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DURALYZER-NIR ™ Laboratory Liquor Analyzer

1. 53 Calibration curves for Example A 6 2 55 Menu sequence for automated calibration curve determination 61 Bias adjustment determination for Example A 8 1 65 Bias adjustment parameters for Example A 8 1 65 Bias adjustment determination for Example A 8 2 66 Menu sequence for implementing bias adjustments 68 Printer WAS OSs oce o dd 70 Power switch and light source enclosure locations 71 Light source enclosure cover removal 72 NIR Tight Source removal at 72 U saturat ed Wat r Spe tfr m nada 73 Saturated water spectrum area tT 73 Menu sequence for the New Bulb function 74 MODBUS Configuration screen 75 Menu sequence for MODBUS configuration 76 R E Hodges LLC viii DURALYZER NIR Laboratory Liquor Analyzer Manual List of Tables 1 1 DURALYZER NIR vs Current Solutions 1 2 General Specifications ett e estate tne nua e nete enn 4 1 Startup PLOCCUURE P 4 2 Main Men SUMMA ans 4 3 Typical Units and Conversion Factors A 6 1 Comparison of Analyzer Values with
2. Figure 4 14 Display Units screen with default units Ib 100gal as Na20 Table 4 3 Typical Units and Conversion Factors Display Units Ib 100gal as Na O Ib 10gal as NaO Ib gal as Na O Ib f as Na O mL HCI 10 mL sample mL HCI 5 mL sample R E Hodges LLC 20 DURALYZER NIR Laboratory Liquor Analyzer Manual Display Units mE ee A A e MTS JN es e Figure 4 15 Display units in lb ft as Na Setting or adjusting the analyzer time and date that is displayed on the Operator Screen and the analysis print out is performed by selecting Time Date The Time and Date Adjustments screen would then appear Figure 4 16 touch the appropriate box to edit Time military hh mm and date dd mm yy must be entered in the exact format shown on the screen for the changes to take effect For the changes to be accepted both the time and the date must be entered For example setting the time and date to 12 01 January 5 2009 is shown in Figure 4 17 Press the Update button for the changes to take effect and then the Back button to return to the Main Menu Time and Date Adjustments Time Format Date Format hh mm dd mm yy J J Figure 4 16 Time and Date Adjustments screen R E Hodges LLC 21 DURALYZER NIR Laboratory Liquor Analyzer Manual Time and Date Adjustments Time Format Date Format hh mm idd mm yy 12 01 05 01 09 Figure 4 17 Exampl
3. Na CO TTA AA Sulfidity e 100 Sulfidity NI 100 NaOH 100 Causticity Na S Na S Na SO PRE 100 NaOH NaOH Na CO CE mass of solution mass of solution 1 291 NaOH 1 259 Na S 1 710 Na CO 100 as Na20 as Na20 as Na20 as Na20 as Na20 as Na20 Na20 basis Na20 basis Na20 basis Na20 basis Na20 basis 100 p 1 10096 pisin g cm mass of Na SO Na SO Na S 0 KCl NaCl Sulfidity AA basis Causticity JRE CE TDS TDS TDD TDD TDS NaOH Na2S and Na CO in Ib 100gal as Na20 p is in g cm in the bottom equation R E Hodges LLC p 1000 0 834 DURALYZER NIR Laboratory Liquor Analyzer Manual Appendix A 4 Setup Cautions When using or storing the DURALYZER NIR laboratory liquor analyzer be sensible with regard to the setup location Care should be taken to avoid the following conditions e High humidity e High temperatures e Volatile materials e Areas susceptible to wetness or splashing e Vibration e Excessive dust levels e Open flames e Abrupt changes in humidity and or temperature e Direct exposure to strong acids or acid vapors R E Hodges LLC 44 DURALYZER NIR Laboratory Liquor Analyzer Manual Appendix A 5 Normal Operating Procedure Supplies Required 1 2 3 4 1 0 N or 0 1 N HCI acid for cleaning s
4. SSSULFIDITY TDD 1 CE STOO FE Update mODBUS Ser Zero Aboot Figure 4 2 Operator Screen Before initiating sample analysis a water reference or baseline is taken Fill a sample container with water typically 200 mL of water in a 250 mL Nalgene bottle Fully compress squeeze the pipetting bulb and then insert the silicon tubing pickup tube into the water Draw the water into the cuvette by slowly releasing the bulb and then let it hang freely Select Set Zero on the LCD touch screen finger or stylus may be used In addition to setting a baseline setting the water zero also ensures the wavelength axis of spectrometer specifically the monochromator in the optics bench is properly aligned The corresponding screens for setting the zero are depicted in Figure 4 3 Scanning is delayed 120 seconds to ensure the water is stabilized the delay can be bypassed by selecting continue The message at the bottom of the screen will change when the water is being scanned spectrum acquired Setting Zero Wait Tap Water Should Be In The Setting Zero Wait Tap Water Should Be In The Sample CompartmentiCuvette Figure 4 3 Set Zero screens Sample CompartmentiCuvette R E Hodges LLC 13 DURALYZER NIR Laboratory Liquor Analyzer Manual The zero should be set once per day plus every time the analyzer is turned on once stabilized and after a
5. 0 and 3 offset only S 0 are considered Table A 8 1 compares analyzer values before bias adjustment with the three bias adjustment methods and the lab values TTA NIR TTA 1 TTA 2 TTA 3 and TTA LAB respectively Examination of Table A 8 1 shows all three bias corrections are in agreement with the lab measured values In this instance R E Hodges LLC 65 DURALYZER NIR Laboratory Liquor Analyzer Manual all three would be an acceptable choice Other cases may point favorably to a particular method Ib ft as Na O SAMPLE TTA NIR TTA LAB White Liquor 1 7 71 7 63 White Liquor 2 7 72 7 62 White Liquor 3 7 79 7 69 White Liquor 4 7 86 7 75 White Liquor 5 7 73 7 64 White Liquor 6 7 85 7 75 X jj 0 8821x rra 0 8203 J NIR Ib ft as Na O 1 Slope and Offset Ib f as Na O SAMPLE TTA NIR TTA LAB I White Liquor 1 7 71 7 63 y 0 9876x White Liquor 2 7 72 7 62 R2 0 9732 White Liquor 3 7 79 7 69 White Liquor 4 7 86 7 75 White Liquor 5 7 73 7 64 White Liquor 6 7 85 7 75 TTA Bias Adjustment y 0 8821x 0 8203 R2 0 9873 LAB Ib ft as Na 0 TTA Bias Adjustment 3 Z a EI E E lt Xp TTA 0 9876x rra 77 7 8 NIR lb ft as Na O 2 Slope Only Ib ft as Na O Ib ft as Na O SAMPLE TTA_NIR TTA_LAB ATTA LAB NIR White Liquor 1 7 71 7 63 0 08 White Liquor 2 T7412 7 62 0 10 White Liquor 3 7 19 7 69 0 10 White Liquor 4 7 86 7 75
6. Calibration curves for EA AA TTA and TDS need to be determined and implemented Figure A 6 1 illustrates the calculation of the curve parameters based on data provided in Ib 100gal as Na A 2 order polynomial fit is utilized for the EA AA and TTA whereas a linear fit is applied to the TDS data The calibration curve equations are clearly highlighted for each calibration model R E Hodges LLC 51 DURALYZER NIR Laboratory Liquor Analyzer Manual 1b 100gal as Na O SAMPLE EA NIR EA LAB Water 0 00 0 00 1 Causticizer 67 36 71 11 y 0 0005x 1 0294x 3 Causticizer 69 02 73 50 R 0 9999 69 61 74 14 15 98 17 03 23 57 24 21 EA Calibration Curve LAB 1b 100gal as Na O 2 3 X EA 0 0005 X3 PA 1 0294 a T 0 00 10 00 20 00 30 00 40 00 50 00 60 00 70 00 80 00 x dd NIR 1b 100gal as Na 0 Ib 100gal as Na 0 SAMPLE AA NIR AA LAB Water 0 00 0 00 1 Causticizer 79 70 85 09 y 7E 05x 1 082x 313 Causticizer 80 40 87 07 R 0 9999 White Liquor 80 94 87 24 Weak Wash 19 18 20 47 Green Liquor 32 73 35 56 AA Calibration Curve LAB 1b 100gal as Na O PEN 2 0 00 20 00 40 00 60 00 80 00 X aa 0 00007 x2 1 082x cc AA nz nz AA NIR Ib 100gal as NaO 1b 100gal as Na O SAMPLE TTA NIR TTA LAB Water 0 00 0 00 1 Causticizer 108 52 103 75 3 Causticizer 107 98 102 40 106 69 101 91 31 83 277 88 101 01 96 12 TTA Calibration Curve y 0 001x 0 8487x R2 0 9999 LAB Ib
7. R E Hodges LLC 25 DURALYZER NIR Laboratory Liquor Analyzer Manual Overwrite Current Configuration Cancel Continue Figure 4 25 Utilizing the Restore function 4 4 4 Informative Submenus The analyzer internal sensor values are viewed through the Status option on the Main Menu The screen Figure 4 26 shows the current internal sensor values The 5V source should read from 4 8 to 5 2 volts and the TEC set point should be between 1 48 and 1 51 volts Detector bias should be less than 0 1 volts and the internal temperature should be below 35 C If the parameters are within the specified range the analyzer is operating normally Analyzer Status Paramater olue 5 Source 5 007 TEC Setpoint V 1499 Detector Blas y 0 095 Internal Temp C 31 28 Figure 4 26 Analyzer Status screen A graphical display of the spectral signature of the last sample analyzed scanned is available by pressing Spectra on the Main Menu screen The spectra can be displayed in terms of Transmission or Absorbance by selecting the appropriate option on the left side of the screen A typical transmission water spectra is displayed in Figure 4 27 R E Hodges LLC 26 DURALYZER NIR Laboratory Liquor Analyzer Manual Sample Spectral Signatures Figure 4 27 Typical transmission water spectrum Replacement of the NIR light source QTH light bulb with reflective coating may req
8. the model in a least squares manner to agree more precisely with lab tests measurements There are two methods for determining calibration curves manual and automated Calibration curve parameters can be computed through the use of a spreadsheet and entered manually on the Component Curves Slopes and Offsets screen accessed by selecting Slope Offset on the Main Menu The default values for the calibration curves are shown in Figure 4 32 Each particular component calibration model has a box for entering the Curve Slope and Offset parameters Due to the water zero function sets the baseline the offset will always be zero Alternatively the Calibration function on the Main Menu can be used to bypass manual computation and parameter entry This is accomplished on the Calibrate Curve Slope and Offset screen Figure 4 33 Values for determining calibration curves for EA AA TTA and Na2SO4 must be in lbs 100gal as Na O At least two liquor samples and one water sample 3 total samples are required for calibration curve parameter determination This is true for both the manual and automated curve determination methods In obtaining lab test values for each sample extra care should be taken to ensure the results are as accurate as possible The repeatability of some testing methods can be less than desirable in many instances If this is the case it is recommended that more than three liquor samples are used and
9. 0 11 White Liquor 5 7 73 7 64 0 09 White Liquor 6 7 85 7 75 0 10 ES Avg A 0 0967 Kia Xerra 0 0967 6 Figure A 8 3 Bias adjustment determination for Example A 8 2 R E Hodges LLC 66 DURALYZER NIR Laboratory Liquor Analyzer Manual Table A 8 1 Bias adjustment method comparison for Example A 8 2 lb ft as Na O E No us White Liquor 1 White Liquor 2 White Liquor 3 White Liquor 4 White Liquor 5 White Liquor 6 Figure A 8 4 illustrates the menu navigation for entering the bias adjustment parameters Starting from the Operator Screen 1 About is selected and screen 2 appears Pressing IM brings up screen 3 to enter the password which allows access to the Main Menu 4 From the Main Menu 4 Set Bias is selected and the sample point to be biased is chosen on the Bias Adjustments screen 5 The bias adjustment parameters are entered at point A on the Edit Bias Values screen 6 Once the bias parameters have been entered press Update B for the changes to take effect Final Notes e Since laboratory measurements can have a significant amount of variability in terms of repeatability optimal bias adjustments will be achieved by utilizing more samples e Make sure the Normal Operating Procedure is followed when analyzing samples e Sometimes only a slope or offset correction is required e n the absence of values that fall over a wide range it may be safer t
10. 100gal as NaO 2 0 00 20 00 40 00 60 00 80 00 100 00 120 00 Xerra 0 001 x rra 0 8487 x rn I i E d NIR 1b 100gal as Na O SAMPLE TDS NIR TDS LAB Water 0 00 0 00 1 Causticizer 20 48 17 98 313 Causticizer 19 89 17 24 19 51 16 94 N A N A 22 94 20 39 TDS Calibration Curve 2 0 00 5 00 10 00 15 00 20 00 25 00 30 00 X srps 0 000x cers 0 8766 rps Sec Figure A 6 1 Calibration curves for Example A 6 1 R E Hodges LLC 52 DURALYZER NIR Laboratory Liquor Analyzer Manual sogas jas ioq uni stun 4oidsia sjeqo 1 dwo sid sidwos vOSZON VIL vv v3 125110 ado s AJ02 juauodwo 5 35 10 PUD sadojs SaA1n uauoduo 4S00 99v v uoddns O 211 sebpoy 3 y q L sezAjeuy doyysueg WE Eo Es Co Co zero 1000 vi Ca an v Lee soooo ado s aaan 11000 001 002 001 agoz SALA Losz 8 28 r0 09 39 68022 ALUMN Leger ALIDULSQ VON Lr s 002VN synsoy sisAjouy woon SHUN 0182 ony A sinsaa jud A 60 90 10 60 Sid zung 201 NOLLOVELXG juod aps 3002 3dd HSYM OY3IA ON ALHM ST ISAW Ea 1500448 arduos ONIS EA dian azAjouy reg u33135 J0 D1300 Figure A 6 2 Menu sequence for manual entry of calibration curve parameters Figure A 6 2 illustrates the menu navigation for entering the calibration curve Starting fro
11. NIR lab values under REA LAB and the bias corrected values under REA B The resulting bias adjustment equation is displayed R E Hodges LLC 64 DURALYZER NIR Laboratory Liquor Analyzer Manual with the data Bias adjustment parameters are entered into the Edit Bias Values screen Figure A 8 2 g L as Na O SAMPLE REA NIR REA LAB REA B Evaporator 3 14 4 03 4 04 Chemiwasher 2 34 3 04 3 07 Secondary Evaporator 2 58 341 3 37 REA Bias Adjustment y 12154x 0 2271 R2 0 9937 LAB g L as Na O X pea 1 2154 x pga 0 2271 3 00 NIR g L as Na O Figure A 8 1 Bias adjustment determination for Example A 8 1 Edit Bias Values Component Slope Offset Update Figure A 8 2 Bias adjustment parameters for Example A 8 1 Example A 8 2 After implementing a TTA calibration curve based on green liquor weak wash clarified white liquor and causticizer samples the clarified white liquor analyzer measurements were slightly high compared to the lab The TTA analyzer measurements for the other sample points were in agreement with the lab Thus a bias adjustment was implemented on the clarified white liquor TTA measurement Six total clarified white liquor samples were collected and tested over a 3 to 4 day period The bias adjustment determination for this data set is illustrated in Figure A 8 3 The three bias adjustment methods 1 slope and offset 2 slope only So
12. Principle of Operation 2 1 Concept The DURALYZER NIR laboratory liquor analyzer is based on the implementation of NIR spectroscopy to determine the chemical composition of process liquors This spectroscopic technique is a subset of a larger class of analytical techniques that fall under the category of optical spectroscopy Figure 2 1 shows the electromagnetic spectrum with the portion relating to optical spectroscopy expanded NIR region highlighted with black arrow Optical spectroscopic techniques have been used quite successfully for decades in a laboratory setting to analyze liquids solids and gases composed of a multitude of chemical species In the past twenty five to thirty years the development of miniaturized and durable electronic and optical components has allowed many of these techniques to be implemented in the process environment Advancements in computational techniques and microcomputers have fueled the increased utilization of optical spectroscopy for qualitative and quantitative analysis in the process environment Cosmic Rays y Rays X Rays UV Vis Infrared Microwaves UHF Radio as l 1013 1012 10 10 10 10 7 106 10 10 103 10 10 10 10 10 Wavelength m Optical Spectroscopy Visible Short Wave Near Mid V Light Near Infrared Infrared Infrared 0 5 5 i 4 40 Wavelength um Wavenumber cn l o Ke N Figure 2 1 E
13. R E Hodges LLC 23 DURALYZER NIR Laboratory Liquor Analyzer Manual Change Password Current Password New Possword Figure 4 21 Change Password screen where the current password is TIGERS Change Password Current Password TIGERS LIGTEST Hew Password Figure 4 22 Password is changed to LIQTEST The Display option on the Main Menu allows the user to adjust the contrast and backlighting of the LCD screen Figure 4 23 shows the Contrast amp Backlight Adjust screen where the adjustments are made by manipulating the appropriate touch screen sliders To accept the changes press Save otherwise select Cancel R E Hodges LLC 24 DURALYZER NIR Laboratory Liquor Analyzer Manual i Contrast amp Backlight Adjust Contrast Backlight Save Figure 4 23 Contrast amp Backlight Adjust screen In order to save a configuration Backup is selected on the Main Menu Selecting this option triggers the message in Figure 4 24 When making configuration changes it is recommended to save backup after each change If it becomes necessary to return to the last saved configuration select the Restore option on the Main Menu The screen Figure 4 25 will give the option of canceling the operation or to continue and overwrite the current configuration Analyzer Configuration Saved Figure 4 24 Saving the current analyzer configuration
14. S w lennenen ee oe 18 0D 2 wavelength um Figure 4 29 Saturated water spectrum Basic analyzer information such as the model number serial number and software version is displayed by selecting Analy Info on the Main Menu screen A sample display is shown in Figure 4 30 The Print Cfg option prints out a hard copy summary of the analyzer configuration Selecting this option will briefly cause a notification screen Figure 4 31 to appear Analyzer Info Paramater Yalue Model Number BTLA BGYWL GO Serial Number BTLAQS1508 001 Software Version VER 4 00 Figure 4 30 Analyzer Info screen R E Hodges LLC 28 DURALYZER NIR Laboratory Liquor Analyzer Manual Analyzer Configuration Printed Figure 4 31 Print Cfg notification screen 4 4 5 Model Tuning Submenus The DURALYZER NIR laboratory liquor analyzer has seven standard calibration predictive models for analyzing green white and black liquor samples The calibration models have been developed through a combination of signal processing steps and mathematical regression techniques In some cases the models need to be tuned by utilizing a calibration curve The seven models are as follows EA REA for black liquor AA RAA for black liquor TTA Na2504 TDS TDD and TDO Each model will have a separate calibration curve and be represented by a second order polynomial The curve tunes adjusts
15. below the soap layer of liquor to minimize the amount of soaps and extractives pulled into the cuvette Select Analyze Sample on the Operator Screen The sample will be analyzed after the delay time default is 120 seconds The delay is necessary to ensure the sample has stabilized in the cuvette an in some cases will need to be increased beyond the default value of 120 seconds When the analysis is complete the Operator Screen will update displaying the current results If the MODBUS communication interface is being used select Update MODBUS on the Operator Screen to send the analysis results to the appropriate registers For a hard copy printout of the analysis results via the thermal printer check the Print Results box R E Hodges LLC 46 DURALYZER NIR Laboratory Liquor Analyzer Manual 12 Place the pickup tubing in the sample waste collection bottle and eject the liquor by holding the bulb in an upright position and compressing squeezing several times to eject all the liquor The tubing should be held or secured when doing this to avoid the possibility of uncontrolled spray Thoroughly flush the sample cuvette with water and eject into the waste bottle 13 If analyzing testing more samples repeat steps 6 12 14 When the testing session is complete all samples acquired from the field have been analyzed fill a clean container with water and draw it into the sample cuvette Allow the water to remain
16. in the cuvette until the next series of samples are to be tested R E Hodges LLC 47 DURALYZER NIR Laboratory Liquor Analyzer Manual Appendix A 6 Manual Calibration Curve Determination Background The DURALYZER NIR laboratory liquor analyzer has seven standard calibration predictive models for analyzing green white and black liquor samples The calibration models have been developed through a combination of signal processing steps and mathematical regression techniques Models are tuned by utilizing a calibration curve Employing a calibration curve allows the individual component EA AA etc models to be adjusted to match the lab test method results in a least squares sense The seven models are as follows EA REA for black liquor AA RAA for black liquor TTA Na5S0 4 TDS TDD TDO Certain measurements may not be required for a given application of the analyzer In which case determining a calibration curve for that model would be unnecessary For example if there is not an interest in Reduction Efficiency then there is not a need for a sodium sulfate calibration curve Likewise TDO total dissolved organics would only have meaning for black liquor samples Y DU Pa y pir For manual determination each calibration curve will be represented by the second order polynomial given by Equation A 6 1 x Ax Bx A 6 1 Constant curve parameters A and B are determined by the manual calibrati
17. is complete set the water zero if this has not been performed recently Refer to Section 4 3 Normal Operation and Appendix A 5 Normal Operating Procedure 5 Test the collected samples on the DURALYZER NIR laboratory liquor analyzer following the procedures set forth in Section 4 3 and Appendix A 5 After each sample has been analyzed record the values shown in the Analysis Results section of the Operator Screen These will be the analyzer or NIR values It is highly recommended to have the Print Results box checked on the Operator Screen and the printer connected prior to analyzing the samples 6 After all collected samples have been lab tested and analyzer tested the mathematical determination of the bias adjustment parameters is performed This requires the use of spreadsheet software such as Microsoft Excel 7 On the spreadsheet make three column headings for the sample the analyzer measurement value and the lab measurement value 8 Construct a scatter plot with the analyzer values being the X data and the lab values being the Y data Fit the data with a linear trendline The resulting trendline equation is the bias adjustment in the form of Equation A 8 1 In some cases it may be preferable to bias adjust the data with just a slope correction So in Equation A 8 1 will be zero or just an offset correction S in Equation A 8 1 will be zero 9 Select Set Bias on the Main Menu From the Bias Adjus
18. labels eneeeneeeeeeeeeeeeseeeseseseseresesesesesesesesess 19 4 14 Display Units screen with default units Ib 100gal as Na20 20 4 15 Display units in Ib f as NaO erento tlc tette cae 21 4 16 Time and Date Adjustments screen 21 4 17 Example of setting time and date cas 22 4 18 MODBUS Configuration screen us A tie ca AA ce dade 22 4 19 Scan Parameters screen with default values for each sample point 23 4 20 Custom scan parameters applied to each sample point 23 4 21 Change Password screen where current password is TIGERS 24 4 22 Password is changed to LIQTEST 24 4 23 Contrast amp Backlight Adjust screen 25 4 24 Saving the current analyzer configuration 25 4 25 Utilizing the Restore function eie desea ee acides 26 4 26 An nal z r Stats SC TORTE n NS o aus a 26 4 27 Typical transmission water SpecHrum conan non eene 27 4 28 Unsaturated water spectrum 27 4 29 Sat rated walter EE 28 4 30 Analyzer Info SOTeen u ul n ai E 28 4 31 Print Cfg Notification screen nude 29 4 32
19. lack of work space in most pulp mill laboratories Test results are displayed on the LCD touch screen panel and can also be printed via the accompanying thermal printer Results can also be sent directly to the DCS through the MODBUS connection Delivery of the sample to the cuvette is simple Silicone tubing is attached to the cuvette with one end placed in the sample container and the other end attached to a syringe or similar device Currently the analyzer is shipped with a 60 mL pipetting bulb The design of the DURALYZER NIR laboratory liquor analyzer allows for custom arrangements Figure 2 7 shows the syringe setup R E Hodges LLC 8 DURALYZER NIR Laboratory Liquor Analyzer Manual DURALYZER NIR Laboratory Liquor i i Analyzer Silicone Tubing Sample Cuvette amp Holder Thermal Printer Touch Screen LCD Panel Figure 2 7 DURALYZER NIR laboratory liquor analyzer syringe setup 3 Installation 3 1 General The DURALYZER NIR laboratory liquor analyzer is designed for straightforward installation setup while minimizing the associated costs monetary and time Highlights and key components are identified in Figure 2 7 The setup location should be in an area safely away from continual exposure to acid vapor Care should be taken to avoid moisture exposure to the LCD panel and the thermal printer panel and printer are attached via cables so this should not be too di
20. net effect of minimizing the overall cost of ownership Scheduled operation and maintenance requirements have been kept to a minimum These include annual bulb replacement in the light source enclosure and occasional acid cleaning of the sample cuvette Periodic validation with lab tests should be performed as well Unscheduled maintenance has been greatly reduced by minimizing the system component count As with any sophisticated hardware common sense care will aid in extending the lifetime of the analyzer Follow standard laboratory safety protocols when using the analyzer such as wearing protective eyewear and clothing R E Hodges LLC 11 DURALYZER NIR Laboratory Liquor Analyzer Manual 4 2 Startup Startup is straightforward entailing setup tasks and power up In some cases R E Hodges LLC personnel can be on hand to perform and oversee startup operations The startup procedure is outlined in Table 4 1 Figure 4 1 shows the LCD screen when power is activated Table 4 1 Startup Procedure Identify a safe convenient and hazzard free location take into account Setup Cautions listed in the Appendix 2 Unpack and arrange accessories printer etc 3 Connect all power cables and communication cords 4 Attach tubing to cuvette and pipetting bulb 5 Secure cuvette in holder with set screw 6 Turn on analyzer and close SS enclosure with key Allow analyzer to be powered on for a MINIMUM of 2 hours before 7 proceding with any
21. to the right Default values for the Edit Bias Values screen are displayed in Figure 4 35 Bias adjustments slope and or offset are made based on the current display units An example of bias adjustment is given in Appendix A 8 Bias Adjustment R E Hodges LLC 30 DURALYZER NIR Laboratory Liquor Analyzer Manual Bias Adjustments Select Sample Point DI Sample Point OH Sample Point OH Sample Point Sample Point OH Sample Point OH Sample Point Q Sample Point 4q gt om o T Q Sample Point Figure 4 34 Bias Adjustments screen with Sample Point 1 selected Edit Bias Values Component Slope Offset EA AA TTA Na25 04 TOS Ye TOD HILT HII TOO Update Figure 4 35 Edit Bias Values screen with default values 4 5 Maintenance The maintenance requirements for the DURALYZER NIR laboratory liquor analyzer are minimal both in terms of time and cost Maintenance tasks should only be performed by qualified personnel that have read and understand this manual There are four maintenance tasks that can be undertaken by mill personnel 1 Acid cleaning the sample cuvette 2 Cleaning the analyzer cabinet and LCD panel 3 Cleaning the thermal printer and 4 Light source replacement Any other maintenance or repair tasks should be carried out by R E Hodges LLC personnel Cleaning the sample cuvette is accomplished with 1 0 N or 0 1 N HCl acid alth
22. via the RS232 port 2 plug the DC end of the power cord into the printer and 3 plug the 3 prong AC end into a standard wall outlet Cables and other images of the printer are shown in Figure A 9 1 Paper Roll Installation The thermal paper roll must have a width of 80 mm thickness of 65 to 85 um and a roll diameter of 90 mm or less 1 Open the printer cover by pushing the lever on the top front of the printer highlighted in Figure A 9 1 2 Place the paper roll in and pull the leading edge of the paper towards the front of the printer paper direction should be such that the leading edge is coming from under the roll not over top 3 Close the printer cover by pressing down on both sides Cleaning and Care The presence of accumulated dust will adversely affect printer performance possibly causing the printout to be unreadable or not to function at all Cleaning the printer is a three part process 1 Cleaning the thermal head 2 Cleaning the paper holder and 3 Cleaning the paper housing Care must be taken when cleaning the thermal head since it is easy to damage Use isopropyl alcohol and a soft clean cloth A soft cloth is sufficient for removal of dust from the paper holder The external housing of the printer can be wiped off with a moist cloth Specifications e Dimensions 199 mm x 142 mm x 132 mm see Figure A 9 1 e Weight 1 4 kg e Paper width 80 mm Maximum print speed 100 mm s 800 dots s e Do
23. 100gal as Na O SAMPLE EA LAB EA NIR EA LAB EA Calibration Curve Water 0 00 0 000 0 00 80 00 Weak Wash 11 22 7 216 9 36 5 y 0 0053x 1 4605x Green Liquor 21 77 12 631 18 17 ZS 60 00 R 0 9996 White Liquor 81 70 59 733 68 18 S 2 40 00 Xec EA 0 0053 E 1 4605 X EA d 20 00 0 00 0 000 10 000 20 000 30 000 40 000 50 000 60 000 70 000 NIR Ib 100gal as Na O g L as Na O 1b 100gal as Na O SAMPLE AA LAB AA NIR AA LAB AA Calibration Curve Water 0 00 0 000 0 00 100 00 Weak Wash 12 81 7 534 10 69 5 Md Green Liquor 35 24 19 152 29 41 E M i HR QUE B White Liquor 95 30 64 179 79 53 60 00 ms z 4000 x 2 Xec AA T 0 0059 X AA 1 6184 X AA E 20 00 4 0 00 0 000 10 000 20 000 30 000 40 000 50 000 60 000 70 000 80 000 NIR 1b 100gal as Na O g L as Na O 1b 100gal as Na O SAMPLE TTA LAB TTA NIR TTA LAB TTA Calibration Curve Water 0 00 0 000 0 00 w Weak Wash 14 42 11 718 12 03 CH pM Green Liquor 114 05 89 713 95 18 DN LAE 2 80 00 4 R 0 9998 White Liquor 110 95 85 018 92 59 60 00 4 _ 2 E 40 00 X rra 0 0002 x rra 1 0485 x rra B n 0 00 T 0 000 20 000 40 000 60 000 80 000 100 000 NIR Ib 100gal as Na O Figure A 6 3 Calibration curves for Example A 6 2 Figure A 6 3 depicts calibration curves for weak wash green liquor and white liquor where the lab values are initially reported in g L as N
24. 120V 60 Hz single phase 10A outlet with line neutral and ground connections The thermal printer is connected to the analyzer via the RS232 port and is equipped with its own power unit and power cord which also connects to any standard 3 prong outlet Further details concerning the thermal printer are located in Appendix A 9 Printer Details The LCD touch screen cable is plugged in to the 4 pin connector located next to the RS232 printer connection A MODBUS RTU 5 pin connection port is also available externally All external connection locations are on the side of the analyzer opposite the cuvette and exhibited in Figure 3 1 Figure 3 1 External connection locations Two internal connections are also present Remote modem support is provided through the RJ11 connection enabling software updates and an ability to assist mill personnel in R E Hodges LLC 10 DURALYZER NIR Laboratory Liquor Analyzer Manual troubleshooting if the need arises A Cat 5 RJ45 ethernet connection is available for MODBUS TCP The internal connections as well as key internal components are identified in Figure 3 2 Power On Off RJ11 Connection RJ45 Connection Figure 3 2 Internal connections and components 4 Operation and Maintenance 4 1 General The DURALYZER NIR laboratory liquor analyzer has been designed for ease of operation and minimization of short and long term maintenance requirements This has a
25. Component Curves Slopes and Offsets screen 30 4 33 Calibrate Curve Slope and Offset screen 30 4 34 Bias Adjustments screen with Sample Point 1 selected 31 R E Hodges LLC Vil DURALYZER NIR Laboratory Liquor Analyzer Manual 4 35 4 36 4 37 A 1 1 A 1 2 A 1 3 A 1 4 A 1 5 A 1 6 A 1 7 A 1 8 A 1 9 A 1 10 A 1 11 A 6 1 A 6 2 A 6 3 A 7 1 A 8 1 A 8 2 A 8 3 A 8 4 A 9 1 A 10 1 A 10 2 A 10 3 A 10 4 A 10 5 A 10 6 A 11 1 A 11 2 Edit Bias Values screen with default values esses 31 NIR light source enclosure eaten tar 32 NIR light source removal iii cd 33 DURALYZER NIR laboratory liquor analyzer dimensions 35 LCD panel dimensions 36 Printer dimensions nn 37 GENEE n au u ai a 38 NIR Quartz Tungsten Halogen QTH light source 38 Accessories and Cable iio 39 Analyzer external connection ports ss 39 Analyzer internal components este weaned 40 Sample cuvette and light source enclosure 40 NIR light source Bic lOSUTe oiov tds 41 Analyzer Side Vii 41 Calibration curves for Example A 6 1 52 Menu sequence for manual entry of calibration curve parameters
26. DURALYZER NIR Laboratory Liquor Analyzer March 2009 User Manual R E Hodges LLC Pioneering Advanced Measurement Solutions for the Process Industries DURALYZER NIR Laboratory Liquor Analyzer Manual Company Profile R E Hodges LLC hereafter referred to as REH LLC was formed in 2001 as a manufacturer of online and laboratory spectroscopic based measurement solutions for the process industries The equipment and instrumentation developed by REH LLC is specifically designed to be easily incorporated into a control strategy In general spectroscopic based measurements hold the key to unlocking the majority of difficult measurement applications in the process industries REH LLC was created to replace or reduce traditional laboratory based testing for quality control by implementing real time online measurements coupled with practical control strategies Unlike traditional spectrometer manufacturers REH LLC provides turnkey sampling and measurement solutions that are tailored to suit the specific application In addition to accuracy and reliability our analyzers are characterized by minimal installation and continuing maintenance requirements At REH LLC we take great pride in the innovation and quality of our products and the continuing service and support we provide for each product We are unique in our ability to work with the customer to develop a customized online or laboratory measurement solution
27. DURALYZER NIR Laboratory Liquor Analyzer Manual determination of reduction efficiency RE For black liquors analysis consists of residual effective alkali REA and TDS As an option residual active alkali RAA and lignin measurements can be provided for black liquor samples 1 2 DURALYZER NIR vs Current Solutions Manual laboratory liquor testing is performed routinely for quality control purposes For pulp mills utilizing online liquor analyzers periodic testing is still necessary in order to validate the online measurements Frequently lab tests are the only source of measurements for process control decisions The rather tedious and cumbersome nature of the standard ABC testing procedure for process liquors does not lend itself to rapid manual testing Unfortunately it does lend itself to induced errors and biases Asa result liquor testing frequency is low once or twice per operator shift and the ability to reduce or correct process variations and disturbances is severely hampered A brief comparison between the standard ABC titration test laboratory autotitrators and the DURALYZER NIR laboratory liquor analyzer is shown in Table 1 1 Table 1 1 DURALYZER NIR vs Current Solutions Characteristic STD ABC Titration Autotitrator DURALYZER NIR 7 EA AA TTA TDS TDD Available Measurements 3 EA AA TTA 3 EA AA TTA Lignin Na SO Inferred inflection pt method Inferred regression mod
28. E A END Med d 79 Aglare Warranty and INO CES scouts ts 80 R E Hodges LLC vi DURALYZER NIR Laboratory Liquor Analyzer Manual List of Figures 1 1 DURALYZER NIR laboratory liquor analyzer 1 2 1 Electromagnetic spectrum related to optical spectroscopy 4 2 2 Basic transmission cell configuration eese 5 2 3 Sample EUVetle EE 5 2 4 SR Ne 6 2 5 TheBesr Lambert law xcs 35 6 besectnala hes n nt MN 7 2 6 Simplified view of regression modeling and prediction 8 2 7 DURALYZER NIR laboratory liquor analyzer syringe setup 9 3 1 External connection locations ita 10 3 2 Internal connections and components 11 4 1 LCD BOOT street sis eet doo do A 12 4 2 Operator iSOreehnu E Dub OS apti edt Cd A USA 13 4 3 SEL Zero SCT BNS tii 13 4 4 ET ET 14 4 5 Analysts TESUIS uoce A db a e sata cioe ade dtes es 14 4 6 UNDOUL e cpt Seles A QS ofc ha Lt 16 4 7 LCD touchscreen Key DOA s ann tintin thin tn 16 4 8 Main Menu SCreen iiie lie deel da 16 4 9 Blank Sample Point Labels SOc eM sc iiie ial iia 18 4 10 Sample Point 1 labeled as GREEN LIQ 18 4 11 All sample points labeled icti eet vetas 18 4 12 Component Labels screen with default values 19 4 13 Customized EA AA and TTA
29. LC DURALYZER NIR Laboratory Liquor Analyzer Manual Appendix A 11 MODBUS The DURALYZER NIR laboratory liquor analyzer is equipped with MODBUS communications ability It is configured by selecting MODBUS on the Main Menu This will pull up the MODBUS Configuration screen shown in Figure A 11 1 with example settings The settings on this screen are used to configure the MODBUS TCP interface to the analyzer Simply touch the box to be edited and enter the new value using the virtual LCD keyboard Entries must conform to the format displayed above each box Figure A 11 2 illustrates the LCD menu sequencing for configuring the MODBUS and Table A 11 1 lists the MODBUS register addresses MODBUS Configuration IP Address Het Mask Format Format Catt ta a eat ae eae tate tata ee eee Gateway Slave ID Format Format IERE ta a ea ae Pss IEE Integer Register Encoding Offset I ua a H m Figure A 11 1 MODBUS Configuration screen e IP Address refers to the IP address assigned to the analyzer Class C address 32 bit e Net Mask mask for the IP address 255 255 255 000 e Gateway IP address assigned to device with which analyzer is communicating without the presence of a router this will usually be 000 000 000 000 Slave ID the analyzer will always be the slave or server and can have an ID ranging from 001 to 247 as defined by MODBUS specifications Integer Enco
30. Lab Values Ex A 6 1 A 8 Bias Adjustment Method Comparison for Example A 8 2 A 11 1 MODBUS Register Addresses A 12 1 Troubleshooting Guide A 13 1 Replacement Parts Lists ses satire R E Hodges LLC 1X DURALYZER NIR Laboratory Liquor Analyzer Manual 1 Introduction and Specifications 1 1 Introduction The DURALYZER NIR laboratory liquor analyzer has been engineered to provide fast reliable and accurate measurements while avoiding the negative issues associated with manual testing and laboratory autotitrators The laboratory liquor liquid analyzer shares the near infrared NIR technology utilized by our online liquor analyzers and is specifically designed to function in the somewhat harsh laboratory environments in the pulping and recovery areas Maintenance requirements have been held to a minimum consisting of periodic acid cleaning of the sample cuvette and annual light source replacement The DURALYZER NIR laboratory liquor analyzer is shown in Figure 1 1 Figure 1 1 DURALYZER NIR laboratory liquor analyzer Effective alkali EA active alkali AA total titratable alkali TTA total dissolved solids TDS and total dissolved dead load TDD are computed for white liquor green liquor and weak wash Additionally Na SO is measured for green liquor to allow for R E Hodges LLC 1
31. Our overall goal is to continually improve and expand our product line capabilities and service to meet the evolving challenges of current and future customers It is our firm belief that the customer s success translates into our success R E Hodges LLC 2217 Pumphrey Avenue Auburn AL 36832 Phone 334 466 0057 Fax 334 466 0058 R E Hodges LLC ii DURALYZER NIR Laboratory Liquor Analyzer Manual About This Manual This manual provides information necessary for proper operation and care of the DURALYZER NIR laboratory liquor analyzer The subject matter is divided into four main headings Introduction and Specifications Principle of Operation Installation Operation and Maintenance Tem The manual is more than a simple set of instructions Specific topics covered include the following e Comparison between the DURALYZER NIR and other current solutions Chapter 1 e General specifications Chapter 1 e NIR spectroscopy and its implementation Chapter 2 e Installation guidelines and procedure Chapter 3 e Startup and normal operation Chapter 4 e Customizing the analyzer settings Chapter 4 e MODBUS configuration Chapter 4 e Calibration model tuning Chapter 4 e Maintenance requirements and procedure Chapter 4 Information contained in the main body of the manual is further detailed in the appendices Careful attention has been paid to accuracy of the contents of this manual R E Hodg
32. SO Word 40111 Na SO Word 40022 Na SO Word P 40067 NaSO Word d 40112 NaSO Word 2 40023 Na58 03 Word 40068 Na S 0 Word 40113 NaS20 Word 40024 E 4009 CI Word E Cam CI Word E 40025 A 40070 Sample Temperature Word A 40115 Sample Temperature Word 40026 Reserved Word 40071 Reserved Word 40116 Reserved Word 40027 40072 Reserved Word 40117 Reserved Word 40028 Reserved Word 40073 Reserved Word 40118 Reserved Word 40029 40074 Reserved Word 40119 Reserved Word 40030 EA REA Word 40075 EA REA Word 40120 Alarm Bit Field Bits 15 0 40031 40076 AA RAA Word 40121 Alarm Bit Field Bits 31 16 40032 TTA Word 40077 TTA Word 40122 Status Bit Field Bits 15 0 40033 6 40078 TDS Word s 40123 Status Bit Field Bits 31 16 40034 TDD Word S 40079 TDD Word bat 40124 Status Bit Field Bits 47 32 40035 TDO Word amp 40080 TDO Word S 40125 Status Bit Field Bits 63 48 40036 Na SO Word 40081 Na SO Word 40126 DCS Control Bit Field Bits 15 0 40037 D 40082 Na SO Word 40127 LCD Control Bit Field Bits 15 0 40038 Na S 03 Word T 40083 Na S 0 Word a 40039 Cr Word E 40084 CI Word 40040 amp 40085 Sample Temperature Word H 40041 Reserved Word 40086 Reserved Word 40042 40087 Reserved Word 40043 40088 Reserved Word 40044 Reserved Word 40089 Reserved Word Notes 1 Offset is assumed to be ZERO but can be set to any value 2 Function Code 3 amp Function Code 16 are the only codes that are recognized 3 Function Code 16 can only access re
33. Sample Cuvette Silicon Tubing R E Hodges LLC Table A 13 1 Replacement Parts List 79 DURALYZER NIR Laboratory Liquor Analyzer Manual Appendix A 14 Warranty and Notices Warranty The DURALYZER NIR laboratory liquor analyzer is warranted by R E Hodges LLC against defects in material and construction for one year from the date of shipment Our liability shall be limited to parts repair or replacement For warranty repair or replacement the customer shall pay for shipping charges to our facility or travel charges if warranty work is performed at the customer s plant or facility This warranty does not cover damages or defects caused by improper use neglect accidents wear inadequate maintenance poor site preparation or modifications and repairs not authorized by R E Hodges LLC or explicitly described in this manual R E Hodges LLC will assume no liability for any incidental indirect or consequential damages arising out of the use or misuse of this product Notices e Information contained in this manual is subject to change without notice e RE Hodges LLC makes no warranty as to the accuracy or completeness of this manual and disclaims any liability in connection with its use e Service maintenance agreements are available contact R E Hodges LLC for details and pricing e No part of this manual may be reproduced without prior written consent of R E Hodges LLC R E Hodges LLC 80
34. Touch Screen LCD Panel Figure A 1 4 System setup Figure A 1 5 NIR Quartz Tungsten Halogen QTH light source R E Hodges LLC 38 DURALYZER NIR Laboratory Liquor Analyzer Manual Analyzer power Printer cable 6 ft Printer AC adapter Sample cuvette 2 wi 5 ft cable Enclosure key Printer power cable 6 ft Printer serial EEN interface cable 6 f panel w 5 ft cord 60 ml rubber pipetting bulb Silicone tubing 4 ft Figure A 1 6 Accessories and cables Figure A 1 7 Analyzer external connection ports R E Hodges LLC 39 DURALYZER NIR Laboratory Liquor Analyzer Manual Power On Off Switch RJ11 Connection RJ45 Connection Figure A 1 8 Analyzer internal components Quartz Tungsten Halogen QTH NIR Light Source Analyzer Sample Cuvette Holder Figure A 1 9 Sample cuvette and light source enclosure R E Hodges LLC 40 DURALYZER NIR Laboratory Liquor Analyzer Manual Figure A 1 10 NIR light source enclosure Figure A 1 11 Analyzer side view R E Hodges LLC 41 DURALYZER NIR Laboratory Liquor Analyzer Manual Appendix A 2 Nomenclature AA CE DCS EA KCl LCD MODBUS Na2CO3 NaS Na25203 NaSO 3 Na2SO4 NaCl NaOH NEMA NIR QTH RAA RE REA REH RTU SCAN SS TAPPI TCP TDD TDS TDO TEC TTA VAC A B C V So Active Alkali Causti
35. a The procedure is analogous to R E Hodges LLC 55 DURALYZER NIR Laboratory Liquor Analyzer Manual the previous example except the lab values are converted from g L as Na20 to Ib 100gal as Na20 XY scatter plots are generated for EA AA and TTA where the NIR values and LAB values in Ib 100gal as Na2O are used for the X and Y values respectively Final Notes e Since laboratory measurements can have a significant amount of variability in terms of repeatability better calibration curves will be achieved by utilizing more calibration samples e Make sure the Normal Operating Procedure is followed when analyzing samples Sometimes a linear fit is better than a 2 order polynomial e Inthe absence of values that fall between the minimum and maximum it is best to use a linear fit e Contact R E Hodges LLC for any further assistance R E Hodges LLC 56 DURALYZER NIR Laboratory Liquor Analyzer Manual Appendix A 7 Automated Calibration Curve Determination Background The DURALYZER NIR laboratory liquor analyzer has seven standard calibration predictive models for analyzing green white and black liquor samples The calibration models have been developed through a combination of signal processing steps and mathematical regression techniques Models are tuned by utilizing a calibration curve Employing a calibration curve allows the individual component EA AA etc models to be a
36. across a wide range and between the upper and lower values 1 e green liquor EA and AA falls between water and white liquor Black liquor with very low REA or high organic and soap content is not ideal for curve parameter determination In this case any black liquor measurement adjustments should be made through the Set Bias function If there is only a white liquor sample available then a white liquor sample may be diluted to form a second liquor sample A one part white liquor to one part water dilution ratio would work fine and yield an EA and AA value roughly half of the undiluted sample The dilute sample must still be tested to obtain a precise lab measurement value do not assume it is exactly half the undiluted value The TTA calibration curve can be determined from green liquor weak wash and white liquor samples Other combinations are possible as well such as weak wash and white liquor or white liquor and diluted white liquor see above paragraph for comments on dilution Reduction efficiency RE computation requires the measurement of sodium sulfate Green liquor samples are used to determine the Na2SO4 curve parameters Obtain a single green liquor sample in an amount suitable to divide into three samples of equal volume Add approximately 5 g L and 10 g L of Na2SO4 to samples one and two respectively Do not add any to the third sample Allow the sodium sulfate added to samples one and two to completely dissolve this wi
37. al samples are required for calibration curve parameter determination If the current lab testing method in place produces less than desirable repeatability more than two liquor samples will be required It is important to note that all samples need to be tested using the same method and by the same person This eliminates potential of conflicting biases being introduced into the lab values and ultimately will yield a less R E Hodges LLC 57 DURALYZER NIR Laboratory Liquor Analyzer Manual than optimal calibration curve Special care should be taken when performing the lab tests to ensure the highest possible precision in the measurement values For example past experience has shown that using an autotitrator for the white liquor ABC test and manual titration for the green liquor ABC test is not a good idea If this is the standard treatment at a mill run the green and white liquor tests for curve parameter determination on the autotitrator After the calibration curves are set and in use go back and run manual tests on the green liquor and make any adjustments by using the Set Bias function on the LCD panel Main Menu Details on setting biases can be found in Section 4 4 5 and Appendix A 8 For EA and AA a white liquor and a green liquor sample is recommended to determine the curve parameters A weak wash sample and or a black liquor sample can be used as well The important idea is to have samples that give values
38. always be 0 00 due to setting the water zero This is arrangement is done for each component 8 Construct a scatter plot with the analyzer values Ib 100gal being the X data and the lab values Ib 100gal being the Y data Fit the data with a 2 order polynomial trendline and set the intercept to zero The resulting trendline equation is the calibration curve in the form of Equation A 6 1 In some cases it may be preferable to fit the data with a linear trendline and the A term in Equation A 6 1 will be zero 9 Repeat step 8 for all components requiring a calibration curve 10 After determining the calibration curve equations parameters enter the corresponding values into the Component Curves Slopes and Offsets screen Referring to Equation A 6 1 A is the Curve value B is the Slope value and 0 0 is the Offset value When done select Update The calibration curves are now set and will be in use the next time a sample is analyzed Two examples are presented to further highlight and explain the procedure and concepts presented above Example A 6 1 In the following example the DURALYZER NIR laboratory liquor analyzer is operated in causticizing area of the mill The following samples will be analyzed on a regular basis 1 causticizer 3 causticizer white liquor weak wash and green liquor Measurements of particular interest are EA AA TTA Sulfidity CE and TDS
39. ample cell in which the liquor interacts with NIR light The transmitted light is then collected via fiber optic cable and sent to the spectrometer Chemical compositions are computed by passing the transmitted NIR light spectrum through the calibration model The calibration model is based on sample spectra of known composition and constructed using a series of signal processing steps R E Hodges LLC 7 DURALYZER NIR Laboratory Liquor Analyzer Manual and employing a variation of partial least squares PLS or other regression techniques A simplified flow diagram of the regression analysis is contained in Figure 2 6 Calibration Spectra Unknown Spectrum Principal Components Regression Chemical Physical Model Property Prediction Figure 2 6 Simplified view of regression modeling and prediction 2 2 Implementation Direct implementation of NIR spectroscopy for laboratory liquor analysis requires an analyzer able to withstand long term use in the harsh lab environments of the pulping and recovery areas The DURALYZER NIR M laboratory liquor analyzer is housed in a 304 SS NEMA 4X enclosure which provides protection from corrosive agents moisture and dust Attaching the sample cuvette holder and light source directly to the enclosure serves to eliminate the need for fiber optic cables and minimize the overall footprint which is important due to the
40. ample cuvette 250 mL or larger Nalgene sample bottles Sample waste collection bottle 1 0 L Nalgene sample bottle Container with room temperature potable water for zeroing the analyzer and flushing the sample cell Cleaning Procedure 1 Acid wash the sample cuvette with 1 0 or 0 1 N HCl once per day the frequency of cleaning may be relaxed depending on scaling conditions and the number of samples being analyzed each day Draw in the acid and let sit for approximately 2 minutes Eject the acid from the sample cuvette and flush with water If samples are not going to be analyzed immediately draw water into the cuvette and let remain until samples are to be tested Otherwise proceed with sample testing procedure When ejecting acid into the waste collection bottle make certain the bottle has been thoroughly washed with water to avoid HS generation Set Zero Procedure l 2 Fill a sample bottle container with water Fully compress the pipetting bulb and then insert the tubing into the water Draw the water into the cuvette by slowly releasing the bulb Allow the bulb to hang freely when uncompressed fully expanded Select touch Set Zero on the Operator Screen After a 2 minute count down the analyzer will scan acquire spectrum the water The Zero has now been set The baseline has been set and the internal spectrometer optical alignment has been checked Eject the water into the sample wast
41. analysis activities internal components need to reach thermal equilibrium and stabilize DURALYZER MIR Benchtop Analyzer by HODGES LIU BOOTING Wait Figure 4 1 LCD BOOT screen 4 3 Normal Operation Normal operation of the DURALYZER NIR laboratory liquor analyzer is comprised of two steps 1 deliver sample to cuvette and 2 analyze the sample A step by step normal operating procedure is in Appendix A 5 Normal Operating Procedure Before performing any analysis the analyzer must be powered on for a minimum of 2 hours 12 or more hours would be ideal Once powered on the analyzer should only be R E Hodges LLC 12 DURALYZER NIR Laboratory Liquor Analyzer Manual turned off when it is being moved to another location or serviced Initially operation will be outlined using the default settings from REH LLC Procedures concerning calibration model tuning and configuration settings are detailed in subsequent sections The LCD should reflect Figure 4 2 at this point showing the Operator Screen Operator Screen CH Sample Point PT 1 Analyze IP J peer pr ample PORT Sample Sample Point PT 4 e Q s Sample Point PT 5 ES Print Results Sample Point PT 6 kj Auto Zero CH Sample Point PT 7 Units LEFIDOGAL iQ Sample Point PT 3 Analysis Results Last Analysis EA MAOH II AA TI HAS TTA HMA2COS MA2SO4 Il WCAUISTICITY TDS
42. ans are averaged and a settling time of 120 seconds is used Black liquor samples may need 5 or more R E Hodges LLC 22 DURALYZER NIR Laboratory Liquor Analyzer Manual scans to be averaged and 180 to 300 seconds of settling time The settling behavior and nature of each liquor sample will dictate the optimal scan parameters used at a particular mill Figure 4 20 illustrates custom scan parameters applied to all eight sample points Scan Parameters 1 E ra Pa So po eil ma o E ra EF Pa eil Emsi Kei Kei ra o EG A MA ES oN oO D bk HM gt Update Figure 4 19 Scan Parameters screen with default values for each sample point Scan Parameters 1 300 300 200 o o 300 Pay fa CH o D 3 r3 o M LM LE CP P me ee ccr A LT Update Figure 4 20 Custom scan parameters applied to each sample point Selecting the Password option form the Main Menu allows the user to change the current password The analyzer ships with the default password ADMIN Consider the case where the current password is TIGERS Figure 4 21 The current password is shown on the left and the new password is entered on the right by selecting the box and entering the new password on the virtual keyboard If the new password chosen is LIQTEST the Change Password screen will appear as shown in Figure 4 22 Press the Update to save the new password
43. atory Liquor Analyzer Manual to the Main Menu A From the Main Menu 4 MODBUS is selected and the MODBUS settings are entered on the MODBUS Configuration screen 5 Screen 5 is divided into steps A through G Once the settings have been entered A F select Update G for the changes to take effect Table A 11 1 MODBUS Register Addresses MODBUS Register Addresses AXXXX Register Register Description Register Description 40000 EA REA Word 40045 EA REA Word 40090 EA REA Word 40001 AA RAA Word AA RAA Word AA RAA Word 40002 TTA Word TTA Word TTA Word 40003 TDS Word TDS Word TDS Word D 40004 TDD Word m TDD Word EN TDD Word d 40005 TDO Word amp TDO Word S TDO Word S 40006 NaSO Word Na SO Word Na SO Word 40007 NaSO Word v NaSO Word NaSO Word P 40010 Sample Temperature Word y Sample Temperature Word E Sample Temperature Word A 40011 Reserved Word Reserved Word Reserved Word 40012 Reserved Word Reserved Word 40013 Reserved Word Reserved Word 40014 Reserved Word Reserved Word Reserved Word 40015 40060 EA REA Word 40105 EA REA Word 40016 AA RAA Word 40061 AA RAA Word 40106 AA RAA Word 40017 40062 TTA Word 40107 TTA Word 40018 TDS Word 40063 TDS Word 40108 TDS Word 40019 e 40064 TDD Word b 40109 TDD Word se 40020 TDO Word amp 40065 TDO Word S 40110 TDO Word amp 40021 Na SO Word 40066 Na
44. caling conditions and the number of samples being analyzed each day Acid is drawn into the cuvette in the same manner as water or a liquor sample and allowed to sit in the cuvette for 2 minutes The acid is then ejected into the waste collection bottle and flushed with water Make certain the waste bottle has been thoroughly washed with water before ejecting the acid to avoid H5S generation As a general guideline each sample point should consistently be tested in the same 10 C window for optimal results i e maintain consistent conditions under which each sample is tested If this is a recurring problem samples can be capped and placed in a water bath For example place the capped samples in a large container in a sink fill with tap water and allow the water to overflow for 2 minutes Remove the samples from the water bath and proceed with testing This is detailed in the Normal Operating Procedure in Appendix A 5 4 4 Settings 4 4 1 Accessing the Main Menu Additional information and the ability to customize the analyzer settings can be accessed by selecting About on the Operator Screen Figures 4 2 4 5 At this point an informational screen appears Figure 4 6 displaying the company logo and the telephone number for support Selecting OK will return the user to the Operator Screen Touching the trademark gray shaded region in Figure 4 6 will access a virtual keyboard on the LCD screen Figure 4 7 The QWERTY vi
45. cid cleaning the cuvette This can be done manually outlined above or by selecting the auto zero check box see Figure 4 2 When sitting idle water is to be in the cuvette at all times The auto zero function takes advantage of this setting the zero every 2 hours Before analyzing a liquor sample place the silicon tube in a sample waste bottle and eject the water Hold the pipetting bulb in an upright elevated position and squeeze Do this several times to thoroughly evacuate the water note the silicon tubing should be held while doing this to avoid the possibility of uncontrolled spray Fully compress the pipetting bulb and place the silicon tubing in the liquor sample Draw the liquor into the cuvette by slowly releasing the bulb and then let it hang freely Select the sample point for testing and Analyze Sample on the Operator Screen Figure 4 2 The current status of the LCD screen is reflected in Figure 4 4 Scanning is delayed 120 seconds default value to ensure the sample is stabilized the delay can be bypassed by selecting continue The message at the bottom of the screen will change when the sample is being scanned spectrum acquired Analyzing Sample Analyzing Sample Testing in 120 s Figure 4 4 Analyze Sample screens Operator Screen CH Sample Point GREEN Lo Analyze Help CH Sample Point CLAR GREEN LIG CH Sample Point I CAUST sample CH Sample Point 3 CAUST e GO Samp
46. cizing Efficiency Digital Control System Effective Alkali Potassium Chloride Liquid Crystal Display Modicon Communications Bus Sodium Carbonate Sodium Sulfide Sodium Thiosulfate Sodium Sulfite Sodium Sulfate Sodium Chloride Sodium Hydroxide National Electrical Manufacturers Association Near Infrared Quartz Tungsten Halogen Residual Active Alkali Reduction Efficiency Residual Effective Alkali R E Hodges LLC Remote Terminal Unit Scandinavian Pulp Paper and Board Testing Committee Stainless Steel Technical Association of the Pulp and Paper Industry Transmission Control Protocol Total Dissolved Dead Load Total Dissolved Solids Total Dissolved Organics Thermoelectric Cooler Total Titratable Alkali Volts Alternating Current Second Order Calibration Curve Parameter First Order Calibration Curve Parameter Offset Calibration Curve Parameter Volume of Sample Bias Offset Parameter Bias Slope Parameter Mass of sample Bias Adjusted Analyzer Value Curve Corrected Analyzer Value Analyzer Water Zeroed Value Prior to Curve Correction Raw Analyzer Value Prior to Water Zero and Curve Correction Density m V R E Hodges LLC 42 DURALYZER NIR Laboratory Liquor Analyzer Manual Appendix A 3 Useful Equations EA AA TTA NaOH NaS Na2CO Sulfidity TT A basis mass of solids EA NaOH Na S AA NaOH Na S TTA NaOH Na S Na CO NaOH 2EA AA Na S 2 AA EA
47. ding will be 16 unless the DCS interprets the higher order bit as a sign bit in which case it will be 15 Register Offset will be O if register 1 is address O for the MODBUS driver used by the DCS otherwise this will be 1 or 1 some devices refer to address instead of register number R E Hodges LLC 75 DURALYZER NIR Laboratory Liquor Analyzer Manual nuaw uiDw buipoauz 33634u reste amp saysibay LDu1 10 4 qi 8ADIS tee eee eee RAR jows04 DMa3JDO Y q35010002 600 Zei HAE He He HE jow 10 4 SS931PPY dl ys Hee Hee eee DU1J0 4 ASDW Lan Log z 8 25 POs 0 39 L6 022 ALIOLWIS 96 4 ALIOLLSNWO L1H8S1 002VN 96222 SZYN 589 t9 HOYN 60 90 10 60 1d tis jouy 450 NOU ONAMLX3 3o02 43ddn HE OU 3LIHM IO 1S0w2 8 29800 Wit ize 28 vv L 96542 va synsoy sisApouy Toon SHUN 0182 orny D Syinsay jud A ajdwos ua3125 J0 D1300 2500 99 PEE uoddns 277 sebpoy 3 Y Aq JezAjeuy doyu ueg Nu 8M REITER Figure A 11 2 Menu sequence for MODBUS configuration Figure A 11 2 illustrates the menu navigation for entering the MODBUS configuration settings is selected and screen 2 t Abou Starting from the Operator Screen 1 appears Pressing TM brings up screen 3 to enter the password which allows access 76 R E Hodges LLC DURALYZER NIR Labor
48. djusted to match the lab test method results in a least squares sense The seven models are as follows EA REA for black liquor AA RAA for black liquor TTA Na5S0 4 TDS TDD TDO Certain measurements may not be required for a given application of the analyzer In which case determining a calibration curve for that model would be unnecessary For example if there is not an interest in Reduction Efficiency then there is not a need for a sodium sulfate calibration curve Likewise TDO total dissolved organics would only have meaning for black liquor samples Y DU Pa y pir For automated determination each calibration curve will be represented by the second order polynomial given by Equation A 7 1 x Ax2 Bx C A 7 1 Constant curve parameters A and B are determined by the automated calibration curve procedure x is the curve corrected measurement value and x is the raw analyzer value prior to water zeroing curve correction and bias adjustment Both x and x a must be in lb 100gal as Na20 The base units for the EA AA TTA and Na2SO4 models are Ib 100gal Water sets the zero value for each curve which is the C parameter in Equation A 7 1 Each calibration model will have its own set of A B and C curve parameters Samples Follow the Normal Operating Procedure Appendix A 5 relating to preparing and drawing samples into the cuvette At a minimum two liquor samples and one water sample 3 tot
49. e Normal Operating Procedure Appendix A 5 for analyzing the samples At a minimum three liquor samples are required to determine the bias adjustment for a particular sample point Water is not used when determining bias adjustments If the current lab testing method in place produces less than desirable repeatability more than three liquor samples will be required It is important to note that all samples need to be tested using the same method and by the same person This eliminates potential of conflicting biases being introduced into the lab values Special care should be taken when performing the lab tests to ensure the highest possible precision in the measurement values Procedure 1 Make sure the analyzer has been powered on for a minimum of 2 hours 12 hours recommended to allow for the analyzer to reach thermal equilibrium and stabilize If calibration curves are to be used perform that procedure before attempting any bias adjustment Set the desired analyzer display units and make sure the current bias values are set to the default values slope 1 and offset 0 See Sections 4 4 3 and 4 4 4 respectively 2 Collect all liquor samples that will be required for determining the bias adjustment for a particular sample point 3 Perform the necessary laboratory tests on the collected samples The tests will yield the LAB values R E Hodges LLC 63 DURALYZER NIR Laboratory Liquor Analyzer Manual 4 After lab testing
50. e bottle by holding the bulb in an upright position and compressing squeezing several times to eject all the water The tubing should be held or secured when doing this to avoid the possibility of uncontrolled spray Note if samples are not to be analyzed immediately leave the water in the cuvette i e do not eject the water until ready to test samples The Zero should be set at least once per day and every time following an acid cleaning or after powering on the analyzer Sample Testing Procedure 1 Collect all samples to be tested from the field Samples need to be large enough to allow for at least a 200 mL viable sample after any settling or filtering see below R E Hodges LLC 45 DURALYZER NIR Laboratory Liquor Analyzer Manual 10 11 For slurry samples such as the No 1 causticizer and raw green liquor samples allow ample settling time before transferring the settled clear liquor to a new clean 250 mL sample bottle For black liquor samples containing chip and or fiber debris pour the sample through a 100 mesh strainer into a new clean 250 mL sample bottle This will remove all of the debris that could possibly interfere with the analysis Optional Samples can be capped and placed in a water bath to bring them closer to room temperature Place the capped samples in a large container such as a pot Put the large container in a sink and fill with tap water Keep the water running and al
51. e laboratory autotitrator At a minimum titration acid and pH standards as well as precision volume measuring equipment are still required Most autotitrators are based on the SCAN Scandinavian Pulp Paper and Board Testing Committee method This method differs from the TAPPI standard ABC titration test in that formaldehyde and barium chloride are not used Instead a pH curve is generated R E Hodges LLC 2 DURALYZER NIR Laboratory Liquor Analyzer Manual as a function of the added titration acid The inflection points on the titration curve are used to estimate the EA AA and TTA values of the liquor sample Problems can arise from difficulties in pinpointing the inflection points especially for the AA The inflection point locations can vary with changes in dead load concentrations leading to erroneous concentration estimates This effect is especially pronounced on the AA inflection point 1 3 Specifications The general specifications of the DURALYZER NIR laboratory liquor analyzer are contained in Table 1 2 Certain specifications may differ from Table 1 2 if unique installation and operating conditions require deviation from the standard setup Table 1 2 General Specifications Analyzer Internal Operating 40 C Temperature Sample Cuvette Fused Silica 1 0 mm path length Connections Power Input 120 240 VAC 1 6A 50 60 Hz R E Hodges LLC 3 DURALYZER NIR Laboratory Liquor Analyzer Manual 2
52. e of setting the time and date If the MODBUS communications interface is to be utilized configure it by selecting MODBUS on the Main Menu This will pull up the MODBUS Configuration screen shown in Figure 4 18 with example settings The settings on this screen are used to configure the MODBUS TCP interface to the analyzer Simply touch the box to be edited and enter the new value using the virtual LCD keyboard Entries must conform to the format displayed above each box A detailed description of this interface and how to configure it is documented in the Appendix A 11 MODBUS MODBUS Configuration IP Address Net Mask Format Format ygccgsgsygsgy ss tate tata gy PPS Gateway Slave ID Format Format IERE PEE ea ae eae IPEF Integer Register Encoding Offset I I gz a H m Figure 4 18 MODBUS Configuration screen Adjusting the number of spectral scans to be averaged and the settling time for sample analysis is accomplished by selecting Scan Params on the Main Menu Custom scan parameters can be specified for each sample point Figure 4 19 shows the Scan Parameters screen with the default values of 1 and 120 for each sample point The left column specifies the number of scans spectra to average for a sample analysis and the right column specifies the settling time in seconds for the sample once it has been drawn into the cuvette Typically for white and green liquor 2 to 3 sc
53. ed a layer of corrosion Out of paper Replace paper roll Appendix A 9 Printer needs cleaning Clean printer Appendix A 9 LCD 1 ti ble not E See Re IP n Disconnect and reconnect LCD panel cable plugged in properly PER ile conection pins have Clean connection pins of cable developed a layer of corrosion Analyzer needs to REBOOT Switch analyzer power OFF wait 15 seconds switch power ON Inspect tubing and cuvette for obstruction or Ber buildup clean or replace if necessar Flow restriction P P y Inspect pipetting bulb clean or replace if necessary Cuvette needs to be acid cleaned Acid clean cuvette Appendix A 5 E mers tesla longer an Adjust scan parameters Sec 4 4 3 cuvette Ensure bulb is secure in holder and wire connection is secure and making good contact Caution light source and holder will be HOT Light source may be nearing end of Check bulb intensity and replace if necessary lifespan Appendix A 10 Light source bulb or connection may be loose Table A 12 1 is a troubleshooting guide for some problems that are easily remedied Other problems could arise that will likely be hardware related and require servicing by R E Hodges LLC R E Hodges LLC 78 DURALYZER NIR Laboratory Liquor Analyzer Manual Appendix A 13 Replacement Parts PART Enclosure Key LCD Control Panel MODBUS Com Device NIR Light Source Pipetting Bulb Printer Printer Cable Printer Paper
54. el Measurement Technique Direct volumetric analysis based on pH titration curve relating NIR spectral signature to SCAN method chemical composition Potential volumetric errors difficulties in pinpointing Measurement Accuracy Factors inflection pts especially for Paes Analysis Speed Slow minutes to 10 s of minutes Stow minutes to 108 of minutes minutes to 10 s of minutes Fast 20 to 60 seconds Moderate acid replacement pH Low annual light source Low maintain glassware and Maintenance probe calibration occasional lab replacement occasional lab chemicals validation validation Potential volumetric errors no volumetric errors The standard ABC titration test requires multiple chemicals and lab equipment to implement Titration chemicals such as certified hydrochloric acid solution formaldehyde barium chloride and various color indicators can be inconvenient in terms of cost and space to maintain in the process testing lab If a pH probe is used to monitor the titration then pH standards must also be kept on hand to calibrate the probe In addition to the chemical requirements precision volume measurement equipment for the sample and titration acid must be maintained in good working order and periodically calibrated Bench top laboratory autotitrators have been implemented to automate the actual titration test However most of the same issues associated with the standard ABC test are also present with th
55. ence to the standard titration test and is depicted in Figure 4 13 Component Labels EA AA TTA Ha2504 NA42504 TDS TDS TODS TDD TDO TOO P oH m Update Figure 4 12 Component Labels screen with default values Component Labels EA AA TTA Ha2504 MAS CA TDS TDS TODA TOC TO TDO Update Figure 4 13 Customized EA AA and TTA labels 4 4 3 Configuration Submenus By default measured component values that are not reported on a percentage basis are reported in Ib 100gal as Na20 This can be changed by choosing Display Units on the Main Menu Each measured component value can have custom units defined Referring to Figure 4 14 the left column contains the unit labels for each measured R E Hodges LLC 19 DURALYZER NIR Laboratory Liquor Analyzer Manual component The right column contains the corresponding conversion factor to convert from Ib 100gal as Na20 to the desired units The procedure is analogous to editing the sample point labels Touch the appropriate editable box button and enter the new values Some typical units and conversion factors are given in Table 4 3 An example of editing the measured units from 1b 100gal as Na O to Ib ft as Na O is shown in Figure 4 15 Display Units LI LB 100GAL LAZIOOGAL LBZ100GAL 2 3 4 LB 100GAL 5 6 7 8 10 1 1 0 2 1 0 3 1 0 4 3 1 0 5 6 7 8 10 10 oO 2 HE IO
56. es welcomes any recommendations suggestions or corrections that would serve to improve the quality and utility of this literature R E Hodges LLC lii DURALYZER NIR Laboratory Liquor Analyzer Manual Disclaimer The information given herein including drawings images illustrations and schematics intended for illustration purposes is believed to be reliable and accurate However R E Hodges LLC makes no warranties to its accuracy or completeness and disclaims any liability in connection with its use R E Hodges LLC s only obligation shall be as set forth in R E Hodges LLC s standard terms and conditions of sale for this product and in no way will R E Hodges LLC be liable for any incidental indirect or consequential damages arising out of the use or misuse of this product Users of R E Hodges LLC products should make their own evaluation to determine the suitability of each product for the specific application R E Hodges LLC iv DURALYZER NIR Laboratory Liquor Analyzer Manual Table of Contents Company PIO TL os oi sa d tuta OR tee Ra ii About This Manual ide o o E ie ree RR RE UD PU 111 Td A O iv LISTO iuris vil IE GOR AD ls TEE ix Introduction and Specifications 1 1 1 eege TEE 1 1 2 DURALYZER NIR M vs Current Solutions 2 1 3 SPCCINCAL OMS os 3 2 Prineiple ot Operation uy y u Ene e
57. fficult A detailed listing of environments to avoid is given in Appendix A 4 Setup Cautions The analyzer comes delivered in a foam shell within a reinforced box that should be stored and used to ship the analyzer back to REH LLC if the need arises for any major repairs 3 2 Tubing Connections Silicone tubing and a 60 mL rubber pipetting bulb are supplied to allow for drawing the sample into the cuvette and ejecting it after analysis 8 12 for cuvette to bulb section and 18 22 for sample bottle to cuvette section This was previously mentioned and R E Hodges LLC 9 DURALYZER NIR Laboratory Liquor Analyzer Manual shown in Figure 2 7 Alternatively custom configurations can be employed An example would be a flow through arrangement whereby the sample is poured into a funnel flows downward through the cuvette to a collection container As the sample is flowing the tubing section downstream of the cuvette would be temporarily clamped for the duration of the analysis 3 3 Air and Water Requirements Instrument air is not required for operation Mill water is required for flushing out the sample cuvette and occasional spectrometer baseline referencing Deionized water is not needed unless the mill water is of unusually poor quality If mill water quality is an issue a suitable solution will be proposed 3 4 Power and Wiring Connections The analyzer is equipped with a detachable power cord connectable to any standard
58. gister 126 4 LCD Control Bit Field Register 127 is a read only register 5 Floating Point numbers are encoded in an n bit integer where n is normally 16 but can be changed to a lower resolution if desired 6 Engineering units can be changed to whatever is desired through the LCD touch panel interface Ranges For Floating Point Numbers Parameter Low Val Units Low Int Hi Int AA 0 200 1b 100gal 0 2 1 NaSO 0 200 Ib 100gal 0 2 1 TDD 0 0 2 1 R E Hodges LLC 77 DURALYZER NIR Laboratory Liquor Analyzer Manual Appendix A 12 Troubleshooting Table A 12 1 Troubleshooting Guide PROBLEM POSSIBLE CAUSE SOLUTION Analyzer will not power on Printer not working LCD panel does not power on or display correctly Difficult to draw sample into cuvette Measurements become erratic or unstable heck inserti f d at anal d Power cord not plugged in securely D QUE PA a power switch if blown replace 3 5 A Internal analyzer temperature too high Relocate analyzer to a location with a cooler triggering thermal shut down switch ambient temperature Repower once the analyzer has cooled down Check insertion of power cords at outlet power Power cord not plugged in securely unit and printer Interface cable not connected properl Propet Y Check interface cable connection or securely Interface cable connection pins have a A Clean connection pins on interface cable develop
59. he absorption of the other components Many times such a wavelength does not exist This is an analogous situation to the application of conductivity for measuring effective alkali EA levels in white liquors The white liquor conductivity is affected the most by the EA concentration but the sulfide and carbonate levels also have an affect on the conductivity As a result periodic recalibration of the conductivity meter is required to compensate for the effects of changing sulfide and carbonate levels The DURALYZER NIR analyzers laboratory and online do not have these drawbacks or shortcomings since the measurement is taken over a continual range of wavelengths Material Under Test LGA Entering light intensity for wavelength 4 I A Exiting light intensity for wavelength 4 C C Cy Concentration of species 1 2 N Ep 5 Ey Absorption coefficients for species 1 2 N for wavelength 4 L Path length of sample A A Total absorption for wavelength A Figure 2 5 The Beer Lambert law The general concept is to utilize NIR spectroscopy via a transmission cell or sample cuvette in conjunction with software to determine the chemical composition EA AA TTA TDS and TDD of causticizing process liquor streams Liquor samples are collected and prepared for analysis in the sample multiplexing amp conditioning system Analysis occurs in the transmission s
60. if necessary For further details concerning light source replacement refer to Appendix A 10 NIR Light Source Replacement Figure 4 37 NIR light source removal Certain other unscheduled maintenance tasks may occur over the operational lifetime of the analyzer These will be relatively simple and covered in Appendix A 12 Troubleshooting Any significant maintenance or major analyzer component replacement would have to be performed by R E Hodges LLC Any repair or maintenance performed on the analyzer that has not been explicitly discussed in this manual will void the warranty R E Hodges LLC 33 DURALYZER NIR Laboratory Liquor Analyzer Manual Appendix R E Hodges LLC 34 DURALYZER NIR Laboratory Liquor Analyzer Manual Appendix A 1 Dimensions and Additional Images DURALYZER NIRM Figure A 1 1 DURALYZER NIR laboratory liquor analyzer dimensions R E Hodges LLC 35 DURALYZER NIR Laboratory Liquor Analyzer Manual TM DURALYZER NIR Benchtop Analyzer 614 by R E Hodges LLC Support 334 466 0057 Z 12 935 Figure A 1 2 LCD panel dimensions R E Hodges LLC DURALYZER NIR Laboratory Liquor Analyzer Manual Figure A 1 3 Printer dimensions R E Hodges LLC 37 DURALYZER NIR Laboratory Liquor Analyzer Manual DURALYZER NIR Laboratory Liquor Analyzer Thermal Printer
61. ight source holder and tighten the set screw Power on the analyzer and replace the enclosure cover Allow the new bulb to stabilize for at least 2 hours Utilize the New Bulb function from the Main Menu to test for detector saturation Adjust the bulb position in the light source holder if necessary Power On Off Switch NIR Light Source Enclosure SNA ge ie le Further Details Figure A 10 1 Power switch and light source enclosure locations R E Hodges LLC 71 DURALYZER NIR Laboratory Liquor Analyzer Manual NIR Light Source Enclosure QTH NIR Light Light Source Holder Source Figure A 10 3 NIR light source removal R E Hodges LLC 72 DURALYZER NIR Laboratory Liquor Analyzer Manual Replacement of the NIR light source QTH light bulb with reflective coating may require a slight adjustment after installation The New Bulb function on the Main Menu will access the New Bulb Adjustment screen After the bulb has been replaced draw water into the sample cuvette Select the Trigger Scan option on the left side of the screen to check if the new bulb saturates the detector Figures A 10 4 and A 10 5 show a water scan without saturation and a water scan in which the detector is saturated An unsaturated water scan Figure A 10 4 indicates the replacement bulb is positioned and functioning correctly If the water scan resembles the spectrum shown
62. in Figure A 10 5 top portion of the two peaks are cut off meaning transmission has reached 100 the detector is saturated Detector saturation occurs even if only one wavelength is 100 The desired transmission is between 75 and 85 for the highest spectral peak The remedy for detector saturation is to slightly reposition the bulb by rotation and or relative location in the light source holder Menu sequencing for the New Bulb function is shown in Figure A 10 6 New Bulb Adjustment q Lata m E beta FE a ee iced 60 GE ec lt a GE sel Trigger x i i Scan d A5 i Geen betta peu E C E m i i Ez B etes iod 18 20 22 wavelength um Figure A 10 4 Unsaturated water spectrum Hew Bulb Adjustment 18 0 22 wavelength um Figure A 10 5 Saturated water spectrum R E Hodges LLC 73 DURALYZER NIR Laboratory Liquor Analyzer Manual Case J i WEA Dessen suma 0095 sneaow J ueos buuebBu 1 nuaw uiDw Logz Z8 345 w0 0 39 66022 ALIGIS 9662 AAD15058 1F8 S1 Son GO IR Ka 1585 9 HOYN LeS6 52 v3 60 60 10 82 60 S Ld mu 4507 Spnsey sisAppuy NOLDVALX Tom 91 SUN WOO2 UBddN 0182 ony A soo sar vee voding yg ch sinsaa jud A entero dian azAjouy Y Jaz jeuy doyyoueg FUERO N U3319S J0 D1300 74 Figure A 10 6 Menu sequence for the New Bulb function R E Hodges L
63. le As with the water the analyzer values will be displayed under the Scan button Do not be R E Hodges LLC 59 DURALYZER NIR Laboratory Liquor Analyzer Manual concerned if the analyzer values look odd possibly negative numbers The calibration procedure will take care of positioning the calibration curve and adjusting its shape 8 Enter the available lab measured values for sample 1 by pressing the corresponding button to the immediate right of the component If a value is not available for a particular component NA must be entered Entered concentration values must be in units of Ib 100gal as Na O These are the base units for the EA AA TTA and Na2S0 calibration models Conversion factors are provided on the Help screen for some commonly used units 9 Repeat steps 6 8 until all of the calibration samples have been processed 10 Entered lab test values can be reviewed for any sample by by pressing the corresponding button Samples can also be rescanned if needed by selecting the corresponding sample button at the top of the screen drawing the sample into the cuvette and then pressing Scan 11 After all collected samples have been processed select Calibrate at the bottom of the screen New Curve Slope and Offset values will be calculated and displayed along with the correlation coefficient Additionally a hard copy summarizing the calibration data and results will be
64. le Point CLAR WHITE LIG tg Print Results Sample Point WEAK WASH M Auto Zero CH Sample Point LIPPER COOK Analysis Results Last Analysis PT 5 09 33 0105 09 EA 75 853 MASH 64 585 AA 37 321 Maes 22 736 TTA 103 162 MA2COS 15 841 MA2SO4 3 174 SCALISTICITY 73 963 TDS 20 816 Ze 22 039 WTEC 7 005 80 304 TDO Update MODBUS 001 M Saz Fab 750 Figure 4 5 MEE results R E Hodges LLC BE 14 DURALYZER NIR Laboratory Liquor Analyzer Manual After scanning is complete the Operator Screen will update to display the analysis results Figure 4 5 is an example for a clarified white liquor sample Checking the Print Results box enables the results to be printed out via the thermal printer If the MODBUS communications interface is being employed select the Update MODBUS option on the screen to send the results to the appropriate registers Flush the sample cuvette with water and eject into the waste bottle Draw water into the cuvette letting it remain until the next round of liquor testing Items such as labels and display units can be customized edited to suit the user Customization options are detailed in the following section Periodically the sample cuvette needs to be cleaned with 1 0 N or 0 1 N HCl acid The frequency of cleaning is initially suggested to be once per day However it may end up being more infrequent depending on the s
65. lectromagnetic spectrum related to optical spectroscopy NIR spectroscopy has many attractive features that make it ideally suited for process analysis Key features include minimal sample preparation remote sensing through the use of fiber optic cables and simple implementation using relatively inexpensive and highly robust components There are a variety of optical attachments available to interface a NIR spectrometer to a sample for collection of spectral information The most common attachments used for liquid analysis are a transmission cell and a sample cuvette The basic configuration of a transmission cell is illustrated in Figure 2 2 Figure 2 3 depicts a sample cuvette R E Hodges LLC 4 DURALYZER NIR Laboratory Liquor Analyzer Manual Liquid Sample Outlet Optical Coupler Fiber Optic Cable Halogen QTH to Spectrometer NIR Light Source Figure 2 2 Basic transmission cell configuration Liquid Sample Inlet lt Em x fog 3 r D APP DP NEC D foh out id E e EA ER 4 x b Pug G o Path Length L Fused Silica Sample Cuvette Liquid Sample Outlet Figure 2 3 Sample cuvette The transmission cell allows NIR radiation to interact with the sample while isolating the light source fiber optic cable and spectrometer from the process A typical transmission cell is composed of a body with appropriate sample inlet and outle
66. ll take more time the cooler the sample is Next test all three samples using the standard laboratory test procedure for sodium sulfate in green liquor Determination of the TDS calibration curve parameters can be carried out using white green and black liquors A convenient relationship for calculating TDS in white and green liquor is depicted in Equation A 7 2 TDS p 1 000 10096 A 7 2 The density o is in g cm and can be measured by a handheld density meter or by a gravimetric method At room temperature measure out a precise volume of sample V R E Hodges LLC 58 DURALYZER NIR Laboratory Liquor Analyzer Manual in mL then determine the mass m in grams The black liquor TDS is usually measured by a moisture analyzer or by oven drying Only green and white liquor samples are used to calculate the TDD calibration curve Lab values for TDD can be calculated from the following equation if the EA AA TTA p and TDS values are known pas ee O 70 A 7 3 p 1000 0 834 Density o is in g cm whereas NaOH NaS and NazCO 3 are in 1b 100gal as Na2O Determining the TDO calibration curve requires black liquor samples with a known TDS A precisely measured mass of black liquor is dried and burned in a furnace to measure the total dissolved organics The TDO is computed by Equation A 7 4 A 7 4 TDO TDS k mass of burned d 100 mass of wet sample Procedure 1 Make su
67. lly measured by a moisture analyzer or by oven drying Only green and white liquor samples are used to calculate the TDD calibration curve Lab values for TDD can be calculated from the following equation if the EA AA TTA p and TDS values are known TDD TDS ee O 70 A 6 3 p 1000 0 834 Density o is in g cm whereas NaOH NaS and Na2CO are in 1b 100gal as NaO Determining the TDO calibration curve requires black liquor samples with a known TDS A precisely measured mass of black liquor is dried and burned in a furnace to measure the total dissolved organics The TDO is computed by Equation A 6 4 A 6 4 TDO TDS cs mass of burned 3 100 mass of wet sample Procedure 1 Make sure the analyzer has been powered on for a minimum of 2 hours 12 hours recommended to allow for the analyzer to reach thermal equilibrium and stabilize Confirm that Curve Slope and Offset on the Component Curves Slopes and Offsets screen are set to 0 1 and 0 respectively for each component model requiring a calibration curve Do the same on the Edit Bias Values screen setting the Slope and Offset to 1 and 0 respectively this must be done for each sample point Accessing these screens was detailed in Section 4 4 5 Model Tuning Submenus It is also helpful to set the display units to Ib 100gal for EA AA TTA and NasSO4 refer to Section 4 4 3 Configuration S
68. low the water to overflow from the container for at least 2 minutes before removing the sample containers from the water bath and proceed with testing Cooling the samples can stability and repeatability in the analysis results As a general rule of thumb each sample point should consistently be tested in the same 10 C window for optimal results If the Auto Zero function is being used uncheck the corresponding box on the Operator Screen to disable the function until sample testing is complete Select touch the circle next to corresponding sample point for testing on the Operator Screen If water is still in the cuvette eject into the sample waste bottle by holding the bulb in an upright position and compressing squeezing several times to eject all the water The tubing should be held or secured when doing this to avoid the possibility of uncontrolled spray Fully compress the bulb and then place the sample pickup tube in the sample bottle corresponding to the sample point selected in step 6 With the tube in the sample bottle slowly release the bulb until completely expanded and then allow it to hang freely Make certain that the end of the sample pickup tube is not in contact with the bottom of the bottle in a manner that will interfere with suction of the sample For slurry samples the very bottom should be avoided if a detectable amount of residual lime mud has settled For black liquor samples ensure the pickup tube end is
69. m the Operator Screen 1 About is selected and screen 2 parameters 53 R E Hodges LLC DURALYZER NIR Laboratory Liquor Analyzer Manual appears Pressing TM brings up screen 3 to enter the password which allows access to the Main Menu 4 From the Main Menu 4 Slope Offset is selected and the calibration parameters are entered on the Component Curves Slopes and Offsets screen 5 Screen 6 shows the parameters determined in Example A 6 1 Once the curve parameters have been entered select Update on screen 6 for the changes to take effect Table A 6 1 Comparison of analyzer values with lab values EA AA NN as oo ooo oo 000 000 09 ME War 0 00 000 00 0 00 009 000 Water um 000 000 000 000 000 SAMPLE Daer 000 000 000 PESO EA s War Units in Ib 100gal as Na O R E Hodges LLC 54 DURALYZER NIR Laboratory Liquor Analyzer Manual Table A 6 1 compares the analyzer values before and after curve correction with the measured lab values The water zeroed analyzer values are listed under NIR calibration curve corrected values are listed under CC and the laboratory measured values are listed under LAB This illustrates the effectiveness of the calibration curve in its ability to tune the base calibration models to lab measurements Example A 6 2 g L as Na 0 Ib
70. nint 4 2 1 CONO P AS oo 4 22 ee Te EE 8 ISA HOME update et Fe c dde Dun well tases ento dot hens 9 3 1 Gene alu nam amaya tunu m m pam E aoa m crim cam dE M ET DE 9 2 Nube Connections enee 9 3 3 Air and Water Requirements EE 10 3 4 Power and Wiring Connections essere enne enne 10 4 Operation and Maintenance 11 4 1 Generals leede 11 4 2 Ar EE 12 4 3 Normal Operation EEN 12 4 4 KE de eb 15 4 4 1 Accessing the Main Mehl a d ERR Ie haem 15 44 2 labeling SUbmen S u cite a u Ee 17 4 4 3 Configuration Submenus esent 19 4 4 4 Informative Submenus eese eene tenente 26 4 4 5 Model Tuning SubIDebus si ee eb sine ENN 29 4 5 Maintenance cuo Uo bu Nl ds iS 31 Ee 34 Al Dimensions and Additional Images 35 22 _NOomenglaf r u u yn eege eras 42 R E Hodges LLC V DURALYZER NIR Laboratory Liquor Analyzer Manual A3 Useful Equations vaa dida 43 A Rs ne ee ai 44 AS Normal Operating Procedure os 45 Ap Manual Calibration Curve Determination Vs 48 AJ Automated Calibration Curve Determination 57 A S Bias Adjustment u qana nasa sasqssnqeaansqashaqasaisasascqisaa 63 A93 Printer D S us Muna SS etu bia ne EN ne 69 A 10 NIR Light Source Replacement ii 71 AJT MODBUS siii 75 A12 Troubleshooting id dit 78 A13 Replacement PATS E Rte L
71. o employ only a slope or offset e In most cases bias adjustment will not be needed if calibration curves are in place e Contact R E Hodges LLC for any further assistance R E Hodges LLC 67 DURALYZER NIR Laboratory Liquor Analyzer Manual Y sDIg Jas 185110 8do S ajogz w stun amp oidsia sjeqo1 duo sid sidwos AM Sw o s Wow A AOR 9 nuaw uiDw 96 ah ALIDUSA IA L1H8S1 002VN oc 22 SZYN 589 t9 HOYN 9654 LE 60 5010 60 e 1d zu 4307 4593 sisApuy NOUOYALX3 1500 esv veE wweddns JO AV OT 3LIHM Met 277 sebpoy uq LSS Ee n JezAjeuy doyu ueg Wi SA GIZA HAT Tro00L 81 SHUN 0182 ony A s nsay jud A ajdwos u33135 J0 D1300 Figure A 8 4 Menu sequence for implementing bias adjustments 68 R E Hodges LLC DURALYZER NIR Laboratory Liquor Analyzer Manual Appendix A 9 Printer Details The DURALYZER NIR laboratory liquor analyzer includes a Star Micronics TSP600 Series Thermal Printer Connection to the analyzer is accomplished via the RS232 port The printer is equipped with its own power unit and power cord which connects to any standard 3 prong outlet Further details not described in this appendix can be found on the Star Micronics webpage Connecting The printer connections should be made in the following order before engaging the power switch located on the lower left side 1 connect to the analyzer
72. on curve procedure x is the curve corrected measurement value and x is the water zeroed analyzer value prior to any curve correction or bias adjustment Both x and xn must be in Ib 100gal as Na O The base units for the EA AA TTA and Na2SO4 models are Ib 100gal There is not a C term in Equation A 6 1 because that has already been incorporated into x by setting the water zero Each calibration model will have its own set of A and B curve parameters Samples Follow the Normal Operating Procedure Appendix A 5 for analyzing the samples At a minimum two liquor samples and one water sample 3 total samples are required for calibration curve parameter determination Due to setting the water zero the analyzer and lab measurement values for water will be 0 0 and 0 0 If the current lab testing method in place produces less than desirable repeatability more than two liquor samples will be required It is important to note that all samples need to be tested using the same method and by the same person This eliminates potential of conflicting biases being R E Hodges LLC 48 DURALYZER NIR Laboratory Liquor Analyzer Manual introduced into the lab values and ultimately will yield a less than optimal calibration curve Special care should be taken when performing the lab tests to ensure the highest possible precision in the measurement values For example past experience has shown that using an autotitrat
73. or for the white liquor ABC test and manual titration for the green liquor ABC test is not a good idea If this is the standard treatment at a mill run the green and white liquor tests for curve parameter determination on the autotitrator After the calibration curves are set and in use go back and run manual tests on the green liquor and make any adjustments by using the Set Bias function on the LCD panel Main Menu Details on setting biases can be found in Section 4 4 5 and Appendix A 8 For EA and AA a white liquor and a green liquor sample is recommended to determine the curve parameters A weak wash sample and or a black liquor sample can be used as well The important idea is to have samples that give values across a wide range and between the upper and lower values i e green liquor EA and AA falls between water and white liquor Black liquor with very low REA or high organic and soap content is not ideal for curve parameter determination In this case any black liquor measurement adjustments should be made through the Set Bias function If there is only a white liquor sample available then a white liquor sample may be diluted to form a second liquor sample A one part white liquor to one part water dilution ratio would work fine and yield an EA and AA value roughly half of the undiluted sample The dilute sample must still be tested to obtain a precise lab measurement value do not assume it is exactly half the undil
74. ough vinegar can be used as well The cleaning frequency will depend on the amount of use and nature of the samples being analyzed Initially acid clean the cuvette once per day and adjust the frequency up or down if necessary Acid is drawn into the cuvette in the same manner as water or a liquor sample and allowed to sit in the cuvette for 2 minutes After 2 minutes eject the acid into the waste collection bottle and flush with water R E Hodges LLC 31 DURALYZER NIR Laboratory Liquor Analyzer Manual Make certain the waste bottle has been thoroughly washed with water before ejecting the acid to avoid H2S generation This procedure is summarized in Appendix A 5 Normal Operating Procedure The analyzer cabinet and LCD panel should be cleaned monthly or whenever there is noticeable dust moisture etc present Simply wipe the stainless steel cabinet with a moist cloth or paper towel A mild cleaner can be used as well When cleaning the LCD panel disconnect it from the analyzer Use a soft dry cloth for the actual screen the LCD panel housing may be cleaned similar to the cabinet The presence of accumulated dust will adversely affect printer performance possibly causing the printout to be unreadable or not to function at all Cleaning the printer is a three part process 1 Cleaning the thermal head 2 Cleaning the paper holder and 3 Cleaning the paper housing Care must be taken when cleaning the thermal head since it is eas
75. own in Figure 2 5 According to Beer s law light intensity decays exponentially as it passes through the material The rate of decay depends on the concentrations of the constituent species of the material and their corresponding absorption coefficients The total amount of decay depends on the length of material the light crosses Equations describing this phenomenon are displayed within Figure 2 5 Total absorption at a particular wavelength can be computed by applying a logarithm to the initial equation The key observation to be made from this equation is that absorption A at a particular wavelength varies linearly with the concentrations of the constituent species Cx With the path length L fixed by the transmission cell the absorption coefficients ec depend only on the wavelength 7 and the molecular structure of species k in the material under test Thus the absorption will change only when the concentrations of the constituent species change Additionally absorption at a particular wavelength depends on the concentration of all of the species that make up the sample under test This is a major drawback for single wavelength instruments that are used to analyze multi component R E Hodges LLC 6 DURALYZER NIR Laboratory Liquor Analyzer Manual materials With these instruments the best that can be done is to select an observation wavelength that is highly absorbed by the component of interest while simultaneously minimizing t
76. printed out provided the printer is connected and powered on 12 Review the results If necessary make changes such as rescanning a sample or changing entered values Press the Calibrate button again to generate updated calibration curves if any changes were made 13 Once the calibration curve procedure is complete press the Back button to return to the Main Menu screen The calibration curve parameters can be accessed and viewed by selecting Slope Offset from the Main Menu Figure A 7 illustrates the menu navigation for automated calibration curve determination Starting from the Operator Screen 1 About is selected and screen 2 appears Pressing TM brings up screen 3 to enter the password which allows access to the Main Menu screen 4 From the Main Menu 4 Calibrate is selected and the calibration parameters are calculated using the Calibrate Curve Slope and Offset screen 5 The current sample is selected at A and then scanned B After the NIR spectrum has been acquired the lab measured values are entered C Once all of the collected samples have been processed Calibrate is pressed D Understanding of the inner workings of the automated calibration curve determination can be reinforced by examining the examples in Appendix A 6 Manual Calibration Curve Determination This basically illustrates the calculations that occur behind the scenes in the automated procedure The examples al
77. ration values must be in units of Ib 100gal as Na20 These are the base units for the EA AA TTA and Na2SQ calibration models e Contact R E Hodges LLC for any further assistance R E Hodges LLC 62 DURALYZER NIR Laboratory Liquor Analyzer Manual Appendix A 8 Bias Adjustment Background Another method for tuning of the DURALYZER NIR laboratory liquor analyzer measurements is implementing bias adjustments Bias adjustments can be used in conjunction with calibration curves or as a standalone tuning method Every measured component for each sample point can have a scale and or offset correction to bias the analyzer in order to match the manual lab tests performed onsite If calibration curves have been generated and are in use the bias corrections will usually be minimal or nonexistent Bias adjustment is represented by the following equation x Sx S A 8 1 where x is the bias corrected adjusted value x is the calibration curve corrected value S is the bias slope and S is the bias offset S and S are the bias adjustment parameters Both x and xec are in the current display units unlike calibration curves which must be determined based on 1b 100gal Bias adjustments can be applied in three ways 1 slope and offset 2 slope only So 0 and 3 offset only S 0 The data will dictate the best choice Two examples are presented to highlight the bias adjustment procedure Samples Follow th
78. re the analyzer has been powered on for a minimum of 2 hours 12 hours recommended to allow for the analyzer to reach thermal equilibrium and stabilize 2 Collect all liquor samples that will be required for determining the calibration curve parameters 3 Perform the necessary laboratory tests on the collected samples The tests will yield the LAB values 4 After lab testing is complete access the Main Menu and select Calibrate to open the Calibrate Curve Slope and Offset screen Once the calibration procedure has been started do not exit the Calibrate Curve Slope and Offset screen until the procedure is completed Otherwise sample spectral data and component values will be lost 5 Test the collected samples on the DURALYZER NIR laboratory liquor analyzer following basically the same procedures set forth in Section 4 3 and Appendix A 5 Start with the water sample make sure Water is selected on the top section of the screen With water in the sample cuvette press the Scan button The current Curve Slope and Offset values for each component curve will be displayed For the water sample zeros are preloaded for each component Do not change these values 6 Eject the water sample and move to the next calibration sample by selecting Sample 1 at the top of the screen 7 Draw the sample into the cuvette as outlined in the Normal Operating Procedure Press the Scan button to analyze the samp
79. rtual keyboard allows upper case letters numerals and some standard symbols to be input Spacebar and lower case functionality is not available The dash may be used in lieu of a space To gain access to the Main Menu Figure 4 8 type in the password and select Enter The default password is ADMIN and can be changed by the end user R E Hodges LLC 15 DURALYZER NIR Laboratory Liquor Analyzer Manual DUBALYZER NIR Benchtop Analyzer by R E Hodges LLC Sup part 334 466 005 7 Figure 4 6 About screen 112 3 14 eI Js Yo Yo J Bock OOE GEE U Jee Je Je Asje JF ETAT Jk tj Enter J Clear Cancel Figure 4 7 LCD touch screen keyboard Main Menu Sample Pts Comp Labels Display Units Time Date stope Ottset New Bulb Analy Info Print Cig Figure 4 8 Main Menu screen R E Hodges LLC 16 DURALYZER NIR Laboratory Liquor Analyzer Manual The Main Menu is the access point to 18 submenus which serve to enhance functionality and provide customization To return to the Operator Screen simply touch Back and then OK when the About screen Figure 4 5 appears The submenus can be categorized under four headings 1 labeling 2 configuration 3 informative and 4 model tuning Table 4 2 shows a summary of the submenus accessible from the Main Menu displaying the name description and category Table 4 2 Main Menu S
80. so highlight the improvements made after calibration curves are implemented R E Hodges LLC 60 DURALYZER NIR Laboratory Liquor Analyzer Manual nuaw uiDw g adwbs C zsdwuos 2500 99p PEE uoddns 971 sebpoy 3 uq L ezAjeuy dojyousg N JIN HIA THENG d Pus T75 000731 4295330 dols 3944nj sazAjouy sjduip duo lduups C gaidums C gadus C pajdu SO apa O WV Logz Z8 355 r0 09 32 L6 022 ALIOS Y L 96 4 ALUS L1H8S1 002VN 96222 SZYN 589 t9 HOYN Laiduns L 96542 va 60 90 10 60 1d tis jouy 450 Spnsey sisApouy NOUOYALX3 HO009 W3ddf1 HSYMOANIM OI 31IHM ANT LSS 8 TOOL aT SHUN 0182 orny D siinsay jud A ajdwos u33135 J0 D1300 Figure A 7 1 Menu sequence for automated calibration curve determination 61 R E Hodges LLC DURALYZER NIR Laboratory Liquor Analyzer Manual Final Notes e Since laboratory measurements can have a significant amount of variability in terms of repeatability better calibration curves will be achieved by utilizing more calibration samples e Make sure the Normal Operating Procedure for preparing and drawing samples into the cuvette e In the absence of values for a particular component remember to enter NA e Once the calibration procedure has been started do not exit the Calibrate Curve Slope and Offset screen until the procedure is completed e Entered concent
81. t connections and a pair of optical couplers to deliver light to the sample and collect light after interaction with the sample The optical couplers house a set of lenses to focus the radiation onto the tip of the fiber optic cable The ends of the couplers in contact with the process sample have windows usually sapphire which provide a transparent optical path for the entering and exiting light as well as providing isolation from the process sample Sapphire is R E Hodges LLC 5 DURALYZER NIR Laboratory Liquor Analyzer Manual usually the material of choice for the coupler windows due to its combination of hardness chemical and heat resistance and inherent transparency over a broad range of wavelengths A sample cuvette functions as a sample cell and is used in a laboratory environment Obviously it would not hold up to the rigors of a process environment Implementation of a cuvette requires a cuvette holder shown in Figure 2 4 that allows the delivery of NIR light and collection of the transmitted light Sample Cuvette Gi D Quartz Tungsten Halogen QTH NIR Light Source Analyzer Sample Cuvette Holder Figure 2 4 Sample cuvette holder Light interaction with the sample is described by the Beer Lambert law also referred to as Beer s law and Lambert Beer s decay This law states that absorbance is directly proportional to the concentration of the absorbing species Details of this relation are sh
82. t density 8 dots mm 203 dpi e Input Voltage 24 Volts DC e Power Unit Input Voltage 100 to 240 Volts 50 to 60 Hz R E Hodges LLC 69 DURALYZER NIR Laboratory Liquor Analyzer Manual plod mod OV SD o qe ILJU eles IJd UOIJ23UUO UOI 22UUO AQLI plod mod DA 39BJ19 UT PLAS Be cf BAIT ae E usado 19402 jjdepy OV uir plod mod DA wW 661 wu cpm s o1ju0 1 JutId mm zt uiu ZET Figure A 9 1 Printer images 70 R E Hodges LLC DURALYZER NIR Laboratory Liquor Analyzer Manual Appendix A 10 NIR Light Source Replacement The maintenance requirements for the DURALYZER NIR laboratory liquor analyzer are minimal both in terms of time and cost All maintenance tasks should only be performed by qualified personnel that have read and understand this manual The typical lifespan of the QTH NIR light source should be approximately one year Before the bulb completely expires there are usually signs the end of lifespan is approaching A drop in bulb intensity combined with erratic measurements will be the most noteworthy characteristics It is recommended that a replacement bulb be ordered and kept on hand Replacement Steps Power off the analyzer Figure A 10 1 Remove the light source enclosure cover Figure A 10 2 Loosen the light source holder set screw Figure A 10 3 Unplug the old bulb and remove Plug in the new bulb Insert the new bulb into the l
83. that each one is tested multiple times Procedures and details concerning calibration curves are located in Appendices A 6 Manual Calibration Curve Determination and A 7 Automated Calibration Curve Determination R E Hodges LLC 29 DURALYZER NIR Laboratory Liquor Analyzer Manual Component Curves Slopes and Offsets Component Curve Slope Offset dieses CH 0 m ms x CU Co Update Figure 4 32 Component Curves Slopes and Offsets screen with default values Calibrate Curve Slope and Offset O Water OH Sample Sample 2 Sample 3 O Sample d Sample 5 J Sampled 9 Sample 7 Comp Sample Analyzer Curve Slope Offset KR LB 100 GAL EA Ka g UULU Masse TDS TOD TOO 58 Figure 4 33 Calibrate Curve Slope and Offset screen Every measured component for each sample point can have a scale and or offset correction to bias the analyzer to match the manual lab tests performed onsite If calibration curves have been generated and are in use the bias corrections will be minimal or nonexistent Select Set Bias on the Main Menu and then from the Bias Adjustments screen Figure 4 34 select the desired sample point to bias and press Edit At the Edit Bias Values screen enter the appropriate Slope and Offset biases and press Update when finished The component value to be measured is listed in the left column with the corresponding slope and offset biases
84. tments screen select the desired sample point to bias and press Edit At the Edit Bias Values screen enter the appropriate Slope and Offset biases and press Update when finished The component value to be measured is listed in the left column with the corresponding slope and offset biases to the right Once Update has been pressed the effects are immediate meaning the display results on the LCD panel will be updated to reflect the new bias adjustment 10 Repeat steps 2 9 for all sample points requiring a bias adjustment Two examples are presented to further highlight and explain the procedure and concepts presented above Example A 8 1 In the following example the black REA analyzer values need to be slightly tuned biased to agree with the laboratory measurements A calibration curve is already in place and was determined based on white green and black liquor The white and green liquor analyzer values are in agreement with the lab However low REA black liquor samples containing an appreciable amount of soap are slightly off from the lab and need fine tuning Figure A 8 1 illustrates the determination of bias adjustment parameters for this case Three black liquor samples evaporator chemiwasher and secondary evaporator are on the same analyzer sample point Thus these samples are used to determine the bias adjustment for REA All values are in g L as Na O with the analyzer values under the heading REA
85. ubmenus 2 Collect all liquor samples that will be required for determining the calibration curve parameters 3 Perform the necessary laboratory tests on the collected samples The tests will yield the LAB values 4 After lab testing is complete set the water zero Refer to Section 4 3 Normal Operation and Appendix A 5 Normal Operating Procedure 5 Test the collected samples on the DURALYZER NIR laboratory liquor analyzer following the procedures set forth in Section 4 3 and Appendix A 5 After each sample has been analyzed record the values shown in the Analysis Results section of the Operator Screen These will be the analyzer or NIR values It is highly recommended to have the Print Results box checked on the Operator Screen and the printer connected prior to analyzing the samples R E Hodges LLC 50 DURALYZER NIR Laboratory Liquor Analyzer Manual 6 After all collected samples have been lab tested and analyzer tested the mathematical determination of the calibration curve parameters is performed This requires the use of spreadsheet software such as Microsoft Excel 7 On the spreadsheet make three column headings for the sample the analyzer measurement value and the lab measurement value If any of the measured values are in units other than Ib 100gal make new columns with the values in 1b 100gal The first sample will always be water and its corresponding analyzer and lab values will
86. uire a slight adjustment after installation The New Bulb function on the Main Menu will access the New Bulb Adjustment screen After the bulb has been replaced draw water into the sample cuvette Select the Trigger Scan option on the left side of the screen to check if the new bulb saturates the detector Figures 4 28 and 4 29 show a water scan without saturation and a water scan in which the detector is saturated An unsaturated water scan Figure 4 28 indicates the replacement bulb is positioned and functioning correctly If the water scan resembles the spectrum shown in Figure 4 29 top portion of the two peaks are cut off meaning transmission has reached 100 the detector is saturated Detector saturation occurs even if only one wavelength is 100 The desired transmission is between 75 and 85 for the highest spectral peak The remedy for detector saturation is to slightly reposition the bulb by rotation and or relative location in the light source holder Details on removal and replacement of the light source are discussed in Section 4 5 Maintenance and Appendix A 10 NIR Light Source Replacement New Bulb Adjustment Trigger Scan 18 0 2 wavelength um Figure 4 28 Unsaturated water spectrum R E Hodges LLC 27 DURALYZER NIR Laboratory Liquor Analyzer Manual New Bulb Adjustment En les beaded d dee Trigger d Scan d 45 hae EN 1 M e E x EN sud m i H H H H H HE 304
87. ummary Display Units Configuration Time Date Configuration lope Offset Model Tuning et Bias Adjust biases to match ab tests Model Tuning MODBUS Configure MODBUS TCP parameters Configuration can Params Configuration Password Configuration aus Display internal analyzer sensor readings Informative pectta Display spectral signature of current sample informativo Display Adjust brightness and contrast of LCD panel Configuration New Bulb Check for saturation on anew bulb change informative Analy Info Informative Print fg Print analyzer configuration Informative Calibrate Perform analyzer calibration function Model Tuning Backup Backup current configuration Configuration Restore Restore last saved configuration Configuration 4 4 2 Labeling Submenus Selecting Sample Pts enables customized labeling of the sample points Each sample point can be labeled with a custom description label that is displayed on the Operator Screen and the analysis print out The sample point number is displayed to the left of the editable label Touch the button to edit the corresponding sample point label Figures 4 9 4 10 and 4 11 show the Sample Point Labels screen progressing from no sample points labeled to eight sample points labeled The default labels are PT 1 PT 2 PT 8 For example select the sample point 1 label button box and the virtual keyboard will appear Figure 4 7 use Clear to remove the pre
88. uted value The TTA calibration curve can be determined from green liquor weak wash and white liquor samples Other combinations are possible as well such as weak wash and white liquor or white liquor and diluted white liquor see above paragraph for comments on dilution Reduction efficiency RE computation requires the measurement of sodium sulfate Green liquor samples are used to determine the Na2SO4 curve parameters Obtain a single green liquor sample in an amount suitable to divide into three samples of equal volume Add approximately 5 g L and 10 g L of Na2SO4 s to samples one and two respectively Do not add any to the third sample Allow the sodium sulfate added to samples one and two to completely dissolve this will take more time the cooler the sample is Next test all three samples using the standard laboratory test procedure for sodium sulfate in green liquor Determination of the TDS calibration curve parameters can be carried out using white green and black liquors A convenient relationship for calculating TDS in white and green liquor is depicted in Equation A 6 2 TDS o 1 000 100 A 6 2 R E Hodges LLC 49 DURALYZER NIR Laboratory Liquor Analyzer Manual The density o is in g cm and can be measured by a handheld density meter or by a gravimetric method At room temperature measure out a precise volume of sample V in mL then determine the mass m in grams The black liquor TDS is usua
89. vious label type in GREEN LIQ or the label of your choice and select Enter Figure 4 10 Continue labeling the remaining sample points in the same fashion Figure 4 11 and touch the Update button when finished To return to the Main Menu select Back R E Hodges LLC 17 DURALYZER NIR Laboratory Liquor Analyzer Manual Sample Point Labels 1 es UA CES inr oe EE opel III Figure 4 9 Blank Sample Point Labels screen Figure 4 10 Samp Sample Point Labels LI GREEN LIG II o ELE LE E SE Update le Point 1 labeled as GREEN LIQ Sample Point Labels Ces dE dee dee deen deeg 7 CUPPERCOOK dE Update Figure 4 11 All sample points labeled R E Hodges LLC DURALYZER NIR Laboratory Liquor Analyzer Manual From the Main Menu changing the component labels is accomplished by selecting Comp Labels Each measured component can be labeled with a custom description that is displayed on the Operator Screen and the analysis print out The measured component label is displayed to the left of the button box Touch the button to edit the corresponding component label The procedure is analogous to editing the sample point labels Figure 4 12 shows the Component Labels screen with the default labels As an example of customized component labels the EA AA TTA can be represented as A B and C in refer
90. y to damage Use isopropyl alcohol and a soft clean cloth A soft cloth is sufficient for removal of dust from the paper holder The external housing of the printer can be wiped off with a moist cloth The typical lifespan of the QTH light source should be approximately one year Before the bulb completely expires there are usually signs the end of the lifespan is approaching A drop in bulb intensity combined with erratic measurements will be the most noteworthy characteristics A good rule of thumb is to order a replacement QTH NIR light source after 11 months of operation and install the new bulb after 12 months Figure 4 36 NIR light source enclosure R E Hodges LLC 32 DURALYZER NIR Laboratory Liquor Analyzer Manual To replace the NIR light source power off the analyzer and remove the light source enclosure lid with a Phillips head screwdriver Figure 4 36 Use an Allen wrench to loosen the light source holder set screw unplug and then remove the old bulb Figure 4 37 WARNING Bulb and light source holder will be extremely hot if the old bulb was not completely burned out Insert the new bulb into the holder tighten the set screw power on the analyzer and replace the cover Allow the new bulb to stabilize for two hours before using the analyzer Utilize the New Bulb function on the Main Menu screen to test for detector saturation see Section 4 4 4 Informative Submenus and adjust the bulb position

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DURALYZER-NIR ™ Laboratory Liquor Analyzer