This experiment was performed to determine chloride and sulfate in a highly viscous oil sample applying sample combustion before anion chromatography with conductivity detection after sequential suppression.
The sample is viscous oil, 40mg sample, Mitsubishi AQF-100 was combusted at 1000°C. The combustion gases were collected in ultrapure water containing 300 ppm H2O2 and subsequently injected.
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Figure 1. Determination of chloride and sulfate (not quantified) in a highly viscous petrochemical sample applying sample combustion followed by anion chromatography with conductivity detection after sequential suppression. The sample has a particularly high sulfate content.
Results
| |
Mean (injected) [mg/L] |
Mean (in sample) [mg/kg] |
| Chloride |
0.28 |
36.5 |
| Nitrite |
n.q. |
- |
| Nitrate |
n.q. |
- |
| Phosphate (internal standard) |
1.00 |
- |
| Sulfate |
n.q. |
- |
Experiment
The experiment details are as follows:
- Sample - Viscous oil
- Sample Preparation – Combustion
- Eluent: 3.2mmol/L sodium carbonate 1.0mmol/L sodium hydrogen carbonate
- Suppressor: Sequential suppression (MSM: 50 mmol/L H2SO4)
- Flow: 0.7mL/min
- Injection Volume: 100µL.
Columns
| Metrosep A Supp 5 - 150/4.0 |
6.1006.520 |
| Metrosep A Supp 4/5 Guard/4.0 |
6.1006.500 |
Solutions
| Eluent |
3.2mmol/L sodium carbonate
1.0mmol/L sodium hydrogen carbonate |
| Suppressor regenerant |
100mmol/L sulfuric acid |
| Rinsing solution |
Ultrapure water |
| Absorbtion solution |
300mg/L hydrogen peroxide
1.0mg/L phosphate |
Analysis
Conductivity after sequential suppression.
Parameters
| Flow rate |
0.7 mL/min |
| Injection volume |
100µL |
| Pmax |
15MPa |
| Recording time |
18min |
| Column temperature |
30°C |
Combustion Parameters
| Oven temperature |
| Inlet/outlet |
900/1000°C |
| Absorption solution |
5.0mL |
Instrumentation
| 881 Compact IC pro – Anion – MCS |
2.881.0030 |
| IC Conductivity Detector |
2.850.9010 |
| Remote box |
6.2148.010 |
| Mitsubishi AQF-100 |
* |
| Mitsubishi ABC-100 |
* |
| Mitsubishi WS-100 |
* |
| Mitsubishi GA-100 |
* |
* from local Mitsubishi distributor/not shown in system graphic below.
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This information has been sourced, reviewed and adapted from materials provided by Metrohm AG.
For more information on this source, please visit Metrohm AG.