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Porotec Workshop 15 & 16 th Nov. 2004 NYSCC Alfred University Mercury Porosimetry Advantages and Limitations Herbert Giesche New York State College of Ceramics at Alfred University

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Page 1: Mercury Porosimetry Advantages and Limitations - Alfred ...giesche/NEWS_files/Porotec Nov...2004/11/03  · NYSCC Alfred UniversityPorotec Workshop 15 & 16th Nov. 2004 Theory θ γ

Porotec Workshop 15 & 16th Nov. 2004NYSCC Alfred University

Mercury PorosimetryAdvantages and Limitations

Herbert GiescheNew York State College of Ceramics

at Alfred University

Page 2: Mercury Porosimetry Advantages and Limitations - Alfred ...giesche/NEWS_files/Porotec Nov...2004/11/03  · NYSCC Alfred UniversityPorotec Workshop 15 & 16th Nov. 2004 Theory θ γ

Porotec Workshop 15 & 16th Nov. 2004NYSCC Alfred University

Outline:

• Introduction / Theory• The Measurement Technique

– Tips and Tricks – Precision and Accuracy

• What Information do we get?• Hysteresis• Pore-Network Models• Alternative Techniques

Page 3: Mercury Porosimetry Advantages and Limitations - Alfred ...giesche/NEWS_files/Porotec Nov...2004/11/03  · NYSCC Alfred UniversityPorotec Workshop 15 & 16th Nov. 2004 Theory θ γ

Porotec Workshop 15 & 16th Nov. 2004NYSCC Alfred University

But first, “Where on earth is Alfred ?”

Page 4: Mercury Porosimetry Advantages and Limitations - Alfred ...giesche/NEWS_files/Porotec Nov...2004/11/03  · NYSCC Alfred UniversityPorotec Workshop 15 & 16th Nov. 2004 Theory θ γ

Porotec Workshop 15 & 16th Nov. 2004NYSCC Alfred University

What type or size of pore is measured ?Closed Pores Blind Pores Cross-linked Pores Through Pores

In all cases, Hg-Porosimetry measures the largest available access to a pore,the size of the “entrance” towards a pore.

Most times this is substantially smaller than the inner pore diameter!

Page 5: Mercury Porosimetry Advantages and Limitations - Alfred ...giesche/NEWS_files/Porotec Nov...2004/11/03  · NYSCC Alfred UniversityPorotec Workshop 15 & 16th Nov. 2004 Theory θ γ

Porotec Workshop 15 & 16th Nov. 2004NYSCC Alfred University

Theoryθγγ cos

r 2

p

= 11 =P :equation - Washburnand -Laplace Young21

lv ⎟⎟⎠

⎞⎜⎜⎝

⎛+∆

rr

Essentially all calculations are based on the assumption of cylinder pores.

This is a major assumption !!!

Page 6: Mercury Porosimetry Advantages and Limitations - Alfred ...giesche/NEWS_files/Porotec Nov...2004/11/03  · NYSCC Alfred UniversityPorotec Workshop 15 & 16th Nov. 2004 Theory θ γ

Porotec Workshop 15 & 16th Nov. 2004NYSCC Alfred University

What are the basic parameters to be measured ?

• Pressure

• Intruded volume

• Contact angle, θ

• Surface tension, γ

Page 7: Mercury Porosimetry Advantages and Limitations - Alfred ...giesche/NEWS_files/Porotec Nov...2004/11/03  · NYSCC Alfred UniversityPorotec Workshop 15 & 16th Nov. 2004 Theory θ γ

Porotec Workshop 15 & 16th Nov. 2004NYSCC Alfred University

Pressure

• Pressure transducer have to cover the entire measurement range.

(> 5 orders of magnitude !)• Use several transducer with overlapping ranges.• Avoid temperature drifts.• Avoid accidental over-range exposure.• Calibrate and check with “Standards”

Page 8: Mercury Porosimetry Advantages and Limitations - Alfred ...giesche/NEWS_files/Porotec Nov...2004/11/03  · NYSCC Alfred UniversityPorotec Workshop 15 & 16th Nov. 2004 Theory θ γ

Porotec Workshop 15 & 16th Nov. 2004NYSCC Alfred University

Volume Measurement

• The “antique” techniques:OpticallyContact wireResistance wire

• Nowadays used in essentially all instruments:Precision capacitance bridge

Page 9: Mercury Porosimetry Advantages and Limitations - Alfred ...giesche/NEWS_files/Porotec Nov...2004/11/03  · NYSCC Alfred UniversityPorotec Workshop 15 & 16th Nov. 2004 Theory θ γ

Porotec Workshop 15 & 16th Nov. 2004NYSCC Alfred University

Contact angle (which one ?)