United States Office of Air Quality EPA-340/1 -85-013b Environmental Protection Planning and Standards December 1984 Agency Washington, D.C. 20460 Stationary Source Compliance Series Field Inspection Notebook for Monitoring Total Reduced Sulfur (TRS) from Kraft Pulp Mills ------- EPA-340/1-85-013b Field Inspection Notebook for Monitoring Total Reduced Sulfur (TRS) from Kraft Pulp Mills Prepared by William T. Winberry, Jr. Engineering-Science 501 Willard Street Durham, North Carolina 27701 Contract No. 68-02-3960 Work Assignment No. 53 EPA Project Manager: John Busik EPA Work Assignment Manager: Sonya M. Stelmack U.S. ENVIRONMENTAL PROTECTION AGENCY Stationary Source Compliance Division Office of Air Quality Planning and Standards Washington, D C 20460 December 1984 ------- DISCLAIMER This report was furnished to the Environmental Protection Agency by Engineering-Science, 501 Willard Street, Durham, N. C., 27701 in fulfill- ment of Contract No. 68-02-3960, Work Assignment No. 53. The opinions, findings, and conclusions expressed are those of the author and not necessarily those of the U. S. Environmental Protection Agency. Mention of company or product names is not to be considered as an endorsement by the Environmental Protection Agency. 11 ------- TABLE OF CONTENTS Page Subject Number Introduction 1 Field Inspection Notebook Objective 2 Inspection Procedures 5 Level I 7 Level II , ,. , .,,..,, 11 Level III 29 Monitor Specific Inspection Procedures 33 Sampling Technology Inc 35 Barton Titrator ,.,,,,..,,,,,.., ,,< 43 Bendix TRS CEM System 51 Level IV., 61 Reference Method 16 Observation Checklist 63 Reference Method 16A Observation Checklist 83 Abbreviated Inspection Procedures , 97 Appendix, , , , , , 109 ------- FIELD INSPECTION NOTEBOOK TOTAL REDUCED SULFUR CONTINUOUS EMISSION MONITORING SYSTEM INTRODUCTION This notebook is intended to assist the field inspector in the inspec- tion of total reduced sulfur (TRS) continuous emission monitoring systems (CEMs). Contained in the notebook are checklists and data entry tables covering preparation for the inspection, preliminary review of records, preliminary on-site meeting with source personnel, and general guidelines for inspection of any type TRS CEM system. Specific audit procedures for three of the most common models of TRS CEMs: - Sampling Technology Inc. Model 100 TRS CEM System (pg. 35); - Barton Titrator TRS System (pg. 43); and - Bendix Gas Chromatograph TRS System (pg. 51) are provided as sectional inserts. In auditing these monitors the inspector should follow the specific procedure rather than the general guidelines given in the body of the field notebook. Conscientious use of this notebook will aid the inspector in conducting a thorough audit of the TRS CEM system and provide a comprehensive original record of all phases of the inspection. ------- FIELD INSPECTION NOTEBOOK OBJECTIVE This notebook is designed to provide a complete unit checklist for inspection of an TRS CEM system. The inspection procedures follow the control agency inspection program, dealing with the "phase" and "level" approach. The "phase" process consists of administrative activities involved with initial CEM system application, performance testing and final approval This enables the state agency to approve the monitoring system through es- tablished certification procedures. The type of activities at each phase are: Phase I - Control agency initial approval of CEM application as required through source permit; Phase II - Control agency observation of performance specification testing (PST) of the installed CEM system; and Phase III - Control agency review of the PST report, with final approval or disapproval. The "level" approach begins after completion of the "phase" evalua- tion. The levels of CEM system inspection extend from agency source records review (lowest level) to stack test compliance determination (highest level). The inspection determines or confirms compliance and identifies causes of excess emissions. The types of activities at each level are: Level I - Control agency records review including excess emission reports, previous inspection reports, source "working" file and and permits; Level II - On-site inspection involving review of monitor record- keeping (maintenance, monitor and control equipment logs), monitor fault indicator, monitor internal zero/span check, strip chart review and electronic checks; Level III - Evaluation of installed CEMS through external audit evaluation involving neutral density filters for opacity monitors and gas cylinders/permeation tubes for gas monitors; Level IV - Comparative evaluation of installed CEMs through perform- ance testing utilizing Federal Reference Methods or portable CEMs. The "phase" and "level" audit procedure has been designed so that each activity indicates whether or not the CEM system has achieved the necessary level of compliance before starting the next phase. ------- The main objective, of this notebook is to cover in detail the inspec- tion procedure covering the "level" section of a control agency CEM system inspection program. During the inspection the inspector may need to add comments, explanations or • her notes to the notebook. To aid in referenc- ing these comments, a colum,, under the heading of Check or Comment has been provided along the right margin of all pages containing inspection data. These blank lines may be used to indicate action items or to enter code numbers referencing entries elsewhere in the notebook. Once a thorough evaluation of the TRS CEM system has been accomplished, control agency personnel may want to perform the next inspection on a less compreshensive basis. To assist the control agency personnel, an abbre- viated inspection procedure checklist has been developed. The abbreviated checklist is applicable to all TRS CEM systems. It does not address moni- tor specific inspection points, but does evaluate the TRS monitor on a system audit basis. The checklist is divided into three major areas: o Control agency records review; o Control agency records update; and o Source TRS CEM system review. The control agency records review consists of a review of permits and/ or any current enforcement actions to determine the purpose of the CEM. In addition, a review of the PST report and current EER is conducted to verify conformance with the appropriate performance specification and re- porting requirements for EERs. The control agency records update is conducted by telephone to verify that the records in agency files correctly describe the current CEM status. Finally, the source TRS CEM system review evaluates a source's record- keeping, data reduction procedures, monitor evaluation through zero/span checks and overall system review. ------- INSPECTION PROCEDURES Concurrent with the "level" approach philosophy, the CEM inspection begins with a "thorough" working knowledge of the facility by reviewing the "permanent" and "working" file of the source in the agency office. Next, the inspection proceeds to the facility where other information is gathered to support the records review activity. While on the premises, the inspector reviews all records which would provide information associated with the monitoring system. Then, a review of the monitoring system is in order. For a TRS extractive system, heat tracing, insulation, weather pro- tection, transport lines, and connection material should be inspected. The field inspector should evaluate monitor location for ease of maintenance, representative sampling, and environmental factors such as vibration and temperature. The calibration gas interface with the sample system should be inspected and their relative proximity noted. The inspector should verify that during calibration the pressure of the calibrator gas at the interface is approximately equal to its pressure during sampling. The inspector should observe CEM calibration procedures to confirm calibration reference values and provide a spontaneous quality assurance check. Documentation of calibration gas values by Protocol 1 traceability or triplicate reference method analysis should be available in plant records and verified during the field inspection. Finally, the CEM control unit and signal recording device should be inspected. The inspector should review previous 24-hour emissions and zero/span check. He should initiate a zero/span check and compare to recorded values. To assist the inspector, the front part of the notebook covers Levels I, II, III, and IV inspection procedures. These are generic in nature, adaptable to any TRS CEM system. The latter part of the notebook covers specific TRS CEM inspection procedures. ------- FIELD INSPECTION NOTEBOOK TOTAL REDUCED SULFUR CONTINUOUS EMISSION MONITORING SYSTEM 1.0 LEVEL I CHECKLIST 1.1 SOURCE IDENTIFICATION Company Name Mailing Address Location of Facility (Include County or Parish) Personnel Name Title Phone o Facility Manager o Environmental Manager o Facility Contact o Confidentiality State- ment Requi red 1.2 PREPARATION FOR INSPECTION 1.2.1 Source Notification o Has the appropriate representative of the source been notified of the time and date of auditor's intended visit? Yes No By phone By letter Name of Representative Date contacted Record of notification filed ------- 1.2.2 Review of Source's Permit to Operate o Permit information pertinent to the CEM audit is contained in the followi ng checkli st. CEM requirement due to: Permit NSPS SIP Enforcement Action Date CEM installation completed Date CEM started up _____ _____ Gases monitored TRS Opacity 0;?_ Allowable emission rates TRS 0 p a c i ty 1.2.3 CEM Equipment Summary Pollutant Manufacturer Model/Type Process Monitor/Analyzer _____ Data Recorder Data Processor 1.2.4 Review of Performance Specification Test Report o A CEM Performance Specification Test (PST) report should be on file. Information to be reviewed is contained in the following checkli st. Dates of Operational Test Period (OTP) (<30 days after perform- ance test) Date PST report submitted (<60 days after OTP) Date of process startup (<180 days prior to OTP)_ Date of initial full-load operation (<60 days prior to OTP) Emission rate conversion formula(s) ------- o PST Summary Results TRS Relative Accuracy 02 NA Opacity NA Response Time 24 Hr. Span Drift 24 Hr. Zero Drift 1.2.5 Review of Excess Emissions Reports o The following checklist summarizes pertinent information to be obtained from excess emissions reports. Months covered by reports Did each excess emission report document: Date, time, and duration of excess emissions? Yes No Magnitude of excess emissions? Yes No Reason for excess emissions? Yes No Corrective action taken to reduce emissions? Yes No_ Conversions factor/formula? Yes No Method for determining conversion or correction factors used in calculating emission rate. Process downtime None Monitor downtime None If significant monitor downtime occurred, briefly discuss corrective action taken to return monitor to operation. ------- What percent availability did the CEM system achieve? % availability = Hours of monitor operation Hours of process operation o Select one excess emission event and record: Date Time Magnitude Reason Corrective Action This information is intended for use during Level II evaluation. 10 ------- 2.0 LEVEL II CHECKLIST 2.1 PRE-INSPECTION MEETING Before the CEM inspection, the inspector should arrange to meet with source representatives directly responsible for CEM operation and mainte- nance, compliance, records and reports. The purpose of the opening con- ference is to inform facility official(s) of the purpose of the inspec- tion, the authority under which it wil be conducted, and the procedures to be followed, and answer any questions they may have. The opening con- ference also offers the inspector the opportunity to completely discuss agency policy and inspection procedures, and to provide relevant informa- tion and other assistance. The inspector's effective execution of the opening conference often sets the tone of the remainder of the inspection. During the opening conference, the discussion should cover the fol1owing items: COVERED o Inspection objectives o Inspection agenda o Facility Information verification o Review of records o Maintenance o CEM Operation Logbook o Strip Charts o Data Log o Control Equipment Records o Excess Emission Reports o Source Permit o Safety Requirements o Scheduling of Source Personnel Interviews o Inspection Techniques to Be Used o Scheduling of Copying Needed Documentation o Any Questions 11 ------- In particular, the inspector should develop his or her understanding of the operation/maintenance of the audited system to ascertain whether the TRS CEM system has been operated according to permit condition since the last inspection. The inspector should be able to support any conclu- sions by: o Examination of CEM maintenance records; o CEM span and zero calibration checks over previous quarter; o Reviewing the CEM program; o Records comparison, i.e., correlation of excess emission reports, strip chart records, operations and maintenance records, and computer printouts ( if available); and o Reviewing files to identify missing documents (if any). The following checklists are provided to assist the inspector in conducting the preliminary meeting. 2.1.1 Personnel In Attendance Phone Name Affi liation Title/Responsi bi 1 ity Number 12 ------- 2.1.2 Review of CEM Maintenance Records. o Describe significant CEM maintenance since last audit. Date/time Description Type* Performed *Routine, Preventive, Emergency, etc. o Recurring Maintenance Problems (Last 12 Months) 2.1.3 Review of Calibration Frequency Calibration Relative Zero Span Error* Accuracy* Estimate of Calibration Frequency *0ptional o Describe Unusual or Persistent Monitor Calibration problems 13 ------- 2.1.4 General Review of CEM Program o Is an alarm connected to CEM control panel or annunciator panel in process control room to signal excess emissions? Yes No o How often is CEM strip chart or computer output checked hy an operator? o What procedures are implemented during an excess emission in- cident to reduce emissions? o Do records contain process data needed for conversion of CEM output to units of the standard (i.e., moisture, velocity, oxygen correction)? Yes No o Are process data measurements conducted? Yes_ No_ o Do records contain current information on calibration reference materials (gases, permeation tubes, cells, filters)? Yes No o Are entries into Maintenance and Operations Logs made on monitor: Malfunction? Yes No_ Calibrations? Yes No_ Maintenance? Yes No QA Checks? Yes No_ o Are charts/printouts for the past two years filed and readily retrievable? Yes No_ 14 ------- 2.1.5 Internal Consistency of Records and Reports It should be possible to relate the emission excursions reported in the Excess Emissions Report with the recorded CEM data showing the occur- rence of excess emissions. Such excursions should also be documented in the CEM Log, which should include a report of the incident and the correc- tive action taken by the source. In those cases where a mechanical problem is cited as the cause of the excess emissions, maintenance records should show corrective action taken by the source. The inspector should try to determine the time between the measured excess emissions incident and the initiation of corrective action. o Report of Excess Emissions (Enter data from Level I Review) Time Date From To Pollutant %02 Magnitude (ppm) o Description of Excess Emissions from CEM or operating Log on above date. o Identification of Excess Emissions Incident in Chart Record Last Last Calculated Above Zero Span Average equivalent Date Time Check Check (ppm) (ppm) corrected) o Subsequent Corrective Action Described in Maintenance Log (if appli cable), and date and time initiated Are dates and times of above records consistent in recording this excess emission event? Yes No_ o If No, explain 15 ------- 2.2 TRS CEM FIELD INSPECTION The general inspection procedures presented on the following pages cover extractive TRS CEM systems. These procedures should be followed when a monitor-specific procedure is unavailable. Check or Conment 2.2.1 TRS CEM Operational Environment o Is the process monitored by the TRS CEM operating within normal limits as com- pared to the source performance test? Yes No (If process is not operating within normal limits, Inspector should delay any part of audit which requires normal process conditions.) o Process Capacity o Process Rate o Stack Gases TRS Opacity Monitored: (Avg. Cone.) 02 o Stack Gas Temperature °F o Pollution Control Device o Is the analyzer unit subject to excessive heat? Yes No o Is the analyzer unit subject to excessive vibration? Yes No [Note: Excessive heat/vibrations are meaningful only if system (1) fails to satisfy the operations specified by vendor or (2) fail to meet PST 5.] o Frequency of sampling: per hour 2.2.2 Measurements and Data Handling The following checklists are intended to assist the inspector in an analysis of the source's data handling and data reduction practices. At some facilities data reduction is done by a computer programmed to convert stack gas concentrations directly and continuously to the units of the applicable emission standard. At other facilities manual calculations of emissions in units of the standard are only done for periods of excess emissions. 17 ------- 2.2.2.1 Data Handling o How is data reduction handled? Manually Electronically o How many data points are used to calculate each average? o Are these data points taken at equally spaced time intervals? Yes No o If yes, what is that time interval? o If data reduction is manual, how often is it done? Check or Comment o Who performs manual data reduction? o Are the data adjusted to account for zero drift measurements? Yes No o Are the data corrected to account for calibration (span) drift measurements? Yes ___ No ___ o Does the source arbitrarily edit the data before reduction? Yes No o If yes, what criteria is used to edit? ________ 2.2.2.2 Electronic Data Reduction: o Who wrote the program for calculating averages? o Is the source's data processing system time shared or dedicated? o Was it installed with the monitoring system or added at a later date? ___ 18 ------- o Who installed the data processing system? Check or Comment o At what interval does the data logger acquire CEM measurements? o Does the system include a data recorder as well as a chart? Yes No o If yes, indicate which kind. Magnetic tape Paper tape Paper print-out o If both automated data processing and chart recording are done, does the CEM value from the automated data processor agree with the value recorded on the chart? Yes No o If no, explain. o Indicate which functions the automated data processing system performs. Data recording Data storage Averaging Period Hourly summary Daily summary Other summary (explain) Identification of excess emissions Display instantaneous value Alarm 19 ------- Check or Comment Records process equipment malfunction codes Records pollution control equipment malfunction codes Records excess emission codes 2.2.2.3 Internal Zero/Span Check o Write date and time on chart or data processor at start of inspection o Record current emissions Current Emissions TRS (ppm) Opacity o Request internal zero and upscale calibratrion, enter results below, and compare results to typical previous values. Monitor Response Zero Span Calibration Value Zero Span o Review previous day's recording for typical emissions, repeated zero/span checks, etc. Yes No Emissions normal Calibration normal Exceedances above the standard Calibrations noted on data processor and reviewed Operator aware of emission limits 20 ------- Check or Comment 2.2.3 Inspection of Monitor Control Unit Although instrumentation differs among the various types and models of TRS CEM's, many will incorporate some or all of these control indi- cators or switches. The inspector should locate those in use and enter their position/status below. TRS 02 Opacity o Reference o Calibration __ o Alarm o Temperature o Sample gas o Stack gas _______ _______ o Heater o Backpurge o Request Calibration o Operating Range o Recorder Readout o Operate o Sample Flow Rate 2.2.4 Calibration Gas System o If system uses compressed gases to routinely calibrate system, note following gas cylinder information: Gas Cyli nder 1 Pollutant Concentration Certification Date Cylinder Number Cylinder Pressure (psi) primary (>150psi) secondary (> 15psi) 21 ------- Gas Cyli nder 2 Pollutant Concentration Certification Date Cylinder Number Cylinder Pressure (psi) primary (>150psi) secondary (> 15psi) Gas Cylinder 3 Pollutant Concentration Certification Date Cylinder Number Cylinder Pressure (psi) primary (>150psi) secondary (> 15psi) Gas Cylinder 4 Pollutant Concentration Certification Date Cylinder Number Cylinder Pressure (psi) primary (>150psi) secondary (> 15psi) 22 ------- Check or Comment 2.2.5 Sample Transport System o Type of tubing o Internal diameter of tubing inches o Enter the distance from sample point to analyzer feet o Is transport line heat traced? Yes No o If yes, how is temperature monitored? o Enter the temperature of the transport line: 2.2.6 Sample Conditioning/Extractive Systems For extractive systems the following checklists describe the sampling point, transport system, and sample conditioning system. 2.2.6.1 Sampling Point - o Location: Stack Duct Horizontal Duct Vertical o Is it downstream of pollution control device? Yes No o Type pollution control device(s) o Estimate distance from nearest flow disturbance and record below. Downstream: feet Upstream: feet o Sketch the cross-section of the duct/stack at the sampling point and show the location of the sampling probe of CEM. Indicate dimensions. 23 ------- Sketch of Duct/Stack and Sampling Probe Location Check or Comment o On the following blank page sketch the components of the Extractive CEM, including the probe, filter, calibration gas interface, pump, moisture removal system, SO? scrubber system (where applicable), and analyzer. 2.2.6.2 Sample Probe - o Type Material: o Singular or multi-point sampling? o If multi-point sampling, enter number of sampling points o Distance of each point from the wall: Point No. 1 2 3 4 5 6 Inches from wal1 o If single point, enter distance from wall: inches 24 ------- Sketch of the Components of the Extractive CEM, Including the Probe, Filter, Calibration Gas Interface, Pump, Moisture Removal System, S02 Scrubber System (where applicable), Analyzer, and Calibration System. 25 ------- Check or Comment 2.2.6.3 Filter - o Type: Internal External o Condition: o Is there a back purge on the sampling system to clean the probe? Yes No o If yes, how often is it activated? o Is the purge air dried prior to use? Yes No_ o Frequency of Replacement: o Typical pressure drop across filter (if monitored): o Current pressure drop across filter (if monitored): 2.2.6.4 Moisture Removal (if applicable): - o Type of moisture removal equipment? Refrigerated or tube type condenser Permeation dryer o Location: o Sample Gas Temperature at Outlet During Audit: 2.2.6.5 Sample Pump - o Type: o Location: o Flow Rate: 2.2.6.6 Heater/Oven (if applicable) - o Location: o Temperature of Gas at Outlet During Audit (if monitored) 26 ------- Check or Comment 2.2.6.7 $02 Scrubber System o Location: o Type: o Frequency of change 2.3 CLOSING CONFERENCE The closing conference enables the inspector to "close-out" the inspection with plant personnel. At this time, questions can also be answered relating to results of the inspection. In general, the following elements should be covered in the closing conference: o Review of Inspection Data o Inspection Discussion o Confidential Information o Deficiencies in monitoring program o Recommendations 27 ------- 3.0 LEVEL III CHECKLIST 3.1 INTRODUCTION The Level III inspection, for the State inspector, is the most costly and labor intensive. Level III inspection becomes necessary only when the Level II inspection indicates deficiencies in the CEM system. The Level III inspection involves a complete evaluation of the monitoring system through a dynamic calibration procedure. Multiple concentration gases are injected, as close to the probe tip as possible, and the monitor response is compared to the certified gas values. From this evaluation, a calibration error is determined. If the error falls outside calibration drift performance specification values, then the monitoring system is "out-of-control." This would necesitate some form of corrective action. 3.2 CYLINDER GAS AUDIT 3.2.1 Attach the proper gas line from the certified gas cylinder to as close to the probe tip as possible. Properly adjust the flow rate to manufacturers' specifications. Check or Comment 3.2.2 List Certified Gases Gas Mixtures: Gas A ppm/% Pollutant TRS 02 Other Cylinder No. Certification Date Pressure (psi) Initial Final Gas B ppm/% Cylinder No. Certification Date Pressure (psi) Initial Fi nal 29 ------- Gas C Cylinder No. __ppm/% Certification Date Pressure (psi) Initial Final Check or Comment 3.2.3 Inject each gas into the monitoring system, as close to the probe tip as practical. Record monitor response on Level III Field Data Sheet. 3.2.4. Calculate % Difference for each calibration gas by the following equation: % Difference = (Avg. Monitor Response) - (Audit value^ (Audit Value! x 100 30 ------- LEVEL III FIELD DATA SHEET PERCENT DIFFERENCE DETERMINATION Person Conducting Audit Analyzer Manufacturer Affiliation Model/Serial No. Date Location Audit Gas Concentration Pollutant Certification Date Expiration Date Low-Range Mid-Range High-Range Run Number 1-Low 2-Mid 3-High 4-Low 5-Mid 6-High 7-Low 8-Mid 9- High 10-Low 11 -Mid 12-High 13-Low 14-Mid 15-High Audit Gas Concentration Instrument Response Arithmetic Mean Arithmetic Difference Low ' - - - - - - - - - - Mid - - - - - - - - - - High - - - - - - - - - - - ------- 3.3 MONITOR-SPECIFIC INSPECTION PROCEDURES If calibration gases are not available, the inspector can evaluate the installed TRS CEM system through monitor-specific inspection procedures. This involves observing various operating parameters as indicated by valves, meters, pressure gauges or switches. Observed values are then referenced to the "baseline" values established during monitor certification. To assist the inspector, monitor-specific inspection procedures have been developed for three commercially available TRS monitoring systems. They are: o Sampling Technology Inc. TRS CEM Model 100; o Barton Titration TRS CEM System; and o Rendix Gas Chromatograph TRS CEM System. To insure that all information is obtained in an orderly fashion, the procedures are presented in the order they are normally encountered in the field, i.e., analyzer/computer system; calibration system, transfer system and probe/conditioning system. 33 ------- 3.3.1 SAMPLING TECHNOLOGY INC. TRS CEM SYSTEM INSPECTION PROCEDURES 3.3.1.1 Analyzer Evaluation Pulse Flourescence Analyzer o Observe reading of S02 as displayed in window (reading is % of monitor range). ire to CRT display and computer printout. ti diagram for inspection points) Check Comment © STI (Q) o Observe that "on" light is illuminated. o Check positions of zero/span pots (potentiometer) and compare to maintenance logs. 0? Analyzer o Observe meter display and compare to CRT and computer printout. o Note position of "Range" switch. Range o Note "sample flow" as indicated by rotameter. (Should be between 400-500 cc/min). cc/min 35 ------- Check Comment Computer o Observe that power light (yellow) on key board is flashing. o Observe that power light (red) on screen display is on. o Observe that printer "power on light" is illuminated. o Observe that screen "format" is updated every 4-!S seconds. o Observe last computer readouts of TRS and 02 and compare to instantaneous values as displayed on nonitor meters. TRS 02 meter meter o Observe previous 12 hour report (see sample). «»»«f«S«*»*»*S*t**«**»*****t*********************** TRS 12 HOUR REPORT - 12:CO:48 JULY 11 1984 12 HOUR CTRS/O2 CORRECTED3 AVERAGE VALUE (PPM) RCVY BLR TRS TBS O2 CO:CO TO O1:OO .3 5.2 01:00 TO O2:OO .3 5.0 02:OQ TO O3:00 .3 5.O 03:OO TO O4:OO .3 4.8 04:00 TO O5:OO .3 4.7 O5:00 TO 06:00 .2 5.2 O6:OO TO 07:00 .2 5.2 O7:OO TO 08:OO .3 5.7 O8:OO TO O9:OO O.O 0.O O9:OO TO 10:OO 0.0 0.0 1O:OO TO 11:OO 2.3 6.9 11:00 TO 1?:00 .1 14.8 UNCORRECTED TRS AVERAGE ,5 O2 CORRECTED TRS AVERAGE .4 02 AVERAGE 6.2 36 ------- where: = tne average concentration corrected for oxygen; Cmeas = the average concentration unconnected for oxygen for previous 12-hours; X = the volumetric oxygen concentration in percentage to be corrected to (8 percent for recovery furnaces and 10 percent for lime kilns, incinerators, or other devices); and Y = the measured 12-hour average volumetric oxygen concentration. Check Comment Review previous 24-hour printouts observing stack gas concentration variation and consistency. Review previous 24 hour calibration drift report and compare to plant standard. (See printout below). o Initiate an internal "zero/span" check or monitor system. Compare to gas cylinder \/^il \tr\e* valves. TRS 02. Gas cylinder Gas cylinder valves valves Monitor response Monitor response % Off Off o Request "Limits Factors" and compare to plant limits. o 02 STD o TRS o 02 cal gas valve 37 ------- Check Comment Dilution Air Conditioning System o Open cabinet door. o Insure pump is running with 30 Ibs pressure. o Air pressure regulator should indicate 60 Ibs pressure. o Listen to insure regenerative dryer working properly. Calibration Gas Cylinder o Check certification of gas cylinders valves and compare to maintenance logs and computer printout. o Check cylinder numbers and compare to certification sheets. o Observe primary/secondary pressure gauge and note setting. (Normal settings should be 300 psi primary and 40 psi secondary). Gas Cylinder #1 Concentration Certificate date Gauge settings P r i ma ry Secondary Gas Cylinder #2 Concentration Certificate date Gauge settings P r i ma ry Secondary Recorder o Observe emissions over previous day. o Inspect previous zero/span readings and compare to gas cylinder valves. 38 ------- Check Comment 3.3.1.2 SO? Scrubber System (located behind monitor racks) o Check moisture level in reservoir. o Observe that scrubber is regenerating in a timely fashion ( 15 minutes). o Review maintenance logs for possible drift problems associated with scrubber system. Positive Drift - Release of S02 from packi ng. Negative Drift - Retention of SO^ during daily zero/span check. o Review maintenance logs for periodic changing scrubber sieves ( 30 day intervals). Thermal Oxidizer o Check temperature display on front of panel. Should be between 1500-1600°F. (825-875°C). o Observe that power light is on. o Review maintenance logs for periodic adjustments of thermal oxidizer temperature. Analyzer Rack o Check for power on. o Check all pressure regulators and relate setting to initial monitor certification setting in maintenance logs. o Check sample by-pass rotameter (should be 1-2 1pm. However, this number depends upon length of sample line. Initial valve should be recorded in log book during certi- fication testing). Switch Central Panel o Check to see all switches are in "auto" position. o Observe if any red lights are lit indicating operating mode. 39 ------- Check Comment 3.3.1.3 Probe/Conditioning System The inspection of the probe/conditioning system involves both a review of the maintenance logs and a physical inspection of the unit itself. (Refer to the following diagram for inspection points). AIR SUPPLY « n-A .AIR PRESSURE SWITCH Jr-7-_ PRESSURE TV KE6ULATOR -c^6 IDUCTOR SUPPLY CALIBRATION VENT &Ai TJJLET 40 ------- Check Commemt o Observe overall condition of system. Vibration Problems Temperature Problems Other Open cabinet and observe internal housekeeping. Loose wires Condenser di rty Other o Cal gas introduced at probe. o Observe "back-purge" if applicable. Check drain for air/water. o Observe automatic calibration cycle. (during automatic calibration cycle, the cal gas is under positive pressure to probe) If a leak in the system occurs, then the 02 valve will never reach zero. o Check "Fault Indicators" on probe controller box. Note. (Refer to following diagram for fault indicator location). Indication On/Off Power Enclosure Temperature Vaporizer Temperature Probe Restriction Air Pressure 41 ------- 8 O ® PROBE CONTROLLER O O O O O ,, Of - POWER ENCLOSURE TEMPERMURE TEMPERATURE RESTRVCTIDN AlR PRESSURE e Check Comment o Check water level in liquid resevoir, (should not be greater than one-fourth of bowl). o Check steam panel regulator (should be between 20-30 psi). o Check maintenance records for periodic maintenance on system. o Inertial filter changes_ Lime Kiln (2-4 weeks) Recovery Boiler (monthly) o Eductor removed/cleaned periodical ly 42 ------- 3.3.2 ITT BARTON TITRATION TRS CEM SYSTEM INSPECTION PROCEDURES 3.3.2.1 Sampling Module (Refer to following figure for inspection points). HEAT TRACED SAMPLE LINE SAMPLING MODULE VENT SAMPLE 250 CC/tfMN AMBIENT AIR 43 ------- Check Comment o Observe pressure of condensate resevoir regulator. 15 psi o Observe LED is lit on panel of heat trace line controller. o Observe "reading" of heat-trace line controller as displayed by meter. (Temperature indication should be 10-20°F higher than the dew point of the sample gas). Titration Module (Refer to following figure for inspection points). SAMPLE 250 CC/MIN TITRATION MODULE •CAL. 3AS VENT 44 ------- Check Comment o Insure the S02 scrubber solution is at the 5UO ml mark. o Insure the titration cell reservoir is between stamped lines on cell. o Observe following setting of regulators. o Vortex tube supply 80-120 psi o Aspirator Pressure 35-50 psf o Purge pressure regulator _ "5-TO" psi o Check high volume pump operation by observing flow at pump vent point. o Verify heater operation by observing orange glow of the element through the observation poi nt. o Observe flowmeter setting and compare to calibration sheet to insure sample flow of 250 cc/mm. Control Module (Refer to following figure for inspection points). 45 ------- Check Comment o Observe range switches. is on. Note range monitor Range o Note settings from zero/span/blank. Compare to historical data. Zero Span Blank ADJ present present present Observe mode switches, is illuminated. previous previous previous Note which mode switch Mode The mode switches (TRS, BLK, CELL CAL and AUTO ) determine the characteristics of the sample reaching the detector cell. The mode switch functions are listed in the following Table. SWITCH SAMPLE CHARACTERISTIC PWR OFF TRS BLK CAL CELL CAL AUTO Instrument power ON/OFF. Sample gas passes through S02 scrubber, remainder oxidized to S0£. Ambient air passes through the charcoal filter. Calibration gas injected at probe. Calibration gas injected just before cell. Automatically cycles instrument through modes. o Press RAW DATA switch and REC CHK switch simultaneously. The recorder should go to min-scale. (Failure to do so indicates the existence of a program in either the recorder or the control power supply). RAW DATA Function o Measure the raw data value in the BLANK mode. RAW DATA o Is it within value range? No Yes 46 ------- Check Comment o Measure the raw data values in either the TRS or CAL mode. TRS/CAL value o Subtract the lowest from the highest value. o Observe range switch setting. o From the following Table, obtain SO? conversion factor. Conversion Factor Data RANGE SWITCH 1 2 3 4 5 6 7 S02 CONVERSION FACTOR 0.035 .82 .26 .75 2.5 7.1 23. UNITY GAIN FULL SCALE 3.5 8.2 26. 75. 250. 710. 2300. FULLSCALE RANGE 1.0-5.0 5-15 15-50 50-150 150-500 500-1000 1000-3000 RAW DATA BLANK READING 20 + 8 12 + 4 6 + 3 3 + 1.5 2 + .5 1.5 + .8 0.7 + .4 o Calculate concentration by multiplying difference between sample and blank values by the SO? conversion factor. ppm = (Sample Raw Data - Blank Raw Data) X Conversion Factor = ( - ) X ( ) Value determined should be within _+ 15%. o Press CELL CAL mode switch. o Note monitor response and compare to gas cyli nder value. Monitor Response Gas Cylinder Value o Calculate % calibration error by the following equation. (Monitor Response) - (Gas Cylinder Response) (Gas Cylinder Response) o Calculated value should be _+ 15%. 47 X100 ------- 3.3.2.2 Probe/Conditioning System The inspection of the probe/conditioning system involves both a review of the maintenance logs and a physical inspection of the unit itself. (Refer to following diagram for inspection points). PROBE HtCOVCtr STACK "I SOLID STATE RELAY CAL OAS NC 1 J T HEAT TRACED SAMPLE LINE THERMOSTAT I THERMO! -]-- PROBE MODULE CONDENSATE TRAP Check Comment o Observe overall condition of system. Vibrational Problems Temperature Problems Other o Open cabinet and observe internal housekeeping. 48 ------- Check Comment Loose wires Condenser trap dirty Other o Observe condensate reservoir, if possible Observe emptying of condensate trap during "blank" mode of operation. o During calibration mode, insure that calibration gas injection solenoid valve opens. o Is condensate trap frozen? o Observe that system back purges periodical ly. o Note whether sample line is heat traced. 49 ------- 3.3.3 BENDIX TRS CEM SYSTEM INSPECTION PROCEDURES 3.3.3.1 Analyzer/Calibration Assemblies The inspection of the above assemblies involves observing gauges/ flowmeters and comparing their indicated values to their "baseline" values. The observed values may change from week to week; but, reference should be made back to the "baseline" value. The following figure illus- trates the assemblies we will be inspecting. fYlrS fHO ^nJ JUO • a* AWK ?n<$ JUO BUST :*tto« ^ JJO M»M^ in. rS CAHKrta ***» ! * 1 ^ •*^ ; L t f : , . t *i *— r: itf i t i. f\ .1 •r '^'t^MtUMIMII |L_ i- £U»I«.MMM** , 1 1 ! - •"— • •UTWMM ktMWMf 1 ' * '— - . L. •MMM |MMM«I i 1 — * | A j . « » JL NK § j & __ , R U —i ^f ' i — i . .I : TYi _/' fi __--l I ^1 0 i --^ !]• ^ A "T C a _-,_£ •^ypt n, • J 4 ju I" 1 11' 3. •t \-' UlS-J trf« Ouu 1 • *w M. •*rf <+-l 1 **• h *«MM i . i- • -. , -T 1 .L .[ -L ' n :ri 1 1 i l-:l - 1. * t -*.*- 51 ------- Check Comment Calibration Gas Cylinder o Check certification of gas cylinders values and compare to maintenance logs and computer printout. o Check cylinder numbers and compare to certification sheets. o Observe primary/secondary pressure gauge and note setting. (Normal settings should be ^ 300 psi primary and ^ 40 psi secondary). o Note following information on each gas cyli nder. Gas Cylinder #1 Pollutant Concentration Certificate date_ Gauge settings Primary Secondary_ Gas Cylinder #2 Pollutant Concentration Certificate date_ Gauge settings P ri ma ry Secondary_ Gas Cylinder #3 Pollutant Concentration Certificate date_ Gauge settings Primary Secondary_ Gas Cylinder #4 Pollutant Concentration Certificate date_ Gauge settings Primary Secondary_ 52 ------- Gas Cylinder #5 Pol 1utant Concentration Certificate date_ Gauge settings Primary Secondary Support Assembly Observe the following gauges/me^e-"-. as part of the Support Assembly. All observations should be reference, -.0 "baseline" values. (Refer to diagram for "p^pection points). Support A««mo»v SotaMMd Onur &rd Flow Switch SwwpAir Ftow Control Alterably Ptont Air Souroi Flow Contra! AMrnbn/ Baseli ne Value Sweep Air Flowmeter (A) Sweep Air Pressure Gauge (B) Plant Air Pressure Gauge (C) Observed Value 53 ------- Calibration Assembly Observe the following gauges/meters as part of the Calibration Assembly. All observations should be referenced to "baseline" values. (Refer to diagram for inspection points). Zero Air Pressure Gauge Nitrogen Pressure Gauge Calibration Gas Pressure Gauge Oxygen Pressure Gauge Dilution Pressure Gauge Other Baseline Observed Value Value 54 ------- Sample Transport Assembly Observe the following gauges/meters as part of the Sample Transport Assembly. All observations should be referenced to "baseline" values. (Refer to diagram for inspection points). g—w M—H w—M—M—M M—Ti H H M M" So OB QOOOOO O Q oO S, (Dual Gas Stream System Illustrated) Baseline Value Oxygen Sample Flowmeter (D) Gas Chromatograph Sample flowmeter (E) Observed Value 55 ------- Analyzer Controls and Indicators Observe the following gauges/meters as part of the Analyzer Controls and Indicator Assembly. All observations should be referenced to "base- line" values. Baseline Value Observed Value Detector Purge Gauge Plant Air Supply Gauge Heater Air Pressure Gauge S/P Valve Switch On Hydrogen Supply Gauge Column #1 Pressure Gauge Column #2 Pressure Gauge Analyzer Oven Temperature Gauge Calibration Pump Gauge Other Other Gas Chromatograph System Type: Detection Technique: Column 1. 2. 3. Column Temperature ( _+ 1°C) 1 ._ 2. Sample Column Size: Detection Temperature:_ Attenuation: Data Processor/Recorder o Observe emissions over previous day. o Consistent values? Check Comment o Exceedances?_ o Problems? o Inspect previous zero/span calibration readings and compare to gas cylinder values, 56 ------- Check Comment o Initiate an internal "zero/span" check of the monitor system. Compare to gas cylinder values. Cylinder Values Monitor Response % Calibration Error H2S CH3SH (CH3)2S (CH3)2S2_ (Are the calculated calibration errors < 20%?) (A typi;al chromatograph of a zero/span check is illustrated below) 57 ------- During the calibration, observe software report as recorded by the Data Printer. A "typical" printout follows: TftS TRS H2S CH3SH PMS DMDS 02 OPACIT) COP flEAS ,-pc.j-j) c='PM> -PPM) (PPh> (PPh'J (PPrt) <•/£> (A) :i< *i iNt'F;- (•(-•i.A'-n ?:• TOO. 190. 100, 33.00 3? 4 00 54,00 J 0 » 3 J :"< . 6 v VL.r.' < f^.^WT 2> 1^9. IS*. 10C-. 3?. 00 - 33,00 34,00 10.1 PI,.' (•I CALTF:fATln,-i KtT'O^'T 0 M T E I / 2 I / " 9 o -.">; 0 * ; O ^ [i'JJT 0001 S'ACK t1 i - M P i i\ r ui.it rv F <•} e: u F-: F •. R F ) % y A K r c % J:i RI F T H2S ISC 1.65 t-^4 .v^^ 27 ,sx CH3.SH 220 3,87 X,S5 ,f.:^ 27 I'MS 1-'90 5..->8 S.63 OX 27 OrtDS -410 '.12 7.13 .Oiv ->7 o Observe if any hardware/software alarms have been observed over the previous 24 hours. Typical hardware alarms include the following: o Low Zero Gas o Low TRS Span Gas o Low 02 Span Gas o Low Plant Air o Low Sweep Air o Probe Restriction Chromatograph related hardware alarms are: o Low Carrier Gas o Low hydrogen o Oven Hi o Oven Lo o Low Purge Air o Flameout Optional system alarms are: o Low Sample Flow o Low Sample Pump Vacuum 58 ------- Check Comment 3.3.3.2 Probe/Conditioning Assembly o Observe overall condition of system. Vibration Problems Temperature Problems Other o Open cabinet and observe internaj housekeeping. Loose wi res Condenser dirty_ Other o Cal gas introduced at probe? o Observe "back-purge" if applicable. Check drain for air/water. o Observe automatic calibration cycle, (during automatic calibration cycle, the cal gas is under positive pressure to probe. If a leak exists, then the 02 valve will never reach zero during cal gas introduction. o Listen for air flow to heat exchanger. o Observe reading of Dew Point meter, if applicable. o Go to opposite side of port and observe probe. 59 ------- 4.0 LEVEL IV CHECKLIST 4.1 Introduction A Level IV evaluation involves a recertification of the installed GEM system utilizing Performance Specification Test 5 and 3. The role of the inspector during this level is to observe that proper sampling and computation of emissions from the source during testing occurs. At this time, additional "baselining" of the control equipment and continuous emission monitoring system can be performed. To assist the inspector, observation checklists have been developed for both Federal Reference Method 16 and 16A. The inspector should use these checklists when performiong a Level IV evaluation. 61 ------- Federal Reference Method 16 Observation Checklist 63 ------- Page of_ In i t i aT Federal Reference Method 16 Observation Checklist 1.0 BACKGROUND INFORMATION 1.1 Source Name: 1.2 Location: 1.3 Affected Facility:_ 1.4 Test Dates: 1.5 Test Team: Leader: Members: 1.6 Plant Contact: 1.7 Corporate Contact: Phone # Title 2.0 PROCESS DATA 2.1 Process Tested: 2.2 Process Description: 2.3 Process Operating Data: 3.0 TEST EQUIPMENT 3.1 Sketch system used for sampling and analysis (including calibration system). 65 ------- Page of_ Initial 3.2 - TEST EQUIPMENT DESCRIPTION 3.2.1 Probe/S02 Scrubber System 3.2.1 Probe Length: ID: Material of Construction: Filter Device: Out-of-stack_ In-Stack Material Heated? 3.2.1.2 SC>2 Scrubber Impinger Technique: Solution: pH of Solution: 3.2.2 Sample Lines/Pump 3.2.2.1 Lines: I.D.: O.D.:_ Material of Construction: Heated? 3.2.2.2 Pump Type: Material of Construction: Heated: 3.2.3 - Dilution System Technique:_ Dilution Ratio: 1. 2. 3. Dilution Gas: Heated? 66 ------- Page of Initial 3.2.4 - Gas Chromatograph System Type: ___Detection Technique: Column 1. 2. Column Temperature (_+ 1°C) 1. Sample Column Size: Detection Temperature: Attenuation: Gas Flow: H2 Flow: Air Flow: N£ Flow Accuracy Range: Detect 0.5 ppm for H2S, MeSH, DMS and DMDS?_ 3.2.5 - Calibration System 3.2.5.1 - Permeation Technique Pollutant Certification Permeation Certification Traceability Number Rate Temperature Technique H?S MeSH DMS DMDS Analysis Date Vendor H2S = Hydrogen Sulfide; MeSH = Methyl Mercaptan; DMS = Dimethyl Sulfide; DMDS = Dimethyl Disulfide 67 ------- Page of_ Initial Remarks: Constant Temperature Bath (_+ 1°C) of Permeation Tube Certification Sheet Flowmeter Calibrated?_ Date Calibration Curve Flow of Calibration System greater than demand of Analytical System? Bubble Meter used to monitor flow? Temperature indicator calibrated? Carrier gas prepurified? ^ Di scuss Diluent Gas - 50ppb S compounds? lOppm each of H20 and HC: Heated prior to mixing? 3.2.5.2 - Cylinder Gases Pollutant Concentration Traceability Analysis Expiration ( in Air) to NBS Per- Date Date meation tube Remarks 68 ------- Page of_ Initial Greater than 200 psi in gas cylinders? Vent valve utilized? 3.2.6 - Integrator or Recorder Type: Averagi ng Tine: Attenuation: Last calibration: 4.0 - SAMPLE PORT LOCATION Stack/Duct Conditions (leaks, particle build-up, corrosion): Number of stack diameters upstream from flow disturbance: Number of stack diameters downstream from flow disturbance: Velocity Traverses Performed: __ Number of points Locati on Avg. Ap Pitot tube calibration factor Date Calibrated Avg. Velocity Stack Temperature Sensor: Type: Range:_ Location in Stack: Date Calibrated: Calibration Papers Rec'd_ Remarks: 69 ------- Page of_ Initial Location of CEM in reference to Sample Port Location: 5.0 PRE-TEST ACTIVITIES System set-up properly? System leak check (optional) 2 inches Hg Vacuum for 1 minute Pass Failed All components operating properly Di scussion: Pre-Test Recovery Determined (optional) Discussion: 5.1 Interference Determination Chromatograph submitted of calibration gases with/without 10% C02? Agreement within 5% Chromatograph submitted showing separation of S0.2 from other peaks? . or S02 Scrubber System used to remove S0£ prior to GC analysis 70 ------- Page of Initial Chromatograph submitted showing resolution of Sulfur Dioxide ($02), Hydrogen Sulfide (H2S), Methyl Mercaptan (MeSH), Dimethyl Sulfide (DMS) and Dimethyl Disulfide (DMDS): Discussion: 5.2 Calibration of GC/FPD and Dilution System 5.2.1 GC/FPD Calibration through S02 Scrubber Dilution System prior to calibration? Permeation tubes in bath 24 hours? Calibration Curve developed from three injections of three known concentrations of H£S, MeSH, DMS, and DMDS? Calibration Curve developed in range data is being collected? Precisions of injections for each known TRS within + 5% of mean value? Temperature of bath +^ 0.1 °C of certification tube temperature Calibration Curve Generated? 5.2.2 Dilution System Injection of H2S in front of Dilution System?_ Three injections? Precision of three injections _+ 5% of mean value?_ Dilution factor calibrated for each stage? Stage 1 Factor Stage 2 Factor 6.0 STACK TEST Port closed around probe? 71 ------- Page of Initial Sample traversed at three points in source (16.7, 50.0 and 83.3%) of stack diameter? Sampling System conditioned 15 minutes prior to test? Sample run consists of a min. of 16 individual injections performed over a period of not less than 3 hours or more than 6 hours? Discussion: Orsat collected during sample run? Orsat collection technique and location GAS CHROMATOGRAPH INFORMATION Run 1 Run 2 Run 3 Date Time Began Time End No. of Injections or Analysis (min 16) Ave H2S cone, ppm Ave MeSH Cone, ppm Ave DMS cone, ppm Ave DMDS Cone, ppm Ave TRS Cone, ppm as S02 Concentration of trace gas Ave 02 Cone, % 72 ------- Page of_ Initial 7.0 - POST TEST PROCEDURES 7.1 - Sample Line Loss - Correction Factor Known concentration of H2S injected as close to probe tip as possible? Concentration of H2$ generated at level of standard (+_ 20%)?_ Generated By: Permeation System Cylinder Gas Dilution_ Recovery 20% (Sample run not to be used) 20% (Sample run corrected) Recovery Correction Factor 7.2 - Recalibration of GC/FPD and Dilution System 7.2.1 - GC/FPD Known concentration of H2S injected into GC/FPD? Compared to original calibration curve?_ Calibration Drift + 10%? Highest sample values chosen if calibration drift 10% Discussion: 73 ------- Page of_ Initial 7.2.2 - Dilution System Known concentration of H2S injected into front of Dilution System? Compared to original calibration curve? Calibration Drift + 10%? 7.3 - LEAK CHECK Sampling system leak checked?_ Technique? 8.0 - CALCULATIONS Individual concentrations of H2S, DMS, DMDS and MESH Recorded? (Oxygen Corrected) Run 1 Run 2 Run 3 (avg. ppm) (avg. ppm) (avg. ppm) H2S MeSH DMS DMDS Total 74 ------- Page of Initial 9.0 - RELATIVE ACCURACY 9.1 Calculation TRS (ppm) Run 1 Run 2 Run 3 Reference Method TRS Cone. (%02 corrected) ZHZ ~HL HZZ CEM TRS Cone. ' ~ (%C>2 Corrected) Difference Avg. Differences ~~~ 9.2 % Relative Accuracy = 1x1 + C.I.i "'" xlOO [RMavg] ( 20%) 10.0 - SUMMARY Are final results expressed in units which satisfy permit or Agency requirements? Does tester have documentation to support emission calculations (only required on smelt dissolving tank vents)? 75 ------- Page of Initial Brief Summary of Test: 11.0 - AUTHORIZATION 11.1 - Regulatory Observer Observer Signature Title Organization_ Address Telephone # ( )_ 11.2 - Company Observer Company Observer Signature_ Title Telephone # 76 ------- Company Address TOTAL REDUCED SULFUR FIELD CALIBRATION DATA SHEET FEDERAL REFERENCE METHOD 16 Date Analyst Sampling Location Company Contact I. Permeation Tube Information PoTTutant I_nfo rma t |p_n J H^S J C H ^ S H Tube I. D. #: Permeation Rate (PR) I • Cal i brat j_gn_Cu_rye Po i n t Jfj_ j Area Time FlowTQl 1 Known Concentration (ppm) 2 H2S: CH3SH: 3 (CH3)2S2j Avg. Poi_nt_£2_ Time Flow fOT 1 Known Concentration (ppm) 2 H2S: CH3SH: 3 (CH3)2S2: Avg. Area 77 ------- Point #3 Time Known Concentration (ppm) H2S: CH3SH: (CH3)2S: J 1 2 3 Avg. Pollutant Area H?S III. o n c — /24.46/if/M-mo/eW T°K \/760 mm Hg (PR)\(M) fJLg/fjL-mole/\^W°K/\P mm Hg f/min Where: c = concentration, p?/ ( or ppm by volume T = temperature of the system, °K P = pressure of the system, mm Hg PR = permeation rate, fjLg/min Q— total flow rate, liters /min M- molecular weight of the permeating gas, 24 .46 = molar volume (V) of any gas at 25 °C & 760 mm Hg, -moli IV. Remarks: c = 78 ------- Page of Initial V. Graph Calibration Curve Using the graph paper below, graph either the peak area, peak height or available integrator information for each of the individual sulfur standards vs. concentration. Draw the best fit line through the plotted points and determine source sample concentration from the established calibration curve. 5 * 7 I » t 79 ------- Federal Reference Method IfiA Observation Checklist 83 ------- Page of Initial Federal Reference Method 16 Observation Checklist 1.0 BACKGROUND INFORMATION 1.1 Source Name: 1.2 Location: 1.3 Affected Facility: 1.4 Test Dates: 1.5 Test Team: Leader: Members: 1.6 Plant Contact: 1.7 Corporate Contact: Phone # Title 2.0 PROCESS DATA 2.1 Process Tested: 2.2 Process Description: 2.3 Process Operating Data: 3.0 TEST EQUIPMENT 3.1 Sketch system used for sampling and analysis (including calibration system). 85 ------- Page Of Initial 4.0 SAMPLE PORT LOCATION 4.1 Stack/Duct Conditions (leaks, particle build-up, corrosion): 4.2 Number of stack diameters upstream from flow disturbance: 4.3 Number of stack diameters downstream from flow disturbance: 4.4 Velocity Traverses Performed: Number of points Locati on Avg. Ap Pitot tube calibration factor Date Calibrated „_____ Avg. Velocity __ 4.5 Stack Temperature Sensor: Type: __ Range:_ Location in Stack: Date Calibrated: Calibration Papers Rec'd_ 4.6 Remarks: 4.7 Location of CEM in reference to sample port location 5.0 SAMPLE TRAIN PREPARATION 5.1 - Probe Material of Construction Heated? Temperature_ 5.2 - S02 Scrubber System Type Citrate Acid Buffer Added? 86 ------- Page of "TnTtiaT" pH of Solution Location of Probe? 5.3 - Oxidizing Furnace Type Material of Construction Tube Dimensions Temperature _ 5.4 - S02 Impinger Train Type Hydrogen Peroxide added to Impingers ? Qua n t i ty Glass Wool plug used? 5.5 - Dry Gas Meter Type Volume Correction Factor Date Calibrated Calibration Papers Revised? Temperature Measured? 6.0 PRE-TEST ACTIVITIES 6.1 - Pre-test leak check (optional) 6.1.1 Complete sampling train checked: 6.1.2 Vacuum of 10 inches mercury? 87 ------- Page of Initial 6.1.3 Leak rate 40 cc/min? 6.1.4 Pump leak checked? 6.2 - System Performance Check 6.2.1 Sketch sampling train and gas dilution system. 6.2.2 List gases available, concentration, traceability, analysis date, expiration date and gas cylinder pres- sure (include information in both calibration gas and dilvent gas). 88 ------- Page _0f rhTtTal Pollutant Concentration Traceabllity Analysis Expiration Cylinder Date Date Pressure 6.2.2.1 Dilvent gases contain 50 ppb total sulphur compound and IQppm 6.2.2.2 Total HC? 6.2.2.3 Calibration gases verified by Reference Method 11, GC/FPD or zinc acetate technique 6.2.2.4 Rotometers used in dilution system calibrated? __ 6.2.2.5 Dry gas meter used in Dilution System calibrated? 6.2.2.6 Flows measures by bubble meter?_ 6.2.2.7 Concentrations generated?_ 6.2.3 System Performance Check Form 6.2.3.1 Two thirty minute samples taken?_ Date Run I.D. Time Began Time Ended Dry Gas Meter Volume 89 ------- Page Of_ Initial Volume of Solution (mm 1) Volume of Solution Titrated (mm 1) Volume of Titrant (mm 1) Normality of Titrant Cone. H£$ Determined Cone. H2$ Generated % Recovery 6.2.3.2 Within +_ 15% of generated H2S_ 6.2.3.3 Two 30-minute samples within + 5% of their mean value? 6.2.3.4 Notes/Remarks: 90 ------- Page Of_ Initial 7.0 SAMPLING 7.1 - General 7.1.1 Leak check performed after system performance check? 7.1.2 Sample extraction involving either: (1) three one hour samples at 20 liters/min? (2) One three hour sample of 120 liters intermittently or continuous 7.1.3 Sampling involves traversing stack? 7.1.4 Oxidizing furnace maintained at 850°C?_ 7.1.5 Citrate buffer solution adequate?_ [Note: The citrate buffer solution volume may change during sampling due to condensed water from sample stream and gas flow rate.] 7.2 - Field Data Required? Date Run I.D. Time Began Time Ended Avg. Rotameter reading Avg. Dry Gas Temperature Dry Gas Meter volume (ft.) 7.2.1 Sampling rate performed 2.0 liters/minutes (_+ 10%)? 7.2.2 Post-Test leak check performed?_ 91 ------- Page Of_ Initial 7.2.3 Impingers containing hydrogen peroxide recovered? - sample recovery bottle labeled? - fluid level indicated on side of bottle? 7.2.4 Probe/Sample line to SC>2 scrubbers rinsed after each run? 1.0 - SAMPLE RECOVERY TEST 8.1 - General 8.1.1 Was a leak test performed prior to the sample recovery test? 8.1.2 Were SC>2 impingers re-charged with hydrogen peroxide? List gases available, concentration, traceability, analysis date, expiration date, date and gas cylinder pressure (include information in both calibration gas and diluent gas): Analysis Expiration Cylinder Pollutant Concentration Traceability Date Date Pressure 8.1.3 Diluent gases contain < 50 ppb total sulfur compound? 8.1.4 Calibration gases verified by Reference Method 11, GC/FPD or Zinc Acetate technique? 8.1.5 Rotameters in dilution system calibrated? 8.1.6 Dry gas meter in dilution system calibrated? 8.1.7 Flows measured by bubble meter? 92 ------- Page of_ Initial 8.2 Sample Recovery Test Field Data Date Run I.D. Time Began Time Ended Dry Gas Meter Volume(ft3) 9.0 - ANALYSIS 9.1 Source Sample Run Number Dry Gas Meter Volume (ft3) " Volume of Solution (ml) Volume of Solution Titrated (ml)" Volume of Sample Titrant (ml) Normality of Titrant Volume of Blank Titrant 9.2 Sample Train Recovery Run Number Dry Gas Meter Volume (ft3) Volume of Solution (ml) Volume of Solution Titrated (ml) Volume of Sample Titrant (ml) Normality of Blank Titrant Volume of Blank Titrant 93 ------- Page Of TnTtTaT" 10.0 CALCULATIONS 10.1 Calculate the volume of gas sampled corrected to standard conditions, for each sample run utilizing the following equation (for Sample and Sample Train Recovery): Where: Vm(Jtrf) = volume of gas sample through the dry gas meter at standard conditions, dscf Vm = volume of gas sampled through the dry gas meter, (cu.ft.) Tm = average dry gas meter temperature, (°R)( °F-I-460) (OR in. Hg 528°R 29.92 in. Hg Y = dry gas meter calibration factor, dimensionless. For our source test, we will assume a dry gas meter calibration factor of Y = 1. ?6«r = barometric pressure, in. Hg [< x )] L ( ) J dscf. 94 ------- Page Of Ini t ia 1 10.2 Calculate concentration (ppm) of both source sample and Sample Train Recovery utilizing the following equation: - N(V — Where: C^QJ — emission rate of sulfur dioxide, opm V, = volume of titrant required for sample (mL), Ba(ClO4)i Vr4 = volume of titrant required for blank (mL), Ba(ClO4)i N = normality of Ba(ClO4)t (meq/mL) V*>in = total volume of sample (mL) VM(«d) = volume of sample corrected to standard conditions (dscf) Va = volume of aliquot titrated (mL) K,= 424.30 424.30 95 ------- Page of TniTTaT 10.0 - SUMMARY Are final results expressed in units which satisfy permit on agency requirements? Does Tester have documentation to support emission calibrations (only required on smelt dissolving tank vents)? Brief Summary of Test 11.0 - AUTHORIZATION 11.1 Regulatory Observer Observer Signature Title Organization Address 11.2 Company Observer^ Company Observer Signature Title Telephone # 96 ------- FIELD INSPECTION NOTEBOOK TOTAL REDUCED SULFUR CONTINUOUS EMISSION MONITORING SYSTEM ABBREVIATED INSPECTION PROCEDURES 97 ------- FIELD INSPECTION NOTEBOOK TOTALS REDUCED SULFUR CONTINUOUS EMISSION MONITORING SYSTEM ABBREVIATED INSPECTION PROCEDURES Once a thorough evaluation of the TRS CEM system has been accomplished, control agency personnel may want to perform the next inspection on a less comprehensive basis. To assist the control, agency personnel, an abbreviated inspection procedure checklist has been developed. The abbreviated check- list is applicable to all TRS CEM systems. It does not address monitor specific inspection points, but does evaluate the TRS monitor on a system audit basis. The checklist is divided into three major areas: o Control agency records review; o Control agency records update; and o Source TRS CEM system review. The control agency records review consists of a review of permits and/or any current enforcement actions to determine the purpose of the CEM. In addition, a review of the PST report and current EER is conducted to verify conformance with the appropriate performance specification and reporting requirements for EERs. The control agency records update is conducted by telephone to verify that the records in agency files correctly describe the current CEM status. Finally, the source TRS CEM system review evaluates a source's record- keeping, data reduction procedures, monitor evaluation through zero/span checks and overall system review. 99 ------- ABBREVIATED INSPECTION PROCEDURES TOTAL REDUCED SULFUR CONTINUOUS EMISSION MONITORING SYSTEM CONTROL AGENCY RECORD REVIEW SOURCE NAME SOURCE ADDRESS SOURCE CONTACT SOURCE TELEPHONE NO. DATE ACTION REQUIRED* 1 - PERMIT REVIEW Is CEM required by permit? CEM requirement due to: NSPS SIP '_ Enforcement Action^ Yes No Is CEM installed? CEM Installation/startup date Allowable emission rate Date of source performance test Yes No 2 - CEM PERFORMANCE SPECIFICATION TEST (PST) REPORT REVIEW Dates of PST (<30 days after performance test) Date PST report submitted (<60 days after OTP^J~ Date of process startup (<180 days prior to DTP) Date of initial full-load operation (<60 days prior to Emission Rate Conversion formula CEM SUMMARY OPACITY TRS Analyzer Manufacturer Model Serial Recorder Manufacturer Model Serial Type PST REPORT REVIEW OPACITY TRS Relative Accuracy Calibration Error Response Time 24 Hr. Span Drift 24 Hr. Zero Drift 1 OTP= Operational Test Period 2 Magnetic Tape, Strip Chart, Data Logger, Other (describe) 101 ------- CALIBRATION REFERENCE MATERIAL REVIEW ACTION REQUIRED OPACITY Full Span Value Upscale Value TRS 0? Mid _Span Value Calibration Value Gas Value Verification RM Triplicate Analysis/Date NBS Traceable (Protocol 1) Other Gas Cell Value Verification Manufacturer/Date Comparison to Gas/Pate Agency Verification Other Was stratification evaluated? Discuss Describe monitor locations (diluent and pollutant' 3 - EXCESS EMISSION REPORT REVIEW Months reported Did each excess emission report document: Date, time, and duration of excess emissions Yes No Magnitude of excess emissions Yes No Reason for excess emissions Yes No Corrective action taken to reduce emissions Yes __ No Conversions factor/formula Yes No Method for determing conversion or correction factors used in calculating emission rate. Moisture content Gas velocity Temperatue ^ Diluent gas concentration (Op) Corrective action taken to reduce emissions Yes No Briefly discuss corrective action Process downtime Yes No Monitor downtime Yes No Corrective action taken to return monitor to operation Yes No Briefly discuss corrective action What percent availability did the CEM system achieve?_ (2190 - # hrs. downtime) /2190 = % availability 102 ------- CONTROL AGENCY RECORDS UPDATE FIELD REVIEW TELEPHONE REVIEW DATE ACTION REQUIRED 1 - SYSTEM OPERATION 8, MAINTENANCE Is monitoring system currently operational? Yes No Is system calibration checked daily? Automatic Manual Yes No Are recommended maintenance schedules/procedures provided by the CEM manufacturer and followed? Yes No What group or person is responsible for CEM maintenance? ^^ ~~~^ Is manufacturer's recommended spare parts list in plant inventory; or on order? Yes ___ No Are CEM system malfunctions documented to identify recurring failures of components or subsystems? Yes No 2 - RECORDKEEPING AND DATA REDUCTION TECHNIQUES What are the engineering units of the data recorded by the CEM system? What data reduction procedure is used in calculating emission rates? Over what time intervals are data averaged? Are chart speed, span value, date and time documented? Yes No Where is this data filed? On site Home office Other Is the following information filed for the previous two years: All system calibrations Yes No All maintenance performed on the CEM system Yes No All CEM system outages Yes No Span gas certified Yes __ No Triplicate reference method analysis of span gas Yes No PST reports Yes ___ No Modifications to the CEM system Yes No Excess Emission Reports Yes No Performance Test Reports Yes No Does span gas value (gas cell or neutral density filter) correspond to appropriate subpart requirements? Yes No Are zero and span calibration checks performed daily? Yes No Are drift values within performance specification Yes No requi rements? 103 ------- SOURCE TRS CEM SYSTEM REVIEW DATE SOURCE CONTACT 1 - Review records and update inspection procedures. Note all items to which unsatisfactory responses were received. Discuss each with source representative via telephone and note status below. 2 - Request copies of unreduced CEM system output including diluent gas and process parameter measurements necessary for conversion to emission rate which correspond to: o an excess emission, o a CEM system malfunction or outage, and o an interval of time during which no excess emission or CEM system malfunction occurred as determined by the EER review. 3 - Request a copy of CEM maintenance log corresponding to a CEM system malfunction and/or outage reported in EER. 4 - Request copies of zero and span calibration (generally shown on strip chart) check. After receiving the requested information reduce CEM data to units of omission standard and compare to corresponding emission rates submitted on EER. Refer to appropriate subpart of 40 CFR 60, 40 CFR 51 Appendix P, operating permit or enforcement action for proper data reduction pro- cedure and conversion factor. Review CEM output during reported process downtime, CEM calibration and monitor malfunction. ACTION REQUIRED ______ Are EER and agency calculated excess emission rates Yes No the same? Do agency calculations of data not reported as excess emissions indicate compliance? Yes No ~~Was CEM malfunction or outage caused by component or subsystem failure? Yes ___ No ^^[^ Was CEM outage scheduled for preventive maintenance? Yes No ____ Do source maintenance and operating records indicate monitor status and corrective action during outage? Yes No Which if any of the following caused the outage: - Calibration gas supply, - Optical surface condition, - Conditioning system, - Ai r purge system, - Optical alignment, - Light source. - Other (describe) 105 ------- ACTION REQUIRED 5 - TRS CEM SYSTEM INSTALLATION INSPECTION Is CEM sampling point in a nonstratified location (for gas monitors)? Yes No If so, how was non-stratification verified? If stratification exists, does sampling method and location of diluent gas sampling interface provide measurement of representative sample? Yes ___ No Is R.M. sampling point as close as possible to CEM sam- ~~~ pi ing point? ~ Yes No Describe access to sampling point. Are CEM sampling and analyzing components free of excessive vibration and extreme ambient temperatures? Yes _ No Describe location of calibration gas bottles (if used). Are transport and conditioning systems designed and in- stalled properly to deliver sample which meets analyzer requirements (temperature, wet, dry etc)? Refer to manufacturer's operation/maintenance manual Yes No Is calibration gas introduced at or near the sample interface at the proper pressure? Yes No Are control panel and recorder located in a controlled envi ronment? Yes ___ No Is purge air supply clean and dry? Yes No Transport line details - Conditioning System CEM SYSTEM OPERATION OBSERVATION Does calibration check indicate satisfactory drift? Yes No Is automatic zero compensation employed? Yes No If so, is zero compensation greater than 4% (opacity Yes No only) or does reference indicator (if used) show TRS CEM system zero signal to be within specified tolerance of zero reference signal? Yes No If calibration gases are used, are they introduced to the TRS CEM system at the sampling interface? Yes No Are calibration references (gas cell, gas cylinder, Yes No neutral density filter) of the appropriate value? 106 ------- ACTION REQUIRED Is recorder span set at value required by the appropri- ate subpart of 40 CFR 60, or by SIP? Yes No Is pollutant concentration easily determined from record- ing device? Yes _ No Is a zero offset employed? Yes No If not, how is negative zero drift quantified? ________ Are any fault indications displayed on control panel? Yes ___ No If so, discuss. 3 - CEM PROGRAM EVALUATION Is an alarm connected to TRS CEM control panel to signal excess emissions? Yes No How often is CEM output checked by an operator? What procedures are implemented during an excess emission incident to reduce emissions? Are process data measurements conducted according to the methods described in applicable NSPS/SIP regulation or permit? Yes No Are changes in calibration reference materials (gas, cell, filter) documented? Yes No How and how often is emission data reviewed for validity by the source? .___ _ . Are entries into Maintenance and Operations Logs made in relation to monitor: Malfunctions Yes No Calibrations Yes No Maintenance Yes No QA Checks Yes " No 107 ------- Conversion Factors International Metric System: Le Systeme International d'Unites (SI Units) Base Units of the International Metric System (SI) Quantity Length Mass Time Temperature Amount of substance Name of the Unit meter kilogram second Kelvin mole Symbol m kg s K mol Recommended decimal multiples and submultiples and the corresponding prefixes and names. Factor 1012 10' 10s 103 102 10 lO" 10-2 10" 10*« 10" 10-" IO-" 10-" Prefix tera giga mega kilo hecto deca deci centi milli micro nano pico femto atto Symbol T G M k h da d c m f- n P f a Meaning One trillion times One billion times One million times One thousand times One hundred times Ten times One tenth of One hundredth of One thousandth of One millionth of One billionth of One triliionth of One quadrilliomh of One quintillionth of 111 ------- Conversion from ppm to g/m3 at STP «< = 273.15°K ?„„=! atm g _ ppmxM.1 g-mole 1 dscm Jiters x 1(r. g-mole KHL \ 273 293.1S°K\ 1 273.15°K / x 10* ppm Atomic Weights and Numbers Name Arsenic Barium Cadmium Carbon Chlorine Hydrogen Iodine Lead Nitrogen Oxygen Phosphorous Potassium Sodium Sulfur Symbol As Ba Cd C Cl H I Pb N O P K Na S Atomic Number 33J 56: 48 6 17 1 53 82 7 8 15 19 11 16 Atomic Weight 74.9216 137.34 112.40 12.01115 35.453 1.00797 126.9044 207.19 14.0067 15.9994 30.9738 39.102 22.9898 32.064 112 ------- Volume From\To cm1 liter mj inj ftj cm' 1 1000 1x10-* 16.39 2.83x10- liter 0.001 1 1000 0.01639 28.32 mj 1x10- 0.001 1 1.64x10- 0.02832 in' 0.06102 61.02 6.10xlO-4 1 1728 ft' 3.53x10-' 0.03532 35.31 5.79x10- 1 Temperature °O5/9(°F-32) "F = 9/5 "032 °K=°C + 273.2 °R=°F + 459.7 Conversion factors—ppm vs. /ig/m3. \vDesired ~. ^vlWtt Givea\^ unit ^v Mg/mJ mg/mj Puts per million by volume 0, 5.10x10- — NO, 5.32 xlO- — SO, 3.83x10- — H,S 7.19x10- — CO — 0.875 HC as methane — 1.53 N. Desired _. \nnit Given\^ unit \ ppm Mg/nv1 0, 1960 NOi 1880 SO, 2610 H,S 1390 mg/m1 CO 1.14 HC 0.654 To convert a value from a given unit to a desired unit, multiply the given value by the factor opposite the given units and beneath the desired unit. U3 ------- TECHNICAL REPORT DATA (Please read Instructions on the reverse before completing) "l. REPORT NO. 340/l-85-013b 3. RECIPIENT'S ACCESSION NO. 4. TITLE AND SUBTITLE Field Inspection Notebook for Monitorinn Total Reduced Sulfur (TRS) from Kraft Pulp Mills 5. REPOR.T DATE December 1984 6. PERFORMING ORGANIZATION CODE . AUTHOR(S) William T. "Jerry" Winberry, Jr. 8. PERFORMING ORGANIZATION REPOI 19. PERFORMING ORGANIZATION NAME AND ADDRESS \ Engineering-Science \ 501 Hi Hard Street ; Durham, NC 27701 10. PROGRAM ELEMENT NO. 11. CONTRACY/GRANt NO.' 68-02-3960 12. SPONSORING AGENCY NAME AND ADDRESS Stationary Source Compliance Division Technical Service Branch Waterside Mall, 401 M Street, S.W. Washington, DC 20460 13 TyJJi OF,flSPORT-ANO PERIOD COVERED 14. SPONSORING AGENCY CODE 15. SUPPLEMENTARY NOTES /m™-v Supplements Technioal_Assistance Document for Monitoring Total Reduced Sulfur (TRS) from Kraft Pulp~MTn.s7~EPA Task Manager-Sonya Stelmack, (202) 382-2851 16. ABSTRACT Field performance audit procedures were developed for three of the most common total reduced sulfur (TRS) continuous emission monitorina systems (CEMS). These procedures were designed to assist state/federal field inspectors, in the evaluation of TRS-CEMS. Contained in the notebook are checklists and data entry tables covering preparation for the inspection, preliminary review of records, preliminary on-site meeting with source personnel, and general auidelines for inspection of any type TRS- CEI^S. Specific audit procedures for three of the most common models of TRS CEMS - Sampling Technology Inc. Model 100 TRS CEM System; - Barton Titrator TRS System; and - Bendix Gas Chromatograph TRS System are provided as sectional inserts. In auditing these monitors the inspector should follow the specific procedure rather than the neneral guidelines given in the body of the field notebook. Conscientious us'e of this notebook will aid the inspector in conducting a thorough audit of the TRS CEMS and provide a comprehensive original record of all phases of the inspection. 17. KEY WORDS AND DOCUMENT ANALYSIS DESCRIPTORS b.lDENTIFIERS/OPEN ENDED TERMS c. COSATI Field/Group Air Pollution Monitoring Kraft Pulp Mills Continuous Emission Monitorina Opacity Monitoring Systems Audit Procedures TRS Continuous Emission Monitors 18. DISTRIBUTION STATEMENT Release to Public TTncIassiflea SS (This Repoi 20. SECURITY CLASS (Thispage} Unclassified 22. PRICE _12IL EPA F«» 2220-1 (R.v. 4-77) *»KKVIOU« COITION it OBSOLETE ------- |