Determination of Bromine Content in Polystyrene

Table of Contents

Introduction
Sample
Sample Preparation
Columns
Solutions
Parameters
Combustion Parameters
Analysis
Instrumentation
Results

Introduction

Bromination of polystyrol is carried out to increase flame retardation. The resulting brominated polystyrene is composed of 25% to 35% of bromine.

For bromine determination using combustion ion chromatography (CIC), a specially optimized absorption solution is required to trap all bromide. This article covers a work showing the optimization of the absorption solution for high-bromine samples.

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Sample

Brominated polystyrene

Sample preparation

The sample analysis is carried out using Combustion IC with flame sensor technology and intelligent partial loop injection technique with inline matrix elimination.

Columns

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

6.1014.200

Solutions

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

Flow rate

0.7 mL/minutes

Injection volume (IC)

10 μL (MiPT)

Pmax

15 MPa

Recording time

14 minutes

Column temperature

45 °C

Combustion parameters

Argon

100 mL/minutes

Oxygen

300 mL/minutes

Oven temperature

1050 °C

Post-combustion time

600 s

Initial volume of absorption solution

4.0 mL

Water inlet

0.2 mL/minutes

Analysis

Conductivity after the sequential suppression

Instrumentation

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)

Results

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 mol/L]

H2O2 [200 mol/L]

H2O2 [400 mol/L]

H2O2 [800 mol/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%

 

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

For more information on this source, please visit Metrohm AG.

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