# Final Report

Emissions Testing For Systems 1, 2, 3, 4A, 7, 8,13A, and the Deep Bed Carbon Scrubber (Class II Air Quality Operating Permit No. AP1041-0158.02 and the Nevada Mercury Control Program) 

# Marigold Mining Company Valmy, Nevada

Prepared for:



### Marigold Mining Company P.O. Box 160 Valmy, Nevada 89438

Prepared by:



### TRC Companies, Inc. 6672 Boulder Highway, Suite 5 Las Vegas, Nevada 89122



# August 2008TRC Project No. 159240

August 2008



### Final Report
Emissions Testing For Systems 1, 2, 3, 4A, 7, 8, 13 A, and the Deep Bed Carbon Scrubber (Class II Air Quality Operating Permit No. AP1041-0158.02 and the Nevada Mercury Control Program) 

### Marigold Mining Company Valmy, Nevada

Prepared for
Marigold Mining Company P.O. Box 160 Valmy, Nevada 89438

Prepared by
TRC Companies, Inc. 6672 Boulder Highway, Suite 5 Las Vegas, Nevada 89122 (702) 437-5800

DISCLAIMER
This document is intended for use solely by Marigold Mi ning Company (Marigold Mining) for the specific purposes described in the contractual documents between TRC Companies, Inc. (TRC) an d Marigold Mining. All professional services performed and reports generated by TRC have been prepared for Marigold Mining's purposes as described in the contract. The information, statements a nd conclusions contained in the document ha ve been prepared in accordance with the work statement and contract terms a nd conditions. The document may be subjec t to differing interpretations and/or may be misinterpreted by third persons or entities who were not involved in the investigative or consultation process. TRC therefore expressly disclaims any li ability to persons other than Marigol d Mining who may use or rely upon this document in any way or for any purpose.TABLE OF CONTENTS

Section Page

L2008-371 ii 1.0 INTRODUCTION............................................................................................................. 1
1.1 OVERVIEW ................................................................................................................... 1 1.2 SCOPE OF WORK......................................................................................................... 3
2.0 SUMMARY AND DISCUSSION OF RESULTS .......................................................... 6
2.1 TEST PROGRAM OBJECTIVES.................................................................................. 6 2.2 FIELD TEST CHANGE S AND PROBLEMS............................................................... 6 2.3 PRESENTATION OF RESULTS .................................................................................. 6

2.3.1 System 13A Carbon Kiln Combus tion Exhaust Stack - S2.012A .......................... 6 2.3.2 System 13A Carbon Kiln Drum Exhaust Stack – S2.013A.................................... 7 2.3.3 Deep Bed Carbon Scrubber Outlet Stack................................................................ 7 2.3.4 System 2 Crushing Circuit Baghouse #2 – S2.001-S2.004 .................................... 7 2.3.5 System 3 Screening System Baghouse #4 – S2.005-S2.008 .................................. 7 2.3.6 Opacity Testing for Systems 1, 4A, 7, and 8 .......................................................... 8
3.0 PROCESS DESCRIPTION ........................................................................................... 15
3.1 INTRODUCTION ........................................................................................................ 15 3.2 SAMPLING LOCATIONS .......................................................................................... 15

3.2.1 System 1................................................................................................................ 1 5 3.2.2 System 2................................................................................................................ 1 5 3.2.3 System 3................................................................................................................ 1 6 3.2.4 System 4A............................................................................................................. 16 3.2.5 System 7................................................................................................................ 1 6 3.2.6 System 8................................................................................................................ 1 6 3.2.7 System 13A........................................................................................................... 16 3.2.8 Deep Bed Carbon Scrubber System...................................................................... 16
4.0 SAMPLING PROCEDURES ........................................................................................ 18
4.1 OVERVIEW ................................................................................................................. 18 4.2 FIELD PROGRAM DESCRIPTION ........................................................................... 18 4.3 PRESAMPLING ACTIVITIES.................................................................................... 19

4.3.1 Equipment Calibration.......................................................................................... 19 4.3.2 Glassware Preparation .......................................................................................... 20 4.3.3 Sample Media Preparation.................................................................................... 21 4.3.4 Continuous Emissions Monitoring for O 2 , CO 2 , NO x , and CO ............................ 21 4.3.5 Interference Gas Test ............................................................................................ 23 4.3.6 NO 2 to NO Conversion Efficiency ....................................................................... 24 4.4 ONSITE SAMPLING ACTIVITIES............................................................................ 24

4.4.1 EPA Methods 1 and 2 for Velocity Measurements and Cyclonic Flow............... 24 4.4.2 EPA Method 4 for Moisture Determination ......................................................... 25 4.4.3 EPA Method 5 for Particulate Matter ................................................................... 25 4.4.4 EPA Methods 201A/202 for Pa rticulate Matter (PM)/PM 10 and Condensibles ... 26 4.4.5 EPA Method 9 for Opacity/Visible Emissions ..................................................... 29 4.4.6 Continuous Emissions Monitoring for O 2 , CO 2 , NO x , and CO ............................ 29TABLE OF CONTENTS

Section Page

L2008-371 iii 4.4.7 EPA Method 29 for Mercury Emissions............................................................... 30 4.5 PRODUCTION SAMPLE COLLECTION.................................................................. 35 4.6 PROCESS MONITORING .......................................................................................... 35
5.0 ANALYTICAL PROCEDURE S AND CALCULATIONS ........................................ 37
5.1 ANALYTICAL PROCEDURES.................................................................................. 37

5.1.1 Particulate Matter from Method 5 Sampling Train............................................... 37 5.1.2 Particulate Matter from Method 201A/202 Sampling Train................................. 37 5.1.3 Particulate Matter and Mercury from Method 29 Sampling Train....................... 38 5.2 CALCULATIONS........................................................................................................ 38

5.2.1 Flow Rates and Isokinetics ................................................................................... 38 5.2.2 Grains Per Dry Standard Cubic Foot .................................................................... 41 5.2.3 Pounds Per Hour – Particul ate Matter and Mercury............................................. 42 5.2.4 Pounds Per Hour – Nitrogen Oxides (NO x ) and Carbon Monoxide (CO)............ 42
6.0 QUALITY ASSURANCE .............................................................................................. 43
6.1 OVERVIEW ................................................................................................................. 43 6.2 FIELD QUALITY CONTROL SUMMARY............................................................... 43

6.2.1 Calibration Procedures.......................................................................................... 43 6.2.2 Equipment Leak Checks ....................................................................................... 43 6.2.3 Cyclonic Flow Check............................................................................................ 44 6.2.4 Calibration Gases.................................................................................................. 44 6.2.5 Instrument Calibrations......................................................................................... 44 6.3 DATA REDUCTION, VALIDAT ION, AND REPORTING ...................................... 44

6.3.1 Field Data Reduction ............................................................................................ 44 6.3.2 Data Validation ..................................................................................................... 45 6.3.3 Data Reporting...................................................................................................... 45 6.4 EXCEPTIONS .............................................................................................................. 46

Appendices
A Field Sampling Data Sheets B Field Reduced Data C Process Monitoring Data D Laboratory Analytical Data E Equipment Calibration DataTABLE OF CONTENTS, continued

L2008-371 ii TABLES

Number Page
1-1 Compliance Emissions Test Program Overview .................................................................4 2-1 Summary of Results for Ca rbon Kiln Combustion Exhaust................................................9 2-2 Summary of Results for Carbon Kiln Drum Exhaust ........................................................10 2-3 Summary of Results for Deep Bed Carbon Scrubber Exhaust ..........................................11 2-4 Summary of Results for Crushing Circuit Baghouse #2....................................................12 2-5 Summary of Results for Screening Baghouse #4 ..............................................................13 2-6 Summary of Results for Sy stem 1, 4A, 7, and 8 Opacity ..................................................14 4-1 Calibration Gas Values and Instrument Ranges ................................................................23 4-2 Performance Criteria....................................................................................................... ...23

FIGURES

Number Page
4-1 Schematic Diagram of EPA Method 5 Sampling Train.....................................................33 4-2 Schematic Diagram of EPA Methods 201A/202 Sampling Train.....................................34L2008-371 1 1.0 INTRODUCTION

1.1 OVERVIEW

Pursuant to the requirements of the Nevada Me rcury Control Program re gulated by the State of Nevada Department of Cons ervation and Natural Resources , Division of Environmental Protection (NDEP), Bureau of Air Pollution Cont rol, Marigold Mining Company (Marigold) was required to perform emissions compliance testing for multiple thermal units that emit mercury at the Marigold mining facility located in Valm y, Nevada. Additionall y, Marigold conducted testing on several sources to justify future permitting of increased permit limitations.

TRC Companies, Inc. (TRC) was retained by Marigold to provide sampling and analytical support for the emissions compliance test pr ogram. TRC supported and managed the test program from the Las Vegas, Nevada office. TR C prepared and received approval of the testing protocol to satisfy the testing re quirements stipulated in the operat ing permit. The purpose of the testing was to:

System 1 – Ore Handling System

- Determine compliance with visible emission st andard limitations of the operating permit at an increased throughput.

System 2 – Crushing Circuit Baghou se #2 Exhaust Stack – S2.001 to S2.004

- Determine the emission rate of particulate matter (PM) and particulate matter equal to or less than an aerodynamic diameter of nominally 10 μm (PM 10 ) at an increased throughput; and

- Determine compliance with visible emission st andard limitations of the operating permit at an increased throughput.

System 3 – Screening System Baghou se #4 Exhaust Stack – S2.005 to S2.008

- Determine the emission rate of particulate matter (PM) and particulate matter equal to or less than an aerodynamic diameter of nominally 10 μm (PM 10 ) at an increased throughput; and

- Determine compliance with visible emission st andard limitations of the operating permitL2008-371 2 at an increased throughput.

System 4A - Radial Stacker System (Alternative Operating Scenario)

- Determine compliance with visible emission st andard limitations of the operating permit at an increased throughput.

System 7 – Baghouse #2 Ma terial Handling System

- Determine compliance with visible emission st andard limitations of the operating permit at an increased throughput.

System 8 – Baghouse #4 Ma terial Handling System

- Determine compliance with visible emission st andard limitations of the operating permit at an increased throughput.

System 13A – Carbon Kiln Comb ustion Exhaust Stack - S2.012A

- Determine the emission rate of nitrogen oxides (NO x ) and carbon monoxide (CO) in regards to limits in the operating permit at an increased throughput.

- Determine compliance with visible emission st andard limitations of the operating permit at an increased throughput.

System 13A – Carbon Kiln Drum Exhaust Stack – S2.013A

- Establish annual mercury emission rates for the source.

Deep Bed Carbon Scrubber Outlet Stack (Control for the retort, electrowinning cells (3), pregnant and barren tanks, and the smelting furnace).

- Establish annual mercury emission rates fo r the sources controlled by the Deep Bed
Carbon Scrubber.

Sampling and analysis procedures described in this document we re conducted using procedures deemed acceptable by the NDEP. TRC was responsible for the collection and analysis of all flueL2008-371 3 gas samples.

1.2 SCOPE OF WORK

The purpose of the test program was to determin e the emission rates and visible emissions for each parameter included in the operating permit for the identified emission units. Triplicate test runs were conducted for all parameters. Table 1- 1 presents a summary of the test parameters,
test methods and run times.L2008-371 4 TABLE 1-1. COMPLIANCE EMISSI ONS TEST PROGRAM OVERVIEW

Source Test Parameter Test Method Run Time (minutes) System 1 Ore Handling System

PF1.001 – PF1.003 Opacity EPA Method 9 6

System 2 Crushing Circuit Baghouse #2
S2.001-S2.004 Flows and Moisture EPA Methods 1 - 4

PM/PM 10 EPA Methods 5 and 201A/202 120 / 180 Opacity EPA Method 9 6 System 3 Screening System Baghouse #4
S2.005-S2.008 Flows and Moisture EPA Methods 1 - 4

PM/PM 10 EPA Methods 5 and 201A/202 120 / 180 Opacity EPA Method 9 6 System 4A Radial Stacker System
PF1.004 (Alternative Operating Scenario) Opacity EPA Method 9 6

System 7 Baghouse #2 Material Handling System
PF1.009 Opacity EPA Method 9 6

System 8 Baghouse #4 Material Handling System
PF1.010 Opacity EPA Method 9 6

System 13A
Carbon Kiln Combustion Exhaust
S2.012A Flows and Moisture EPA Methods 1 – 4

NOx and CO EPA Methods 7E and 10 60L2008-371 5 Opacity EPA Method 9 6

Source Test Parameter Test Method Run Time (minutes) System 13A
Carbon Kiln Drum Exhaust
S2.013A Flows and Moisture EPA Methods 1 – 4

Mercury EPA Method 29 120 Deep Bed Carbon
Scrubber Outlet Stack (1-scenario) Flows and Moisture EPA Methods 1 – 4

Mercury EPA Method 29 120

The required measurement parameters and test me thods to accomplish these test objectives were
as follows: • 40 CFR Part 60, Appendix A, EPA Methods
· Methods 1 & 2 - Velocity and Flow Rate · Method 3/3A - Oxygen and Carbon Dioxide · Method 4 - Moisture · Method 5 - Particulate Matter · Method 7E - Oxides of Nitrogen · Method 9 - Visible Emissions/Opacity · Method 10- Carbon Monoxide · Method 29 - Mercury
• 40 CFR Part 51, Appendix M, EPA Methods

· Method 201A/202 - PM/PM 10L2008-371 6 2.0 SUMMARY AND DISCUSSION OF RESULTS

2.1 TEST PROGRAM OBJECTIVES

The purpose of the test program was the following:

• Obtain emission rates of nitrogen oxides (NO x ) and carbon monoxide (CO) at elevated throughput for the Carbon Kiln Combustion Exhaust Stack;

• Obtain emission rate of particulate matter (P M) and particulate matter equal to or less than an aerodynamic diameter of nominally 10 μm (PM 10 ) at elevated throughput for the System 2 Crushing Circuit Baghouse #2, and th e System 3 Screening System Baghouse #4 ;

• Demonstrate compliance with the visible emission limits in the operating permit at elevated throughput for the System 1 Ore Handling, System 2 Crushing Circuit Baghouse #2, System 3 Screening Baghouse #4, System 4A Radial Stacker, System 7 Material Handling Baghouse #2, System 8 Material Ha ndling Baghouse #4, and the System 13A Carbon Kiln Combustion Exhaust; and

• Establish mercury emission rates for the Ca rbon Kiln Drum Exhaust and the Deep Bed Carbon Scrubber Outlet (one operating scenario).

2.2 FIELD TEST CH ANGES AND PROBLEMS

No problems were encountered, and no field test changes were required during the sampling

program.

2.3 PRESENTATION OF RESULTS

2.3.1 System 13A Carbon Kiln Combustion Exhaust Stack - S2.012A

Testing of System 13A, Emission Unit S2.012A wa s conducted on June 10, 2008. Triplicate test
runs were conducted at the exha ust stack for nitrogen oxides (NO x ) and carbon monoxide (CO) in accordance with EPA Methods 7E and 10, respec tively. In addition, trip licate test runs were conducted for visible emissions (opacity) in ac cordance with EPA Method 9. A summary of the test results is presen ted in Table 2-1.L2008-371 7 2.3.2 System 13A Carbon Kiln Drum Exhaust Stack – S2.013A

Testing of System 13A, Emission Unit S2.013A wa s conducted on June 12, 2008. Triplicate test
runs were conducted at the exhaust stack for mercury (Hg) in accordance with EPA Method 29. A summary of the test results is presented in Table 2-2.

2.3.3 Deep Bed Carbon Scrubber Outlet Stack

Testing of Deep Bed Carbon Scrubber Outlet wa s conducted under one operating scenario on June 11, 2008. Triplicate test runs were conducte d at the exhaust stack for mercury (Hg) in accordance with EPA Method 29. A summary of th e test results is presented in Table 2-3.

2.3.4 System 2 Crushing Circuit Baghouse #2 – S2.001-S2.004

Testing of System 2, Emission Units S2.001- S2.004 was conducted on June 17 and June 20, 2008. Triplicate test runs were conduc ted at the exhaust stack for PM/PM 10 in accordance with EPA Methods 5 and 201A/202. In addition, tripli cate test runs were conducted for visible emissions (opacity) concurrent with the PM/PM 10 testing. A summary of the test results is presented in Table 2-4.

2.3.5 System 3 Screening System Baghouse #4 – S2.005-S2.008

Testing of System 3, Emission Units S2.005- S2.008 was conducted on June 18 and June 19, 2008. Triplicate test runs were conduc ted at the exhaust stack for PM/PM 10 in accordance with EPA Methods 5 and 201A/202. In addition, tripli cate test runs were conducted for visible emissions (opacity) concurrent with the PM/PM 10 testing. A summary of the test results is presented in Table 2-5.L2008-371 8 2.3.6 Opacity Testing for Systems 1, 4A, 7, and 8

Triplicate test runs were conduc ted for visible emissions (opacity) on June 19, 2008 for System 1 Ore Handling, System 4A Radial Stacker, and Sy stems 7 and 8 Material Handling Baghouses. A summary of the results is presented in Table 2-6.Source/Test Parameters Results Units Emission Limit (Average of three test runs) Carbon Kiln Combustion Exhaust

NOx 0.20 lb/hr 0.73 0.88 tpy 3.18

CO 0.440 lb/hr 0.099 1.93 tpy 0.43
Opacity 0 % 20 Marigold Mining Company Valmy, Nevada Table 2-1 Summary of Results System 13A, Source No. S2.012A June 10, 2008Source/Test Parameters Results Units Emission Limit (Average of three test runs)
PARTICLE BOUND Hg Net Weight 0.0067 mg Emission Concentration 1.33E-06 gr/dscf Emission Concentration 3.05E-06 g/dscm Emission Rate 4.38E-06 lb/hr NA
GASEOUS Hg Net Weight 0.0132 mg Emission Concentration 2.63E-06 gr/dscf Emission Concentration 6.02E-06 g/dscm Emission Rate 8.63E-06 lb/hr NA
TOTAL Hg COLLECTED Net Weight 0.0199 mg Emission Concentration 3.96E-06 gr/dscf Emission Concentration 9.08E-06 g/dscm Emission Rate 1.30E-05 lb/hr NA PARTICULATE MATTER Net Weight 10.73 mg Emission Concentration 2.14E-03 gr/dscf Emission Concentration 4.91E-03 g/dscm Emission Rate 7.00E-03 lb/hr Marigold Mining Company Valmy, Nevada Table 2-2 Summary of Mercury Emission Results System 13A, Source No. S2.013A

June 12, 2008 Carbon Kiln Drum OutletSource/Test Parameters Results Units Emission Limit (Average of three test runs)
PARTICLE BOUND Hg Net Weight 0.0599 mg Emission Concentration 1.06E-05 gr/dscf Emission Concentration 2.44E-05 g/dscm Emission Rate 1.42E-04 lb/hr NA
GASEOUS Hg Net Weight 1.079 mg Emission Concentration 1.91E-04 gr/dscf Emission Concentration 4.39E-04 g/dscm Emission Rate 2.56E-03 lb/hr NA
TOTAL Hg COLLECTED Net Weight 1.139 mg Emission Concentration 2.02E-04 gr/dscf Emission Concentration 4.63E-04 g/dscm Emission Rate 2.70E-03 lb/hr NA PARTICULATE MATTER Net Weight 51.67 mg Emission Concentration 9.14E-03 gr/dscf Emission Concentration 2.10E-02 g/dscm Emission Rate 1.22E-01 lb/hr Marigold Mining Company Valmy, Nevada Table 2-3 Summary of Mercury Emission Results Deep Bed Carbon Scrubber June 11, 2008Source/Test Parameters Results Units Emission Limit (Average of three test runs )

PARTICULATE MATTER (M5) Net Weight 23.1 mg Emission Concentration 0.0043 gr/dscf Emission Rate 0.281 lb/hr 0.50 Emission Rate 1.23 tpy 2.19

PM10/CONDENSIBLE PARTICULATE MATTER (M201A/202) Net Weight 0.0129 grams Net Weight 12.93 mg Emission Concentration 0.0030 gr/dscf Emission Rate 0.18 lb/hr 0.50 Emission Rate 0.807 tpy 2.19

OPACITY June 17, 2008 0 % 20 June 19, 2008 1.3 % 20 Marigold Mining Company Valmy, Nevada Table 2-4 Summary of Results System 2, Source No. S2.001-S2.004

June 17, 2008 June 20, 2008 Crushing Circuit Baghouse #2Source/Test Parameters Results Units Emission Limit (Average of three test runs )

PARTICULATE MATTER (M5) Net Weight 16.9 mg Emission Concentration 0.0034 gr/dscf Emission Rate 0.291 lb/hr 0.30 Emission Rate 1.27 tpy 1.31

PM10/CONDENSIBLE PARTICULATE MATTER (M201A/202) Net Weight 0.0144 grams Net Weight 14.43 mg Emission Concentration 0.0033 gr/dscf Emission Rate 0.283 lb/hr 0.30 Emission Rate 1.24 tpy 1.31

OPACITY June 18, 2008 0 % 20 June 19, 2008 0 % 20 Marigold Mining Company Valmy, Nevada Table 2-5 Summary of Results System 3, Source No. S2.005-S2.008

June 18, 2008 June 19, 2008 Screening System Baghouse #4Source/Test Parameters Results Units Emission Limit (Average of three test runs) Ore Handling System
Opacity 0.27 % 10
Radial Stacker System
Opacity 1.39 % 20
Material Handling Baghouse #2
Opacity 0 % 20
Material Handling Baghouse #4
Opacity 3.16 % 20 Marigold Mining Company Valmy, Nevada Table 2-6 Summary of Results Systems 1, 4A, 7 and 8 June 19, 2008L2008-371 15 3.0 PROCESS DESCRIPTION

3.1 INTRODUCTION

Marigold Mining Company operates a gold produci ng mine on property located four miles south of I-80 (Exit 216) in Valmy, Nevada. There ar e several processing facilities located on the property which separate the gold fr om the recovered ore. Part of this mining process utilizes Systems 1, 2, 3, 4A, 7, 8, 13A, and the Deep Bed Carbon Scrubber.

3.2 SAMPLING LOCATIONS

The procedures specified by EPA Method 1, " Sample and Velocity Traverses for Stationary
Sources ", were followed to determine the number and location of traverse points to be used for the stratification testing and velo city traverses. The number of straight run stack diameters (equivalent diameters) upstream and downstream from the sample ports were used to determine the minimum number of traverse points required.

Additional detail has been provided for each syst em in this Final Report, including diameters upstream and downstream, internal diameters of each exhaust stream, sampling point locations and distances. These details are provided in Appendix A.

3.2.1 System 1

The emissions from System 1 emission units (PF1.001-PF1.003) are controlled by best operating practices.

3.2.2 System 2

The emissions from System 2 emission units (S2.001-S2.004) are ducted to a control system consisting of a Mikropul 144-8-20 Baghouse (Ba ghouse #2) with 100% ca pture and a nominal volume flow rate of 4,800 dry standard cubic fe et per minute. The exhaust of the baghouse is
vertical with an internal diam eter of 24 inches. There are 2 sampling ports located at 90 degree
intervals.L2008-371 16 3.2.3 System 3

The emissions from System 3 emission units (S2.005-S2.008) are ducted to a control system consisting of a Mikropul 144-8-20 Baghouse (Ba ghouse #4) with 100% ca pture and a nominal volume flow rate of 7,400 dry standard cubic fe et per minute. The exhaust of the baghouse is
vertical with an internal diam eter of 24 inches. There are 2 sampling ports located at 90 degree
intervals.

3.2.4 System 4A

The emissions from System 4A emission unit (PF 1.004) is controlled by be st operating practices.

3.2.5 System 7

The emissions from System 7 emission unit (PF1 .009) is controlled by be st operating practices.

3.2.6 System 8

The emissions from System 8 emission unit (PF1 .010) is controlled by be st operating practices.

3.2.7 System 13A

System 13A includes two separate stacks for the carbon kiln system which manufactured by Lockheed Haggerty Engineering and Manufact uring Company, Ltd. Emission unit S2.012A represents the carbon kiln combustion emissions which are uncontrolled and discharge to a
horizontal stack with an internal diameter of 15 inches. Emission unit S2.013A represents the
carbon kiln drum emissions which are controlled with a Venturi scrubbe r/carbon scrubber system and discharge to a horizontal stack with an internal diameter of 7.5 inches.

3.2.8 Deep Bed Carbon Scrubber System

The Deep Bed Carbon Scrubber System includes one deep bed carbon scrubber outlet. The DeepL2008-371 17 Bed Carbon Scrubber System controls emissions from the retort, electrowinning cells(3), pregnant and barren tanks, and the smelting furnace), The outlet stack is vertical with an internal
diameter of 9.5 inches.L2008-371 18 4.0 SAMPLING PROCEDURES

4.1 OVERVIEW

This section describes the procedures that TRC followed during the field sampling program. Throughout the program TRC followed EPA Met hods 40 CFR Part 60 Appendix A and 40 CFR Part 51 Appendix M sampling procedures.

The remainder of this section is divided into several subsections: Field Program Description; Pre-sampling Activities; and Onsite Sampling Activities.

4.2 FIELD PROGRAM DESCRIPTION

The field sampling was conducted by TRC over a tw o week period. On the first day equipment was set up and preliminary measurements were made. On the following days, TRC collected samples for the parameters listed below on the permitted units:

O 2 , CO 2 , NO x , CO, PM, and PM 10 Velocity and Percent Moisture Mercury Visible Emissions

TRC personnel used the following EPA Methods as listed in 40 CFR Part 60, Appendix A.

• EPA Method 1 Sample Velocity Tr averse for Stationary Sources

• EPA Method 2 Determination of Stack Gas Velocity and Volumetric Flow Rate (Type S pitot tube)

• EPA Method 3 Gas Analysis for the Determination of Dry Molecular Weight

• EPA Method 3A Determination of Oxygen and Carbon Dioxide Concentrations in Emissions from Stationary Sources (Instrumental Analyzer Procedure)

• EPA Method 4 Determination of Moisture Content in Stack Gases

• EPA Method 5 Determination of Pa rticulate Matter Emissions from Stationary SourcesL2008-371 19 • EPA Method 7E Determination of Nitrogen Oxides Emissions from Stationary Sources (Instrumental Analyzer Procedure)

• EPA Method 9 Visual Determination of the Opacity of Emissions from Stationary Sources

• EPA Method 10 Determination of Ca rbon Dioxide Emissions from Stationary Sources (Instrumental Analyzer Procedure)

• EPA Method 29 Determination of Metals Emissions from Stationary Sources

• EPA Method 201A Determination of PM 10 Emissions (Constant Sampling Rate Procedure)
Additionally, TRC personnel used the following EPA Methods as listed in 40 CFR Part 51, Appendix M:

• EPA Method 202 Determination of Conde nsible Particulate Emissions from Stationary Sources

4.3 PRESAMPLING ACTIVITIES

Presampling activities included eq uipment calibration, precleaning of the sample train glassware,
and other miscellaneous tasks. Each of these activities are described or referenced in the following subsections. Other pres ampling activities included team meetings, equipment packing,
and finalization of all details l eading up to the coordi nated initiation of the sampling program.

4.3.1 Equipment Calibration

TRC follows an orderly program of positive acti ons to prevent the failure of equipment or instruments during use. This preventative main tenance and careful calibration helps to ensure accurate measurements from field and laboratory instruments.

Once the equipment had gone throug h the cleaning and repair proce ss it was then calibrated. All equipment that was scheduled for field use was cleaned and checked prior to calibration. OnceL2008-371 20 the equipment had been calibrated, it was packed and stored to ensure the integrity of the equipment.

Inspection and calibration of the equipment is a crucial st ep in ensuring the successful completion of the field effort. All equipment was inspected for proper operation and durability prior to calibration. Calibrati on of the following equipment we re conducted in accordance with the procedures outlined in EPA documents entitled " Quality Assurance Handbook for Air Pollution Measurement Systems; Volume III - Stationary Source Specific Methods " (EPA-600/4- 77-027b), EPA 600/R-94-038C, and 40 CFR Part 60 Appendix A, and 40 CFR Part 51 Appendix M. All calibrations were pe rformed prior to the test program.

• Probe Nozzles (QA Handbook, Vol III, Section 3.4.2, pp. 19) - average three internal diameter measurements of th e nozzle; difference between high and low

 + 0.1 mm. Recalibrate, reshape and sharpe n when nozzle becomes nicked, dented or corroded.

• Pitot tubes (QA Handbook Vol III, S ection 3.1.2, pp. 1-13) - measured for appropriate spacing and dimensions or cal ibrated in a wind tunnel. Rejection criteria is given on the calibration sheet. A post-test check inspects for damage.

• Thermocouples (EPA Alternate 011) – verified against a mercury-in-glass thermometer at one point. Acceptance limit: + 2oF.

• Dry gas meters (EPA 40 CFR Part 60, Me thod 5) - calibrated against a critical orifice. Acceptance criteria - pretest Y i = Y = + 0.02; post test Y = + 0.05 Y i .

• Orifice meter calibrated ag ainst a wet test meter. Acceptance criteria is ∆ H@ i = + 0.2 from the average value.

• Field barometer (EPA Method 2) – co mpared against a mercury-in-glass barometer or use Airport Station BP a nd correct for elevation. Acceptance criteria -

 0.02 in. Hg; post-test check will be the same.

• Analytical balances (QA Handbook, Vol III, Section 3.4.2, pp. 19) – Acceptance criteria - calibrate with Standard Class-S weights within

 0.5 mg of stated value. Corrective action: Have manuf acturer recalibrate or adjust.

4.3.2 Glassware Preparation

Sample train glassware requires specialized precleaning to avoid contamination of the sampleL2008-371 21 from the collection container or devices. The sample train glassware necessary for the EPA Methods 5 and 201A/202 sampling trains was precleaned using an Alconox ® soap and water wash. Acetone was used for rinsing followe d by air-drying. The glassware for the EPA Methods 201A/202 sampling trains was then rinsed with methylene chloride followed again by air-drying. The glassware was then sealed with Parafilm ®

.

The sample train glassware necessary for th e EPA Method 29 sampling trains was precleaned using an Alconox ® soap and water wash. Deionized water was used for rinsing followed by airdrying. The glassware was then soaked in nitric acid bath (10% nitric acid) followed again by a
deionized water rinse followed by air-drying. The glassware wa s then sealed with Parafilm ®

.

4.3.3 Sample Media Preparation

All reagents were checked in accordance with the TRC’s existing QC Program to minimize the probability of using contaminated solvents. This included the use of spectro-grade solvents from the same lot and the collection and analysis of the appropriate blanks. All filters were desiccated and weighed to the nearest 0.5 mg constant weight.

4.3.4 Continuous Emissions Monitoring for O 2 , CO 2 , NO x , and CO

TRC conducted continuous emissions monitori ng for oxygen (EPA Method 3A), carbon dioxide (EPA Method 3A), oxides of nitrogen (EPA Method 7E), and carbon monoxide (EPA Method 10) for the applicable Systems. TRC followed procedures outlined in the EPA Publication 340/1-83-016 regarding setup a nd operation of its Transpor table Continuous Emissions Monitoring System (TCEMS).

The TCEMS consisted of three subsystems: sa mple acquisition/conditioning, sample analysis, and a data acquisition system. Sample acqui sition/conditioning is designed to deliver a representative sample of the gas stream to the sa mple analysis subsystem. Since the stream must be clean and dry for O 2 , CO 2 , NO x , and CO analyzers, a gla ss fiber filter and noncontact moisture condenser were used for particulate an d moisture removal. The sample line was heat traced to eliminate inline condensation prior to the condenser.L2008-371 22 In each case, accurate interpretati on of analyzer response required the systematic calibration of the instrument against gases of known concentrations.

The data acquisition subsystem consisted of a dig ital data logger design ed to receive and log instrument signals (raw voltages) at user-defin ed intervals. Once the system was set up, the TCEM was connected to a power source and brought online. Sample line and signal wires were strung between the sampling and TCEM locations, and the probe was placed in the sampling port at the sampling location.

Prior to insertion of the probe into the sampling location, the samp le/acquisition system was leak checked by the following procedure:

a. plugged probe; b. observed that flow in ro tameter reached zero lpm; c. observed vacuum; and d. confirmed that sample vacuum during sampling did not exceed vacuum attained during leak check.

The initial phase of instrumental analysis met hods required calibration of all involved monitors. At the beginning of each day, system instrume nt calibrations for zero and upscale gases were performed prior to initiat ion of testing by system calibration gas injection. System calibrations were performed both prior to and followi ng each run using a zero and one upscale gas concentration. This was accomplished by directing calibration gas through the sample line and conditioning system to assess system bias. Fo llowing completion of the required runs, final system calibrations were performed. These proce dures allowed for determination of initial and final system calibration error, as well as system drift. The calib ration gas values and instrument range settings are li sted in Table 4-1.

Calibration gases used were EPA Protocol 1, traceab le to the National Institute of Standards and Technology (NIST). The measurement system perf ormance specifications as stated in 40 CFR 60 Appendix A, for Methods 3A, 7E, and 10 are lis ted in Table 4-2 and were the performance criteria for this program.L2008-371 23 TABLE 4-1. CALIBRATION GA S VALUES AND INSTRUMENT RANGES

Analyzer Range Conc. High Mid Low Zero
NO x 0-110 ppm 102.0 51.20 N/A nitrogen CO 0 – 100 ppm 101.0 40.10 N/A nitrogen
CO 2 0 – 20 % 17.87 9.81 N/A nitrogen
O 2 0 – 25 % 17.97 10.10 N/A nitrogen

TABLE 4-2. PERFORMANCE CRITERIA

Procedure Performance Criteria O 2 /CO 2 (M3A) NOx (M7E) CO (M10) Zero Drift, % of high span gas < ± 3 < ± 3 < ± 3 Calibration Drift, % of high span gas < ± 3 < ± 3 < ± 3 Response time, seconds 60 60 60 Interference Response, % of high span gas < ± 2 < ± 2 < ± 2 NO2 to NO Converter, % efficiency NA < ± 2 NA Calibration Error, % of cal gas < ± 2 < ± 2 < ± 2 Sytsem Bias, % of calibration span < ± 5 < ± 5 < ± 5

4.3.5 Interference Gas Test

Before mobilizing for the field portion of this program, the NO x analyzer was checked for interference using the following gases:

Gas Concentration
Carbon Monoxide 500 ± 50 ppm Oxygen 20.9 ± 1 percent
Carbon Dioxide 10 ± 1 percent

Corrections to the measurement system or analyz er were made if the performance specifications

were not met.L2008-371 24 4.3.6 NO 2 to NO Conversion Efficiency

The NO 2 to NO converter check was conducted at the beginning and at the end of each measurement day by the NO bag dilution pro cedure in Section 16.2.2.2 of EPA Method 7E.

4.4 ONSITE SAMPLING ACTIVITIES

Onsite sampling activities included the emissions testing of the previously mentioned outlet stacks and collection of operational data.

4.4.1 EPA Methods 1 and 2 for Velocity Measurements and Cyclonic Flow

Velocity traverses were conducted on the outle t stacks with an S-type pitot assembly in
accordance with EPA Reference Methods 1 and 2. An S-type pitot tube with an attached
inclined manometer was used to measure the exha ust velocities from the sampling location. An attached Type-K thermocouple with remote digita l display was used to determine the flue gas temperature. During the test program, velocity measurements were conducted during each EPA Methods 5 and 201A/202 sampling test runs. The required number of velocity measurements points for each sampling location was determined following EPA Method 1.

Cyclonic flow checks were conducted at the samp ling location in accordance with Section 2.4 of EPA Method 1. This procedure is referred to as the nulling technique. An S-type pitot tube
connected to an inclined manometer was used in this method. The pitot tube was positioned at each traverse point so that the face openings of the pitot tube were perp endicular to the stack cross-sectional plane. Th is position is called the "0 ° reference". The velocity pressure ( Δ P)
measurement was noted. If the Δ P reading was zero, the cycloni c angle was recorded as 0 ° . If
the Δ P reading was not zero, the pitot tube was ro tated clockwise or counter clockwise until the
Δ P reading became zero. This angle was then measur ed with a leveled protractor and reported to the nearest degree. After this null technique was applied at each traverse point, the average of the cyclonic angles was calculated. If this average was less than 20 ° , the flow condition was acceptable to test.L2008-371 25 4.4.2 EPA Method 4 for Moisture Determination

Moisture was determined for each test run according to EPA Reference Method 4,

" Determination of Moisture Content in Stack Gases ". The principle of this method is to remove the moisture from the sample stream and determine moisture either volumetrically or gravimetrically. Sampling was conducted in co njunction with the particulate matter and/or mercury emissions sampling test runs.

4.4.3 EPA Method 5 for Particulate Matter

The emissions of particulate matter (PM) we re determined according to EPA Method 5,

" Determination of Particulate Emissions from Stationary Sources " (40 CFR Part 60 Appendix A).

The sampling train consisted of a glass or stai nless steel button-hook nozzl e, glass lined probe, filter assembly and impinger train. A thermocouple and S-type pitot tube were attached to the probe for the measurement of gas temperature a nd velocity. The sample gas passed through the probe assembly to the heated glass filter holder assembly containing a quartz fiber filter and a
Teflon ® frit support. The filter holder was maintain ed at 248oF ± 25oF throughout each test run. Downstream of the heated filter, the sample gas passed through a series of four ice-cooled impingers kept below 68oF to enable condens ation of entrained moisture. The first two impingers each contained 100 mL of deionized wa ter. The third was empty and the fourth impinger contained a preweighed amount of silica gel. The impingers were followed by a dry gas meter, pump, and a calibrated orifice meter. A schematic diagram of the sampling train is presented in Figure 4-1.

Leak checks of the entire Method 5 sampling tr ain were performed before and after each sampling run. All leak checks and leakage rates we re documented on the relevant field test data sheets. The acceptance criterion for th e Method 5 train was a leak rate of ≤ 0.02 cfm at the highest vacuum obtained during the te st run. Sampling was isokinetic ( ± 10 percent) with readings of flue gas parameters recorded at each sampling point during the traverse.L2008-371 26 Following the completion of each test run, the Met hod 5 train was transported to a recovery area onsite and the recovery sequence proceeded as follows:

● Removed the sampling train to the recovery area.

● Noted the condition of the train (i.e., filter condition, impinger contents color, silica gel color, etc.).

● Disassembled the filter housing and transferred the filter to its original petri dish. Sealed the container with Teflon ® tape and labeled it with the appropriate sample information.

● The front half of the train, nozzle, pr obe, and front-half filter housing were brushrinsed with acetone into an ambe r glass container with a Teflon ® -lined cap. The rinse procedure was performed three times after which the container was sealed and labeled.

● The contents of the first three impingers were measured for volume and the contents discarded.

● The silica gel was returned to its origin al container and weighed to obtain a final weight.

● All containers were checked to ensure proper sealing, proper labeling, and that all liquid levels were marked.

● All samples were logged onto a chain-of-custody form.

The filter and front-half rinse were used to determine PM concentrations. The impinger catches (impingers 1 thru 4) were used to determine moisture.

The Method 5 train produced the following samples:

● Container No. 1 - Filter

● Container No. 2 - Front-Half Acetone Rinse

4.4.4 EPA Methods 201A/202 for Particulate Matter (PM)/PM 10 and Condensibles

Particulate matter (PM), particulate matter equal to or less than an aerodynamic diameter of nominally 10 μm (PM 10 ) and condensible PM were determined according to EPA Method 201A,L2008-371 27 “ Determination of PM 10 Emissions (Constant Sa mpling Rate Procedure) ” (40 CFR Part 60 Appendix A) and Method 202, “Determination of Condensible Particulate Emissions from Stationary Sources” (40 CFR Part 51, Appendix M). Sampling was conducted for three 180
minute test runs.

The sampling train consisted of a pre-cutter nozzle, an in-stack sizing device (cyclone), an instack filter, a heated glass probe with a S-type Pitot tube attach ed, four chilled impingers, and a metering console. A schematic of the sa mpling train is presented in Figure 4-2.

The particulate with an aerodynamic size of ≤ 10 microns (PM 10 ) was collected using an Anderson 280 Series cyclone followed by a 63 mm Whatman EPM2000 glass fiber filter. The Anderson cyclone and 63 mm filter was pre-heated prior to sampling. The first three impingers
contained 100 mL of HPLC Gr ade deionized, distilled (DI) wa ter. The fourth impinger contained a preweighed amount of silica gel. The impingers were followed by a dry gas meter, pump, and a calibrated orifice meter. Initial weights for all impingers were determined gravimetrically prior to the run.

Sampling was isokinetic ( ± 10 percent) with readings of flue gas parameters recorded at every sampling point during the traverse.

Leak checks of the entire Method 201A/202 sampling train were performed before and after each sampling run. All leak checks and leakage rates we re documented on the relevant field test data sheets. The acceptance criterion for the Me thod 201A/202 train is a leak rate of ≤ 0.02 cfm at the highest vacuum obtai ned during the test run.

Following the completion of each test run, th e Method 201A/202 train was transported to a recovery area onsite. The pre-cutter nozzle/cyclone, probe, and filter were removed and the impinger contents were purged for 60 minutes @20 liters per minut e with nitrogen (N 2 ) to remove dissolved sulfur dioxide (SO 2 ) gases and the recovery sequence proceeded as follows:

● Note the condition of the train (i.e., filter condition, impinger contents color, silica gel color, etc.).L2008-371 28 ● The pre-cutter and cyclone was brush-ri nsed with acetone into an amber glass container with a Teflon ® -lined cap. The rinse procedure was performed three times after which the container was sealed and labeled.

● The filter housing was dissembled, and the filter was transferred to its original petri dish. The containe r was sealed with Teflon ® tape and labeled with the appropriate sample information.

● The front half of the filter holder was rins ed with acetone and the rinse was placed into a separate sample containe r which was sealed and labeled.

● The post weight of the impingers were de termined and the contents of the first three impingers were collected in an amber glass container with a Teflon ® -lined cap. The silica gel was returned to its original container.

● The back half of the filter holder, pr obe, impingers, and connecting glassware were rinsed twice with water and placed into the same sample container as the impinger contents.

● The back-half of the filter holder, probe, impingers, and connecting glassware were rinsed three times with methylene chloride (MeCl 2 ) into a separate amber glass container with a Teflon ® -lined cap.

● All containers were checked to ensure proper sealing, proper labeling, and that all liquid levels were marked.

● All samples were logged onto a chain-of-custody form.

The filter, front, and back-half rinses were used to determine PM concentrations. The impinger catches (impingers 1 thru 4) were also used to determine moisture and condensable material.

The Method 201A/202 train produced the following samples:

● Container No. 1 - Filter

● Container No. 2 - Front-Half Acetone Rinse (Cyclone)

● Container No. 3 - Impinger Catches

● Container No. 4 - Back-Half Methylene Chloride RinseL2008-371 29 4.4.5 EPA Method 9 for Opac ity/Visible Emissions

Three 6-minute runs were conducted on each appli cable source for visible emissions utilizing EPA Method 9, “Visual Determination of the Opacity of Emissions from Stationary Sources”.

The applicable sources tested were the following:

• System 1 – Ore Handling System;

• System 2 – Crushing Circuit;

• System 3 – Screening System;

• System 4A – Radial Stacker System (Alternative Operating Scenario);

• System 7 – Baghouse #2 Material Handling System;

• System 8 – Baghouse #4 Material Handling System; and

• System 13A (S2.012A) – Carbon Kiln Combustion Exhaust.

Visible emissions tests were conduc ted concurrent with the PM/PM 10 test runs for Systems 2 and
3.

A certified Method 9 observer conducted these tests during the compliance testing.

4.4.6 Continuous Emissions Monitoring for O 2 , CO 2 , NO x , and CO

TRC conducted a series of three 1-hour test runs using EPA Me thods. Emissions testing were conducted for oxygen (EPA Method 3A), carbon di oxide (EPA Method 3A), oxides of nitrogen (EPA Method 7E), and carbon dioxide (EPA Met hod 10) for the applicable Systems. Single point sampling was conducted.

The applicable source tested was the following:

• System 13A (S2.012A) – Carbon Kiln Combustion Exhaust.

The CEM system sampling was conducted at a single point located at the centroid of the stack. The CEMS sampling train started with a stainles s-steel sampling probe. The sample stream wasL2008-371 30 then drawn through a glass fiber filter, heated (248 ° F ± 25 ° F) Teflon ® sample line, and a sample conditioner to remove the moisture and particulat e from the gas stream. The sample was then drawn through Teflon ® tubing by a leak-free Teflon ® double diaphragm pump to a stainless-steel sample manifold with and atmos pheric by-pass rotometer. The O 2 , CO 2 , NO x , and CO analyzers withdrew samples from this manifold.

All CEMS data was recorded as averages by a di gital data logger design ed to receive and log instrument signals. The result s were expressed in ppm for NO x and CO and in percent for O 2 and CO 2 .

4.4.7 EPA Method 29 for Mercury Emissions

Mercury (Hg) was determined via EPA Method 29 “Metals Emissions from Stationary Sources”.

The applicable sources tested were the following:

• Carbon Kiln Drum System; and

• Deep Bed Carbon Scrubber.

The sampling train utilized the EPA Method 29 sa mpling configuration and consisted of a quartz button-hook nozzle, quartz lined heated probe, a nd heated filter housing. A thermocouple and Stype pitot tube were attached to the probe for the measurement of gas temperature and velocity.

The sample gas passed through the probe and fi lter assembly which was connected to an impinger train. The impinger train consisted of a series of six-ice bath cooled impingers, kept
below 68 ° F to enable condensation of entrained mois ture and the gaseous mercury species. The first and second impingers each contained 100 mL of a 5% HNO 3 /10% H 2 O 2 solution. The third impinger was empty to separate the two chemical solutions. The fourth and fifth impingers each
contained 100 mL of a 4% KMnO 4 /10% H 2 SO 4 solution. The sixth impinger contained 200 - 400 grams of silica gel. All filled impingers were weighed prior to placing th e impingers in the train. The impingers were followed by a leak free pump, dry gas meter, and calibrated orifice meter. The second and fourth impingers were the modified Greenburg design. The first, third, fifth andL2008-371 31 sixth impingers were the standard Greenburg Smith impingers. No silicone grease was used in
the train.

TRC conducted three EPA Method 29 test runs on each source, with each test run having a
duration of 120 minutes. Sampling was isokinetic ( ± 10%) with all stacks and train operating parameters recorded at each sampling point.

Leak checks of the entire EPA Method 29 sampli ng train were performed before and after each sampling run. All leak checks and leakage rates we re documented on the relevant field test data sheets. The acceptance criterion was a post run leak rate of ≤ 0.02 cfm at the highest vacuum obtained during the test run. The pre run leak check criterion was ≤ 0.02 cfm at 15 in. Hg.

Following the completion of each test run, th e EPA Method 29 train was transported to a recovery area onsite. The sample recovery sequence was as follows:

• All openings on the probe, inlet to cyclone/or filter holder an d impingers were sealed with Teflon ® tape.

• The sampling train was removed to the recovery area.

• The condition of the train was noted (i.e., filter, impinger contents colo r, silica gel color, etc.).

• Container No. 1 - Disassembled the filter housin g and transferred the filter to its original glass petri dish. Sealed the petri dish with Teflon ® tape and labeled it with the appropriate sample information. Any filter fibers adhering to the support gasket were transferred to the petri dish.

• Container No. 2A - The front half of the train, nozzle, probe, and front-half filter housing, cyclone and flask were brush-rinsed with 100 mL of acetone into an amber glass container with a Teflon ® -lined cap. The container was sealed and labeled.

• Container No. 2B - The front ha lf of the train, nozzle, probe , and front-half filter housing, cyclone and flask were brush-rinsed with 100 mL of 0.1N nitric acid into an amber glass container with a Teflon ® -lined cap. The containe r was sealed and labeled.

• Container No. 3 - The contents of the two 5% HNO 3 /10% H 2 O 2 impingers were weighed. The filter support, backhalf of the filter holde r and connecting glassware were rinsed three times with 100 mL of 0.1N HNO 3 into a glass amber container with a Teflon ® lined cap.L2008-371 32 The impingers and connecting glassware were rinsed with 0.1N HNO 3 . The container was sealed and labeled.

• Container No. 4 - The contents of the third im pinger were weighed and transferred to a glass amber container with a Teflon ® -lined cap. The impinger and U-tubes were rinsed three times with a 100 mL portion of 0.1N nitric acid into a sample c ontainer. The container was sealed and labeled.

• Container No. 5 (Impingers 4 and 5, H 2 SO 4 /KMnO 4 Impinger Contents and Rinses) - Dried the exterior surfaces of Impinge rs 4 and 5, then weighed and recorded the weight of each impinger (to the nearest 0.5 g). Poured all of the liquid from the two H 2 SO 4 -KMnO 4 impingers into a glass sample, Container 5. Rinsed the impingers and connecting glassware three times with a tota l of 100 mL of fresh H 2 SO 4 /KMnO 4 solution and poured into Container 5. Similarly, rinsed the impingers and connecting glasswar e three times with 100 mL of DI water. Added these rinses to Cont ainer 5. The container wa s sealed and labeled.

• Container No. 6 - Rinsed the contents of im pingers 4 and 5 and conn ecting glassware with 25 mL of 8N HCl and transferred the rinsate into Container 6 filled with 200 mL of DI water. The container was sealed and labeled.

• The silica gel impinger was weighed to obtain a final weight.

• All containers were checked to ensure prope r sealing, proper labeli ng, and that all liquid levels were marked. All samples were logged onto a chain-of-custody record.

The EPA Method 29 train produced the following samples:

• Container No. 1 - Filter

• Container No. 2A - Front-Half Acetone Rinse (for PM bound Hg determination)

• Container No. 2B - Front-Half 0.1N HNO 3 Rinse

• Container No. 3 - Impingers 1 and 2 - 5% HNO 3 /10% H 2 O 2 Impingers Catch & Rinse

• Container No. 4 - Impinger 3 - Impinger Catch & Rinse

• Container No. 5 - Impingers 4 and 5 - H 2 SO 4 /KMnO 4 Impingers Catch & Rinse

• Container No. 6 - Impingers 4 and 5 - 8N HCl RinseL2008-37133FIGURE 4-1. Schematic Diagram of EPA Method 5 Particulate Matter Sampling TrainL2008-37134FIGURE 4-2. Schematic Diagram ofEPA Method 201A/202 Sampling TrainL2008-371 35 4.5 PRODUCTION SAMPLE COLLECTION

Marigold facility person nel collected a series of production samples during the test program and analyzed them for mercury using a Nevada Certified Laboratory a nd 7471 testing methodology. Marigold collected samples as follows:

• Carbon Kiln Mercury Testing - The carbon kiln is a batch pr ocess. The carbon loaded into the feed hopper was sampled. Two samp les were taken depending on the amount of
carbon loaded into the feed hopper.

• Deep Bed Scrubber - The Deep Bed Scrubber provides mercury emission control for the smelting furnace, retort, pregnant and barren tanks, and electrowinning cells (3).

o Smelting furnace – the smelting furnace is a batch process and one sample representative of the material charge fo r the entire testing period was collected.

o Retort – the retort is a batch process and one sample representing the batch was
collected.

o Pregnant and Barren Tanks – No samples collected.

o Electrowinning Cells (3) – No samples collected.

The sample results were collected by Marigold, provided to TRC, and included as Appendix C of this report.

4.6 PROCESS MONITORING

Marigold facility personnel monitored and recorded the following during each test run;

Crushing Circuit – tons of material pr ocessed and hours operated.
Carbon Kiln – tons of material processed, hour s of operation, propane consumption.
Retort – tons of material processed and hours of operation. Smelting furnace – tons of material pro cessed and hours of operation. Pregnant and Barren Tanks – verify that they are operating. Electrowinning Cells (3) – verify that they are operating.L2008-371 36 The process monitoring data was collected by Ma rigold, provided to TRC, and included as Appendix C of this report.L2008-371 37 5.0 ANALYTICAL PROCEDURE S AND CALCULATIONS

This section delineates the analytical procedures and calculations that were used by TRC during the Compliance Test Program.

5.1 ANALYTICAL PROCEDURES

5.1.1 Particulate Matter from Method 5 Sampling Train

Particulate Matter sampling analysis was acco mplished by following the procedures in EPA Method 5, and the analyses were conducted by TRC.

The glass fiber filters were desiccated to a constant weight and were placed in glass petri dishes
and sealed with Teflon ® tape prior to testing. An identif ication label was placed on the petri dish. The beakers used for the dry down of th e acetone rinse were cleane d and dried in and an
oven at 250 ° F. The containers were desicc ated to a constant weight.

The filter was desiccated and weighed to consta nt weight. The front-half acetone rinse was air
dried in a tared container and then desiccated and weighed to a constant we ight. The sum of the net weights for the probe wash a nd filter catch were used to calculate the concentration of filterable particulate matter. The net weights fo r the filterable particulate fraction were reported as concentrations in milligrams (mg) and gr ains per dry standard cubic foot (gr/dscf).

5.1.2 Particulate Matter from Method 201A/202 Sampling Train

Particulate matter and particulate matter concentra tions equal to or less than an aerodynamic diameter of nominally 10 μm (PM 10 ) sampling were accomplished by following the procedures
in EPA Method 201A/202. Particulate ma tter analysis was conducted by TRC.

The glass fiber filters were desiccated to a consta nt weight and placed in glass petri dishes and
sealed with Teflon ® tape prior to testing. An identification label was placed on the petri dish. The beakers used for the dry down of the acetone rinse were cleaned and dried in and an oven at
225oF. The beakers were desic cated to a constant weight.L2008-371 38 The front-half acetone rinse was air dried in a tared container and th en desiccated and weighed to a constant weight. The filter was desiccated and weighed to constant weight. The sum of the net weights for the probe wash and filter catch were us ed to calculate the concentration of filterable particulate matter. The net weights for the f ilterable particulate fraction were reported as concentration in grains per dry standard cubic f oot (gr/dscf) and emission rate in pounds per hour (lbs/hr).

The back-half DI water reagent and the back-half MeCl 2 rinses were combined and extracted
with MeCl 2 to separate the organic a nd inorganic fractions. The or ganic and inorganic fractions were desiccated and weighed to a constant weig ht. The organic and inorganic fractions were reported as concentration in grains per dry sta ndard cubic foot (gr/dscf ) and emission rate in pounds per hour (lbs/hr). The sum of the organi c and inorganic fractions was reported as the total condensable particulate. The sum of the filterable and conde nsable particulate fractions was reported as the total PM 10 .

5.1.3 Particulate Matter and Mercury from Method 29 Sampling Train

At the conclusion of the field effort TRC p ackaged the mercury (EPA Method 29) emission samples and provided delivery to the analytical laboratory. Sample Container nos. 1 (quartz filter) and 2A (front half acetone rinse) were first analyzed at TRC’s laboratory in accordance
with section 5.1.1 to determine the amount of particulate matter collect ed in the front half of the Method 29 sampling train. The filter, front-half acetone rinse dry-down container and remaining sample containers (nos. 2B through 6) were shipped to the TRC’s subcontract analytical laboratory, Test America, locate d in West Sacramento, Califor nia for mercury determination.

5.2 CALCULATIONS

5.2.1 Flow Rates and Isokinetics

Time = T Dry Gas Meter, ft 3 = VM Pitot ∆ P, in. H 2 O = ∆ PL2008-371 39 Orifice ∆ H, in. H 2 O = PM Dry Gas Temp In, oF = TMI Dry Gas Temp Out, oF = TMO Stack Static Pressure, in. H 2 O = PST Stack Temp, oF = TS
1. DN = Nozzle Diameter, inches
2. PB = Barometric Pressure, inches Hg
3. TT = Net Sampling Time, minutes
4. VM = VM final - VM initial = Sample Gas Volume, ft 3
4A. VML = Use only if any final or intermediate leak check rate is over 0.02 cfm
LI = Leak rate after any given sampling period, cfm TLI = Total time of sample period in which leak occurred, minutes VML = VM - [(L1 - 0.02) TLI + (L2 - 0.02) TL2 + (L3 - 0.02) TL3 + (L4 - 0.02) TL4]
5. Average Dry Gas Temperature at meter, oF

TM = Average TMI + Average TMO 2
6. Average Orifice Pressure Drop, inches Hg
PM = Average ∆ H, in. H 2 O 13.6
7. Volume of dry gas sampled at standard conditions, dscf a
VMSTD = 528 × (Y) × (VM) × (PB + PM) 29.92 × (TM + 460)
Y = dry gas meter calibration factor

8. Total Water Collected
VW = gm H 2 O silica gel + gm impinger H 2 O

Note: If ml H 2 O is measured - (ml × 0.9982 gm/ml)
9. Volume of water vapor at standard conditions, scf bL2008-371 40 VW gas = 0.04715 × VW
10. Percent moisture in stack gas
100 × VW gas % M = VMSTD + VW gas
11. Mole Fraction of dry gas (dimensionless)

100 - %M MD = 100

12. Molecular weight of dry stack gas
MWD = (% CO 2 × 0.44) + (% O 2 × 0.32) + [(% CO + % N 2 ) × 0.28]

12a. % Excess Air
%EA = [(% O 2 ) - 0.5 × (% CO)] × 100 [(0.264) × (% N 2 )] - (% O 2 ) + 0.5 × (% CO)
13. Molecular Weight of wet stack gas
MW = (MWD × MD) + 18 × (1 - MD)
14. AS = Stack Area, square inches

Circular = π 2
2 diameter stack ⎟ ⎠ ⎞ ⎜ ⎝ ⎛

Rectangular = Length × Width
15. PS = Stack Pressure, absolute, inches Hg = PB ± Avg PST
PST = Stack static pressure

PST = PST in. H 2 O 13.6

PS = PB ± Average PST

16. TS avg = Average Stack TemperatureL2008-371 41 17. SDE avg = 

# ( ) 460 TS P avg + × Δ avg 18. Stack gas velocity at stack conditions, afpm

VS = 2 / 1

avg c MW PS 1 SDE Cp 5130 ⎥ ⎦ ⎤ ⎢ ⎣ ⎡

× × × × Cp = pitot tube coefficient
19. Stack gas volumetric flow rate at stack conditions, acfm d

Q a = VS × AS 144
20. Stack gas volumetric flow rate at standard conditions, dscfm e
Q s = Q a × 528 × MD × PS (29.92) × (TS avg + 460)

21. Percent Isokinetics

%ISO = 1039 f × (TS avg + 460) × VMSTD VS × TT × PS × MD × (DN) 2

a = Dry standard cubic feet at 68oF (528oR) and 29.92 in. Hg b = Standard conditions at 68oF (528oR) and 29.92 in.Hg

c = 5130 = 

## ( ) ( ) ( )( ) min sec/ 60 O H in. R Hg in. mole

- lb/lb

sec ft 85.5

2 × ⎥ ⎦ ⎤ ⎢ ⎣ ⎡

× ° ×

d = Actual cubic feet per minute

e = Dry standard cubic feet per minute at 68oF (528oR) and 29.92 in.Hg f = 1039 = 29.92 in. Hg 144 in. 2 4 528oR × ft 2 × π × 100

5.2.2 Grains Per Dry Standard Cubic Foot

Particulate matter rates in terms of grains per dr y standard cubic feet (gr/dscf) were calculated using the pollutant rate in terms of milligrams (mg) divided by the volume of gas collected (dscf).

gr/dscf = 

## ( ) ( ) ( ) ( ) ⎥ ⎦ ⎤ ⎢ ⎣ ⎡ ⎭ ⎬ ⎫ ⎩ ⎨ ⎧

+ × + × × × ÷ × 460 TM 29.92 PM PB VM Y 528 mg 0.0154L2008-371 42 where:
dscf = Dry standard cubic feet at 68oF (528oR) and 29.92 inches Hg 0.0154 = 0.0154 grains per milligram Y = Dry gas meter calibration factor VM = Volume metered, ft 3 PB = Barometric Pressure, inches Hg PM = Average Orifice Pressure Drop, inches Hg (Avg. Δ H inches H 2 O ) 13.6) TM = Average Dry Gas Temperature at Meter, oF

5.2.3 Pounds Per Hour – Particulate Matter and Mercury

Emission rates in terms of pounds per hour (lbs/hr) were calculated using the particulate matter and mercury concentrations in terms of grains pe r dry standard cubic feet (gr/dscf), flowrate - dscfm (Qs), 60 minutes/hour, divided by 7,000 grains per pound (gr/lb).

lbs/hr = gr/dscf × Qs × 60 7000

5.2.4 Pounds Per Hour – Nitrogen Oxides (NO x ) and Carbon Monoxide (CO)

Emission rates in terms of pounds per hour (lbs/hr) for NO x and CO were calculated using the pollutant concentrations in terms of parts per million (ppm/dry volume), flowrate - dscfm (Qs), molecular weight of the pollutant (M W), 60 minutes/hour, divided by 385.3 × 10 6 dscf/lb-mole @ 68oF (20oC).

lbs/hr = ppm × Qs × MW × 60 385.3 × 10 6

where:

NO x molecular weight = 46 CO molecular weight = 28L2008-371 43 6.0 QUALITY ASSURANCE

6.1 OVERVIEW

TRC management is fully committed to an effect ive Quality Assurance/Quality Control Program whose objective is the delivery of a quality product. For much of TRC's work, that product is data resulting from field measurements, sa mpling and analysis ac tivities, engineering assessments, and the analysis of gathered data for planning purposes. The Quality Assurance Program works to provide complete, precise, accurat e, representative data in a timely manner for each project, considering both the project's needs and budget constraints.

This section highlights the specific QA/QC procedures followed for this Test Program.

6.2 FIELD QUALITY CONTROL SUMMARY

6.2.1 Calibration Procedures

Calibrations of the field sampling equipment were performed prior to the field sampling effort. Copies of the calibration sheets were submitted to th e field team leader to take onsite and for the project file. Calibrations were performed as describe d in the EPA publications " Quality Assurance Handbook for Air Pollution Measuremen t Systems; Volume III - Stationary Source Specific Methods " (EPA-600/4-77-027b) , EPA 600-R4- 038C, EPA 40 CFR Part 60 Appendix A, and 40 CFR Part 51 Appendix M. Equipm ent calibrated included the sample metering system, thermocouples, and pitot tube s. All calibrations were availabl e for review at the test site. Copies of the equipment calibration forms are contained in Appendix E.

6.2.2 Equipment Leak Checks

Prior to sampling, each Method 5, Methods 201A/202, and EPA Method 29 sampling train was leak checked according to the procedures outlin ed in EPA Reference Method 5. During the course of a test run, a leak check was conducted be fore and after every test, or if replacement of a component became necessary. Final leak chec ks were performed to ensure that no leaksL2008-371 44 developed in the train during the course of the te st run. All leakage ra tes, if any found, were recorded on the appropriate field data sheet.

6.2.3 Cyclonic Flow Check

The absence of cyclonic flow within the sampli ng location was verified prior to sampling in
accordance with Section 2.4 of EPA Method 1.

6.2.4 Calibration Gases

All calibration gases used to conduct instrument calibrations were prepared in accordance with the EPA Protocol 1, and are traceable to NIST.

6.2.5 Instrument Calibrations

All instrument calibrations met the performan ce criteria defined in 40 CFR 60 Appendix A, Methods 3A, 7E, and 10. Any test not meeting these criteria was consid ered questionable and the test run repeated.

6.3 DATA REDUCTION, VALI DATION, AND REPORTING

Specific QC measures were used to ensure the generation of reliable data from sampling activities. Proper collection and organization of accurate information followed by clear and concise reporting of the data is a primary goal in all projects.

6.3.1 Field Data Reduction

The field sampling data sheets are presented in A ppendix A. The data collected was reviewed in the field by the Field Team Leader and at leas t one other field crew member. Errors or discrepancies, if any, were noted in the field book.L2008-371 45 6.3.2 Data Validation

TRC supervisory and QC personnel use validation me thods and criteria appropriate to the type of data and the purpose of the measurement. Record s of all data were maintained, including that judged to be an "outlying" or s purious value. The persons who va lidated the data have sufficient knowledge of the technical work to identify questionable values.

Field sampling data were validated by the Field Team Leader and/or the QC Coordinator based on their review of the adherence to an approved sampling protocol and written sample collection procedure.

The following criteria were used to evaluate the field sampling data:

● Use of approved test procedures;

● Proper operation of the process being tested;

● Use of properly operating and calibrated equipment;

● Leak checks conducted before and after tests; and

● Proper chain-of-custody maintained.

The criteria listed below were used to evaluate the analytical data:

● Use of approved analytical procedures;

● Use of properly operating and calibrated instrumentation; and

● Acceptable results from analyses of QC samples (i.e., the reported values should fall within the 95 percent confidence interval for these samples).

6.3.3 Data Reporting

All data has been reported in standard units depending on the measurement and the ultimate use
of the data. The bulk of the data was co mputer processed and reported as follows:L2008-371 46 • Exhaust Gas Stream - Gas Properties: a. Moisture, dscf and percent by volume b. Flow rate, dscfm and acfm c. Pressure, in. of Hg d. Temperature, ° F

- Gas Diluents and Pollutants a. O 2 , percent b. CO 2 , percent
c. NO x , ppm, and lb/hr d. CO, ppm, and lb/hr

e. Hg, gr/dscf , and lbs/hr f. PM and PM 10 , gr/dscf, and lbs/hr g. Opacity, %

6.4 EXCEPTIONS

No deviations from the approved test plan were required for the completion of the test program.