Analytical Testing for Germanium Sesquioxide
..............Titration: An un-buffered saturated solution of Germanium Sesquioxide has a pH around 2.6. Based on the known structure, and the weight of the sample, the amount of NaOH needed to neutralize the product is a simple calculation. This test is conducted a minimum of three times. Dangerous levels of inorganic forms of Germanium will produce a low titration. Keep in mind that there are derivatives of germanium sesquioxide in the form of salts. These are not harmful but will also give a low titration.
..............Solubility: The solubility of a known amount of Germanium Sesquioxide is conducted in a known amount of boiling distilled water. GeO2 is not readily soluble in boiling water and is much more soluble in acid. Dangerous levels of GeO2 will produce a cloudy solution or insoluble material in the bottom of a flask.
..............Elemental Analysis: In its pure form, Germanium Sesquioxide contains 42.7% elemental Germanium. Dangerous levels of inorganic forms of Ge will register higher than 43.1% by atomic absorption. This will invariably be supported by a low titration and likely by a failed solubility.
..............X-ray Fluorescence: This sophisticated method for detecting germanium content is both easy and quantifiable. This method can be used to verify the results of elemental analysis.
..............X-ray Diffraction: This is a very sensitive method for detecting the presence of inorganic germanium contaminates. With the ability to detect less than 0.001%, this method is more than adequate for detecting harmful levels of inorganic germanium.
..............IR spectral analysis: While gross contamination with inorganic forms of Germanium will be evident with this method, IR analysis is generally used to quickly determine whether pure inorganic forms of Germanium are being mistaken for organic forms. Different polymorphs (crystal structures) of germanium sesquioxide will give slightly different IR spectra. This should be taken into consideration when being used to identify germanium sesquioxide.
..............13C-NMR: This method will reveal the presence of a germanium/carbon bond, an essential element in all organic forms of germanium. The presence of germanium and the lack of a germanium/carbon bond is a dead giveaway of a toxic inorganic form.
..............Kjedahl total nitrogen: Years ago, Designed Nutritional Products recommended this test as a screening method for certain manufacturing processes. This recommendation has now been picked up and echoed by numerous other individuals, though few could even tell you what a positive result indicates. Total nitrogen is a simple method to screen out germanium sesquioxide produced by an inferior manufacturing process utilizing acrylonitrile. More on this
..............HPLC: Properly designed HPLC analysis will positively determine the identity and purity of germanium sesquioxide. The identity of any trace impurities can be determined through additional testing.
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