Calmetrix I-Cal 8000 User Manual

Isothermal calorimeter for concrete and cement

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Page 2 Calmetrix I-Cal 8000 User Manual CALMETRIX INC. I-CAL 8000 ISOTHERMAL CALORIMETER FOR CONCRETE AND CEMENT USER MANUAL...
Page 4 • wet environment. DISCLAIMER Calmetrix does not assume any liability as related to the accuracy, relevance or interpretation of results while using I-Cal or the CalCommander software. COPYRIGHT This User Manual is subject to copyright and may not be reproduced in whole or part without permission.
Page 6: Table Of Contents
Calmetrix I-Cal 8000 User Manual © 2010 - 2012 Calmetrix Inc. – All rights reserved TABLE OF CONTENTS __________ BEFORE YOU START USING THE EQUIPMENT …………………………………. Page 7 GENERAL USE …………………………………………………………………………. Page 9 HANDLING INSTRUCTIONS ………………………………………………………….. Page 9 CALIBRATION……………………………………………........... Page 10 OPERATING YOUR EQUIPMENT –...
Page 8: Before You Start Using The Equipment
Place the Calorimeter Unit into the Temperature Control Unit and connect the Calorimeter USB cable to the internal USB plug Never lift or transport your I-Cal 8000 while the Calorimeter Unit is placed inside the Temperature Control Unit. Always remove the Calorimeter Unit first.
Page 9 NOTE: your I-Cal 8000 includes one free software license for the I-Cal Logger logging interface and one license for the I-Cal Reports report generator. The computer you register for the use of your I-Cal will be the only computer registered. To purchase additional licenses, please email support@calmetrix.com...
Page 10: General Use
Cups must be properly sealed to avoid erroneous measurement data. Only use the Suction Cup that was provided with your I-Cal 8000 to remove Plastic Cups from the unit. Other removal methods may damage the unit or cause sample material to spill.
Page 11: Calibration
D. CALIBRATION Your I-Cal 8000 was calibrated before shipping. You do not need to recalibrate the equipment. The Calmetrix team will email you the calibration file corresponding to your equipment. Once received, place calibration file (“xxxxx-xxx.ccicalcal”) into calibration folder: C:\Users\Public\Documents\Calmetrix\CalCommander\Calibration.
Page 12: Operating Your Equipment - I-Cal Logger
© 2010 - 2012 Calmetrix Inc. – All rights reserved E. OPERATING YOUR EQUIPMENT – I-CAL LOGGER With your computer connected to your I-Cal 8000, open the CalCommander software. You will see the Welcome Screen. Click on the I-Cal Logger tab on top and familiarize yourself with the main window of the I-Cal module:...
Page 13 Mix Configuration area: This part of the screen is used to capture all mix and sample related data. Please note that there are eight individual tabs: one for each sample. Units can be changed from US to metric by clicking on the SETTINGS tab on top of the screen. Box (a) –...
Page 14 Calmetrix I-Cal 8000 User Manual © 2010 - 2012 Calmetrix Inc. – All rights reserved cementitious material. You MUST enter the data for each SCM if included in the sample in order to be able to plot Power per Unit later.
Page 15 Command area. This area is used to operate the I-Cal’s logging functions Select output to plot: Voltage is raw data measured by heat sensors. Power is heat flow normalized per unit of dry cement or cementitious material. Energy is accumulated heat per unit of dry cement or cementitious material.
Page 16 Calmetrix I-Cal 8000 User Manual © 2010 - 2012 Calmetrix Inc. – All rights reserved Note: raw data files are saved in the folder C:\Users\Public\Documents\Calmetrix\CalCommander\Logs once a measurement has been finished and saved. This allows the user to correct mix design data until the measurement has been finished.
Page 17: Sample Preparation And Recommended Test Procedure
F. SAMPLE PREPARATION AND RECOMMENDED TEST PROCEDURE Ensure that the mixing procedure is sufficient to disperse binder properly. If the w/c ratio is pre-defined, perform a pre-test mix with blank cement paste or mortar (no admixtures) and another pre-test with the highest desired dosage of admixtures. Adjust w/c ratio if necessary.
Page 18 Calmetrix I-Cal 8000 User Manual © 2010 - 2012 Calmetrix Inc. – All rights reserved For paste calorimetry, the following procedure is recommended: Weigh up 100 grams of cement in a plastic 800ml beaker and cover. Place a clean empty specimen cup onto the scale and weigh out the required amount of...
Page 19: Visualizing Results - I-Cal Reports
(a1) (a2) (a1) Open Data Folder – this command is a direct link to open the Calmetrix folder on your computer, which contains the default folders where data logs, images, batches and reports are stored. (a2) Load Batch – lets you load a combination of data logs that you previously saved as a Batch (using the Save Batch command).
Page 20 Calmetrix I-Cal 8000 User Manual © 2010 - 2012 Calmetrix Inc. – All rights reserved (a3) - Add Logs – lets you load data logs from completed tests. A new window will appear. Browse to the folder where you stored your completed test file data.
Page 21 (b) - Actual log data is displayed in this area. (c) - Use Graphing tools to Zoom In/Out, click on the legend to change colors or style of graphs. (d) - Click on the min/max values on the x or y-axis to modify the range and scale of the graph. (e) - “Save Selected Log as Text File”...
Page 22 Calmetrix I-Cal 8000 User Manual © 2010 - 2012 Calmetrix Inc. – All rights reserved (g) – Indicate “Time to Iso” for each Sample channel. Time to Iso is the time it takes for the calorimeter to reach isothermal conditions. “Time to Iso” varies with sample type and size and can be estimated by running duplicate samples.
Page 23 Standard Practice C1679 from ASTM and review the examples of interpretation given in the appendix of this standard. Calmetrix does not warrant the fitness for purpose of any equipment, software, training or other commercial and non-commercial products marketed, distributed or recommended by Calmetrix, its principals, employees and other representatives.
Page 24: Determining Activation Energy - I-Cal Ae
Calmetrix I-Cal 8000 User Manual © 2010 - 2012 Calmetrix Inc. – All rights reserved H. DETERMINING ACTIVATION ENERGY – I-CAL AE (Optional Module) What is Activation Energy? The temperature dependency of the hydration rate of portland cement can be described by Arrhenius’ law, with faster hydration the warmer the concrete.
Page 25 In the Setting tab, choose the method you would like to use. Once selected, make sure you press “Apply New Settings” for the change to take effect: Now click on the I-Cal AE tab on top. The following window will appear.
Page 26 Calmetrix I-Cal 8000 User Manual © 2010 - 2012 Calmetrix Inc. – All rights reserved Click add Logs to add test results from tests conducted at three (or more) different temperatures for the same mix. In this example, tests were performed at 50, 73 and 95°F.
Page 27 “Generic” method “S-shape” method At any time, you can switch from “Power” to “Energy” plots by selecting the type of graph from the drop down menu located at the top of the graph.
Page 28 Calmetrix I-Cal 8000 User Manual © 2010 - 2012 Calmetrix Inc. – All rights reserved Examples of use of Arrhenius plots. Figure 1 below shows the effect of temperature on the heat flow rate (power) and the produced energy (approximation for the overall degree of hydration) for a portland cement paste without admixture, w/c 0.45.
Page 29 (a) Heat flow (b) Energy (integrated heat flow) Figure 2: Arrhenius plot based on the results in Figure 3 using Eqv (1). The slope is the apparent activation energy for the overall cement hydration process. Arrhenius law applies only if a change in temperature merely changes the speed of reaction and not the major path of reaction.
Page 30 Calmetrix I-Cal 8000 User Manual © 2010 - 2012 Calmetrix Inc. – All rights reserved (a) Heat flow (b) Arrhenius plot Figure 3: Example of temperature induced cement – admixture incompatibility Cement-admixture incompatibility issues associated with hot weather concrete are often based on sulfate imbalance, since higher temperatures generally make the aluminate reactions faster while the solubility of calcium sulfate is lower compared to lower temperatures.
Page 31 Arrhenius plot assumes that the path of reaction is the same at all temperatures. In other words it is assumed that the reaction taking place in the second peak that was only observed at 40°C is similar to the reaction taking place in the first peak at all three temperatures. More knowledge is needed about the general hydration mechanism before one can assume that the activation energy concept is valid and useable for predicting engineering properties such as strength development before applying it to novel binders such as alkali activated fly ash.
Page 32: Predicting Compressive Strength - I-Cal Strength
Calmetrix I-Cal 8000 User Manual © 2010 - 2012 Calmetrix Inc. – All rights reserved I. PREDICTING COMPRESSIVE STRENGTH DEVELOPMENT – I-CAL STRENGTH (Optional Module) I-Cal Strength is based on the assumption that for a given mix design with a given porosity there is a correlation between the energy released (degree of hydration) and the compressive strength development.
Page 33 the extrapolation. The “Extrapolation Start Time” must be shorter than the time of actual data that was logged. The extrapolation will be displayed as a gray add-on to the original curve. NOTE: Data must be logged long enough to capture most of the heat generation from any given mix to enable reasonable extrapolation of energy and prediction of compressive strength at later ages.
Page 34 Calmetrix I-Cal 8000 User Manual © 2010 - 2012 Calmetrix Inc. – All rights reserved Optional advanced use: The following tools are available to fine tune the extrapolated part of the energy curve in the modeling section: Entering a measured or calculated hydration energy in the “Hydration Energy” field (i), or Entering known energy values (for examples from separate verification tests) at specified hydration times in the “Visual Feedback”...
Page 35 Compressive Strength Data can be entered manually, or can be copy-pasted from a spreadsheet application such as Microsoft Excel by using “Paste CS(t)” (h) The compressive strength data used should be for identical mixtures and cured at the same temperature as in the calorimeter test. For example, if you used a standard mixture and conducted a calorimetry test at 23°C, you would perform compressive strength testing on cubes or cylinders of the same mixture, cured at 23°C.
Page 36 Calmetrix I-Cal 8000 User Manual © 2010 - 2012 Calmetrix Inc. – All rights reserved Just like in the Modeling tab, carefully select the “Maturity Start Time” (C) for each curve you added. The Maturity Start Time is the beginning of the main hydration, when strength is starting to build in your mix.
Page 37 Enter the ages (F) at which you want the predicted compressive strength based on the measured energy Read the predicted compressive strength in the “Estimated Compressive Strength” fields (G) Optional advanced use: For verification and fine-tuning of predicted Compressive Strength values, you can perform physical strength testing as an “adjustment data point”...
Page 38: Predicting Setting Times - I-Cal Set
Calmetrix I-Cal 8000 User Manual © 2010 - 2012 Calmetrix Inc. – All rights reserved J. ESTIMATING SETTING TIMES FROM CALORIMETRY CURVES – I-CAL SET I-Cal Set will help you predict initial and final setting times within close approximation by applying the “Fractions Method”...
Page 39 12. You can later open and edit an existing model by clicking on Load Model (g) Now you’re ready to use the setting time prediction tool Once a model has been established for a given mixture, it can be used to predict early and late times of set of the same mixture by using only a calorimetry curve.
Page 40 Calmetrix I-Cal 8000 User Manual © 2010 - 2012 Calmetrix Inc. – All rights reserved You can remove one or several logs by clicking on Remove Analysis Logs (B). 10. Once you have loaded all curves you would like to analyze, select the calibration field to use for each by clicking on the drop-down menu in (C).
Page 41 12. The upper right hand side graph (F) displays the calculated initial set, final set and the Finishability time window.
Page 42 Calmetrix I-Cal 8000 User Manual © 2010 - 2012 Calmetrix Inc. – All rights reserved Questions? - Find us at: +1 617 203-2090 support@calmetrix.com http://www.calmetrix.com The Calmetrix Team ENJOY YOUR I-CAL 8000 EQUIPMENT v. 102742-1.43...
Page 43 Calmetrix Inc. PO Box 70 Arlington, MA 02476-0001 T: +1 617 203-2090 e: info@calmetrix.com w: http://www.calmetrix.com © 2010 - 2013 Calmetrix Inc. - All rignts reserved...