Table of Contents 1. 2. 3. 4. 5. 6. 7. AFM/Bruker AFM/Asylum CombiFlash Contact Angle Delsa Nano AT&C Dynamic Light Scattering Differential Scanning Calorimetry (DSC) 7.1. Flash DSC 8. Fourier Transform Infrared Spectrophotometer (FTIR) 9. Gel Permeation Chromatography 9.1. Chloroform 9.2. Dimethylformamide 9.3. Tetrahydrofuran-Light Scattering 9.4. Tetrahydrofuran-UV-Visible 9.5. Preparatory 10. Glove Box 11. High Performance Liquid Chromatography 12. Microscopes 13. QCM-D 14.
Asylum AFM SOP1 Model: Serial Number: MFP Controls Before flipping over Housing, raise the stage to its MAX as to not crash the tip into the surface 1. Flip over Housing; make sure Housing is level 2. Click Live Video (Screen Image on bottom) 3. Turn on light at computer. Align at instrument to find the cantilever 4. Adjust back & right dials to increase SUM to its MAX VALUE 5. Adjust left dial to make REFLECTION = 0 6. Turn light off, close live video Tune Tab 1.
2. Raise Z VOLTAGE to MAX VALUE (150 is MAX VALUE; if 150 is reached, reengage tip by lowering the tip until the Z VOLTAGE = 30-40; Click Set Point Dot and raise Z VOLTAGE to MAX VALUE again. Repeat until MAX VALUE ≠ 150) 3. Click Clear Image 4. Click Do Scan 5. Change Dots between Set Point/Integral Gain/Drive Amplitude to match the Trace to be close to the Retrace (Click Slow Scan Disabled to hold the scan line steady) 6. Unclick Slow Scan Disabled, click Clear Image, and click Frame Up/Frame Down. 7.
Comment [D1]: Title Arial 14 Contact Angle Analyzer (Theta, optical tensiometer) 1. Turn on the instrument and start program. 2. Experimental Setup Click Contact Angle experiment Write the Name of the experiment. Select User, Solid, Liquid (Heavy phase) Then, click Start 3. Image Recording Lift or lower the sample stage until the solid is visible on the bottom part of the screen. If nothing is seen on the screen, restart from the first step. There might be some error in the system.
Click on the image near the border between the drop and the background and the Focusing window will open. To adjust the focus of the image turn the camera lens focus adjustment until the image is focused. Click Adjust Camera Setting to get appropriate intensity (green on Focusing window). Approach the sample stage to touch the drop. Click Record and wait for the images to be recorded and then press Done. 4.
5. Data Analysis From the main menu select Browse Experiments. Use the Find Experiment parameters to find the wanted experiment and select it. Right click on it and select Graph. The default graph shows contact angle against time. If the contact angle is stable from the beginning of the graph onwards then simply press Calculate and from the Calculated Values window press Calculate again to view the relevant statistical information available.
Differential Scanning Calorimetry (DSC)2 Model: Serial Number: The following is the Standard Operating Procedure (SOP) for the Mettler Toledo DSC 822e. All Mettler Toledo instruments are operated using the STARe software v10.00d. I. General Use 1. Double click STARe Software 2. A prompt will appear asking for the User Name and Password. The User Name is METTLER; there is no password. Hit OK. 3. Two windows will open; one controlling each of the attached devices. Open the window controlling the DSC 822e.
4. On the left hand portion of the window, select Routine Editor. 5. Hit Reset in the lower right hand corner of the window. 6. If a method needs to be created, select New and create a program for the TGA (for specifics on creating a new Method, please refer to the person/s in charge of the instrument). If a method is already created, select it using the Open tab. The pans used are 40 µL aluminum pans with a pin on the bottom. The pin allows for accurate sample placement on the sensor.
temperature possible without sample degradation. Most runs should not come within 25 °C of the Td. When choosing a method, determine if the method is appropriately made.
9. Open up the nitrogen line. Make sure the leftmost flowmeter by the DSC is reading between 10 and 50 mL. 10. Before opening the liquid nitrogen dewar, check the level. If it is empty, ask someone in charge of the instrument for help in how to fill it up. If it is sufficiently full, turn it on 11. Click Start at the bottom right hand of the window. This will open the experiment on the module. A prompt wil appear in the green bar that says Going to Insert Temperature. Click OK.
High Performance Liquid Chromatography (HPLC) Model: Serial Number: Before switching on the instrument 1. Sign-in with date, name and sample information on the HPLC log book 2. Check solvent levels in each container at the top of the DGU-20As degasser and make sure that the tube filters are fully immersed in the liquids. If the solvent levels are low, sonicate HPLC grade solvent in a separate container for about 10 min and refill the containers with appropriate solvents 3.
9. Instrument: On the LC-20AD liquid chromatograph, open the drain by turning the knob anti-clockwise, and press purge. When purging is complete, close the drain by turning the knob clockwise 10. Instrument: Press pump to turn on the pump and allow for pressure to stabilize and record the final pressure (allow solvent flow for about ~ 10 min and monitor pressure) Setting parameters for the analysis 11.
created method file, click on the black arrow at the right corner of the box on the table and load the already saved method file 14. Software: Once the table is complete, save batch file by clicking on File>Save batch file as 15. Software: Click on batch start (green triangle on the left) 16. During the analysis make sure that the solvent levels do not run below ~300 mL and that the waste bottle does not overflow 17.
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Solvent Purification System (SPS) On an everyday basis, each solvent should look like figure 1. Please check the argon tank to ensure that it is above 500 before using. If it is below 500, notify those in charge and it will be replaced by one of them. In addition, make sure the gauge (located on the left side) on the SPS is between 10 -15. Argon Vacuum Figure 1 – system is open to argon Argon Vacuum Figure 2 – system is closed When a solvent flask is empty: 1.
Argon Figure 3 – system is closed Vacuum Argon Vacuum Figure 4 – system is open to vacuum 10. After 30 minutes, switch the system to argon for 5 – 10 seconds (should look like figure 1). 11. Repeat steps 8 – 10. 12. Repeat step 8 and 9. 13. Close the system by turning the bottom knob to its horizontal position (should look like figure 3). Argon Vacuum 14. Switch the top knob to argon (should look like figure 2). 15.
Spectrofluorophotometer Standard Operating Procedure Model: Serial Number: For the Panoroma Fluorescence 2.1 software: 1) Hit the white switch to turn on the spectrofluorophotometer. Do not touch the XE lamp switch (black). Listen for the clicking sounds. Once the instrument is on, the power indicator lamp (front face) will light up. 2) Wait for 15 minutes. 3) Open software “Panoroma Fluorescence 2.1”. 4) Insert cuvette into sample holder (position 1). 5) Under “RF5301”tab, click on “2D emission”.
Spectrum type EM wavelength EX wavelength range Recording range Scan speed Sampling interval EX / EM Slit width Sensitivity Response time OK to validate the parameters. Insert cuvette with distilled water into sample holder. Click on START. When scan is completed, filename box appears. Enter file name and comment. Select SAVE. Select PRESENTATION, GRAPH to change the looks of the screen plot. For a hard copy, choose PRESENTATION, PLOT to bring up the PLOT LAYOUT window.
Concentration range (Low to High) Recording range (Low to High) Sensitivity Auto scan (if necessary) Response time (0.02) Repetitions If using Mulitpoint Curve, select order of curve and zero intercept Select OK to validate Prepare standards (at least 4). Auto zero the instrument with sample compartment empty or with a cuvette with solvent used as a blank. Select STANDARD push button. Place first standard in cuvette and put into the sample compartment. Select READ. The EDIT STANDARD box appears.
EX / EM slit width Sensitivity Response time (auto) Reaction time Timing mode (auto) Units (seconds) Select OK to validate Verify contents of sample compartment (may be empty) Auto zero Select START to plot noise When completed, enter file name (will be a .tmc file) and SAVE Presentation—Graph—Limits to manually input values for Y and X axes. Select OK. Push Buttons Go to wavelength will allow setting of both emission and excitation wavelengths.
Thermogravimetric Analysis (TGA) The following is the Standard Operating Procedure (SOP) for the Mettler Toledo TGA/DSC 1. The instrument is coupled to a Pfeiffer Vacuum Mass Spectrometer (Prisma Plus QMG 220). All Mettler Toledo instruments are operated using the STARe software v10.00d. The Mass Spectrometer is operated using the QUADERA software v4.40. I. General Use 13. Double click STARe Software 14. A prompt will appear asking for the User Name and Password.
16. On the left hand portion of the window, select Routine Editor. 17. Hit Reset in the lower right hand corner of the window. 18. If a method needs to be created, select New and create a program for the TGA (for specifics on creating a new Method, please refer to the person/s in charge of the instrument). If a method is already created, select it using the Open tab. The most common method for the TGA is 25-500 °C at a rate of 10 °C/min entitled 25-500 C; Ar 10 ml/min; Alumina 70ul.
For coupled TGA/MS runs (either individual or multiple samples), the method used should have a 5 minute Argon “purge” at 25 °C to equilibrate the signals detected by the MS. For further TGA/MS instructions, please refer to Section II. When creating a new method/using an old method, make certain that the pan being used matches the pan as outlined in the method. The most commonly used pans are the 70μl Alumina pan and the 100μl Aluminum pan.
In the window, select Pan and hit OK. This will weigh out the pans for all experiments. Each pan takes between 3-5 minutes to weigh. 23. When the pans are weighed, add your samples to the pans. Right click on the experiments, select Weigh In Auto… then select Sample and hit OK. 24. When all samples are weighed, select Start at the bottom right hand of the window. This will open the experiment on the module and will begin the experiment. Samples will run sequentially until all samples are finished.
. When the sample is done running, follow the procedures for cleaning the alumina crucibles below. If an aluminum pan was used, the crucible can be disposed. Alumina Crucible Clean Up General Note: The white alumina crucibles are not disposable and should be reused. Please clean these after use. 1. 2. 3. After completion of the TGA program, remove the alumina crucible and place it in a solution of 1 M hydrochloric acid solution. Sonicate the solution to remove as much charred residue in the crucible.
Window 1 Window 2 3. In Window 1, select the first line.
Under Template, select the template you would like to run for your first TGA sample. Templates are located in My Documents > My QUADERA > QMG220 > Templates. A premade template is available for general use: Kevin Unknown Bargraph Cycle. This template will measure from 0-300 mass units over a span of 30 seconds (10 ms/amu). If you do not know what will come off your sample, use this sample.
Add and delete task as necessary using the Add Task and Delete Task buttons. Once done, click Save. 4. When all samples are added, select Start on the TGA/DSC1 window.
Once start is hit, open up the Triggered Run window (Window 1). Click Connect. Once the system is connected, click Start. The TGA/MS run is now complete and should run. If the first experiment in the MS did not run, there was too long of a delay between hitting Start in the Triggered Run window. If the subsequent experiments did not run, there was too long of a delay between the end of the first experiment and the start of the second experiment.
UV Probe Demonstration Procedure Features UVProbe has the following features: 1. Abundant processing functions 2. User Interface Customization 3. Spectrum 4. Photometrics/Quantitation 5. Kinetics 6. Report Generator Outline 1. Starting the Software 2. Spectrum Window 3. Connecting the Instrument 4. Setting Measurement Parameters 5. Data Collection 6. Data Saving 7. Data Display 8. Data Processing 9. Report Generator 10. Photometrics 11. Quantitation 12. Kinetics 13.
This screen should appear once the software is started. The software is divided into 4 modules: Spectrum, Photometrics (Quantitation), Kinetics, and Report Generator. These Modules can be selected by clicking on the correct Icon or selecting the module from the Window pull down menu. Choose the spectrum module if that is your customer’s main application. If they prefer to use the Photometric, Skip to step10 or Quantitation module, Skip to step11. For a Kinetics demo, skip to Step 12. 2.
Method Pane Graph Pane These various windows can be customized for the users preference by turning them on or off in the View Menu. 3. To Connect Instrument (Skip to Step 7 if you are just showing the features of the software) The current version of the UVProbe Software will control the UV-1601, UV-1700, UV-2401, UV-2501, UV-2101, and the UV-3101. A. Select [Window] > Spectrum to open the Spectrum module. A module must be active before the spectrophotometer can be connected. B.
The Instrument Parameters tab is used to determine the instrument settings. Options will vary slightly depending on the instrument being used. The important settings here are the measuring mode and the Slit Width. Set these for your sample. The Attachments Tab is used to set the parameters for any accessories that are being used. As you select the various accessories, the parameter setting boxes on the right will change.
5. Data Collection Click [Baseline] on the Photometer Button bar at the bottom of the screen and click [Ok] in the Baseline Parameters dialog box. Remember, Baseline corrects over the entire selected wavelength range. The Autozero function corrects at one wavelength. Perform a spectral scan by inserting the sample into the spectrophotometer. Click the [Start] button. After the scan, enter a file name in the New Data Set dialog box and click [Ok]. 6.
The Overlay tab will show all open spectral data on the same graph. This allows easy comparison between samples. During data collection, the spectra will appear in the Overlay tab. The Stacked tab displays all open spectral data in individual graphs. Spectra can be chosen to be displayed or not by using the legend function.
8. Data Processing UV Probe has vast data processing capabilities. Most calculations that a customer wants to do can be done under the Manipulation menu. The Manipulation pane is in the top left corner of the screen. Calculation results and information will show up in this pane. A. Data Print: Shows a table of the raw data of Absorbance or Transmittance versus the wavelength for the open spectra. This table can be copied and pasted into other programs such as Excel B.
D. Point Pick: Gives a table of results for specified wavelengths in a spectra. These wavelengths can be saved as a template for repeat use on multiple spectra. E. Peak Area: Provides area under peak results for wavelength regions within the spectra. These areas are indicated by shading on the graph. F. Sewing Box: This function allows the customer to isolate regions of a spectra by cutting off defined wavelength ranges. (Many features of this function are not available in GLP mode) 9.
A. Insert Typed Text: Refers to text that may be input by the user directly onto the report. This text may include the Report Title, Company Name, or any other information that will not change with each report. 1. Go to [Insert]>Text. A Text Box will appear in the Report Window, type in desired text. This Text may be the report title, Company Name, or any other information that will not change with each report. 2.
You have now gone through the Spectrum Module. If your customer wants to also see Photometrics, continue to Step 10. For Quantitation, skip to Step 11 If your customer is more interested in Kinetics, skip to Step 12. 10. Photometrics The Photometrics/Quantitation module is very flexible and easy to use. This procedure will take you through setting up a general photometrics table. A. Data Collection Method 1. Select [Edit] > [Method] and click on the [Wavelengths] tab.
2. Click on the [Calibration] tab. a. Select [Multi Point] in the Type box and [Fixed Wavelength] in the Formula box. b. Select [WL224.0] in the WL1 box. In the Order of Curve box, select [1st] 3. Click on the [Instrument Parameters] tab and ensure that the Measuring Mode is set to [Absorbance], and click [Close]. B. Read the Standard and view a Calibration Curve 1. Click anywhere in the Standard table to activate it. Enter the appropriate standards and their concentration values into the table. 2.
2. Click on the [Instrument Parameters] tab and select [Absorbance] as the Measuring Mode. Click [OK] and the Photometer status bar will display “Slewing” and then the current wavelength value of 550 nm. B. To Prepare a Powder Sample 1. Place a cuvette of deionized water into the sample compartment of the spectrophotometer. 2. Click [Auto Zero] on the Photometer Button bar. (This step will zero the Photometer unit at a designated wavelength, i.e.
On the Y-axis, click the minimum absorbance value, then change the value to [0.0]. Click the maximum value and change it to 4.0. 2. Click [Start] on the Photometer Button bar to initiate Time Course measurement. When measurement is completed, enter a file name into the New Data Set dialog box and click [Finish]. 1. 13. Help Functions The UVProbe Help section is a key tool to learning the software and understanding UV-Vis measurements in general.
Sampling Interval (nm) 0.05 0.10 0.20 0.50 1.0 2.
Appendix B Saving Data with UVProbe UV Probe consists of three units in the filing system- the FILE, the STORAGE, and the DATA SET. FILE- This is the basic data container that will be opened for use in UV Probe. It will also be what is seen in Windows Explorer. A new FILE is created only when new data is acquired from the instrument. STORAGE- This is a subunit of the FILE and helps to organize and keep track of data and manipulations. Each FILE will contain at least one STORAGE.
Step 2. Choose to save all spectra under the same file. This is done by selecting File and then Properties. A window will appear showing the File Properties of the open files. Highlight the File that you wish to save all data under (Customer A Demo in this example) and enable the “Store All Data in Single File” option. The Enable/Disable button at the bottom of the window will toggle to Enabled when the function is activated and Disable Step 3. Collect Additional Spectra.
Repeat collection of spectrum for Holmium Oxide Filter. Since all spectra have been saved under the same File, the properties will appear as follows: In the Properties window, you can see each spectrum in a separate Data Storage. The data set for each spectrum is listed as Raw Data. Step 4. Manipulation of Data. Perform the transformation from Absorbance to % Transmittance on the Didymium Spectrum. When this is done, a window appears asking for a name for the Data set.
transformations are always saved with the Raw Data sets. After this is done, the File Properties will appear as follows: Saving all data in the same file has many advantages including easy organization of data and the ability to recall many data sets by simply opening one file. If you choose not to save all data in the same file, after running the three spectra from above, your file properties may appear as follows: This is certainly more confusing and time consuming than the other method.
Additional Helpful Hints When the number of loaded files becomes large, the File Properties Dialog box can be resized using the gripper bar in the bottom right corner. When clearing files from memory, multiple files may be selected by using the shift or control key. When there is a Red Asterisk in the folder of a File Properties listing, the file has been modified and has not been saved. Deleting a file in this condition will result in a loss of data.
Miscellaneous 50
Nanopure Water Important: When not in use, the system must be kept in “standby” Dispensing water: Press “start” Press “” Auto dispense menu ? Press “enter” Dispense method (vol) Press “enter” Change volume by “” or “” Press “enter” Press “dispense” Press “standby” when done 51
