Determination of Sulfur and Halogen Contents in Chlorinated and Brominated Halobutyl Rubber Using Combustion IC

Halobutyl rubber is widely used in the manufacture of pharmaceutical stoppers. This material is ideally suited for this application as it has chemical resistance and exhibits low permeability to gases.

This Application Note describes the analysis of halogen and sulfur content of chlorinated and brominated butyl rubber stoppers. Hydropyrolysis of the sample results in the release of halogen and sulfur compounds, which are subsequently analyzed using ion chromatography (IC).

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Sample

Halogenated butyl rubber

Sample preparation

In this work, the sample analysis is performed by Combustion IC with flame sensor technology and intelligent partial loop injection technique with inline matrix elimination.

Columns

Metrosep A Supp 16 - 150/4.0

6.1031.420

Metrosep A Supp 16 Guard/4.0

6.1031.500

Metrosep A PCC 1 HC/4.0

6.1006.310

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 mg/L hydrogen peroxide

Parameters

Flow rate

0.8 mL/minutes

Injection volume (IC)

20 μL (MiPT)

Pmax

20 MPa

Recording time

18 minutes

Column temperature

45 °C

Combustion parameters

Argon

100 mL/minutes

Oxygen

300 mL/minutes

Oven temperature

1100 °C

Post-combustion time

500 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

Chlorinated butyl rubber

Brominated butyl rubber*)

Conc. [mg/kg]

RSD [%]

Conc. [mg/kg]

RSD [%]

1

Fluorine

36

1.2

< 100

2

Chlorine

6582

2.6

290

23

3

Bromine

n.d

-

8595

1.9

4

Sulfur

62

2.9

2509

3.

*) Chromatogram shown above

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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    Metrohm AG. (2019, April 02). Determination of Sulfur and Halogen Contents in Chlorinated and Brominated Halobutyl Rubber Using Combustion IC. AZoM. Retrieved on June 19, 2019 from https://www.azom.com/article.aspx?ArticleID=15424.

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    Metrohm AG. "Determination of Sulfur and Halogen Contents in Chlorinated and Brominated Halobutyl Rubber Using Combustion IC". AZoM. 19 June 2019. <https://www.azom.com/article.aspx?ArticleID=15424>.

  • Chicago

    Metrohm AG. "Determination of Sulfur and Halogen Contents in Chlorinated and Brominated Halobutyl Rubber Using Combustion IC". AZoM. https://www.azom.com/article.aspx?ArticleID=15424. (accessed June 19, 2019).

  • Harvard

    Metrohm AG. 2019. Determination of Sulfur and Halogen Contents in Chlorinated and Brominated Halobutyl Rubber Using Combustion IC. AZoM, viewed 19 June 2019, https://www.azom.com/article.aspx?ArticleID=15424.

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