Combustion Ion Chromatography (CIC) for Halogen and Sulfur Analysis in Petrochemicals

Consistent compliant analysis of Aromatic Hydrocarbons & their mixture samples from customers across the MENA region using Combustion Ion Chromatography (CIC).

Halogen and sulfur content in aromatic hydrocarbons and liquid organics can be determined using CIC, as outlined in ASTM D7359/UOP 991. Measuring these contaminants is critical, as high levels of halogens and sulfur can cause environmental pollution, catalyst poisoning, and corrosion.

Metrohm offers a comprehensive CIC solution featuring full system control utilizing MagIC Net software, i.e., both IC and Combustion modules will be controlled via a single software.

Optimized combustion for each sample eliminates the need to develop a specific combustion approach for different sample types or matrices. An inbuilt flame sensor is used to automate the boat movement, ensuring complete combustion of the sample.

This process prevents smooth formation and contamination of the combustion tube, enhancing the system's reliability and cleanliness. This approach significantly improves throughput, precision, and accuracy, making the process more efficient and reducing the potential for errors or delays during analysis.

Chromatogram 1.: Treated naphtha sample was injected directly into CIC for Chlorine & Sulphur determination without sample preparation

Chromatogram 1. The treated naphtha sample was injected directly into CIC for Chlorine & Sulphur determination without sample preparation. Image Credit: Metrohm Middle East FZC

Table 1. Results for treated naphtha sample. Source: Metrohm Middle East FZC

Sample Average n
Chloride (mg/Kg) 0.504 ± 0.008 3
Sulphur (mg/Kg) 12.55 ± 0.058 3

 

Chromatogram 2.: Nontreated naphtha sample was injected directly into CIC for Chlorine and Sulphur determination without sample preparation

Chromatogram 2. The nontreated naphtha sample was injected directly into CIC for Chlorine and Sulphur determination without sample preparation. Image Credit: Metrohm Middle East FZC

Table 2. Results for non-treated naphtha sample. Source: Metrohm Middle East FZC

Sample Average n
Chloride (mg/Kg) 0.551 ± 0.005 3
Sulphur (mg/Kg) 426.76 ± 1.503 3

 

Chromatogram 3.: Fuel oil sample 10 times diluted with toluene was injected into CIC for Chloride determination

Chromatogram 3. Fuel oil sample 10 times diluted with toluene was injected into CIC for Chloride determination. Image Credit: Metrohm Middle East FZC

Chromatogram 4.: Fuel oil sample 200 times diluted with toluene was injected into CIC for Sulphur determination

Chromatogram 4. Fuel oil sample 200 times diluted with toluene was injected into CIC for Sulphur determination. Image Credit: Metrohm Middle East FZC

Table 3. Results for Chloride & Sulphur determination Source: Metrohm Middle East FZC

Sample Average n
Chloride (mg/Kg) 7.79 ± 0.13 3
Sulphur (%) 4.49 ± 0.025 3

 

 Table 4. Columns. Source: Metrohm Middle East FZC

   
Metrosep A Supp 5 - 150/4.0 6.1006.520
Metrosep A Supp 5 Guard/4.0 6.1006.500
Metrosep A PCC 2 HC/4.0 6.1006.340

 

Table 5. Solutions. Source: Metrohm Middle East FZC

   
Eluent c(Na2CO3) = 3.2 mmol/L
c(NaHCO3) = 1.0 mmol/L
Regenerant c(H2SO4) = 0.1 mol/L
Rinsing solution STREAM
Absorber solution 100 mg/L Hydrogen peroxide

 

Table 6. Analysis. Source: Metrohm Middle East FZC

 
Conductivity after sequential suppression

 

Table 7. Parameters. Source: Metrohm Middle East FZC

   
Flow rate 0.7 mL/min
Injection volume (IC) 200 μL (MiPT)
Recording time 20 min
Column temperature 30 °C

 

Table 8. Combustion system parameters. Source: Metrohm Middle East FZC

   
Argon 100 mL/min
Oxygen 300 mL/min
Oven temperature 1050 °C
Post-combustion time 120 sec
Initial volume of absorption solution 2 mL
Water addition 0.1 mL/min
Absorption solution addition 0.2 mL/min
Total Makeup volume 7 mL
Combustion volume 100 μL
Injection volume 100 μL
Post rinse PCC Volume 2 mL

 

Table 9. Instrumentation. Source: Metrohm Middle East FZC

   
2.930.2560 930 Compact IC Flex Oven/SeS/PP/Deg
2.850.9010 IC conductivity detector
2.136.0700 Combustion Module
2.136.0800 Autosampler MMS 5000
6.7303.000 Liquid sampling Kit
2.920.0010 920 Absorber Module
6.7302.100 Quartz boat 40 x 9 mm (AJ)
6.7301.150 Quartz substrate for liquid samples

Image Credit: Metrohm Middle East FZC

Image Credit: Metrohm Middle East FZC

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

For more information on this source, please visit Metrohm Middle East FZC.

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