APPENDIX III 

MATES III 

FINAL REPORT 

MATES III Monitoring and Laboratory Analysis Protocol 

Authors

Rudy Eden 

Steve Barbosa 

Solomon Teffera 
MATES III Final Report

Appendix III-1 

MATES III 

APPENDIX III 

MONITORING AND LABORATORY ANALYSIS PROTOCOL 

March 2004 

Science and Technology Advancement 

South Coast Air Quality Management AQMD

Draft Approved for Review Date Approved 

 

Rudy Eden 

Senior Manager, Laboratory Services 

Applied Science & Technology 
MATES III Final Report

Appendix III-2 

DISCLAIMER 

Any or all reference made in this Protocol to a specific product or brand name does not constitute 

an endorsement of that product or brand by the South Coast Air Quality Management District. 
MATES III Final Report

Appendix III-3 

Table of Contents 

List of Figures 

List of Tables 

List of Appendices 

Chapter 1.0 Introduction 

 1.1 Background 

 

Chapter 2.0 Monitoring Equipment 

 2.1 Introduction 

 2.2 Equipment Characteristics 

 2.2.1 Siting 

 2.2.2 Acceptance Testing 

 2.2.3 Calibration 

 2.2.4 Sample Pickup 

 2.2.5 Trouble Shooting 

 2.2.6 Repair 

 2.3 Sampling Equipment 

 2.3.1 XonTech 910A and 912 

 2.3.1.1 XonTech 910A, Description 

 2.3.1.2 XonTech 912, Description 

 2.3.1.3 Pre-Testing 

 2.3.1.4 Cleanliness Check 

 2.3.1.5 Sample Pickup 

 2.3.2 XonTech 920 and XonTech 924 

 2.3.2.1 Description 

 2.3.2.2 Operation 

 2.3.3 ATEC 800 Sequential Sampler 

 2.3.3.1 Description 

 2.3.3.2 Operation 

 2.3.4 MET One SASS 

 2.3.4.1 Description 

 2.3.4.2 Module and Media Description 

 2.3.5 Gil Solent 2 Axis Ultrasonic Anemometer 

 2.3.5.1 Description 

 2.3.5.2 Siting 

 2.3.5.3 Installation 

 2.3.5.4 Telemetry Interfacing 

 2.3.5.5 Routine Service 

 2.3.5.6 Diagnostics 

 2.3.5.7 Calibration 

 2.3.5.8 Data Handling 

 2.3.6 Graseby-GMW 1200 PM10 Sampler 

 2.3.6.1 Description 
MATES III Final Report

Appendix III-4 

Chapter 3.0 Laboratory Procedures 

 3.1 Introduction 

 3.2 Sample Handling 

 3.2.1 Canister Cleaning 

 3.2.2 Field Canister Use 

 3.2.3 Sample Distribution in the Laboratory 

 3.3 Analysis Methods 

 3.4 Sampling and Analysis - Table 1 Compounds 

 3.5 Sampling and Analysis - Table 2 Compounds 

 3.6 Sampling Schedule 

Chapter 4.0 Quality Assurance and Quality Control 

 4.1 Introduction 

 4.2 Objectives 

 4.3 Procedures 

 4.3.1 Quality Assurance Procedures 

 4.3.2 Quality Control Procedures 

 4.4 Documentation 

 4.5 Data Review 

Chapter 5.0 Data Processing and Reporting 

 5.1 Introduction 

 5.2 Data Base Compilation 

 5.3 Periodic Reports 

 5.4 Final Report 

Glossary 

Acronym List 
MATES III Final Report

Appendix III-5 

List of Tables 

 Table 2-1 Performance Specifications Gill Solent 2 Axis Ultrasonic Meteorological 

 Anemometer Specifications 

 Table 3-1 Mobile Platform Sampling Schedule 

 Table 4-1 QA/QC Data Quality Objectives 

List of Figures 

 Figure 2-1 Graseby-GMW PM10 Sampler, Model 1200 with Two-Stage, SSI Head 

List of Appendices 

Appendix A Proposed Table 1 Air Contaminants for Inclusion in the Measurement Program 

Appendix B Proposed Table 2 Air Contaminants that Potentially May Be Monitored on a 

Limited Basis 

Appendix C Size-Selective Inlet PM10 Sampler Envelope

Appendix D Monthly WSD Quality Control Maintenance Check Sheet 

Appendix E High Volume Monthly Control Maintenance Check Sheet 

Appendix F MATES III Sample Log 

Appendix F-1 Microscale Sample Log 

Appendix G VOC Canister Tag 

Appendix H Method Description for Sampling and Analysis of Carbonyls by HPLC at the 

AQMD Laboratory 

Appendix I Method Description for Sampling and Analysis of Elements by Energy Dispersive 

X-Ray Fluorescence Spectrometry at the AQMD Laboratory 

Appendix J Method Description for Sampling and Analysis of Elements by Energy Dispersive 

X-Ray Fluorescence Spectrometry at the AQMD Laboratory 

Appendix K Method Description for Sampling and Analysis of Organic and Elemental Carbon 

by Thermal/Optical Carbon Analyzer at the AQMD Laboratory 

Appendix L QA/QC Matrix Summary 

Appendix M Method Description for Sampling and Analysis of VOCs by GC/MS at the 

 AQMD 
MATES III Final Report

Appendix III-1 

Chapter 1.0 

Introduction

This protocol document provides detailed information about the procedures and processes 

required to conduct the field measurement element of the Multiple Air Toxics Exposure 

Study III (MATES III). 

1.1 BACKGROUND 

In 1998, the South Coast Air Quality Management District (AQMD) conducted an 

intensive ambient air toxics monitoring program, the Multiple Air Toxics Exposure Study 

(MATES II). The objective of MATES II was to establish a baseline of existing air toxics 

ambient emissions, exposure and risk level data and an assessment of model accuracy. 

The AQMD conducted MATES II over a one-year period at ten sampling sites in the 

South Coast Air Basin (Basin). The MATES II Final Report was approved by the AQMD 

Board in March 20001. 

The microscale monitoring element of MATES II was conducted to determine if 

communities were experiencing localized hot spots not otherwise identified through the 

regional modeling. Microscale sampling was conducted over six-week intervals at 

selected locations throughout the Basin using three mobile sampling platforms. During 

the year-long monitoring period, the platforms were deployed to collect ambient toxics 

measurements. 

For MATES III, specific compounds will be sampled and analyzed. These compounds 

are identified in Appendices A and B. Compounds listed in Table 1 (Appendix A) will be 

measured on a routine basis, while compounds listed in Table 2 (Appendix B) will 

undergo more limited measurement and sampling due to methodological limitations, high 

cost of analysis, or other limitations. 

Field sampling will begin in April 2004 and continue for a minimum of one year. This 

document describes the monitoring, laboratory analysis, quality control (QC), and quality 

assurance (QA) activities necessary to support both the regional and microscale sampling 

programs. 

 

1

 South Coast Air Quality Management District (2000). MATES II Final Report. Diamond Bar, CA 
MATES III Final Report

Appendix III-2 

Chapter 2.0 

Monitoring Equipment 

2.1 INTRODUCTION 

For the purposes of this protocol, the descriptions and operational and maintenance 

procedures of the following equipment used in MATES III sites will be delineated. 

Sampler Type Vendor and Model Number

Volatile Organic Compounds (VOC) XonTech 910A/ 912 

Metals; Carbonyls XonTech 920 and 924 

Carbonyls ATEC 800 Sequential Sampler 

PM2.5 Speciation Air Sampling System Met One Instruments SASS 

Wind, Speed, and Direction (WSD) Gill Solent 2 Axis Ultrasonic Anemometer (Met-One) 

PM10 Graseby-GMW 1200 PM10 Sampler 

The siting, acceptance testing, and calibration functions for each type of equipment 

identified above are basically identical. Therefore, these functions are defined below. 

Non-generic functions will be discussed under each equipment heading. 

2.2 EQUIPMENT CHARACTERISTICS 

2.2.1 Siting 

A) Monitoring site selection criteria will be the same in most regards whether the site 

will be used for a fixed or mobile site. Site uniformity will be achieved to the greatest 

degree possible. Descriptions will be prepared for all sampling sites. The description 

should include, at a minimum, the type of ground surface, the direction, distance, and 

approximate height to any airflow obstruction, and the direction and distance to any 

local pollutant sources. 

B) The sampler platform will be located in an area with unobstructed airflow, especially 

in the direction of any recognized sources of the sampled compounds. Turbulence 

and eddies from obstructions will cause non-representative results. The distance 

between the obstruction and the sampler should not be closer than two times the 

height of the obstruction. 
MATES III Final Report

Appendix III-3 

C) Locations unduly influenced by nearby sources or activities or where reactive surfaces 

may cause chemical changes in the air sampled will be avoided. Micrometeorological influences caused by nearby hills, bodies of water, valley drainage 

flow patterns, etc. will be taken into consideration. 

D) The recommended intake probe height for criteria pollutants is 3 to 15 meters above 

ground level as near breathing height as possible, but not where a building is an 

obstruction or the equipment is easily vandalized. 

E) The probe should extend at least two meters away from the supporting structure. If 

the probe is located on a building, it must be mounted on the windward side. 

2.2.2 Acceptance Testing 

Acceptance testing will be performed on all instrumentation for approximately one month 

after receipt. After acceptance testing is conducted on the instruments, they will be 

deployed in the field and ambient sampling will commence. Acceptance testing will be 

conducted through the following steps: 

A) All instruments will be carefully unpacked from their shipping containers and 

checked for completeness, broken parts, and correct subunits. 

B) The units will be assembled according to manufacturer guidelines and prepared for 

start-up. 

C) The flowrate/flow meter portion of the pneumatic system will be checked using the 

most appropriate calibration-transfer standard to verify the operating flow/flowrate. 

D) Timer accuracy will be evaluated by comparing it to an elapsed-timer standard. All 

timers must hold their accuracy to ±5 minutes over a 24-hour period. 

E) Any deficiency will be corrected following the manufacturer’s procedures. 

F) Each microscale site will be operated for an intensive six to eight-week sampling 

period. Following sampling, each microscale monitoring mobile platform will be 

loaded on the transport vehicle and moved to the next sampling site. The lease 

agreement for each monitoring site will be executed for a minimum eight-week 

period. Within this contractual time frame, the temporary power can be hooked up, 

temporary fencing installed and all samplers at the new site can be calibrated prior to 

beginning the next intensive eight-week sampling period. Sampling will be 

conducted at each microscale site on the same one-day-in-three schedule as the 

MATES III fixed sites. 
MATES III Final Report

Appendix III-4 

2.2.3 Calibration 

At each sampling site, final dynamic calibration will be performed on each analyzer prior 

to the start of the intensive six-week sampling period. At the end of this sampling period, 

an “As Is” dynamic calibration will be performed on each analyzer to ascertain the 

amount of analyzer drift. 

2.2.4 Sample Pickup 

The AQMD Senior Chemist sample custodian will distribute the sampling media to the 

field technician. Filters and carbonyl cartridges will be transported in coolers with blue 

ice, and the canisters will be kept capped at all times during transportation. Once the 

filter and carbonyl cartridge has been used to collect a sample, they must be refrigerated 

until they are returned to the AQMD. The sampling media will be returned to the Senior 

Chemist sample custodian as soon as possible following sampling. 

2.2.5 Troubleshooting 

A maintenance guide based on the equipment manufacturers’ suggested operating 

procedures will be available for each instrument. If an instrument falls out of the correct 

operating range, or if there is a component failure, the operator will immediately place a 

call to the AQMD STA/AM Support and Repair Section to schedule a repair. 

2.2.6 Repair 

Due to anticipated failure of standard components such as pumps and flow controllers, 

the AQMD will warehouse standard component spare parts. Since the sampling time at 

each location will be relatively brief, repair of microscale monitoring platform samplers 

will receive priority. 

2.3 SAMPLING EQUIPMENT 

2.3.1 XonTech 910A and 912 

2.3.1.1 XonTech 910A - Description 

The XonTech 910A air sampler is designed to take air samples at a constant flow 

rate for a known sampling period. It is durable, serviceable and accurate making it 

useful for sampling a wide variety of gases. Its compact, constructed simply, and 

offers long term reliability. 

Specifically, the 910A sampler takes air from the sample inlet and injects it into a 

canister at a constant flow rate for the preset period of time. Excess air is exhausted 

through a bypass exhaust. The constant flow rate and elapsed time allow the 

operator to calculate the integrated air sample volume. The sample will be pumped 
MATES III Final Report

Appendix III-5 

through a metal bellows pump that develops sufficient pressure to control the flow 

with a mass flowmeter. The XonTech 910A is operated according to the guidelines 

set forth in XonTech’s Model 910 Toxic Air Sampler Operations Manual2. 

2.3.1.2 XonTech 912 - Description 

The XonTech 912 adapter may be added to the XonTech 910A to enhance sampling 

capability over a reduced period of time. It cannot operate independent of the 910A. 

It is designed to route gas samples to a maximum of 16 canisters. An internal time 

base can be used to step a rotary valve from canister to canister at a user-selected 

rate. The 912 will also accept timing signals from the model 910A. The XonTech 

912 adapter is operated according to the guidelines set forth in XonTech’s Model 910 

Toxic Air Sampler Operations Manual3.

2.3.1.3 Pre-Testing 

All canister samplers will be test run at the AQMD headquarters to assure proper 

operation. Most samplers are also field tested during field sampling. 

2.3.1.4 Cleanliness Check 

To perform a system bias check, ultra-pure air or nitrogen will be injected into the 

sample manifold to fill one, 3-hour canister. Additionally, the 24-hour sampler can 

be tested by maximally increasing its sample flow to fill a canister in approximately 

6 hours. A field blank will be filled at the site by flowing pure air or nitrogen into an 

evacuated cylinder. A difference of less than 1 part per billion (ppb) per compound 

between the field blank and the bias samples indicates that the system is non-biasing 

(non-contaminated). A value greater than 1 ppb per compound requires corrective 

action. A system bias check will be repeated until all biases are demonstrated to be 

eliminated. The AQMD’s Ambient Monitoring Support Group will perform system 

repairs. This group will assemble, leak check, disassemble, and clean the sample 

manifold, and the Auditing Group will calibrate the mass flow controller (MFC) for 

flow. 

2.3.1.5 Sample Pickup 

An AQMD Instrument Specialist will pick up clean VOC canisters in the Laboratory. 

Evacuated canisters will be transported by vehicle to the respective air monitoring 

stations. Each canister has a tag attached (Appendix G). This tag will be completed 

to contain the following information: sample site, operator initials, sample date, and 

canister number in sampling sequence. The air monitoring station operator should 

complete this tag once the canister is set up for sampling. Once the canister is filled

and disconnected from the 910A or 912 sampler, and prior to returning the sampled 

 

2

 XonTech, Inc. (1987). Model 910 Toxic Air Sampler Operations Manual. Van Nuys, CA: Author. 

3

 Ibid. 
MATES III Final Report

Appendix III-6 

canister to the Laboratory, the canister number, start vacuum, end pressure (psig), 

and elapsed time will be recorded on the canister sample log (Appendix F and F-1). 

The time on the QC chart must also be checked and adjusted. This value must be 

within ± 10 minutes of actual Local Standard Time. The canister will be delivered to 

the Senior Chemist sample custodian as soon as possible. 

2.3.2 XonTech 920 and XonTech 924 

2.3.2.1 Description 

 

The Model 920 and equivalent Model 924 Toxic Air Samplers are designed to 

collect ambient air particulate samples on a variety of filter materials and sorbent 

media in unattended field use. These samples will be brought to the AQMD 

headquarters for Laboratory analysis. The sampler precisely controls the sampling 

time and flowrate through each sampling head using a microprocessor and mass flow 

controller (MFC). Sampler design is modular to facilitate installation of individual 

sampling channels. Each sampler may accommodate eight sampling channels for 

two types of sample collection media: one that accepts 37 or 47 millimeter filters and 

another that accepts sorbent tubes. 

The sampler consists of three modules, each contained in a separate enclosure. The 

heart of the system is the control module. This module contains the microprocessor, 

controller, mass-flow controllers, and front panel, displays, printer, and keypad. The 

difference between the Model 920 and 924 is the electronics have been upgraded to 

reflect the increase in microprocessor functionality presently available that was not 

available in the circa 1995 Model 920. The sampling module is equipped with 

isolation valves that protect the sampling media from passive sampling before or 

after sampling or sample loss after sampling. The sampling module and the pump 

module have not changed between the Model 920 and 924. The sampling inlet 

height is 1.2 meters above ground level. The third element of the sampler is the 

pump module. It contains the vacuum pump that provides adequate capacity for 

simultaneous operation of three, 30 liters per minute (lpm) and 200 cubic centimeters 

per minute (ccm) sampling channels. 

2.3.2.2 Operation 

To use the sampler, the operator will insert the sample filter cassette or sorbent tube 

into the sampling head and will key in the filter or sorbent head number. Start and 

stop times, and flow rates are pre-programmed or can be manually input. Following 

the sampling period, a report is automatically printed which may be removed from 

the printer and submitted to the Laboratory with the filter for analysis. 

When the sampling period concludes, a report is automatically printed. This report is 

removed from the printer and submitted with the sample to the Laboratory. Sampler 

start up may be achieved by either a cold or warm start. Warm and cold-start options 
MATES III Final Report

Appendix III-7 

as well as all other operational specifications are discussed in XonTech, Inc. Model 

920 Toxic Air Sampler Operations Manual4

. 

2.3.3 ATEC 800 Sequential Sampler 

2.3.3.1 Description 

 

An ATEC Model 800 sequential sampling instrument will be used to perform 6 or 8 

hour integrated carbonyl sampling. The ATEC 800 instrument contains multiple 

channels that can be independently programmed for specific flowrates. Channel 1 is 

a multi-port channel containing eight ports. Each port can be programmed to sample 

over a specific time period. Optional Channels 2 and 3 consist of single ports that 

can be activated for parallel or different time periods than Channel 1. The Xontec 

920/924 samples carbonyl compounds for an integrated 24-hour period only. 

2.3.3.2 Operation 

The sampler can be operated in either program or run modes, depending on the 

position of the program/run switch on the front panel. In program mode, all of the 

front panel function keys can be used to program operation cycles, display or print 

data, perform manual operations, set the MFC flowrate, or change the date and time. 

In the run mode, the sampler is activated according to the cycle programmed. If a 

sample is being collected, the sampler will display the current data for the active port 

or channel. For a full explanation of ATEC 800 operational procedures, refer to 

Models 800 and 1600 Automated Samplers Operations and Maintenance Manual5

. 

Following sampling, the operator will remove the cartridges from the sampler, place 

them in a sealed container, and chill them in preparation for transport back to the 

Laboratory for analysis. The operator will record all appropriate data on the sample 

log. Note; if a power failure should occur during port sampling, the data collected 

for that port before the power failure will be lost. The sampler will resume operation 

at whatever port is active at the time power is restored. 

 

4

 XonTech, Inc. (1987). Model 920 Toxic Air Sampler Operations Manual. Van Nuys, CA: Author. 

5

 ATEC. (1996). Models 800 and 1600 Automated Samplers Operations and Maintenance Manual. 

Calabasas, CA: Author. 
MATES III Final Report

Appendix III-8 

2.3.4 MET One SASS 

2.3.4.1 Description 

The MET One Speciation Air Sampling System (SASS) accommodates up to five 

sampling canisters to hold multiple 47 millimeter filters to capture PM2.5 particles. 

The PM2.5 separation is produced by a sharp cut cyclone (SCC) that removes both 

solid and liquid coarse particles. Particle penetration through the SCC mimics the 

PM2.5 cutoff curve of the WINS impactor as defined by the U.S. Environmental 

Protection Agency. All routine maintenance can be done in the field. Filter 

containers are transported to the Laboratory for inspection, cleaning and changing of 

sampling substrates. Every element of the sampler that is contacted by the sampled 

air stream ahead of the filter, including the inlet can be cleaned with each sample 

change. The SASS was designed with individual sharp cut cyclone inlets. Particles 

larger than 2.5 micron aerodynamic diameter are removed by the cyclonic inlet 

mounted with each filter container. The filter containers may be equipped with a 

diffusion denuder ahead of the filter to remove selected gaseous compounds. 6

.

2.3.4.2 Module and Media Description 

The integrated SASS canister contains the following components: a sharp cut 

cyclone, a denuder to remove nitric acid or ammonia gases, a 47 mm front 

filter for particle capture, a 47 mm tandem or backup filter as needed, and a 

cover to protect the components. 

Several types of filter media are needed for assaying the different chemical 

constituents of ambient particles. The filter media must be suitable for the 

type of analysis to be done. For example, Teflon filters are used for 

gravimetric mass and trace metal determinations. Quartz fiber filters are used 

for elemental and organic carbon analysis as well as anions and cations 

analysis. 

2.3.5 Gill Solent 2 Axis Ultrasonic Anemometer 

 2.3.5.1 Description 

The Gill 2 Axle Ultrasonic Anemometer is used to measure wind speed and direction 

(WSD) data. The performance specifications of this anemometer are delineated in 

Table 2-1. Data is stored in a data logger until it is telemetered to the AQMD’s 

information system. 

 

6

 MET One Instruments, Inc. (2001), Model SASS & SuperSASS PM2.5 Ambient Chemical Speciation 

Samplers, Grants Pass, Oregon: Author. 
MATES III Final Report

Appendix III-9 

The wind-observer, ultrasonic anemometer consists of a sensing head with four 

transducers arranged in two pairs, surmounting a cylindrical electronic base 

enclosure. The onboard electronics provide all ultrasonic processing and vector 

computation required to output wind data in digital and analog form. For a complete 

description of anemometer operations, refer to Solent 2 Axis Ultrasonic Anemometer 

(Heated & NonHeated) User Manual and Product Specification7.

TABLE 2-1 Performance Specifications - Gill Solent 2 Axis Ultrasonic Anemometer 

 Wind Speed Wind Direction

 1. Starting Threshold 0 mph 0 degrees 

 2. Range 0-145 mph 0-360\540 degrees 

 3. Accuracy ± 5% rms ±4 degrees 

2.3.5.2 Siting

WSD measurement, barometric pressure, relative humidity, and temperature 

monitoring equipment is housed in monitoring stations located in buildings or 

mobile monitoring platforms. The stations meet Environmental Protection Agency 

(EPA) criteria for National Air Monitoring Stations (NAMS) and State and Local Air 

Monitoring Stations (SLAMS) as cited in part 40 Code of Federal Register (CFR) 

Part 58 attached and included herein by reference. 

If the meteorological equipment is located in a one-story building, it is installed on a 

6.1-meter tower in an unobstructed position. If the equipment is installed in a 

platform, it is mounted on a 6.1-meter mast. In those cases involving buildings 

higher than one story, the mast is made sufficiently high to rise above the 

surrounding geography. 

2.3.5.3 Installation

WSD equipment is assembled and oriented according to the manufacturer's 

instructions. The manufacturer’s manuals are used as the primary installation guide. 

The mast base support is hinged to allow quick raising of the tower. The base will 

be welded to the top of the platform or secured to a cement base when positioned on 

a building. If the tower is erected close to an existing building, it will be secured to 

that building by an L-bracket. If the mast is mounted on the housing roof, guy wires 

will secure it. Tower vertical alignment may be checked during this process using a 

bubble level. If the tower is out of vertical alignment, shimming and the use of 

 

7

 Gill Instruments, Ltd. Solent 2 Axis Ultrasonic Anemometer (Heated & Non-Heated) User Manual and 

Product Specification (Doc No 1172 - 0003 - lss3). Lymington, Hampshire, England: Author. 
MATES III Final Report

Appendix III-10 

turnbuckles may be necessary. When the tripod is secured, the mast is fully extended 

with the sensor orientated in the generally correct direction. Additional guy wires 

further secure the tower. 

Once the WSD monitoring equipment has been assembled, mounted on the mast, 

and raised to its full height in the correct orientation, the direction sensor will be 

aligned to true north using a true-north-calibrated compass. Although alignment 

must be performed from a distance, accuracy within five degrees is possible. 

2.3.5.4 Telemetry Interfacing 

A telemetry system is used at existing AQMD sites where such capabilities now 

exist. This system transfers WSD data from the station to the AQMD central 

computer. The telemetry system accepts direct current (DC) voltage signals from 0 

to 5 volts. Since sensors other than WSD are not DC compatible, they must be 

converted to 0 to 5 volts DC. To convert to DC, input the barometric pressure, 

temperature, and humidity sensor outputs through the converter box that changes the 

sensor output to the proper voltage. The converter box consists basically of ± 15 and 

± 5-volt DC power supply and an alternating current (AC) to DC converter. The 

input to the converter box comes directly from the sensors. 

2.3.5.5 Routine Servicing 

The air quality instrument specialist responsible for each monitoring site will 

perform routine servicing and periodic checks of the WSD system, barometric 

pressure, and temperature. The instrument specialist must note and initial the type of 

service performed and the results of each periodic check on the strip chart, in the 

system’s daily log, and on the WSD Monthly Quality Control Maintenance Sheet 

(Appendix D). 

Any suspected operational problem must be communicated in detail by the 

instrument specialist to the appropriate supervisor. The supervisor, when informed 

of the problem, will contact the station operator to determine if the problem can be 

corrected in-house. If the problem cannot be corrected in-house (by the station 

operator), the AQMD supervisor will arrange for a system repair team. Anemometer 

servicing will be conducted on daily, weekly, and monthly basis as described below. 

A) Daily Checks (where chart recorder is used) 

Each day a site is visited, the station operator will write the date, station designation, 

comments, and initials on the strip chart. The operator will also provide a distinct 

and accurate time check on the chart. If the time is off, the operator must provide 

time checks both before and after adjusting the strip chart. 
MATES III Final Report

Appendix III-11 

B) Weekly Checks 

The sonic anemometer, barometric pressure, and temperature will be checked for 

daily trends as an indication of proper operation. 

 

C) Monthly Checks 

The sonic anemometer will be lowered from the tower and the transducers will be 

cleaned with a dry towel and water when necessary. The mounting of all three 

sensors will be checked to verify they are securely attached. The WSD sensor will 

be aligned with true north. 

2.3.5.6 Diagnostics 

The Gill 2 Axle Ultrasonic Anemometer microprocessor-based system is designed 

with continuous internal diagnostics. These diagnostics are used to ensure that the 

unit is operating correctly within calibration and without potential problems. In the 

unlikely event of a problem with the anemometer, or if anything physically obstructs 

its ultrasonic pulses, the anemometer will display different status codes. The 

transducers will not display inaccurate data. Thirteen different status codes may 

result. These codes are: 

Status code 00 - System is okay 

Status code 01 - Transducer pair 1 failed 

Status code 02 - Transducer pair 2 failed

Status code 04 - Transducer pairs 1 and 2 failed 

Status code 08 - Non-volatile checksum error 

Status code 09 - Volatile memory checksum error 

Status code 10 - System gain at maximum 

Status code 50 - Marginal system gain condition 

Status code 51 - Measurement average building

Status code 60 - Heating operational 

Status code 61 - Heating operational but under power 

Status code 62 - Heating tripped 

Status code 63 - Temperature sensor fault 

Status code 64 - Heating operational but over power

A status code will result when an object partially blocks the transducer pulse or the 

transducer begins to lose efficiency. WSD transducers normally receive pulses from 

each other within a specific range of intensity amplified and fed to the receiving and 

recording electronics. When the intensity is lower than normal, the transducer will 

display the status code 10 as a percentage output. A status code 10 is normally 

reported just before transducer failure. The amplifier gain is automatically increased 

to keep the system stable and maintain transducer accuracy. 

 
MATES III Final Report

Appendix III-12 

Transducers have stainless steel bodies capable of handling a harsh marine 

environment. They are manufactured to meet National Equipment Manufacturer’s 

Association (NEMA) 4X or IP 65 Standards and are pretested in a wind tunnel. 

The unit, consisting of a transducer and electronics, continuously checks itself, the 

transducers, and the calibration integrity and describes random access memory 

(RAM) faults. During each measurement cycle, the unit will perform 39 WSD 

measurements every second. This data is averaged and output one to four times per 

second. 

 2.3.5.7 Calibration 

The calibration process is completely computer controlled. However, operator 

intervention is necessary to change the erasable prompt chip (EPROM) found in the 

anemometer. An anemometer undergoing calibration is initially fitted with special 

firmware that operates within reciprocal tables and transducer delays stored in RAM 

rather than EPROM as is customary. The first requirement is to input the two axis 

path lengths and the wind tunnel temperature requirements. At this point, the wind 

tunnel is switched off and the air is still. Reciprocal tables are produced for each 

axis based upon the path lengths entered and transmitted to the anemometer. The 

wind tunnel is operated up to a speed of 40 knots and the anemometer is rotated 

through 360 degrees at 5-degree steps. The perceived WSD is recorded for 5 

seconds at each step and the results are averaged and stored. 

Because the unit has no moving parts, calibration and accuracy will not drift. The 

unit has been designed to announce calibration corruption. Anemometer calibration 

can be tested by inputting a zero value for the WSD and checking the outputs or by 

using a calibrated fan. The unit should only be placed in a chamber that does not 

reflect ultra-sonic pulses. The only way the unit can lose its calibrations is if the 

distance between the traducers (path length) is altered. The path length can only be 

altered if the stainless steel arm is bent or physically damaged. To verify path length 

accuracy, the path length is measured and checked against the original calibration. 
MATES III Final Report

Appendix III-13 

2.3.5.8 Data Handling

All data generated from the WSD system will be recorded. Specifically, the station 

name or number, time and date of the data run, and a brief discussion of any 

maintenance or repair work required will be noted on the strip chart each day the 

station is visited. The wind charts may not be cut at any time. When the wind chart 

is removed from the recorder and the data is reduced, the time and date of chart 

removal, the station location, and the station reporter's signature must be noted on 

the bottom of the printed side of the strip chart. The expended chart will be returned 

to the box in which it was received. The station name or number and the dates of the 

strip chart will be noted on the end flap of the box. Completed Wind Data Summary 

Sheets and strip charts will be submitted to the Principal Air Quality Instrument 

Specialist responsible for the station. 

2.3.6 Graseby-GMW 1200 PM10 Sampler 

2.3.6.1 Description 

A cross-sectional drawing of the Graseby-GMW Model 1200 two-stage, sizeselective inlet (SSI) head is shown in Figure 2-1. This sampler is used to sample 

particulate with an aerodynamic diameter of 10 microns and less. The inlet head is 

symmetrical and therefore insensitive to wind direction and relatively insensitive to 

wind speed. The air is drawn through the acceleration nozzles at 40 cfm. Particles 

larger than 10 microns (aerodynamic diameter) cannot follow the air stream and are 

deflected below the nozzles onto the flat surface. The air sample is then drawn 

through vent tubes, the second-stage fractionator, and the filter where the particulate 

matter is collected. The height of the vent-tube inlets above the acceleration nozzle 

plate prevents re-entrainment of particles. 

The PM10 sampler draws air into a specially shaped inlet at a flowrate of 40, ±4, 

cubic feet per minute (cfm). PM10 particulate matter collects on an 8 x 10 inch 

matted quartz fiber filter surface. The concentration of PM10 particulate matter (in 

micrograms per cubic meter) is calculated by weighing the particulates collected on 

the filter and dividing by the measured air sample volume. The standard sampling 

frequency is every sixth day. 

To initiate sampler start-up, the operator will complete a PM10 sampler site report 

and send it to the appropriate AQMD supervisor for review of compliance with 

SLAMS total suspended particulates (TSP) siting criteria 40 CFR Part 58, Appendix 

E included herein by reference. The PM10 sampler may be calibrated according to 

Appendix A, Section A.5.9 of the AQMD’s Quality Assurance Plan for Air 

Monitoring8.

 

8

 Applied Science & Technology. (1996). Quality Assurance Plan For Air Monitoring. Diamond Bar, 

CA: South Coast Air Quality Management District. 
MATES III Final Report

Appendix III-14 

The matted, quartz-fiber filter is very delicate and can be easily torn or gouged. 

Because a damaged filter will be invalid or invalidate results, it is important to 

carefully handle it by the edges. To avoid electrical shock, the 115V AC power 

should be disconnected before working on the motor. Complete operational details 

are contained in Instruction and Operation Manual High Volume PM10 Sampler9.

FIGURE 2-1 Graseby-GMW PM10 Sampler, Model 1200 with Two-Stage, SSI Head 

 

9

 Graseby Anderson. (1988). Instruction and Operation Manual High Volume PM10 Sampler. Atlanta, 

GA: Author. 
MATES III Final Report

Appendix III-15 

Chapter 3.0 

Laboratory Procedures 

3.1 INTRODUCTION 

Since 1994, the AQMD has implemented the U.S. EPA PAMS program to gather data on 

ozone precursors. Some of the same sampling instruments currently used in the PAMS 

program may be used in the MATES III and microscale efforts. Hence, many of the 

procedures and protocols for the MATES III program will be taken from the AQMD 

Quality Assurance Plan for Air Monitoring10 (updated July 1997). However, MATES III 

also utilizes several analytical methods not performed in the PAMS program and the 

protocols include herein will parallel accepted ARB and EPA procedures. 

The AQMD will rely upon Air Quality Instrument Specialists to take the field samples 

and deliver them to the Laboratory sample custodian. The Laboratory sample custodian 

will handle logging and distribution within the AQMD. Procedures for proper sampling 

and initial chain-of-custody are outlined in the AQMD PAMS Air Monitoring Network 

Quality Assurance Plan11, Section 7E Parts 1 and 2. 

3.2 SAMPLE HANDLING 

All sampling media will be handled according to the Laboratory practice for 

implementation of toxics analysis and particulate matter network programs as applicable. 

Field instrument specialists will complete the sampling information and chain-of-custody 

forms12, and deliver the samples to the Laboratory sample custodian. 

3.2.1 Canister Cleaning 

The AQMD Laboratory has a canister cleaning oven system. This system utilizes 

humidified nitrogen to flush and clean canisters in a heated oven to less than 5-ppb 

carbon of total organic compounds. The canisters are held at a 80oC temperature and are 

flushed a minimum of seven times over a 2 1⁄2 -hour period. Every canister is removed 

from the canister cleaning oven and analyzed for residual hydrocarbons. Long-term 

experience has proven that the canister-cleaning oven system is sufficient to provide clean 

canisters. Any hydrocarbons (above the threshold concentrations) found in the checked 

canister are cause for investigation and corrective action. The cleaning date and operator 

are noted on the canister tag and in an electronic database that serves as the primary 

chain-of-custody. 

 

10 Applied Science & Technology. (1996). Quality Assurance Plan For Air Monitoring. Diamond Bar, 

CA: South Coast Air Quality Management District. 

11 Applied Science & Technology. (1977) PAMS Air Monitoring Network Quality Assurance Plan.

Diamond Bar, CA: South Coast Air Quality Management District. 

12 These forms consist of the Size-Selective Inlet PM10 Sampler Envelope (Appendix C), MATES II Sample 

Log (Appendix F), and VOC Canister Tag (Appendix G). 
MATES III Final Report

Appendix III-16 

3.2.2 Field Canister Use 

The canisters are transported by the instrument specialist to the site and installed in 

accordance with the sampling SOP included in the PAMS Air Monitoring Network 

Quality Assurance Plan13. The sample is taken and the sample time, canister number, 

and start and stop vacuum are noted on the MATES III Sample Log (Appendix F) that 

follows the canister from the field onward. The sample is promptly returned to the 

Laboratory for log-in and distribution to the appropriate Senior Chemist. 

3.2.3 Sample Distribution in the Laboratory 

The Laboratory sample custodian (Senior Chemist) will log in the samples received from 

the courier and distribute them to the appropriate Chemist following established 

Laboratory protocol. The sample custodian will distribute samples to the Laboratory 

personnel starting with the responsible Senior Chemist. 

3.3 ANALYSIS METHODS 

Table 1 gaseous compounds (Appendix A) will be analyzed using gas chromatography 

with multiple detection for the gaseous compounds. The method generally follows the 

EPA Method TO-15; Determination of Volatile Organic Compounds (VOCs) in Specially 

Prepared Canisters and Analyzed by Gas Chromatography/Mass Spectrometry (GC/MS). 

Carbonyl analysis will be conducted using EPA Method TO-11, Determination of 

Formaldehyde in Ambient Air Using Adsorbent Cartridge Followed by High Pressure 

Liquid Chromatography. These methods are detailed in the EPA Compendium of 

Methods for the Determination of Toxic Organic Compounds14

. 

 

13 Ibid. 

14 Winberry, William, Murphy, Norma & Riggan, R.M. (1988). Compendium of Methods for the 

Determination of Toxic Organic Compounds in Ambient Air. Research Triangle Park, NC: Quality 

Assurance Division, Environmental Monitoring Systems Laboratory, Office of Research and Development, 

US Environmental Protection Agency. (EPA-600/4-84-041) 
MATES III Final Report

Appendix III-17 

3.4 SAMPLING AND ANALYSIS - TABLE 1 COMPOUNDS 

The VOCs and halogenated VOCs found in Table 1 (Appendix A) will be analyzed by 

cryogenic freeze-out to obtain the lowest possible detection limits. These compounds

will be detected using a combination of gas chromatography with mass spectrometry and 

flame ionization detection. A short method description for sampling and analysis of 

VOCs by GC/MS can be found in this document as Appendix M. 

Carbonyl measurement will be conducted utilizing the PAMS sampling and analysis 

methodology delineated in the PAMS Air Monitoring Network Quality Assurance Plan15. 

The Waters ® silica gel cartridge impregnated with dinitrophenyl hydrazine will be used 

to sample for carbonyl compounds. A potassium-iodide-coated ozone denuder will be 

used in all carbonyl samplers. The California Air Resources Board (CARB) toxic 

network design method will be followed using the XonTech 920/924 with a carbonyl 

channel. A short method description for the carbonyl sampling and analysis can be found 

in this document as Appendix H. The ATEC Model 800 sampler will be used for 

sampling at the microscale sites. This model is similar to the AQMD’s PAMS sampler. 

Inorganic measurements will be taken on Teflon filters using XonTech 920/924 samplers 

and analyzed by Energy Dispersive X-ray fluorescence (EDXRF). For the PM2.5 samples, 

a Teflon filter will be used, and EDXRF will be used for analysis of elemental 

constituents. A short method description for sampling and analysis of elements by energy 

dispersive X-ray fluorescence spectrometry is attached to this document as Appendix J.

Proposed for particulate filter samples both in the coarse (PM10) and fine (PM2.5) 

aerodynamic diameter regions will be analyzed for metals, ions, total mass, OC, EC, and 

total carbon (TC). The protocol for mass and ions will follow the same methodology as 

used in the AQMD (federally recognized) PM10 Network. Analysis for EC, OC and TC 

upon the PM10 filter samples will be analyzed using the Interagency Monitoring of 

Protected Visual Environments (IMPROVE) method with some overlapping National 

Institute of Occupational Safety and Health (NIOSH) Method 5040 analysis. Analysis for 

EC, OC and TC upon the PM2.5 filter samples will be analyzed using the IMPROVE 

method with some overlapping NIOSH analyses. Both methods similarly evolve carbon 

from the filters by heating but differ operationally in their temperature and optical 

monitoring protocols. The results of the overlapping analyses between the NIOSH and 

IMPROVE methods will be compared. The results from the IMPROVE and NIOSH 

methods are expected to not be directly comparable, a factor may be realized which will 

allow for a comparison of the future NIOSH data with AQMD’s historical PM database 

consisting of data measured by the IMPROVE method. Furthermore, seasonal and annual 

trend analysis will be conducted on data acquired from air monitoring stations used in 

both MATES II and MATES III. 

 

15 Applied Science & Technology. (1977) PAMS Air Monitoring Network Quality Assurance Plan.

Diamond Bar, CA: South Coast Air Quality Management District. 
MATES III Final Report

Appendix III-18 

The preceding discussion covers all Table 1 compounds (Appendix A) that will be 

sampled on a regular, one-day-in-three sampling schedule synchronized with the national 

PM10 and PM2.5 network schedules. The samples will be integrated over a 24-hour 

period. AQMD personnel will conduct the sampling and analysis. Hired contract 

Instrument Technicians and Chemists will assist regular AQMD employees. 

3.5 SAMPLING AND ANALYSIS - TABLE 2 COMPOUNDS 

Although many Table 2 compounds (Appendix B) do not have a widely recognized 

analytical method, every effort will be made to follow American Society of Test Methods 

or American Industrial Hygiene Laboratory methodologies. The compounds ethylene 

dibromide and ethylene dichloride can be seen on chromatograms of the halogenated 

hydrocarbons analyzed for Table 1 compounds. Since these compounds are rarely used in 

the Basin, they are on the Table 2 list because they will be evaluated on an infrequent 

basis. 

Compounds found in Table 2 are difficult to measure. Some Table 2 compounds may be 

sampled by the AQMD and analyzed by external laboratories. Special efforts may be 

directed to analyzing the ambient air for naphthalene, one of the PAHs. 

3.6 SAMPLING SCHEDULE 

MATES III sampling will be conducted on the same schedule as utilized by the airmonitoring network. The air monitoring network sampling schedule can be found on the 

U.S. EPA website at; www.epa.gov/tnn/amtic , and is for the six-day and three-day 

monitoring schedule for TSP, Pb, PM10, PM2.5 and VOC. Using the same sampling 

schedule results in several benefits: 

1) Data from MATES III can be correlated with the ambient data taken on the 

same day. 

2) Additional staff time to service and maintain MATES III sampling equipment 

and instrumentation is minimized because the existing sampling schedule can 

be largely utilized. 

3) Sample set-up, retrieval, and delivery time to the Laboratory is minimized. 
MATES III Final Report

Appendix III-19 

Microscale site sampling shall be conducted on a similar schedule to MATES III 

sampling. The AQMD will operate two to three microscale site sampling platforms. 

Platforms will be sited for eight weeks at each of a variety of different locations. 

Sampling will occur on days the MATES III fixed sites are sampling. The schedule for 

microscale site sampling is depicted in Table 3-1. Sampling at the microscale sites will 

coincide with the MATES III sampling schedule (that is on a one-day-in-three schedule 

for approximately six weeks. 

Table 3-1 Sample Mobile Platform Sampling Schedule

Mon Tues Wed Thurs Fri Sat Sun 

Week 1 X X X 

Week 2 X X 

Week 3 X X 

Week 4 X X X 

Week 5 X X 

Week 6 X X 
MATES III Final Report

Appendix III-20 

Chapter 4 

Quality Assurance and Quality Control 

4.1 INTRODUCTION 

To achieve the highest possible data quality level in the MATES III, the AQMD has 

implemented the following Quality Assurance/Quality Control (QA/QC) plan. This Chapter 

contains the objectives, procedures, documentation, and data review techniques that will be used 

by the AQMD to assure that the MATES III will produce accurate data. 

4.2 OBJECTIVES 

There are three objectives of the QA/QC procedures for the MATES III. These objectives are: 

(1) to provide accurate and precise data to meet AQMD monitoring requirements; (2) to 

minimize data loss; and (3) to assess air monitoring data quality and provide data that meets the 

QA/QC data quality objectives displayed in Table 4-1. 

TABLE 4-1 QA/QC Data Quality Objectives

 CRITERIA/PARAMETER 

ASSESSMENT MEASURES PROCEDURE VOCs Carbonyls PM10 PM2.5

Accuracy Percent Deviation from 

True Value 

Audits ± 25% ± 25 % ± 10% ± 10% 

 95% Probability Limits < 30% < 30% < 15% < 15% 

Precision Percent Deviation from 

True Value 

Collocation ± 25% ± 25% < 10% < 10% 

 95% Probability Limits < 30% < 30% < 15 % < 15 % 

Completeness Percent of Valid Data 85% 75% 90% 90%

4.3 PROCEDURES

4.3.1 Quality Assurance Procedures 

The AQMD will perform annual flow audits on all PM10 and PM2.5 samplers. These flow audits 

will be conducted according to the procedures outlined in the AQMD’s Quality Assurance Plan 

for Ambient Monitoring, Appendix K. In addition the California Air Resources Board (CARB) 

performs quarterly audits of flows at District air monitoring stations. The CARB also annually 

audits laboratory systems related to mass measurement in the PM2.5 and PM10 networks. The 

EPA and CARB will annually audit the performance of the AQMD Laboratory for VOCs, 

carbonyls and lead (Pb) using the EPA’s National Performance Audit Program and the CARB’s 

toxic VOC performance audit. 

Resources permitting, the AQMD will operate a Xontec 920 for collocated measurement of 

metals, hexchrome and carbonyls at the Rubidoux fixed site. The AQMD will operate collocated 

Hi-Vol PM10 samplers at Rubidoux for a 24-hour average. The collocated samplers will operate 
MATES III Final Report

Appendix III-21 

on a one-day-in-six sampling schedule. VOC sampling will be collocated at Pico Rivera on a 

one-day-in-three sampling schedule. 

The AQMD will endeavor to enlist outside laboratories to analyze a small number of split 

samples for a majority of the compounds measured. The ARB has the capability of performing 

system audits of the AQMD Laboratory, through the probe toxics audits, whole air samples 

(round robins) and will be the primary outside auditor of the program. 

4.3.2 Quality Control Procedures 

A) Field Checks 

 

AQMD staff will perform a number of functions when conducting a field check. Specifically, 

staff will: 

1) observe and record all required data for each sampler’s monthly maintenance sheet, chainof-custody form, and sample identification tag 

2) check and reset all timers if off by more than ± 5 minutes Local Standard Time 

3) check and adjust the flow settings if they are not within ± 5% of the calibrated setting 

B) Laboratory Daily Checks 

AQMD staff will monitor the balance using a NIST traceable check standard; conduct a gas 

chromatograph standard check using a NIST traceable gas standard; will observe, record, and 

correct all sample media equilibration conditions if they are out of tolerance. 

C) Semi-Annual Checks 

AQMD staff will conduct multipoint calibrations of all mass-flow controllers in all samplers; 

perform instrument leak checks; determine the level of detection (LOD) for each analytical 

method; and will clean the PM10 inlet head. 

D) Annual Checks 

AQMD staff will clean the sample probe using de-ionized water and a soft cloth; conduct sample 

probe leak checks and repair if necessary; and will conduct 24-hour tests by operating the 

sampler with a daytime start-stop time to observe actual run length. Actual start and stop must 

be observed. The timer will be repaired if the sample period varies from setting by more than ±

20 minutes. 
MATES III Final Report

Appendix III-22 

4.4 DOCUMENTATION

A critical element of an effective QA/QC system is proper documentation. To ensure that all 

samples are properly handled, inspected, collected, analyzed, and reported, a comprehensive set 

of QA/QC documents will be completed. The information reported in these documents is crucial 

to determining the validity of reported data. Lack of proper documentation can be grounds for 

data invalidation. A summary of QA/QC sampling activities is attached as Appendix L. 

A) Chain-of-Custody Forms 

Chain-of-custody forms (Appendices C, F, F-1 and G) are necessary to identify and control the 

disposition of the samples through the multiple steps of preparation, sampling, retrieval, analysis, 

and data reporting. As appropriate, by sample type, chain-of-custody forms will accompany all 

samples collected in the MATES III and MSS Programs. These forms will be originated by the 

field operators, delivered to the Laboratory, and submitted to the assigned Laboratory staff. The 

Laboratory will be responsible for storing all chain-of-custody documents.

B) Maintenance Check Sheets 

Maintenance check sheets (Appendices D and E) will be completed by field instrument operators 

for the PM10 sampler and ultrasonic wind speed and direction anemometer. These monthly 

maintenance sheets will be submitted to senior field operators for review, approval, and storage.

C) Calibration Reports 

Field and Laboratory staff performing semi-annual and post-repair multipoint calibrations will 

prepare calibration reports. The calibration reports will be reviewed, approved, and retained by 

field and Laboratory staff. 

D) Equipment Relocation Notes (ERN) 

ERNs are an element of the documentation required in MATES III. Because the microscale 

monitoring element involves frequent relocation of equipment, it is the responsibility of the field 

operations supervisor or repair supervisor to note in the station logbooks for each instrument the 

location and time period the instrument was in service. 

E) Station and Equipment Logbooks 

Logbooks are provided for each sampling site and piece of sampling equipment. Each and every 

monitoring station visitor will note the station logbook at each and every visit. The notation 

should include the date, reason for the visit, and the visitor’s clearly identifiable signature or 

initials. Instrument logbooks will be noted each time an instrument is repaired, calibrated, or 

audited. 
MATES III Final Report

Appendix III-23 

4.5 DATA REVIEW

Program data validity is directly attributable to the proper implementation of all the operating and 

QA/QC procedures described in this protocol. To assure that the program’s data quality 

objectives are met, responsibility for data review is distributed between the field operators, 

calibrators, auditors, and supervisors, Laboratory Chemists and Supervisors, QA Supervisors, 

and the Laboratory and Air Monitoring Managers. 

A) Field Supervisors 

Field supervisors are responsible for locating and setting up the sites, scheduling operators, 

training field operators, coordinating supply ordering, supply receipt and distribution, and review 

of monthly QC maintenance sheets. The field supervisors are responsible for notifying the 

Laboratory supervisor of every event that could invalidate the sample. 

B) Field Operators 

Field operators are responsible for operating all samplers and analyzers according to the 

operating procedures specified in this protocol. The field operators must observe and annotate all 

information in the monthly QC maintenance sheets, chain-of-custody forms, sample tags, and 

logbooks. The field operators are responsible for notifying their supervisors of every out-ofcontrol flow setting, timer setting, expected start or ending pressure, or any other instrument 

malfunction. 

C) Field Calibrators 

Field calibrators are responsible for performing semiannual multipoint calibrations on all flow 

control-devices according to AQMD calibration procedures. Any as-is calibration showing a 

deviation from design flowrate in excess of ± 15% will be reported to the field supervisor. Any

samples collected while flow percentage deviation from design flow exceeded ± 15% will be 

invalidated back to the previous flow calibration, audit, or malfunction date. 

D) Field Auditors 

AQMD field auditors will conduct flow audits on 25 percent of the entire network each calendar 

quarter. Auditors are responsible for notifying the QA supervisor of any audit indicating a 

greater than ± 15% average percent deviation from design flow. 

E) QA Supervisor 

The QA Supervisor is responsible for reviewing field audit reports, scheduling audits, 

coordinating with ARB QA staff, and compiling and reporting QA flow accuracy reports. 
MATES III Final Report

Appendix III-24 

F) Laboratory Chemists 

The Laboratory Chemists are responsible for receiving field samples, maintaining and storing 

chain-of-custody documents, performing and documenting QC activities on the QC monthly 

maintenance sheets, performing Laboratory audit analyses, and conducting preliminary data 

analysis for outliers and out-of-control conditions. 

G) Laboratory Supervisor 

The Laboratory Supervisor is responsible for final raw data review; calculation of precision based 

upon collocated sampling; reviewing monthly QA/QC sheets; making final evaluation of data 

validity based on satisfactory reports from QA supervisor and field supervisor; and assessment of 

Laboratory precision data. 

H) Air Monitoring Manager 

The Air-Monitoring Manager is responsible for overseeing field operations and QA auditing 

operations. 

I) Laboratory Manager 

The Laboratory Manager is responsible for overall coordination of MATES III and for ensuring 

that all staff fulfills their responsibilities as detailed in this protocol. Additionally, the 

Laboratory Manager is responsible for establishing the final acceptance criteria for sample 

validity once actual precision and accuracy data become available. 
MATES III Final Report

Appendix III-25 

Chapter 5.0 

Data Processing and Reporting 

5.1 INTRODUCTION 

MATES III monitoring for ambient air toxics will develop a large data resource for future 

analysis. Table 1 compounds, when multiplied by the projected frequency of sampling in 

MATES III, will result in more than 20,000 individual data points representing a concentration of 

a toxic compound at a particular time and location. The purpose of this chapter is to outline the 

data handling of such a large database. This section will only pertain to the laboratory work 

performed and not to the meteorological, criteria pollutant, or monitor calibration data. 

The AQMD Laboratory has had prior experience handling such a large data base as part of 

MATES II. Reporting templates for the carbon analysis and XRF elemental analysis (inorganics) 

will follow the outline used in MATES II. Reporting templates for the VOCs, halogenated 

hydrocarbons, and carbonyls will follow the PAMS format. 

The aim of the reporting will be to generate Excel data files for electronic transfer to interested 

parties. The data will be checked for transcription errors and quality assured to represent the 

most accurate determinations possible. The Laboratory will strive to disseminate the data in a 

timely fashion to facilitate feedback. 

5.2 DATA BASE COMPILATION 

The Laboratory Chemists will generate a data point representing the concentration of a particular 

compound found over a particular time period at a particular site. The instrument analyzes the 

sample and determines the volume concentration on a parts-per-billion basis. These 

concentration numbers will be compiled into a spreadsheet along with the name of the sampling 

site and the date the sample was taken. The Chemist (analyst) is responsible for checking data 

point accuracy. The technician in charge of copying the data points into the spread sheet is 

responsible for their accurate transcription. The Senior Chemist is in charge of double checking 

the Chemists’ and technicians’ data transcription work. 

If resources permit, one Chemist will operate the instrument while another Chemist reduces the 

data and transcribes it to the Excel spreadsheet. This method would lead to the quickest 

turnaround time possible. One Chemist may reduce the data from several instruments depending 

on the workload. 

MATES III data will encompass PM10 and PM2.5 mass, ions for both fractions, VOCs, carbonyls, 

XRF, ICP/MS and carbon analysis results. The run date will be encoded with the year, month, 

and day in six numerals. This information will be followed by a two-letter acronym representing 

the station and concentration. The column header has the name of the compound and the 

concentration units. Uncertainties were given for each data point. These uncertainties 

encompass the calculated limits for the sampling and analysis errors introduced into the 

measurement system. 
MATES III Final Report

Appendix III-26 

The MATES III data will be compiled into several spreadsheets. These spreadsheets will 

conjugate components along the lines of the analysis technique. Each instrument will have a 

separate spreadsheet for the compounds it analyzes. 

The Laboratory can work with the end data user to supply the electronic version in whatever file 

length or configuration is desired. The data can also be translated into ASCII flat files. 

5.3 PERIODIC REPORTS 

The Laboratory will strive to meet a two-month turnaround time from the date of sampling to the 

finished and checked report. The VOCs, carbonyls, XRF, and carbon analyzer will all be 

sampled individually, yet in very similar formats. Extra effort will be made to analyze duplicate 

samples and other QC samples and compile into a separate report for monthly reporting. The 

reports will be available in electronic file and printed spreadsheets. 

5.4 FINAL REPORT 

Past experience has proven that the final report including the QA report can take from four to six 

months after the last day of sampling to complete. The data will be compiled on a monthly basis, 

and the final report is slated to be complete within two months of the end of sampling. 

Resources permitting, Laboratory staff will migrate the Excel spreadsheets to the Access 

database software. The final report will be stored in several files segregated by date and analysis. 

The AQMD Laboratory has the ability to write the files to CD-ROM. Only limited hard copies 

of the report will be printed. 
MATES III Final Report

Appendix III-27 

Glossary 

Quality Assurance (QA) 

 The practice of establishing procedures external to the day-to-day monitoring operations that 

indicate whether or not air quality data is accurate, representative, precise and complete enough 

to satisfy the needs of the data users. QA activities include, but are not limited to, system and 

performance audits and collocated and parallel sampling. These activities are described in detail 

in Chapter 4. 

Quality Control (QC) 

 Any procedure incorporated into the internal, day-to-day operations of collection and analysis of 

air quality samples to satisfy the data user’s need for valid data. These activities are described in

detail in Chapter 4. 

Accuracy 

A determination of how closely reported data values are to true values. Annually conducted 

performance audits will challenge the various samplers and instruments used in this program to 

assess their accuracy. All program data accepted as valid will meet the criteria set forth in Table 

4-1. Accuracy is expressed as “percent” deviation from true and is calculated as follows: 

 Percent Deviation from 

True 

= Indicated Value - True Value

True Value 

x 100 

Precision 

The measure of monitoring system repeatability. Precision is determined by amassing a variety 

of measurements of the same true value over a period of time and assessing the variability of 

those measurements. Precision objectives for the various monitoring methods used in MATES II 

and MSS programs are presented in Table 4-1. 

Data Completeness (DC) 

 The percent of valid data points actually collected out of the total number of data points possible. 

The data completeness objectives for the MATES II and MSS programs are presented in Table 4-

1. DC is calculated using the following formula: 

 percent DC = Total valid data points 

Total number of possible data points 

 x 100 

 

Representativeness 

 The goal that samples are representative of both temporal and/or spatial scales at all sites. This is 

accomplished by conforming to 40CFR58 siting and sampling requirements for PM10. 

Performance Audit 

 A procedure conducted to establish individual analyzer and overall sampling and analysis 

accuracy. Probe audits are used to measure the integrity of both the sampling and analysis 
MATES III Final Report

Appendix III-28 

systems. Flow audits measure the accuracy of the flow metering devices that assure the sample’s 

temporal representativeness. Gas standard audits determine accuracy of laboratory analyzers in 

measuring known concentrations of toxic compounds. 

System Audit 

An on-site inspection and review of the entire monitoring program. 

Collocated Sampling 

 The process of running two identical samplers concurrently at the same location. Collocated data 

measures a method’s precision. One of the samplers is designated A and is treated as the true 

value; while the other sampler is designated B and is regarded as the indicated value. 

Parallel Sampling 

 The process of two different agencies such as the AQMD and ARB operating two different 

samplers side-by-side. 
MATES III Final Report

Appendix III-29 

ACRONYM LIST 

AC alternating current 

AIHL American Industrial Hygiene Laboratory 

AM Air Monitoring 

AQMD South Coast Air Quality Management District 

ARB Air Resources Board 

AST Applied Science and Technology 

ASTM American Society of Test Methods 

Basin South Coast Air Basin 

cc cubic centimeters 

ccm cubic centimeters per minute 

cfm cubic feet per minute 

CFR Code of Federal Records 

DC direct current 

DNPH 2, 4-dinitrophenyl-hydrazine 

EDB ethylene dibromide 

EDC ethylene dichloride 

EJ-2 Environmental Justice Initiative Number 2 

EPA Environmental Protection Agency 

EPROM erasable prompt chip 

ERN equipment relocation notice 

ETM elapsed time meter 

FPC filter paper cartridge 

HPLC High Performance Liquid Chromatograph 

ICP/MS Ion coupled Plasma/Mass Spectrometry 

LIMS Laboratory Information Management System 

LOD Level of Detection 

lpm liters per minute 

MATES II Multiple Air Toxics Study II 

MATES III Multiple Air Toxics Study III 

MFC mass flow controller 

mph miles per hour 

MSS Microscale Study 

MTBE methyl tert butyl ether 

NAMS National Air Monitoring Stations 

NEMA National Equipment Manufacturer’s Association 

PAH polycyclic aromatic hydrocarbon 

PAMS Photochemical Assessment Monitoring Station 

PM particulate matter 

ppb parts per billion 

ppbC parts per billion carbon 

PSI pounds per square inch 

PST Pacific Standard Time 

PTEP Particulate Technical Enhancement Program 
MATES III Final Report

Appendix III-30 

PUF polyurethane foam 

QA quality assurance 

QC quality control 

RAM random access memory 

rms root mean standard 

SASS speciation air sampling system 

SCAQMD South Coast Air Quality Management District 

SCC sharp cut cyclone 

SCFM standard cubic feet per minute 

SLAMS State and Local Air Monitoring Stations 

SOP standard operating procedure 

SSI size selective inlet 

TAC toxic air contaminant 

TSP total suspended particulates 

V Volt 

VOC volatile organic compound 

WSD wind speed and direction 

XRF X-ray fluorescence
MATES III Final Report

Appendix III-31 

APPENDIX A Proposed Table 1 Air Contaminants for Inclusion in the Measurement 

Program 

 (Compounds in bold are proposed for U.S EPA AIRS database reporting) 

CAS No. Chemical Name Lab Test Method Sampling Freq. Comment 

VOCs 

71-43-2 Benzene GC/MS/FID 1 in 3 days 

106-99-0 Butadiene [1,3] GC/MS/FID 1 in 3 days

(o-) 95-50-1 Dichlorobenzene [ortho- & para] GC/MS/FID 1 in 3 days

100-41-4 Ethyl Benzene GC/MS/FID 1 in 3 days

100-42-5 Styrene GC/MS/FID 1 in 3 days

108-88-3 Toluene GC/MS/FID 1 in 3 days

(m-) 108-38-3 Xylene [m+p, o-] GC/MS/FID 1 in 3 days

75-01-4 Vinyl chloride GC/MS/FID 1 in 3 days

Halo-HCs 

56-23-5 Carbon tetrachloride GC/MS/FID 1 in 3 days

67-66-3 Chloroform GC/MS/FID 1 in 3 days

75-09-2 Methylene chloride (Dichloromethane) GC/MS/FID 1 in 3 days

127-18-4 Perchloroethylene (tetrachloroethene) GC/MS/FID 1 in 3 days

78-87-5 Propylene Dichloride (1,2-dichloropropane) GC/MS/FID 1 in 3 days Not in MatesII 

79-01-6 Trichloroethylene GC/MS/FID 1 in 3 days

Carbonyls 

75-07-0 Acetaldehyde HPLC 1 in 3 days

67-64-1 Acetone HPLC/ GC/MS/FID 1 in 3 days Not Reported 

50-00-0 Formaldehyde HPLC 1 in 3 days

78-93-3 Methyl ethyl Ketone (MEK) HPLC/GC/MS/FID 1 in 3 days Not Reported 

1634-04-4 Methyl tert-Butyl Ether (MTBE) HPLC/GC/MS/FID 1 in 3 days Not Reported 

Inorganics 

7429-90-5 Aluminum ICP/MS:XRF 1 in 3 days

7440-38-2 Arsenic ICP/MS:XRF 1 in 3 days

7440-41-7 Beryllium ICP/MS:XRF 1 in 3 days

7440-43-9 Cadmium ICP/MS:XRF 1 in 3 days

7440-70-2 Calcium ICP/MS:XRF 

7440-47-3 Chromium (total) ICP/MS:XRF 1 in 3 days

 Chromium (hexavalent) IC 1 in 3 days 

7440-48-4 Cobalt ICP/MS:XRF 1 in 3 days

7440-50-8 Copper ICP/MS:XRF 1 in 3 days

7439-89-6 Iron ICP/MS:XRF 1 in 3 days

7439-92-1 Lead ICP/MS:XRF 1 in 3 days

7439-95-4 Magnesium ICP/MS:XRF 

7439-96-5 Manganese ICP/MS:XRF 1 in 3 days

7440-02-0 Nickel ICP/MS:XRF 1 in 3 days

7723-14-0 Phosphorous ICP/MS:XRF 1 in 3 days

7440-09-7 Potassium ICP/MS:XRF 1 in 3 days

7782-49-2 Selenium ICP/MS:XRF 1 in 3 days

CAS No. Chemical Name Lab Test Method Sampling Freq. Comment 

7440-21-3 Silicon ICP/MS:XRF 1 in 3 days 

7440-62-2 Vanadium ICP/MS:XRF 1 in 3 days 

7440-66-6 Zinc ICP/MS:XRF 1 in 3 days

Others

Elemental & organic carbon C analyzer 1 in 3 days

Criteria Pollutants

PM2.5 SASS 1 in 3 days Speciation

PM10 SSI-Hivol 1 in 3 days PM network
MATES III Final Report

Appendix III-32 

APPENDIX B Proposed Table 2 Air Contaminants that Potentially May Be Monitored on 

 A Limited Basis

Laboratory 

CAS No. Chemical Name Test Method Comment 

VOCs 

 Acrolein No ambient method

 

Halo-HCs 

106934 Ethylene dibromide {EDB} GC/MS 

107062 Ethylene dichloride {EDC} GC/MS 

 

Others 

 PAHs HPLC Send out for analysis 

 Napthalene HPLC Send out for analysis 

Diesel exhaust “Markers” TBD Send out for analysis 
MATES III Final Report

Appendix III-33 

APPENDIX C Size-Selective Inlet PM10 Sampler Envelop

South Coast Air Quality Management District 

Applied Science & Technology 

Size-Selective Inlet PM10 Sampler Envelop 

 

 FIELD OPERATOR USE  LABORATORY USE ONLY 

 



STATION #  SAMPLE # 

 

LOCATION  FLOWRATE, CFM 

 

SAMPLER #  VOLUME OF AIR, M3

 

QUARTZ 

FILTER #  FINAL WEIGHT (gm) 

 

DATE  TARE WEIGHT (gm) 

 

TIME  SAMPLE WEIGHT (gm) 

 

 END  PM10(μg/M3) 

 

 START  SAMPLE RECV’D 

 

 TOTAL 

 

REMOVED FROM SAMPLER  SAMPLE WEIGHED 

 

SENT TO HQ  SAMPLE EXTR. 

 

RECEIVED AMB  SAMPLE ANALYSIS 

 

  REF. 

 DATE SAMPLER CALIBRATION 

 STATION OPERATOR 

 Remarks (unusual activities sampling conditions, etc.): 
MATES III Final Report

Appendix III-34 

APPENDIX D WSD Monthly Quality Control Maintenance Check Sheet

SOUTH COAST AIR QUALITY MANAGEMENT DISTRICT 

MONTHLY QUALITY CONTROL MAINTENANCE CHECK SHEET 

MAKE/MODEL Wind Speed and Direction System 

Location Month/Year 

Station No. Specialist 

Control No. Reviewed by Date 

Zero Speed Zero Direction Visual Wind Chart Time 

Date As Found Final As Found Final Transmitter Check As Found Final 

 

 

 

 

 

 

 

 

OPERATOR INSTRUCTIONS: 

Daily Checks: Chart trace and time. 

Weekly Checks: Zero speed and direction inking system 

Visual wind transmitter check. The station operator will visually check the wind transmitter to confirm the 

direction coincides with recorder. Notify supervisor immediately if problem occurs. 

Bi-monthly 

Maintenance: 

DATE COMMENTS OR MAINTENANCE PERFORMED 

Calibration Date: Operator 
MATES III Final Report

Appendix III-35 

APPENDIX E High Volume Monthly Quality Control Maintenance Check Sheet 

High Volume 

Monthly Quality Control Maintenance Check Sheet 

MAKE/MODEL HIGH VOLUME SAMPLER 

Location Month/Year 

Station No. Specialist 

Control No. Reviewed by/Date 

Operating Set Point Cubic Feet per Meter 

Date SSI Head Cleaned Due Date 

Sample 

Date 

Initial 

Flow 

cfm 

Final Flow 

cfm 

Filter 

No. 

Initial 

Elapsed 

Time 

Final 

Elapsed 

Time 

Total 

Time 

1 

2 

3 

4 

5 

6 

7 

8 

9 

10 

11 

12 

13 

14 

15 

16 

17 

18 

19 

20 

21 

22 

23 

24 

25 

26 

27 

28 

29 

30 

31 
MATES III Final Report

Appendix III-36 

APPENDIX F MATES III Sample Log 

South Coast Air Quality Management District 

	

 	



Location: 

Sample Date: 

Station No.: 

Retrieved By: 

Retrieval Date: 

Canister Log – XonTech 910 

Sample 

Time 

Canister 

 No. 

Start 

Vacuum 

End 

Pressure 

Comments 

24 hour 

Blank 

Collocated 

DNPH Cartridge Log – XonTech 920 

Sample 

Time 

Cartridge 

No. 

Elapsed 

Time 

Flow Rate Comments 

24 hour 

Blank 

Collocated 

Filter Log – XonTech 920 

Sample Time Filter No. Flow Rate Comments 

Teflon (Metals) 

Cellulose (Chrome VI) 

PM10 (Hi-Vol) 

 

 Lab No.: 

 Date Sample Received: 

 Reference No.: 

 Analyst: 

 Lab No.: 

 Date Sample Received: 

 Reference No.: 

 Analyst: 

(Staple Printout Here) 
MATES III Final Report

Appendix III-37 

APPENDIX F-1 MATES III Sample Log 

South Coast Air Quality Management District 


	

 
	



Location: 

Sample Date: 

Station No.: 

Retrieved By: 

Retrieval Date: 

Canister Log – XonTech 910 

Sample 

Time 

Canister 

 No. 

Start 

Vacuum 

End 

Pressure 

Comments 

24 hour 

0-8 hour 

8-16 hour 

16-24 hour 

DNPH Cartridge Log – XonTech 920 

Sample 

Time 

Cartridge 

No. 

Elapsed 

Time 

Flow Rate Comments 

24 hour 

0-8 hour 

8-16 hour 

16-24 hour 

Filter Log – XonTech 920 

Sample Time Filter No. Flow Rate Comments 

Teflon (Metals) 

Cellulose (Chrome VI) 

PM10 (Hi-Vol) 

 Lab No.: 

 Date Sample Received: 

 Reference No.: 

 Analyst: 

 Lab No.: 

 Date Sample Received: 

 Reference No.: 

 Analyst: 

(Staple Printout Here) 
MATES III Final Report

Appendix III-38 

APPENDIX G VOC Canister Tag

 VOC CANISTER TAG

SCAQMD PAMS CAN 

# 

 

STATION LAB 

Code Date Time Initial Analysis Clean 

 

Notes 

 

Notes 

 

Notes 

 

Notes 

 

Notes 

 

Notes 

 

Notes 

 

Notes 

 

Notes 

 

Notes 

 

Notes 

 
MATES III Final Report

Appendix III-39 

APPENDIX H Method Description for Sampling and Analysis of Carbonyls by 

 HPLC at the AQMD Laboratory

Sampling - Ambient air is drawn through a glass and/or stainless steel probe at the air 

monitoring site and pulled through DNPH coated silica cartridges mounted in the A-Tech 800 

sampler. The sampling cartridges are coated with a minimum of 300 mg of DNPH on Waters 

Sep-Pak silica cartridges. The sample is pulled through the cartridge at approximately one lpm 

for 8-hour sampling and at 0.7 lpm for 24-hour sampling. Before and after sampling the 

cartridges are kept capped and refrigerated in small vials to prevent loss and contamination. 

Laboratory Analysis- The laboratory uses a Waters Millennium system high performance liquid 

chromatograph (HPLC) with autosampler. After elution of the Sep-Pak cartridge with 3 

milliliters of acetonitrile, the samples are placed in the autosampler. Samples are run 

isocratically (55% acetonitrile and 45 % H20) on a Waters C-18, 5 micron, 4.6 mm by 250-mm 

column. Flow is one milliliter per minute. Twenty microliters are injected onto the column by 

the autosampler. 

Quantification - A calibration curve is derived from multipoint injections of standards obtained 

from Radian Corporation. One point control standards are run daily with the sample analysis. 

PAMS compounds, acetaldehyde, formaldehyde, and acetone, are quantified by comparison to 

the calibration curve. 

QA/QC- The limit of detection is determined for the HPLC response and the system LOD is 

calculated for a typical air volume sampled. A collocated cartridge is run every 6 days of 

sampling in the field. Blank cartridges are run at a similar frequency. Replicate samples are run 

every ten samples. 

 
MATES III Final Report

Appendix III-40 

APPENDIX I Method Description for Sampling and Analysis of Elements by Energy 

 Dispersive X-ray Fluorescence Spectrometry at the AQMD Laboratory

Sampling-Ambient air is drawn through a 47 mm Teflon filter loaded in a TSP or PM2.5 sampler. 

Typically, 24 hour sampling at about 20 lpm provides sufficient sample mass on the filter for a 

successful analysis. The sampler must collect a homogeneous sample across the surface of the 

filter. The Kevex XRF instrument examines a very small cross section of the filter near the 

center. 

Laboratory Analysis-A Kevex Energy Dispersive X-ray fluorescence spectrometer is used to 

analyze 35 elements in the filter sample. There is no need for sample preparation other than 

bringing the filters to room conditions. Each filter is loaded onto a sample wheel brought to a 

vacuum and scanned under five different instrumental conditions. Each condition is optimized 

for certain groups of elements. After spectral acquisition, an identification and deconvolution 

process extracts the net contributions of counts of each of the 35 elements. 

Speciation and Quantification-Each element has a unique spectral pattern. After accounting 

for overlaps, each of the elements is identified qualitatively. By using previously calibrated 

standard values the net counts for each element are converted to actual concentrations in 

μg/filter. Using air volume data gathered during sampling, the μg/filter concentrations of the 

elements are converted to μg/M3

. 

QA/QC-The X-ray analytical instrument is calibrated using 35 single element standards. These 

calibration standards are checked using an NIST multi-element film standard. Filter blanks are 

analyzed for subsequent background correction during the spectral analysis of the run. Field 

blanks are taken at specified times depending on the frequency of sampling. Field blank results 

are either subtracted or reported in accordance with data reporting and analysis requirements. 

Finally, collocated runs are utilized to check precision. 
MATES III Final Report

Appendix III-41 

APPENDIX J Method Description for Sampling and Analysis of Elements by Energy 

 Dispersive X-ray Fluorescence Spectrometry at the AQMD Laboratory

Sampling-Ambient air is drawn through a 47 mm Teflon filter loaded in a TSP or PM2.5 sampler. 

Typically, 24 hour sampling at about 20 lpm provides sufficient sample mass on the filter for a 

successful analysis. The sampler must collect a homogeneous sample across the surface of the 

filter. The Kevex XRF instrument examines a very small cross section of the filter near the 

center. 

Laboratory Analysis-A Kevex Energy Dispersive X-ray fluorescence spectrometer is used to 

analyze 35 elements in the filter sample. There is no need for sample preparation other than 

bringing the filters to room conditions. Each filter is loaded onto a sample wheel brought to a 

vacuum and scanned under five different instrumental conditions. Each condition is optimized 

for certain groups of elements. After spectral acquisition, an identification and de-convolution 

process extracts the net contributions of counts of each of the 35 elements. 

Speciation and Quantification-Each element has a unique spectral pattern. After accounting 

for overlaps, each of the elements is identified qualitatively. By using previously calibrated 

standard values the net counts for each element are converted to actual concentrations in 

μg/filter. Using air volume data gathered during sampling, the μg/filter concentrations of the 

elements are converted to μg/M3

. 

QA/QC-The X-ray analytical instrument is calibrated using 35 single element standards. These 

calibration standards are checked using an NIST multi-element film standard. Filter blanks are 

analyzed for subsequent background correction during the spectral analysis of the run. Field 

blanks are taken at specified times depending on the frequency of sampling. Field blank results 

are either subtracted or reported in accordance with data reporting and analysis requirements. 

Finally, collocated runs are utilized to check precision. 
MATES III Final Report

Appendix III-42 

APPENDIX K Method Description for Sampling and Analysis of Organic and Elemental 

 Carbon by Thermal/Optical Carbon Analyzer at the AQMD Laboratory 

Sampling-Ambient air is drawn through a 47-mm quartz filter loaded in a PM2.5 sampler or an 8 

x 10 inch quartz fiber filter loaded in a SSI-Hi-Vol sampler. Typically, 24-hour sampling 

provides sufficient sample mass on the filter for a successful analysis. The sampler must collect 

a homogeneous sample across the surface of the filter. A one-centimeter diameter punch from 

any quadrant of the filter is used in the instrument. 

Laboratory Analysis-A Desert Research Institute (Reno, Nevada) thermal/optical carbon 

analyzer is used to determine the total carbon content of aerosol deposited on quartz filters. The 

analyzer is able to distinguish and characterize organic and inorganic carbon by a thermal/optical 

method with flame ionization detection. There is no need for sample preparation other than 

bringing the filters to room conditions. A small circular filter area is punched out from the quartz 

filter and loaded on to the carrier quartz tube. The filter is pushed into an oven whose 

temperature is raised in steps from ambient to approximately 850 degrees Celsius. An inert gas, 

such as nitrogen is continuously passed over the filter. At the same time the surface of the filter 

is monitored with a laser beam to determine the exact point at which all the elemental carbon 

(soot) is burned off. The combusted carbon forms carbon dioxide that is carried over to a 

methanizer. The methanizer (active nickel with the addition of hydrogen gas) converts the 

carbon dioxide to methane. The methane flows to a flame ionization detector. The detector 

output is integrated and converted to μg of carbon per filter using previously calibrated standards. 

Speciation and Quantification-The light organic fraction is driven off the filter at the early 

stages of heating. The elemental carbon fraction is then oxidized at a higher temperature with an 

oxygen enriched carrier gas. A laser beam constantly scanning the filter surface indicates the 

exact point at which the organic and elemental carbon fractions are removed from the filter. The 

two fractions are summed to give the total carbon concentration of the sample. The analysis 

results in the elemental, organic, and total carbon content of the sample. Using air volume data 

gathered during sampling, the μgC/filter concentrations are converted to μgC/M3 of air. 

QA/QC-The optical-thermal carbon analyzer is calibrated using two types of standards. One set 

consists of carbon containing gases, methane and carbon dioxide in an inert gas mixture. These 

are passed through the entire system to calibrate the instrument. In addition, filters impregnated 

with solution containing a known concentration of carbon are run as external standards. Filter 

blanks are analyzed for subsequent background correction during the run. Field blanks are taken 

at specified times depending on the frequency of sampling. Field blank results are either 

subtracted or reported in accordance with the data reporting and analysis requirements. Finally, 

collocated runs are utilized in checking precision.
MATES III Final Report

Appendix III-43 

APPENDIX L QA/QC Matrix Summary 

Process Interval Activity Criteria Correctiv Before & After Each 

Sampling Event

QC - Note Activities in Log Book, Canister Tag, Chain-of-Custody

Notes For Each Canister N/A 

 QC - Check Chart Time ± 10 Minutes of Actual PST AQIS ReseField Canister Annually QC - Clean Manifold Pass Leak Check AM SuppoSampler QC - Calibrate Flow ± 5 % True Flow AM Opera 1 Day in 3 QA - Collocated Sample 10 % Of Network Run A + B  Annually QA - ARB Through-the-Probe Audit Within ± 25 % of True For all Compounds Isolate & R QA - Flow Audit Indicated Flow Must Be Within ± 10 % of True Flow Notify Ope Before & After Each QC - Note Activities in Log Book N/A N/A 

Sampling Event QC - Check Start & Stop Times & Volume 

For Each Sample.

Note On Canisters Log Sheet AQIS Rese

Field Carbonyl QC - Clean Manifold Pass Leak Check AQIS CleaSampler Annually QC - Calibrate Flow Controller ± 5 % True Flow AM OperaIf Equipment 1 Day in 6 QA - Collocated Sample 10 % of Network Run A + B Available Annually QA - Through-the-Probe Audit By ARB Within ± 25 % of True For All Compounds Isolate & R QA - Flow Audit Indicated Flow Must be Within ± 10 % of True Flow Notify Ope QC - Chain-of-custody Log Sheet & Cartridge Numbers Agree Chemist C QC - Propane Peak ± 10 % Of Previous Chemist A

Daily QC – System Blank < 10 ppb/C Total NMOC Chemist R QC – Replicate Sample Visual Evaluation of Chromatogram Chemist R

Laboratory GC

Semiannually QC – Replicate Standard Analysis ± 10 % on All Compounds Chemist R

 QC - Bias Check 2 ppb/C Per Compound Chemist RAnnually QC - LOD Check All Loads Must Be Less Than 1 ppb/C Chemist R1 Day In 6 QA – Collocated Samples ± 25 % On All Compounds Chemist RQuarterly QA – Parallel Sampling All Compounds Must Be Within ± 30 % Annually QA – NPAP Performance Audit Within ± 30 % of True For All Compounds Chemist R QC – Standard Response ± 10 % of Previous Chemist RDaily QC – Purge Cycle System Pressure Between 800 & 1700 PSIG Chemist L

Laboratory Carbonyl

Semiannually QC – Multipoint Calibration ± 10 % Of Previous Chemist D

 QC - Bias Check <3 ppb Per Compound Chemist RAnnually QC - LOD Check <1 ppb Per Compound Chemist RQuarterly QA – Parallel Sampling All Compounds Must Be Within ± 30 % Annually QA – NPAP Performance Audit Within ± 30 % of True For All Compounds Chemist R

 Before & After Each Sample 

Run

QC - Note the Maintenance Sheet, Log Book, & Sample Envelope

Notes as Required N/A 

 Semiannually QC – Change Motor & Multipoint 

Calibration

Create New Calibration Curve N/A 

 QC - Clean Inlet Field PM10 SSI Annually QC - Timer Check Timer Tested For Start With 20 Minutes of Setting & Elapsed 

Time to Within 20 Minutes

Repair or R

 1-Day-in- 6 QA - Collocate Run At 10 % Of Sites N/A  Annually QA - Flow Audit Actual Flow Must be Within ± 10 % of True Flow Request R QC - Balance Checks Laboratory Daily QC - Inspect Filters No Light Leaks or Tears PM10 SSI QC - Equilibrate Filters 

1 Day in 6 QA - Collocate Filters Agreement Within ± 20 %, all Compounds 
MATES III Final Report

Appendix III-44 

Appendix M Method Description for Sampling and Analysis of VOCs by GC/MS at 

 the AQMD 

Sampling- Ambient air is pumped into an evacuated Summa® polished 6 liter canister by 

a Xontech 910A air sampler at the sample location through a properly sited probe and 

manifold. The sample is integrated over 24 hours to fill the canister to approximately 10 

PSI. The canister is returned to the laboratory for subsequent analysis by Gas 

Chromatography with a Mass Spectrometer Detector (GC/MS). 

Laboratory Analysis- The Laboratory uses a Hewlett-Packard 6890 Gas Chromatograph 

with an HP 5973 Mass Selective Detector. The sample is concentrated with an Entech 

7100 cryo-concentrator for input to the GC/MS. The sample canister is attached to the 

cryo-concentrator and a 400-milliliter aliquot (600 ml for MSS samples) is chilled in a 

trap to minus 150 degrees centigrade. For removal of the fixed gases the trap is heated to 

20 degrees centigrade and transferred to a second trap cooled to -45 C for mitigation of 

the CO2 and H2O collected. The concentrator loop is then heated and the contents cryofocused at the head of the GC column for subsequent separation of the VOCs. The mass 

selective detector records the mass spectrum of each peak (compound) and the analyst 

uses previously determined standards to compare selected ions for each compound to 

determine the concentration. 

Quantitation- A calibration curve is derived by injection of a gas standard containing the 

compounds of interest at ppb levels. Every sample run is preceded and ended with a 

calibration check. Every analysis day is begun with a system blank run. Selected 

quantitation ions for each compound are compared to the gas standards injected to 

determine concentration in parts per billion. 

QA/QC-The Limit of Detection (LOD) is determined for the GC/MS by multiple 

injections of the lowest standard amount available (within 10 times the estimated LOD). 

Collocated samples are run in the field at one station. All canisters from the canister 

cleaning system are filled with the purified nitrogen and tested for the presence of the 

compounds of interest. Above 0.2 ppb of any compound of interest or 4 ppb total of all 

compounds (ppbc) is cause for corrective action.