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Procedure of free and total glycerol determination in biodiesel

Method · June 2016

DOI: 10.13140/RG.2.1.2528.7283

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Dang Nguyen Thoai Chakrit Tongurai

Quy Nhon University Prince of Songkla University
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 PROCEDURE FOR FREE AND TOTAL GLYCEROL
DETERMINATION IN BIODIESEL
Dang Nguyen Thoai and Chakrit Tongurai

Department of Chemical Engineering, Faculty of Engineering,Prince of Songkla University,

Songkhla 90112, Thailand

1. Procedure for free glycerol determination:

1.1. Use a 250 mL glass: weigh an exact amount of biodiesel sample between
50 and 100 g.

1.2. Extraction of glycerol from biodiesel by washing:

a. put the glass on the heater (control from 60 to 65 oC) including

magnetic stirrer machine (stirring speed about 600 rpm)

b. add 20 mL of HCL 5 wt.% into the glass as above , stir about 20 min

c. be careful in transfer process the whole mixture to the funnel

d. wait about 5 – 10 min, separate and collect the aqueous phase into a
250 mL Erlenmeyer flask

e. put the biodiesel phase into the used glass and repeat the washing using
20 mL of HCl 2.5 wt.%

f. wait about 5 min, separate and collect the aqueous phase into the 250
mL Erlenmeyer flask as above

g. repeat step e and f but using 40 ml distilled water instead of HCl 2.5
wt.%

h. rinse the glass with 40 ml distilled water, and add it to the funnel
containing the biodiesel phase. Transfer the aqueous phase to the Erlenmeyer
flask containing the previous washing phase.

i. weigh the total amount of aqueous phase exactly.

1.3. Analyze the glycerol content in the aqueous phase

a. weight 50 g of aqueous phase

b. add 5 – 6 droplets of bromothymol blue as an indicator. At that time,

the color of the mixture is yellow
 c. neutralization by adding NaOH 0.1 mol/L (drop by drop) until the
color turns to blue (using magnetic stirrer for this process, using pH paper to
test color correctly if needed)

d. repeat steps from b to c but using 50 g of distilled water as a blank

sample

e. add 50 ml NaIO4 solution (60g NaIO4, 60 ml H2SO4 in 1000 mL

solution) into both samples (aqueous phase and blank), check and keep it in the
dark for 30 min

f. continue to add 10 ml C2H4(OH)2 50% (in H2O), check and keep it in

the dark for 20 min

g. titrate the solution by NaOH 0.125 mol.L (the concentration can be

lower than) with bromothymol blue as an indicator (5 – 7 droplets) until the
color chance to blue.
∑
Calculation:

where %GF : g of glycerol/100 g of biodiesel sample, V1: volume titrated of

NaOH (mL) for aqueous phase, V2: volume titrated of NaOH (mL) for blank
sample, NNaOH: exactly concentration of NaOH solution, ∑ : total amount of
aqueous phase in step i of section 1.2, W: amount of biodiesel sample (g).

2. Procedure for total glycerol determination:

2.1. Use a 500 mL three-necked flask: weigh an exact amount of biodiesel

sample between 50 and 100 g.

2.2. Do transesterification reaction: the reaction should be carried out in a

batch reactor with reflux condenser:

a. put the three-necked flask in a oil bath (temperature from 60 to 65 oC)

on a magnetic stirrer (stirring speed about 800 rpm)

b. add 1.6 wt.% of CH3ONa (to weighed biodiesel) and 40 wt.% of

CH3OH (to weighed biodiesel) into the three-necked flask

c. keep the temperature and the stirring speed during 2 h at 60 – 65 oC.

2.3. Extraction of glycerol from biodiesel by washing:

a. remove the reflux condenser

 b. add a weight of HCL 5 wt.%, equal to the amount used in step b of
section 2.2 into the flask, keep the temperature from 60 to 65 oC with strong
stirring (800 – 1000 rpm), approximately 20 min

c. without cooling, be careful in transfer process the whole mixture to the

separatory funnel

d. wait about 5 – 10 min, separate and collect the aqueous phase into a
250 mL Erlenmeyer flask

e. return the biodiesel phase into the used flask and repeat the washing
using a weight of HCl 2.5 wt.% equal to half of that weight in step b

f. wait about 5 min, separate and collect the aqueous phase into the 250
mL Erlenmeyer flask as above

g. repeat step e and f but using distilled water instead of HCl 2.5 wt.%

h. rinse the three-necked flask with distilled water (about 20 ml), and add
it to the funnel containing the biodiesel phase. Transfer the aqueous phase to the
Erlenmeyer flask containing the previous washing phase.

i. discard the biodiesel phase. Rinse the separatory funnel with distilled
water (about 20 ml) and collect it in the same Erlenmeyer flask

j. weigh the total amount of aqueous phase exactly.

2.4. Analyze the glycerol content in the aqueous phase

a. weight 50 g of aqueous phase

b. add 5 – 6 droplets of bromothymol blue as an indicator. At that time,

the color of the mixture is yellow

c. neutralization by adding NaOH 0.1 mol/L (drop by drop) until the

color turns to blue (using magnetic stirrer for this process, using pH paper to
test color correctly if needed)

d. repeat steps from b to c but using 50 g of distilled water as a blank

sample

e. add 50 ml NaIO4 solution (60g NaIO4, 60 ml H2SO4 in 1000 mL

solution) into both samples (aqueous phase and blank), check and keep it in the
dark for 30 min
 f. continue to add 10 ml C2H4(OH)2 50% (in H2O), check and keep it in
the dark for 20 min

g. titrate the solution by NaOH 0.125 mol.L (the concentration can be

lower than) with bromothymol blue as an indicator (5 – 7 droplets) until the
color chance to blue.
∑
Calculation:

where %GT : g of glycerol/100 g of biodiesel sample, V1: volume titrated of

NaOH (mL) for aqueous phase, V2: volume titrated of NaOH (mL) for blank
sample, NNaOH: exactly concentration of NaOH solution, ∑ : total amount of
aqueous phase in step j of section 2.3, W: amount of biodiesel sample (g).

Reference
M.L. Pisarello, B.O.D. Costa, N.S. Veizaga, and C.A. Querini. Volumetric method for
free and total glycerin determination in biodiesel. Ind. Eng. Chem. Res. 2010; 49:
8935–8941.

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