Standard Operating Procedure Malvern Zetasizer Nano ZS Tool Manager: Rohit Singh TM e-mail: [email protected] TM Phone #: 607-379-3953 Daniel Group contact: [email protected] Safety: Independent use of the Zetasizer requires the following EHS trainings: Laboratory Safety Chemical Waste Disposal Cryogen Safety Formaldehyde Awareness Compressed Gas Safety Equipment Damage Warning: Keep large solutions away to prevent catastrophic spillage damage. Do not wear gloves when using the computer mouse or keyboard. Equipment Sharing Policy: Users are required to bring their own cuvettes. Many people’s projects depend on a properly working Zetasizer - so please be careful! Please reserve the machine 12hrs in advance through our Google Calendar. Contact the Tool Manager for access to the calendar. If you make/cancel an appointment before 12 hours until usage, please notify the Daniel Group so that others can change their plans. Document and report any malfunction to the Tool Manager. For immediate assistance, ask anyone in the Daniel Group for help (Olin Hall 265). Startup procedure: The power switch for the Zetasizer is located in the back right of the machine. Turn the machine on. It should make several “beeps:” o One beep immediately after being turned on o A second beep to indicate that it has finished its initialization routine and status checks o Two beeps to indicate that the machine has reached 25°C. The computer should be on. If not, turn it on and ask a Daniel Group member to login to it. Double-click on the “Zetasizer Software” icon on the Desktop. Sample preparation: Getting an appropriate concentration: o Often the correct concentration must be determined empirically. o A concentration that is too high is more likely than a concentration that is too low. o Ideal concentration depends on particle size. See table of recommended concentrations for more information. o The concentration should be low enough that particle interactions do not occur. o Gels cannot be measured with DLS. Filter all dispersants or solvents to avoid contaminating the sample. Use the correct cell: o Size measurements on samples with aqueous solvents: disposable polystyrene cuvettes (DTS0012) o Size measurements with organic solvents or molecular weight or protein measurements: glass or quartz cuvettes o Zeta potential: DTS1070 (not resistant to organic solvents), dip cell (ZEN1002) for organics Fill the cell: o Size and Molecular weight: the sample depth should be between 10 mm and 15 mm (the measurement is made 8 mm from the bottom of the cell) o Zeta potential: (DTS 1070 only, see Tool Manager for dip cell instructions) 1. Prepare the sample in a syringe of at least 1 ml capacity. 2. Place the sample syringe into one of the sample ports. 3. Invert the cell. 4. Slowly inject the sample until the U tube is filled just over half way. 5. Tap the cell gently to dislodge any air bubbles. 6. Turn the cell upright and continue injecting slowly until the liquid reaches the bottom of the outlet on the other side. 7. Tap gently to dislodge bubbles, make sure electrodes are immersed, remove syringe, and insert cell stoppers. SOP measurements: Create a new measurement file: File-New-Measurement File Name and save the file. Start SOP measurement: Measure-Start SOP Select desired SOP: MicroCuvetteSize.sop should work as a template for size measurements. Follow the instructions on the screen, including inserting the cell and pressing Start to start the measurement. o Inserting the folded capillary cell for Zeta potential (DTS1070): 1. Place a thermal contact plate into the recess on either side of the folded capillary cell. 2. Open the cell area lid and insert the cell. Either orientation should be OK, but it may be better to make sure the weld line is closer to the front of the machine. o Size and molecular weight: the “V” should face the front. Measurement data will be saved automatically. Data can be transferred to Excel or other software using Edit-Copy. Creating an SOP: Create a new file or edit an existing file: File-New-SOP or File-Open-SOP. Select the Measurement type. This will change the options available in the editor. Fill in the parameters for the material used, the cell used, and the desired measurement parameters. Name and save the file. Recommended Concentrations of Samples for Different Particle Sizes Particle Size Min. Concentration Max. Concentration (Recommended) (Recommended) < 10 nm 0.5 g/l Only limited by the sample material interaction, aggregation, gelation, etc. 10 nm to 100 nm 0.1 mg/l 5% mass (assuming a density of 1 g/cm3) 100 nm to 1 µm 0.01 g/l (10-3 % mass) 1% mass (assuming a density of 1 g/cm3) > 1µm 0.1 g/l (10-2 % mass) 1% mass (assuming a density of 1 g/cm3)
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