Application of Sample Combustion to Determine Chloride and Sulfate Content

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.

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.

About Metrohm

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This information has been sourced, reviewed and adapted from materials provided by Metrohm.

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