Rating 2. Verification shows that the student neither uses the parameters of the analytical assays, including selectivity, specificity, repeatability, reproducibility, resolution and recovery, nor meets the criteria for a higher grade.

EK5 Written test

Rating 5. The verification shows that the student predicts interference of the analytical signal by interfering substances without any noticeable shortcomings.

Rating 4.5. The verification shows that the student almost correctly predicts the interference of the analytical signal by interfering substances, but does not meet the criteria for a higher rating.

Rating 4. The review shows that the student predicts interference with the analytical signal by interfering substances to a large extent, but does not meet the criteria for a higher grade.

Rating 3.5. The review shows that the student largely correctly but inconsistently predicts interference with the analytical signal by interfering substances, but does not meet the criteria for a higher rating.

Rating 3. Verification shows that the student predicts interference with the analytical signal by interfering substances in most test cases, but does not meet the criteria for a higher rating.

Rating 2. The verification shows that the student neither predicts interference with the analytical signal by interfering substances, nor meets the criteria for a higher grade.

EC6. Written test

Rating 5. Verification shows that without noticeable shortcomings, the student proposes methods of instrumental chemical analysis that are best suited to solve the given problem of analyte determination.

Rating 4.5. The verification shows that the student proposes the methods of instrumental chemical analysis that are best suited to solve the given problem of analyte determination, but does not meet the criteria for a higher grade.

Rating 4. Verification shows that the student proposes methods of instrumental chemical analysis most suitable for solving the given problem of analyte determination to a large extent, but does not meet the criteria for a higher evaluation.

Rating 3.5. The verification shows that, to a large extent, correctly but inconsistently, the student proposes the methods of instrumental chemical analysis best suited to solve the given problem of analyte determination, but he or she does not meet the criteria for a higher grade.

Rating 3. Verification shows that in most test cases the student proposes the methods of instrumental chemical analysis best suited to solve the given problem of analyte determination, but does not meet the criteria for a higher assessment.

Rating 2. Verification shows that the student neither proposes methods of instrumental chemical analysis that are best suited to solve the given problem of analyte determination, nor meets the criteria for a higher grade.

The written test covers solving 10 tasks.

The final grade x is determined based on the value:

st(w) = 5 if 4.5 < w; st(w) = 4.5 if 4.25 < w ≤ 4.5; st(w)= 4 if 3.75 < w ≤ 4.25; st(w) = 3.5 if 3.25 < w ≤ 3.75; st(w)= 3 if 2.75 < w ≤ 3.25; st(w)= 2 if w ≤ 2.75

and based on the following rule:

● if each of the final grades for the related classes is positive and their average is y, then x is determined from the formula x = st((y+z)/2), where z is the weighted average of grades from the verifications carried out, in which grade weights from exams are 2, and the weights of grades from other forms of verification are equal to 1

● if at least one final grade in related activities is 2 or failure, then x = 2.