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بنام خدا عباس بهرامی عضو هیات علمی گروه بهداشت حرفه ای دانشکده بهداشت دانشگاه علوم پزشکی کاشان

بنام خدا عباس بهرامی عضو هیات علمی گروه بهداشت حرفه ای دانشکده بهداشت دانشگاه علوم پزشکی کاشان Bahrami_a@kaums.ac.ir. انتظار میرود در پایان جلسه دانشجو بتواند :. 1-روش تیتریمتری را توضیح دهد. 2- انواع تیتریمتری را بیان کند. Titration. Titration

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بنام خدا عباس بهرامی عضو هیات علمی گروه بهداشت حرفه ای دانشکده بهداشت دانشگاه علوم پزشکی کاشان

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  1. بنام خدا عباس بهرامی عضو هیات علمی گروه بهداشت حرفه ای دانشکده بهداشت دانشگاه علوم پزشکی کاشان Bahrami_a@kaums.ac.ir

  2. انتظار میرود در پایان جلسه دانشجو بتواند : • 1-روش تیتریمتری را توضیح دهد. • 2- انواع تیتریمتری را بیان کند.

  3. Titration • Titration • A procedure in which one substance (titrant) is carefully added to another (analyte) until complete reaction has occurred. • The quantity of titrant required for complete reaction tells how much analyte is present. • Volumetric Analysis • A technique in which the volume of material needed to react with the analyte is measured

  4. Titration Vocabulary • Titrant • The substance added to the analyte in a titration (reagent solution) • Analyte • The substance being analyzed • Equivalence point • The point in a titration at which the quantity of titrant is exactly sufficient for stoichiometric reaction with the analyte.

  5. Titration Vocabulary • End point • The point in a titration at which there is a sudden change in a physical property, such as indicator color, pH, conductivity, or absorbance. Used as a measure of the equivalence point. • Indicator • A compound having a physical property (usually color) that changes abruptly near the equivalence point of a chemical reaction.

  6. Titration Vocabulary • Titration error • The difference between the observed end point and the true equivalence point in a titration • Blank Titration • One in which a solution containing all reagents except analyte is titrated. The volume of titrant needed in the blank titration should be subtracted from the volume needed to titrate unknown.

  7. Titration Vocabulary • Primary Standard • A reagent that is pure enough and stable enough to be used directly after weighing. Then entire mass is considered to be pure reagent. • Standardization • The process whereby the concentration of a reagent is determined by reaction with a known quantity of a second reagent.

  8. Titration Vocabulary • Standard Solution • A solution whose composition is known by virtue of the way it was made from a reagent of known purity or by virtue of its reaction with a known quantity of a standard reagent. • Direct Titration • One in which the analyte is treated with titrant, and the volume of titrant required for complete reaction is measured.

  9. Titration Vocabulary • Back Titration • One in which an excess of standard reagent is added to react with analyte. Then the excess reagent is titrated with a second reagent or with a standard solution of analyte.

  10. Titration Calculations • Titration Calculations rely heavily on the ability to perform stoichiometric calculations. • Examples

  11. 1. Neutralization 2. NaOH + HCl  H2O + NaCl 2NaOH + H2SO4  2H2O + Na2SO4 3. Twice as much HCl was required. Because it takes twice as much HCl (one H) as H2SO4 (two Hs) to neutralize the same amount of NaOH

  12. 0.60 mol NaOH L H2SO4 1 mol H2SO4 x x x L NaOH 0.175 mol H2SO4 2 mol NaOH 4. H2SO4(aq) + 2NaOH(aq)  2H2O + Na2SO4(aq) # L H2SO4= 5. #H x MA x VA = #OH x MB x VB 0.010 LNaOH = 0.01714 L = 17.1 mL

  13. Titration problems • What volume of 0.10 mol/L NaOH is needed to neutralize 25.0 mL of 0.15 mol/L H3PO4? • 25.0 mL of HCl(aq) was neutralized by 40.0 mL of 0.10 mol/L Ca(OH)2 solution. What was the concentration of HCl? • A truck carrying sulfuric acid is in an accident. A laboratory analyzes a sample of the spilled acid and finds that 20 mL of acid is neutral-ized by 60 mL of 4.0 mol/L NaOH solution. What is the concentration of the acid? • What volume of 1.50 mol/L H2S will neutral-ize a solution containing 32.0 g NaOH?

  14. Titration problems 1. (3)(0.15 M)(0.0250 L) = (1)(0.10 M)(VB) VB= (3)(0.15 M)(0.0250 L) / (1)(0.10 M) = 0.11 L 2. (1)(MA)(0.0250 L) = (2)(0.10 M)(0.040 L) MA= (2)(0.10 M)(0.040 L) / (1)(0.0250 L) = 0.32 M 3. Sulfuric acid = H2SO4 (2)(MA)(0.020 L) = (1)(4.0 mol/L)(0.060 L) MA = (1)(4.0 M)(0.060 L) / (2)(0.020 L) = 6.0 M 4. mol NaOH = 32.0 g x 1 mol/40.00 g = 0.800 (2)(1.50 mol/L)(VA) = (1)(0.800 mol) VA= (1)(0.800 mol) / (2)(1.50 mol/L) = 0.267 L

  15. Titration summary • For titrations we use the formula: #H x MA x VA = #OH x MB x VB Or NA x VA = NB x VB • NA is the combination of MA and #H • N is also known as normality • You can think of it a neutralizing power • We will stick with the first equation, you do not have to know N or what it stands for • This is a simplification of stoichiometry. We could get the same answer by working with moles (n = MV) and by using the balanced chemical equation

  16. Titration showdown • Titration competition (best with a burette): find the concentration of an H2SO4 solution – it could be anywhere from 0-18 mol/L • You will use the NaOH that you prepared two weeks ago and your vast knowledge of titration procedures and formulas. • The wining team, is the team closest to the correct value. • The only restriction is : don’t put base in the burette – only acid.

  17. Sources of error • NaOH was not exactly 0.10 mol/L • Calculation errors (e.g. converting mL to L) • Not rinsing and drying the beaker for the acid • Over titrating (ideally, 2 titrations should be done – one to get a rough estimate, and one to get the exact value). • Acid or base left on the side of the flask or on the tip of the burette (for greater precision, water is used to rinse the tip of the burette). • Errors reading volumes. • Using pipette (10 mL is measured from 0 mL to 10 mL, not from 10 mL to empty) • Using 10 mL of base vs. 25-50 mL For more lessons, visit www.chalkbored.com

  18. ALKALINE DUSTS 7401 NaOH, KOH, LiOH, MW : 40.00 (NaOH); CAS: 1310-73-2 RTECS: WB490000 (NaOH) and basic salts 56.11 (KOH) 1310-58-3 TT2100000 (KOH) 23.95 (LiOH) 1310-65-2 OJ6307070 (LiOH)

  19. METHOD: 7401, Issue 2 EVALUATION: FULL Issue 1: 15 February 1984 Issue 2: 15 August 1994 OSHA : 2 mg/m3 (NaOH) NIOSH: C 2 mg/m3/15 min (NaOH); Group I Pesticide ACGIH: C 2 mg/m3 (NaOH) PROPERTIES: basic, hygroscopic, caustic solids and aerosols; VP not significant SYNONYMS: alkali; caustic soda; lye; sodium hydroxide; potassium hydroxide

  20. SAMPLING SAMPLER: FILTER (1-μm PTFE membrane) FLOW RATE: 1 to 4 L/min VOL-MIN: 70 L @ 2 mg/m3 -MAX: 1000 L SHIPMENT: routine SAMPLE STABILITY: at least 7 days @ 25 °C [1,2] BLANKS: 2 to 10 field blanks per set PTFE Polytetrafluoroethylene; polyperfluoroethylene; tetrafluoroethene homopolymer; Teflon.

  21. MEASUREMENT TECHNIQUE: ACID-BASE TITRATION ANALYTE: OH- (alkalinity) EXTRACTION: 5.00 mL 0.01 N HCl, 15 min under nitrogen with stirring TITRATION: 0.01 N NaOH under nitrogen, endpoint by pH electrode CALIBRATION: 0.01 N NaOH standardized with 0.01 N HCl RANGE: 0.14 to 1.9 mg (as NaOH) per sample [1] ESTIMATED LOD: 0.03 mg per sample (as NaOH) [1] (7 x 10-4 moles of alkalinity) PRECISION (S r): 0.033 @ 0.38 to 1.5 mg NaOH per sample [1]

  22. ACCURACY RANGE STUDIED: 0.76 to 3.9 mg/m3 [1] (360-L samples) BIAS: 5.6% OVERALL PRECISION (Sˆ rT): 0.062 [1] ACCURACY: ± 16.2% APPLICABILITY: The working range is 0.4 to 5.4 mg/m 3 for a 360-L air sample. The method measures total alkalinity of alkali hydroxides, carbonates, borates, silicates, phosphates, and other basic salts, expressed as equivalents of NaOH.

  23. INTERFERENCES: Carbon dioxide in the air may react with alkali on the filter to produce carbonates but does not interfere when titrated. The carbonates will produce the equivalent amount of strong alkali that was consumed on the filter [1]. Acid a erosols may neutralize the sample, if present, producing a negative interference. OTHER METHODS: This revises Methods S381 [2] and P&CAM 241 [3]. NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94

  24. REAGENTS: 1. Sodium carbonate, primary standard grade. 2. Hydrochloric acid stock solution, 0.1 N. Standardize with sodium carbonate primary standard. 3. Dilute hydrochloric acid, 0.01 N. Dilute 10.0 mL 0.1 N stock HCl to 100 mL in a volumetric flask with distilled water. 4. Water, distilled, CO 2-free. Boil and cool under N2 or bubble nitrogen through distilled water for 30 min. Store with an Ascarite trap. 5. Nitrogen, compressed. 6. Sodium hydroxide, 50% w/v.* Dissolve 50 g NaOH in CO 2-free distilled water and dilute to 100 mL. 7. Stock sodium hydroxide, 0.1 N. Dilute 8 mL 50% NaOH to 1.0 L with CO 2-free distilled water. Store under Ascarite or other CO 2- absorbing trap. 8. Working sodium hydroxide solution, 0.01 N. Dilute 10 mL stock (0.1 N NaOH) to 100 mL with CO2-free distilled water. 9. Standard buffer solutions, pH 4 and 7. * See Special Precautions

  25. EQUIPMENT: 1. Sampler: 37-mm diameter PTFE membrane filter (Millipore, Fluoropore or equivalent), 1.0- μm pore size, supported by a cellulose backup pad in a cassette filter holder. 2. Personal sampling pump, 1 to 4 L/min, with flexible connecting tubing. 3. pH meter with pH electrode and recorder. 4. Titration vessel, 150 to 200 mL beaker, flask or jar with cover containing openings for the pH electrode and N 2 inlet and outlet. 5. Stirrer, magnetic, and stir bar. 6. Glass rod, ca. 5-mm diameter and 10 cm long to hold filter under liquid surface in titration vessel. 7. Pipets, 5- and 10-mL. 8. Volumetric flasks, 100-mL and 1-L. 9. Burets, 50-mL, readable to 0.1 mL. 10. Tweezers. SPECIAL

  26. SPECIAL PRECAUTIONS: NaOH solutions are corrosive to tissue [4]. Handle with care. 1. Calibrate each personal sampling pump with a representative sampler in line. 2. Sample at an accurately known flow rate between 1 and 4 L/min for a sample size of 70 to 1000 L. Do not exceed a filter loading of ca. 2 mg total dust.

  27. SAMPLE PREPARATION: 3. Transfer the sample filter to a titration vessel with tweezers. Place the filter face down in the titration vessel. 4. Place the end of a glass rod in the center of the filter to maintain the filter below the liquid surface during the analysis. 5. Cover the titration vessel, add 5.00 mL 0.01 N HCl, start the magnetic stirrer and N 2 purge (ca. 0.1 L/min). 6. Allow to stand 15 min (with stirring).

  28. CALIBRATION AND QUALITY CONTROL: 7. Calibrate the pH meter with pH 4 and pH 7 buffer solutions. 8. Standardize aliquots of the 0.1 N HCl stock solution with sodium carbonate in triplicate [3]. a. Dry 3 to 5 g primary standard grade Na 2CO3 at 250 °C for 4 h. Cool in a desiccator. b. Weigh ca. 2.5 g Na 2CO3 to the nearest mg. Dissolve and dilute to exactly 1 L with CO 2-free distilled water. The concentration is ca. 0.05 N Na2CO3. c. Place 5.00 mL 0.05 N Na2CO3 solution into a titration vessel and titrate potentiometrically to a pH of 5. NIOSH Manu

  29. d. Remove electrodes, rinse them into the titration vessel, and bubble N 2 gas through contents of the titration vessel for 3 to 5 min to remove dissolved CO 2. e. Proceed with the titration to the inflection point. f. Calculate the normality of the stock HCl solution

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