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Membrane Based Triethylene Glycol Separation and Recovery from ...

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Process of preparation<br />

1. Sample dilution in the solvent Methanol when received the sample need to assess<br />

the probability that the concentration of TEG in the calibration curve or not (0.1-<br />

2%). Used the concentration 10% of TEG <strong>and</strong> then have to sample dilution 10 times<br />

before injection by pipette the volume of sample 100 µL into vial that has size 1.5<br />

mL <strong>and</strong> then adding more methanol 900 µL. After that analytical by gas<br />

chromatograph (GC).<br />

2. TEG sample to be analyzed must be stored in the refrigerator at 4 °C before<br />

analyzed <strong>and</strong> should be left at room temperature for about one hour.<br />

3. Appropriate sample volume for analysis should have a minimum volume of 3 ml.<br />

Process of preparing a st<strong>and</strong>ard solution to Calibration curve<br />

1. Preparation of st<strong>and</strong>ard solution concentration 10% TEG stock solution.<br />

2. Diluted st<strong>and</strong>ard solution <strong>from</strong> the number 1 of process of preparation by various<br />

concentrations <strong>from</strong> 0.1, 0.25, 0.5, 1.0 <strong>and</strong> 2.0%, respectively.<br />

3. <strong>Triethylene</strong> <strong>Glycol</strong> compounds analyzed with GC Agilent HP 6890.<br />

State of a GC Agilent HP 6890 for analysis of compounds triethylene glycol.<br />

1. Detector 250°C<br />

- Air <strong>and</strong> adjusting the pressure to 400 psi.<br />

- H2 gas <strong>and</strong> adjusting the pressure to 40 psi.<br />

- N2 gas <strong>and</strong> adjusting the pressure to 20 psi.<br />

2. Temperature program<br />

Parameter<br />

Temperature<br />

(°C)<br />

Hold<br />

(min)<br />

Runtime<br />

(h)<br />

Initial 100 2 3<br />

Ramp. 1, (25 °C/min) 250 10 18<br />

3. Column : Restex Rxi 624 sil MS 30m x 0.25m x 1.4m<br />

Mode: Constant Pressure<br />

Flow: 1.2 ml/min<br />

Outlet: Ambient<br />

Average: 25 cm/sec time 18 min<br />

4. Inlet<br />

Inlet: Back<br />

Mode: Splitless<br />

Heater: 250 °C, 7.78 psi, flow 24.1 ml/min<br />

Split vent: 19.9 ml/min at 0.1 ml<br />

36

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