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Chemical Reagent Used in Closed Reflex Method

This document provides instructions for preparing chemical reagents and standards used in the closed reflux titrimetric and colorimetric methods for measuring chemical oxygen demand (COD). It describes how to make a standard potassium dichromate digestion solution, sulfuric acid reagent with silver sulfate, a ferroin indicator solution, and a standard ferrous ammonium sulfate titrant. It also provides directions for standardizing the titrant solution and preparing a potassium hydrogen phthalate standard. Precision testing showed the methods had a coefficient of variation between 6.5-10.8% for COD values ranging from 160-200 mg/L with and without chloride interference.

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303 views3 pages

Chemical Reagent Used in Closed Reflex Method

This document provides instructions for preparing chemical reagents and standards used in the closed reflux titrimetric and colorimetric methods for measuring chemical oxygen demand (COD). It describes how to make a standard potassium dichromate digestion solution, sulfuric acid reagent with silver sulfate, a ferroin indicator solution, and a standard ferrous ammonium sulfate titrant. It also provides directions for standardizing the titrant solution and preparing a potassium hydrogen phthalate standard. Precision testing showed the methods had a coefficient of variation between 6.5-10.8% for COD values ranging from 160-200 mg/L with and without chloride interference.

Uploaded by

IAabbasi
Copyright
© Attribution Non-Commercial (BY-NC)
We take content rights seriously. If you suspect this is your content, claim it here.
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Chemical reagent used in closed reflex method

5220 C. Closed Reflux, Titrimetric Method Standard potassium dichromate digestion solution, 0.01667M:

5220 D. Closed Reflux, Colorimetric Method Standard potassium dichromate Digestion solution, No defined M: 1.1) high range: Add to about 500 mL distilled water 10.216g Potassium dichromate( K2Cr2O7), Primary standard grade, previously dried at 150C for 2 h, 167 mL conc Sulfuric acid H2SO4, and 33.3 g Mercury sulfate (HgSO4). Dissolve, cool to room temperature, and dilute to 1000 mL. 1.2) low range: repare as in above , but use only 1.022 g potassium dichromate.

Add to about 500 mL distilled water 4.903 g Potassium dichromate( K2Cr2O7), Primary standard grade, previously dried at 150C for 2 h, 167 mL conc Sulfuric acid H2SO4, and 33.3g Mercury sulfate (HgSO4). Dissolve, cool to room temperature, and dilute to 1000 mL.

Sulfuric acid reagent : H2SO4 Add Silver sulfate (Ag2SO4), reagent or technical grade, crystals or powder, to conc H2SO4 at the rate of 5.5 g Ag2SO4/kg H2SO4. Let stand 1 to 2 d to dissolve. Mix Ferroin indicator solution: Dissolve 1.485 g 1,10-phenanthroline monohydrate and 695 mg FeSO47H2O in distilled water and dilute to 100 mL. This indicator solution may be purchased Already prepared. Standard ferrous ammonium sulfate titrant (FAS), approximately 0.10M: Dissolve 39.2 g Fe (NH4)2(SO4)26H2O in distilled water. Add 20 mL conc H2SO4, cool, and dilute to 1000 mL.

Sulfuric acid reagent : H2SO4 Add Silver sulfate (Ag2SO4), reagent or technical grade, crystals or powder, to conc H2SO4 at the rate of 5.5 g Ag2SO4/kg H2SO4. Let stand 1 to 2 d to dissolve. Mix Ferroin indicator solution: Dissolve 1.485 g 1,10-phenanthroline monohydrate and 695 mg FeSO47H2O in distilled water and dilute to 100 mL. This indicator solution may be purchased Already prepared. Standard ferrous ammonium sulfate titrant (FAS), approximately 0.10M: Dissolve 39.2 g Fe (NH4)2(SO4)26H2O in distilled water. Add 20 mL conc H2SO4, cool, and dilute to 1000 mL.

4.1 Standardize solution daily against

NO

standard K2Cr2O7 digestion solution as follows:


Pipet 5.00 mL digestion solution into a small beaker. Add 10 mL reagent water to substitute for Sample. Cool to room temperature. Add 1 to 2 drops diluted ferroin indicator and titrate with FAS titrant.

Molarity of FAS solution=

Potassium hydrogen phthalate standard : HOOCC6H4COOK: Lightly crush and then dry KHP to constant weight at 110C. Dissolve 425 mg in distilled water and dilute to 1000 mL.KHP has a theoretical COD1 of 1.176 mg O2/mg and this solution has a theoretical COD of 500 g O2/ mL. This solution is stable when refrigerated, but not indefinitely. Be alert to development of visible biological growth. If practical, prepare and transfer solution under sterile conditions. Weekly preparation usually is satisfactory.

Potassium hydrogen phthalate standard : HOOCC6H4COOK: Lightly crush and then dry KHP to constant weight at 110C. Dissolve 425 mg in distilled water and dilute to 1000 mL.KHP has a theoretical COD1 of 1.176 mg O2/mg and this solution has a theoretical COD of 500 g O2/ mL. This solution is stable when refrigerated, but not indefinitely. Be alert to development of visible biological growth. If practical, prepare and transfer solution under sterile conditions. Weekly preparation usually is satisfactory.

Precision and Bias:

Precision and Bias:

A set of synthetic samples containing potassium Forty-eight synthetic samples containing hydrogen phthalate KHP and NaCl was tested by potassium hydrogen phthalate KHP and 74 laboratories. NaCl were tested by five laboratories. At a COD of 200 mg O2/L in the absence of chloride, The standard deviation was 13mg/L (Coefficient of variation, 6.5%). At COD of 160 mg O2/L and 100 mg Cl/L, The standard deviation was 14 mg/L (Coefficient of variation, 10.8%). At an average COD of 193 mg O2/L in the absence of chloride, The standard deviation was 17 mg O2/L (coefficient of variation 8.7%). At an average COD of 212 mg O2/L and 100 mg Cl/ L, The standard deviation was 20 mg O2/L (coefficient of variation, 9.6%).

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