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Industrial Minerals Association – Europe A.I.S.B.L.

REACH Consortium for Borates substances


c/o IMA-Europe (Coordinator), rue des Deux Eglises 26/2 – B-1000 Brussels

Brussels, 7 July 2010

To: Members of the SIEF for Sodium tetraborate (CAS: 1330-43-4) & related hydrates

Recommended Analytical Methods for Substance Identification and Purity

 Substance: Disodium tetraborate: EC# 215-540-4; CAS# 1330-43-4

As you may already be aware, each individual registrant must provide information on which analytical
methods (ref. IUCLID section 1.4) should be used to determine the identity of the substance as well as
providing relevant spectral data. The Borates REACH Consortium has reviewed the above mentioned
substance and has made recommendations on the analytical methods it deems relevant for
Substance Identity and measurement of purity. Since each registrant must provide this data as part of
his individual submission, the decision on which information to provide remains with the registrant.

The Borates REACH Consortium recommends the following analytical methods:

 Substance Identity
Analytical methods recommended to be used for Substance Identification:

Methods
Fourier Transform Infrared (FTIR)
Titrimetric

Description of the Titrimetric method

Standard number: BS 5688-3:1979, ISO 1916:1972


Title: Methods of test for boric acid, boric oxide, disodium tetraborates, sodium perborates and crude
sodium borates for industrial use. Determination of sodium oxide and boric oxide contents and loss on
ignition of disodium tetraborates.

Description: The sodium oxide and boric oxide content are determined on the same solution. An
aqueous solution is treated with excess standard hydrochloric acid solution followed by back titration
with standard sodium hydroxide solution in the presence of methyl red as indicator. From this the
sodium oxide can be calculated. The subsequent titration with standard sodium hydroxide in the
presence of mannitol and phenolphthalein as indicator enables the boric oxide content to be
calculated. The boron chemistry ensures that the B2O3 content identifies and quantifies each pure
borate compound. The determination of Sodium tetraborate anhydrous would yield a B2O3 content of
69.2 wt.%. Similarly, the identification of sodium borates is revealed and confirmed when the Na2O
value is determined, and the unique ratio of the two oxides (B2O3 and Na2O) is determined. For
sodium tetraborate anhydrous, this yields the distinctive ratio of 0.5, thereby in combination with the
borate assay this uniquely identifies the compounds.

It is up to each individual registrant to provide a description of the analytical methods or the


appropriate bibliographical references for the identification of the substance. The information shall be
sufficient to allow the methods to be reproduced.

Industrial Minerals Association Europe aisbl, in short “IMA-Europe”


Established under the Belgian law under the enterprise / VAT number BE 0452.946.151
Twin Gardens (6° floor), rue des Deux Eglises 26, B - 1000 Brussels, Belgium
Tel: 32 2 210 44 10, Fax: 32 2 210 44 29, E-mail: secretariat@ima-europe.eu, www.ima-europe.eu
For the following spectral analysis and chromatographic methods, it is not considered relevant to
perform the analysis. Instead it is recommended that a scientific justification is given to waive the need
for analysis. A suggested justification is provided below.

Method Justification
X-Ray Diffraction (XRD) X-Ray Diffraction is not relevant to identify or analyse an
amorphous inorganic substance such as disodium
tetraborate.
Ultra-Violet/Visible spectrum UV/Vis is not relevant to identify or analyse an inorganic
substance such as disodium tetraborate because there are
no absorption maxima between 200 and 750 nm.
Mass Spectrum Mass spectroscopy is not relevant to identify or analyse an
inorganic substance such as disodium tetraborate.
Nuclear Magnetic Resonance NMR is not relevant to identify or analyse an inorganic
substance such as disodium tetraborate.
High Pressure Liquid Chromatogram HPLC is not relevant to identify or analyse an inorganic
substance such as disodium tetraborate.
Gas Chromatogram GC is not relevant to identify or analyse an inorganic
substance such as disodium tetraborate.

Optical activity: The substance is not optically active.

 Purity

The method below is recommended to be used to analyse the purity of the substance:

Standard number: BS 5688-8:1979, ISO 2216:1972

Title: Methods of test for orthoboric acid (boric acid), diboron trioxide (boric oxide), disodium
tetraborates, sodium perborates and crude sodium borates for industrial use. Determination of sodium
oxide and boric oxide contents of crude sodium borates.

Description: The sodium oxide and boric oxide content are determined on the same solution. An
aqueous solution is treated with excess standard hydrochloric acid solution followed by back titration
with standard sodium hydroxide solution in the presence of methyl red as indicator. From this the
sodium oxide can be calculated. The subsequent titration with standard sodium hydroxide in the
presence of mannitol and phenolphthalein as indicator enables the boric oxide content to be
calculated. The boron chemistry ensures that the B2O3 content identifies and quantifies each pure
borate compound. The determination of Sodium tetraborate anhydrous would yield a B2O3 content of
69.2 wt.%. Similarly, the identification of sodium borates is revealed and confirmed when the Na2O
value is determined, and the unique ratio of the two oxides (B2O3 and Na2O) is determined. For
sodium tetraborate anhydrous, this yields the distinctive ratio of 0.5, thereby in combination with the
borate assay this uniquely identifies the compounds.
Recommended Analytical Methods for Substance Identification and Purity

 Substance: Sodium tetraborate pentahydrate: EC# 215-540-4; CAS# 12179-04-03


Sodium tetraborate decahydrate: EC# 215-540-4; CAS# 1303-96-4

 Substance Identity
Analytical methods recommended to be used for Substance Identification:

Method
Fourier Transform Infrared (FTIR)
X-Ray Diffraction (XRD)

It is up to each individual registrant to provide a description of the analytical methods or the


appropriate bibliographical references for the identification of the substance. The information shall be
sufficient to allow the methods to be reproduced.

For the following spectral analysis and chromatographic methods, it is not considered relevant to
perform the analysis. Instead it is recommended that a scientific justification is given to waive the need
for analysis. A suggested justification is provided below.

Method Justification
Ultra-Violet/Visible spectrum UV/Vis is not relevant to identify or analyse an inorganic
substance such as disodium tetraborate because there are
no absorption maxima between 200 and 750 nm.
Mass Spectrum Mass spectroscopy is not relevant to identify or analyse an
inorganic substance such as disodium tetraborate.
Nuclear Magnetic Resonance NMR is not relevant to identify or analyse an inorganic
substance such as disodium tetraborate.
High Pressure Liquid Chromatogram HPLC is not relevant to identify or analyse an inorganic
substance such as disodium tetraborate.
Gas Chromatogram GC is not relevant to identify or analyse an inorganic
substance such as disodium tetraborate.

Optical activity: The substance is not optically active.

 Purity

The method below is recommended to be used to analyse the purity of the substance:

Standard number: BS 5688-8:1979, ISO 2216:1972

Title: Methods of test for orthoboric acid (boric acid), diboron trioxide (boric oxide), disodium
tetraborates, sodium perborates and crude sodium borates for industrial use. Determination of sodium
oxide and boric oxide contents of crude sodium borates.

Description: The sodium oxide and boric oxide content are determined on the same solution. An
aqueous solution is treated with excess standard hydrochloric acid solution followed by back titration
with standard sodium hydroxide solution in the presence of methyl red as indicator. From this the
sodium oxide can be calculated. The subsequent titration with standard sodium hydroxide in the
presence of mannitol and phenolphthalein as indicator enables the boric oxide content to be
calculated. The boron chemistry ensures that the B2O3 content identifies and quantifies each pure
borate compound. The determination of Sodium tetraborate anhydrous would yield a B2O3 content of
69.2 wt.%. Similarly, the identification of sodium borates is revealed and confirmed when the Na2O
value is determined, and the unique ratio of the two oxides (B2O3 and Na2O) is determined. For
sodium tetraborate anhydrous, this yields the distinctive ratio of 0.5, thereby in combination with the
borate assay this uniquely identifies the compounds.

Standard number: BS 5688-3:1979, ISO 1916:1972

Title: Methods of test for boric acid, boric oxide, disodium tetraborates, sodium perborates and crude
sodium borates for industrial use. Determination of sodium oxide and boric oxide contents and loss on
ignition of disodium tetraborates.

Description: Determination of the loss on ignition at 900°C, expressed conventionally as the water
content.

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