Method 0023A: Sampling Method for Polychlorinated Dibenzo-p-Dioxins and Polychlorinated Dibenzofuran Emissions from Stationary Sources, part of Test Methods for Evaluating Solid Waste, Physical/Chemical Methods

Analyte
Concentration
Concentration
Method 0023
Method 8290
(pg/µL)
(pg/µL)
1
Internal Standards
C -2,3,7,8-TCDD
13
12
C -1,2,3,7,8-PeCDD
13
12
C -1,2,3,6,7,8-HxCDD
13
12
C -1,2,3,4,6,7,8-HpCDD
13
12
C -OCDD
13
12
C -2,3,7,8-TCDF
13
12
C -1,2,3,7,8-PeCDF
13
12
C -1,2,3,6,7,8-HxCDF
13
12
C -1,2,3,4,6,7,8-HpCDF
13
12
Surrogate Standards
Cl -2,3,7,8-TCDD
37
4
C -1,2,3,4,7,8-HxCDD
13
12
C -2,3,4,7,8-PeCDF
13
12
C -1,2,3,4,7,8-HxCDF
13
12
C -1,2,3,4,7,8,9-HpCDF
13
12
Recovery Standards
C -1,2,3,4-TCDD
13
12
C -1,2,3,7,8,9-HxCDD
13
12
Alternate Standard
C -1,2,3,7,8,9-HxCDF
13
12
100
10
100
10
100
25
100
25
100
50
100
10
100
10
100
100
25
100
100
100
100
25
100
500
50
500
50
100
--
Provided as reference only; also see Method 8290.
1

CD-ROM
0023A - 24
Revision 1
December 1996
TABLE 2
SAMPLING QC PROCEDURES SUMMARY
QC Procedure
Frequency
Criteria
Sample equipment
See Sec. 6.3.1
See Sec. 6.3.1
calibrations
Dry gas meter sample leak
Before and after each
0.00057 cmm (
# 0.02 cfm) or
check
test run
4% of sample rate whichever
is less at highest vacuum
O and CO sampling system
Once per test
See Method 3, or equivalent
2
2
leak check
for Method 3A
)P meter leveling
Before and after each
Level
test run
Pitot tube leak check
Before and after each
No visible leak observed at
test run
75 mm (3 in.) H O for
2
15 seconds
Pitot tube orientation check
Every test
Pitot tube is level with no
visible rotation from
perpendicular to flow
Cyclonic flow check
Made at every location
< 20
E average offset from
perpendicular to flow
Probe, filter, trap, and silica
Every test
See Sec. 4.0
gel impinger are maintained
at specified temperature
ranges
Overall isokinetic sampling
Every test
± 10% of 100%
rate
Sampling blanks
See Sec. 8.2
See Sec. 8.2

CD-ROM
0023A - 25
Revision 1
December 1996
TABLE 3
REQUIREMENTS FOR ANALYTICAL PREPARATION, 
SURROGATE RECOVERIES AND SAMPLE BLANKS
Item
Description
Control Limit
Precleaning filters
Soxhlet extraction
Detection limits listed in Sec. 9.2
Precleaning sorbent
Soxhlet extraction
Detection limits listed in Sec. 9.2
Filter and sorbent
Isotopically-labeled
70 to 130% recovery
surrogate spikes
compounds
Field blank
Collect one for every 9
< 5 times the detection limits
sample runs at each test
location
Method blank
Prepared at analytical
Criteria decided by laboratory QA
laboratory (laboratory
officer
blank). One per analytical
batch
Reagent blanks
One per lot of solvent used. 
Analyze only if requested by
Archive for possible analysis
Agency to determine source of
field blank confirmation
Proof Blank
One per set of glassware. 
Analyze only if requested by
Archive for possible analysis
Agency to determine source of
(collect only if requested by
field blank contamination
Agency)

CD-ROM
0023A - 26
Revision 1
December 1996
TABLE 4
SAMPLE EQUIPMENT CALIBRATION SUMMARY
Equipment
Procedure
Frequency
Control Limits
Primary WTM or
Primary calibration
Every 12
± 1% average
a
DGM
months
a
Sample DGM
Full calibration
Every 6 months
Y
# 2% from Y
i
avg
Sample DGM
Post calibration
After each test
Y
# 5% from Y
program
post
full
Thermometers, 
Calibration check
Initially
± 2
EC (3.6EF) at 3
Thermocouples 
point calibration from
reference
thermometer
Nozzle
ID calibration
Before every
Repeated
test program
measurements
± 0.1 mm (0.004 in.)
Pitot tube
Wind tunnel
Before every
Specifications listed in
calibration or
test program
Method 2
construction
specifications
verification
)P gauge (if not an
See Method 2
Once/test
Within 5% of
inclined manometer)
program
reference at three
readings
Balance
Calibration check
Initially
Observed weight
# 0.5 g from Class S
weight
Barometer
Calibration check
Initially
< 0.1 in. Hg from
primary barometer
WTM = wet test meter; DGM = dry gas meter.
a

CD-ROM
0023A - 27
Revision 1
December 1996
Figure 1

CD-ROM
0023A - 28
Revision 1
December 1996
Figure 2

CD-ROM
0023A - 29
Revision 1
December 1996
FIGURE 3

CD-ROM
0023A - 30
Revision 1
December 1996
FIGURE 4

CD-ROM
0023A - 31
Revision 1
December 1996
APPENDIX A 
RECOMMENDED AUDITING PROCEDURES
An audit is an independent assessment of data quality. Both performance audits and system
audits may be performed.
Performance Audit - A performance audit is conducted to evaluate quantitatively the quality
of data produced by the sampling, analysis, or the total measurement system (sample
collection, sample recovery, sample analysis, and data processing).
Audit Sample - A performance audit sample contains tetra- through octa-isomers of
PCDD and PCDF. Audit samples are not normally required.
Performance Audit of the Field Test - A field test performance audit may be conducted
by checking the dry gas meter for accuracy using procedures located in the Quality
Assurance Handbook for Air Pollution Measurement Systems (EPA 600/4-77-027b).
Performance audits on thermocouple readings, )P gauges, barometric pressure
gauges and others, may also be conducted.
Performance Audit of Data Processing - The data processing procedures may be
audited by requiring the testing laboratory to provide an example calculation for one
sample run. This example calculation will include all the calculations used to determine
the emissions based on the raw field and laboratory data.
System Audit - A system audit is an on-site, qualitative inspection and review of the total
measurement system.
The functions of the auditor are:
a)
Observe procedures and techniques of the field team during sample collection and
sample recovery; and
b)
Examine records of apparatus calibrations and other quality control procedures
used in sampling and analytical activities
When on-site, the auditor observes the source test team's overall performance,
including the following operations:
a)
Setting the sampling system and leak checking the sample train and pitot tube;
b)
Collecting the samples isokinetically;
c)
Conducting the final leak checks; and
d)
Sample documentation procedures, sample recovery, and preparation of the
samples for shipment.