NETCHEM Remote Access Laboratory Guide NETCHEM Screening analysis

NETCHEM Remote Access Laboratory Guide NETCHEM Screening analysis of landfill leachate by GC -MS Author: Ph. D Ivana Mihajlović, assistant professor Technical assistance: Ph. D 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, 21000 Novi Sad Course: Modern Instrumental Methods of Pollutants Analysis in the Environment ___________________________________________________ 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.

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 ___________________________________________________ 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.

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 m. L), Spoon, Glass vials (2 m. L), Stands and clamps, Automatic pipette (5 m. L and 1000 μL), Graduated cylinders (50 m. L), Volumetric flasks (1 L) ___________________________________________________ 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.

Procedure: Sample preparation: 1. Measure 1 L of landfill leachate sample for analysis. 2. Spike the sample with 100 μL of internal standard solution (phenathrene d-10, 0. 02 ppm) 3. Shake the volumetric flask to homogenize the sample 4. Transfer prepared sample into the separatory funnel and add 20 m. L of solvent (dichloromethane or n-Hexane) 5. Shake the separatory funnel for 30 minutes. 6. Separate the extract (solvent) to glass beaker. 7. Repeat procedure two more times. 8. Add 1 spoon (approximately 5 g) of anhydrous sodium sulphate to remove water from the extract. 9. Transfer separated extract into the Kuderna-Danish apparatus. 10. Evaporate the extract to 2 m. L or less. 11. 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.

Gas chromatography – mass spectrometry (GC-MS) analysis Set the GC and MS parameters for screening analysis: GC Parameters : MS 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: Ion source temperature: 230 °C Quadrupole temperature: 150 °C Electron energy: 70 e. V Time delay: 10 min Acquisition mode: SCAN m/z 47 -500 • 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 m. L/min (He 5. 0, Messer) Flow control mode: constant pressure, 100 k. Pa (or liner velocity can also be selected) Transfer line temperature: 250 °C Column type: HP-5 MS, 30 m x 0. 25 mm x 0. 25μm ___________________________________________________ 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.

Data analysis 1. Identify specific pollutants from the landfill leachate by comparing MS spectra of identified peaks in GC chromatograms with NIST Mass Spectral Library. 2. Calculate ratios of peak area vs. internal standard area for each identified peak in GC chromatograms. 3. Compare results obtained from analysis of samples extracted by dichloromethane and n-hexane. 4. 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.

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 (http: //mdl. netchem. ac. rs/course/view. php? id=29 ) Moodle page

Remote access classroom-laboratory DESCRIPTION OF REMOTE ACCESS 1. 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 Participant’s PC in the classroom users to join the session) guest side Participant’s PC in the laborotory (NOTE: Guest side of NETCHEM Communication is defined as PC who joins the invitation to session) 1. COMMUNICATION SOFWARE Meeting: No Remote control: Yes Team Viewer Meeting and Remote control simultaneously: Yes Call 1: 1: No Skype Conference Call: No 1. COMUNICATION HARDWARE on host side 1 PC for each participant on guest side 1 PC, headset with microphone and camera 1. INFORMATION EXCHANGE TYPE Educational (one side is dominantly receptive) Consultative (two sides are equal in giving-receiving information) Place of Educator participant: Number of educator(s): Place of student participant: Number of student participant(s): Yes Number of host side participant(s): up to 5+ professor Number of guest side participant(s): 1 educator in laboratory ___________________________________________________ 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.

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: http: //netchem. ac. rs/remote-access 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. - Team. Viewer: You can obtain a free download at: https: //www. teamviewer. com/en/index. aspx - 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.

Remote Access Connection Instructions V. You will need: a) Computer with administrator access to install plug-ins and software b) An internet connection c) Speakers d) Microphone e) Projector connected to the same computer f) Web browser (Firefox preferred) VI. 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. a) 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. b) 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. c) Switch to full screen mode by selecting the maximize screen option in the top right corner of the screen. d) 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.

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.

References and Supplemental Material The NETCHEM platform was established at the University of Nis in 2016 -2019 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.