1. NETCHEM Remote Access Laboratory Guide
Screening analysis of landfill leachate by GC-MS
Author: PhD Ivana Mihajlović, assistant professor
Technical assistance: PhD Maja Sremački, assistant
Technical processing: Nikola Maoduš
Institution: University of Novi Sad, Faculty of Technical Sciences, Department of Environmental Engineering and Occupational Safety and Health, Trg Dositeja Obradovića 6, Novi Sad
Course: Modern Instrumental Methods of Pollutants Analysis in the Environment
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This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

2. Background Educational objectives
1. To learn how to prepare sample by liquid-liquid extraction and Kuderna- Danish evaporation for GCMS analysis
2. To learn how to make a method for GC-MS screening analysis
3. To analyze GC chromatograms and MS spectra
4. To gain experience in GC-MS usage
4. To gain experience in identifying specific pollutants from the landfill leachate
5. To gain knowledge on the influence of different polarity of the used solvent for liquid-liquid extraction to the results of GCMS analysis

3. Equipment and materials
Chemical substances:
Dichloromethane (DCM),
n-Hexane (HEX),
Sodium sulphate (anhydrous)
Internal standard (phenanthrene d-10)
Laboratory equipment and consumables:
Digester,
Kuderna-Danish apparatus (KD),
Water bath,
Separatory funnel (2 L),
Glass beakers (100 mL),
Spoon,
Glass vials (2 mL),
Stands and clamps,
Automatic pipette (5 mL and 1000 μL),
Graduated cylinders (50 mL),
Volumetric flasks (1 L)
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This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

4. Procedure: Sample preparation:
Measure 1 L of landfill leachate sample for analysis.
Spike the sample with 100 μL of internal standard solution (phenathrene d-10, ppm)
Shake the volumetric flask to homogenize the sample
Transfer prepared sample into the separatory funnel and add 20 mL of solvent (dichloromethane or n-Hexane)
Shake the separatory funnel for 30 minutes.
Separate the extract (solvent) to glass beaker.
Repeat procedure two more times.
Add 1 spoon (approximately 5 g) of anhydrous sodium sulphate to remove water from the extract.
Transfer separated extract into the Kuderna-Danish apparatus.
Evaporate the extract to 2 mL or less.
Transfer the evaporated extract to glass vial for GCMS analysis.
______________________________________________________________________________________________________
This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

5. Gas chromatography – mass spectrometry (GC-MS) analysis
Set the GC and MS parameters for screening analysis:
GC Parameters :
Injector temperature: 220 ° C (can be higher, up to 270 °C)
Sample injection: splitless, sampling time: 1 min
Sample volume: 1μL
Column temperature program:
Aquision delay: 10 min (1 min would be better)
Initial temperature: 40 ° C for DCM, and 70 ° C for n-hexane
Temperature gradient: 2 ° C/min (20° C/min for 2 min and then 2 ° C/min would be better)
End program temperature: 300 ° C
Carrier gas flow: 1 mL/min (He 5.0, Messer)
Flow control mode: constant pressure, 100 kPa (or liner velocity can also be selected)
Transfer line temperature: 250 °C
Column type: HP-5MS, 30m x 0.25mm x 0.25μm
MS Parameters:
Ion source temperature: 230 °C
Quadrupole temperature: 150 °C
Electron energy: 70 eV
Time delay: 10 min
Acquisition mode: SCAN m/z
______________________________________________________________________________________________________
This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

6. Data analysis
Identify specific pollutants from the landfill leachate by comparing MS spectra of identified peaks in GC chromatograms with NIST Mass Spectral Library.
Calculate ratios of peak area vs. internal standard area for each identified peak in GC chromatograms.
Compare results obtained from analysis of samples extracted by dichloromethane and n-hexane.
Discuss influence of the polarity of solvent for liquid-liquid extraction to the results of GCMS analysis.
______________________________________________________________________________________________________
This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

7. Prerequisites Students should to:
familiarize themselves with basics of GC/MS technique
familiarize themselves with Team Viewer software (a guide is provided at NETCHEM page),
see materials uploaded at the course's Moodle page ( )

8. Remote access classroom-laboratory
DESCRIPTION OF REMOTE ACCESS
NETCHEM COMMUNICATION SIDES
(NOTE: NETCHEM Communication is defined as event that involves all kinds of internet interactions (in real time and not in real time) between participants via devices (PCs, laptops, tablets and mobile phones))
host side
(NOTE: Host side of NETCHEM Communication is defined as PC who invites other users to join the session)
Participant’s PC in the classroom
guest side
(NOTE: Guest side of NETCHEM Communication is defined as PC who joins the invitation to session)
Participant’s PC in the laborotory
COMMUNICATION SOFWARE
Team Viewer
Meeting: No
Remote control: Yes
Meeting and Remote control simultaneously: Yes
Skype
Call 1:1: No
Conference Call: No
COMUNICATION HARDWARE
on host side
1 PC for each participant
on guest side
1 PC, headset with microphone and camera
INFORMATION EXCHANGE TYPE
Educational (one side is dominantly receptive)
Place of Educator participant:
Number of educator(s):
Place of student participant:
Number of student participant(s):
Consultative (two sides are equal in giving-receiving information)
Yes
Number of host side participant(s): up to 5+ professor
Number of guest side participant(s): 1 educator in laboratory

9. Remote Access Connection Instructions
What makes these labs different and unique from other classroom experiments is that we have incorporated a section in each activity to remotely characterize your samples from your classroom.
Request a remote lab session specifying information such as: the day, the time, and the instrument you are interested in using by visiting our web site:
You will see the list of partners with the instruments provided to chose from.
You will be contacted by a Remote Access staff member to set up a test run to ensure you are set up properly and have the required infrastructure.
Send samples or verify the in-house sample you would like us to prepare and load for characterization.
Send your samples to the Remote Access center that you chose on your request.
There are two communications soft-ware packages, that will allow us to communicate instructions and answer questions during the session.
- TeamViewer: You can obtain a free download at:
- Skype
______________________________________________________________________________________________________
This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

10. Remote Access Connection Instructions
You will need:
Computer with administrator access to install plug-ins and software
An internet connection
Speakers
Microphone
Projector connected to the same computer
Web browser (Firefox preferred)
During the test run you can refer to this guide to perform the following steps, but it’s very important that you only proceed with these steps during your scheduled times. You may interfere with other remote sessions and potentially damage equipment if you log in at other times.
Open and logon to your Zoom/Team-viewer account. You will be given the access code to enter at the time of your test and then again during the remote session.
If you are using the Zoom software, Remote Access staff will give you the access code.
If you are using the Team-viewer software, Remote Access staff will give you the ID & password.
You should soon see the Remote Access desktop and at this point you can interact with the icons on the screen as if it were your desktop.
Switch to full screen mode by selecting the maximize screen option in the top right corner of the screen.
Upon completion of the session, move your mouse to the top right corner of the screen, and click on the X to disconnect the remote session. It will ask if you want to end the remote session. Click Yes.
______________________________________________________________________________________________________
This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

11. Author, Editor and Referee References
This remote access laboratory was created thanks to work done primarily at University of Niš.
Contributors to this material were: dr Ivana Mihajlović
Refereeing of this material was done by: _____________________
Editing into NETCHEM Format and onto NETCHEM platform was completed by: ______________
______________________________________________________________________________________________________
This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

12. References and Supplemental Material
The NETCHEM platform was established at the University of Nis in through the Erasmus Programme. Please contact a NETCHEM representatives at your institution or visit our website for an expanded contact list. The work included had been led by the NETCHEM staff at your institution.
______________________________________________________________________________________________________
This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.