Optimization Of The Absorption Solution For Measuring Bromine Content In Polystyrene Using Combustion IC

To enhance flame retardation, polystyrene is brominated to achieve a final composition containing 25-35 % bromine. Determining the bromine content through combustion ion chromatography (CIC) requires a specially optimized absorption solution to effectively trap all bromide.

Optimization Of The Absorption Solution For Measuring Bromine Content In Polystyrene Using Combustion IC

Image Credit: Metrohm Middle East FZC

This study demonstrates the optimization of an absorption solution tailored for high-bromine samples.

Results

Source: Metrohm Middle East FZC

. . . . . .
1 Bromine NaOH [0 mol/L] NaOH [10 mol/L] NaOH [20 mol/L] NaOH [30 mol/L]
Change in NaOH (400 mg/L H2O2)

241.0 g/kg RSD = 4.9 %

287.6 g/kg RSD = 3.6 % 287.6 g/kg RSD = 1.5 % 283.8 g/kg RSD = 1.8 %
  H2O2 [100 mg/L] H2O2 [200 mg/L] H2O2 [400 mg/L] H2O2 [800 mg/L]

Change in H2O2  (20 mmol/L NaOH)

288.2 g/kg RSD = 2.8 %

270.6 g/kg RSD = 2.0 %

281.5 g/kg RSD = 1.8 %

284.8 g/kg RSD = 2.9 %

 

Sample Preparation

The brominated polystyrene sample was analyzed using a Combustion IC with flame sensor technology and an intelligent Partial Loop Injection Technique with Inline Matrix Elimination.

Columns

Source: Metrohm Middle East FZC

. .
Metrosep A Supp 16 - 100/4.0 6.1031.410
Metrosep A Supp 4/5 Guard/4.0 6.1031.500
Metrosep A PCC 1 HC/4.0 6.1006.310
Metrosep A Trap 1 - 100/4.0 6.1014.000
Metrosep I Trap 1 - 100/4.0 6.1014.2

 

Solutions

Source: Metrohm Middle East FZC

. .
Eluent 7.5 mmol/L sodium carbonate 0.75 mmol/L sodium hydroxide
Suppressor regenerant 250 mmol/L sulfuric acid
Rinsing solution STREAM
Absorber solution 100 - 800 mg/L hydrogen peroxide 0 - 30 mmol/L sodium hydroxide

 

Parameters

Source: Metrohm Middle East FZC

. .
Flow rate 0.7 mL/min
Injection volume (IC) 10 μL (MiPT)
Pmax 15 MPa
Recording time 14 min
Column temperature 45 °C

 

Combustion Parameters

Source: Metrohm Middle East FZC

. .
Argon 100 mL/min
Oxygen 300 mL/min
Oven temperature 1050 °C
Post-combustion time 600 s
Initial volume of absorption solution 4.0 mL
Water inlet 0.2 mL/min

 

Analysis

Source: Metrohm Middle East FZC

.
Conductivity after sequential suppression

 

Instrumentation

Source: Metrohm Middle East FZC

. .
930 Compact IC Flex Oven/SeS/PP/Deg 2.930.2560*
IC Conductivity Detector 2.850.9010*
MSM Rotor A 6.2832.000*
Adapter sleeve for Suppressor Vario 6.2842.020*
920 Absorber Module 2.920.0010*
Combustion Module (oven and ABD) 2.136.0700*
Autosampler MMS 5000 2.136.0800
Kit for solid sampling 6.7302.000

* available as 930 Metrohm Combustion IC (2.930.9010)
 

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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