GUIDE TO PRACTICAL EXERCISES IN ANALYTICAL CHEMISTRY
The manual for laboratory exercises on analytical Chemistry for Pharmacy students is designed to support practical classes in qualitative and quantitative analysis in the Analytical Chemistry course. It contains three main sections - qualitative analysis of cations and anions, volumetric quantitative analysis and instrumental methods for quantitative analysis, including the basic laboratory principles and practices that students become familiar with during the course of study.
In each section, the principles of the given method (theoretical part) are discussed, combined with a practical part - individual tasks to be performed, which allow students to work independently and actively. The volume of information presented and planned practical material are in accordance with the curriculum and the minimum requirements for a specialty of the regulated professions.
The developed aid complements and builds on the information in the existing editions by including the quantitative characterization of a number of substances with application in pharmaceutical practice, for which, in addition to the necessary structural and analytical information, additional data on their biological activity are presented. The aid complements the two-semester lecture course in analytical chemistry for students from the Master's degree in Pharmacy, but would also be useful for students from the biological and chemical specialties at SU "St. Kliment Ohridski".
CONTENTS
I. Introduction to analytical chemistry / 9
II. Qualitative analysis / 10
1. Introduction / 10
2. First group of cations (hydrochloric) – Ag+, Pb2+, Hg2 / 15
2.1. Analytical reactions of the first group of cations / 17
Silver / 17
Lead / 19
Mercury (mercury ion) / 21
2.2. Systematic move to detect and prove the ions from the first group of cations / 22
3. Second group of cations (hydrogen sulfide) – Pb2+, Hg2+, Cu2+, Cd2+, Bi3+, As(III), As(V), Sb(III), Sb(V), Sn2+, Sn(IV) / 24
3.1. Analytical reactions of the second group of cations / 26
Mercury (mercurion) / 26
Copper / 28
Cadmium / 30
Bismuth / 31
Arsenic(III) / 33
Antimony(III) / 34
Tin Sn2+ / 35
Tin(IV) / 36
3.2. Systematic move to detect and prove the ions from the second group of cations / 36
4. Third group of cations (ammonium sulphide) – Fe3+, Fe2+, Ni2+, Co2+, Mn2+, Cr3+, Al3+, Zn2+ / 40
4.1. Analytical reactions of the third group of cations / 41
Iron (ferrion) / 41
Iron (ferroion) / 43
Nickel / 45
Cobalt / 46
Manganese / 47
Chrome / 48
Aluminum / 50
Zinc / 52
4.2. A systematic move to discover and prove of the ions of the third group of cations / 54
5. Fourth group of cations (ammonium carbonate) – Ca2+, Sr2+, Ba2+ / 57
Calcium / 58
Strontium / 59
Barium / 60
6. Fifth group of cations – Mg2+, Na+, K+, NH4+ / 62
Magnesium / 63
Sodium / 65
Potassium / 66
Ammonium cation / 67
7. Anions / 68
Carbonate anion / 68
Sulfite anion / 68
Nitrite ion / 69
Phosphates / 71
Sulfate anion / 72
Chromate and dichromate anion / 72
Fluoride anion / 72
Halide anions / 73
Nitrate anion / 73
Acetate anion / 74
8. Analysis of a solid with an unknown composition / 75
III. Quantitative analysis / 80
1. General provisions for calculations / 80
1.1. Percent concentration / 80
1.2. Molar concentration / 81
1.3. Normal concentration / 81
2. General provisions in volumetric analysis / 83
3. Laboratory glassware / 89
4. Preparation of solutions for the purposes of volumetric analysis / 93
5. Acid-base titration in an aqueous medium / 98
Preparation and standardization of solutions
of hydrochloric acid and sodium base / 98
Determination of sodium bicarbonate content
in solution for intravenous administration / 103
Determination of the purity of salicylic acid substance / 107
Determination of acetylsalicylic acid content in medicinal product "Aspirin" / 109
Determination of acetic acid content in commercial product "Vinegar" / 113
Determination of total acidity of citrus juice / 115
6. Acid-base titration in a non-aqueous medium / 118
Preparation and standardization of potassium base solution in ethanol / 118
Determination of salicylic acid content in commercial product "Salicylic spirit" / 120
Determining the purity of a substance 5,5-diethylbarbituric acid (barbital, veronal) / 122
7. Complexometry / 126
Preparation and standardization of Na2EDTA solution / 126
Determination of CaCl2.2H2O content in Ringer's solution / 133
Determination of aluminum and magnesium content in the medicinal product "Almagel" / 135
Determination of zinc content in food supplement (tablets) / 139
8. Sediment volumetric analysis / 143
Preparation and standardization of solutions of silver nitrate and ammonium thiocyanate / 143
Determination of NaCl content in physiological solution ("physiological serum") / 148
Determining the purity of a commercial product "Nishadar" (ammonium chloride) / 150
Determination of the purity of technical silver nitrate / 152
9. Oxidation-reduction volumetric analysis (redoximetry) / 155
Preparation and standardization of potassium permanganate solution / 155
Determination of hydrogen peroxide content in medicinal preparation "Oxygen water" / 158
Preparation and standardization of solutions of sodium thiosulphate and iodine / 161
Determination of iodine content in ethanol solution of iodine ("iodine tincture") / 167
Determination of ascorbic acid content in tablets "Vitamin C" / 170
Determination of the content of metamizole sodium in medicinal products containing it (spasmalgon/analgin) / 173
Determination of glucose content in infusion solution / 176
10. Instrumental methods for quantitative analysis / 180
Spectrophotometric determination of content of salicylic acid in the commercial product "Salicylic spirit" by the method of the standard addition / 180
Spectrophotometric determination of content of hemoglobin in blood / 184
Potentiometric determination of content of phosphoric acid in Coca-Cola® / 187
Used literature / 191
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The Practical Guide to Analytical Chemistry is an essential learning resource designed to prepare chemistry students for the real-world practice of analytical work. This textbook provides a detailed explanation of the basic principles, methods, and techniques used in analytical chemistry, as well as instructions for conducting various analytical procedures and experiments.
At the beginning of the textbook, the main theoretical basis of analytical chemistry is presented, including the principles of qualitative and quantitative analysis, methods of separation and identification of constituents in different samples. Here, students learn fundamental concepts such as accuracy, precision, sensitivity and specificity in the context of analytical methods.
After the theoretical part, the textbook provides a number of practical exercises that allow students to apply their knowledge in a real laboratory environment. These exercises cover various aspects of analytical work, including preparing solutions, measuring concentrations, calibrating instruments, and using various analytical methods.
Each exercise is presented with assignments that guide students toward specific analytical goals and procedures. The instructions are clear and detailed, allowing students to follow the procedures step by step and draw useful conclusions from the results obtained.
In addition, the textbook also includes reference materials such as tables, graphs and charts that support students in their learning process and help to understand the key concepts and techniques in analytical chemistry.
Analytical Chemistry Practice Guide is an indispensable source of knowledge and skills for students preparing for a professional career in analytical chemistry. This textbook provides them with the necessary tools and guides to develop their skills in the analysis of a variety of materials and understand the basic principles of analytical chemistry.
