1. Low Volatility Vapor Pressure Tester
MINIVAP VPL VISION
Low Volatility
Vapor Pressure Tester
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2. Agenda About Grabner Instruments Global regulations for VP Testing
The MINIVAP VPL VISION
Applications
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3. Vapor Pressure Global Regulations
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4. Globally Harmonized System for Classification and Labelling of Chemicals (GHS)
United Nations Regulation
Initiated in 1992
Effective since 200
Basis: Major regulations already in place
USA and Canada (e.g. US D.O.T., ANSI)
EU directive for classification and labelling (ADR)
United Nations Recommendations on the Transport of Dangerous Goods (UNECE/OECD)
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5. Impact of GHS GHS Transport Regulations Registration and Communication
UN Globally Harmonized System for
Classification and Labeling of Chemicals (GHS)
Registration and Communication
(Workplace, Customer)
Registration, Evaluation, Authorisation and Restriction of CHemicals
OSHA
Hazard Communication Standard (HDS)
Transport Regulations
US DOT
Transport Regulations
Subchapter C
Hazardous Materials Regulations (Hazmat)
European Agreement concerning the International Carriage of Dangerous Goods by Road (ADR)
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6. Safety Data Sheets
GHS regulates the minimum information required for a safety data sheet (SDS). The development of the safety data sheet (*) is based on ISO, ANSI, OSHA and EU Standards
The SDS section 9 „Physical and chemical properties“ requires that the vapor pressure is listed.
Listing of the vapor pressure has to include the temperature at which it was measured.
The absolute vapor pressure has to be tested
(*) See
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7. Vapor Pressure Test Methods
Method (liquids + solids) r R
Range
Static Method
5-10%
0.01 – 100 kPa
Isoteniscope Method
0.1 – 100 kPa
Dynamic Method
< 25%
1-5%
1-2 kPa
2-100 kPa
Effusion (Pressure balance)
5-20%
<50%
Up to 1 Pa
Effusion (Knudsen cell)
10-30% -
Effusion (Thermogravimetry)
5-30%
Gas Saturation Method
10-10 to 1000 Pa
Rotation Method
10-20%
10-4 to 0.5 Pa
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8. Static Method • Sample filled (1)2 3 4 5 6 7 8 9
• Sample filled (1)
• Evacuation (3/8): Must not alter sample composition; IBP required, to determine the right temperature for evacuation
• Valve (3) closed
• Sample (1) heated
• Vapors build (2)
• Equilibrium in the U-tube (4) changes
• Nitrogen or air added (9), to compensate vapor pressure increase in U-tube
• VP of N2 and air is known; when differential pressure in U-tube (4) is zero again, pressure is read from indicator (5)
1: Test substance
2: Vapor phase
3: High vacuum valve
4: U-tube (auxiliary manometer)
5: Pressure indicator
6: Temperature bath
7: Temperature measuring device
8: To vacuum pump
9: Ventilation/Nitrogen
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9. Isoteniscope Method (ASTM D2879)
Is a static method for absolute VP determination
Isoteniscope is evacuated and purged with N2 three times
 Impurities more volatile than the substance are removed
System pressure reduced to 133 Pa and sample warmed to remove dissolved gases
Sample tip (5) slowly heated, until vapor-filled, nitrogen-free space builds (4)
Isoteniscope placed in temperature bath
Nitrogen pressure is adjusted, until it equals sample pressure
Nitrogen pressure is measured 1 2 3 4 5 6
1: Pressure control
2: 8 mm OD Tube
3: Dry Nitrogen in system
4: Sample vapors
5: Sample tip
6: Liquid Sample
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10. Isoteniscope Method (ASTM D2879)
Downsides of the Isoteniscope:
Very complex procedure
Vacuum Pump, Nitrogen and temperature bath required
User has to evacuate carefully at temperature <IBP to retain sample characteristics
Used for single components
VP not affected by evacuation
Not used for multi-components
Impurities more volatile than the substance are removed by degassing or heavy boiling 1 2 3 4 5 6
1: Pressure control
2: 8 mm OD Tube
3: Dry Nitrogen in system
4: Sample vapors
5: Sample tip
6: Liquid Sample
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11. Better Solution Grabner Triple Expansion Method: Is a static method
No careful evacuation required
Air/gases removed automatically from result
Calculation according to gas law:
 (p*V) / T = constant
 Ptot – Pgas = Pabs
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12. Principle of Triple Expansion (D6378)
Filling
Expansion 1
Expansion 2
Expansion 3
*Vgas
0ml
1ml
2ml
4ml
Vliquid
pgas -
4/1=4
4/2=2
4/4=1
pliquid
8/2=4
16/4=4
Sample
Cell
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13. Principle of Triple Expansion (D6378)
p1 = pliquid + pgas(1) = 10
p2 = pliquid + pgas(2) = 9.5
p3 = pliquid + pgas(3) = 9.25
Boyle - Mariotte:
T = const
p x V = const V3 p1 p2 p3
pgas(1) x V1 = pgas(2) x V2 = pgas(3) x V3
(p1-pliquid) x V1 = (p2-pliquid) x V2 = (p3-pliquid) x V3 V2 V1
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14. Static measurement of absolute VP
MINIVAP VPL VISION
Static measurement of absolute VP
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15. VPL VISION Ideal for Petrochemicals: Gasoline, Jet Fuels, Oils
Chemicals, low volatile solvents
Flavors and Fragrances
Includes all standard methods (ASTM D6378, D5191, etc.)
Includes 2 static VOC methods
Shaker installed for rapid equilibrium
Sampling Pro™ valves minimize cross contamination
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16. Advantages VPL VISION Vastly improved precision
Repeatability: <0.1 kPa
Range optimized for: 0.1 – 150 kPa
Replaces static Isoteniscope method (ASTM D2879)
No vacuum pump required
Fully automated measurement
No sample composition changes
For single- and multi-component samples
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17. VPL VISION: VOC methods
VOC Direct:
Direct measurement of the absolute vapor pressure based on triple expansion
VOC Extrapolated
Extrapolation can be used,
If the VP is expected to be either < 0.1 kPa or >150 kPa
If the required VP temperature is <0°C or >120°C
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18. Comparison: VP VISION vs. VPL VISION
Pressure Range
0 – 2000 kPa
0 – 150 kPa
Measuring Range
2 – 2000 kPa
0.1 – 150 kPa
Temperature Range
0 – 120°C
Precision r / R [kPa]
0.2 / 0.5
0.1 / TBD
Applicable
Methods
ASTM D5191, D5188, D6377, D6378, D6897, TVP, etc.
ASTM D5191, D5188, D6377, D6378, VOC methods
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19. Measurement examples Samples N-Decane N-Hexane N-Pentane Gasoline
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20. Applications Samples Industries Chemicals Flavors & Fragrance Gasoline
Jet Fuels
Solvents
Industries
Automotive
Aviation
Chemical
Flavors
Laboratories
Military
Petroleum
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21. Tips for sample handling
New samples with low VP (< 2 kPa)
Rinse with pentane
Do an extra air rinsing
Attach the new sample
Increase No. of rinsings (5-9)
Set measuring cycles to 2
Dismiss the first result and use the result from the second measuring cycle
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22. Calibration Check Test D6378, reference absolute vapor pressure
2.2 Dimethylbutane – 68.8 kPa (Tolerance ± 1.2 kPa)
2.3 Dimethylbutane – 51.7 kPa (Tolerance ± 1.2 kPa)
Pentane – kPa (Tolerance ± 1.2 kPa)
Test D5191, use cooled and air saturated sample, reference total vapor pressure
44.0/56.0 Blend Pentane/Toluene – 70.0 kPa (Tolerance ± 1.2 kPa)
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23. THANK YOU! www.grabner-instruments.com www.ametek.com
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