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Sorbent Trap Analysis with RA-915M and M-324

1. 91 Onto O f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Appendix l Method 30B Spiked Sample Calculations Method 30B requires that 3 runs be conducted where one of the paired traps is spiked with a known quantity of mercury on section 1 These runs are used as the Field Recovery Test to demonstrate a suitable recovery for the spiked mercury These 3 runs can also be used as 3 of the RATA runs if the Relative Deviation of the 2 paired traps is sufficient when the spike amount is subtracted from the spiked trap and other requirements are met Here is an example demonstrating how these results might be calculated in a real world environment e Suppose for one run of the Field Recovery Test the following data was collected Trap A was unspiked collected 14 dry standard liters of sample and upon analysis was found to contain 58ng of mercury Trap B was initially spiked at 60ng collected 15 5 dry standard liters of sample and upon analysis was found to contain 126ng of mercury e First we will calculate the spike recovery for the spiked trap The first step will be to calculate the mercury concentration of the sample gas as indicated by the unspiked trap This will be 58ng 14 Liters 4 14ng L 4 14uUg dscm dry standard cubic meters e Next we need to subtract an amount from the spiked trap that was due to the gas sample that was deposited on it so we can see what s left and compare that to the am
2. For both locations the front plug must have minimum amount of particulate or discoloration from white color Please note Large amount of particulate or moisture on the front plug will skew the Total and speciation ratio and make the run invalid We have found that the aforementioned sampling procedures will yield the most consistent and reproducible results 99 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 1 SPECIATION TRAP ANALYSIS PROCEDURE RECOMMENDATIONS Flow SO Acid Gas Scrubber AGS S1 Oxidized Mercury Analytical Bed KCI S2 Oxidized Mercury Breakthrough Bed KCI S3 Elemental Mercury Analytical Bed Carbon S4 Elemental Mercury Analytical Bed Carbon Figure 1 Illustration of a Speciation Trap For full analytical procedure please refer to the Speciation Traps Analytical SOP 1 Clean the furnace and analyzer windows before heating up the furnace Calibrate analyzer as per method 30B using carbon as calibration substrate Change temperature set point on Watlow controller use up down arrow keys to 590 C The furnace must look almost dark if looking inside through the ladle entry hole Only one calibration curve is required for the analysis of AGS KCI and carbon Cover all sections with soda except for the AGS section Soda must be pressed using a sheet of Aluminum Foil Never place KCL on top of carbon Use upgraded pump station and set flow rate to 0 5
3. For coal ash standards weigh from 100 to 200 mg using a 1mg resolution balance Load standard into ladle spreading evenly on the mid to front bottom part of the ladle Cover with a layer of Ohio Lumex carbon then fill ladle to the top with sodium carbonate Wipe away excess sodium carbonate then compress ladle sample with foil Analyze as usual Analysis time is close to 120 seconds Results will be reported in Calculated ng g ppb column on an AS IS basis 51 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment O 9263 Ravenna Rd Suite A 3 HIO Twinsburg OH 44087 UMEX Toll Free 888 876 2611 APPENDIX C SORBENT TRAP ANALYSIS PROCEDURE Subject Mercury Emissions Monitoring Program Sorbent Trap Analysis Prepared by Analytical Laboratory of Ohio Lumex Company Revised on October 23 2013 52 Onto f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 1 INTRODUCTION TO THE ANALYSIS METHOD WITH THE RA 915M RP M324 MERCURY ANALYZER SYSTEM This document describes the procedure of sorbent trap analysis using the Ohio Lumex RA915M with the RP M324 attachment for total mercury Hg determination by thermal decomposition with atomic absorption and Zeeman Correction The analytical method at Ohio Lumex is based on the thermal desorption per EPA Method 7473 direct thermal desorption with atomic absorption and no gold amalgamation The method is applicable for t
4. 43 QOuio o UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment I Peel off carefully and scrape all debris off with knife Picture 7 17 Picture 7 17 m Dip hose in water to lubricate and insert onto quartz barb 1 2 inch Pictures 7 18 7 20 Picture 7 18 Picture 7 19 44 Oulo Da UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Picture 7 20 n Secure Carrier Gas Hose Guards Picture 7 21 Picture 7 21 Onto DS UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment O Heating cartridge replacement and reattaching cover do not forget to use the soft sealing gasket comes with replacement cartridge between heating cartridge and furnace Picture 7 21 Replicable heating cartridge Remove four screws positioned around the flange Picture 7 21 p Tighten Securely Picture 7 22 RP M324 Att Tmeman Spec Aow Ohiolurr REE ID IN i AS ae Picture 7 22 46 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 3 Heating cartridge cleaning Unscrew four small bolts holding cartridge flange to furnace Pull cartridge out Use Vinegar and weak solution of hydrogen peroxide 9 1 mixture to clean cartridge from excess of soda and iodine Leave cartridge in the mixture for 15 minutes wash with tap water and dry in the same position coil down as presented on pictures Pre
5. and d columns 14 Calibration is valid if calculated calibration points are within 10 of expected value AND calibration correlation coefficient R is 0 99 15 Give a name to the calibration and click save Example 10 10 13 Cal Curve 60 Onto f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 2 3 2 Calibration Criteria Multipoint calibration is required Three or more standards should be used to make a calibration curve An independent standard for example a NIST solid standard or a NIST traceable mercury standard from a separate lot will be analyzed to ensure the accuracy of the calibration The calibration criteria is 1 Calibrations must be performed on the day of the analysis before analyzing any of the samples 2 Three or more upscale calibration points must be used 3 The lowest point in the calibration curve must be at least 5 and preferably 10 times the MDL 4 The field samples analyzed must fall within a calibrated quantitative range and meet the performance criteria of Method 30B or PS 12B 5 For each calibration curve the value of the square of the linear correlation coefficient i e R must be 0 99 and the analyzer response must be within 10 of the reference value at each upscale calibration point 6 Following calibration and an initial calibration verification standard ICVS or a second source standard must be analyzed The measured value of th
6. 18 Onto DS UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment RAPID version 1 00 307 A Sample Analysis z Serviceability checkup TT aaa b if Md ae a zi O ni Jen baa C i 5 Instrument information Picture 3 3 5 Once the chart graph are open configure the view settings as seen below by clicking the gt lt icon Click Apply when finished Sample analysis window settings Data view settings Uae 7 Baseline interpolation by one point C by two points Number of points For mean and SD calculation Number of points for averaging Sample Concentration oar Units Units Decimals Decimals Plot view settings D plot Plot view Show Signal plot Color Color i Line Style Line Style Show on measurements Alldata Inthe specified interval Interval duration min 10 i Cancel Picture 3 4 19 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 6 Click the Table to the right of the plot icon Ls see Picture 3 5 Marked as 1 7 Make sure External amp Calibration are selected under operating cell amp operation mode respectively see Picture 3 5 Marked as 2 8 Click the Start button see Picture 3 5 Marked as 3 Note The Start button will change to Pause and the graph will begin taking readings Sample analysis File View Help wr r
7. A pages 45 49 Note With older versions of the software it is necessary to click a START and END button however the Manual Integration Method herein DOES NOT require this function 21 Ono UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 4 Remove the Standard sample from the atomizer once the Hg has been read by the analyzer Note The Hg is fully desorbed from the sample AFTER the peak returns to baseline Note The Signal Column indicates the baseline peak Picture 4 2 Sample analysis SAES File View Help Dla alaale s eee Operating cell Operation mode Current signal x mean Pause External Erate Ss 0 0 1 2 0 38 0 5 0 6 0 9 0 8 1 0 DA 0 0 0 2 0 5 0 4 0 0 pea TNA SODAN D A D Sample description Std_io ref data 10 Mass olume i N Sample description Blank refF data U Mass U Height z Interval s Integrate DE lete alibration settings Calculate calibration Processing Picture 4 2 5 Create a zoom box by clicking and dragging your cursor over the peak ensuring only the beginning and end of it lie within the zoom box 6 Click Integrate Picture 4 3 e Note The baseline signal will continue to count even when zoomed in e Note You may zoom in multiple times if necessary till you fee confident with your zoom box 22 UMEX Sorbent Trap Analysis with the Lu
8. PS 12B for the Ohio Lumex RA 915 RA 915M RP M324 Sorbent Trap Mercury Analyzers Method 30B requires that prior to sample analysis a Bias Test be performed on the mercury analyzer The PS 12B Method requires that a Spike Recovery Test be performed on the analyzer prior to analyzing samples using that method Since the two tests are very similar it is advantageous to perform them at the same time This document will outline the steps necessary to perform the Bias Test and then list the extra steps to provide a valid Spike Recovery Test The Method 30B Bias Test is required in order to show that the analytical instrument is able to measure both elemental and oxidized mercury without bias Three sorbent traps spiked with elemental mercury at each of two levels a low level and a high level between which actual samples are expected to fall are analyzed to demonstrate instrument accuracy in quantifying elemental mercury Then two sets of three standards made with aqueous mercury solutions are analyzed at the same mercury levels as the sorbent traps As the water evaporates during analysis for a short instance the mercury exists as a mercury salt oxidized mercury until it is then broken down thermally and measured Here are steps to perform a Bias Test on the Ohio Lumex Sorbent Trap Mercury Analyzer 1 Put the instrument in its most sensitive mode profile 1 or in the configuration that you will use for analyzing 30B samples 2 Calibrate
9. e Note ref data refers to the expected mass of the Standard being used e Note When analyzing sorbent traps the Mass Volume will ALWAYS be 1 Sample analysis File View Help aae Beam s seep sO ea cs a Opersting cell Operation mode Curren t signa Graph description x mean 2 949 Pause Calibration A 0 524 Signal Time E Signal ParamD 16 04 2013 10 35 51 2 92 0 0 151 16 04 2013 10 35 50 2 97 0 0 150 16 04 2013 10 35 49 E FL Fd 0 0 149 16 04 2013 10 35 45 2 59 0 0 145 16 04 2013 10 35 47 2 93 0 0 147 16 04 2013 10 35 46 2 20 0 0 146 16 04 2013 10 35 45 3 15 0 0 145 16 04 2013 10 35 44 3 24 0 0 144 16 04 2013 10 35 43 3 05 0 0 143 16 04 2013 10 35 42 3 15 0 0 142 16 04 2013 10 35 41 3 07 0 0 141 16 04 2013 10 35 40 3 16 0 0 140 16 04 2013 10 35 39 3 09 0 0 139 16 04 2013 10 35 35 3 35 0 0 136 16 04 2013 10 35 37 2 22 0 0 137 16 04 2013 10 35 36 3 42 0 0 136 16 04 2013 10 35 35 3 16 0 0 135 16 04 2013 10 35 34 4 15 0 0 134 16 04 2013 10 35 33 2 97 0 0 133 16 04 2013 10 35 32 3 70 0 0 16 04 2013 10 35 31 0 0 IEL LNA DNI I N eee ou rt reF data 10 Blank T iil Height Measur Interval s AD ref data E Pe Integrate Mark Calibration settings Calibration list Processing Picture 4 1 3 Prepare your first Hg Standard amp place it inside the atomizer chamber
10. remove contact lenses Get medical attention if symptoms persist Most important symptoms effects acute and delayed SDS_US SDS000000960 135 Version 1 0 AVANTOR Revision date 05 12 2014 Symptoms Harmful if inhaled Irritating to eyes respiratory system and skin indication of immediate medical attention and special treatment needed Treatment Treat symptomatically Symptoms may be delayed 5 Fire fighting measures General fire hazards No unusual fire or explosion hazards noted Suitable and unsuitable extinguishing media Suitable extinguishing Use fire extinguishing media appropriate for surrounding materials media Unsuitable extinguishing None known media Specific hazards arising from None known the chemical Special protective equipment and precautions for firefighters Special fire fighting Move containers from fire area if you can do so without risk Use water procedures spray to keep fire exposed containers cool Special protective equipment Firefighters must use standard protective equipment including flame for fire fighters retardant coat helmet with face shield gloves rubber boots and in enclosed spaces SCBA 6 Accidental release measures Personal precautions Keep unauthorized personnel away Keep upwind Ventilate closed spaces protective equipment and before entering them Avoid inhalation of dust Do not touch damaged emergency procedures containers or spilled material unless we
11. 10 2013 17 08 19 23 10 2015 17 08 18 23 10 2013 17 08 17 23 10 2013 17 08 16 23 10 2013 17 08 15 23 10 2013 17 08 14 23 10 2013 17 08 13 23 10 2013 17 08 12 23 10 2015 17 08 11 23 10 2013 17 08 10 23 10 2013 17 08 09 23 10 2013 17 08 08 23 10 2013 17 08 07 23 10 2013 17 08 06 23 10 2013 17 08 05 23 10 2013 17 08 04 lt rer 2 mnnn Pr Picture 4 11 Integrate Mark Delete Save 3 Select the proper calibration curve to apply to the forthcoming sorbent trap samples from the drop down menu then click Apply Picture 4 12 Details Picture 4 12 28 Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 4 Prepare sorbent trap sample according to pages 48 to 53 and follow the Manual Integration Method or Mark amp Integrate Method to analyze your sample Picture 4 13 Picture 4 13 5 Saving you data When it comes time to save your data press the Save button and label your graph under Graph description A save disk icon will appear next to all saved runs PROGRAM DOES NOT SAVE AUTOMATICALLY so be sure to save data early and often Picture 4 14 File View Help Lali EA ea Gare 2s Operating cell Pause E nal 23 10 2013 17 16 45 23 10 2013 17 16 44 23 10 2013 17 16 44 23 10 2013 17 16 42 23 10 2013 17 16 41 23 1
12. 2 Make sure that the standards being used are good and run a 5 or 6 point calibration ranging from 5ng to 100ng or 300ng using proper pipetting techniques Use the average of the response factors of your standards to determine your calibration curve The RSD of these response factors should not be more than 5 or 6 if the analyzer is operating properly Run a continuing calibration verification standard after each pair of traps to limit the amount of data lost if a standard fails Method Detection Limit MDL It is important to have a good MDL determination Weighing out the amount of carbon used in each replicate can decrease precision variances due to the native mercury present in the carbon To assure that the area for each replicate represents mercury measured and not baseline noise you need to isolate the baseline from the peak either by manually integrating the peaks or just waiting 30 to 35 seconds before starting integration after the sample has been inserted in the oven Standards at 3 ng are frequently used for MDL studies 88 Onto i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Sample Preparation When traps are analyzed the glass can be cut after removing the section 1 materials so that the section 2 materials can be removed without dragging them through any debris that may be in the front half of the glass tube This can help avoid false high breakthrough readings 30 B is the Reference
13. Depending on the spare space in the ladle the plug can be tested with sorbent together or tested individually For a speciation trap 5 sections the plug prior to the sorbent section is usually tested together with the sorbent in one ladle Description and analysis procedure for Ohio Lumex speciation traps are described here 1 Speciation trap AGS Hp2 absorption Carbon SO Acid Gas Scrubber AGS S1 Oxidized Mercury Analytical Bed KCl S2 Oxidized Mercury Breakthrough Bed KCI S3 Elemental Mercury Analytical Bed Carbon S4 Elemental Mercury Analytical Bed Carbon Figure 3 Illustration of a speciation trap 115 QOuio i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment The speciation trap is a 5 sections trap The first section is called the AGS section followed by two oxidized mercury absorption sections and two carbon sections As shown in Figure 7 The first 3 sections will be analyzed at temperature 580 C while the rest 2 sections will be performed at regular profile 1 temperature i e 680 C The operation procedure is described below 1 Warm up the oven to 580 C set up the flow to 2L min Let system stabilize until no baseline drifting and RSD value is stable 2 Perform calibration Pull carbon into ladle load Hg standard on carbon bed cover the bed with Sodium Carbonate use aluminum foil to press the material tightly Press the START bution insert the
14. Method Keep in mind when performing RATAs against CEMMs that below a certain level the CEMM will not be able to measure as accurately as the sorbent traps Even if the data passes the numbers might not match Remember 30 B is the reference method and if all is working properly the CEMM must match the 30 B results and not the other way around Summary of Low Level Techniques Method e Samples from Sources lt 0 5 ug dscm don t have to be within the bounds of the Initial Calibration or the Bias Test e Calculate Low Level Samples with the Low Level Standard The Breakthrough Limit Increases based on the concentration of the source See STS RATA Criteria The Limit for Relative Deviation for Paired Traps Increases from 10 to 20 for sources that are lt 1 0 ug dscm Spike Levels are Based on Expected Sample amounts no Penalty for Failing e Field Recovery is Calculated using the Average of the 3 Runs e CFR 40 Only Requires Agreement Within 1 0 ug dscm 89 Ono f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Summary of Low Level Techniques PS 12B e Sources lt 1 0 ug dscm are allowed up to 20 Relative Deviation Between Paired Traps or lt 0 03 ug dscm maximum variance e Spike Levels Should be 50 to 150 of Expected Sample Amount No Penalty for Missing e Spike Recovery must be a Generous 75 to 125 e Sample Amount Section 1 plus Section 2 Summary of Low Level Techn
15. Mrecoverea Mass of spiked Hg recovered in Analytical Bias or Field Recovery Test ug Ms Total mass of Hg measured on spiked trap in Field Recovery Test ug Mspikead Mass of Hg spiked in Analytical Bias or Field Recovery Test ug my Total mass of Hg measured on unspiked trap in Field Recovery Test ug R Percentage of spiked mass recovered RD Relative deviation between the Hg concentrations from traps a and b vs Volume of gas sampled spiked trap in Field Recovery Test dscm Vt Total volume of dry gas metered during the collection period dscm for the purposes of this method standard temperature and pressure are defined as 20 C and 760 mm Hg respectively Vu Volume of gas sampled unspiked trap in Field Recovery Test dscm 121 Omog UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 12 2 Calculation of Spike Recovery Analytical Bias Test Calculate the percent recovery of He and HgCl using Equation 30B 1 R a Premera 100 Eq 30B 1 a 12 3 Calculation of Breakthrov sh Use Equation 30B 2 to calculate the percent ugh to the second section of the sorbent trap 100 Eq 30B 2 M B 12 4 Calculation of Hg Concentration Calculate the Hg concentration measured with sorbent trap a using Equation 30B 3 p Gm m C Eq 30B 3 V For sorbent trap b replace C with C in Equation 3058 3 Report the average concen
16. SS e ee et GS Se Sample description I Std _i0 refF dsts io Massfvolume J l mM Sample descript Blank ref data Units SS I Units l zJ Processing Picture 4 7 25 UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 4 Once the peak has returned to baseline click Mark and Integrate to finish the run a Note The Mark and Integrate button will revert back to Mark once clicked Picture 4 8 Sample analysis File view Help Aaaale Ae a a a aawa ee 17 04 2013 15 26 34 17 04 2013 15 26 33 17 04 2013 15 26 31 17 04 2013 15 26 30 17 04 2013 15 26 29 17 04 2013 15 26 29 17 04 2013 15 26 27 17 04 2013 15 26 26 17 04 2013 15 26 26 17 04 2013 15 26 24 17 04 2013 15 26 24 17 04 2013 15 26 22 17 04 2013 15 26 21 17 04 2013 15 26 21 17 04 2013 15 26 19 17 04 2013 15 26 15 17 04 2013 15 26 17 17 04 2013 15 26 16 17 04 2013 15 26 15 gbo ooo pooooddgaoooooONS Yoooooo0o0000000000 NADADNNND AD D D UNDO No0 a W oa a ND e A a a A OONNONONANON YA N OS 1 Sample description Std_10 ref data 10 Massf olume 1 N Sample descript Blank Processing Picture 4 8 5 Repeat steps 2 thru 4 till you ve ran at least three Hg standards 6 Mark the check box next to each Standard you want used in your calibration amp click Calculate calibration Picture 4 9 Sampte eee File View 17
17. be 7 24 Onto or UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Sample ee File View se eal ed Roa T at sce oe S Fe ge I a aa ee ee ee ee ee ee ee ae ee ee a riM ea rer ere nr are MMMM ere eer eer ee ane gt ee aaa ee eee ee eee T MMMM reenact ere nr re eer aaa ec ere eee ea rw d N A ph pod pd pb pb pb pd pb jb jb pd pab jb jb pd b jah jb fh jab pah Processing Picture 4 6 3 Prepare first Hg Standard as outline on pages 45 49 click Mark then place the ladle inside atomizer chamber Picture 4 7 a Note The Mark button will change to Mark and Integrate once clicked Sarn E le analysis File Help Operating cell CE eS mode Current Pause Estermsi Calibration Cae ee aS SS ee pere er S Ee Se eya Ee PEE E PPE AE ee E PE SS Pe SE re Se g E e e ee ee e n ee 2o AN a ee ee a TD ee ee eee ee SS A a Ee Se aa a a ae CE a ee ee aaa Oe Se ee eee ee SS ee a a 45 eS a Se ee ee ee ee ee Se Oe ee SS Se ee ee se SS a M i a l X X X i li il A E l X Xi X i i al il l l l X X X l i M li Ml i i E 2s amp 5s6re i B OOPERIT TAE CERU ee FEE ee ee ee eS eS q e OS SS gt ee Se
18. current profiles for the Ohio Lumex M324 pump station with an EZ Zone Controller Table 1 Profiles and Settings of an EZ Zone Controller Profiles Starting Test Range Duration Temp ng sec 1 2 300 10 100 2 000 2 10 4 000 120 3 l 5 000 10 000 350 4 10 000 30 000 700 es 2 300 180 220 EZ Zone Controller settings for speciation traps only No profile configured parameters must be adjusted manually 57 Onto f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 2 3 Analyzer Calibration A certified analyzer is used to test sorbent traps The analyzer certificate provides the information on Method Detection Limitation MDL bias and spike recovery study results MDL is the minimum amount of the analyte that can be detected and reported lt is statistically derived from replicate low level measurements near the analytical instrument s detection level The bias test demonstrates the analyzer s ability to recover and accurately quantify Hg and HgCl2 from sorbent media The bias test is performed at a minimum of two distinct sorbent trap Hg loadings that represent the lower and upper bound of sample Hg loadings from application A Spike recovery study is required by Performance Specification 12B PS 12B It shows the ability of laboratory to recover and quantify Hg from sorbent media traps spiked with elemental mercury The analyzer certificate is available upon customer reques
19. disk to cut trap Picture 6 1 and break glass open just above the first plug and remove the plug with a glass wool extractor Picture 6 2 Picture 6 1 Picture 6 2 Picture 6 3 2 Use gloves when handling sorbent traps Carefully remove the glass wool plug Picture 6 4 and discharge sorbent on a fresh 8 5 x 11 inch piece of printer paper folded in half Picture 6 5 Picture 6 4 Picture 6 5 34 Onto DS UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 3 Roll up the glass wool plug in a small piece of aluminum foil Picture 6 6 Be sure no glass wool is exposed Picture 6 7 Picture 6 6 Picture 6 7 4 Place the plug in the ladle along with the carbon A second piece of folded 8 5 x 11 inch printer paper should be placed under the ladle to catch any spilled carbon Picture 6 9 Picture 6 9 35 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 5 Sprinkle sodium carbonate soda on top ensuring no carbon is exposed Wipe away any excess soda with glass wool extractor or spatula tool F Po fE PA hy Picture 6 10 Picture 6 11 6 Again cover loaded ladle with fresh foil and apply slight finger pressure to oress pack down the sample The picture below shows a properly prepared sampled ready for analysis Picture 6 12 36 Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Section 7 Maintenance Cle
20. granular sodium carbonate is ALWAYS placed on top of the sorbent media to capture the acid gas and eliminate the acid gas interferences Calibration substrate is the same media in the sorbent trap If a different substrate is used as the calibration purpose calibration adaptability to the different media must be demonstrated before analyzing any trap 3 ANALYTICAL PROCEDURE DETAILS The sorbent trap tube end cap is removed The empty tube before the first plug is cut down by the trap cutter blade Using the tweezers or extractor the glass wool plug at the front of the appropriate sorbent bed is carefully removed and separated from the sorbent fraction The sorbent is transferred into a quartz ladle and then covered with anhydrous sodium carbonate The ladle is inserted into the analyzer thermo catalytic conversion chamber As a result elemental mercury Hg is liberated into the gas stream and oxidized mercury Hg is converted from a bound status to the atomic status by thermal decomposition in the furnace and is then detected by atomic absorption with Zeeman correction The mercury concentration is measured and recorded using an automated data collection system Both the glass wool plug and the sorbent of each section are analyzed and the final Hg mass is figured by adding the measurements together 103 QOuio i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment The procedure for the trap analysis is d
21. in Gaithersburg Maryland Profile A temperature control program loaded into controller by Ohio Lumex Company prior to selling the system RATA Relative Accuracy Test Audit Sorbent Media used in traps to adsorb mercury May be halogenated or non halogenated carbon Trap Glass tube packed with one two or three beds of carbon sorbent held in place and separated by glass wool The sample trap is placed in the sampling probe and flue gas is pulled through the sample trap The carbon in the trap adsorbs mercury which is then used to determine the mercury concentration in the flue gas 5 CALCULATIONS AND DATA ANALYSIS All calculations and data analysis are explained in section 12 0 of Method 30B These calculations are listed below Nomenclature The terms used in the equations are defined as follows B Breakthrough Bws Moisture content of sample gas as measured by Method 4 percent 100 Ca Concentration of Hg for the sample collection period for sorbent trap a ug dscm Cy Concentration of Hg for the sample collection period for sorbent trap b ug dscm Ca Hg concentration dry basis ug dscm Crec Concentration of spiked compound measured ug m3 Cw Hg concentration wet basis ug m3 m Mass of Hg measured on sorbent trap section 1 ug 120 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment m Mass of Hg measured on sorbent trap section 2 ug
22. ladle into the oven watch the Hg release process Press the END when no more Hg come out and RSD value comes back to initial value Each run takes about 200 seconds Take a few Hg Standard tests for example 5 ng 10ng 20ng 5Ong Calibrate the system and check the calibration by loading a second standard Pull some Potassium Chloride into a ladle load a Hg standard on it Make sure the Hg mass is within the above calibration range Cover the materials with sodium carbonate and finger press them tightly through a piece of aluminum foil Insert the ladle into the oven and test it The Hg recovered from this test should be with 10 of the original loading Otherwise troubleshoot the system 3 Test the trap AGS section section 0 and first 2 oxidized mercury absorption sections section 1 and 2 116 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 4 Cap the remaining trap section 3 and 4 label it clearly and leave it away fora later test 5 Take the other speciation trap repeat step 3 and step 4 until all traps are finished Do standard verification 6 Bring the oven temperature to 680 C calibrate profile 1 7 Test the remaining parts of each trap section 3 and section 4 under profile 1 condition 8 Do standard verification at the end Save file and report the results The analysis procedure is shown in Figure 4 Figure 4 Analysis of a Speciation T
23. the sorbent Remove the aluminum foil from the ladle before analysis 59 Onto i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 5 Click the Mark button located in the lower left hand portion of the software window and immediately insert the prepared ladle into the furnace Note The Mark button will change to Mark and Integrate 6 The mercury signal is shown as red on the graph The reading of the current value is shown in the box to the right of the graph in the Signal column 7 Once the current value readings have spiked and returned to the original starting point and the RSD reading value is around the originally static value click the Mark and Integrate button located in the lower left hand portion of the software window to stop the analysis run 8 Remove the ladle from the furnace and place on a heat resistant surface aluminum foil Once cooled dispose ladle contents into a heat resistant metal tray 10 Repeat steps 1 thru 9 until three or more calibration points have been run 11 CREATING CALIBRATION CURVE Click the check mark box in the far left column next to each calibration point you want used in the calibration curve 12 Click the Calculate calibration button in the lower right hand portion of the software window 13 On the pop up window under Data view click Table view and use the left to right scroll bar to locate the Calculated ng g
24. 0 2013 17 16 40 23 10 2013 17 16 40 23 10 2013 17 16 38 23 10 2013 17 16 37 23 10 2013 17 16 36 23 10 2013 17 16 36 23 10 2013 17 16 34 23 10 2013 17 16 34 23 10 2013 17 16 33 23 10 2013 17 16 32 23 10 2013 17 16 31 Mass Volume Units Concentration Units Height Interval s 1 0 mg 753 5 ng g 0 1 30745 00 3074 1 0 mg 7388 0 na a 1 0 30735 00 30735 1 0 mg 10590 0 na a 0 0 30726 00 3072 ur eee Integrate Mark n lt P ptatistics Choose Calibration Measurement database f Picture 4 14 29 Ouro Da UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 6 Retrieving your data To access your saved data press the Measurement database button and choose how you d like to export your data Pictures 4 15 and 4 16 23 10 2013 17 19 40 23 10 2013 17 19 39 23 10 2013 17 19 38 23 10 2013 17 19 37 23 10 2013 17 19 36 23 10 2013 17 19 35 23 10 2013 17 19 34 23 10 2013 17 19 33 23 10 2013 17 19 32 23 10 2013 17 19 31 23 10 2013 17 19 30 23 10 2013 17 19 29 23 10 2013 17 19 28 23 10 2013 17 19 27 23 10 2013 17 19 26 23 10 2013 17 19 25 Picture 4 16 30 Ouio Sa Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Section 5 Ladle Preparation 1 Universal for 6mm and 10 mm length traps Ladle for Sorbent Trap testing placed on folded 8 5 x 11 inch printer paper Picture 5 1 2 For calibrat
25. 00 107 Onto UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 3 3 Analyzer Calibration A certified analyzer is used to test sorbent traps The analyzer certificate provides the information on Method Detection Limitation MDL bias and spike recovery study results MDL is the minimum amount of the analyte that can be detected and reported It is statistically derived from replicate low level measurements near the analytical instrument s detection level The bias test demonstrates the analyzer s ability to recover and accurately quantify Hg and HgCl2 from sorbent media The bias test is performed at a minimum of two distinct sorbent trap Hg loadings that represent the lower and upper bound of sample Hg loadings from application Spike recovery study is required by Appendix K to Part 75 It shows the ability of laboratory to recover and quantify Hg from sorbent media traps spiked with elemental mercury The analyzer certificate is available upon customer request lt is important to clean ladles and tools before testing any standards or samples Mercury deposited on the ladle would influence the calibration and testing By inserting an empty ladle into a heated furnace Temperature gt 500 C for at least 90 seconds any potential mercury contamination on the ladle will be removed The glass wool extractor and tweezers should be cleaned by a 5 seconds torch burning Calibration sorbent media must be stored in a sealed
26. 04 2013 14 59 08 17 04 2013 14 59 07 17 04 2013 14 59 06 17 04 2013 14 59 05 17 04 2013 14 59 04 17 04 2013 14 59 03 17 04 2013 14 59 02 17 04 2013 14 59 01 17 04 2013 14 59 00 17 04 2013 14 55 59 17 04 2013 14 58 55 17 04 2013 14 58 57 17 04 2013 14 55 56 17 04 2013 14 55 55 17 04 2013 14 55 54 17 04 2013 14 55 53 17 04 2013 14 56 52 17 04 2013 14 58 51 17 04 2013 14 55 50 f Mass olume j 1 N Sample descript Blank 5 g asa Height Measurement Date Time Interval s 3 Std_100 EF 3943 1 1 7 04 2013 14 51 50 333 00 433 00 2 Std_50 EN 2079 0 17 04 2013 14 51 50 184 00 276 00 1 sStd_10 S 399 4 16 04 2013 15 08 58 6365 38 6404 95 Measurement is suspended Picture 4 9 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 7 Under Data view click Table view amp use the scroll bar to locate the Calculated ng g mass per each Standard used in the calibration 8 Once satisfied name your calibration and click Save Picture 4 10 Calibration results Ew rrr Correlation coef Residual standerd deviation Calibration S Sbisnk t Picture 4 10 27 4 3 Analyzing Sorbent Trap Samples 1 Select Analysis from the Operation mode drop down menu 2 Choose your just completed calibration by clicking the Choose calibration button Picture 4 11 N Sample description 23
27. 1 0 Revision date 05 12 2014 No data available 1 0 No data available THE INFORMATION PRESENTED IN THIS MATERIAL SAFETY DATA SHEET MSDS SDS WAS PREPARED BY TECHNICAL PERSONNEL BASED ON DATA THAT THEY BELIEVE IN THEIR GOOD FAITH JUDGMENT IS ACCURATE HOWEVER THE INFORMATION PROVIDED HEREIN IS PROVIDED AS IS AND AVANTOR PERFORMANCE MATERIALS MAKES AND GIVES NO REPRESENTATIONS OR WARRANTIES WHATSOEVER AND EXPRESSLY DISCLAIMS ALL WARRANTIES REGARDING SUCH INFORMATION AND THE PRODUCT TO WHICH IT RELATES WHETHER EXPRESS IMPLIED OR STATUTORY INCLUDING WITHOUT LIMITATION WARRANTIES OF ACCURACY COMPLETENESS MERCHANTABILITY NON INFRINGEMENT PERFORMANCE SAFETY SUITABILITY STABILITY AND FITNESS FOR A PARTICULAR PURPOSE AND ANY WARRANTIES ARISING FROM COURSE OF DEALING COURSE OF PERFORMANCE OR USAGE OF TRADE THIS MSDS SDS IS INTENDED ONLY ASA GUIDE TO THE APPROPRIATE PRECAUTIONARY HANDLING OF THE MATERIAL BY A PROPERLY TRAINED PERSON USING THIS PRODUCT AND IS NOT INTENDED TO BE COMPREHENSIVE AS TO THE MANNER AND CONDITIONS OF USE HANDLING STORAGE OR DISPOSAL OF THE PRODUCT INDIVIDUALS RECEIVING THIS MSDS SDS MUST ALWAYS EXERCISE THEIR OWN INDEPENDENT JUDGMENT IN DETERMINING THE APPROPRIATENESS OF SUCH ISSUES ACCORDINGLY AVANTOR PERFORMANCE MATERIALS ASSUMES NO LIABILITY WHATSOEVER FOR THE USE OF OR RELIANCE UPON THIS INFORMATION NO SUGGESTIONS FOR USE ARE INTENDED AS AND NOTHING HEREIN SHALL BE CONSTRUED AS A RE
28. 11 8 39 100 x 0 013 1 31 For sources with mercury concentrations gt 1ug dscm the maximum allowable Relative Deviation between the 2 traps is 10 so in this case with the Relative Deviation at 1 31 this run easily meets the requirement for a good RATA run as far as Relative Deviation is concerned For sources with mercury concentrations less than or equal to 1 0ug dscm the maximum allowable Relative Deviation between the 2 traps is 20 93 QOuio i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Appendix J SOP to calculate R squared per PS 12B and Method 30B requirements After you finish the multipoint calibration and save the date 1 Export to Excel and open Excel file 2 Separate cut and paste Calibration Standards Data and Area Data in two columns next to each other Note the data must be a numerical value delete the Std__ part for the standard part of the data 3 Select both columns and click on Chart Wizard 4 Select XY scatter and chart sub type Scatter with data points connected be smooth lines 5 Click Finish 6 On the graph position mouse on the line and right click 7 Select Add Tredline go to Options and check Display R squared on chart 94 Onto UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Appendix K Troubleshooting Sorbent Traps in case of Breakthrough and or Spike Loss The following is
29. 3 85 QOuio i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment This method also allows if absolute difference between concentrations from paired traps is lt 0 03 ug ms3 Spike Recovery Similar to method 30 B the PS 12B method says that spike levels should be matched to the expected sample amounts 50 and similarly there is no penalty for failure The PS 12B spike recovery limits are calculated on each trap but are wider than the 30 B limits at 75 to 125 of the actual spike amount These things make it difficult to fail the spike recovery provisions of this method PS 12B Sample Amount Keep in mind that for PS 12B the sample amount is defined as the sum of the section 1 and section 2 mercury masses Breakthrough Under the new Mats Rule 40CFR part 63 Subpart UUUUU sect 4 1 2 2 the breakthrough criteria is as shown below when performing a RATA STS RATA Criteria Section 2 breakthrough depends on stack gas Hg concentration The allowable breakthrough is lt 10 of Section 1 mass if HG is gt 1 uaii lt 20 of Section 1 mass if HG is gt 0 5 and lt 1 uaia lt 50 of Section 1 mass if HG is gt 0 1 and lt 0 5 aa 3 There is no breakthrough criterion if HG is lt 0 1 ug m 86 Onto UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Optimizing the Measurement System for Low Level Analysis While optimizing the measurement system used for 30 B an
30. A Not regulated 15 Regulatory information US federal regulations TSCA Section 12 b Export Notification 40 CFR 707 Subpt D US OSHA Specifically Regulated Substances 29 CFR 1910 1001 1050 None present or none present in regulated quantities CERCLA Hazardous Substance List 40 CFR 302 4 None present or none present in regulated quantities Superfund amendments and reauthorization act of 1986 SARA Hazard categories x Acute Immediate Chronic Delayed Fire Reactive E Pressure Generating SARA 302 Extremely hazardous substance None present or none present in regulated quantities SARA 304 Emergency release notification None present or none present in regulated quantities SDS_US SDS000000960 140 Version 1 0 AVANTOR Revision date 05 12 2014 SARA 311 312 Hazardous chemical Chemical identity Threshold Planning Quantity SODIUM CARBONATE 500 ibs SARA 313 TRI reporting None present or none present in regulated quantities Clean Water Act Section 311 Hazardous Substances 40 CFR 117 3 None present or none present in regulated quantities Clean Air Act CAA Section 112 r Accidental Release Prevention 40 CFR 68 130 None present or none present in regulated quantities US state regulations US California Proposition 65 No ingredient regulated by CA Prop 65 present US New Jersey Worker and Community Right to Know Act No ingredient reguiated by NJ Right to Know Law present US Mas
31. Be sure no sorbent is exposed through the sodium carbonate 5 The ladle is now ready for analysis and may be run in accordance with steps 5 thru 8 listed under section 3 3 1 Calibration procedure Note The glass wool plug wrapped into aluminum foil may be analyzed separately if both the plug and the sorbent don t fit into a single ladle Some traps come with dust pre filter or acid gas scrubber AGS section The pre filter and AGS are part of the total mercury collected during sampling however they are tested and reported independently from the other sorbent sections 62 Onto or UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Description and analysis procedures for Ohio Lumex Sorbent Traps 1 PS 12B Trap Figure 1 is an illustration of a three section PS 12B sorbent trap These traps are commonly used for compliance reporting The first section is the primary flue gas mercury capture the second section is the breakthrough section and the third section is a spiked QA QC section According to flow direction each sorbent section is labeled as 1 S2 and S3 while the glass wool plugs are labeled P1 P2 P3 and P4 respectively The analysis flow chart of a PS 12B trap is illustrated in Figure 1 2 Flow ERE EE hi Pl P2 P3 P4 Figure 1 Illustration of a PS 12B Trap Figure 1 2 Analysis procedure for PS 12B Traps 63 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and
32. COMMENDATION TO INFRINGE ANY EXISTING PATENTS OR TO VIOLATE ANY FEDERAL STATE LOCAL OR FOREIGN LAWS AVANTOR PERFORMANCE MATERIALS REMINDS YOU THAT IT IS YOUR LEGAL DUTY TO MAKE ALL INFORMATION IN THIS MSDS SDS AVAILABLE TO YOUR EMPLOYEES 142 MATERIAL SAFETY DATA SHEET Ohio Lumex Company Inc 9263 Ravenna Rd Unit A 3 Twinsburg Ohio 44087 Phone 330 405 0837 Emergency Phone 330 405 0837 Section I PRODUCT NAME Activated Carbon Type K 2050 1 Section II HAZARDOUS INGREDIENTS Name CAS Number By Weight l1 Carbon 7440 44 0 gt 90 Activated Carbon Non Regulated 2 Iodine T3939 07 lt 10 ACGIH OSHA and other TLV are not applicable for activated carbon Caution Wet activated carbon removes oxygen from air causing a severe hazard to workers inside carbon vessels and enclosed or confined Spaces Before entering such an area sampling and work procedures for low oxygen levels should be taken to ensure ample oxygen availability observing all local state and federal regulations rr SECTION III PHYSICAL DATA rr noe Boiling Point F SINE Specific Gravity water 1 1 9 2 2 Vapor Pressure N A Packing Density g cc z OOS Solubility In Water N A pH N A Appearance amp Odor Black granular or powder odorless St SECTION IV FIRE amp EXPLOSION HAZARD DATA rege Flash Point N A Gee 7a Ignition Temperature C 300 Flammable Limits N A UEL N A Extinguish
33. E EXCLUSIVE REMEDY FOR ANY BREACH OF WARRANTY OR ANY CLAIM ARISING IN ANY WAY OUT OF THE MANUFACTURE SALE OR USE OF ITS PRODUCTS OHIO LUMEX SHALL NOT BE LIABLE FOR ANY LOSS OR DAMAGE DIRECTLY OR INDIRECTLY ARISING FROM THE MANUFACTURE SALE OR USE OF ITS PRODUCTS OR ITS PERFORMANCE OF WORK INCLUDING LABORATORY ANALYSIS OR ONSITE WORK IN NO EVENT SHALL OHIO LUMEX BE LIABLE FOR ANY CONSEQUENTIAL INDIRECT SPECIAL INCIDENTAL OR ANY OTHER DAMAGES OF ANY NATURE WHATSOEVER Extended Warranty amp Service Agreement optional not applicable to all products The terms of the warranty extend for an additional one 1 year beyond the standard one year warranty period In addition the service agreement consists of one annual calibration cleaning and adjustments to optics and electronics one internal rechargeable battery replacement one zero mercury filter replacement and one intake port filter replacement The Extended Warranty amp Service Agreement commences at the end of the one year standard warranty period and must be pre paid Revised 4 28 2014 133 Version 1 0 7 ANTOR Revision date 05 12 2014 SAFETY DATA SHEET Product identifier SODIUM CARBONATE Other means of identification Product No 3642 7528 7527 7521 3606 3605 3604 3602 4923 29704 29420 Recommended use and restriction on use Recommended use Not available Restrictions on use Not known Manufacturer Importer Supplier Distributor information M
34. FTER ESP SCR NSCR or DRY STACK LOCATION Traps should be sampled directly in the stack and not externally TEMPERATURE The recommended trap temperature range for Speciation traps is between 220 F and 300 F A cooling probe is only needed if you experience breakthroughs after 30 minutes of sampling high SO2 gt 1000ppm and or SO3 gt 30ppm concentration or if the flue gas temperature exceeds 350 F 126 Onto O f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment FLOW RATE The recommended flow rate for Speciation traps is between 200cc min and 250cc min SAMPLE VOLUME The recommended sample volume is close to 20L depending on the source concentration This will provide sufficient mercury capture that can be easily distinguished from background levels and make analysis easy to perform STARTING PUMPS The standard leak check procedure should be done and documented The sampling pumps should be started before the probe is inserted into the duct This is extremely important if there is positive pressure at the sample location or if you are using a mass flow controller to control the flow as it will prevent initial direct particulate entrainment on the front plug SHROUD A shroud of 6 to 12 inches in length MUST be used to prevent particulate from entering the trap during the test run Please use thin aluminum available as roofing material in Home Depot and a clamp to hold it to the end of t
35. Lom Use low level calibration from 2ng to 20 ng and use averaged calibration coefficient in calculations 100 Onto O f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 2 Please burn off ladles before you proceed with analysis After heating in the furnace let the ladle cool before cleaning off the residue Remove sticking residue by gently scraping the ladle or washing it in water Melting or fusing of the KCL with soda indicates overheating so you must drop the temperature on the controller 10 or 20 degrees Wash ladle with water at the end of the day of testing Use ceramic ladles 3 Average analysis time is 180 220 seconds Wait for KCL peak to come back to baseline it will tail Extended analysis time in the furnace over 300 sec indicates that the temperature is too low Manually integrate the peaks to ensure only the captured sampled mercury is accounted for not the baseline noise 4 Do not pull the glass wool through the trap ash bonded mercury will bias the results Cut the traps with a dremel fitted with a diamond wheel blade right before the front plug 5 Wrap the plug wool in aluminum foil before ladle goes in the furnace and wear rubber gloves to ensure there is no additional mercury transferred to the plugs Test the foil for mercury adsorbed from air and discard if positive Test the carbon used in calibration Do not leave carbon open to lab air for long time 6
36. Orio fume A Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment User Manual Version 4 0 April 2014 Ohio Lumex Company Inc 9263 Ravenna Rd unit A 3 Twinsburg OH USA Phone 1 330 405 0837 Email mail ohiolumex com Web site www ohiolumex com Onto f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Table of Contents Section 1 Technology and Technical Specifications 4 Section 2 Getting Started 6 2 1 Setting Up 6 2 2 Selecting and Running Temperature Profiles with EZ ZONE RP M324 controller 15 Section 3 Launching RAPID Software 18 Section 4 Multi Point Calibration amp Ladle Technique 21 4 1 Manual Integration Calibration Method 21 4 2 Mark amp Integrate Calibration Method 24 4 3 Analyzing Sorbent Trap Samples 28 Section 5 Ladle Preparation 31 Section 6 Sample Preparation 34 Section 7 Maintenance 37 Appendix A User Experiences 49 Appendix B Coal Ash amp Solids Analysis 51 Appendix C Sorbent Trap Analysis Procedure 52 Appendix D Determining the Method Detection Limit MDL for the Ohio Lumex RA 915 RA 915M RP M324 Sorbent Trap Mercury Analyzers 75 Appendix E Performing a Bias Test Method 30B and Spike Recovery Test PS 12B for the Ohio Lumex RA 915 RA 915M RP M324 Sorbent Trap Mercury Analyzers __77 Onto ee UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Appendix F Performing a Spike Recovery Study PS 12B o
37. RP M324 Attachment 2 30B Trap A 30B trap Figure 2 is a two section trap most commonly used for RATAs and short term testing projects The glass wool plugs and sorbent sections are labeled along the same guidelines as the PS 12B traps The first section S1 quantitatively captures Hg and the second section S2 is used for the breakthrough calculation The testing procedure for a 30B trap is shown in Figure 2 1 Flow ss te Z P1 P2 P3 Figure 2 Illustration of a 30B Tarp Figure 2 1 Analysis procedure for 30B Traps 64 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 3 Speciation Trap The speciation trap is a 5 sections trap Figure 3 Section zero or simply SO is the AGS section Following the AGS the first two potassium chloride KCI sections used for capturing oxidized mercury are labeled sections one and two or simply S1 and S2 respectively The final two carbon sections used for elemental mercury capture are labeled sections three and four or simply S3 and S4 S0 S1 and S2 should be analyzed at a temperature 585 C S3 and S4 may also be analyzed at a temperature of 585 C however if you wish to speed up the analysis time a temperature of 680 C may be used as well R AGS Hp2 absorption Carbon SO Acid Gas Scrubber AGS S1 Oxidized Mercury Analytical Bed KCl S2 Oxidized Mercury Breakthrough Bed KCl S3 Element
38. RP M324 Attachment Appendix D Determining the Method Detection Limit MDL for the Ohio Lumex RA 915 RA 915M RP M324 Sorbent Trap Mercury Analyzers In accordance with Method 30B all analyzer systems must undergo an MDL study As a rule of thumb the MDL is considered to be that amount of an analyte that creates a response such as a peak that is approximately 3 times greater than the average variance in response to a blank baseline A commonly used method to determine an instrument s official MDL can be found in the EPA s SW 846 protocols Using this method 8 replicates of a low standard are analyzed and the MDL is defined as the standard deviation of the responses of the 8 measurements times 3 0 The significance of the 3 0 is that it is a factor for the statistical technique known as the Student s T Distribution which is used to determine an MDL with a 95 confidence level that you are actually seeing the analyte being measured mercury and not just baseline noise If the number of replicates changes or if you want a confidence level other than 95 you would use a factor other than 3 0 It s important to use a standard level for your replicates with a response not too much higher than what will be the MDL to get a good determination Here are steps to perform an MDL determination on the Ohio Lumex Sorbent Trap Mercury Analyzer e Put the instrument in its most sensitive mode profile 1 with the carrier flow at the l
39. TION IX SPILL OR LEAK PROCEDURE Notify EPA If Product Spills Report in accordance with local state and federal regulations Cleaning Procedure Sweep up unused carbon and discard in refuse container or repackage for further use a ener rte SECTION X OTHER OPERATIONAL INSTRUCTIONS ea a ee SSS Prepared By Joseph Siperstein Date February 24 2006 ee nn nn anne en OHIO LUMEX MA O WARRANTY WITH RESP RETO AND DISCLAIMS ALL LIABILITY FROM RELIANCE THEREQ 144
40. Trap Analysis with the Lumex RA 915M and RP M324 Attachment 7 Note Alignment Tabs Make Sure Furnace alignment tab is against RA 915M tab stop please clean the window see Picture 2 7 Picture 2 7 8 Set up Gas Scrubber as pictured see Picture 2 8 Acid scrubber on the right and carbon media on the left to catch Hg Please make sure hoses and connections are not twisted or kinked Important Leak Test Pull hose and plug filter nozzle with a cap finger Observe flow meter reading slowly approaching Zero Picture 2 8 7 f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 9 Tighten Screw with 2mm Allen wrench Firm but don t over tighten see Picture 2 9 Picture 2 9 10 Attach USB Cable to USB 2 0 Type B Jack on RA 915M amp to USB 2 0 Type A Jack on Laptop see Picture 2 10 Warning You must have your computer operational with Lumex software open before you make a connection To the message No connection Continue Click on Retry button Picture 2 10 10 QOuio i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 11 Connect Power Cord to back of RA 915M amp Power on Analyzer see Picture 2 11 Picture 2 11 12 Open the Pump Module case see Picture 2 12 POWER EXHAUST CONNECT TO SCRUBBERS CARRIER FLOW CARRIER FLOW ADJUST Picture 2 12 11 QOuio i UMEX Sorbent Trap Analysis with the Lume
41. You may combine first and second wool plugs PO P1 to save on analysis time You may analyze section 0 acid gas scrubber and section 1 1 bed of KCL together P2 and section 2 must be analyzed separately to determine if breakthrough is present 7 The remaining carbon sections are to be analyzed just like a 30B sorbent trap 8 Oxidized mercury is equal to the loading on section O acid gas scrubber section 1 KCL and section 2 KCL breakthrough as well as PO P1 P2 combined If breakthrough is experienced sampling conditions must be altered to prevent this from happening again Elemental mercury is equal to the loading on section 3 and section 4 as well as P3 P4 P5 combined 101 Onto f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 9 Try not to spill soda in the oven Clean oven when still hot at the end of the day with vacuum cleaner nozzle approaching from the ladle intake port Disconnect silicone lines before filter to provide unrestricted flow back through the Furnace Connect lines back 2 INTRODUCTION TO THE ANALYSIS METHOD WITH RA 915 RP M324 MERCURY ANALYZER This document describes the procedure of sorbent trap analysis using the Ohio Lumex RA915 with the RP M324 attachment for total mercury Hg determination by thermal decomposition with atomic absorption and Zeeman Correction The analytical method at Ohio Lumex is based on the thermal desorption per EPA Method 7473 d
42. a synopsis of knowledge in Troubleshooting Appendix K Stack Sampling in case of spike loss breakthrough and wet or hard carbon For Wet stack After Scrubber Sampling There is a problem if traps are coming back with wet carbon in the tube after sampling This is a major cause of Breakthrough Spike loss Problems with flow and hard plugging of the traps To troubleshoot these problems please do the following a Please use shroud which extends at least 5 inches over the end of the trap b Do not tilt probe with trap side down when removing it from the stack for trap changeovers Condensate accumulated in the lines may leak back towards trap and upon contact with trap heated lines turn into steam causing steam stripping of mercury from the back of the trap spiked section toward the front into breakthrough section c Post run leak check vacuum should NOT be released through the trap cap but rather from the after trap connection umbilical to probe This will prevent a surge of line condensate back into the trap d Test each trap well temperature with an independent handheld thermocouple thermometer by inserting it into each trap holder for the length of the trap Compare the handheld reading and units F or C with setting on the sampling console Trap not Probe or Stack temperature e Exposing the traps to high temperatures may lead to Spike Loss In general the trap t
43. a to capture the acid gas and eliminate the acid gas interferences Calibration substrate is the same media in the sorbent trap If a different substrate is used as the calibration purpose calibration adaptability to the different media must be demonstrated before analyzing any trap 2 ANALYTICAL PROCEDURE DETAILS The sorbent trap tube end cap is removed The empty portion of the tube before the first plug should be cut down using a Dremel cutter blade Using the tweezers or extractor the glass wool plug at the front of the appropriate sorbent bed is carefully removed and separated from the sorbent faction The sorbent is transferred into a quartz ladle and then covered with anhydrous sodium carbonate The ladle is inserted into the analyzer s thermo catalytic conversion chamber As a result elemental mercury Hg is liberated into the gas stream and oxidized mercury Hg is converted from a bound status to the atomic status by thermal decomposition in the furnace and is then detected by atomic absorption with Zeeman correction The mercury concentration is measured and recorded using an automated data collection system Both the glass wool plug and the sorbent of each section are analyzed and the final Hg mass is figured by adding the measurements together The procedure for the trap analysis is described here step by step 2 1 Instrument Start up 2 2 Preliminary Determination of Mercury Mass 2 3 Analyzer Calibration 54 QOuio
44. aboratory An extended lab report includes the following 6 Analyzer certificate 7 Mercury standards certificates 118 Onto O f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 8 A formal report showing all standards and traps testing time Sequence and corresponding results 9 Pre calibration report 10 Post calibration verification report 4 TERMS AND DEFINITIONS Acid Gas Scrubber Appendix K quality assurance and operating procedures published by US EPA for sorbent trap monitoring systems Blank Any raw carbon sample not spiked with liquid mercury solution or elemental mercury gas Calibration NIST certified or traceable mercury standards used to Standards TO determine an instrument calibration Oxidized Mercury 0 1 1 3 HgCl Mercury Chloride 0 1 1 4 HCI Hydrochloric Acid Independent NIST traceable or certified mercury standards from separate lot Elemental Mercury standards or manufactures than the calibration standards MDL Method detection limit the minimum concentration of mercury that can be analyzed measured and reported within 99 confidence that the concentration is greater than zero Method 30B a procedure published by US EPA for measuring total vapor phase mercury emissions from coal fired combustion source 119 A f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment National Institute of Standards and Technology located
45. al Mercury Analytical Bed Carbon S4 Elemental Mercury Analytical Bed Carbon Figure 3 Illustration of a Speciation sorbent trap 65 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Special Considerations for Analyzing Speciation Traps e KCI sections MUST be analyzed at a temperature of 585 C and 0 5 L min e Separate calibration curves must be developed if KCI and Carbon sections are analyzed at different temperatures e Melting or fusing of the KCI with the sodium carbonate indicates overheating Drop the temperature 10 to 20 degrees e Extended analysis time over 300 seconds indicates too low of a temperature set point Increase temperature 10 to 20 degrees Figure 3 1 Analysis procedure for Speciation Traps 66 Onto UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 4 Trap with AGS or dust filter some traps come with Ohio Lumex particulate dust pre filter static or coil or AGS section The pre filter or AGS section is named as S0 and tested separately with other sections An example of a trap is illustrated in Figure 4 Test procedure is shown in Figure 4 1 Flow Figure 4 1 Analysis procedure for trap with AGS or Particulate dust Pre Filter 67 QOuio i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 2 5 Continuous Calibration and Post Calibration Verifications 2 5 1 Analysis of Continuing Ca
46. alysis is always beneficial it is crucial for success at low level sources Sorbent Traps Utilizing good quality well designed sorbent traps can prevent many problems with breakthrough spike recovery the ability to collect sufficient mercury mass and other issues It is important that the sorbent material used in the traps has a low native mercury level and it should be assured that spiked traps have been prepared using guidelines that assure that the spike levels are accurate Using traps that can allow higher flow levels when sampling can allow the capture of a suitably high level of mercury in a shorter time If a RATA is being done on a PS 12B system PS 12B RATA traps should be used These traps have less resistance and can be used at higher flow rates to make analysis easier Ohio Lumex also makes a special sorbent trap for RATA on very low level sources called the 30B LEE which have special high flow glass and are packed to withstand up to 4 L min flow rates The background level on the carbon for these sorbent traps is also exceptionally low because the carbon is taken through an additional step in attempt to take as much background Hg off of the carbon as possible Probes and Sampling Pumps As with the traps low level testing is quicker if the sampling pumps used can sample at higher flow rates At least one company sells a booster pump that can be used in conjunction with your existing pumps if they are not up to the task The accu
47. alyze front plug wool with the front section of carbon Analyze the second section breakthrough section together with the plug before the section and the plug following it Do the same for all other sections 10 Maintenance a use shop vacuum to clean the cell as noted earlier b clean windows and wipe the internal cell with wet Windex Kim Wipe periodically every 100 200samples c observe hoses on the furnace output for kinks or cracks d replace filter assembly once per year or when the pump starts to cut out Dispose of Hazardous Materials per local regulations 11 Perform a leak test 50 OHA ex 4 Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Appendix B Coal Ash amp Solids Analysis Power furnace on adjust temperature to 700 C flow rate to 1 or 2 LPM then allow system to warm up for 45 minutes Calibration A Calibration using Liquid Standards Use 50 uL of 0 1 ug mL standard 100uL of 0 1ug mL use 50uL of 1ug mL The calibration chart should appear as shown below ng g ppb N Sample Description ref data _ _C ng g Area 1 100 ppb 50 100 740 2 100 ppb 100 100 1480 3 1000 ppb 50 1000 7400 B Alternative Calibration using single point calibration Use NIST Coal Standard 1632d Hg concentration 92 8ppb or NIST Ash 1633c Hg concentration 1 00 ppm N Sample Description ref data C ng g Area 1 92 8 ppb 176 93 4220 Prepare Standard or Coal Ash sample
48. ample s description in the appropriate cell and enter the sample s mass in grams in the cell labeled 131 QOuio i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Mass Volume This way the software will calculate the concentration of the mercury in your sample in ng g ppb e Analyze the sample as usual press Mark and insert the ladle into the furnace e This analysis will take longer than a typical analysis usually about 120 seconds The peak may have 2 apexes as the elemental mercury is released followed by the oxidized mercury e When the sample is done and the signal returns back to normal press the Mark and Integrate button e The calculated sample concentration will be expressed in ng g ppb e Keep in mind that the results will be wet A separate analysis must be performed to get a dry weight result e Coal is not very homogenous For best results analyze each lot sample three times e Ash samples are analyzed in a similar fashion but are less of a problem because of the ash s high mercury concentration and minimal smoke production Weigh out the ash sample as stated above but do not worry about covering the sample with carbon or sodium carbonate e Soil Samples are analyzed similarly to Ash samples e This technique can be used to analyze other solid or complex samples if they are within reason Ohio Lumex will not be responsible for da
49. aning lenses Cleaning of the lenses is required when RSD value in Graph window exceeds 5 or 10 units The reading represents baseline noise RSD and must be observed at the beginning of testing after warm up period or between samples when baseline stabilizes Picture 7 1 Left amp Right Lenses require cleaning First rub with a Windex wet Kimwipe If that will not clean soak in concentrated nitric acid for 1 hour The analyzer window on the connection to attachment side also requires cleaning Use wet Kimwipe only Cleaning Furnace At the end of the runs with furnace still hot Disconnect two quick connect fittings from the furnace and filter scrubber end Use a shop vacuum to suck the spilled soda from the front of the furnace intake where you insert the ladle Apply vac for 10 seconds 37 Onto PEERI UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment a On cooled Oven Loosen Thumb Screw Picture 7 2 Picture 7 2 b Slide Apart Horizontal Plane Picture 7 3 Picture 7 3 38 QOuio D UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment C Slide Cover Back Pictures 7 4 7 5 Picture 7 4 Note Two Window holders lf marked Left and Right do not interchange Picture 7 5 39 QOuio o UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment d Fragile parts inside Turn Clockwise 5 Picture 7 6 _ A s be
50. anufacturer Company Name Avantor Performance Materials Inc Address 3477 Corporate Parkway Suite 200 Center Valley PA 18034 Telephone Customer Service 855 282 6867 Fax Contact Person Environmental Health amp Safety e mail info avantormaterials com Emergency telephone number 24 Hour Emergency 908 859 2151 Chemtrec 800 424 9300 2 Hazard s identification Hazard classification Health hazards Acute toxicity Inhalation dust and Category 4 mist Skin corrosion irritation Category 2 Serious eye damage eye irritation Category 2A Specific target organ toxicity single Category 3 exposure Unknown toxicity Acute toxicity dermal 100 Unknown toxicity Chronic hazards to the aquatic 100 environment Label elements Hazard symbol SDS_US SDSO000000960 134 k Version 1 0 AVANTOR Revision date 05 12 2014 Signal word Warning Hazard statement Harmful if inhaled Causes skin irritation Causes serious eye irritation May cause respiratory irritation Precautionary statement Prevention Avoid breathing dust fume gas mist vapors spray Wear protective gloves protective clothing eye protection face protection Use only outdoors or in a well ventilated area Wash hands thoroughly after handling Response IF INHALED Remove victim to fresh air and keep at rest in a position comfortable for breathing Call a POISON CENTER doctor if you feel unwell IF IN EYES Rinse cautiously with water for se
51. aring appropriate protective clothing See Section 8 of the MSDS for Personal Protective Equipment Methods and material for Sweep up and place in a clearly labeled container for chemical waste containment and cleaning Clean surface thoroughly to remove residual contamination up Notification Procedures Inform authorities if large amounts are involved Environmental precautions Do not contaminate water sources or sewer Prevent further leakage or spillage if safe to do so 7 Handling and storage Precautions for safe handling Avoid inhalation of dust Avoid contact with eyes skin and clothing Do not taste or swallow Use only with adequate ventilation Wash hands thoroughly after handling See Section 8 of the MSDS for Personal Protective Equipment Conditions for safe storage Keep container tightly closed Store in a well ventilated place Store in a dry including any place Store locked up incompatibilities SDS_US SDS000000960 136 AGANTOR Version 1 0 Revision date 05 12 2014 8 Exposure controls personal protection Control parameters Occupational exposure limits Appropriate engineering controls None of the components have assigned exposure limits No data availabie Individual protection measures such as personal protective equipment General information Eye face protection Skin protection Hand protection Other Respiratory protection Hygiene measures Good general v
52. aximum and diminish with warm up 3 2 Preliminary Determination of Mercury Mass The expected mercury mass is an estimate of the total mercury collected in section 1 of a sorbent trap The estimation for this amount is very important to decide the calibration range and choose a profile Knowledge of estimated stack mercury concentrations and total sample volume may be required prior to analysis Information may be received from the stack testers However an analyst should always evaluate the traps based on the information shown in the 106 QOuio i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Chain of Custody i e the sampling duration flow rate dust temperature meter temperature dry gas volume and pre spiked Hg mass A proper testing profile can be chosen after the evaluation Table 1 shows the most current profiles at Ohio Lumex new M324 attachment system with an EZ Zone Controller Table 2 lists profiles and their settings for M324 attachment system with a SD controller Table 1 Profiles and Settings of an EZ Zone Controller Profiles Starting Temp Flow Rate Test Range Duration L min ng sec 1 1 1 000 100 2 10 2 000 120 3 10 20 000 350 4 10 50 000 700 Table 2 Profiles and Settings of a SD Controller Profiles Starting Temp Flow Rate Test Range Duration L min ng sec 1 1 2 000 100 2 100 20 000 500 3 500 50 000 750 4 l 500 100 000 10
53. ceed 300 F This will ensure that any moisture remains in the vapor phase as it passes through the trap It is also important to make sure the probe is fully heated before it is inserted into the stack 98 Onto i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment FLOW RATE The recommended flow rate is between 200cc min and 250cc min SAMPLE VOLUME The recommended sample volume is approximately 20L depending on the source concentration This will provide sufficient mercury capture that can be easily distinguished from background levels and make analysis easy to perform STARTING PUMPS The pump should be started before the probe is inserted into the stack SHROUD A shroud of 6 to 12 inches in length MUST be used to prevent direct moisture entrainment during the test run ADDITIONAL NOTES For inlet or dry stack locations the shroud used must be made from a material that will not be atfected by the high temperatures of the flue gas as described above The shroud used in a wet stack location can be made out of plastic tube or metal The distribution of oxidized mercury over the AGS and KCI sections is dependent upon many factors but it is important to know that the plugs will capture oxidized mercury The bond that is created between these sections and the oxidized mercury is a very weak physical bond and too much temperature or flow will cause these bonds to fail and result in breakthrough
54. container Any media exposed to air for more than 5 hours should not be used for calibration purposes Only National Institute of Standards and Technology NIST certified or NIST traceable calibration standards and standard reference materials shall be used for the analytical procedures The entire set of Ohio Lumex calibration standards consists of 0 01 ug ml 0 1 ug ml 1 0 ug ml 10 0 ug ml 100 0 ug ml 1000 0 ug ml and second source of 0 1 ug ml 1 0 ug ml 10 0 ug ml 100 0 ug ml Hg solution Depending on the calibration range not all standards are needed to make a calibration However to avoid misleading a Calibration due to bad standards at least 3 standards are required to use for making any calibration The expiration date of a standard must always be checked before a calibration is run Manufacturer concurs with state and federal regulatory agencies 108 Onto f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment recommendations that solution standards be assigned a one year expiration date The expiration date is printed in the document of standard certification 3 3 1 Calibration procedure 1 In the Table Complex sample analysis window enter the appropriate testing description information For example sample type analysis date etc into the top box just below the menu icons on the table window Save table 2 Check the RSD and baseline The baseline can be slightly positive or negati
55. cribed in section 1 c and d Stacks with High SO2 and SO3 a High SO2 and SOS concentrations in the stack gas have a drastic effect on mercury They basically fight for space against mercury on the activated carbon by filling up the active sites on the carbon The Acid Gases wind up forcing the mercury to pass through the trap or displacing the mercury They have a tendency to lead to extreme breakthrough and spike loss b With these conditions please be wary of the temperatures the traps are exposed to This means please follow the technique described in section 1 c and d c Also consider using sorbent traps with an Acid Gas Scrubber before the first section of sorbent This will scrub the Acid Gases out of the flue gas and allow mercury to deposit on the first Activated Carbon bed 96 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 9263 Ravenna Rd Suite A 3 Onog Twinsburg OH 44087 UMEX Toll Free 888 876 2611 APPENDIX L SPECIATION TRAP ANALYSIS PROCEDURE Subject Mercury Emissions Monitoring Program Speciation Sorbent Trap Analysis Prepared by Analytical Laboratory of Ohio Lumex Company Revised on January 21 2013 97 Onto oe as UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment FGD INLET AFTER ESP SCR NSCR or DRY STACK LOCATION Traps should be sampled directly in the stack and not externally TEMPERATURE The recommended trap te
56. curs with state and federal regulatory agencies recommendations that solution standards be assigned a one year expiration date The expiration date is printed in the document of standard certification 2 3 1 Calibration Procedure Note This SOP only outlines the Mark amp Integrate method of calibration and analysis using the Ohio Lumex RAPID Computer Software h RUNNING CALIBRATION POINTS Review Table 1 Profiles and Settings for an EZ Zone Controller and select proper profile range a Double check that Calibration is selected under the Operation Mode drop down menu Fill in the Sample Description and ref data with the expected calibration point mass if calibration point is 10 ng then place the number 10 in Sample Description and ref data rows The number 1 should always be placed in the Mass Volume row whether running calibration points or analyzing sorbent traps 2 Place calibration sorbent into ladle and pipette the desired volume of the appropriate standard onto the sorbent For example 100 ul of 10 ug ml standard equals 10 ng mercury enter 10 in both the Sample Description and ref data row 3 Cover the sorbent with anhydrous sodium carbonate 4 Gently pack the sorbent and sodium carbonate in the ladle by covering the opening with a piece of aluminum foil and compressing the solids through the foil with your finger Sodium carbonate must completely cover
57. d the analyzer can be used to analyze samples that have section one sample amounts between the high and low points that you chose Please note Calibration ranges and spike values may be different based upon analyzer profile settings and expected sorbent trap field sample masses 80 Onto oe as UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Appendix G Tips to Streamline Sorbent Trap Analysis using Ohio Lumex For an experienced analyst using the Ohio Lumex sorbent trap analyzer in profile 1 Watlow SD controller or profiles 1 amp 2 Watlow EZ Zone controller calibration may take as little as 20 minutes including a blank and a second source standard once the instrument has warmed up Here are some shortcuts that make the progress a bit quicker e Leave Analyzer System powered on To avoid waiting for the furnace to warm up at the beginning of the day leave it powered on overnight so that it is ready to go first thing in the morning Please note however that it is not recommended to keep the analyzer system powered on for more than a day at a time Leaving the analyzer powered on for an extended period of time will severely shorten the life of the mercury lamp e Vacuum out the front of the furnace There is no reason to clean the furnace daily Sodium Carbonate that accumulates in the furnace can be removed by pulling it through the front of the furnace with a shop vac vacuum cleaner takes 10 secon
58. ds after disconnecting the hoses from the scrubber This can be done any time throughout the day without the need for recalibration The furnace must be hot This saves time compared to disassembling the furnace to remove the debris Please remember to reconnect the hoses e Use a Multipoint Calibration Curve of 3 instead of 6 To save time during initial calibration perform a 3 point calibration instead of a 6 point Method 30B section 11 1 Analytical System Calibration only requires a 3 point calibration however using more points will yield a better calibration For the second source standard use 500ng if not pass 10 retry Suggested calibration points 20ng use 20ul of 1 0ug ml standard 100ng use 100ul of 1 0ug ml and 1000ng use 100ul of 10ug ml Second source 500ng use 50ul of 10ug ml 81 QOuio i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment e Use Glossy Printer Paper If you have problems with the carbon from the traps sticking to the paper you are working with try using glossy paper or aluminum foil which will allow the carbon to slide off easier e Use Ohio Lumex Sorbent Traps For short term testing or low level testing we recommend using Method 30B two section traps part number RPM021 30B or new PS 12B RATA three section traps RPM021 RATA All of the traps mentioned have smaller carbon sections that make it easier to analyze the carbon and the foil wrapped glas
59. e Only one calibration curve is required for the analysis of AGS KCI and carbon Cover all sections with soda except for the AGS section Soda must be pressed using a sheet of Aluminum Foil Never place KCL on top of carbon Use upgraded pump station and set flow rate to 0 5 Lom Use low level calibration from 2ng to 20 ng and use averaged calibration coefficient in calculations 2 Please burn off ladles before you proceed with analysis After heating in the furnace let the ladle cool before cleaning off the residue Remove sticking residue by gently scraping the ladle or washing it in water Melting or fusing of the KCL with soda indicates overheating so you 129 Onto O f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment must drop the temperature on the controller 10 or 20 degrees Wash ladle with water at the end of the day of testing Use ceramic ladles 3 Average analysis time is 180 220 seconds Wait for KCL peak to come back to baseline it will tail Extended analysis time in the furnace over 300 sec indicates that the temperature is too low Manually integrate the peaks to ensure only the captured sampled mercury is accounted for not the baseline noise 4 Do not pull the glass wool through the trap ash bonded mercury will bias the results Cut the traps with a dremel fitted with a diamond wheel blade right before the front plug 5 Wrap the plug wool in aluminum foil befo
60. e independently prepared standard must be within 10 of the expected value 7 The analysis of blanks is optional yet must not be used in calibration The Hg amount in each sample must fall into the calibrated range of the analyzer and within the lower and upper mass limits established during the initial Hg and HgClz analytical bias test For extra low level samples Hg mass is below the lowest point in the calibration curve and above the MDL a response factor e g area count per Hg mass is established based on a single standard at level greater than the MDL and less than the lowest point in the calibration The amount of Hg present in the sample is calculated based on the analytical response and this response factor 61 QOuio i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 2 4 Preparation of Sorbent Traps for Analysis and Analysis Procedures 1 The end cap of a sorbent trap is removed and the trap is scored using a Dremel glass cutter just above the first glass wool plug The trap should then be broken at the score mark 2 Carefully remove the first glass wool plug and tightly wrap it in a small piece of aluminum foil Be sure entire plug is covered 3 Transfer the sorbent AND proper plug rolled in foil into a quartz ladle and then cover with anhydrous sodium carbonate until the ladle is full 4 Cover the ladle opening with a piece of aluminum foil and finger press the materials in the ladle
61. e such as lamps and the like c Any defect caused by misuse negligence accident or improper installation by the Customer d Certain parts such as mercury lamps quartz windows filters heater cartridges and ladles are expendable in normal use and their service life is unpredictable These items are covered by this warranty for ninety 90 days only from the delivery date to the customer site e Damage to Product resulting from failure of the Customer to provide the required conditions for proper operation of the Product f Customer induced contamination Warranty Claims A defective product will be shipped to Ohio Lumex Co Inc 9263 Ravenna Road Unit A 3 Twinsburg Ohio 44087 All products returned for warranty work must be assigned a Return Authorization Number RA by Ohio Lumex before the product is returned to Ohio Lumex Products returned to the factory without an RA will not be accepted The cost of removal reinstall and shipment to Ohio Lumex will be the responsibility of the Customer cost of return shipment to the Customer will be paid by Ohio Lumex Repair or replacement of a defective item shall not extend the initial warranty term Ohio Lumex shall have the right of disposal of items replaced by it Ohio Lumex may at is discretion travel to the location of installation to handle warranty claims for products that Ohio Lumex installed Exclusive Remedy Limitation of Liability THE REMEDY PROVIDED FOR HEREIN SHALL BE TH
62. e RSD reading value is around the originally static value The run time for the blank test is about 90 seconds as measured by the elapsed time 9 Remove the ladle from the furnace wait until cool down then dispose contents into a heat resistant metal tray put the ladle on a heat resistant surface before reloading it The integration area and maximum peak height will be displayed in the Integration window These values will also be automatically entered into the appropriate columns in the Table 10 CALIBRATION Switch to the Table Complex analysis window Place the cursor in the description column second column beside No 2 Double left click mouse and select STD_ Type in the standard Hg mass in ng after the dual underscore for example STD__10 Check the mass column M mg There should always be a 1 entered there Tab the curser to the concentration column C ng g 11 Switch back to the Complex analysis graph click on it to view the analysis 12 Load the ladle as in Step 5 above Pipette the desired volume of the appropriate standard onto the sorbent For example 10 ul of 10 ug ml standard equals 100 ng mercury enter 100 after STD _ 13 Cover the spiked sorbent with anhydrous sodium carbonate Gently pack the sorbent and carbonate in the ladle using aluminum foil 110 Onto O f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 14 Check the RSD and basel
63. emperature for a wet stack should be higher than the stack to prevent condensation However elevated temperature is bad for spike retention The best range is 260 350 F and is unique for each stack due to Its conditions Test 95 Onto O f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment the temperature as described in D confirm that the trap well temperatures are correct and only after that start decreasing the temperature in 50 F intervals f We have incredibly strenuous QAQC procedures making spiking absolutely error proof Therefore it is very unlikely that the spike is wrong In case of doubt send a couple of unexposed traps back to Ohio Lumex for testing You will be credited for the shipping and the traps If we ever find a problem we will credit your account and replace all of the traps free of charge g Consider switching to the High Moisture Resistant extended length Sorbent Traps We custom make these sorbent traps for wet source clients Dry Stack with Urea or Anhydrous Ammonia Spray a If traps are coming back with hard carbon or the loss of flow vacuum is too high increase the temperature gradually up to 350 F b Loss of Spike might still be an issue At dry stacks the temperature could be just 25 F elevated above the stack temperature Decrease the temperature in 25 F intervals c After the trap condensation may still be a problem Practice technique des
64. entage will display automatically The mercury mass for each tested sample is calculated by multiply A and each corresponding area count Detailed instruction is with the software MINICAL915 112 QOuio i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 3 3 2 Calibration criteria Multipoint calibration is required Three or more standards should be used to make a calibration curve An independent standard for example a NIST solid standard or an NIST traceable mercury standards from a separate lot will be analyzed to ensure the accuracy of the calibration The calibration criteria is 1 Calibrations must be performed on the day of the analysis before analyzing any of the samples 2 Three or more upscale calibration points must be used 3 The lowest point in the calibration curve must be at least 5 and preferably 10 times the MDL 4 The field samples analyzed must fall within a calibrated quantitative range and meet the performance criteria of Method 30B or Appendix K 5 For each calibration curve the value of the square of the linear correlation coefficient i e R must be 0 99 and the analyzer response must be within 10 of the reference value at each upscale calibration point 6 Following calibration a second source standard is analyzed The measured value of the independently prepared standard must be within 10 of the expected value 7 The analysis of blanks is op
65. entilation typicaily 10 air changes per hour should be used Ventilation rates should be matched to conditions If applicable use process enclosures local exhaust ventilation or other engineering controls to maintain airbome levels below recommended exposure limits If exposure limits have not been established maintain airborne levels to an acceptable level An eye wash and safety shower must be available in the immediate work area Wear safety glasses with side shields or goggles Chemical resistant gloves Wear suitable protective clothing In case of inadequate ventilation use suitable respirator Air purifying respirator with a high efficiency particulate filter Provide eyewash station and safety shower Always observe good personal hygiene measures such as washing after handling the material and before eating drinking and or smoking Routinely wash work clothing to remove contaminants Discard contaminated footwear that cannot be cleaned 9 Physical and chemical properties Appearance Physical state Form Color Odor Odor threshold pH Melting pointifreezing point initial boiling point and boiling ran Flash Point Evaporation rate Flammability solid gas Solid Powder White Odorless No data available 11 4 11 7 25 C Aqueous solution 851 C ge Decomposes Not applicable No data available No data available Upper lower limit on flammability or explosive limits Flammability limit upp
66. er No data available Flammability limit lower Explosive limit upper Explosive limit lower Vapor pressure Vapor density Relative density Solubility ies SDS_US SDS000000960 No data available No data available No data available No data available No data available 2 53 20 C 137 PAWANTOR fete oe et Oe eS Solubility in water Solubility other Version 1 0 Revision date 05 12 2014 Soluble No data available Partition coefficient n octanol water No data available Auto ignition temperature Decomposition temperature Viscosity Other information Molecular weight No data available No data available No data available 105 99 g mol CH203 2Na 10 Stability and reactivity Reactivity Chemical stability Possibility of hazardous reactions Conditions to avoid Incompatible materials Hazardous decomposition products No dangerous reaction known under conditions of normal use Material is stable under normal conditions Hazardous polymerization does not occur Excessive heat Moisture Strong oxidizing agents Strong acids Aluminum Sodium oxides Carbon monoxide Carbon dioxide 11 Toxicological information Information on likely routes of exposure ingestion inhalation Skin contact Eye contact May be harmful if swallowed Irritating to respiratory system Causes skin irritation Causes serious eye irritation infor
67. ered during the collection period dscm For the purposes of this method standard temperature and pressure are defined as 20 C and 760 mm Hg respectively Vu Volume of gas sampled unspiked trap in Field Recovery Test dscm 71 Omog UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 12 2 Calculation of Spike Recovery Analytical Bias Test Calculate the percent recovery of Hg and HgeCh using Equation 30B 1 Raed 100 Eq 30B 1 12 3 Calculation of Breakthrough Use Equation 30B to calculate the percent ugh to the second section of the sorbent trap 100 Eq 30B 2 mM B 12 4 Calculation of Hg Concentration Calculate the Hg concentration measured with sorbent trap a using Equation 30B 3 C m m Eq 30B 3 a 7 q For sorbent trap b replace C with C in Equation 30B 3 Report the average concentration ie 2 Ca Cy 12 5 Moisture Correction Use Equation 30B 4 if your mea corrected to a wet basis C C 1 B Eq 30B 4 72 Onto DS UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 12 6 Calculation of Paired Trap Agreement Calculate the relative deviation RD between the Hg concentrations measured with the paired sorbent traps using Equation 305 5 C C RD Cu 6l 100 Eg 30B 5 Ca 12 7 Calculation of Measured Spike Hg Concentration Field Recovery Test Calculate the measured spi
68. escribed here step by step 3 1 Instrument start up 3 2 Preliminary determination of mercury mass in the traps 3 3 Analyzer calibration 3 4 Trap analysis 3 5 Verification of calibration during testing and post calibration 3 6 Data saving and results reporting 3 1 Instrument Start up 3 1 1 Setup the connections among RA 915 analyzer RP M324 attachments and laptop computer Analyzer setup with new EZ Zone controller is shown in Figure 1 with SD controller in Figure 2 3 1 2 Connect power cord to RA 915 RP M324 and laptop computer 3 1 3 Complete setup with heat shield 3 1 4 Turn on computer 3 1 5 Turn on RA 915 power toggle switch and ignite mercury lamp by pressing and holding lamp ignition button for 1 5 seconds 3 1 6 Turn on the RP M324 power supply Warm up the analyzer and choose a proper profile to run The carrier pump flow rate is now bounded to the profiles for the new RP M324 power supply system with EZ Zone controller When the profile is selected the pump will automatically adjust to the desired flow rate However for the SD series controllers flow setting is manual The profiles and their setting information for an EZ Zone controller and a SD controller are listed in Table 1 and Table 2 104 Onto DS UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 3 1 7 Start the RA 915 software from the Windows main screen by double click i the icon The RA 915 Main menu sc
69. g takes 10 minutes Temperatures and air flow Profile 1 Temp 680 C Isothermal Flow 0 5 2 LPM Profile 2 Temp 652 C Isothermal Flow 4 LPM Profile 3 start at Temp 653 C Ramping Flow 4 LPM Profile 4 start at Temp 654 C Ramping Flow 4 LPM 16 Ounlo Da UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Actuating a profile sequence Press AdvK Select File 1 2 3 or 4 by pressing Up Down Arrow Key Press AdvK to select PROF and press InfK To start Sample Run Press Green Start Button only for Profile 3 4 1 PressAdvK Select File use 2 PressAdvK Select Action Up Down Arrows PROFILE and press InfK to exit to home screen Profile Indicator 3 When it comes time to run a sample press the Green Start Button before placing the ladle in the furnace only for Profile 3 4 17 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Section 3 Launching RAPID Software 1 Open RAPID Software by clicking the icon located on your desktop 2 On the pop up menu click amp open Instrument information Picture 3 1 Ma Sample Analysis Ee Serviceability checkup Picture 3 1 3 Select amp connect to the appropriate analyzer then click Exit Picture 3 2 Instrument information Connected instrument Instrument type a E Serial number E ae Zell a Console firmware version LEE Mainboard Firmware version a Picture 3 2
70. he probe WET STACK LOCATION AFTER FGD Traps should be sampled directly in the stack and not externally TEMPERATURE The 4 8 inches before the first section on the trap must be heated inside of the probe to at least 230 F and must not exceed 300 F This will ensure that any moisture remains in the vapor phase as it passes through the trap It is also important to make sure the probe is fully heated before it is inserted into the stack FLOW RATE The recommended flow rate is between 200cc min and 250cc min SAMPLE VOLUME The recommended sample volume is approximately 20L depending on the source concentration This will provide sufficient mercury capture that can be easily distinguished from background levels and make analysis easy to perform 127 QOuio i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment STARTING PUMPS The pump should be started before the probe is inserted into the stack SHROUD A shroud of 6 to 12 inches in length MUST be used to prevent direct moisture entrainment during the test run ADDITIONAL NOTES For inlet or dry stack locations the shroud used must be made from a material that will not be affected by the high temperatures of the flue gas as described above The shroud used in a wet stack location can be made out of plastic tube or metal The distribution of oxidized mercury over the AGS and KCI sections is dependent upon many factors but it is important t
71. i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 2 4 Preparation of Sorbent Traps for Analyzing and Analysis Procedure 2 5 Calibration Verification 2 6 Data Saving and Reporting 2 1 Instrument Start up 2 1 1 Setup the connections among RA 915M analyzer RP M324 attachments and laptop computer Analyzer setup with EZ Zone controller is shown in Figure 2 1 2 Connect power cord to RA 915M RP M324 and laptop computer 2 1 3 Complete setup with heat shield 2 1 4 Turn on computer 2 1 5 Turn on RA 915M by pressing the power button on the top of the analyzer The mercury lamp will ignite automatically 2 1 6 Turn on the RP M324 power supply Warm up the analyzer and choose a proper profile to run The carrier pump flow rate is bounded to the profiles of RP M324 power supply system with EZ Zone controller When the profile is selected the pump will automatically adjust to the desired flow rate The profiles and their setting information for EZ Zone controllers are listed in Table 1 2 1 7 Start the RA 915M software from the Windows main screen by double clicking the 7 icon The RA 915M Main menu screen will appear 55 Ono UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Figure 1 Analyzer setup with an EZ Zone controller 2 1 8 Select Sample Analysis on RA 915M s main menu screen then configure the window view to Table to the right of the plot by cl
72. icking the icon 2 1 9 Under the Operating cell drop down menu select External and under the Operation mode drop down menu select Calibration 2 1 10 Click the Start button and allow the system to warm up for at least 45 minutes before calibration 2 1 11 The average baseline value and the baseline RSD is located under the Current signal box to the right of where the Operation mode was adjusted After 45 minutes if the RSD is higher than 5 shut off the furnace allow it to cool down and clean the analytical cell windows 2 1 12 No baseline check is necessary with the RAPID software 56 Onto O f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 2 2 Preliminary Determination of Mercury Mass The expected mercury mass is an estimate of the total mercury collected in section 1 of a sorbent trap The estimation for this amount is very important to decide the calibration range and choose a profile Knowledge of estimated stack mercury concentrations and total sample volume may be required prior to analysis Information may be received from the stack testers However an analyst should always evaluate the traps based on the information shown in the Chain of Custody i e the sampling duration flow rate duct temperature meter temperature dry gas volume and pre spiked Hg mass A proper testing profile can be chosen after the evaluation Table 1 shows the most
73. ine The baseline can be slightly positive or negative Adjust the baseline for 10 seconds clicking on Baseline check and click again to terminate in 10 seconds if necessary 15 Click START on the integration window Immediately insert the prepared ladle loaded with sorbent spiked standard and sodium carbonate into the furnace 16 Allow the peak mercury signal to develop until it returns to the baseline 17 When the peak has returned to the baseline 0 0 click END on integration window to stop the integration Remove the ladle from the furnace cool it before disposing the waste then place the ladle on a heat resistant surface The value of integration area and maximum peak height will be automatically entered into the appropriate columns in the Table 18 Repeat the step 12 to 17 until all of the planned standards have been analyzed 19 To perform the calibration there are two options to be chosen Option 1 RA 915 analyzer come with manufacture calibration software By running the software calibration coefficient square of the linear correlation coefficient R2 and the calibration curve will show up on a pop up calibration window The detail on how to run the calibration is described below a Return to the Table Complex analysis window Under the Table heading click the SELECT icon or from the Table pull down menu Highlight all of the Standard rows using the Shift and Arrows on the keyboard Afte
74. ing Media Flood with plenty of water or inert gas such as N and CO special Fire Fighting Procedure None Se ee SECTION V REACTIVITY ne Stability gt Stable Hazardous Polymerization Will not occur Hazardous Decomposition CO may be generated in the event of fire Condition To Avoid Contact with strong oxidizers such as ozone liquid oxygen chlorine permanganate and ketone may cause fire Incompatibility gt Avoid contact with high concentration of ketone in air or liguid SECTION VI HEALTH HAZARD DATA Carcinogenicity N A Skin N A Ingestion N A Acute or Chronic N A NTP N A IARC Monograph N A Inhalation Dust may be OSHA N A inhaled Signs amp Symptoms of Exposure Slight irritation of eyes and nose may result from contact with carbon fines Medical Conditions Generally Aggravated By Exposure N A SS a ert et SECTION VII EMERGENCY amp FIRST AID PROCEDURE SS enn Skin N A Ingestion N A Inhalation N A Eye Flush with plenty of water at least for 15 minutes Follow up with physician exam if necessary ae SECTION VIII SAFE HANDLING amp STORAGE a Protective Gloves Rubber Gloves Protective Clothing Not required Eye Protection gt Safety Glasses Respirator Protection A NIOSH approved particulate filter Ventilation gt Local amp Mechanical exhaust recommended Storage amp Handling Avoid generation of dust and fines during handling Se eter SEC
75. ion with NIST traceable Mercury standard pour calibration sorbent carbon in ladle position pipette above sorbent distributing drops in one middle point on top of the carbon Do not use pipettes capacities less than 20 or larger than 50 micro liters for small 6mm traps and 20 100 micro liters for large 10mm traps Picture 5 2 31 Oun o _ UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 3 Sprinkle soda Sodium Carbonate on top of the spiked sorbent covering it completely Picture 5 3 Picture 5 3 4 Brush off excessive soda Picture 5 4 then cover loaded ladle with fresh foil and apply slight finger pressure to press pack down the sample Picture 5 5 Do not reuse foil Wipe the edges of the ladle and the bottom clean from soda grains Picture 5 6 Be careful not to spill soda in the oven Picture 5 4 Picture 5 5 Picture 5 6 32 Onto or UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 5 Slowly not to spill soda insert Ladle with gold dot facing up and seat completely inside furnace Picture 5 7 After removal place ladle on foil to cool and use narrow metal spatula to empty The ladle comes out of the furnace mercury free and is ready to be reused Picture 5 7 Onto DS UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Section 6 Sample Preparation 1 Use a Dremel tool with a diamond
76. iques Measurement Optimization Use Good Quality Traps e Low Native Mercury Accurately Spiked Amenable to Higher Flow Rates e Use PS 12B RATA Traps for PS 12B Systems Sampling Equipment e Use Sampling Pumps that can Accommodate Higher Flow Rates or a Booster Pump Ensure Sampling System is In Good Repair Moisture e Use Sufficient Probe Temperature e Use Moisture Resistant Traps Probe Shrouds or Trap Shields Thermal Zeeman AA Analyzer Optimization In Good Repair 90 Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Use Lowest Flow down to 0 5 L min e Make Sure Cell Windows are Clean Assure that Baseline RSD is less than 1 2 e Use Good Standards Use a 5 or 6 Point Calibration 5ng to 100ng or 300ng e Use Average RF Calibration Calculation Assure that the RSD of the Calibration RFs is lt 5 6 Don t Forget to Run the Low Level Standard Analyze a CCVS after each Pair of Traps Have a Good MDL Determination e Cut Traps if Needed to Remove Section 1 amp 2 In Summary Using Method 30 B to perform mercury RATAs at low level sources will continue to be somewhat more challenging than those at other sources For a power plant this is a good thing because the ultimate goal will be low mercury emissions Hopefully this information on system optimization and the details of the methods will make performing RATAs on even very low level mercury sources easier
77. irect thermal desorption with atomic absorption and no gold amalgamation The method is applicable for total mercury direct testing of 40 CFR Part 75 Appendix K EPA Method 30B sorbent traps and speciated mercury measurement sorbent traps The reporting limit RL is equal to the method detection limit MDL determined for the instrument of total mercury testing Analysis time depends on the type of controller used and the selected profile Typically the run time is about 90 seconds per sample The required instrument and accessories for performing the analysis include Ohio Lumex RA 915 with RP M324 Attachment Computer Ohio Lumex 6 inch ladles Assorted laboratory equipment which includes spatulas glass wool extractor tweezers adjustable pipettes aluminum weigh boats aluminum foil torch trap cutter and so on 102 Onto f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Reagents and standards include NIST certified and NIST traceable mercury calibration standards Second source NIST standard Sodium Carbonate Calibration sorbent media Although the Zeeman correction used by the Ohio Lumex analyzer eliminates spectral interferences in the analyzer halogens and especially iodine and chlorine will form acid gases in the furnace These acid gases will react with the elemental mercury and plate out mercury salts on the optical lenses in the analytical chamber Therefore
78. is no penalty for falling outside these bounds Also since Field Recovery Test values are calculated using the average of the 3 runs 15 and since the limits are 85 to 115 of the spiked value it is not difficult to meet these requirements even at very low level sources Relative Accuracy HG Cems According to CFR 40 part 63 a RATA passes if the 30 B measurements and the HG CEMs system have a relative accuracy of lt 20 or if they agree within 1 0 ug dscm This is a pretty big barn door to hit For low level sources the 2 measurement systems could differ by a factor of 10 and still pass the RATA The full leniency of the method comes into play below 0 5 ug dscm At this level sampling at 2 L min 60 ng can be collected in an hour which is a sufficiently high mass to make things work easily Below this level the changes in the method constraints detailed above compensate for any difficulties associated with the smaller mass loadings Performing RATAs on PS 12B Systems The RATA criteria for a sorbent trap sampling system under the new Mats rule is in 40 CFR Part 63 sect 4 1 2 and the special considerations that apply for the RATA are shown in sect 4 1 2 2 Paired Trap Relative Deviation PS 12B Relative Deviation limits from table 12B 1 for sources are as follows lt 10 Relative Deviation RD if the average concentration is gt 1 0 ug m3 lt 20 Relative Deviation RD if the average concentration is lt 1 0 ug m
79. ke concentration using Equation 30B 6 m m C _ 308 6 TE Eq Then calculate the spiked Hg recovery K using Equation 30B 7 R C we xY x100 Eq 30B 7 1 chest 73 QOuio i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 5 HEALTH AND SAFETY 5 1 Sampling Safety If performing the test sampling follow the Source Plant safety protocol to ensure any hazards are avoided 5 2 Laboratory Safety Proper protective equipment lab coats safety glasses particulate respirator nitrile gloves shall be worn while performing analysis 5 3 Reagents Please refer to the provided Material Safety Data Sheets for every chemical used in order to avoid injury or reactions 6 REFERENCES 1 Thermal analysis for field sorbent trap mercury testing Instruction hand book Ohio Lumex Company Inc 2006 2 Method 7473 Mercury in solids and solutions by thermal decomposition amalgamation and atomic absorption spectrophotometry US EPA 2007 www epa gov sw 846 pdts 7473 pdf 3 Method 30B Determination of total vapor phase mercury emissions from coal fired combustion sources using carbon sorbent traps US EPA 2008 http www epa gov ttn emc promgate Meth30B pdf 4 Appendix K to Part 75 Quality assurance and operating procedures for sorbent trap monitoring system US EPA 2005 74 Onto UMEX Sorbent Trap Analysis with the Lumex RA 915M and
80. libration Verification Standard CCVS After no more than 10 analyses a continuing calibration verification standard must be analyzed The standard should fall into the calibration range The measured value of the CCVS must be within 10 of the expected value 2 5 2 Post Calibration Verification At the end of each set of analysis a calibration standard will be tested The standard should be within the calibration range and the measured value of this standard must be with 10 of the expected value 2 6 Data Saving and Reporting At the end of testing all data should be saved in the Ohio Lumex database Data can be reported as an Excel file xls pdf file odf or in a report format qrp Customer can request an extended laboratory report from the Laboratory An extended lab report includes the following 1 Analyzer certificate 2 Mercury standards certificates 3 A formal report showing all standards and traps testing time sequence and corresponding results 4 Pre calibration report 5 Post calibration verification report 68 Onto O f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 3 TERMS AND DEFINITIONS AGS Acid Gas Scrubber Quality assurance and operating procedures published by US EPA for sorbent trap monitoring systems Any raw carbon sample not spiked with liquid mercury solution or elemental mercury gas Calibration NIST certified or traceable mercury standard
81. mage caused by the analysis of inappropriate samples If you are unsure of the sample use caution start with small amounts and or call Ohio Lumex Technical Support 132 9263 Ravenna Rd Unit A 3 Twinsburg Ohio 44087 Toll Free 888 876 2611 330 405 0837 Fax 330 405 0847 www ohiolumex com O Ohio Lumex Company HIO umex Warranty Warranty Ohio Lumex warrants that its products will be free from defects in material and workmanship for a period of one 1 year from the date of shipment provided the product is maintained and operated consistent with Ohio Lumex s guidelines This warranty does not apply to consumables such as Mercury Lamps Scrubbers Calibration Cells Filters and Heater Cartridges or parts delivered by Ohio Lumex but manufactured by others Ohio Lumex does not warrant that the operation of products will be uninterrupted or error free Ohio Lumex will repair or replace at no charge products which are defective and returned to Ohio Lumex within one 1 year of delivery or at Ohio Lumex s sole option refund Customer s purchase price THIS WARRANTY IS EXPRESSLY GIVEN IN LIEU OF ANY AND ALL OTHER EXPRESS OR IMPLIED WARRANTIES INCLUDING ANY IMPLIED WARRANTY OR MERCHANTABILITY OR FITNESS FOR A PARTICULAR PURPOSE Exclusions The warranty of Ohio Lumex does not cover the following terms and events a Failure of mechanical parts due to normal wear and tear b Electrical components that deteriorate due to ag
82. mation on toxicological effects Acute toxicity list ali possible routes of exposure Oral Product Dermal Product Inhalation Product Repeated dose toxicity Product Skin corrosioni irritation Product LD 50 Rat 4 090 mg kg No data available LC 50 Mouse 2 h 1 2 mg l LC 50 Guinea pig 2 h 0 8 mg l No data available Causes skin irritation Serious eye damage eye irritation Product SDS_US SDS000000960 Causes serious eye irritation 138 Version 1 0 AVANTOR Revision date 05 12 2014 Respiratory or skin sensitization Product Not a skin sensitizer Carcinogenicity Product This substance has no evidence of carcinogenic properties IARC Monographs on the Evaluation of Carcinogenic Risks to Humans No carcinogenic components identified US National Toxicology Program NTP Report on Carcinogens No carcinogenic components identified US OSHA Specifically Regulated Substances 29 CFR 1910 1001 1050 No carcinogenic components identified Germ cell mutagenicity in vitro Product No data available In vivo Product No data available Reproductive toxicity Product No components toxic to reproduction Specific target organ toxicity single exposure Product Respiratory tract irritation Specific target organ toxicity repeated exposure Product None known Aspiration hazard Product Not classified Other effects None known 12 Ecological information Ecotoxicity Acute haza
83. mex RA 915M and RP M324 Attachment sampile analysis Opersking ool ed Operation mode eera 1 Calibration 16 04 2013 14 35 16 16 04 2083 14 35 17 16 04 2013 14 35 16 16 04 2013 14 35 15 16 04 2013 14 35 14 16 04 2013 14 935 13 16 04 2015 14 35 12 16 04 2013 14 35 11 16 04 2013 14 35 10 16 04 2013 14 3509 see BBUSSaRBs SBSH sash 16 04 2013 14 16 04 2013 14 16 04 2013 i 16 04 2013 14 16 04 2013 i 35 o o o o o i o o i o o o oO i 0 2 o i aan oon D Blank Lee 1 U Massf U Aree eight Measur Interval s Picture 4 3 7 Repeat steps 2 thru 6 till you ve ran at least three Standards 8 Mark the check box next to each Standard you want used in your calibration amp click Calculate calibration Picture 4 4 Sample analysis Fie View Help y galen az sz gt Operating cell Seere mode CUN a A description Pause e calibration O a ee See seen 0 582 Ee oal 16 04 2013 17 04 36 16 04 2013 17 04 35 16 04 2013 17 04 34 16 04 2013 17 04 33 16 04 2013 17 04 32 16 04 2013 17 04 31 16 04 2013 17 04 30 16 04 2013 17 04 29 16 04 2013 17 04 28 16 04 2013 17 04 27 16 04 2013 17 04 26 16 04 2013 17 04 25 16 04 2013 17 04 24 16 04 2013 17 04 23 16 04 2013 17 04 22 16 04 2013 17 04 21 16 04 2013 17 04 20 16 04 2013 17 04 19 16 04 2013 17 04 15 Sample description Std_100 ref data 100 Mass olume 1 Blank l N Sample de
84. mperature range for Speciation traps is between 220 F and 300 F A cooling probe is only needed if you experience breakthroughs after 30 minutes of sampling high SO2 gt 1000ppm and or SO3 gt 30ppm concentration or if the flue gas temperature exceeds 350 F FLOW RATE The recommended flow rate for Speciation traps is between 200cc min and 250cc min SAMPLE VOLUME The recommended sample volume is close to 20L depending on the source concentration This will provide sufficient mercury capture that can be easily distinguished from background levels and make analysis easy to perform STARTING PUMPS The standard leak check procedure should be done and documented The sampling pumps should be started before the probe is inserted into the duct This is extremely important if there is positive pressure at the sample location or if you are using a mass flow controller to control the flow as it will prevent initial direct particulate entrainment on the front plug SHROUD A shroud of 6 to 12 inches in length MUST be used to prevent particulate from entering the trap during the test run Please use thin aluminum available as roofing material in Home Depot and a clamp to hold it to the end of the probe WET STACK LOCATION AFTER FGD Traps should be sampled directly in the stack and not externally TEMPERATURE The 4 8 inches before the first section on the trap must be heated inside of the probe to at least 230 F and must not ex
85. n the Ohio Lumex RA 915M RP M324 Sorbent Trap Mercury Analyzer System 79 Appendix G Tips to Streamline Sorbent Trap Analysis using Ohio Lumex 81 Appendix H Tips for Successfully Using Method 30 B to Perform Mercury RATAs at Low Level Sources 83 Appendix l Method 30B Spiked Sample Calculations 92 Appendix J SOP to calculate R squared per PS 12B and Method 30B requirements 94 Appendix K Troubleshooting Sorbent Traps in case of Breakthrough and or Spike Loss 95 Appendix L Speciation Trap Analysis Procedure 97 Appendix M Speciation Trap Standard Operating Procedure 125 Appendix N Analyzing Coal Ash Soils and Other Solids with the RA 915M RP M324Analyzer 131 Product Warranty 133 Safety Data Sheet Sodium Carbonate 134 Material Safety Data Sheet Activated Carbon 143 Onto UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Section 1 Technology and Technical Specifications TU Zeeman mercury triplet Absorption line envelope Polarization modulator Ag a pa Serres 5 a N if gt f 5 14 ena A ATIAN taal NPG F TA 2 Dry Catalytic Converter 800 C Multi path cell Photodetector Lumex 915M_ with RP M324 is designed for field on site and laboratory Direct testing of EPA PS 12B Method 30B sorbent traps in accordance with the Mercury and Air Toxics Standards MATS rule Analysis time is less than 2 minutes per sample and generates zero chemical waste This a
86. n two minutes 4 Calibration Direct spiking of sorbent with Mercury NIST traceable Standard Referenced Materials 5 Set up or take down time less than one hour 6 Utilities 110v 60Hz 1000Watt 7 Dimensions and weight Two Rolling Pelican Cases 82 Ib Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Section 2 Getting Started 2 1 Setting Up 1 Make sure you have all the system components see Picture 2 1 Note components arrangement may slightly vary Picture 2 1 RA 915M amp RP M324 in Pelican Shipping Cases 2 In one of the two blue cases you will find the M324 Power Supply amp Pump Module see Picture 2 2 Sn Iecasem Per MSS4 Attachment Aoo Af Zee Mean SpPcooctromeoter a t 4 4g Toor nore f Barini w gt TET SS SS ee j s bia Prrre ech A Picture 2 2 M324 Power Supply amp Pump Module UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 3 Another blue case contains the M324 Furnace amp Spare Parts Kit see picture 2 3 Picture 2 3 M324 Furnace amp Spare Parts Kit 4 Remove Furnace from Case see Picture 2 4 Picture 2 4 7 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 5 Clean Lens Before Attaching Furnace see Picture 2 5 Picture 2 5 6 Attach Furnace rotate gently to RA 915M see Picture 2 6 Picture 2 6 Onto UMEX Sorbent
87. nalyzer may also be used for Direct testing of ash coal and Ontario Hydro method generated liquid samples A sorbent trap is cut and the sorbent media is transferred into a quartz ladle The ladle is inserted into the analyzers thermo catalytic conversion chamber which is heated to 680 C Mercury is then converted from a bound state to an unbound atomic state by thermal decomposition This approach enables the operator to achieve analytical results of the highest quality in a short period of time The use of a multipath cell combined with a dry converter provides the highest sensitivity with no interferences Mercury measurements take place in the heated cell zone of the converter directly coupled to a spectrometer High temperature and short residence time prevents mercury atoms from recombining with 4 Ono UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment any active species generated due to high temperature decomposition of the sample matrix An external pump with a mass flow controller draws ambient air into the catalytic chamber to aid in combustion and act as a carrier gas No cylinders of oxidizer or compressed gases are required No clean room is required TECHNICAL SPECIFICATIONS 1 Detection limit 0 5ng 100 000ng of mercury in sorbent or 1 ug kg 1000mg kg mercury concentration in coal or fly ash 2 Precision 5 Accuracy 5 3 Direct analysis results i
88. o know that the plugs will capture oxidized mercury The bond that is created between these sections and the oxidized mercury is a very weak physical bond and too much temperature or flow will cause these bonds to fail and result in breakthrough For both locations the front plug must have minimum amount of particulate or discoloration from white color Please note Large amount of particulate or moisture on the front plug will skew the Total and speciation ratio and make the run invalid We have found that the aforementioned sampling procedures will yield the most consistent and reproducible results 128 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 2 SPECIATION TRAP ANALYSIS PROCEDURE RECOMMENDATIONS s AGS Hp2 absorption Carbon Flow SO Acid Gas Scrubber AGS S1 Oxidized Mercury Analytical Bed KCl S2 Oxidized Mercury Breakthrough Bed KCl S3 Elemental Mercury Analytical Bed Carbon S4 Elemental Mercury Analytical Bed Carbon Figure 1 Illustration of a Speciation Trap For full analytical procedure please refer to the Speciation Traps Analytical SOP 1 Clean the furnace and analyzer windows before heating up the furnace Calibrate analyzer as per method 30B using carbon as calibration substrate Change temperature set point on Watlow controller use up down arrow keys to 590 C The furnace must look almost dark if looking inside through the ladle entry hol
89. orted including the rejected data The minimum time per run is 30 minutes if the RATA is being performed against a PS 12A Instrumental Hg CEM or PS 12B Sorbent Traps CEM A lot of frustration has been reported from crews attempting to complete mercury RATAs using method 30 B at sources where the mercury levels are low Successfully completing one of these RATAs with minimal frustration can be achieved by focusing on strategies in 2 key areas e Optimizing the measurement system e Being aware of and taking advantage of the method s built in leniency for low level sources 83 Onto UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Method Information Method 30 B has actually been well crafted to deal with the challenges of low level sources Let s review some of the provisions of the method and how they can help with low level measurements Low Level Standard One of the least understood parts of the method is the provision to allow quantification of low level samples using a one point calibration based on a low level standard that should be run each day analysis are performed at a level gt the MDL level and lt the lowest point in the Initial Calibration This is explained in section 11 3 of the method The response factor from this low level standard should be used to quantify anything analyzed that produces a response less than that of the lowest point in the multi point calibration This includes blank
90. otal mercury direct testing of 40 CFR Part 75 PS 12B EPA Method 30B sorbent traps and speciated mercury measurement sorbent traps The reporting limit RL is equal to the method detection limit MDL determined for the instrument of total mercury testing Analysis time depends upon the temperature and flow rate of the analyzer pump station Typically the run time is about 90 seconds per sample The required instrument and accessories for performing the analysis include Ohio Lumex RA 915M with RP M324 Attachment Computer Ohio Lumex 6 inch ladles Assorted laboratory equipment which includes spatulas glass wool extractor tweezers adjustable pipettes aluminum weigh boats aluminum foil torch trap cutter and so on Reagents and standards include NIST certified and NIST traceable mercury calibration standards Second source NIST standard Sodium Carbonate Calibration sorbent media activated iodinated Carbon 53 Onto f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Although the Zeeman correction used by the Ohio Lumex analyzer eliminates spectral interferences in the analyzer halogens and especially iodine and chlorine will form acid gases in the furnace These acid gases will react with the elemental mercury and plate out mercury salts on the optical lenses in the analytical chamber Therefore granular sodium carbonate is ALWAYS placed on top of the sorbent medi
91. ount that was spiked on to it 15 5 Liters of sample where placed onto the spiked trap From the above calculation we know that each liter of this gas should contain 4 14ng of mercury for a total of 64 2ng Subtracting this 64 2ng from the total of 126ng we get 61 8ng This is the 61 8ng remaining that is due to the 60ng of mercury that was spiked on the trap initially So the spike recovery is 61 8ng 60ng x 100 103 If the average recovery of the 3 spiked runs is within 15 the field recovery test has passed e Now we can see if this example used above can also be used as a valid RATA run 92 QOuio i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment For the unspiked trap Trap A we know from the calculations above that the mercury concentration of the sample was 4 14uUg dscm For Trap B we can calculate the sample concentration once we subiract out the amount of mercury that was spiked onto the trap So 126ng minus the 60ng that was spiked onto the trap equals 66ng This 66ng is the mercury from the 15 5 Liters of sample that passed through the trap So the indicated concentration from this data is 66ng per 15 5 Liters 66ng 15 5 L 4 25ng L 4 25 ug dscm The Percent Relative Deviation of the 2 traps is 100 times the absolute value of the difference between the 2 concentrations divided by the sum of the 2 concentrations or 100 x 4 25ug dscm 4 14 dscm 4 25 pg dscm 4 14ug dscm 100 x 0
92. owest level that it will commonly be used in and the furnace in its most aggressive mode 680 C at 2L min Calibrate the instrument as you would typically to make sure it s measuring with accuracy and precision run 5 or 6 points typically from 10ng to 2 000ng also run a blank and a second source standard Using zero mercury carbon make and analyze 8 standards at a 3ng level e For these standards it is important that the mercury peak is isolated from 75 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment baseline noise during integration This can be accomplished by either waiting to start integration about 30 seconds after the standard is inserted into the furnace and then promptly ending integration after the mercury has all been released or by manually integrating the peaks e For these 8 replicates calculate the average response in ng of mercury and the standard deviation in the responses in ng of mercury The MDL is defined as 3 times this standard deviation As an example If the 8 replicates of a 3ng standard produced responses of 2 79 3 04 2 89 3 00 2 67 2 85 3 04 and 3 17ng of mercury the average response would be 2 93ng the standard deviation would be 0 161ng and the MDL would be 3 times 0 161ng 0 483ng 76 Onto UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Appendix E Performing a Bias Test Method 30B and Spike Recovery Test
93. p gt gt rg gt B a v2 4 ji gt gt t Picture 7 6 e Remove Carefully Keep Plane Parallel to Cell Surface Picture 7 7 ay Boss fittings Must be aligned to prevent quartz cell 7 O iana j from breaking Keep i aa surfaces parallel in latest design cells are metal I uo Picture 7 7 40 Ouio o UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Note Boss Must be aligned to prevent quartz cell from breaking Keep surfaces parallel In latest design cell is made from stainless silco coated Picture 7 8 g Remove Right and Left Lenses Picture 7 9 Bosses Bayonete Fittings Picture 7 9 41 On o Da UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment h Remove Graphite Gasket and Window Gasket must be compressed tightly and have no wrinkles Picture 7 10 and 7 11 pm L Picture 7 10 Picture 7 11 I Reassemble Lenses Pictures 7 12 and 7 13 Picture 7 12 Picture 7 13 42 Onto UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment j Hoses will become brittle Unscrew Hose Guards Use Caution Fragile Quartz Cell and Hose fittings Picture 7 14 an Picture 7 14 k To Replace Hose cut and peel with box cutter knife Pictures 7 15 7 16 Fa pelg fly f 4 Picture 7 15 Picture 7 16
94. p or Down Arrow Keys 3 Press AdvK and select Prof by cycling Up or Down Arrow Keys Press InfK to save selection and exit 4 Wait for Green Ready Light to come on before starting profiles 3 4 Profiles 1 and 2 Light is always ON Change Profile profile must be ended before the new one is loaded 1 Press AdvK and using Up or Down Arrow keys select END Press InfK to enter 2 Reset controller by cycling the power button on the back of controller Table 2 1 Profiles Temperature Flow Technique Range ng C LPM Profile 1 680 0 5 2 Light is ON Insert ladle at gt 300 10 2 000 P1 any time not ramping P2 652 653 4 54 Profile 3 P3 Profile 2 4 Light is ON Insert ladle at 10 4 000 any time not ramping EE vva Tor Agnt pusmto start S og10 000 Ramping Wait for light push to start 40 000 30 000 Ramping 15 Profile 4 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Note Because a single sample run in P3 amp P4 requires a substantial amount of time it s more beneficial to break up a sample section for example 20 000 ng spike over multiple ladles and analyze in P1 or P2 Ranges Profile 1 up to 0 5 2 hours sampling RATA Testing takes 2 minutes Profile 2 up to 7 days sampling wet scrubber Testing takes 2 minutes Profile 3 up to 5 days sampling no scrubber Testing takes 6 minutes Profile 4 up to 7 days sampling no scrubber Testin
95. r rr rr mr gr rr rrr mr srr rere cern gt IB GR i a te eer rrr ee a wee tee bn ee Jee ten boston Se mde nm bn ee Je eda ete ele ede ede eb eine eee deen lee dee de ew wena Bee ahs as a Ra eae a eS ea GEN DAGI ee a ar ee AE Se ot A aH SAE ee Se Hs oafa a ae a6 bie a ale oe bata 6 Se os E oie 2 4 oS 46 oe sie Ske O S oS to oe A aS a Sten OE ee ee Nee a ee ee ee ee ee ee a R ed ee eee ee ee eee ee eee ote ata ba teal aaan Cea atte ata cin baie feted Deak Aakn aibs bali Cae hte a Be ted pt ee tes A n KOS ete et tee ead mete wae tae bw cle oe So od we be cline Me ede wba cle ede ew be ek Sole ade oe seek ool dood wetn Heed wote cbc clan Sample description ref data Mass olume Blank al N Sample description Blank ref data U Mass U 4rea Height Measur Interval s AD i ate l MAINS me ia Delete Calibration settings Calc 5 alibration list Instrument is connected RA915M 1644 Picture 3 5 20 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Section 4 Multi Point Calibration amp Ladle Technique 4 1 Manual Integration Calibration Method 1 Allow RA 915M M 324 System to warm up for at least 45 minutes 2 Fill in Sample description ref data amp Mass Volume Picture 4 1 e Note The example used below assumes an initial calibration point of 10 nanograms Yours may be different depending on sample parameters
96. r the standards have been highlighted click on the CALIBRATE icon under the Calibrate heading A calibration graph will appear and the new calibration 111 Onto f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment coefficient will be listed as A Click on the apply icon VY then click on the EXIT icon b While the standards are still highlighted in the Table Complex analysis A pop up window will ask you to save the calibration coefficients Click YES window Click on the CALCULATE icon under the Table heading The program will fill in the calculated values of the standards based on the current calibration The calibration coefficient A and the intercept Co will be found at the upper right corner of the Table Complex analysis window c Save the data in the Table by clicking on the SAVE icon header or use Save as in the file pull down menu Create a folder for saving the under the File data Do not save files in the RA915P directory Option 2 Another option to do the calibration is to use Ohio Lumex Company calibration software MINICAL915 In this software by entering the corresponding area count number of each tested standard into an Excel table a calibration curve calibration coefficient A square of the linear correlation coefficient R calculated mercury mass of each loaded standard standard deviation RSD and recovery perc
97. racy and precision of your sampling equipment is particularly critical wnen sampling at these low level sources so extra attention to maintenance and calibration is called for Moisture Excessive water in the traps can cause breakthrough and poor dual trap agreement Moisture is best dealt with by making sure that your probe temperature is high enough 87 Onto UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment to eliminate liquid water in the trap sections The short term sampling working range for good quality traps is quite large up to 450 C so it should be easy to find a temperature to prevent water in the traps Shrouds or Trap Shields on the probe can prevent liquid water from being sucked into the traps Moisture resistant traps are also available and can be used in situations where in stack moisture levels are causing problems Like after a Wet FGD Optimizing the Thermal Zeeman AA Analyzer For low level sources the analyzer like the sampling components should be in top shape and well maintained Additionally there are a few techniques that can help with these sources Lowering the flow on the analyzer will increase the sensitivity and precision and make analysis of lower mercury amounts easier You will have precise flow on the pump station down to 0 5 l min Make sure the cell windows are clean and all parts are in good working order The baseline should be stable with a steady state RSD of lt 1 or
98. rap 117 Onto O f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Analysis Tip Be VERY careful when analyzing speciation traps It is imperative to keep the Potassium Chloride and Sodium Carbonate separate Sodium Carbonate is used to cover every sample before entering it into the oven Since the two look similar label the dishes accordingly so that Potassium Chloride is not mistaken for Sodium Carbonate when performing analysis When a speciation trap is analyzed please ALWAYS remember the temperature needs to be down to 580 C for analyzing the first 3 non carbon sections 3 5 Calibration Verification 3 5 1 Analysis of continuing calibration verification standard CCVS After no more than 10 analyses a continuing calibration verification standard must be analyzed The standard should fall into the calibration range The measured value of the CCVS must be within 10 of the expected value 3 5 2 Post calibration verification At the end of each set of analysis a calibration standard will be tested The standard should be within the calibration range and the measured value of this standard must be with 10 of the expected value 3 6 Data Saving and Reporting At the end of testing all data should be saved in the Ohio Lumex database Data can be reported as an Excel file xls pdf file odf or in a report format qrp Customer can request an extended laboratory report from the L
99. rds to the aquatic environment Fish Product LC 50 Bluegill Lepomis macrochirus 96 h 300 mg Aquatic invertebrates Product EC 50 Water flea Ceriodaphnia dubia 48 h 156 6 mg l Chronic hazards to the aquatic environment Fish Product No data available Aquatic invertebrates Product No data available Toxicity to Aquatic Plants Product No data available Persistence and degradability Biodegradation Product Expected to be readily biodegradable SDS_US SDS000000960 139 Version 1 0 ANTOR Revision date 05 12 2014 Ce CH RE Wo BOD COD ratio Product No data available Bioaccumulative potential Bioconcentration factor BCF Product The product is not bioaccumuiating Partition coefficient n octanol water log Kow Product No data available Mobility in soil The product is water soluble and may spread in water systems Other adverse effects The product components are not classified as environmentally hazardous However this does not exclude the possibility that large or frequent spills can have a harmful or damaging effect on the environment 13 Disposal considerations Disposal instructions Discharge treatment or disposal may be subject to national state or local laws Contaminated packaging Since emptied containers retain product residue follow label warnings even after container is emptied 14 Transport information DOT Not regulated IMDG Not regulated IAT
100. re ladle goes in the furnace and wear rubber gloves to ensure there is no additional mercury transferred to the plugs Test the foil for mercury adsorbed from air and discard if positive Test the carbon used in calibration Do not leave carbon open to lab air for long time 6 You may combine first and second wool plugs PO P1 to save on analysis time You may analyze section 0 acid gas scrubber and section 1 1 bed of KCL together P2 and section 2 must be analyzed separately to determine if breakthrough is present 7 The remaining carbon sections are to be analyzed just like a 30B sorbent trap 8 Oxidized mercury is equal to the loading on section O acid gas scrubber section 1 KCL and section 2 KCL breakthrough as well as PO P1 P2 combined If breakthrough is experienced sampling conditions must be altered to prevent this from happening again Elemental mercury is equal to the loading on section 3 and section 4 as well as P3 P4 P5 combined 9 Try not to spill soda in the oven Clean oven when still hot at the end of the day with vacuum cleaner nozzle approaching from the ladle intake port Disconnect silicone lines before filter to provide unrestricted flow back through the Furnace Connect lines back 130 Onto f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Appendix N Analyzing Coal Ash Soils and Other Solids with the RA 915M RP M324 Analyzer Coal ash soils and o
101. reen will appear Figure 1 Analyzer setup with an EZ Zone controller Figure 2 Analyzer setup with a SD controller 3 1 8 Select Complex on RA 915 s main menu screen a table window Table Complex analysis and a graph window Complex Sample analysis Graph 105 Onto UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment both activate Click on the window headers to alternate between the two screens 3 1 9 Click the run icon d from graph window Mercury signal will begin to be recorded with a sampling frequency of 1 second Expand the Current Value window to see the second by second readings which are also graphed as the red line 3 1 10 Enter information in table window Name and Save the table file into a specified folder 3 1 11 Allow the system to warm up for at least 30 minutes before calibration 3 1 12 Click the statistics icon to view the average baseline value and the baseline RSD After 20 minutes if the RSD is higher than 5 shut off the furnace allow it to cool down and clean the optical detector windows 3 1 13 Click the icon Y baseline check and allow the baseline to adjust for 10 seconds Click on Y again to turn off the baseline adjustment and complete the baseline correction Repeat this step until the average baseline is near zero and the RSD is less than 4 After the initial start up of the instrument baseline drift will be at its m
102. rmine the mercury concentration in the flue gas 4 CALCULATIONS AND DATA ANALYSIS All calculations and data analysis are explained in section 12 0 of Method 30B These calculations are listed below Nomenclature The terms used in the equations are defined as follows B Breakthrough Bws Moisture content of sample gas as measured by Method 4 percent 100 Ca Concentration of Hg for the sample collection period for sorbent trap a ug dscm C Concentration of Hg for the sample collection period for sorbent trap b ug dscm Ca Hg concentration dry basis ug dscm Crec Concentration of spiked compound measured ug m3 70 QOuio i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Cw Hg concentration wet basis ug m3 m Mass of Hg measured on sorbent trap section 1 ug m z Mass of Hg measured on sorbent trap section 2 ug Mrecovered Mass of spiked Hg recovered in Analytical Bias or Field Recovery Test ug Ms Total mass of Hg measured on spiked trap in Field Recovery Test ug Mspiked Mass of Hg spiked in Analytical Bias or Field Recovery Test ug mu Total mass of Hg measured on unspiked trap in Field Recovery Test ug R Percentage of spiked mass recovered RD Relative deviation between the Hg concentrations from traps a and b vs Volume of gas sampled spiked trap in Field Recovery Test dscm Vt Total volume of dry gas met
103. rophotometry US EPA 2007 www epa gov sw 846 pdfs 7473 pdf 3 Method 30B Determination of total vapor phase mercury emissions from coal fired combustion sources using carbon sorbent traps US EPA 2008 http www epa gov ttn emc promgate Meth30B pdf 4 Appendix K to Part 75 Quality assurance and operating procedures for sorbent trap monitoring system US EPA 2005 124 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 9263 Ravenna Rd Suite A 3 Onog Twinsburg OH 44087 UMEX Toll Free 888 876 2611 APPENDIX M SPECIATION TRAP STANDARD OPERATING PROCEDURE Subject Mercury Emissions Monitoring Program Speciation Sorbent Trap Sampling and Analysis Brief Prepared by Analytical Laboratory of Ohio Lumex Company Revised on January 15 2013 125 Ono UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 1 SPECIATION TRAP SAMPLING PROCEDURE RECOMMENDATIONS AGS Hp2 absorption Carbon SO Acid Gas Scrubber AGS S1 Oxidized Mercury Analytical Bed KCI S2 Oxidized Mercury Breakthrough Bed KCl S3 Elemental Mercury Analytical Bed Carbon S4 Elemental Mercury Analytical Bed Carbon Figure 1 Illustration of a Speciation Trap There are two types of sampling locations and each has its own set of procedures and recommendations to follow Please use the following procedures when sampling and analyzing Speciation traps FGD INLET A
104. s section 2 breakthrough amounts and most importantly for section 1 sample amounts that are very low Looking at table 9 1 in the method we see that sample analysis only have to be within the valid calibration range if the mercury concentration of the source is greater than or equal to 0 5 ug dscm We also see that section 1 sample amounts only have to be within the bounds of the Bias Test if the source is greater than or equal to 0 5 ug dscm In other words according to the method section 1 sample amounts do not have to be bracketed by the multi point calibration or the Bias Test for sources that are lt 0 5 ug dscm This means that you don t have to make heroic efforts to successfully perform a special Bias Test or Initial Calibration at very low levels for these sources Section 2 Breakthrough and Paired Trap Relative Deviation Further review of table 9 1 shows that for sources where the mercury concentration is lt 1 0 ug dscm the limits for acceptable breakthrough and Relative Deviation for paired trap agreement double from 10 to 20 This is a big help especially when dealing with breakthrough for section 1 amounts that are very small 84 Onto O f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Field Recovery Test The method requires that the spike levels for the Field Recovery Test must be within 50 to 150 of the expected sample amount but not the actual sample amount and there
105. s used to Standards determine an instrument calibration CCVS Continuing Calibration Verification Standard Hg Mercury Hg Elemental Mercury Oxidized Mercury 0 1 1 1 HgCle Mercuric Chloride 0 1 1 2 HCl Hydrochloric Acid Independent NIST traceable or certified mercury standards from separate lot standards or manufactures than the calibration standards Method detection limit the lowest mass of Hg greater than zero that can be estimated and reported by your analytical technique Method 30B a procedure published by US EPA for measuring total vapor phase mercury emissions from coal fired combustion source using sorbent trap sampling and an extractive or thermal analytical technique NIST National Institute of Standards and Technology located in 69 Onto i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Gaithersburg Maryland Profile A temperature control program loaded into EZ Zone Controller by Ohio Lumex Company prior to shipping the system to the end user RATA Relative Accuracy Test Audit sorbent Media used in traps to adsorb mercury May be halogenated or non halogenated Trap Glass tube packed with one two three or more beds of sorbent held in place and separated by glass wool The sample trap is placed in the sampling probe and flue gas is pulled through the sample trap The carbon in the trap adsorbs mercury which is then used to dete
106. s wool plug in one ladle Using these traps can streamline the trap analysis procedure e Analyze the plug and carbon separately If you need to analyze the larger section traps 1 0 gram it may be easier to analyze the carbon and the glass wool plugs separately 82 Onto or UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Appendix H Tips for Successfully Using Method 30 B to Perform Mercury RATAs at Low Level Sources it s Easier than You Think Be careful with these recommendations and make sure that the RATA you are performing also complies with any specific state mandates The new Mats Rule referenced in 40 CFR Part 60 amp 63 has changed some of the criteria for a Mercury RATA as shown 4 1 2 2 The special considerations specified in paragraph 4 1 1 5 1 of this section apply to the RATA of a sorbent trap monitoring system Also special consideration changes have been made to breakthrough criteria when performing a RATA on a sorbent trap sampling system as referenced below 4 1 1 5 1 Special Considerations A minimum of nine valid test runs must be performed directly comparing the CEMS measurements to the reference method More than nine test runs may be performed If this option is chosen the results from a maximum of three test runs may be rejected so long as the total number of test results used to determine the relative accuracy is greater than or equal to nine however all data must be rep
107. sachusetts RTK Substance List No ingredient regulated by MA Right to Know Law present US Pennsylvania RTK Hazardous Substances No ingredient regulated by PA Right to Know Law present US Rhode Isiand RTK No ingredient regulated by R Right to Know Law present Inventory Status Australia AICS On or in compliance with the inventory Canada DSL Inventory List On or in compliance with the inventory EINECS ELINCS or NLP On or in compliance with the inventory Japan ENCS List On or in compliance with the inventory China Inv Existing Chemical Substances Not in compliance with the inventory Korea Existing Chemicals Inv KECI On or in compliance with the inventory Canada NDSL Inventory Not in compliance with the inventory Philippines PICCS On or in compliance with the inventory US TSCA Inventory On or in compliance with the inventory New Zealand Inventory of Chemicals On or in compliance with the inventory Japan ISHL Listing On or in compliance with the inventory Japan Pharmacopoeia Listing Not in compliance with the inventory 16 Other information including date of preparation or last revision NFPA Hazard ID Flammability Health Reactivity Special hazard Hazard rating 0 Minimal 1 Slight 2 Moderate 3 Serious 4 Severe Issue date 05 12 2014 SDS_US SDS000000960 141 AGANTON PERRA E tet A Revision date Version Further information Disclaimer SDS_US SDS000000960 Version
108. script Blank reF data Units DE SES Ta S Srea Height Measurement Date Time Interval s ban E ng g mg 37080 3539 7 16 04 2013 15 08 58 661 7 43 6717 28 ae ng g mg 17570 1934 2 16 04 2013 15 06 58 6507 28 6580 90 Std _10 ng g mg 3792 399 4 16 04 2013 15 08 58 6365 38 6404 95 a Haa ii at aa a A ria t a a a a de e n a Processing Picture 4 4 23 QOuio D UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 9 Under Data view click Table view amp use the scroll bar to locate the Calculated ng g mass per each Standard used in the calibration 10 Once satisfied name your calibration and click Save Picture 4 5 Calibration results S Sblank Update view Correlation coe 0 9997 Residual standard deviation SS Calibration S Sbleank om 367000 0000 Sbtenk 0 0000 Help Save Picture 4 5 4 2 Mark amp Integrate Calibration Method 1 Allow RA 915M M 324 System to warm up for at least 45 minutes 2 Fill in Sample description ref data amp Mass Volume Picture 4 6 e Note The example used below assumes an initial calibration point of 10 nanograms Yours may be different depending on sample parameters e Note ref data refers to the expected mass of the Standard being used e Note When analyzing sorbent traps the Mass Volume will ALWAYS
109. t It is important to clean ladles and tools before testing any standards or samples Mercury deposited on the ladle would influence the calibration and testing By inserting an empty ladle into a heated furnace Temperature gt 500 C for at least 90 seconds any potential mercury contamination on the ladle will be removed The glass wool extractor and tweezers should also be cleaned using a torch by burning the ends of both instruments for approximately 5 seconds Calibration sorbent media must be stored in a sealed container Any media exposed to air for more than 5 hours should not be used for calibration purposes Only National Institute of Standards and Technology NIST certified or NIST traceable calibration standards and standard reference materials should be used for the analytical procedures The entire set of Ohio Lumex calibration standards consists of 0 01 ug ml 0 1 ug ml 1 0 ug ml 10 0 ug ml 100 0 ug ml 1000 0 ug ml and second source of 0 1 ug ml 1 0 ug ml 10 0 ug ml 100 0 ug ml Hg solution Depending on the calibration range not all standards are needed to make a calibration Section 11 1 of Method 30B states that the user must Perform a multipoint calibration of the analyzer using at least 58 Onto O f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment three calibration points The expiration date of a standard must always be checked before a calibration is run Manufacturer con
110. the anticipated range of masses collected in the field samples Steps on how to properly perform a Spike Recovery Study on the Ohio Lumex RA 915M RP M324 Sorbent Trap Mercury Analyzer System are listed below e Put the instrument in the configuration you intend to use for analyzing PS 12B samples This example uses Profile 2 settings e Calibrate the instrument by running 5 or 6 calibration points ranging 10ng 4 000ng Ensure the calibration is valid by running an Initial Calibration Verification Standard The calibration should meet all the performance criteria as described in PS 12B Analyze Continuing Calibration Verification Standards CCVS routinely as you continue e Analyze three low level PS 12B spiked traps 10ng or 20ng The average spike recovery for each trap must fall between 85 and 115 of expected mass e Analyze three mid level PS 12B spiked traps 1 000ng or 2 000ng The average spike recovery for each trap must fall between 85 and 115 of expected mass e Analyze three high level PS 12B traps 3 000ng or 4 000ng The average spike recovery for each trap must fall between 85 and 115 of expected mass e The Spike Recovery Study meets all the necessary guidelines outlined in PS 12B if all three sets of traps had average recoveries within 15 of expected spike 79 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment values Spike Recovery Study meets the necessary PS 12B guidelines an
111. the instrument as you would typically to make sure it s measuring with accuracy and precision run 5 or 6 points typically from 10ng to 2 000ng also run a blank and a second source standard The calibration should meet the requirements of Method 30 B and the PS 12B method Analyze Continuing Calibration Verification 77 Onto O f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Standards CCVSs routinely as you continue 3 Analyze three low level traps 10ng or 20ng is a good level The average recovery for the three traps must be within 10 of expected spike value 4 Analyze three high level traps choose a level that is just below the highest point in your calibration to provide the maximum range The average recovery for these three traps must be within 10 of expected spike value 5 Next make three standards using aqueous solutions preserved in acid at the same mercury mass level as the low level spiked sorbent traps i e 20ng in this example and analyze them The average recovery for these three traps must be within 10 of expected spike value 6 Make three standards using aqueous solutions preserved in acid at the same mercury mass level as the high level spiked sorbent traps and analyze them making sure that the average recovery for these three traps is within 10 of expected spike value 7 lf all the sets of three had average recoveries within 10 of expected spike values the Bias Test meets
112. the method guidelines and the analyzer can be used to analyze samples that have section 1 sample amounts between the high and low points that you chose Section 1 sample amounts below the amount you chose can be analyzed as well if they are from a low level source Additional Steps to Complete the PS 12B Spike Recovery Test Once the steps above have been performed very little is needed to complete the Spike Recovery Test 1 Analyze three sorbent traps spiked with elemental mercury at a medium level that is between the low level and high level used above 2 lf the average recovery of these three sorbent traps is within 15 of the expected spike value then these results and those of the spiked traps above represent a valid PS 12B Spike Recovery Test Since the recovery requirement for the PS 12B method is within 15 of the expected spike value the passing results for the 30B sorbent traps 78 Onto or UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment within 10 of the expected spike value are more than adequate for this method Appendix F Performing a Spike Recovery Study PS 12B on the Ohio Lumex RA 915M RP M324 Sorbent Trap Mercury Analyzer System A Spike Recovery Study must be performed in order to demonstrate the ability of the analytical system to recover and quantify elemental Hg from the sorbent media Three 3 section PS 12B style traps are spiked at three different mass loadings representing
113. ther solid samples can be analyzed and quantified easily using the Ohio Lumex RA 915M RP M324 Sorbent Trap Mercury Analyzer Here are some guidelines and tips to make the analysis go smoothly e Use the instruments most sensitive setting usually Profile 1 e Calibrate the instrument as you would for trap analysis e The coal to be analyzed should be reasonably pulverized e Place the sample ladle on a suitable balance a 3 place balance that can measure down to 0 000 g and tare the ladle e Evenly distribute 100 200 mg of the coal sample on the bottom of the ladle and record the mass e Remember coal has relatively low mercury content so enough needs to be added in order to form a good peak but using too much will produce a lot of smoke which will overwhelm the filtering layers described below A mass of 100 200 mg has proven to be a suitable amount e On top of the coal add a layer of iodinated carbon to cover the coal This layer of carbon filters the smoke and helps make a well defined peak Do not use too much make sure to leave room for the next step e On top of this add a heavy layer of sodium carbonate e Wipe excess sodium carbonate off the top then pack the sample down using a clean piece of aluminum foil e Add some more sodium carbonate and again compress this with the aluminum foil Be careful not to use so much that you spill any in the furnace e Inthe analyzer s software spreadsheet window enter the s
114. tional yet they cannot be used in the calibration 113 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment The Hg amount in each sample must fall into the calibrated range of the analyzer and within the lower and upper mass limits established during the initial Hg and HgClz analytical bias test For extra low level samples Hg mass is below the lowest point in the calibration curve and above the MDL a response factor e g area count per Hg mass is established based on a single standard at level gt MDL and less than the lowest point in the calibration The amount of Hg present in the sample is calculated based on the analytical response and this response factor 114 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 3 4 Preparation of Sorbent Traps for Analyzing and Analysis Procedures The end cap of a sorbent trap is removed the glass wool plug prior to the appropriate carbon bed is carefully removed and separated from the sorbent section The sorbent is transferred into a quartz ladle and then covered with anhydrous sodium carbonate until the ladle is full Cover the ladle opening with a piece of aluminum foil and finger press the materials in the ladle Make sure the sodium is on the top of the sorbent and be pressed very tightly The ladle is then inserted into the M 324 thermo catalytic conversion chamber The glass wool plug is tightly wrapped into aluminum foil
115. tration Le 2 Ca Cy 12 5 Moisture Correction Use Equation 30B 4 if your measurements need to be corrected to a wet basis C C 1 B Eq 30B 4 122 Onto DS UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 12 6 Calculation of Paired Trap Agreement Calculate the relative deviation D between the H ions measured with the paired sorben i Equation 30B 5 C C RD Ca Cl 100 Eq 30B 5 C 6 12 7 Calculation of Measured Spike Hg Concentration Field Recovery Test Calculate the measured spike concentration Equation 30B 6 Coo _30B 6 my Fq Then calculate the spiked Hg recovery R using Equation 30B 7 Ramm 5100 Eq 30B 7 I gest 123 QOuio i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 6 HEALTH AND SAFETY 6 1 f performing the test sampling follow the Source Plant safety protocol to ensure any hazards are avoided 6 2 Proper protective equipment lab coats safety glasses particulate respirator nitrile gloves should be worn while performing analysis 6 3 Please refer to the provided Material Safety Data Sheets for every chemical used in order to avoid injury or reactions 7 REFERENCES 1 Thermal analysis for field sorbent trap mercury testing Instruction hand book Ohio Lumex Company Inc 2006 2 Method 7473 Mercury in solids and solutions by thermal decomposition amalgamation and atomic absorption spect
116. ve The current value window shows the mercury intensity for each second Zero the baseline for 10 seconds if necessary At a static state RSD should be a stable value 3 BLANK Place cursor in description column second column beside No 1 Double click left mouse and select BLANK Using the tab button on the keyboard tab to the mass column third column labeled M mg enter number 1 into the box then tab over to the concentration column labeled C ng g 4 Switch back to the Complex analysis graph to view the graph of analysis 5 Place calibration sorbent into a ladle about 0 4g sorbent when Method 30B Speciation traps are going to be tested Cover the sorbent with anhydrous sodium carbonate Gently pack the sorbent and sodium carbonate in the ladle by covering the opening with a piece of aluminum foil and compressing the solids through the foil with your finger Sodium carbonate must completely cover the sorbent Remove the aluminum foil from the ladle before analysis 6 Click START on the integration window Immediately insert the prepared ladle into the furnace 7 Mercury signal is shown as red in the graph The reading of the current value is shown in a separately small window 109 QOuio i f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 8 Click END on the integration window to stop the analysis once the current value readings come back to the original starting point and th
117. vent water from getting inside the cartridge head Pictures 7 23 and 7 24 Warning do not get liquid inside the flanged part of the cartridge Picture 7 23 Picture 7 24 4 Pump The Mass Flow controller maintains constant pump flow and usually does not require adjustments Plugged filters or kinked hoses may cause pump to exceed auto compensation range which causes an Alarm on the mass flow controller screen If adjustments to flow rate are necessary change flow set point by using the up amp down arrows Press Enter to store new set point Flow for Profile 1 may be adjusted from 0 5 LPM to 2 LPM Flow for Profiles 2 3 amp 4 is 4 0 LPM 47 QOuio i UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 5 Shut Down Procedure Save your work on computer in a designated folder BEFORE shutting down Turn the Power Switch off on the pump station Power Lumex Off by pressing the Power button on top of the analyzer To preserve lamp do not leave analyzer powered ON unless needed 48 Onto O f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment Appendix A User Experiences 1 Analyze Continuous Verification Standard after every paired train samples This will prevent any invalid runs in the future 2 Do not be afraid to recalibrate analyzer during analysis if you observe a consistent shift in Cont Verif Standard values A 3 point calibration done in the middle of the da
118. veral minutes Remove contact lenses if present and easy to do Continue rinsing If eye irritation persists Get medical advice attention IF ON SKIN Wash with plenty of water Take off contaminated clothing and wash it before reuse If skin irritation occurs Get medical advice attention Specific treatment see this label Storage Store in a well ventilated place Keep container tightly closed Store locked up Disposal Dispose of contents container to an appropriate treatment and disposal facility in accordance with applicable laws and regulations and product characteristics at time of disposal Other hazards which do not None result in GHS classification 3 Composition information on ingredients Substances Common name CAS P Chemical identity Content in percent SODIUM CARBONATE 497 198 99 100 Ali concentrations are percent by weight unless ingredient is a gas Gas concentrations are in percent by volume 4 First aid measures General information ingestion Inhalation Skin contact Eye contact Get medical advice attention if you feel unwell Show this safety data sheet to the doctor in attendance Rinse mouth Call a POISON CENTER or doctor physician if you feel unwell Move to fresh air Get medical attention Wash skin thoroughly with soap and water Get medical attention if symptoms occur Immediately flush with plenty of water for at least 15 minutes If easy to do
119. x RA 915M and RP M324 Attachment 13 Align Red Dots amp Attach Power Supply to Furnace see Picture 2 13 Picture 2 13 14 See below what the M 324M Workplace looks like see Picture 2 14 Picture 2 14 12 OHA nex Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 15 To start the pump Press Power Button on Power Supply see Picture 2 15 Picture 2 15 16 Complete Setup with Heat Shield see Picture 2 16 Were if tea RPM 089 Heat Shield for M324 RP91C Mirne RP M324 Attachment Zeeman Spectrometer www ohiolumex com RU Re ODLU ANLI DDA IN Picture 2 16 13 Ouio o UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 17 Turn Power ON select Profile 1 on the Watlow EZ Zone controller see Picture 2 17 and allow Furnace to Heat up for 45 minutes with pump ON Green number is a Set Temperature and Red number is Furnace Temperature Infinity Key Advance Key Furnace Temperature Profile Signal Up Key Down Key Set Point Picture 2 17 14 Onto UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 2 2 Selecting and Running Temperature Profiles with EZ ZONE RP M324 controller Start up and Profile selection Denotations InfK Black infinity key AdvK green advance key 1 Turn Power ON warm up furnace at 680 C for approximately 45 min with pump ON 2 Press AdvK Select profile 1 2 3 or 4 by pressing U
120. y will only improve your data quality 3 If a ladle comes out of the furnace with carbon burning in the middle and soda fused to quartz happens only in profile 1 your furnace is too hot This is major cause of broken ladles Reset power of temperature controller without initiating Profile change by using the down arrow key on the controller to drop temperature from preset 680 to 650 or 630 C This setting will be remembered by the controller but will be overridden once profile 1 is initiated 4 Use a lot of soda on top of the carbon If you spill some inside the oven use a shop vacuum to suck the hot furnace from the ladle port intake disconnect output hoses of the furnace from the filter to get the full flow Remember to reconnect hoses 5 Never introduce samples or calibrate with the pump OFF or filters disconnected furnace contamination will occur 6 To clean furnace contamination leave it ON overnight with Pump ON in profile 1 analyzer should be OFF 49 Ono f UMEX Sorbent Trap Analysis with the Lumex RA 915M and RP M324 Attachment 7 Baseline noise a dirty ladles wash in hot water b contaminated furnace see above c dirty windows all windows need cleaning 2 in the furnace and 1 on the analyzer 8 If you expect continuous testing and would like to save on the furnace warm up time in the morning keep the pump and furnace on in profile 1 overnight 9 To save time and minimize analysis an

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