2018년 8월 5일 일요일

분석실험 메뉴얼입니다

분석실험 메뉴얼입니다
분석실험 메뉴얼입니다.doc


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Analytical Chemistry Laboratory Manual
Ed. by Prof. Yeong Il Kim
Rev. by Prof. Yong-Cheol Kang
Department of Chemistry
Pukyong National University
2017. 03 Revised Table of Contents
Lab 1. Argentometric Titration: Determination of Chloride 3
Lab 2. Gravimetric Determination of Calcium as CaC2O4.H2O 6
Lab 3. Statistical Evaluation of Acid-Base Indicators 8
Lab 4. Analysis of an Acid-Base Titration Curve: The Gran Plot 12
Lab 5. Iodometric Titration of Vitamin C 17
Lab 6. Chemical Oxygen Demand (COD) 19
Lab 7. Determination of Ca2+ Using an Ion-Selective Electrode 23
Lab 8. Spectrophotometric Determination of Iron in Vitamin Tablets 28
Lab 9. RF Sputter Deposition of Metal Oxide Thin Film 31
Lab 10. Determination of Ethanol Content in Liquor by Gas Chromatography 35
Lab 11. Determination of Calcium by Atomic Absorption Spectrometer 37
Lab 12. Spectrofluorometric Determination of Riboflavin (Vitamin B2) 41
Lab 1. Argentometric Titration: Determination of Chloride.
Silver nitrate is employed for the determination of anions that precipitate as silver salts. Titrimetric methods based upon silver nitrate are termed argentometric titrations. The Mohr method uses CrO42- ion as an indicator in the titration of chloride ion with silver nitrate. The first excess of titrant results in the formation of a red silver chromate precipitate, which signals the end point. The concentration of the silver nitrate is most conveniently determined by standardization against primary-standard sodium chloride, although direct preparation by weight is also feasible. In the Volhard method, excess silver ions are back-titrated with a standard of thiocyanate ion. In this case Fe3+ serves as the indicator. The solution turns red with the first slight excess of thiocyanate ion. The titration must be carried out in acidic solution to prevent precipitation of Fe3+ as the hydrated oxide.
Reagents*
Silver nitrate (FW 169.87), approximately 0.1 M solution: Dissolve about 8.5 g of AgNO3 in about 500 mL of distilled water.
Potassium chromate (FW 194.17), 0.1 M: Dissolve about 1.94 g of K2CrO4 in about 100 mL of distilled water.
Potassium thiocyanate (FW 97.18), 0.1 M: Dissolve about 4.9 g of KSCN in about 500 mL of distilled water.
Iron(Ⅲ) alum solution: A saturated solution of (NH4)Fe(SO4)2 in 1 M nitric acid.
* Those solutions are prepared by only one group indicated by lab TA
Standardization of Silver Nitrate Solution (Mohr Method)
Weigh accurately two samples of pure, dry sodium chloride* of about 0.20 to 0.25 g each into 250 mL Erlenmeyer flasks.
Dissolve each sample in 50 mL of distilled water and add 2 mL of 0.1 M potassium chromate. Titrate the first sample with silver nitrate, swirling the solution constantly, until the reddish color of silver chromate begins to spread more widely through the solution, showing that the end point is almost reached. The formation of clumps of silver nitrate is also an indicator that the end point is near. Continue the addition of silver nitrate dropwise until there is permanent color change from the yellow of the chromate ion to the reddish color of silver chromate precipitate.

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