An overview of Pressurized Liquid Extraction

Pressurized Fluid Extraction (PFE) or Pressurized Liquid Extraction (PLE) is a new sample extraction method that employs liquid solvents at elevated temperatures and pressures to prepare samples for analysis by either gas chromatography or liquid chromatography. Pressurized liquid extraction is similar to Soxhlet extraction, except that during the extraction process the solvent condition inside the PLE cell approaches the supercritical region which results in more efficient extractions. The elevated temperature allows the sample to become more soluble and achieve a higher diffusion rate while the elevated pressure keeps the solvent below its boiling point. At elevated pressures and temperatures solvents can penetrate solid samples more efficiently which reduces solvent usage.

A pressurized liquid extraction when compared to a traditional Soxhlet extraction shows a reduction in extraction time to 22 minutes from 18 hours and a decrease of total organic solvent consumption to 80 mL or less of organic solvent from 300 mL.

To perform a pressurized liquid extraction, between 5 grams and 100 grams of sample is mixed with sodium sulfate, loaded in the extraction cell and capped with two filtration end fittings. The PLE™ system then automatically starts pressurizing and heating the samples. The pressure is maintained at 1500-3000 PSI, at a temperature of 70-200 ºC. The extracted solvent containing the target analytes is then automatically transferred to a concentration/evaporation vessel where it is brought to final volume directly in a gas chromatography (GC) or liquid chromatography (LC) vial. The vial can then be transferred to the analytical instrument for final analysis.


 

Pressurized Liquid Extraction (PLE) System

The PLE® system is a high-speed pressurized liquid extraction system designed to perform sample extraction of multiple samples simultaneously. The PLE system delivers high recoveries and excellent precision for all analytes in minutes instead of hours. Inexpensive stainless steel extraction cells with end cap filtration keep operational costs at a minimum. Optional disposable end cap filtration increases productivity and saves valuable time. 

Reduce Solvent Costs
Pressurized liquid extraction uses as little as 15 mL of solvent compared to more than 500 mL of solvent required to perform Soxhlet extractions.

Reduce Solvent Waste
The PLE system reduces solvent waste by using solvents more efficiently.

Increase Productivity
The entire extraction and cleanup may be performed in less than 30 minutes. Traditional methods can take 10 to 16 hours.

Reduce Operating Costs
Rapid extraction and clean-up, along with reduced solvent use and waste, reduces operating costs by as much as 70 percent.

Five to 250 mL Extraction Cell Sizes
The PLE™ system offers 5-250 mL low cost stainless steel extraction cells with Teflon endcap filtration. This wide range of extraction cell volumes allows the use of the same unit for all sample sizes, even in the same run.

Modular, Expandable and Affordable
The modular design of the PLE system allows you to purchase a one, two or three sample system to fit your budget. The system can be expanded to a five or six sample system as your application grows.

Eliminate cross contamination
Optional low-cost disposable extraction cells and Teflon filtration endcaps ensure trouble-free extraction and eliminate the risk of cross contamination.

One-Step Sample Extraction and Cleanup
The optional in-line cleanup module performs the entire sample extraction and cleanup in one step with increased speed and reduced cost.

Automatic Operation and Documentation
Real-time software allows six channels of pressure and six channels of temperature data to be plotted simultaneously. This powerful feature allows automatic documentation of all extraction data. Temperature and pressure data can be superimposed and printed in either graphic or tabular format and stored for future reference.

PC Control and Monitoring
The entire extraction process is PC controlled enabling the laboratory technician to store and edit extraction protocols, as well as monitor and store extraction data.The DMS-6000 Editor allows multiple methods to be stored. Parameters such as time, solvent, volume and final temperature can be set for each step of each method. Pressure and temperature, as well as dispensed volumes, are displayed every second and stored for future reference. Six channels of pressure and six channels of temperature may also be plotted in real time. This powerful feature allows automatic documentation of the entire extraction data.

A Versatile Method Development Tool
The powerful DMS 6000 real time software along with a variety of extraction cell capacities and the ability to select multiple solvents, different temperature settings, as well as storage of data makes the PLE sytem an ideal tool for method development.

Modular Construction Provides for Easy Maintenance
The modular desgin of the PLE sytem combined with its exposed plumbing enables efficient system maintenance. The PLE system's channels are designed to operate independently, so if one channel fails the others will continue to perform. This versatility ensures easy replacement with no down time.

Leak and Clog Free Operation
Simple design combined with large bore plumbing enables the PLE system to operate virtually leak and clog free.

Multiple Extractions
Programming of variable pressure and temperature allows extraction of a variety of compounds.

 
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PLE 
 

Technical Specification

Extraction cell size:

5 mL, 10 mL, 20 mL, 40 mL, 70 mL, 100 mL, 250 mL

Simultaneous Extractions

1 to 6 independent extraction modules for simultaneous extraction

Variable Cell Size per Simultaneous Extraction Run

Run different cell sizes in the same simultaneous run 5 mL, 10 mL, 20 mL, 40 mL, 70 mL, 100 mL or 250 mL

Modular Design

Individual Extraction Modules can be isolated from the system without interrupting the running system, no down time.

Automated Sample Cleanup

Incell Sample Cleanup, Pre-packed Incell End Cap Sample Cleanup, Inline Column Sample Cleanup,

Interface to Automated Cleanup Systems

Seamless programmable interface to PowerPrep™ Multi-Column Sample Cleanup System

Interface to Automated Concentration Systems

Seamless Programmable interface to the SuperVap Concentrator to provide one step extraction and concentration or one step extraction, sample cleanup and concentration

Flow Rate

0 to 35 mL per minute

Pressure

0 to 2500 PSI

Temperature

Ambient to 200 ºC

Solvents

No limitation, mixing or selection of up to six different solvents

Collection Vessels

Direct to a SuperVap Concentration Vessel or SuperVap Direct to GC Vial Concentration Vessel. All other standard collection vessels.

Automatic Documentation

The DMS-6000 software allows multiple methods to be stored. Each parameter such as time, solvent volume, and final temperature can be set for each step. Pressure, temperature and dispensed volumes are displayed real time. All parameters for each run are documented and stored for future reference.

DMS 6000 Software

 

The PLE™ system uses a PC to control the entire extraction, sample cleanup and concentration process. The DMS-6000 real time software allows multiple samples to be processed simultaneously.

Recoveries and Reproducibility

Method compliance or better

Real Time Monitoring, Plotting of Pressure and Temperature 

 

 

The DMS-6000 real time software allows six channels of pressure and six channels of temperature to be plotted in real time. This powerful feature allows automatic documentation of the entire extraction data. The temperature and pressure can be superimposed and printed in graphic or tabular format.

One Step Automated Extraction, Sample Clean up and Concentration Control Software

Used to write, and edit extraction protocols, monitor, and store the extraction, ample cleanup and concentration data. It also controls the entire sample prep process.

Automatic Extraction Data Report

 

The DMS-6000 real time software allows the creation of an automatic data report based on the sample sequence set up. Printed data contains the graph and parameters of the sample extraction.

 

Weights:

PLE Pump module = 10 lbs

PLE Control module = 15 lbs

PLE valve module = 15 lbs

PLE structure = 27 lbs

PLE Large cabinet = 18 lbs

PLE small cabinet = 24 lbs

PC = 21 lbs

Monitor = 10 lbs

Weights:

Small cart = 35 lbs

Small tray = 20 lbs

Medium cart = 40 lbs

Medium tray = 25 lbs

Large cart = 45 lbs

Large tray = 35 lbs

 

Small cabinet + pump module + control module = 50 lbs

Large cabinet + valve module + structure = 60 lbs

PC + monitor = 30 lbs

PLE1 = 110 lbs + 30 lbs = 140 lbs

PLE2 = 170 lbs + 30 lbs = 200 lbs       

PLE3 = 230 lbs + 30 lbs = 260 lbs       

PLE4 = 290 lbs + 30 lbs = 320 lbs

PLE5 = 350 lbs + 30 lbs = 380 lbs

PLE6 = 410 lbs + 30 lbs = 440 lbs

 

Dimensions:

PLE1 = 15” (38 cm) W X 35” (90 cm) H X 18” (45 cm) D

PLE2 = 23” (58 cm) W X 35” (90 cm) H X 18” (45 cm) D

PLE3 = 31” (78 cm) W X 35” (90 cm) H X 18” (45 cm) D

PLE4 = 39” (98 cm) W X 35” (90 cm) H X 18”(45 cm) D

PLE5 = 47” (118 cm) W X 35” (90 cm) H X 18” (45 cm) D

PLE6 = 55” (138 cm) W X 35” (90 cm) H X 18” (45 cm) D

 

Dimensions with cart and tray:

PLE2 = 37” (94 cm) W X 64” (162 cm) H X 30” (75 cm) D

PLE3 = 45” (114 cm) W X 64” (162 cm) H X 30” (75 cm) D

PLE4 = 64” (162 cm) W X 64” (162 cm) H X 30” (75 cm) D

PLE5 = 64” (162 cm) W X 64” (162 cm) H X 30” (75 cm) D

PLE6 = 64” (162 cm) W X 64” (162 cm) H X 30” (75 cm) D