Quantification of surface acidity on a low surface area material
AssigneeSaint-Gobain Ceramics & Plastics, Inc.
InventorsTritti Siengchum, James M Ralph
Life of this patent
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Abstract
Methods and systems of analyzing and quantifying a surface acidity on a low surface area sample are disclosed. The methods include analyzing a quantity of an effluent molecular probe desorption from a temperature programmed desorption (TPD) process and system, by employing a mass spectroscopy (MS) system. The molecular probe is chemically adsorbed on a clean surface of the sample before the TPD process. The sample has a surface area to mass ratio of less than 5 m2/g. In some embodiments, the total surface area analyzed in the method can be as low as 3 m2.
Claims11
A method of quantification of surface acidity of a sample, the method comprising the steps of:
- (1) removing surface moisture of the sample using a pretreatment process comprising:
- heating the sample at about 6-10° C./min, from an initial temperature of about 50-100° C. to about 500-600° C., and
- maintaining a temperature of the sample of about 500-600° C. for about 15 to 30 minutes,
- wherein the sample is within a Helium or Argon gas flow at a flow rate of about 20-50 cm3/minute;
- (2) adsorbing a molecular probe on a surface of the sample comprising:
- maintaining a temperature of the sample of about 50-180° C. for about 10 to 20 minutes within a Helium or Argon gas mixed with 5% of the molecular probe flowing at a flow rate of about 10-50 cm3/minute;
- (3) removing physically adsorbed molecular probe from the surface of the sample comprising:
- maintaining a temperature of the sample of about 50-180° C. for about 60 to 120 minutes within a Helium or Argon gas flow at a flow rate of about 25-50 cm3/minute;
- (4) releasing the physically adsorbed molecular probe by a method that includes a temperature programmed desorption (TPD) process comprising:
- heating the sample with the molecular probe adsorption at about 6-10° C./min, from an initial temperature of about 50-100° C. to about 500-900° C., and
- maintaining a temperature of the sample of about 500-900° C. for about 15 to 30 minutes,
- wherein the sample is within a Helium or Argon gas flow at a flow rate of about 20-50 cm3/minute;
- and
- (5) measuring a total amount of the molecular probe physically desorbed from the TPD process by a method that includes mass spectroscopy (MS),
- wherein the sample has a surface area to mass ratio of less than 5 m2/g.
Dependencies are inferred from the claim text.