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User manual I-Cal 2000 1.51

1. Page 25 PREDICTING COMPRESSIVE STRENGTH I CAL STRENGTH Page 33 J ESTIMATING SETTING TIMES I CAL SET 4 Page 39 DETERMINING HEAT OF HYDRATION I CALHOH Page 43 Calmetrix l Cal 2000 HPC User Manual O 2016 Calmetrix Inc All rights reserved A BEFORE YOU START USING THE EQUIPMENT Unpacking and Installing your I Cal 2000 HPC Your 2000 HPC is shipped in one single carton All accessories are included in white boxes placed in the main carton 2 Place the stacks of three reference masses into the reference cells 1 Remove all protective packaging material 3 Place the lids on the reference cells and active sample cells Connecting your I Cal 2000 HPC Your calorimeter includes a computer with pre installed software Use the power cable to connect your I Cal to a suitable electrical plug Your 2000 HPC functions with 110 240V 50 60 Hz electrical supply Connect your Cal 2000 HPC to the computer using the two USB cables included in the Accessories box Open the CalCommander software Congratulations You are now ready to use your l Cal equipment Installing the CalCommander Software on additional computers Minimum requirements Windows XP or later 2 GB RAM and 250MB hard drive space screen resolution of 1024x768 or higher Do not yet connect your I Cal unit to the new computer
2. mans oo SCM2 None F Content kgm sf sow 0 0 2 00 00 273 1 SCM3 Type None Content kg m 3 0 00 Source 2 E 1 Coarse Aggregate gt 4 mm kg m 3 0 00 Source Fine te 4 fs 0 00 Sour Fe j Add Logs Export Logs as Text Files Admix 1 Dose ml m 3 0 00 Total Mass g 50 3 Remove Al Logs Remove Selected Log Admix 2 Name Dose ml m 3 0 00 Mix T degC 32 0 Shift Log Left Shilft Log Right Admix 3 Name Dose mljm 3 0 00 Logging hh mm 48 00 Non Dry SCM Additive kg m 3 0 00 Source Mix Date Time 15 2010 12 36 El Comment w c 0 45 Save Updated Log Save All Updated Logs Log Details Logger 063 664 Cell 3 Tset 23 0 degC 1 2 3 4 nu a 50 6 7 8 For examples and guidance on interpretation of results it is highly recommended to obtain a copy of 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 Calmetrix does not assume any liability as related to the accuracy relevance or interpretation of results while using and CalCommander 24 Calmetrix l Cal 2000 HPC User Manual O 2016 Calmetrix
3. the Set Tenv box in the l Cal Logger tab and press Turn Controller On The controller should be on for at least 24 hours before test runs to reach a stable test temperature Pre dilute admixtures to ensure accurate weighing or use high accuracy micro pipettes for accurate volumetric dosing If the mixing procedure is new to the operator run 5 10 practice mixes to ensure a consistent mixing method throughout a test series Use the same mixing sequences and times as far as possible within a test series Prepare mortar or concrete according to standard For a better signal to noise ratio you can remove the coarse aggregates 4 mm using a sieve Be sure to enter all the different materials used in the software to ensure proper calculation of power and heat The software reports power and heat normalized to total weight of cementitious materials or portland cement making it easy to visualize any effect of admixtures and SCM s on the portland cement reaction Please be careful not to spill any material outside of the 125 ml sample cup For paste calorimetry several methods ca be used including hand mixing and using a benchtop mixer You can visualize a video tutorial on the Calmetrix website in the Support Section The following procedure is commonly used by operators of Calmetrix calorimeters Weigh up 100 grams of cement in a plastic 800 beaker and cover b Place a clean empty specimen cup onto the scale and
4. 23 0 degC 43 a Add or Remove Logs to be analyzed You can load up to eight logs b Choose a calibration to be applied to a calorimetric curve you load Any available calibration files for this calorimeter will automatically be displayed in a list This can be used when you would like to apply a calibration file that is different from the one you used while conducting the test like for example if you conducted a heat of hydration test and re calibrated the equipment right after your test You can save a copy of the logs with the new calibration file by clicking on Create Copies of Logs with new Calibration in b1 Choose at what curing age you would like to see the heat of hydration HoH value for each of the Samples 1 8 below d Choose the Time to Iso i e the time after the initial aluminate peak and any thermal disturbances which do not contribute to strength developing hydration energy The software will only account for energy released after Time to Iso was reached e Heat of Hydration J g The heat of hydration values are displayed in these fields f Mix data the mix data entered during logging Section E I Cal Logger is displayed in this area You can modify these fields and click on h Save Updated HoH Logs to save the modified data g Create PDF and Print report Use this section to create or print a standard report of your analysis If using the AS
5. ID 25degC Chi 2010 08 09 18 59 33 ccicallog 2 VSR08 386 MixID 25degC Chi 2010 10 03 11 08 13 ccicallog 2 V amp ROR 326 Miv IM 254 Ch 2010 10 02 16 28 14 cricallan Sample 1 Date modified 10 3 2010 8 32 PM 10 3 2010 6 06 PM 10 3 2010 8 32 PM 10 3 2010 6 06 PM 10 3 2010 8 32 PM 10 3 2010 6 06 PM 10 3 2010 8 32 PM 10 3 2010 6 06 PM 10 3 2010 8 32 PM 10 3 2010 6 06 PM 10 3 2010 8 32 PM 8 9 2010 7 00 PM 10 3 2010 4 21 PM 10 3 2010 4 28 DM T hh mm Settings Log Data Voltage V Sample 1 Sample 2 Sample 3 Sample 4 Sample 5 Sample 6 Sample 7 Sample 8 CCICALLOG File CCICALLOG File CCICALLOG File CCICALLOG File CCICALLOG File CCICALLOG File CCICALLOG File CCICALLOG File CCICALLOG File CCICALLOG File CCICALLOG File CCICALLOG File CCICALLOG File CCIC ALI OR File File name Files of type Cal AdiaCal TC IsoCal File ccicallog icallog txt Browse to the folder where you stored your completed test file data Select the logs you would like to import For multiple selections press the lt CTRL gt key while selecting Repeat the steps above to add more files form other log files You can add up to 8 files on any Report Generator graph Click OK and the files you selected will appear in the Report Generator window 21 22 hh mm 00 00 00 01 00 02 00 03 9 52 5 9 42E 5 9
6. gt Power per Unit Cemmat Wig In Tau n 3 1 c JI gt 5 4 I 1 I I I 1 3 6E 3 3 6E 3 3 7E 3 3 7E 3 3 8E 3 3 8E 3 3 9 3 0 1 I I I 00 00 03 00 06 00 09 00 12 00 15 00 16 00 21 00 24 00 27 00 1 T 1000 K Time since Start hh mm a Heat flovv b Arrhenius plot 31 32 References 1 Schindler and Folliard K J Heat of hydration models for cementitious materials ACI Mat Journal V 102 No 1 pp 24 33 2005 2 Schindler A K Effect of temperature on hydration of cementitious materials ACI Mat Journal V 101 No 1 pp 72 81 2004 3 Riding K A Poole J L Juenger M C G Schindler A K and Folliard K J Calorimetry Performed On Site Methods and Uses ACI SP 241 4 Poole J L Hydration Study of Cementitious Materials Using Semi Adiabatic Calorimetry PhD Dissertation The University of Texas at Austin Austin TX 2007 Calmetrix l Cal 2000 HPC User Manual O 2016 Calmetrix Inc All rights reserved PREDICTING COMPRESSIVE STRENGTH DEVELOPMENT I CAL STRENGTH Optional Module Strength is based on the assumption that for a given mix design with a given porosity there 1 a correlation between the energy released degree of hydration and the compressive strength development As with traditional maturity the assumption is only valid for mixes with the same materials and pr
7. 2016 Calmetrix Inc All rights reserved SAMPLE AND RECOMMENDED TEST PROCEDURE 1 Ensure that the mixing procedure is sufficient to disperse binder properly 2 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 If the water demand of the cement admixture combination to be tested is unknown perform test to determine required water to binder ratio binder comprises of cement and any pozzolan used as cement replacement How to accommodate different sample sizes of mortar concrete or paste 2000 HPC 1 equipped with variable reference cells to accommodate different sample sizes and types in the sample cells You can use either one two or three of the supplied metal references or use any custom made reference such as a sample of inert sand In general the thermal mass of the reference should be similar to that of the sample The table below serves as a guide for using the supplied metal references Sample type Reference 20 100 g cement paste 1 metal cylinder 100 200 g cement paste or mortar 2 metal cylinders 250 g cement paste mortar or concrete 3 metal cylinders Metal references Reference Cell 17 Recommended preparation of cement paste mortar or concrete samples 4 18 Dial in desired test temperature
8. 30 5 9 25 5 9 7 5 9 SES 94255 9 33 5 8 03 5 7 97 5 7 87 5 7 85 5 8 85 8465 8065 8 28 5 1174 11 4 1134 1124 A e im 15 2010 12 35 b Actual log data is displayed 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 saves the information including all temperature values from the currently selected Sample tab in a txt file Data from txt files can easily be copied and pasted in an application such as Microsoft Excel for spreadsheet calculations on plotted data Note that data displayed in the Mix data section i can be edited for PDF reports create PDF Reports Prints Print Report or when saving data as a text file f Press Shift Log left right to change the order in which Samples are ranked and displayed e g to make Sample 2 take the position of Sample 1 select the Sample 2 tab and press Shift Left Calmetrix l Cal 2000 HPC User Manual O 2016 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 lso varies with sample type and size and can be estimated by running duplicate samples When plotting Energy and Power Tim
9. Coarse Aggregate gt kgm 3 000000 Fine Aggregate lt 4 mm 3 0 00 Source Admix 1 Name Dose ml m 3 0 00 Total Mass 9 50 3 Admix 2 Name Dose ml m 3 0 00 Mix T degc 32 0 Admix 3 Name Dose ml m 3 0 00 Logging hh mm 48 00 Save Batch Open Data Folder Load Batch Non Dry SCM Additive kg m 3 0 00 Source Mix Date Time May 15 2010 12 36 El Comment w c 0 45 Save Updated Log Save All Updated Logs Log Details Logger AT063 664 3 Tset 23 0 degC Create PDF PrintReport Save as Image k Switch between Voltages Power or Energy data by clicking on the box on top of the graph as shown in the example below Energy plot 23 Voltage V X m gt m Power W EN tome F Cal Logger Power W g Cement F Cal Reports I Cal Reports Settings Power W g Mat J 4 Energy J A m Log Data Energy J 3 0k Energy J g Cement 00 00 00 01 00 02 Energy J g Cem Mat Sample 1 1 98E 1 4 35 1 6 71E 1 9 07 1 2 5k Sample 2 1 52 1 3 33 1 5 14E 1 6 93 1 Sample 3 1 59 1 3 49E 1 5 39 1 7 28E 1 Sample 4 1 60 1 3 52 1 5 42 1 7 33E 1 2 21 1 4 85 1 7 48 1 Sample 4 Sample 5 Report Title Time to ISO hh mm Tset degC Conf Changed Samper Smoe2 Samples sampe4 IN
10. 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 See equation 1 where IR J 7 pem 7 4 i aut e 1 is the rate constant for the reaction Z is a proportionality constant that varies from one reaction to another Ea 1 the activation energy for the reaction which in case of most cementitious systems 1 the so called apparent activation energy since several complex chemical reactions may take place during the hardening process 1 the ideal gas constant in joules per mole Kelvin and T 1 the temperature in Kelvin According to this equation a plot of In k versus 1 T should give a straight line with a slope of Ea R The calculation of the apparent activation energy is based on the assumption that the overall reaction proceeds along the same path at different temperatures according to the Arrhenius law It is assumed that the activation energy is only dependent on the produced energy the degree of hydration and therefore the activation energy can be evaluated at different degrees oh hydration from the slope of the logarithm of the thermal power vs the inverse of the absolute temperature How to use the I Cal AE module To utilize the Activation Energy module you will need
11. Install your software first 1 Insert the Calmetrix USB Flash Drive in your computer s USB port and browse to the Software Installation folder Double click on the CalCommSetup icon and follow the on screen installation instructions Refer to detailed instructions on the Quick Set Up sheet enclosed in the Accessories box Do not restart the computer during installation even if prompted to do so 2 the installation is finished connect your 2000 HPC and wait for 30 seconds for the operating system to recognize the equipment Then open CalCommander 3 Click on the Settings tab 4 Email your ID number to registration calmetrix com or call 1 617 203 2090 to obtain your Registration number Once received key in the number in the Reg ID field NOTE in addition to the pre installed software on the computer that came wit your 2000 HPC your 2000 HPC includes one free software license for the I Cal Logger logging interface one license for the l Cal Reports report generator and one license for the l Cal HoH heat of hydration software The computer you register for the use of your will be the only computer registered To purchase additional licenses please email support calmetrix com or call 617 203 2090 5 Once you received your 7 digit registration numbers for Logger I Cal Reports I Cal HoH any additional modules you purchased enter them in the Settings tab 6 Once the registra
12. a calorimetry test at 23 C you would perform compressive strength testing on cubes or cylinders of the same mixture cured at 23 For best results a minimum of 5 to 6 compressive strength data points at various ages should be entered In our example we used 6 data points The left hand graph window m displays the relationship between Energy and time left axis and Compressive Strength over time right axis The right hand graph window n displays the relationship between Energy and Compressive Strength A Power function is used as a default fit but other models can be chosen from the CS E fit Type drop down menu Equations corresponding to the curves that are displayed are shown in boxes o and p Once finished you can Save your Model for this mixture by clicking on Save Model q You can later use Load Model to retrieve and edit any previously saved model Now you re ready to use the prediction tool Once a model has been established for a given mixture it can be used to predict compressive strength of the same mixture by using only a calorimetry curve This means that whenever you work with the same mixture again in the future you only need to perform a calorimetry test to infer compressive strength Hence you can significantly cut back on physical compressive strength testing and you do not have to wait until you reach a given curing age to get an estimate of compressive strength gain To use the pred
13. anl BR daa cree ERR HH Lo int i TEM cem ed E de eee 9 You 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 11 The software will calculate and display the Thermal Indicators of Set D 41 42 PASS LU 309 40 Cemex Tmix 32 0 deg 313 40 Cemex TIPA 0 4 Tmix 32 0 dec 12 The upper right hand side graph displays the calculated initial set final set the Finishability time window Calmetrix I Cal 2000 HPC User Manual O 2016 Calmetrix Inc All rights reserved H DETERMINING HEAT OF HYDRATION I CALHoH l Cal HoH helps you determine the total heat of hydration usually expressed in J g of your cement cementitious binder system when you follow the protocol outlined in ASTM 1702 NOTE as mentioned in Section E Logger only curves generated the HoH Logging mode can be opened and analyzed in Cal HoH Calmetrix CalCommander v 1 68 4 Energy J g 6 8 S 8 File name AQ517 750 creation date 01 Jan 2000 Logger AQ517 750 1 Tset
14. calibrated before shipping You do not need to recalibrate the equipment The calibration file is already placed in the computer that was shipped with your equipment The calibration file is placed C Users Public Documents Calmetrix CalCommander Calibration and can be copied to another computer you use to operate your equipment Always make sure that the Yellow Calibration light is lit on the upper right hand side of the l Cal Logger screen when operating your equipment as shown in Part E Operating your Equipment I Cal Logger below Please email us at support calmetrix com or call 1 617 203 2090 for any help with calibration and calibration files E OPERATING YOUR EQUIPMENT I CAL LOGGER Important Operating instructions e Your computer has to be connected to the equipment at all times while running a test Do not plug and unplug your Cal while CalCommander is running as this will cause the program to fail e While running test the CalCommander software is continuously communication with the equipment It is recommended to disable all energy saving features of the computer to avoid possible interruption in the communication With your computer connected to your 2000 HPC open the CalCommander software Click on the l Cal Logger tab on top and familiarize yourself with the main window of the I Cal Logger module Plot area Command area Mix Information area 10 Calmetrix l Cal 2000 HPC User
15. reports With CalCommander open on your computer click on the l Cal Reports Tab on top A new window appears as in the picture below I Cal Logger I Cal Reports Voltage V Log Data Voltage Sample i Report Title Time to ISO hh mm Tset degC Conf Changed 1 00 00 273 1 00 00 273 1 00 00 273 1 2 Mix ID Total Water Content kg m 3 0 00 3 Cement Source 1D Cement Content kg m 3 0 00 3 SCM 1 Type None Cotentkgm 3 0 00 2 6 7 8 00 00 273 1 00 00 2731 00 0 2731 2731 2751 SCM2 Content ko m 3 0 00 Source SCM3 None Content kg m 3 0 00 Source Coarse Aggregate gt 4 mm kg m 3 0 00 Source Fine te 4 0 00 Sour Mae ccm ii Add Logs a3 Export Logs as Text Files Admix 1 Name Dose ml m 3 0 00 Total Mass 9 0 0 Remove All Logs Remove Selected Log Admix 2 Name Dose mi m 3 0 00 MixT degC 0 0 Shift Log Left Log Right Admix 3 Name Dose ml m 3 0 00 Logging hh mm 00 00 Save Batch Open Data Folder Load Batch Non Dry SCM Additive kg m 3 0 00 Source Mix Date Time 12101 2000 01 00 Comment Save Updated Log Save All Updated Logs Create PDF Print Report Save as Image a1 Open Data Folder this command is a direct link to open the Calmetrix folder on your computer which contai
16. to run tests at at least three different temperatures for any given mix CalCommander uses two different methods to determine activation energy the S shaped method developed by Anton Schindler and the Generic method developed by Lars Wadso While there 1 no strict guideline as to which method is best in general terms we recommend use of the S shaped method for mixes where Portland cement is the predominant cementitious material and the Generic method for very high substitution levels or geopolymer type mixes 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 25 Now click on the Cal AE tab on top The following window will appear e 8 8 8 Click add Logs to add test results from tests conducted at three or more different temperatures for the same mix 26 Calmetrix l Cal 2000 HPC User Manual O 2016 Calmetrix Inc All rights reserved I Cal AE Settings Arrhenius Plot Data Points 3 0 Best Lin Fit In this example tests were performed at 50 73 and 95 F y Power per Unit Cemmat W g d Make sure you key in Time FF D Deer nant to Iso i e the time at which Tre oh the system reached isothermal conditions after 00 00 00 00 00 0 00 00 the sample was inserted into the ca
17. weigh out the required amount of admixture C Add water and diluted admixture for mix water addition to bring the total weight to 45 grams for a W C of ratio of 0 45 Immediately start the logger for this cell Calmetrix l Cal 2000 HPC User Manual O 2016 Calmetrix Inc All rights reserved Use a commercial laboratory mixer at a speed of 400 rpm for 4 minutes after the addition of the water Delayed addition admixtures are added at the 60 second mark and mixed for the remaining 3 minutes Tail End addition admixtures are added at the 15 second mark and mixed for the remaining 3 minutes and 45 seconds Note that mix water must be adjusted for any water in the admixture as the water to cement ratio is kept constant unless otherwise requested Place an empty clean 125 ml plastic cup on the scale and tare Carefully weigh out approximately the paste amount required to reach 25 grams of paste You must be careful not to get any paste outside of the 125 ml sample cup Record the total mass of the sample and update in the Mix Configuration part on the I Cal tab in CalCommander Quickly place the plastic lid on the sample cup and make sure cup is perfectly clean and sealed Target the same time between start of mixing i e when cement and water get in contact and loading into the calorimeter for all mixes in a test series 19 VISUALIZING RESULTS I CAL REPORT GENERATOR Using 1 Reports to plot and interpret data or create
18. Manual O 2016 Calmetrix Inc All rights reserved Command area This area is used to operate the 5 logging functions Select output to plot Voltage 1 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 Detects if a Calibration file is present A Green indicator means that the Calibration file is present and loaded If the indicator is Red locate and install the Calibration file as in Section D of this Manual Voltage real time measurement by sensor Status yellow with time if logging is active gray if logging is inactive Last logged displays last value logged by sensor Choose between two ways to log data a select HoH Logging if you would like to determine the absolute heat of hydration value for example according to ASTM C1702 In HoH Logging mode you can choose a logging interval for an Initial Phase and a another usually longer interval after the Initial Phase of hydration Refer to ASTM C1702 for guidance on logging intervals b select Generic Logging for all other experiments Control the temperature in your calorimeter Set T env enter desired test temperature between 5 C and 45 C and press Turn Controller ON Remember to set the desired temperature and let the equipment stabilize to isothermal conditions for at least 24 hours before testing begins Actual T env actual
19. TM C1702 Method B option the report will automatically contain all the information as required by the standard h Export Logs as Text Files Use this function to create a text file of all data points which can easily be copied and pasted into a spreadsheet calculator software such as Microsoft Excel 44 Calmetrix l Cal 2000 HPC User Manual O 2016 Calmetrix Inc All rights reserved Questions Find us at 1 617 203 2090 support calmetrix com http www calmetrix com calmetrix The Calmetrix Team ENJOY YOUR I CAL 2000 HPC v 102626 1 68 45 calmetrix Calmetrix Inc PO Box 70 Arlington MA 02476 0001 USA T 1 617 203 2090 info calmetrix com vv http www calmetrix com O 2010 2013 Calmetrix Inc All rignts reserved
20. calmetrix 2000 HPC USER MANUAL Calmetrix I Cal 2000 HPC User Manual CALMETRIX INC I CAL 2000 HPC ISOTHERMAL CALORIMETER FOR CONCRETE AND CEMENT USER MANUAL Calmetrix l Cal 2000 HPC User Manual O 2016 Calmetrix Inc All rights reserved IMPORTANT SAFETY RULES e Exercise caution when lifting the calorimeter to avoid back or other injuries Consider a two person lift or mechanical aid e Never operate the calorimeter or temperature control unit in a wet environment DISCLAIMER Calmetrix does not assume any liability as related to the accuracy relevance or interpretation of results while using or the CalCommander software COPYRIGHT This User Manual is subject to copyright and may not be reproduced in whole or part without permission Calmetrix l Cal 2000 HPC User Manual O 2016 Calmetrix Inc All rights reserved TABLE OF CONTENTS A BEFORE YOU START USING THE EQUIPMENT Page 7 GENERAL USE ec Page 8 C HANDLING INSTRUCTIONS mestra sms tas bog tet e tt En alls 9 CALIBRATION TL a n r Page 9 E OPERATING YOUR EQUIPMENT I CAL LOGGER Page 10 F SAMPLE PREPARATION AND RECOMMENDED TEST PROCEDURE Page 17 VISUALIZING RESULTS I CAL REPORTS 2 2 Page 20 H DETERMINING ACTIVATION ENERGY
21. e to lso 1 used as a point of origin i e all values before Time to Iso are ignored in Energy and Power calculations See ASTM C1679 for more details Use Save Batch to save the current configuration of data logs so they can be called up as on batch using Load Batch in the future j Data in area j can be edited If data is edited a yellow light will light up for the corresponding Sample number in the Conf Changed field on the right as shown in the picture below The light will switch off after you saved your changes by pressing Save Updated Log or Save All Updated Logs Please note that changes cannot be undone once saved 1 cal Logger F Cal Reports I Cal Reports Voltage V El Log Data Voltage Sample 1 00 00 00 01 00 02 9 52 5 9 42 5 9 30 5 9 72 5 9 55 5 9 42 5 3 8 03E 5 7 97E 5 7 87 5 4 8 48E 5 8 40E 5 8 30E 5 1 17 4 1 15E 4 1 13E 4 Sample 2 Sample 5 E Report Title A UR mer Time to ISO hh mm Tset degC Conf Changed Indicates a change re has been made in MxID Calbratonmx 23C 7 TotalWaterContentkg m 3 0 00 the configuration SCM 1 OO Noe Content ko m s 0 00 data area j for SCM2 Type None Content homes NE SCM3 Type _ we El Content kajm 3 20 A sample 4
22. eak For example if the main hydration peak was reached after 24 hours we recommend that the Extrapolation Start Time be set at 48 hours or later Calmetrix I Cal 2000 HPC User Manual O 2016 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 o Entering a measured or calculated hydration energy in the Hydration Energy field i or o Entering known energy values for examples from separate verification tests at specified hydration times in the Visual Feedback boxes j With a number entered in the Hydration Energy box i the user can then use the up down arrows or simply type different numbers in the box to adjust the extrapolated energy curve up or down for a better long term fit with the data entered in visual feedback 6 Enter measured compressive strength data in fields f Time since Mix and Measured Compressive Strength 1 Logger QMR 78 453 Cell 8 Tset 20 0 degC CS 7 28E 4 E 1 93E 0 H0 00E 0 2 0 9956 35 36 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
23. ed Hu Alpha Beta and Tau values are inputs for Texas ConcreteWorks a free software application for maturity calculations including crack prediction The Activation Energy is shown in the field ConcreteWorks was developed by the University of Texas Durability Center and funded by the Texas Department of Transportation It can be downloaded at http www texasconcreteworks com In the Generic method Activation Energy is calculated at five different points along the test curves Values for these calculations are shown in the E act fields The average of these values should be used and is shown in the E aver field 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 481 145 0 67 3000 1 0000 28 Calmetrix l Cal 2000 HPC User Manual O 2016 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 Note that the initial non isothermal heat flow is excluded from the energy calculation Figure 1 b The measured data was then fitted mathematically to an S shaped hydration development curve that is known to work well for portland cem
24. elopment However a major change in the reaction path 29 going from one temperature to another would invalidate this concept Cement admixture incompatibility issues are sometimes induced by a temperature change such that the major path of cement reaction has changed and therefore could be undetected by standard laboratory room temperature tests Figure 8 shows an example where an industrial concrete with 20 fly ash and 0 3 low range water reducer by weight of cement hydrated normally at 10 and 23 C The slower hydration rate at 10 C is expected however note the complete different path at 40 C as evident by both the timing and abnormal shape of the main exotherm and the abnormal Arrhenius plot Arrhenius Plot o 4 Data Points 2 9 ime Reo BestLinFit Power per Unit Cemmat Wig 3 1 In Tau 3 9 4 40 6 47 I I I I 3 6E 3 3 7E 3 3 7 3 3 8E 3 3 3 3 3 9 3 1 T 1000 a Heat flow b Arrhenius plot ALIE I I I 00 00 05 00 10 00 15 00 20 00 25 00 30 00 35 00 40 00 Time since Start hh mm 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 The response red curve in Figu
25. ent based mixtures according to Schindler Ref 1 amp 2 below Figure 2 shows the corresponding Arrhenius plot as a fitted straight line representing the apparent activation energy Figure 1 Effect of curing temperature on rate of reaction heat flow and degree of hydration energy integrated heat flow Hydration Progress Hydration Progress Isothermal heat flow power rate of reaction Energy integrated heat flow degree of B0 C hydration 5 1 1 1 1 I 1 1 1 I 1 1 1 1 E RO dis cnt dde Aldo all 0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 36 38 40 42 44 46 48 50 52 54 56 58 60 62 64 66 68 70 0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 36 38 40 42 44 46 48 50 52 54 56 58 60 62 64 66 68 70 Hydration Time hrs Hydration Time hrs a Heat flow b Energy integrated heat flow Arrhenius Plot Data Points 2 0 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 In 0 m e 1 Arrhenius law applies only if a change in temperature merely changes the speed of reaction and not the major path of reaction This is usually the case for straight portland cement mixtures which in turn makes the 3 0 3 ee m 383 foundation for the use of Maturity models for predicting degree of hydration and strength dev
26. grams of each material you used when preparing your sample on a benchtop mixer as long as you use the same units for all these fields The total mass in box a has to be expressed in grams as it is used to compute and display Power and Energy per unit weight of material 13 14 Mix Information Area Logging mode h Box a Water Content Enter the total water content contained in your sample b Cement or Content Enter the total mass of cement if logging an active sample or of inert material if logging a reference sample to determine the correction factor as ASTM 1702 SCM content Enter the total mass of Supplementary Cementitious Material contained in your sample e Total Mass Water Binder Ratio are calculated values f Mix Date Time Make sure to enter the mix time when water gets in contact with the cement g Indicate the Mixing Method if applying ASTM C1702 h Logging time A typical heat of hydration test should last 168 hours or more Please enter a value that allows for at least 168 hours of logging from Mix time Calmetrix l Cal 2000 HPC User Manual O 2016 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 m
27. hanged in the Settings tab Box b Logging hh mm enter the desired total length of the experiment Mix Date Time enter the mixing time when the water gets in contact with the cement Make sure you fill in this part properly as the mix time 1 used in all other software tabs to display and analyze data properly d Content SCM 1 2 83 Enter SCM unit mass as per mix design This mass is regarded as a filler inert material if plotting Power per unit of dry cement and considered active if plotting Power per unit of dry 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 Box e Content Coarse and Fine Aggregate Enter coarse and fine aggregate mass per mix design if testing mortar or concrete Do not enter coarse aggregates if these have been removed from mix prior to sampling As with SCMs you MUST enter data for coarse and fine aggregate if included in sample Box f Total Water Content and Total Cement Content Enter data as per your mix design cement content and total water to reach the design water cement ratio Box g Admixture data These fields are for informational purposes only The values are not used in any calculations Add any aqueous part of admixtures to the Total Water Content f Note that for boxes a d and f you can use the proposed units or any other unit e g
28. iction tool proceed as follows Click on the Data Analysis tab Select the mix specific model to use by clicking on the down arrow of the Model field A then click on Add Analysis Logs B to select the calorimetry data for which you would like to predict the strength development You can add up to 8 calorimetry curves Strength will use the average of al curves to infer compressive strength values Calmetrix I Cal 2000 HPC User Manual O 2016 Calmetrix Inc All rights reserved DataPoints Best it 47 06 00 00 00 1 00 00 00 00 00 00 1 00 00 1 00 00 00 00 67200 2202 Jasso 1 69241 ase 47 1 5 081 0 3 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 This should be the Initial Set Time of the mix if known and in any case at least 30 minutes longer than the Time to lso which can be determined l Cal Reports using the guidelines on page 21 of this manual 4 As in the Modeling tab use extrapolation D to help you predict values beyond the total duration of the calorimetry test Optional advanced use 37 38 You can specify the Hydration Energy E if you know it from a calculated or measured value for this mixture Enter the ages F at which you want the predicted compressive strength based on the meas
29. ix design data until the measurement has been finished You can also copy finished data sets to your designated network drive Be sure to create a sub folder for each individual project to facilitate good record keeping Plot area f w 4 W w w Right click the x or y axis to change scaling from Automatic to Manual Manual mode you can adjust the min and max by double clicking on a number on the axis and typing in desired values b Click on a graph legend color on the right of the screen to change the appearance color line type etc c Click on the Zoom and Motion tools on top f to zoom in out or move the graph 15 Units and Channel Color Coding Units metric or standard US and colors assigned to the curves corresponding to each test channel can be modified in the SETTINGS tab Click on a color to change it Make sure to press Apply New Settings to save any changes Change units from Metric to US Click on a default color to change and select a new color in the pop up window C Users Public Documents Calmetrix CalCommander Logs 4574350 9469881 Select or deselect the Software application tabs you would like to show in the tab list on the top of the window lt Ial AE Ial Set CalHoH SSSSe8s8 Click on a Apply New Settings to validate your changes 16 Calmetrix l Cal 2000 HPC User Manual O
30. lorimeter 1 1 1 1 00 00 08 00 16 00 24 00 32 00 40 00 48 00 56 00 64 00 72 00 80 Time since Start hh mm ame samez sales Mix ID 50 Slag Hot b Total Water Content Ib yd 3 273 00 Cement Source ID Cement Content b yd 3 310 00 SCM 1 Type Slag Content 3 310 00 Source SCM 2 Type None kd Content lb yd 3 0 00 Source SCM3 Content 4 3 0 00 Source Coarse Aggregate gt 4 b yd 3 2032 00 Source 57 Limestone Fine Aggregate lt 4 mm b yd 3 1173 00 Source Natural Sand 00 00 Tau hrs oo 00 foo 00 foo 10 0 100 Individual R Factors 0 0000 0 0000 0 0000 0 0000 0 0000 A 0 0000 0 0000 0 0000 Hu J g Beta AE J mol Factor Admix 1 Name WRDA 64 Dose oz hlb 4 00 Total Mass g 189 7 O Click Analyze Admix 2 Name Dose 0 00 Mix T degF 95 0 Admix 3 Name Dose ozfhib 0 00 Logging hh mm 00 00 Non Dry SCM Additive 0 00 Source Mix Date Time DD vvv 00 00 Bj comet 000000000 Log Details Logger Cell 6 Tset 95 0 degF Add Logs Shift Log Left Shilft Loa Bi Remove All Logs 2 o Log Analyze Save Result The values of Activation Energy might differ depending on the method used S Curve or Generic In the S Curve method several values indicative of the shape of the curve are display
31. ns 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 This lets you load sets of curves from previous work with Cal Reports saved as batches without having to import individual logs one by one 20 Calmetrix I Cal 2000 HPC User Manual a3 Add Logs lets you load data logs from completed tests A new window will appear I Cal Logger Voltage V y 2016 Calmetrix Inc All rights reserved I Cal Reports Look P eh Recent Places Desktop Libraries Jj Logs Name gt VSR08 386 No MixID 23degC Ch3 2010 10 03 20 21 47 ccicallog 21 VSRO8 386 No Mix ID 23degC Ch4 2010 10 03 16 46 47 ccicallog VSR08 386 No ID 23degC Ch4 2010 10 03 20 21 47 ccicallog gt VSR08 386 No ID 23degC Ch5 2010 10 03 16 46 47 ccicallog gt VSR08 386 No MixID 23degC Ch5 2010 10 03 20 21 47 ccicallog VSR08 386 No ID 23degC Ch6 2010 10 03 16 46 47 ccicallog VSRO8 386 No Mix ID 23degC Ch6 2010 10 03 20 21 47 ccicallog VSR08 386 No ID 23degC Ch7 2010 10 03 16 46 47 ccicallog gt VSR08 386 No ID 23degC Ch7 2010 10 03 20 21 47 ccicallog gt VSR08 386 No MixID 23degC Ch8 2010 10 03 16 46 47 ccicallog VSR08 386 No ID 23degC Ch8 2010 10 03 20 21 47 ccicallog 7 VSR08 386 No
32. oportions How to use the Strength module To be able to predict compressive strength development for a given mix design you will first have to create a model which establishes the relationship between degree of hydration and compressive strength IMPORTANT NOTE Any given model is only valid for prediction of other mixes WITH THE SAME MIX DESIGN tested at the same temperature Hence Strength works well for standard mixes or high volume mixes used often in next to similar conditions Experience has also demonstrated that the model works for predictions of mortar mixes with minor deviations such as using a slightly different admixture type or dose However the mixing method as well as binder water air and sand type and content cannot be changed without having to re develop the model The use of defoamer 1 also recommended to minimize variable air entrainment whenever possible Hence First build a model To build a new Model for a given mixture proceed as follows Go to Strength and select the Modeling tab Click on New Model a 2 Click on Add Modeling Log b A new window will pop up letting you browse to the file containing the calorimetry curve for the mix for which you would like to build a model You can load up to 8 curves for the same mix 3 Select one or several curves for this mix As shown in the example below the software will plot Energy Cementitious Material for the cur
33. re 3 is somewhat typical As the concrete was mixed at room temperatures before curing at three different temperatures inside three separate isothermal calorimeter units the initial positive or negative power readings represent non isothermal conditions and are not included in the calculation of activation energy along with the initial heat of dissolution Note however the higher activity of the 40 C sample after having reached isothermal conditions after some 60 minutes The accelerating effect of temperature on aluminate hydration coupled with a negative effect on gypsum solubility likely caused the mixture at 40 C to temporarily run out of soluble calcium sulfate at early age causing a poisoning effect on the strength giving alite hydration that is often observed as a result of poorly controlled aluminate hydration The alumina activity then reached a stage of lower activity which was low enough to allow for enough gypsum to dissolve to reach sulfate balance and allow for some alite hydration until the mix most likely ran out of gypsum after about 18 hours as indicated by 30 Calmetrix l Cal 2000 HPC User Manual O 2016 Calmetrix Inc All rights reserved the very steep exotherm The steep slope and amount of heat released by this exotherm 1 typical of un controlled alumina hydration which in turn effectively poisoned any further alite hydration during the test The sample cured at 40 was soft without any appreciable mechanical strength a
34. t the end of the test which is also typical for the type of response seen by calorimetry at 40 C red curve Not all cases of non compliance with Arrhenius law are as clear cut as the example shown in Figure 3 Figure 4 shows an example of alkali activated fly ash concrete where the power plots have somewhat different shape at 40 relative to 23 and 10 C The different shape seen by calorimetry at 40 may indicate a partially different reaction path or possibly an added reaction at high temperature while the Arrhenius plot assumes that the path of reaction is the same at all temperatures In other words it 1 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 1 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 Nevertheless calorimetry is a very useful tool for characterizing the reactivity of both conventional and non conventional binder systems to identify areas of potential concern for the practitioner as well as where more work is needed for the researcher Arrhenius Plot BEN Data Points hp 3 2 Best Lin Fit 3 4 3 6 3 8 4 0 ES 4 2 4 4 4 8 5 0 5 2
35. temperature inside the calorimeter Copy Paste functions for data contained in the Mix Configuration area These commands facilitate copying a mix configuration from one channel to another Configuration Templates are for frequently used mixes Press Update Configuration to save any changes to configuration data Start logging each channel as close as possible to the time when water enters in contact with the cement Stop logging the selected channel you can stop an experiment at any time up to the logging time defined in b 11 12 IMPORTANT NOTES Data files for curves generated in the HoH Logging and the Generic Logging modes are structured differently 1 Only curves generated HoH Logging mode be opened and analyzed in the HoH Software tab Make sure you are logging in HoH Logging mode if you plan on using l Cal HoH 2 Conversely curves generated in HOH Logging mode cannot be opened in the reports software tab Make sure you are logging in the Generic Logging mode if you plan on using l Cal reports Mix Information area Generic Logging mode Calmetrix l Cal 2000 HPC User Manual O 2016 Calmetrix Inc All rights reserved Box a Total Mass enter the total mass of specimen as sampled Target 20 50 for cement paste 100 0 for mortar and full cup for concrete This information is used to normalize readings across samples Please note that units US or metric system can be c
36. this mix by checking or un checking the Valid box d The average fraction values of all Valid mixes will display in the Initial Set Fraction and Final Set Fraction fields to the right e 11 Save your model by clicking on Save f You will be asked to provide a name for your model Once saved your model will be stored in the Calibration folder and can later be selected when predicting setting times for the same mix design using the Data Analysis tab 39 12 You can later open and edit an existing model by clicking on Load Model 9 Now you re ready to use the setting time prediction tool 40 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 To use the prediction tool proceed as follows 7 Click on the Data Analysis tab 8 Click on Add Analysis Logs A to select the calorimetry data for which you would like to make setting time prediction and click OK You can add up to 8 calorimetry curves Calmetrix I Cal 2000 HPC User Manual O 2016 Calmetrix Inc All rights reserved aa mu PH EAE LAM T PC ney dedi ae EI ECA Hc ef LL H NEE EEE DEL LL der _ Rund di du TH n EN CERE LO
37. tion numbers have been keyed the corresponding boxes should be checked You are now ready to use your Cal 2000 HPC on the new computer B GENERAL USE Calmetrix calorimeters measure the heat flow from concrete mortar or cement paste samples over time in a close to constant temperature environment The heat flow curve provides a fingerprint of the chemical reactions in the sample We recommend that you review ASTM C1679 general practice before using your calorimeter 8 Calmetrix I Cal 2000 HPC User Manual O 2016 Calmetrix Inc All rights reserved C HANDLING INSTRUCTIONS The reusable plastic sample cups must be clean on the outside before inserting them into the calorimeter Cement or admixtures on the outside will cause vials to get stuck in the calorimeter with expensive and time consuming repair as a result Cups must be properly sealed to avoid erroneous measurement data Only use the Suction Cup that was provided with your l Cal calorimeter to remove Plastic Cups from the unit Other removal methods may damage the unit or cause sample material to spill When opening the lid while performing a test immediately close the lid when finished to minimize heat exchange caused by keeping the lid open Use gloves and paper towels to ensure NO admixtures cement dust fingerprints or other material get left on the outside of sample cups when loading them into the calorimeter D CALIBRATION Your calorimeter was
38. ured 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 on a sample at any curing age and enter the corresponding result in the Correction Age and Correction Strength fields I Cal Strength will adjust all predicted compressive strength values proportionally In the example below physical strength testing was done at 36 hours This data point is plotted as a square on the graph and the overall CS t curve adjusted accordingly Adjustment 2 Jr data CS Estimated p CS Model Fit 7 1 Logger QMR78 453 Cell 3 Tset 20 0 degC 00 00 12 00 24 00 36 00 ff 48 00 4 72 00 168 00 00 00 0 00 00 4 00 00 1d 00 00 4 00 00 E 369 9 exp 92186 t 1 06 R2 1 0000 Calmetrix l Cal 2000 HPC User Manual O 2016 Calmetrix Inc All rights reserved J ESTIMATING SETTING TIMES FROM CALORIMETRY CURVES I CAL SET Optional Module Set will help you predict initial and final setting times within close approximation by applying the Fractions Method and generate Thermal Indicators of Set TIS This method is based on the assumption that for a given mix design there is a correlation between the heat evolution and setting times Initial set is reached
39. ve s you selected 4 For each curve select the Maturity Start Time c The Maturity Start Time is the beginning of the main hydration when strength is starting to build in your mix This should be the Initial Set Time of the mix if known and in any case at least 30 minutes longer than the Time to Iso which be determined in Reports using the guidelines page 21 of this manual 5 Define your extrapolation l Cal Strength lets you extrapolate a calorimetry curve Enter Extrapolation Start Time d and a Max Extrapolation Time e to determine the time window for 33 34 the extrapolation The Extrapolation Start Time must be shorter than the time of actual data that was logged 1 Logger QMR 73 453 Cell 8 Tset 20 0 degC 00 00 00 00 00 00 000 E 489 9 exp 94644 1 0 63 R2 1 0000 Ax 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 For most Portland cement based mixes tested at room temperature data must be logged for a minimum of 48 hours and preferably beyond 72 hours For best results we recommend that the Extrapolation Start Time 1 at least twice a long as the time to reach maximum power in the main hydration p
40. when the temperature level in a sample placed in the reaches a certain fraction of the peak Each mix has its very own fraction values corresponding to initial and final set Once the fraction values are determined for a given mix design they can be used to predict setting times when the same mix is used again in the future How to use the Set module To be able to predict setting times for a given mix design you will first have to create a model which establishes the relationship between the temperature curve and initial and final set as measured by a standard method for example ASTM C403 First build a model To build a new Model for a given mixture proceed as follows 7 Gotol Set and select the Modeling tab Click on New Model a 8 Click on Add Modeling Log b A new window will pop up letting you browse to the file containing the calorimetry curve for the mix for which you would like to build a model You can load up to 8 curves for the same mix 9 Select one or several curves for this mix and click on Accept The selected curve s will appear on the screen as shown below 10 For each curve enter the measured Initial Setting time in the Initial TIS field and the Final Setting time in the Final TIS field c These values should be measured using the standard you normally use to determine setting times e g ASTM C403 Now select the curves that you want to use to build your Fractions Model for

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