InfraCal TOG/TPH Analyzer
Contents
1. The instrument must be made to read lower A divider is needed instead of a multiplyer As in example 1 divide the lowest number into the highest number to get the correlation factor 124 divided 49 2 5 divider The divider for this example is 2 5 Therefore divide the value from the Calibration Standard in Desired Units CO1 CO2 column in the Relative absorbance Versus Calibration Standard or Alternate Method Table section 3 4 2 by 2 5 This will correlate the values to an alternate method The new Calibration Standard values can be re entered into Edit program see section 3 4 3 Appendix C Solvent Options Hexane A volatile hydrocarbon that is specified for EPA Method 1664 Because it is a hydrocarbon it must be evaporated prior to making the infrared measurement to determine TOG or TPH levels in a sample which takes approximately 3 5 minutes Since hexane is lighter than water the solvent after extraction will rest on top making it easy to deliver a measured amount of extract to the sample platform or plate with a 50 microliter auto pipette without losing any of the sample Pentane A volatile hydrocarbon preferred in Scandinavian countries over Hexane Similar in performance and use to hexane although it has a lower boiling point and therefore will retain more of the low boiling point components Pentane is lighter than water and like hexane will rest on top after the extraction Vertrel MCA A volatile HFC solvent tha2. Press the CAL button for two seconds until CAL appears on the display Press the RECALL button to display the active table one of uSEr Edit or oF F Press and release the RECALL button repeatedly until the desired mode is displayed e Press the ZERO button to exit the calibration mode idLE will be displayed 3 4 2 Setting the evaporation timer Overview The InfraCal TOG TPH Analyzer contains a built in user programmable evaporation timer intended for use with model HATR T2 For model CH the evaporation time can be measured using the timer although the IR plate needs to be manually placed into the holder for the run time Timer Programming The CAL lockout switch must be in the on I position to set the timer see figure 3 section 1 3 2 Press and hold the RUN button until the current timer value is displayed The value is displayed as 1 or 2 digits in minutes and 2 digits in seconds separated by a period Release the RUN button once the current value initially 0 00 is displayed Use the up arrow and down arrow keys to scroll the timer to the desired value Five minutes 5 00 is recommended The optimum time will vary with the type of oil and atmospheric conditions at the point of use To zero the timer during programming press the ZERO button Once the desired time has been programmed press the CAL button The display will read idLE Timer Operation The timer is disabled when programmed to zero 0 00 When the timer is non
3. a portion of the solvent to be used for extraction If using a graduated bottle with a septa cap solvent can be mixed directly in the bottle without using the separatory funnel 2 Adjust the pH to less than 2 with Hydrochloric acid or Sulfuric Acid typically 3 5 drops depending on buffers in sample 14 Add one tenth of the sample size of solvent to the sample collection container to rinse interior surfaces and cap With the 177 ml prescription bottle it is convenient to collect 140 ml of sample and add 14 ml of solvent Pour this solvent into separatory funnel containing sample Shake the separatory funnel or prescription bottle vigorously for 2 minutes with periodic venting to release excess pressure Allow the phases to separate Place a filter paper in a filter funnel and add approximately 1 gram 1 Tablespoon of sodium sulfate Drain the solvent lower layer from the separatory funnel through the sodium sulfate into a clean container 10 mL graduated cylinder can be used With the prescription bottle invert the bottle so that the solvent layer fills the neck Using a 5 ml syringe withdraw 4 5 mL of the solvent layer and deliver through the sodium sulfate into a clean container Note Use of the sodium sulfate is necessary to prevent water from interfering with the analysis With totally hydrophobic solvents this step may be skipped It is not necessary to collect all of the solvent but it is necessary to preclude water to prevent
4. caking of the sodium sulfate 8 4 2 4 Eject 50 microliters of solvent extract using a pipette or syringe onto the center of the HATR T2 plate and press RUN For the CH Model remove the sample plate and lay on a flat surface Eject the standard from the pipette or syringe onto the center of the plate and allow the solvent to evaporate The evaporation time can be measured using the programmable timer Insert the IR sample plate into sample stage and press run Press twice if the timer is preset to override the timer Total Oil and Grease TOG Extraction from Water for Solvents Lighter than Water ie Hexane Pour sample into a stopper graduated cylinder and measure Rinse the sample collection container with a portion of the solvent to be used for extraction If using a graduated bottle solvent can be mixed directly in the bottle Adjust the pH to less than 2 with Hydrochloric acid or Sulfuric Acid typically 3 5 drops depending on buffers in sample Add one tenth of the sample size of solvent to the sample collection container to rinse interior surfaces and cap With the 125 ml graduated bottle it is convenient to collect 100 ml of sample and add 10 ml of solvent Pour this solvent into graduated cylinder containing sample Shake the graduated cylinder or graduated bottle vigorously for 2 minutes with periodic venting to release excess pressure Allow the phases to separate Place a filter paper in a filter funnel and add approx
5. concentration of oil and grease in the solvent The analyzer can be calibrated to read out directly in the desired units 1 3 Analyzer description Infracal Figure 1 The InfraCal TOG TPH Analyzer Front View of Analyzer 1 3 1 Front operating panel The front panel consists of a 4 digit LED display and four labeled touch sensitive push button controls as illustrated in Figure 2 The LED display remains illuminated while the analyzer is plugged in switched on When the instrument is on and not in use the display may either show the result of the last analysis or it may show idLE Figure 2 The Display and Control Panel 1 3 2 Back panel The main power socket for the 12 Volt power supply is located on the back panel The back panel also provides a standard nine pin female DB9 connector for serial RS232 C data communications with the analyzer This requires the use of a standard straight through serial data cable See Appendix C for details of data communications with the TOG TPH Analyzer The CAL lockout switch deactivates the front panel CAL button to keep the internal calibration table from being inadvertently changed or turned off For calibration the switch is ON I After calibration the switch may be moved to the locked position O The back panel also contains the CE Mark designation indicating compliance with the codes for operation within the European Community countries and the analyzer serial number Make a perman
6. displayed 12 2 Press CAL The display will read n for a short time followed by the number of entries currently in the calibration table Scroll to the desired number of entries 0 20 Selecting O will erase any existing calibration table 3 Press CAL to proceed The display will read A01 for a short time followed by the current absorption value for the first calibration table entry Scroll this to the desired value from the relative absorbance versus calibration standard table 4 Press CAL again and the display will read C01 followed by the current analyzer concentration value for the entry Scroll this to the desired value from the table Continue to press CAL to step through all absorption and concentration values for the table size n entered Once all entries have been created press CAL and the display will read idLE 3 4 5 User Calibration Mode Procedure Note that this is not the preferred method to use for calibration of the InfraCal Analyzer If you would like to use this method please contact tech wilksir com for instructions 3 4 6 Calibration printing With the optional printer the current calibration table can be printed by momentarily pressing and releasing the ZERO button when the analyzer is idle The first line indicates which calibration is active followed by the date and time The second line gives the headings for the calibration table that follows ABS represents absorption and CON represents co
7. dry surface Rubbing back and forth on the crystal tends to spread any residual oil rather than removing it If the previous sample had high TOG or TPH levels this procedure may need to be repeated two or three times to remove hydrocarbon residues Check zero see section 2 2 2 e For Model CH place the clean IR sample plate in the sample stage e Press and hold the ZERO button until the display reads BAL Release the button A multiplier value to 3 decimal places will be displayed when zero is established The actual value is only of interest when reporting problems to the factory e Press RUN The display should read 00 02 If not repeat the zero process 2 2 2 Zero Check The zero value is retained in permanent memory and is restored each time the instrument is powered up It is recommended that the zero be checked and if necessary reestablished on a daily basis e To check the zero value press the RUN button For Model CH first place the clean IR sample plate in the sample stage e If the result is not 02 re clean the trough plate or IR sample card e Check zero again e If the result is not 02 reestablished the zero as described in 2 2 1 3 Analyzer Calibration 3 1 Data Presentation The standard display format for the TOG TPH Analyzer is relative absorbance ABS This is the format the analyzer is preset for unless the customer specified otherwise Other formats are available and these may be set for specif
8. is the number of calibration table entries The RC n command response is C n x y where n is the entry number as received x is the raw measurement data as it appears on the display during calibration and y is the actual value as set by the user during calibration The format is determined by the display mode absolute percent or decimal Calibration commands should not be used when in ratio mode since ratio mode does not use a calibration table An RC command requesting data for a table entry number greater than the current table size returns erroneous data The RC command with no arguments returns the complete calibration table one entry at a time starting with the table size information The individual entries are then returned in numerical order up to the number of entries Read Calibration Table Example Assume the instrument is calibrated in the absolute mode using three standards Assume the calibration results were as follows Entry Measured Actual 1 15 30 2 26 50 3 33 70 The RC command will return the following C 0 3 C 1 15 30 C 2 26 50 C 3 33 70 The RC O command will return C 0 3 The RC 2 command will return C 2 26 50 The WC command can be used to download calibration table data based on previously uploaded data or as determined by a host program The command format is WC n x y where the parameters are identical in format to the RC command The parameters must match the current display mode When using the WC command
9. shipping charges Normal one week turn around is offered for all InfraCal instruments that are returned to the factory for service For users requiring faster service times Wilks Enterprise also offers an advance replacement program that can respond to a user s needs with instrument replacement typically in less than 24 hours For extended service contracts advanced replacement programs factory service charges or sample system installation procedures please contact Wilks Enterprise Inc for details Appendix A Alternate Data Presentation The standard display format for the TOG TPH Analyzer is relative absorbance ABS It provides relative absorbance value Other formats are available and these may be set for specific applications NOTE The TOG TPH Analyzer must be calibrated in the selected data presentation mode Changing the data presentation mode requires re calibration The following are the different data presentation modes available of the InfraCal analyzer Percent Mode PCt Calculated values are displayed to a single decimal place 0 0 Decimal Mode dEC Calculated values are displayed to two decimal places 00 Absorption Mode ADS An arbitrary scale related to the raw absorption of the sample 00 NOTE Inserting a decimal point does not change the raw relative absorbance value displayed for a given sample ie an Abs reading of 25 becomes 2 5 pct or 25 dec Ratio Mode RAt A threshold based scale where a value
10. the table size and all necessary table entries should always be downloaded Once all table entries have been downloaded the table size should be set Write Calibration Table Example To download the calibration table described in the previous example send the following commands WC 1 15 30 WC 2 26 50 WC 3 33 70 WC 0 3 8 Service and Customer Support Your InfraCal TOG TPH Analyzer may have been purchased either directly from Wilks Enterprise or from a local dealer or representative In cases of any difficulties or problems associated with operation you are recommended to contact your local representative or dealer first If the analyzer was purchased 27 direct or if there are problems that are unanswered by the local representative or you have a technical question relative to the operation of the instrument or relative to the analysis please contact Wilks Enterprise at the contact address provided below Customer Services Department Wilks Enterprise Inc 25 Van Zant Street Suite 8F East Norwalk CT 06855 USA Telephone 203 855 9136 FAX 203 838 9868 E mail tech WilksIR com Service and Repair During the warranty period Wilks Enterprise Inc offers free factory service for all failures that occur from normal instrument usage The user is only required to cover the cost of shipping the instrument to the factory After the warranty period the user is required to cover the factory s cost of servicing plus all
11. the timer is preset to override the timer If the result is above the calibration range see section 4 4 for dilution procedure Total Petroleum Hydrocarbon TPH Extraction from Soil The difference between TPH Total Petroleum Hydrocarbon and TOG Total Oil and Grease is the polar organics are removed from the extract using silica gel The remaining hydrocarbons are the non polar components considered to be TPH l 4 4 Follow the above procedure steps 1 6 For Step 3 Silica Gel may be used in place of the sodium sulfate Place a filter paper in a filter funnel and add approximately 1 teaspoon of silica gel Pour extract from container though the silica gel into a clean container Eject 50 microliters of solvent extract using a pipette or syringe onto the center of the HATR T2 plate and press RUN For the CH Model remove the sample plate and lay on a flat surface Eject the standard from the pipette or syringe onto the center of the plate and allow the solvent to evaporate The evaporation time can be measured using the programmable timer Insert the IR sample plate into sample stage and press run Press twice if the timer is preset to override the timer If the result is above the calibration range see section 4 4 for dilution procedure Dilution Procedures If the sample reading is above the highest calibration point a dilution must be performed to bring it into the measurement range 17 4 4 1 10 1 dilution Po
12. 40ul 10 ml 3000 300 30ul 10 ml 2000 200 20ul 10 ml 1000 100 10 ul 10 ml Note To convert ppm to mg l multiple by the specific gravity of the oil used for the calibration standard for 3 in 1 Oil or 30W motor oil use 0 865 by the ppm value to get a mg l value 3 3 2 Preparing Gravimetric Standards Supplies needed for gravimetric calibration 125 ml Teflon wash bottle 10 ml graduated cylinder 10 ml volumetric 40 ml vials with Teflon lined caps at least 3 for holding standards Solvent see Appendix C for solvent options Calibration oil Analytical Balance that reads to 001 gram Prepare a stock solution and make the appropriate dilutions to cover analysis range For water analysis with an extraction ratio of 10 1 the oil and grease is concentrated 10 times in the solvent The actual value of the standard is divided by 10 in order to match the concentrated value of the extract 1 Weigh about 0 1 gram of oil in a 10 ml volumetric flask 2 Record the exact weight 3 Fill with solvent up to the 10 ml line Calculate the exact concentrations as shown below Oil weight x 10 000 mg l multiply grams x 1000 to equal mg and divide 10 ml by 100 to equal liters 0 1 1000 divided by 0 1 10 000 For an oil weight of 0 110 gram in 10 ml the Stock solution will be 0 110g x 10 000 1 100 mg l Using the above hypothetical stock solution an example of dilutions for the desired range for a particular analysis that is typically 10 mg l w
13. None ID Return firmware ID 2 02 06 7 5 Data logging Data logging provides results output at the end of each RUN or BALANCE cycle The results are output when data logging is enabled both for functions initiated from the instrument control panel and functions initiated by the host The format of the data returned after a RUN cycle is as shown for the RR command and is determined by the display mode The format of the data returned after a BALANCE cycle is as shown for the RB command The RA command allows the host to initiate a run cycle and data log a result that is not adjusted by the calibration procedure This can be used by an intelligent host resident calibration table generator 7 6 Remote zero balance control The instrument zero balance can be controlled via the communications port The RB WB and BA commands provide the necessary controls This feature can be used to store multiple zero values for different operating conditions This feature combined with the calibration controls described in the next section can be used to maintain multiple calibration curves when using the instrument for multiple applications The RB command will retrieve the current zero balance data The WB command can then be used to reset the current zero balance to a previously recorded value The WB data field is identical in format to the data returned in response to the RB command The BA command can be used to initiate a zero balance function under remote c
14. TTT Environmental Instruments and Supplies The preferred source for instrument Wi S Rentals Sales Service and Supplies 4201 B Street 25420 74th Avenue S simple analytical solutions Anchorage AK 99503 Kent WA 98032 907 770 9041 253 373 9041 www tttenviro com info tttenviro com InfraCal TOG TPH Analyzer Model HATR T2 and CH User s Guide InfraCal is a registered trademark of Wilks Enterprise Inc Copyright 2008 Wilks Enterprise Inc East Norwalk CT www WilksIR com Rev 4 3 November 2009 Table of Contents 1 InfraCal TOG TPH Analyzer Overview ccsscsscssesscesscesseeesenesseesseeseeeeeneeesenesenaenneenaes 4 1 1 MTEL OAUCHOM siene a E e AE E E E 4 1 2 Basic measurement CoNCEpt ssssisirsnisissrisrsites ateni arinina iaaa iaaea i ana E Ae Eaa ENa a iaaea 4 1 3 Analyzer descripUonisvecssivs sess ae E E ates E E T eae 4 1 3 1 Front operating panel sssrinin ee ei EE EEEa esi Ea 5 Bede Back panel nirean eneren VA AE sane EEA ARRO RENK TEES ERDER 5 1 3 3 Description of the push button controls ssssesesseessesesresresreresresrestrerssresrnrrnrestestenresresrerene 6 1 4 Analyzer Features gemo oaar a e a A A ibe A E E io iaeaesess 6 141 Internal Calibration essegi ceee irepair aes aie Ena a eE EER 6 1 4 2 External Communicationy ecceecccesceeesceceseeeeseecseeeseecseeceaeecseeesaeecseeeseessaeeeeeeseneeeeaeees 6 1 4 3 Recall Function Averaging Results ssssssesser
15. can cause the sample to dry in a non uniform way or for the oil to migrate over time once the hexane has evaporated These problems can be corrected as follows Clean the sapphire plate with a solvent such as methyl alcohol Remove the sapphire plate from the analyzer and fill the window with enough methyl alcohol to cover the surface Allow the plate to soak for 10 seconds Dry the window with an anti static wipe cotton ball or a swab intended for use with alcohol Check the zero value and re zero if necessary Section 2 2 This can be done each time a new sample is to be analyzed immediately prior to sample application 6 6 1 Analyzer Specifications External power requirements The InfraCal TOG TPH Analyzer operates off external 12 volt power The power sources can be either regulated DC power supplies or an external battery This power can be provided by the user or by Wilks Enterprise Inc The suggested minimum requirement specifications for the 12 volt power source applied to the analyzer are described below Wall Supply Specifications Input 100 250 VAC 50 60 Hz 0 5A Output 12 VDC 1 25 Watts Battery Supply Specifications Output 14 VDC Maximum 11 VDC Minimum Load Specifications 6 2 6 3 1 5 Amperes Peak Physical Dimensions 6 5 in x 6 5 in x 5in 165 mm x 165 mm x 127 mm Weight 4 5 lb 2 0 kg Control Display output 4 digit 7 segment red LED 5 8 in character height User input 4
16. converted to the amount of oil in the original sample if the ratio of solvent to water is carefully controlled The InfraCal TOG TPH Analyzer Model CH is designed as an equitable substitute for EPA Method 1664 for hexane extraction and gravimetric determination for higher levels of TOG or TPH Since hexane is not transparent at the analytical wavelength used for hydrocarbon absorption a fixed volume of the extract is placed directly in the IR Sample Plate and the hexane is allowed to evaporate When the IR Sample Plate is placed into the sample stage IR energy is focused from the source through the sapphire window on to the dual detector package Figure 9 21 The energy collected at the analytical wavelength I is reduced when compared to the energy collected at the reference wavelength Ip The oil concentration is determined by a calculation of the logarithm of the ratio of the light transmission at the reference wavelength to the light transmission at the analytical wavelength Beer Lambert law as shown in Figure 6 The Beer Lambert law assumes a linear relationship between absorbance and concentration Deviations from linearity if any can be determined by obtaining absorbance values from known samples This data can be used to prepare an internal point to point calibration table Section 3 so that actual concentration is directly presented on the display If the concentration ratio used during extraction typically 10 parts sample to 1 pa
17. de section 3 4 1 4 Set the timer for five minutes 3 4 2 5 Eject 50 microliters of standard using a pipette or syringe onto the center of the HATR T2 plate and press RUN For the CH Model remove the sample plate and lay on a flat surface Eject the standard from the pipette or syringe onto the center of the plate and allow the solvent to evaporate The evaporation time can be measured using the programmable timer Insert the IR sample plate into sample stage and press run Press twice if the timer is preset to override the timer 6 Record the result on the table below AO1 Record the standard value in CO1 Standards may be run several times and an average can be entered on the table below 7 Repeat for the remaining standards Note The results can plotted graphically as a calibration curve The resulting plot can be used to prepare a reference chart for users who prefer not to use the analyzer s internal calibration or for data points to be edited into calibration Relative absorbance Versus Calibration Standard or Alternate Method Table Relative absorbance Value Calibration Standard in Desired Units AOl C01 A02 C02 A03 C03 A04 C04 A05 C05 A20 C20 N Number of calibration points or calibration standards 3 4 4 Entering Calibration Data into Edit program 1 Press the CAL button for two seconds until CAL appears on the display Press RECALL until Edit is
18. defining an acceptable limit for maximum or minimum acceptable concentration is set to the value of 1 000 All values less than 1 000 indicate that the concentration is less than the threshold while all values greater than 1 000 indicate that the concentration is greater than the threshold The TOG TPH Analyzer display format can be switched between modes by pressing and holding both the CAL and ZERO buttons for two seconds Each time the CAL and ZERO buttons are pressed the display mode changes Release both buttons and repeat until the desired mode is displayed The display will read ABS for absorption mode PCt for percent mode dEC for decimal mode and RAt for ratio mode Press RUN to exit the data presentation mode one the desired mode is displayed 28 Appendix B Correlation to an Alternate method If values for sample analysis were taken with the Edit program on and calibration data in the Edit program The following can be used to calculate revised calibration points to re enter into the Edit program Rule Of Thumb e If the laboratory s analysis is greater in concentration than the Field analyzer s analysis use a multiplier with the field instrument e If the laboratory s analysis is less in concentration than the Field analyzer s analysis use a divider with the field instrument Example 1 Assume the sample analysis on the Wilks InfraCal read as follows SAMPLE A 25 ppm SAMPLE B 13 ppm SAMPLE C 11 ppm Assume th
19. e alternate method to analyze the duplicate samples read as follows SAMPLE A 63 ppm SAMPLE B 33 ppm SAMPLE C 28 ppm In this case the alternate method read higher Oil and Grease concentrations than the Wilks InfraCal Analyzer Therefore the difference must be determined by dividing the lowest number into the highest number The instrument must be made to read higher A multiplier must be determined as shown in the example below InfraCal results 254 13 11 49 ppm Alternate Method Results 63 33 28 124 ppm 124 divided by 49 2 5 multiplier The multiplier for this example is 2 5 Therefore multiply the value from the Calibration Standard in Desired Units CO1 C02 column in the Relative absorbance Versus Calibration Standard or Alternate Method Table section 3 4 2 by 2 5 This will correlate the values to an alternate method The new Calibration Standard values can be re entered into Edit program see section 3 4 3 Example 2 Assume the sample analysis on the Wilks InfraCal read as follows SAMPLE A 63 ppm SAMPLE B 33 ppm SAMPLE C 28 ppm Assume the analysis using the alternate method to analyze the duplicate samples read as follows SAMPLE A 25 ppm SAMPLE B 13 ppm SAMPLE C 11 pip 29 In this case alternate method read higher Oil and Grease concentrations than the Wilks InfraCal Analyzer Therefore the difference must be determined by dividing the lowest number into the highest number
20. eaes 13 42 2 Considerations ecrire a E E E E T O 14 4 2 3 Total Oil and Grease TOG Extraction from Water for Solvents Heavier than Water ie Vertrel MCA 14 4 2 4 Total Oil and Grease TOG Extraction from Water for Solvents Lighter than Water ie Hexane 15 4 2 5 Total Petroleum Hydrocarbon TPH Extraction from Water ecceeceeseeeeseeeeteeeeeeeeeee 16 4 3 1 to 1 Extraction Procedure for oil in soil ooo eee eee seeeseeeeeeeeeeeeeaeeesaeeeeaeersneeenaeessaeeetatersaeeenaes 16 43l Stipples Meeded as s 1ctescotvosed auebiacpateeds oiai vies thas sagste cds scab a EEE a a eria 16 4 3 2 Total Oil and Grease TOG Extraction from Soi ccccccccesscecsesseeeessneeeeseneeeessneeessees 17 4 3 3 Total Petroleum Hydrocarbon TPH Extraction from Soil ee eeeeceeeeeeeeeeeeeteeeeeeeees 17 4 4 Dilution Proc ed r S reiese ine e E E E E DE R 17 AAT TOV dilution onenen a e a a E E id ae eA 18 4 5 Averaged Results Display 0 ceccesscceeceeeenecescecesneeeceeesnecesaecenecesaecseeceseeceseeceeeceaeeseeeeeeeeens 18 5 Detailed Sample Stage DeScription csscesscssecsseesseesseesseesseeeseeseneeseeeneneseneseneeaneenaes 18 5 1 IR Model HATR T2 platform sample stage description eee eeeeeeeeeeeeeeeeeeeeeeeseeeneeeaees 18 5 1 1 IR platform model HATR T2 measurement CONCEPt eee ee eee eee eseeeseeeseeeaeteeeeees 19 5 1 2 IR platform considerations 0 0 eee eeeeseeeseceseeecesecesece
21. ee ar Ae e a A E EER E RES 26 7 6 Remote zero balance controleren eerren e ER E A 26 7 1 Remote calibration controls isecen e E E AE E R 26 8 Service and Customer Support ass sssssssunssunnnunnnunnnunnnunnnnnnnunnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnn nnmnnn 27 Appendix A Alternate Data Presentation e esseeessseseeesoreroreeseseseecrceroreeseserorerersesesercrororsreeseneeee 28 Appendix B Correlation to an Alternate method e sesessesseossoesesoesesoesosoeseeoesocoesoesesoesoeossoesse 29 Appendix C Solvent Options cccsccssscscccscscscssssssscssssssscssssssccsscescssessesssesssssscssssessesessesees 30 List of Figures Figure 1 The InfraCal TOG TPH Analyzer Front View of Analyzer 0s00004 Figure 2 The Display and Control Panel csccssscssssssscssccssscssscsscscssscssesssessseeened Figure 3 The TOG TPH Analyzer Rear View scsscsssscssscsssscssscsscscssscsscssscsesesened Figure 4 The TOG TPH Analyzer Model HATR T2 Sample Stage Front View 19 Figure 5 The TOG TPH Analyzer Model HATR T2 Top View scsssssseseseeee 19 Figure 6 Measurement of IR Absorption with an IR Platform scsssssssseseeee 20 Figure 7 Model CH Sample Stage csssocsssssssssssssscscssscscsssscssscscssscssssscsssesscsssssessses 2L Figure 8 The TOG TPH Analyzer Model CH Top View ssccsscssecessee2 Figure 9 Measurement of IR Absorptions with an IR Card Reade
22. ent note of the serial number and quote this when contacting Wilks Enterprise with a service or warranty related issue CALLOCK o I EN 61010 1 EN 55022 Class B POWER INPUT EN 50082 1 12V 1AMP p Made In U S A Figure 3 The TOG TPH Analyzer Rear view 1 3 3 Description of the push button controls RN RUN initiates sample analysis Section 4 Also used in CAL to record a calibration sample Section 3 UP arrow control used to increase numerical values used in the CAL function Section 3 CAL Hold for 2 seconds to select calibration type uSEr Edit or oF F Also used to generate a new user calibration Quickly press and release to print the last result fe E el bE ZERO Hold for 2 seconds to zero balance the instrument bAL appears on display during operation Section 2 Also used to exit CAL Quickly press and release to print the current calibration table RECALL Quickly press and release to recall up to the last ten results recall mode RECALL section 4 5 or to display the average averaging mode section 4 5 Hold for 2 seconds to reset the printer sequence number DOWN arrow control used to decrease numerical values used in the CAL function Section 3 1 4 Analyzer Features 1 4 1 Internal Calibration The InfraCal TOG TPH Analyzer reads in relative absorbance units that are proportional to concentration An internal microprocessor allows the user to enter a calibration
23. eseeeaeeeaeceaeeceeseeeaeeeaeeeaeesaessaetneeaes 20 5 2 IR card reader sample stage description sseessesesessesresreeresrsstsresresrrstesresrnsrsrententesrenresresresent 20 5 2 1 Card reader model CH measurement concept 0 eceeeceeeseeeeseeeeteeeeeeeseeceeeseeeenenerens 21 9 2 2 IR Card reader c nsiderati NnS srei ci cisensiss cassatadsvecicsasval ocesceaodisacuactaicdeaseassvetvebecsasaivastersees 22 6 Analyzer Specifications ccsccssccsensessseeesneeseeesseesseesseeeneseeeeneeeseneseneseneeaeeessnensessoees 23 6 1 External power requirements s cscsccseciscee cts fetes staccess shaceshetuguenscspacdsdhsdastoneidadteascapesebevessabertoness ey 23 6 2 Physical nises e a E E E A E A E E EEEE a EEES 23 6 3 Environmental sesira N E EA che aad E ea ees 23 6 4 Electrical sessed saciid seas eden bande na certo steaves siasdecavtusdeaed E E E A E 24 6 5 Cali Dra Ons scectaccteaceceses e e daccsosesaaeeda se E A EE A 24 7 Analyzer Communications Interface csscscssesseessesesnesenneneeeseneseneseneseneesneesseensoess 24 7 1 ADSIT a E E E E 24 7 2 Physical connection 2i cc25s cavics tasdeves ee sneleccetsetiesegsceneseadction oyeebiecersedvessancdubvasertusestectistelecdbeeetsveeas 25 7 3 Communications port setup parameters eee cece cess cece cesecseeeseeeseeeseeeaeseaesseesseeeaeseaeenaeen 25 7 4 Op ratiofi reneisse n atrae o Ea E a E E a eSEE E a Ee a E EE 25 To Data LOS BING saracene arr
24. esseresreerrsreeresrerreresrrstrsrrstesresrnsrsenrenresresrerent 6 14A Printins the Results sorre asa a E E E E E E AAN 6 2 Getting Started aise asco eccece tie eslee da hvcccentce cocestnncucbeutcenccstvatesatstucsectececeslteutiesteuedsceutesberenevecestues 7 Delis Win tall AG OMe meeer an E E A A E E ascte ser caussetvtce E E 7 2l Loca enee A E a E e a EE E aA A A a A EN 7 212 POWETIREGUITEMEMES cessen iea a Ee e N ER 7 BM Sie Warmup ime nerna a A N a 7 225 ACTOS the AN Al YZEl ss cscs lt cssseegvacessvevadesunvadeeisaeodn deen nsdacedeevsceaanseedea esedecing nodded vaseessecesseceseseeeacdestaes 7 DDMe Establishing Zero sek sviceveecoseaacesacedvcs cd satestedessvivense RE KEE ENKE E EERE cds 7 PAE AI MET A L O EEE A E E oa tavebe Ladundes adeataades 8 3 Analyzer Calibratiomcrcs iccccccctsccctececteasteceeceenteenttenuerececceasseuenccedsieesceesiensetersuvectescueesterucreect 8 3 1 Data Presentation vist cecuri rnane a avevasbavedvaseet a aaa a aie 8 3 2 Considerations for Calibration Standards eceeecceescecescesenceceenecececeaeeceeeesanecsaeeeseessaeeenaeers 8 3 2 1 Calibration correlated to an Alternate Method ou eee eescceeseceeseceeeeeeeecesaeessaeeesnessaeeeeaeers 8 3 3 Preparing Calibration Standards ssc ccciscdiscvetivecesivasssicedvecescevabesabevarsssevsansscteluescnsvedavasuvieeraiseaseces 9 3 3 1 Preparing Volumetric Standards sessirnar scesu siikaa 9 3 3 2 Preparing Gravimetric Standards isssessisesssssi
25. he InfraCal memory using the Edit program that is described in section 3 6 Note Data can be collected with the calibration from standards programmed into the Edit program with the edit program on Refer to Appendix B for the calculations needed to correlate the alternate method values to the calibrated InfraCal TOG TPH values for new values to enter into the Edit program 3 3 Preparing Calibration Standards Standards can be made gravimetrically mg L for water mg kg for soil or volumetrically ppm Customers can prepare their own standards using a non volatile heavy weight oil such as 3 in 1 or an actual oil sample Calibration standards should cover the desired range for the analysis An ideal calibration set contains three to five samples A maximum of 20 samples can be used The calibration curve for oil and grease is typically linear up to 3000 ppm 300 ppm for oil in water with a 10 1 extraction ratio Above 4000 ppm or 400 ppm for oil in water samples the curve flattens out Because the InfraCal TOG TPH Analyzer performs a point to point calibration samples above the linear range will be accurate up to the highest calibration standard It is best to calibrate to 4000 ppm 400ppm for 10 1 extraction ratios and dilute the extract for samples above this range See section 4 4 for dilution procedures The lowest concentration standard should measure at least 10 on the InfraCal in the oF F mode for calibration All successive sample
26. he last 10 measurements from newest to oldest in a circular fashion First the TOG TPH Analyzer must be switched from the average mode factory default to the recall mode as described below Once the recall mode is selected momentarily press the RECALL button repeatedly to display the previous results The TOG TPH Analyzer recall mode can be switched by pressing the ZERO button first immediately followed by the RECALL button and holding both buttons for two seconds The display will read rCL when switched to the recall mode Repeat the procedure to return to average mode The display will read Ag 5 Detailed Sample Stage Description 5 1 IR Model HATR T2 platform sample stage description The InfraCal TOG TPH Analyzer Model HATR T2 is supplied with a removable IR Platform sample stage with an integrated optics sensing system The sample stage includes the infrared source modulated and detector system positioned such that an elliptical energy beam is transmitted through the IR Platform crystal and focused directly on the detector sensing window 18 8 32 x 11 32 Long Ball Plunger Use small flat screwdriver for adjustment Detector Location Source Location Figure 4 The InfraCal TOG TPH Analyzer Model HATR T2 Sample Stage Side View os ES Go ks Figure 5 The TOG TPH Analyzer Model HATR T2 Top View 5 1 1 IR platform model HATR T2 measurement concept Model HATR T2 makes use of the fact that hydrocarbons such as oi
27. ial communications port This capability allows for collection of sample measurement data and instrument control by a host computer The host can also maintain calibration tables and download them to the instrument as required This is particularly useful when more than one table is being used with a single instrument Specification details for interfacing user customized host software are as follows 24 7 2 Physical connection The InfraCal TOG TPH Analyzer is connected to the external device via the 9 pin female DB9 connector located on the rear panel in the lower left hand corner The InfraCal TOG TPH Analyzer operates as a DCE device To connect to a PC a standard straight through 9 pin cable can be used but only 3 wires are required The required signals are Transmit Data TXD Receive Data RXD and Ground GND The pinout is as follows Function Pin RXD 3 TXD 2 GND 5 Systems with serial numbers lower than 10200 require a null modem cable or null modem adapter 7 3 Communications port setup parameters The port setup required by the InfraCal TOG TPH Analyzer is e 9600 baud e 8 data bits 1 stop bit e No parity 7 4 Operation The TOG TPH Analyzer accepts ASCII commands from the host and returns data as a response to certain commands or in datalogging mode on completion of a measurement cycle All commands are two characters in length Certain commands have parameters that follow the command Parameters are separa
28. ic applications Details for other formats are in Appendix A Alternate Data Presentation Modes 3 2 Considerations for Calibration Standards There are five choices for calibration Prepare your own standards Standard preparation is described in detail in section 3 3 Purchase pre prepared standards from Wilks Enterprise Calibrate to an alternate laboratory method Non certified factory calibration Wilks Enterprise can provide the InfraCal TOG TPH Analyzer with a non certified 5 point factory calibration using either Freon or Hexane calibration standards 5 Certified laboratory calibration Wilks Enterprise can recommend a certified laboratory for analyzer calibration fo D 3 2 1 Calibration correlated to an Alternate Method Each type of oil and grease analysis sees different physical properties and will sometimes give different results from each other The InfraCal TOG TPH Analyzer can be calibrated against an alternate method rather than with prepared standards For calibration against an alternate method obtain duplicate samples or if possible test the same sample with the InfraCal and the alternate method Data collected for this purpose should be obtained with the calibration in the oFF mode With a minimum of 10 data points make a graph with InfraCal relative absorbance data vs the alternate method values Select 3 to 5 data points within the desired measurement range of operation and enter these calibration points into t
29. imately 1 gram 1 Tablespoon of sodium sulfate Using a disposable polyethylene pipette withdraw 4 5 mL of the solvent layer and deliver through the sodium sulfate into a clean container Note Use of the sodium sulfate is necessary to prevent water from interfering with the analysis With totally hydrophobic solvents this step may be skipped It is not necessary to collect all of the solvent but it is necessary to preclude water to prevent caking of the sodium sulfate 7 Eject 50 microliters of solvent extract using a pipette or syringe onto the center of the HATR T2 plate and press RUN For the CH Model remove the sample plate and lay on a flat surface Eject the standard from the pipette or syringe onto the center of the plate and allow the solvent to evaporate The evaporation time can be measured using the programmable timer Insert the IR 15 4 2 5 sample plate into sample stage and press run Press twice if the timer is preset to override the timer If the result is above the calibration range see section 4 4 for dilution procedure Total Petroleum Hydrocarbon TPH Extraction from Water The difference between TPH Total Petroleum Hydrocarbon and TOG Total Oil and Grease is the polar organics are removed from the extract using silica gel The remaining hydrocarbons are the non polar components considered to be TPH 1 4 3 4 3 1 Follow the above procedure steps 1 5 for solvents heavier than water and 1 4 f
30. in order to read in the desired units The Analyzer contains three different user selectable calibration modes These are oFF uSEr or Edit Section 3 explains the calibration functions in detail 1 4 2 External Communication The InfraCal TOG TPH Analyzer supports communications to a PC printer or controller via an RS 232C asynchronous serial communications port This capability allows for collection of sample measurement data and instrument control by a host computer The RS 232 interface also allows for data transmission into an excel spreadsheet on a PC It also allows for multiple calibration tables if more than one table is being used with a single instrument Specification details for communication parameters are in Section 7 1 4 3 Recall Function Averaging Results The analyzer has the ability to store ten results for use with the averaging function or for local recall and display see Section 4 5 1 4 4 Printing the Result An optional printer can be connected to the analyzer through the RS 232C port located on the back To print the result momentarily press and release the CAL button Note that the Cal Lock switch must be in the I position The result is printed on one line The first number printed is a 5 digit sequence number The sequence number is followed by the result The remainder of the line contains the date time and day of the week To reset the print sequence number unplug the printer and plug it back in The next re
31. ith values up to 100 mg l in water could be as follows Stock solution 1 100 mg l divided by 10 for a 10 1 extraction in water 110 mg l 1 Pour half of the stock solution 5 ml into a 10 ml graduated cylinder 2 Fill with solvent up to 10 ml This will cut the 110 mg l standard in half to be 55 mg l 3 Repeat this again with the 55 mg l standard for a 27 5 mg l standard 10 This makes three standards 110 mg l 55 mg l and 27 5 mg l covering the operating range of 10 100 mg l for oil in water analysis 3 4 Calibrating in the Analyzer The Analyzer contains three different user modes in the calibration These are wSEr Edit or oF F If a factory calibration is installed there will be a fourth mode FAC In the oF F mode the instrument measures levels in arbitrary absorption units that are proportional to concentration levels Higher values indicate increased levels of hydrocarbons This mode should be used to collect raw data for the Edit mode or for comparing to an alternate method The Edit mode allows the user to edit an existing calibration table or to create one from scratch using absorption values obtained in the oF F mode In this mode standards or samples used to calibrate to an alternate laboratory method may be run several times and an average can be entered into the table The wSEr mode enters the calibration at the time the standards are presented to the analyzer 3 4 1 Selecting the Calibration Mode e
32. ity are determined by obtaining absorbance values from known samples and an internal point to point calibration table is prepared Section 3 so that actual concentration is directly presented on the display If the concentration ratio used during extraction typically 10 parts sample to 1 part hexane for liquid samples and 1 1 for soil samples is taken into account during calibration the display will read directly in the desired units Internal Reflectance Element IRE PA Source Filters I 1 Dual Detector A log I Figure 6 The Measurement of IR Absorption of an Oil Sample with a IR Platform 5 1 2 IR platform considerations 1 Only use IR Platforms supplied by Wilks Enterprise Inc made with infrared transmitting cubic zirconia ATR crystals Note Changing IR Platforms may require analyzer re calibration due to variances in IR Platform crystal characteristics 2 For best reproducibility use precision fixed volume pipettes or syringes 3 Always clean the IR Platform crystal with HPLC or Spectrophotometric grade hexane or other suitable solvent that leaves no residue 4 The InfraCal Model HATR T2 must be placed on a flat surface The bubble level and leveling feet are provided for this purpose 5 Repeatability and drift problems occur when the surface becomes contaminated with foreign matter or a charge buildup occurs These conditions can cause the sample to dry in a non uniform way or for the oil to migrate ove
33. l and grease can be extracted from water or soil through the use of an appropriate solvent The extracted hydrocarbons absorb infrared energy at acommon IR wavelength and the amount of energy absorbed is proportional to the concentration of the oil grease in the solvent This can be directly calibrated or converted to the amount of oil in the original sample The InfraCal TOG TPH Analyzer Model HATR T2 is designed as an equitable substitute for EPA Method 1664 for hexane extraction and gravimetric determination A fixed volume of the extract is placed directly in an IR Platform trough with a known path length and the solvent is allowed to evaporate When the IR Platform is placed on the sample stage an IR beam is internally reflected down the ATR crystal and the output is focused directly on the dual detector package Since there is an evanescent wave that penetrates the sample at each internal reflection point energy is absorbed at the analytical wavelength by the sample 19 The energy collected at the analytical wavelength I is reduced when compared to the energy collected at the reference wavelength Ip The oil concentration is determined by a calculation of the logarithm of the ratio of the light transmission at the reference wavelength to the light transmission at the analytical wavelength Beer Lambert law as shown in Figure 6 The Beer Lambert law assumes a linear relationship between absorbance and concentration Deviations from linear
34. lvent options Analytical balance that reads to 1 gram 16 4 3 2 4 3 3 Total Oil and Grease TOG Extraction from Soil Collect a soil sample directly in a washed and weighed to the nearest 0 1 gram EPA VOA 40 ml vial The sample should be about 34 of the volume of the vial Weigh the sample to the nearest 0 1 gram subtracting the tare weight of the vial If the sample is wet and clumpy add up to 5 grams of sodium sulfate Use the spatula to break up the clumps Add the same amount of solvent in mililiters as the soil sample weight in grams do not include the weight of the sodium sulfate ie for 11 2 grams of soil add 11 2 ml of solvent This will give a 1 1 extraction ratio Cap the vial with the Teflon side of the liner toward the sample Shake vigorously for 2 minutes Pour the solvent into the plastic air syringe with filter frit leaving as much of the soil in the vial as possible Place the plunger into the air syringe force the solvent through the filter frit into a clean container Eject 50 microliters of solvent extract using a pipette or syringe onto the center of the HATR T2 plate and press RUN For the CH Model remove the sample plate and lay on a flat surface Eject the standard from the pipette or syringe onto the center of the plate and allow the solvent to evaporate The evaporation time can be measured using the programmable timer Insert the IR sample plate into sample stage and press run Press twice if
35. multi function push button switches Connectors Power Switchcraft Model 760 plug or equivalent Communications 9 pin D Sub female Environmental Temperature Non operating O F 18 C to 125 F 52 C Operating 40 F 4 C to 110 F 45 C Humidity Relative 10 to 60 non condensing 23 6 4 6 5 T 7 1 Electrical Noise Rejection 60 dB minimum Drift Short term Ambient lt 1 Hr 0 3 of full scale Long term Ambient gt 1 Hr 0 1 of full scale Temperature 0 03 of full scale per degree C Repeatability 0 1 of full scale Response On Delay 5 10 15 or 20 second factory set intervals Measure Time 5 seconds Modes Local control or remote PC control Resolution Conversion 16 Bits 0 0015 Ranging Digital Ranging 256 step automatic ranging Analog Range 0 to 4 096 volts Answer Range Absolute 00 to 9999 Percent 0 0 to 100 0 Decimal 00 to 99 99 Measure Range Dependant on sample concentration ratio Measurement Accuracy 1 of full scale Measurement Repeatability 0 1 1 digit Memory Non volatile memory for calibration and configuration data Calibration e Electronic zero balance adjustment e Up to 20 point curve fitting calibration e Modes Edit Table Off Factory special order Analyzer Communications Interface Abstract The InfraCal TOG TPH Analyzer supports communications to a PC or other host via an RS 232C asynchronous ser
36. ncentration The table headings are followed by the balance value One additional line is printed for each calibration table entry The absorption and concentration values are given 4 Analyzing an Oil Sample These extraction procedures are a simplified version of ASTM and EPA methods The ASTM or EPA extraction methods may be used if desired 4 1 Analyzer Pre Check 1 For calibration allow the analyzer to warm up and stabilize for one hour 2 Ensure that the HATR T2 trough plate or IR sample plate is clean section 2 2 1 Use clean solvent to rinse the HATR T2 trough plate or IR sample plate after each use see section 5 1 3 for additional cleaning options 3 Perform a zero check section 2 2 2 4 Make sure glassware and sample containers are clean 4 2 10 to 1 Extraction Procedure for oil in water 4 2 1 Supplies needed for Extraction in water 125 ml Teflon wash bottle 13 100 ml stoppered graduated cylinder or Sample bottle graduated in mL ie 125 ml graduated bottles 125 ml stopper separatory funnel or sample bottles with septa caps for solvents heavier than water ie Vertrel MCA Hydrochloric HCI or sulfuric acid H2SO dilute with water 1 1 pH indicator strips or pH meter 10 ml or 25 ml Graduated cylinder depending on sample size Sodium sulfate Na SO ACS granular anhydrous For TOG only not necessary for TPH readings Glass funnel Whatman 40 filter paper 11cm or equivalent Silica gel f
37. ontrol The operation is identical to initiating a zero balance from the instrument control panel The user must insert the zero sample in the instrument prior to issuing this command If data logging is enabled the result will be returned on completion of the function The data format is identical to the RB command response The result can optionally be read with the RB command if data logging mode is not used 7 7 Remote calibration control Calibration data can be retrieved or set under remote control Due to the complexity of the calibration function and the need to utilize multiple calibration standards initial calibration can only be performed from the instrument panel Another approach is to use the host to generate one or more calibration curves from uncorrected data log results collected with the RA command This technique is extremely useful if the user desires to generate a calibration curve based on an average result of several measurements from a lot of each calibration standard The RC command is used to retrieve the current calibration table A Calibration table consists of zero to twenty entries The RC command can take the following forms RC Read entire calibration table RC O Read calibration table size RC n Read a single calibration table entry where n is the entry number 26 The RC 0 command response is C n where n is the number of calibration table entries from 0 to 20 If 0 the instrument is not calibrated Otherwise n
38. or TPH anhydrous 75 150 micrometers Disposable polyethylene pipette or equivalent 100 microliter syringe or pipette 5 mL syringe for use with prescription bottles Solvent see Appendix C for solvent options 4 2 2 Considerations e Make sure glassware for used for analysis is clean Any residual hydrocarbons in the glassware and sampling containers will be extracted and added to the TOG or TPH reading To check the glassware rinse with solvent then test the solvent rinse by ejecting 50 microliters onto the HATR T2 trough plate or IR sample plate A reading above 04 shows contaminated glassware e Oil and grease tends to adhere to the surfaces it comes in contact with Use the entire sample collected Either mix the solvent and sample in the sample collection container or rinse the sample collection container with a portion of the solvent to be used for extraction e The mechanical details of the extractions are a little different depending on whether the solvent is lighter than water hexane or is heavier than water Vertrel MCA but in all other respects the methods are identical NOTE Any hydrocarbons in the sample that have a lower boiling point than the extracting solvent will be lost in the evaporation process 4 2 3 Total Oil and Grease TOG Extraction from Water for Solvents Heavier than Water ie Vertrel MCA 1 Pour measured sample into separatory funnel Rinse the sample collection container and graduated cylinder with
39. or solvents lighter than water The Sodium Sulfate procedure is not necessary as the silica gel will remove any water in the solvent Place a filter paper in a filter funnel and add approximately 1 teaspoon of silica gel Pour extract from container though the silica gel into a clean container Eject 50 microliters of solvent extract using a pipette or syringe onto the center of the HATR T2 plate and press RUN For the CH Model remove the sample plate and lay on a flat surface Eject the standard from the pipette or syringe onto the center of the plate and allow the solvent to evaporate The evaporation time can be measured using the programmable timer Insert the IR sample plate into sample stage and press run Press twice if the timer is pre set to override the timer If the result is above the calibration range see section 4 4 for dilution procedure 1 to 1 Extraction Procedure for oil in soil Supplies needed 40 mL vials with Teflon faced caps 10 mL or 25 mL Graduated cylinder depending on sample size Sodium sulfate Na2S014 ACS granular anhydrous For TOG Only not necessary for TPH readings Glass funnel for TPH Whatman 40 filter paper 11cm or equivalent for TPH Silica gel for TPH anhydrous 75 150 micrometers 50 microliter syringe or pipette Disposable polyethylene disposable pipette or equivalent Plastic air syringe with filter frit and plunger or equivalent Sample spatula Solvent see Appendix C for so
40. r 22 Figure 10 The IR Sample Plates ssccssvssicaseesvesvanscdecevscnsac sneseasvessccsvarsevesesens 22 1 InfraCal TOG TPH Analyzer Overview 1 1 Introduction The InfraCal TOG TPH Analyzer is designed to measure solvent extractable material hydrocarbons or oil and grease by infrared determination in water or wastewater Models HATR T2 and CH are designed to correlate with EPA Method 1664 with hexane extraction and gravimetric determination The HATR T2 and CH have an evaporation step to accommodate solvents containing hydrocarbons such as hexane or Vertral MCA The HATR T2 uses a cubic zirconia crystal on which the oil film is deposited and measured by internal reflection The model CH uses a reusable IR sample plate with a sapphire window on which the oil is deposited and measured by transmission Hydrocarbons with boiling points lower than the extracting solvent used will be lost in the evaporation process A dual detector is used in the TOG TPH Analyzer to measure hydrocarbon concentrations at 3 4 micrometers 2940cm with a reference at 2 7 micrometers 3700cm 1 2 Basic measurement concept The InfraCal TOG TPH Analyzer makes use of the fact that hydrocarbons such as oil and grease can be extracted from water or soil through the use of an appropriate solvent and extraction procedure The extracted hydrocarbons absorb infrared energy at a specific wavelength and the amount of energy absorbed is proportional to the
41. r time once the hexane has evaporated These problems can be corrected as follows Clean the trough plate with methyl alcohol Fill the trough with enough methyl alcohol to cover the crystal Allow the crystal to soak for 10 seconds Dry the crystal with an anti static wipe or a foam swab intended for use with alcohol Check the zero value and re zero if necessary Section 2 2 This can be done each time a new sample is to be analyzed immediately prior to sample application 5 2 IR card reader sample stage description Model CH is supplied with a removable IR Card Reader sample holder and an integrated optics sensing system The sample stage includes the infrared source modulated and detector system positioned such that an elliptical energy beam is transmitted through the IR Card Reader crystal and focused directly on the detector sensing window 20 Detector Location Source Location Figure 7 The InfraCal TOG TPH Analyzer Model CH Sample Stage Side View Figure 8 The InfraCal TOG TPH Analyzer Model CH Top View 5 2 1 Card reader model CH measurement concept Model CH makes use of the fact that hydrocarbons such as oil and grease can be extracted from water or soil through the use of an appropriate solvent The extracted hydrocarbons absorb infrared energy at a common IR wavelength and the amount of energy absorbed is proportional to the concentration of the oil grease in the solvent This can be directly calibrated or
42. rt hexane for liquid samples and 1 1 for soil samples is taken into account during calibration the display will read directly in the desired units 5 2 2 Sample Filters Ip l4 Source Detectors Figure 9 The Measurement of IR Absorption of an Oil Sample with a IR Card Reader Infracal Sample Well Figure 10 The IR Sample Plate IR Card reader considerations Only use IR sample plates supplied by Wilks Enterprise Inc made with infrared transmitting sapphire windows For best reproducibility use precision fixed volume pipettes or syringes Always clean the IR sample plate window with HPLC or Spectrophotometric grade hexane or a suitable solvent that leaves no residue Hold the plate vertically flow a small amount of solvent down the plate and shake to ensure all oil is removed and that the solvent is dry For best results clean with methyl or ethyl alcohol and dry with an anti static wipe Differences in transmission characteristics between plates may introduce quantitative errors when multiple plates are used In this case check each clean IR sample plate for zero value after zeroing on one of the plates If the zero values are different zero to each plate prior to applying a sample for measurement Place the IR plate on a flat surface when applying a sample 22 Repeatability and drift problems occur when the window becomes contaminated with foreign matter or a charge buildup occurs These conditions
43. ry which retains the factory and user calibration tables could be erased from a voltage spike or surge on the 120 220VAC line The use of a surge protection device between the user s AC line and the 12V DC power supply is recommended to prevent the loss of calibration tables 2 1 3 Warm up time For normal operation it is recommended that the instrument be allowed to warm up for 1 hour prior to use However the analyzer is sufficiently stable after 15 minutes and meaningful measurements may be obtained at this time If the analyzer is used under the 1 hour warm up time frequent checking of the zero is recommended for best results The longer warm up time is recommended prior to making critical measurements and when performing analyzer calibration The TOG TPH Analyzer draws very little power and if used daily it can be left on at all times unless operated from an external battery pack 2 2 Zeroing the Analyzer For initial set up establish zero for the analyzer using the following procedure Once a zero has been established subsequent zero checks should use the zero check procedure described in section 2 2 2 2 2 1 Establishing Zero Ensure that the HATR T2 trough plate or IR sample plate is clean Clean the HATR T2 trough plate or IR sample plate with solvent after each use To clean the HART T2 trough plate add enough solvent to cover the HATR crystal Wipe slowly across the crystal in one direction with a clean anti static wipe to
44. s should be spaced apart by at least 10 absorption units 3 3 1 Preparing Volumetric Standards Supplies needed for volumetric calibration 125 ml Teflon wash bottle 10 ml graduated cylinder 40 ml vials with Teflon lined caps at least 3 for holding standards 100 microliter syringe Solvent see Appendix C for solvent options Calibration oil Below is a chart for mixing volumetric standards For water analysis with an extraction ratio of 10 1 the oil and grease is concentrated 10 times in the solvent The actual value of the standard is divided by 10 in order to match the concentrated value of the extract The water analysis column below makes this correction For standards below 1000 ppm 100 ppm for water samples it is best to mix a concentrated stock solution to be diluted for lower standards For example the desired range for a particular analysis is typically 10 ppm with values up to 100 ppm in water 1 Prepare a stock solution for 100 ppm for water analysis 10 ul oil in 10 ml of solvent 2 Pour half 5 ml into a 10 ml graduated cylinder 3 Fill with solvent up to 10 ml This will cut the 100 ppm standard in half to be 50 ppm 4 Repeat this again with the 50 ppm standard for a 25 ppm standard This makes three standards 100 ppm 50 ppm and 25 ppm within the operating range of 10 100 ppm 9 Actual ppm Corrected ppm for Oil Solvent 1 1 Extraction 10 1 extraction ratio soil analysis water analysis 4000 400
45. seisersopeseresiueirsessseserossrerosesisearosssssrsssssessss 10 3 4 Calibrating in the AnalyZet ce enice ireen ri anen EE E nE AE EEE E 11 3 4 1 Selecting the Calibration Mode eee cecceeceeseceseceseeeseseseseeecseesaeenaeseaeeeeesseeeseeeneeeaees 11 3 4 2 Setting the evaporation timer ee ee cee eeceseeseeeseeeseeesecesecseecseeeaeenseseaseesecsseesseeeeeaees 11 Timer Programming ccccccsseeeeeeee eee eeneeeeeeeeeeeeeeeneeeceeeeeeeeeenggseaeeeeeeeeeggaeseeeeeeeeeeagaeeseeeeeeeeseneseseeees 11 Overriding the Timer eserse aaneen aaaea aAa a Eanan E aE eE EEEE APARE REAA EnA AE EnA 12 3 4 3 Collectine calibrattom Gata csisscceis cecscssseceastescenss thacechetevencsesasdsabesgsiensssnctonbonssdsiesen cancsegbiaess 12 3 4 4 Entering Calibration Data into Edit program 0 eee ec eesececeseeceseeeseceaeeesecseeesneeeeeaees 12 3 4 5 User Calibration Mode Procedures eeceeccceesceesseeeeneeeeeeeeseessaeeeeaeeseaeeesaeessaeeeseeessaeeenaes 13 3 4 0 Calibration prnune s isteg tiniest de ena E see ies 13 4 Analyzing an Oil Sample ccsccsseceensseessnessneeseeesseesseeesneesneeneneneeenenessnesenessneesneenseessoess 13 4 1 Analyzer Pre CHeck2s3secdshtsias ste soxeeates ae Er ge E a E EEE E E Ea 13 4 2 10 to Extraction Procedure for oil in Water 0 eeceesceeeseeesneeeeeeeeneeeeaeeceaeeceaeecsaeeenaeeeeaeeenaes 13 4 2 1 Supplies needed for Extraction in water cece eseeseceeeeeeeseeeseceseceeeseeeseeeseeeseseseeeee
46. sult will print as sequence number 000001 2 Getting Started 2 1 Installation 2 1 1 Location The InfraCal TOG TPH Analyzer may be installed virtually anywhere It is not affected by vibration and it can operate over a broad range of ambient temperatures 40 F 4 C to 110 F 45 C Model HATR T2 must be level A bubble level and leveling feet are provided to level the analyzer 2 1 2 Power Requirements The analyzer is powered from a 12 volts d c power source A standard 12 volt power supply is provided with the analyzer and this may be operated from any grounded a c outlet line power requirements 100 250 VAC 50 60 Hz 0 5 0 3 amps When operating the TOG TPH Analyzer consumes approximately 8 watts 0 67 amps For field use the instrument may be connected to other sources of 12 volt d c power such as an external battery pack or the cigarette lighter output of an automobile contact Wilks Enterprise for details Plug in the external 12 volt supply to the power connector at the rear of the instrument When plugged in the instrument display will show init for a short time Once the power on initialization is complete the instrument displays idLE The TOG TPH Analyzer is now ready for use Note the connector is polarized with the center pole positive Failure to use the correct power supply or the correct cable can result in permanent damage to the analyzer and may invalidate the warranty The InfraCal internal memo
47. t has been used primarily as a replacement solvent for Freon in cleaning operations Because of its hydrocarbon absorption like hexane it must be evaporated prior to making the infrared measurement to determine TOG or TPH levels Recent tests have indicated that Vertrel MCA is a suitable solvent to use instead of hexane It reaches a stable level much quicker than hexane 1 1 2 2 vs 3 5 min and because of its lower boiling point fewer light end volatiles components are lost in the evaporation process Vertrel MCA has no ozone depleting potential is non flammable and has low toxicity As Vertrel MCA is heavier than water the solvent after extraction will rest on the bottom A microliter glass pipette can be used when preparing a sample however because of the weight of Vertrel the extract should be delivered to the sample platform or plate with a 50 microliter syringe rather than a pipette for analysis Wilks Enterprise Inc 25 Van Zant Street Suite 8F East Norwalk CT 06855 www WilksIR com Tel 203 855 9136 Fax 203 838 9868 info wilksir com tech wilksir com 30
48. ted by commas All commands are terminated by a carriage return character All data responses are comma separated ASCII fields terminated by a carriage return character The first field indicates the result type the remaining fields are the result Result types are B for balance results R for run results or C for calibration data The result format is determined by the presentation mode and is identical to the LED display data The Read Display Mode command returns a two character mode code Alphabetic characters can be sent in upper or lower case Response data is always upper case Command Set Command Description Response Examples RB Read balance B 1 025 B 0 865 RR Read displayed result R 27 5 R 315 R 1 873 RU Run same as RUN button None RA Run amp display uncalibrated result None BA Balance same as Zero switch None LR Enable results data logging None DR Disable results data logging None RM Read display mode MA MP MD or MR MA Set display mode to absolute None MP Set display mode to percent None MD Set display mode to decimal None MR Set display mode to ratio None WB lt params gt Set balance data None RC lt params gt Read calibration table See detailed description WC lt params gt Set calibration table None 25 CM Read Calibration Mode CD CE or CF CD Disable Calibration None CE Enable User Calibration None CF Enable Factory Calibration None ES Return error status E 0 E 2 RE System reset
49. ur 1 ml of solvent extract into a 10 mL graduated cylinder Add 9 mL of solvent for a 10 to 1 dilution 3 Mix and eject 50 microliters of solvent extract using a pipette or syringe onto the center of the HATR T2 plate and press RUN For the CH Model remove the sample plate and lay on a flat surface Eject the standard from the pipette or syringe onto the center of the plate and allow the solvent to evaporate The evaporation time can be measured using the programmable timer Insert the IR sample plate into sample stage and press run Press twice if the timer is preset to override the timer 4 Add a zero to the result on the InfraCal s digital display and record your reading 1 e if the result is 465 the extract value after dilution is 4650 ppm 5 This procedure may be repeated if the extract is still not within the calibration range Add two zero s to the InfraCal s digital display if two dilutions are performed Ne 4 5 Averaged Results Display The InfraCal Analyzer can display the average of up to ten sample measurements To use the averaging mode use the following procedure e Momentarily press the RECALL button once and ignore the result displayed e Analyze up to ten replicate samples using the measurement procedure described above e Momentarily press the RECALL button to display the average The next sample measurement will then start a new average accumulation The Analyzer alternatively can be configured to recall t
50. zero it is invoked during the normal RUN ZERO and CAL functions Press and release RUN and the timer value is displayed The timer will count down one second at a time The dot separating minutes and seconds flashes to indicate the timer is counting Once the timer reaches zero the display will read run during the sample measurement cycle The result is displayed on completion 11 The ZERO function is initiated by pressing and holding the ZERO button until the timer value is displayed The timer will count down as described above and bAL will then be displayed On completion the balance result is displayed The timer is also invoked during calibration each time the RUN button is pressed to analyze a sample Overriding the Timer For a zero check or to do a second reading on an evaporated sample the timer may be overridden To override the timer press and release the RUN button twice and the analyzer will go directly into the measurement cycle 3 4 3 Collecting calibration data Calibration data can be collected from standards section 3 3 or from actual samples compared to an alternate oil and grease measurement method section 3 2 2 If the data is to come from actual samples skip to section 4 for extraction procedures 1 Allow the analyzer to warm up at least one hour 2 Always zero the Analyzer prior to calibration or collecting data for calibration analysis see section 2 2 3 Make sure the calibration is in the oF F mo
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