GL-7400 series

Technical Note No.59

Analysis Analysisof ofBiodiesel BiodieselFuel Fuelby byHPLC HPLC

Resources and Energy Agency are considering to amend the following regulation, which is to strictly control the quality of Biodiesel Fuels (BDF). Enforcement Regulation of controlling the quality of volatile oils As a result, a regulation has been added as the chart on the right shows. In an HPLC method, FAME and Triglyceride (TG) are required to be analyzed. Currently, determining the calibration curve of Methyl Stearate (from FAME) and Trilinolein (from TG) are being considered as a method.
FAME Triglyceride (TG) Methanol Acid Number (Value) Formic Acid, Acetic Acid, Propionic acid Target Method HPLC-RI HPLC-RI Oxygen Detection GC Method Potentiometer Titration Ion Chromatography

Oxidation Stability Potentiometer Titration (Increased volume of acid number)

Analysis of Standard Solution

1. Methyl Stearate ( 2000 mg/L ) 2. Trilinolein ( 20 mg/L )
2.0 RIU 1.0

80

60

RIU

0.0

40

1
Enlarged View

0 0

20

Time (min)
20000000

10

Analytical Conditions: Column: Inertsil SIL-100A (5020-01712) (5um, 250 x 4.6 mm I.D.) Mobile Phase: A) n-Hexane 15000000 B) 2-Propanol A/B = 996 / 4, v/v A Flow Rate: 1.0 mL/min R 10000000 Column Temp.: 40C E Detector: RI A Injection Volume: 10 uL

5000000

250000

Methyl Stearate

Trilinolein
200000

R2 = 0.9998
150000

R2 = 0.9991

100000

Column Performance Test

When analyzing the standard solution using the above HPLC condition (However, the injection volume shall be 5uL) 1. 2. The retention time of Methyl Stearate shall be more than 3.5 minutes. Separation between Methyl Stearate and Trilinolein shall be more than 3.
0 0 200 400 600 800 1000

50000

0 0 2 4 6 8 10 12

Concentration (ug/10uL) g/10L

Solution for Calibration Curve

Concentration (ug/10uL) g/10L

Concentration (ug/10uL) Methyl Stearate Trilinolein 10 100 1 200 2 500 5 1000 10

1 2 3 4
5 (Standard undiluted solution)

Results Retention Time of Methyl Stearate: Separation:

4.05 minutes 4.7

Concentration of Standard Solution and Calibration Curve

Analysis of Biodiesel Fuel

Filtrated a Biodiesel Fuel using a 0.45um filter(disk) and then diluted with diesel fuel.

200

RIU

100

RIU 10

20

Enlarged View

0 0

Time (min)

10

* The Biodiesel Fuel was supplied from our customer, which is still in a developmental stage.

ISO14001: Save Energy and Resources!! Reduce Amount of Eluent with Smaller ID Inertsil Columns!!