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 2008
TRC Project No. 159240 

August 2008 

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 

(702) 437-5800 

DISCLAIMER

This document is intended for use solely by Marigold Mining Company (Marigold Mining) for the specific purposes 

described in the contractual documents between TRC Companies, Inc. (TRC) and 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 and conclusions contained in the document have been prepared in accordance with 

the work statement and contract terms and conditions. The document may be subject 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 liability to persons other than Marigold 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 CHANGES AND PROBLEMS............................................................... 6 

2.3 PRESENTATION OF RESULTS .................................................................................. 6 

2.3.1 System 13A Carbon Kiln Combustion 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................................................................................................................ 15 

3.2.2 System 2................................................................................................................ 15 

3.2.3 System 3................................................................................................................ 16 

3.2.4 System 4A............................................................................................................. 16 

3.2.5 System 7................................................................................................................ 16 

3.2.6 System 8................................................................................................................ 16 

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 O2, CO2, NOx, and CO ............................ 21 

4.3.5 Interference Gas Test ............................................................................................ 23 

4.3.6 NO2 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 Particulate Matter (PM)/PM10 and Condensibles ... 26 

4.4.5 EPA Method 9 for Opacity/Visible Emissions ..................................................... 29 

4.4.6 Continuous Emissions Monitoring for O2, CO2, NOx, and CO ............................ 29 
TABLE 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 PROCEDURES 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 – Particulate Matter and Mercury............................................. 42 

5.2.4 Pounds Per Hour – Nitrogen Oxides (NOx) 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, VALIDATION, 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 Data 
TABLE OF CONTENTS, continued 

L2008-371 ii 

TABLES 

Number Page

1-1 Compliance Emissions Test Program Overview .................................................................4 

2-1 Summary of Results for Carbon 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 System 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.....................................34 
L2008-371 1 

1.0 INTRODUCTION 

1.1 OVERVIEW 

Pursuant to the requirements of the Nevada Mercury Control Program regulated by the State of 

Nevada Department of Conservation and Natural Resources, Division of Environmental 

Protection (NDEP), Bureau of Air Pollution Control, 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 Valmy, Nevada. Additionally, 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 program. TRC supported and managed the test 

program from the Las Vegas, Nevada office. TRC prepared and received approval of the testing 

protocol to satisfy the testing requirements stipulated in the operating permit. The purpose of the 

testing was to: 

System 1 – Ore Handling System 

- Determine compliance with visible emission standard limitations of the operating permit 

at an increased throughput. 

System 2 – Crushing Circuit Baghouse #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 (PM10) at an increased 

throughput; and 

- Determine compliance with visible emission standard limitations of the operating permit 

at an increased throughput. 

System 3 – Screening System Baghouse #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 (PM10) at an increased 

throughput; and 

- Determine compliance with visible emission standard limitations of the operating permit 
L2008-371 2 

at an increased throughput. 

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

- Determine compliance with visible emission standard limitations of the operating permit 

at an increased throughput. 

System 7 – Baghouse #2 Material Handling System 

- Determine compliance with visible emission standard limitations of the operating permit 

at an increased throughput. 

System 8 – Baghouse #4 Material Handling System 

- Determine compliance with visible emission standard limitations of the operating permit 

at an increased throughput. 

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

- Determine the emission rate of nitrogen oxides (NOx) and carbon monoxide (CO) in 

regards to limits in the operating permit at an increased throughput.

- Determine compliance with visible emission standard 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 for the sources controlled by the Deep Bed 

Carbon Scrubber. 

Sampling and analysis procedures described in this document were conducted using procedures 

deemed acceptable by the NDEP. TRC was responsible for the collection and analysis of all flue 
L2008-371 3 

gas samples. 

1.2 SCOPE OF WORK 

The purpose of the test program was to determine 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 EMISSIONS 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/PM10 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/PM10 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 60 
L2008-371 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 methods 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/PM10 
L2008-371 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 (NOx) and carbon monoxide (CO) at elevated 

throughput for the Carbon Kiln Combustion Exhaust Stack; 

• Obtain emission rate of particulate matter (PM) and particulate matter equal to or less 

than an aerodynamic diameter of nominally 10 μm (PM10) at elevated throughput for the 

System 2 Crushing Circuit Baghouse #2, and the 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 Handling Baghouse #4, and the System 13A 

Carbon Kiln Combustion Exhaust; and 

• Establish mercury emission rates for the Carbon Kiln Drum Exhaust and the Deep Bed 

Carbon Scrubber Outlet (one operating scenario). 

2.2 FIELD TEST CHANGES 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 was conducted on June 10, 2008. Triplicate test 

runs were conducted at the exhaust stack for nitrogen oxides (NOx) and carbon monoxide (CO) 

in accordance with EPA Methods 7E and 10, respectively. In addition, triplicate test runs were 

conducted for visible emissions (opacity) in accordance with EPA Method 9. A summary of the 

test results is presented 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 was 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 was conducted under one operating scenario on 

June 11, 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 2-3. 

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 conducted at the exhaust stack for PM/PM10 in accordance with 

EPA Methods 5 and 201A/202. In addition, triplicate test runs were conducted for visible 

emissions (opacity) concurrent with the PM/PM10 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 conducted at the exhaust stack for PM/PM10 in accordance with 

EPA Methods 5 and 201A/202. In addition, triplicate test runs were conducted for visible 

emissions (opacity) concurrent with the PM/PM10 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 conducted for visible emissions (opacity) on June 19, 2008 for System 1 

Ore Handling, System 4A Radial Stacker, and Systems 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, 2008
Source/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 Outlet
Source/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, 2008
Source/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 #2
Source/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 #4
Source/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, 2008
L2008-371 15 

3.0 PROCESS DESCRIPTION 

3.1 INTRODUCTION 

Marigold Mining Company operates a gold producing mine on property located four miles south 

of I-80 (Exit 216) in Valmy, Nevada. There are several processing facilities located on the 

property which separate the gold from 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 velocity 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 system 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 (Baghouse #2) with 100% capture and a nominal 

volume flow rate of 4,800 dry standard cubic feet per minute. The exhaust of the baghouse is 

vertical with an internal diameter 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 (Baghouse #4) with 100% capture and a nominal 

volume flow rate of 7,400 dry standard cubic feet per minute. The exhaust of the baghouse is 

vertical with an internal diameter 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 (PF1.004) is controlled by best operating practices. 

3.2.5 System 7 

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

3.2.6 System 8 

The emissions from System 8 emission unit (PF1.010) is controlled by best 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 Manufacturing 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 scrubber/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 Deep 
L2008-371 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 Methods 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 two 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: 

O2, CO2, NOx, CO, PM, and PM10

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 Traverse 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 Particulate Matter Emissions from 

Stationary Sources 
L2008-371 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 Carbon Dioxide Emissions from 

 Stationary Sources (Instrumental Analyzer Procedure) 

• EPA Method 29 Determination of Metals Emissions from Stationary 

Sources 

• EPA Method 201A Determination of PM10 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 Condensible Particulate Emissions from 

Stationary Sources 

4.3 PRESAMPLING ACTIVITIES 

Presampling activities included equipment calibration, precleaning of the sample train glassware, 

and other miscellaneous tasks. Each of these activities are described or referenced in the 

following subsections. Other presampling activities included team meetings, equipment packing, 

and finalization of all details leading up to the coordinated initiation of the sampling program. 

4.3.1 Equipment Calibration 

TRC follows an orderly program of positive actions to prevent the failure of equipment or 

instruments during use. This preventative maintenance and careful calibration helps to ensure 

accurate measurements from field and laboratory instruments. 

Once the equipment had gone through the cleaning and repair process it was then calibrated. All 

equipment that was scheduled for field use was cleaned and checked prior to calibration. Once 
L2008-371 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 step in ensuring the successful 

completion of the field effort. All equipment was inspected for proper operation and durability 

prior to calibration. Calibration of the following equipment were 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 performed prior to the test program. 

• Probe Nozzles (QA Handbook, Vol III, Section 3.4.2, pp. 19) - average three 

internal diameter measurements of the nozzle; difference between high and low  

+ 0.1 mm. Recalibrate, reshape and sharpen when nozzle becomes nicked, dented 

or corroded. 

• Pitot tubes (QA Handbook Vol III, Section 3.1.2, pp. 1-13) - measured for 

appropriate spacing and dimensions or calibrated 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, Method 5) - calibrated against a critical 

 orifice. Acceptance criteria - pretest Yi = Y = + 0.02; post test Y = + 0.05 Yi. 

• Orifice meter calibrated against a wet test meter. Acceptance criteria is ∆H@i = 

 + 0.2 from the average value. 

• Field barometer (EPA Method 2) – compared against a mercury-in-glass 

barometer or use Airport Station BP and 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 manufacturer recalibrate or adjust. 

4.3.2 Glassware Preparation 

Sample train glassware requires specialized precleaning to avoid contamination of the sample 
L2008-371 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 followed 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 the 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 was 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 O2, CO2, NOx, and CO 

TRC conducted continuous emissions monitoring 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 and operation of its Transportable Continuous Emissions 

Monitoring System (TCEMS). 

The TCEMS consisted of three subsystems: sample acquisition/conditioning, sample analysis, 

and a data acquisition system. Sample acquisition/conditioning is designed to deliver a 

representative sample of the gas stream to the sample analysis subsystem. Since the stream must 

be clean and dry for O2, CO2, NOx, and CO analyzers, a glass fiber filter and noncontact 

moisture condenser were used for particulate and moisture removal. The sample line was heat 

traced to eliminate inline condensation prior to the condenser. 
L2008-371 22 

In each case, accurate interpretation of analyzer response required the systematic calibration of 

the instrument against gases of known concentrations. 

The data acquisition subsystem consisted of a digital data logger designed to receive and log 

instrument signals (raw voltages) at user-defined 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 sample/acquisition system was leak 

checked by the following procedure: 

a. plugged probe; 

b. observed that flow in rotameter 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 methods required calibration of all involved monitors. 

At the beginning of each day, system instrument calibrations for zero and upscale gases were 

performed prior to initiation of testing by system calibration gas injection. System calibrations 

were performed both prior to and following 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. Following completion of the required runs, final 

system calibrations were performed. These procedures allowed for determination of initial and 

final system calibration error, as well as system drift. The calibration gas values and instrument 

range settings are listed in Table 4-1. 

Calibration gases used were EPA Protocol 1, traceable to the National Institute of Standards and 

Technology (NIST). The measurement system performance specifications as stated in 40 CFR 

60 Appendix A, for Methods 3A, 7E, and 10 are listed in Table 4-2 and were the performance 

criteria for this program. 
L2008-371 23 

TABLE 4-1. CALIBRATION GAS VALUES AND INSTRUMENT RANGES 

Analyzer Range Conc. High Mid Low Zero

NOx 0-110 ppm 102.0 51.20 N/A nitrogen 

CO 0 – 100 ppm 101.0 40.10 N/A nitrogen 

CO2 0 – 20 % 17.87 9.81 N/A nitrogen 

O2 0 – 25 % 17.97 10.10 N/A nitrogen 

TABLE 4-2. PERFORMANCE CRITERIA 

Procedure Performance Criteria 

O2/CO2

(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 NOx 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 analyzer were made if the performance specifications 

were not met. 
L2008-371 24 

4.3.6 NO2 to NO Conversion Efficiency 

The NO2 to NO converter check was conducted at the beginning and at the end of each 

measurement day by the NO bag dilution procedure 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 outlet 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 exhaust velocities from the sampling location. An 

attached Type-K thermocouple with remote digital 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 sampling 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 perpendicular to the stack 

cross-sectional plane. This position is called the "0° reference". The velocity pressure (ΔP) 

measurement was noted. If the ΔP reading was zero, the cyclonic angle was recorded as 0°. If 

the ΔP reading was not zero, the pitot tube was rotated clockwise or counter clockwise until the 

ΔP reading became zero. This angle was then measured 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 conjunction 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) were 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 stainless steel button-hook nozzle, 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 and 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 maintained 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 condensation of entrained moisture. The first two 

impingers each contained 100 mL of deionized water. 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 train were performed before and after each 

sampling run. All leak checks and leakage rates were documented on the relevant field test data 

sheets. The acceptance criterion for the Method 5 train was a leak rate of ≤ 0.02 cfm at the 

highest vacuum obtained during the test 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 Method 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, probe, and front-half filter housing were brushrinsed 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 contents of the first three impingers were measured for volume and the 

contents discarded. 

● The silica gel was returned to its original 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)/PM10 and Condensibles 

Particulate matter (PM), particulate matter equal to or less than an aerodynamic diameter of 

nominally 10 μm (PM10) and condensible PM were determined according to EPA Method 201A, 
L2008-371 27 

“Determination of PM10 Emissions (Constant Sampling 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 attached, four chilled impingers, and a 

metering console. A schematic of the sampling train is presented in Figure 4-2. 

The particulate with an aerodynamic size of ≤ 10 microns (PM10) 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 Grade deionized, distilled (DI) water. 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 were documented on the relevant field test data 

sheets. The acceptance criterion for the Method 201A/202 train is a leak rate of ≤ 0.02 cfm at 

the highest vacuum obtained during the test run. 

Following the completion of each test run, the 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 minute with nitrogen (N2) to 

remove dissolved sulfur dioxide (SO2) 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-rinsed 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 container was sealed with Teflon® tape and labeled with the 

appropriate sample information. 

● The front half of the filter holder was rinsed with acetone and the rinse was placed 

into a separate sample container which was sealed and labeled. 

● The post weight of the impingers were determined 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, probe, 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 (MeCl2) 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 Rinse 
L2008-371 29 

4.4.5 EPA Method 9 for Opacity/Visible Emissions 

Three 6-minute runs were conducted on each applicable 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 conducted concurrent with the PM/PM10 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 O2, CO2, NOx, and CO 

TRC conducted a series of three 1-hour test runs using EPA Methods. Emissions testing were 

conducted for oxygen (EPA Method 3A), carbon dioxide (EPA Method 3A), oxides of nitrogen 

(EPA Method 7E), and carbon dioxide (EPA Method 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 stainless-steel sampling probe. The sample stream was 
L2008-371 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 particulate 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 atmospheric by-pass rotometer. The O2, CO2, NOx, and CO analyzers 

withdrew samples from this manifold. 

All CEMS data was recorded as averages by a digital data logger designed to receive and log 

instrument signals. The results were expressed in ppm for NOx and CO and in percent for O2

and CO2. 

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 sampling configuration and consisted of a quartz 

button-hook nozzle, quartz lined heated probe, and 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 filter 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 moisture and the gaseous mercury species. The 

first and second impingers each contained 100 mL of a 5% HNO3/10% H2O2 solution. The third 

impinger was empty to separate the two chemical solutions. The fourth and fifth impingers each 

contained 100 mL of a 4% KMnO4/10% H2SO4 solution. The sixth impinger contained 200 - 400 

grams of silica gel. All filled impingers were weighed prior to placing the 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 and 
L2008-371 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 sampling train were performed before and after each 

sampling run. All leak checks and leakage rates were 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, the 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 and 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 color, silica gel color, 

etc.). 

• Container No. 1 - Disassembled the filter housing 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 half 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 container was sealed and labeled. 

• Container No. 3 - The contents of the two 5% HNO3/10% H2O2 impingers were weighed. 

The filter support, backhalf of the filter holder and connecting glassware were rinsed three 

times with 100 mL of 0.1N HNO3 into a glass amber container with a Teflon® lined cap. 
L2008-371 32 

The impingers and connecting glassware were rinsed with 0.1N HNO3. The container was 

sealed and labeled. 

• Container No. 4 - The contents of the third impinger 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 container. The container was 

sealed and labeled. 

• Container No. 5 (Impingers 4 and 5, H2SO4/KMnO4 Impinger Contents and Rinses) - Dried 

the exterior surfaces of Impingers 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 H2SO4-KMnO4

impingers into a glass sample, Container 5. Rinsed the impingers and connecting glassware 

three times with a total of 100 mL of fresh H2SO4/KMnO4 solution and poured into 

Container 5. Similarly, rinsed the impingers and connecting glassware three times with 100 

mL of DI water. Added these rinses to Container 5. The container was sealed and labeled. 

• Container No. 6 - Rinsed the contents of impingers 4 and 5 and connecting 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 proper sealing, proper labeling, 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 HNO3 Rinse 

• Container No. 3 - Impingers 1 and 2 - 5% HNO3/10% H2O2 Impingers Catch & Rinse 

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

• Container No. 5 - Impingers 4 and 5 - H2SO4/KMnO4 Impingers Catch & Rinse 

• Container No. 6 - Impingers 4 and 5 - 8N HCl Rinse 
L2008-371 33 

FIGURE 4-1. Schematic Diagram of EPA Method 5 Particulate Matter Sampling Train 
L2008-371 34 

FIGURE 4-2. Schematic Diagram of EPA Method 201A/202 Sampling Train 
L2008-371 35 

4.5 PRODUCTION SAMPLE COLLECTION 

Marigold facility personnel collected a series of production samples during the test program and 

analyzed them for mercury using a Nevada Certified Laboratory and 7471 testing methodology. 

Marigold collected samples as follows: 

• Carbon Kiln Mercury Testing - The carbon kiln is a batch process. The carbon loaded 

into the feed hopper was sampled. Two samples 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 for 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 processed and hours operated. 

Carbon Kiln – tons of material processed, hours of operation, propane consumption. 

Retort – tons of material processed and hours of operation. 

Smelting furnace – tons of material processed 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 Marigold, provided to TRC, and included as 

Appendix C of this report. 
L2008-371 37 

5.0 ANALYTICAL PROCEDURES 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 accomplished 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 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 250°F. The containers were desiccated to a constant weight. 

The filter was desiccated and weighed to constant weight. The front-half acetone rinse was air 

dried in a tared container and then desiccated and weighed to a constant weight. The sum of the 

net weights for the probe wash and filter catch were used to calculate the concentration of 

filterable particulate matter. The net weights for the filterable particulate fraction were reported 

as concentrations in milligrams (mg) and grains per dry standard cubic foot (gr/dscf). 

5.1.2 Particulate Matter from Method 201A/202 Sampling Train 

Particulate matter and particulate matter concentrations equal to or less than an aerodynamic 

diameter of nominally 10 μm (PM10) sampling were accomplished by following the procedures 

in EPA Method 201A/202. Particulate matter analysis was conducted by TRC. 

The glass fiber filters were desiccated to a constant 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 desiccated to a constant weight. 
L2008-371 38 

The front-half acetone rinse was air dried in a tared container and then 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 used to calculate the concentration of filterable 

particulate matter. The net weights for the filterable particulate fraction were reported as 

concentration in grains per dry standard cubic foot (gr/dscf) and emission rate in pounds per hour 

(lbs/hr). 

The back-half DI water reagent and the back-half MeCl2 rinses were combined and extracted 

with MeCl2 to separate the organic and inorganic fractions. The organic and inorganic fractions 

were desiccated and weighed to a constant weight. The organic and inorganic fractions were 

reported as concentration in grains per dry standard cubic foot (gr/dscf) and emission rate in 

pounds per hour (lbs/hr). The sum of the organic and inorganic fractions was reported as the 

total condensable particulate. The sum of the filterable and condensable particulate fractions was 

reported as the total PM10. 

5.1.3 Particulate Matter and Mercury from Method 29 Sampling Train 

At the conclusion of the field effort TRC packaged 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 collected 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, located in West Sacramento, California for mercury determination.

5.2 CALCULATIONS 

5.2.1 Flow Rates and Isokinetics 

Time = T 

Dry Gas Meter, ft3

 = VM 

Pitot ∆P, in. H2O = ∆P 
L2008-371 39 

Orifice ∆H, in. H2O = PM 

Dry Gas Temp In, oF = TMI 

Dry Gas Temp Out, oF = TMO 

Stack Static Pressure, in. H2O = 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, ft3

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. H2O 

 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 H2O silica gel + gm impinger H2O 

Note: If ml H2O is measured - (ml × 0.9982 gm/ml) 

9. Volume of water vapor at standard conditions, scfb
L2008-371 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 = (% CO2 × 0.44) + (% O2 × 0.32) + [(% CO + % N2) × 0.28] 

12a. % Excess Air 

%EA = [(% O2) - 0.5 × (% CO)] × 100 

[(0.264) × (% N2)] - (% O2) + 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

stack diameter⎟

⎠

⎞ ⎜

⎝

⎛

Rectangular = Length × Width 

15. PS = Stack Pressure, absolute, inches Hg = PB ± Avg PST 

PST = Stack static pressure 

PST = PST in. H2O

 13.6 

PS = PB ± Average PST 

16. TSavg = Average Stack Temperature 

 
L2008-371 41 

17. SDEavg = ( ΔP) avg× TSavg + 460

18. Stack gas velocity at stack conditions, afpm 

 VS = 

1/ 2

avg

c

PS MW

1 5130 Cp SDE ⎥

⎦

⎤ ⎢

⎣

⎡

×

× × ×

Cp = pitot tube coefficient 

19. Stack gas volumetric flow rate at stack conditions, acfmd

Qa = VS × AS

 144 

20. Stack gas volumetric flow rate at standard conditions, dscfme

 

Qs = Qa × 528 × MD × PS 

(29.92) × (TSavg + 460) 

21. Percent Isokinetics 

%ISO = 1039f

 × (TSavg + 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 = ( ) ( )

( )( ) 60sec/ min

R in. H O

lb/lb - mole in. Hg

sec

85.5 ft

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 × ft2

 × π × 100 

5.2.2 Grains Per Dry Standard Cubic Foot 

Particulate matter rates in terms of grains per dry 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 = ( ) ( ) ( )

( ) ⎥

⎦

⎤ ⎢

⎣

⎡

⎭

⎬

⎫

⎩

⎨

⎧

× +

× × × +

× ÷

29.92 TM 460

528 Y VM PB PM 0.0154 mg
L2008-371 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, ft3

PB = Barometric Pressure, inches Hg 

PM = Average Orifice Pressure Drop, inches Hg (Avg. ΔH inches H2O ) 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 per 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 (NOx) and Carbon Monoxide (CO) 

Emission rates in terms of pounds per hour (lbs/hr) for NOx 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 (MW), 60 minutes/hour, divided by 385.3 × 106

 dscf/lb-mole 

@ 68oF (20oC). 

lbs/hr = ppm × Qs × MW × 60

 385.3 × 106

where: 

 NOx molecular weight = 46 

CO molecular weight = 28 
L2008-371 43 

6.0 QUALITY ASSURANCE 

6.1 OVERVIEW 

TRC management is fully committed to an effective 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, sampling and analysis activities, engineering 

assessments, and the analysis of gathered data for planning purposes. The Quality Assurance 

Program works to provide complete, precise, accurate, 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 the field team leader to take onsite and for the 

project file. Calibrations were performed as described in the EPA publications "Quality 

Assurance Handbook for Air Pollution Measurement 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. Equipment calibrated included the sample metering 

system, thermocouples, and pitot tubes. All calibrations were available 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 outlined in EPA Reference Method 5. During the 

course of a test run, a leak check was conducted before and after every test, or if replacement of 

a component became necessary. Final leak checks were performed to ensure that no leaks 
L2008-371 44 

developed in the train during the course of the test run. All leakage rates, if any found, were 

recorded on the appropriate field data sheet. 

6.2.3 Cyclonic Flow Check 

The absence of cyclonic flow within the sampling 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 performance criteria defined in 40 CFR 60 Appendix A, 

Methods 3A, 7E, and 10. Any test not meeting these criteria was considered questionable and 

the test run repeated. 

6.3 DATA REDUCTION, VALIDATION, 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 Appendix A. The data collected was reviewed in 

the field by the Field Team Leader and at least 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 methods and criteria appropriate to the type of 

data and the purpose of the measurement. Records of all data were maintained, including that 

judged to be an "outlying" or spurious value. The persons who validated 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 computer 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. O2, percent 

b. CO2, percent 

c. NOx, ppm, and lb/hr 

d. CO, ppm, and lb/hr 

e. Hg, gr/dscf , and lbs/hr 

f. PM and PM10, 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.