IEEE

Std 548-1984
(Revision of ANSI/IEEE
std 648-1981)

IEEE Standard Criteria and

Guidelines for the Laboratory Measurement and
Reporting of Fly Ash Resistivity

Sponsor

Power Generation Committee

of the
IEEE Power Engineering Society

@Copyright1984 by

The Institute of Electrical and Electronics Engineers, Inc

345 East 47th Street,New York, NY 10017, USA

No part of this publication maybe reproduced in any form,

in an electronic retrieval system or otherwise,
without the prior written permission of the publisher.

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 Foreword

(This Foreword is not part of IEEE Std 548-1984,IEEE Standard Criteria and Guidelines for the LaboratoryMeasurementand
Reporting of Fly Ash Resistivity.)

This 1984standard has been contemplated since the time of development of the 1981edition; most of the
limitations recognized in the 1981 standard have now been overcome as a result of ongoing work.
The appendixes in this edition are new, with the exception of Appendix A, which is the same as the
previous Appendix D. This appendix is repeated here because of its historical importance in support of the
need for this standard on resistivity measurement.
Since the publication of the 1981 standard, the results of two additional Round Robin programs (RR I11
and RR IV) have become available. Among important items accruing from the RR I11 program was the need
for improved instructions regarding test cell preparation and resistivity test starting conditions. Statistical
evaluation of data generated using this standard was begun with Round Robin IV results.
In addition, it has now become possible to write specific test procedures in 6.3.3,thereby eliminating the
need for what were Appendixes B and C in the 1981 edition. The Ascending and Descending Temperature
Methods described in those appendixes have now been combined as a "round trip" test procedure and
incorporated here as.part of 6.3.3. The interpretation of the results of this new procedure is given in 7.4.
Included as 7.4.2 and 7.4.3 are statements applying to within-laboratory repeatability and between-
laboratory reproducibility, respectively.The background supporting 7.4 is given in Appendixes D and E.
This standard establishes a test procedure with a d e f i e d precision. It should not be expected that the
results obtained with the laboratory procedure will be identical to results obtained from an in situ
measurement. Foremost, this laboratory procedure does not require a test environment that duplicates the
in situ environment, especiallywith respect to sulfuric acidvapor. Secondly,this standard does not attempt
to account for any effects due to method of sample acquisition, sample storage, or age of sample. The scope
of this standard is limited to a laboratory procedure for the measurement and reporting of the resistivity of
as-submittedfly ash samples.
Appendix E of the 1981 edition referred to some of the problems encountered when attempting to make
laboratory resistivity measurements in test environments containing sulfur trioxide. Reference was made
to EPA document EPA-600/7-78-035. Detailed tests are described that provide what appears to be
conclusive evidence that the ASME PTC-28 parallel plate test apparatus could not be used in its present
form for measuring the effect of SO, (sulfuric acid) upon ash resistivity. Significant modifications in the
test apparatus and laboratory procedure would be required before they could be used for this purpose.
Because of these limitations and other factors (as described in Appendix B of this edition), a standard for
the measurement of ash resistivity in an enwonment of sulfur trioxide vapor is beyond the scope of this
standard.

At the time it approved this 1984 edition of the standard, the IEEE Power Plant Control, Protection and
Automation Subcommittee had the following membership:
T.D. Younkins, Chairman
A. T. Baker A. H. Ferber M. I. Olken
R. S. Bilski R. J. Fleming W. S. Pearce
G. G. &$e D. C. Garvey N. Petroro
R. L. Castleberry A. Gross R. J. Reiman
E. F. Chelotti M. E. Jackowski T. D. Russell
C. H. Clarridge H. M.Jimenez W. J. Spengel
D. J. Damsker W. H. von KleinSmid A. J. Spurgin
R. S . Darke C. E. Kneeburg R. B. Squires
P. M. Davidson G. L. Luri V. D. Thonias
A. C. Dolbec R. E. Mattson D. Tondi, Jr.
V. F. Estcourt T. J. McGrath K. L. West
M. H. Ewer W. S. Morgan J. P. Whooley
E. B. Nobile

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 This standard was prepared by a working group of the IEEE Power Plant Control, Protection and
Automation Subcommittee. The membership of the working group was:
V. F. Estcourt, Chairman
R. E. Bickelhaupt G. B. Nichols
H. R. Fletcher G. A. Rmard
N. W. Frisch 0. J. Tassicker
J. Greco C. L. Wagoner

When the IEEE Standards Board approved this standard on December 8, 1983, it had the following
membership:
James H. Beall, Chairman Edward Chelotti, Wee Chairman
Sava I. Sherr, Secretazy
J. J. Archambault Donald N. Heirman Frank L. Rose
John T. Boettger Irvin N. Howell Robert W. Seelbach
J. V. Bonucchi Joseph L. Koepfmger* Jay A. Stewart
Rene Castenschiold Irving Kolodny Clifford 0. Swanson
Edward J. Cohen George Konomos Robert E. Weiler
Len S. Corey John E. May W. B. Wilkens
Donald C. Fleckenstein Donald T. Michael* Charles J. Wylie
Jay Forster John P. Riganati

*Member emeritus

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 Contents
SECTION PAGE

1. Scope ................................................................................. 7
2 . Purpose ............................................................................... 7
3. Definitions............................................................................. 7
4. References ............................................................................. 8
5. Requirements .......................................................................... 8
6. Equipment and Procedures for Resistivity Test ............................................. 8
6.1 Test Variables ..................................................................... 8
6.1.1 Environmental Water Concentration .......................................... 8
6.1.2 Temperature ............................................................... 8
6.1.3 Electric Field ............................................................... 9
6.2 Test Hardware .................................................................... 9
6.2.1 General .................................................................... 9
6.2.2 Environmental System ...................................................... 9
6.2.3 Resistivity Test Chamber ..................................................... 9
6.2.4 Resistivity Test Cell Description ............................................... 9
6.2.5 High-Voltage Power Supply ................................................. 10
6.2.6 Current Measuring Device .................................................. 10
6.2.7 Physical and Electrical Arrangements ......................................... 10
6.3 TestProcedure ..................................................................... 10
6.3.1 Sample Acquisition and Preparation .......................................... 10
6.3.2 Resistivity Test Cell Preparation .............................................. 12
6.3.3 Procedures for Taking Resistivity Data ........................................ 13
7. Reporting Procedure with Example ....................................................... 14
7.1 Standard Resistivity Report (Part 1) ................................................. 14
7.1.1 Test Gas Phase ............................................................. 14
7.1.2 Expected Gas Phase ........................................................ 17
7.1.3 Electric Field ............................................................... 17
7.1.4 Bulk Density ............................................................... 17
7.1.5 True Density ............................................................... 17
7.1.6 Porosity ................................................................... 17
7.1.7 Mean Particle Size .......................................................... 17
7.1.8 Remarks ................................................................... 17
7.1.9 Chemical Composition ...................................................... 17
7.1.10 Losson Ignition(LO1) ....................................................... 17
7.2 Calculation of Resistivity Values ..................................................... 17
7.3 Resistivity-Electric Field Report (Part 2) ............................................ 18
7.4 Interpretation of Test Results ....................................................... 18
7.4.1 Choice of Data from Ascending or Descending Mode ............................ 19
7.4.2 Precision (Within-Laboratory Repeatability) ................................... 19
7.4.3 Precision (Between-Laboratory Reproducibility) ................................ 20
8. Bibliography ........................................................................... 20

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 FIGURES

1 Electrical Resistivity Test Cell .Guarded. Parallel Plate Design .......................... 10

2 General Apparatus Arrangement for Resistivity Measurement .
Chamber and All Plumbing of Stainless Steel ........................................... 11
3 Stainless Steel Environmental Resistivity Chamber ....................................... 12
4 Schematic Wiring Diagram for Four Guarded Parallel Plate Resistivity Cells Housed
in a Thermally and Environmentally Controlled Chamber ................................ 13
5 Standard Resistivity Report .......................................................... 15
6 Standard Resistivity Report Form ..................................................... 16
7 Resistivity - Electric Field Report .................................................... 18
8 Resistivity - Electric Field Report Form ............................................... 19

APPENDIXES

Appendix A History. Present Status. and Objectives of the Round Robin Laboratory Tests
OfFlyAshResistivity ............................................................ 21
Appendix B Influence of Sulfuric Acid on Laboratory Measurement of Fly Ash Resistivity .......... 24
Appendix C Background in Support of Resistivity Test Procedure (6.3.3) and Interpretation
of Results (7.4). ................................................................ 25
Appendix D Background in Support of Precision Statements (7.4.2 and 7.4.3) .................... 30

APPENDIX FIGURES

C1 Resistivity .
Temperature Report, Ash Sample No J-1 ................................. 27
C2 Resistivity .
Temperature Report, Ash Sample No 1-2 ................................. 28
C3 Resistivity .
Temperature Report. Ash Sample No 6-2 ................................. 29

APPENDIX TABLES

A1 Resistivity Test Procedure Comparison of Certain Features Used by Various

Laboratories ................................................................. ..... 22

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 IEEE Standard Criteria and
Guidelines for the Laboratory Measurement and
Reporting of Fly Ash Resistivity
1. Scope
This standard presents uniform criteria and
guidelines for measurement and reporting of fly
ash resistivity data obtained in the laboratory. It
applies to fly ashes produced from the burning of
any rank of coal. It includes consideration of
methods for ashing core bore samples of coal that
have not been burned previously in a full-scale
boiler.
2. Purpose
The purpose of this standard is:
(1) To provide uniform procedures to be used
in the measurement and reporting of fly ash
resistivity.
(2) To provide additional requirements to those
given in ANWASME Pl'C 28-1965, Determining
the Properties of Fine Particulate Matter [ 11.
(3) To provide additional recommendations to
the Informative Report No 2-June 1965 of the
Air Pollution Control Association's Committee No
TA-5 [7].
This standard is not intended to replace the
earlier efforts of documents described in the
preceding paragraphs except where updating is
clearly indicated.
3. Definitions
fly ash. The finely divided particles of ash en-
trained in flue gases arising from the combustion
of coal. The particles of ash may contain incom-
pletely burned fuel. The term has been applied
'The numbers in brackets correspond to the references listed
in Section 4 of this standard.
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predominantly to the gasborne ash from boilers
with spreader stoker, underfeed stoker, and
pulverized fuel (coal) fring [2].
NOTE:The above definition is consistent with the generic con-
cept of the word ash. However, all the particulates (including
unburned carbon) in suspension in the flue gases are generally
called fly ash and the term herein is used in this sense [SI.
simulated@ash. The entrained ash produced by
suspension fiing in a small-scale pulverized coal
combustor designed and operated with the objec-
tive of closely approximating certain selected
properties of the fly ash produced in the full-scale
steam generator of interest. The combustor should
have the capability of providing approximately the
same timehemperature profile for combustion as
would occur in a full-scale boiler furnace. This
process is applicable particularly when coal from a
new source has never been burned in a full-scale
boiler.
electric field strength (kV/cm). The ratio of the
applied voltage to the ash layer thickness in a test
cell used for the laboratory measurement of elec-
trical resistivity of fly ash.
laboratory resistivity (n-cm). Laboratory resis-
tivity (n-cm) of a fly ash deposit is the ratio of the
applied electric field across the layer to the in-
duced current density. The value of resistivity is
specific for a given ash sample and depends upon
the test variables or conditions: temperature, com-
position of the gaseous environment (especially
water and sulfuric acid vapor content), the magni-
tude of the applied electric field strength, as well as
the porosity of the ash layer.
Measured resistivity also is a function of test
procedure details, including items such as initial
test temperature, the rate of heating or cooling,
and the time that the voltage is applied prior to
reading current.
 IEEE
Std 548-1984
bulk density (g/cm3). Bulk density of the ash
layer is the ratio of the mass of the particulate in
the test cell to the cellvolume in a test cell used for
the laboratory measurement of electrical resistiv-
ity of fly ash.
true density (g/em3). The weight of the particles
divided by the solid volume of the particles.
ash layer porosity (cm3/cm3). The ratio of the
ash layer void volume to the test cell volume in a
test cell used for the laboratory measurement of fly
ash resistivity.
size distribution. Size distribution of particulate
matter is the cumulative frequency of particle
diameter, generally expressed on a mass basis. It
describes the probability that a particle diameter x
takes a value equal to or less than probability I?
Size distribution rather than mean particle size
shall be reported.
loss on ignition (LOI). Loss on ignition in a fly ash
sample is a measure of the completeness of the
combustion process. It is calculated as the ratio of
weight loss upon ignition at 750 "C of a previously
dried (100 "C) sample to the weight of the dry
sample, expressed in a percentage [4].
test gas phase. The gaseous environment to which
the ash layer being tested is exposed in a test cell
for the laboratory measurement of electrical resis-
tivity of fly ash.
4. References
[ l ] ANSUMME PTC 28-1965 (R 1980), Deter-
mining the Properties of Fine Particulate Matter2
[ Z ] ANSI/ASTM D 1356-73a (1979), Definition of
Terms Relating to Atmospheric Sampling and
Analysis
[3] ANSI/ASTM D 3682-78, Test for Major and
Minor Elements in Coal and Coke Ash by the
Atomic Absorption Method
[4] ASTM D 3174-73 (1979), Test for Ash in the
Analysis Sample of Coal and Coke3
2ANSI documents are available from the American National
Standards Institute, 1430 Broadway, New York, N.Y. 10018.
'ASTM documents are available from American Society for
Testing and Materials, 1916 Race St., Philadelphia, Pa. 19103.
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IEEE STANDARD CRI?'ERIAFOR THE MORATORY
[5] BICKELHAUPT, R. E., Comments on Fly Ash
Resistivity, Proceedings of International Confer-
ence on Electrostatic Precipitation, Electric Power
Research Institute, Industrial Gas Cleaning Insti-
tute, Air Pollution Control Association, Monterey,
California, Oct 1981
[6] BICKELHAUPT,R. E., Measurement of Fly Ash
Resistivity Using Simulated Flue Gas Environ-
ments, US Environmental Protection Agency, EPA-
600/7-78-035 (NTIS PB 278758), March 1978
[7] INFORMATIVE REPORT. Air Pollution Con-
trolAssociation, Committee No TA-5, no 12, June
1965
[8] WHITE, H.J., Electrostatic Precipitation of Fly
Ash. Journal of Air Pollution Control Association,
vol27, no 2, Feb 1977, p 116
[9] Ibid, vol24, no 4, Apr 1974, p 324
5. Requirements
The measurement of ash resistivityis predicated
upon selection of meaningful ash samples. This
presupposes that there are available either (1)
isokinetically obtained fly ash samples from a full-
scale boiler, (2) proportionately blended hopper
ash samples from a full-scale high efficiency pre-
cipitator, or (3) a procedure for producing a simu-
lated fly ash comparable to that which will result
when the coal is burned in a full-scaleboiler having
a specifk furnace design.
6. Equipment and Procedures for
Resistivity Test
6.1 Test Variables
6.1.1 Environmental Water Concentration.
The standard environmental water vapor concen-
trations for laboratoryresistivity tests shall be 0,6,
9, and 15%byvolume at the specified temperature.
For investigations involving only one water con-
centration, 9%shall be used.
6.1.2 Temperature. The standard temperature
range for the measurement of resistivity shall be
95 "C to 450 "C.

MEASUREMENT AND REPORTING OF FLY ASH RESISTIVITY
6.1.3 Electric Field. During the determination
of r e s s t i ~ t yas a function of temperature, the
applied direct-current potential across the fly ash
layer under test shall yield an average electric field
strength of 4 kV/cm unless the dielectric strength
is less than this applied electric field due to the
effect of temperature, the presence of carbon, or
other material properties. However, to avoid the
effect of ohmic heating of the fly ash sample under
test, the appliedvoltage shall be limited so that the
current density through the samples does not
exceed 2 * A/cm2.
During the determination ofresktin.tyasa func-
tion of applied direct-currentpotential, measure-
ments shall be made at 150 "C or 350 "C depending
on the intended precipitator design temperature.
These measurements shall be made at one or more
environmental water concentrations; typically,
this measurement shall be made using the stand-
ard water concentration most closely approximat-
ing the expected full-scale moisture condition.
Starting with an applied electric field strength of
not more than 2 kV/cm, resistivity as a function of
electric field strength shall be determined using
increments of 2 kV/cm until dielectric breakdown
occurs, holding the applied voltage foir not more
than 60 s.
6.2 Test Hardware
6.2.1 General. The test apparatus shall include
one or more electric resistivity test cells enclosed in
such a manner that the fly ash under test is main-
tained in intimate contact with the specified
gaseous environment. The test cells shall be housed
in a thermally controlled chamber so that resistiv-
itycan be determined at any temperature between
95 "C and 450 "C. A direct-current high-voltage
power supply shall be used to impress the required
magnitude of electric field strength across the fly
ash layer. The resulting current shall be measured
with an electrometer.
6.2.2 Environmental System. Either air-water
mixtures or oxygen-carbon dioxide-nitrogen-
water mixtures shall be acceptable environments.
An oil-free laboratory air line or pressurized gas
cylinders shall supply the required gases. The gases
shall be passed through a drying column before
use. The composition of the gaseous mixture shall
be controlled by adjusting the flow rate of the
components using adequately precise flow measur-
ing devices. The flow rate of the gaseous mixture
shall be sufficient to renew the resistivity test
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IEEE
Std 548-1984
environment between 5 and 10 times each hour.
The environmental water concentration shall be
introduced by bubbling all or a portion of the dry
gas through distilled water maintained at a
selected temperature in a thermostatically con-
trolled water bath.
The equipment and technique selected to pro-
duce the environment shall have sufficient preci-
sion to assure that the environmental moisture is
controlled to +5%of the desired level. Other major
environmental components shall be controlled in a
manner commensurate with good laboratory
practice. Water concentration shall be determined
gravimetricallyusing tubes filled with desiccant, or
with dewpoint meter. At least one determination
shall be made for each day for each water concen-
tration used in a test. The gas sample shall be
drawn from the heated environmental exhaust
line of the resistivity test chamber.
6.2.3 Resistivity Test Chamber. Almost any
natural or forced convection laboratory oven cap-
able of operating in the temperture range of 95 "C
to 475 "C is suitable. For isothermal tests, the oven
shall be capable of maintaining the set tempera-
ture to within 0.01 T where T is the desired tem-
perature in degrees Celsius. Natural convective
cooling should allow the test apparatus to cool
from 475 "Cto 95 "C in 4 to 6 hours.
The inside volume of the oven can serve as the
environmental chamber, or one or more test cells
can be housed within a separate environmental
chamber inside the oven. Whatever design is used,
the test environment always must be maintained
under a small positive pressure; for example, 1or 2
inches of water.
6.2.4 Resistivity Test Cell Description. The
guarded, parallel plate configuration shall be the
generic type of test cell. The Standard Test Cell,
Fig 1,represents essentially the equipment shown
in Fig 8 of ANWASME PTC 28-1965 [l].The cell
shall be constructed using a type 304stainless steel
or steel of equivalent corrosion resistance for con-
ductive components and a high grade technical
alumina having an aluminum oxide concentration
of 99%or more for dielectric components.
Other test cells of this generic type, in order to
q u a l e as equal to the Standard Test Cell, shall
conform to the requirements of 6.3.2 and shall be
capable of providing substantially the same bulk
density of the loaded ash sample. Deviations in
bulk density shall be within +5% of that obtained
with the Standard Test Cell.
 IEEE
Std 548-1984 IEEE STANDARD CRITERIA FOR THE LABORATORY

n
INA BAR

-4-
0.95 cm (318 IN )

L
S.S. ROD 4.8 cm 11.81 IN ) LONG /S.S. WEIGHT " W '
SILVER SOLDEREDTO ELECTRODE (APPROX) 2.54 cm (1 IN I DIA

ALUMINA SLEEVES O.D. 0.64 cm (1/4 IN 1

I.D. 0.48 cm 13/16 IN 1

S.S. ROD 2.9 cm (1 118 I N ) LONG

SILVER SOLDERED TO GUARD RING
ELECTRODE TO
ELECTROMETER
ALUMINA BAR 4.5 cm (1.75 IN IX
GUARD RING 0.95 cm (318 IN
ELECTRODE
TO GROUND S.S. RING . DEPTH OF CUP AFTER
BOTTOM I S WELDED AND MACHINED
TO BE 0.5 cm (0.2 IN 1
SINTERED 25 MI

SINTERED 25 MIC
S.S. GUARD RING
4.3 cm (1.7 IN I 0.
2.7 cm (1.06 IN I I.

TO HIGH VOLTA
SOURCE
8.25 cm (3.25 IN )
S.S. CUP BOTTOM
FLY.ASH A l d GAP 0.08 cm (0.031 IN 1

NOTES
(1) ALL ELECTRODE SURFACES I N THE REGION OF THE ASH LAYER SHALL BE WELL ROUNDED TO ELIMINATE HIGH ELECTRIC FIELD STRESSES.
ELECTRODE SURFACES SHALL BE FLAT.
(2) WEIGHT " W SIZED TO MAKE PRESSURE OF UPPER ELECTRODE AND GUARD RING EQUAL TO 10 g/Cm2.
(3) ALL THREADS NO 6-32.
(4) ALL METAL PARTS OF STAINLESS STEEL (SS) TYPE 304 OR EQUIVALENT
(5) ALL ALUMINA PARTS >99.0% ALUMINA (AI2 Os).

Fig 1
Electrical Resistivity Test Cell - Guarded, Parallel Plate Design

6.2.6 High-Voltage Power Supply. The supply
shall have a range of 0 to 10kV de with a maximum
rms ripple of 1%of range.
6.2.6 Current Measuring Device. Resistivity
cell current shall be measured using a sensitive
electrometer capable of reading current in the
range of A to 10-l' A with an accuracy of +2%
of the particular full scale reading. When neces-
sary, the investigator shall proof test thevalidity of
the measuring system by inserting a known resist-
ance in place of a fly ash sample.
6.2.7 Physical and Electrical Arrangements.
Typical physical arrangements of equipment and
the electric circuits employed are illustrated in
Figs 2, 3, and 4.
6.3 Test Procedure
6.3.1 Sample Acquisition and Preparation.
Using a sample thief or the quartering method, a
representative resistivity test sample having a
volume slightly greater than needed to fill a resis-
tivity test cell shall be acquired from the total
volume of ash delivered to the laboratory. The
sample shall be passed through an 80 mesh (1 77
pm) screen to remove foreign objects. Break up

10

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 IEEE
MEASUREMENT AND REPORTING OF FLY ASH RESISTIVITY Std 548-1984

THERMOCOUPLE SELECTOR. FEMALE PHONE JACKS

SWITCH, TERMINAL BLOCK, FOR FOUR TEST
AND DIGITAL READOUT

OVEN DOOR
ENVIRONMENTAL
CHAMBER HOUSING
\ RESISTIVITY TEST CELLS
B U B B L ~ RTO OVEN
CONFIRM CONTROL
ENVIRONMENTAL
FLOW
\
GAS OUTLET
PANEL

SAMPLING PORT

Fig 2
General Apparatus Arrangement for Resistivity Measurement.
Chamber and All Tubing of Stainless Steel

11

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 IEEE
Std 548-1984 IEEE STANDARD CRITERIA FOR THE MORATORY

CABLE CENTER, TO ELECTROMETER,

TO GROUND
POSITIVE GUARD ELECTRODE
TO COAXIAL CABLE SHIELD.TO GROUND

FINISHED
SURFACE

t
GAS
OUTLEl -
-
THERMOCOUPLE

V I /
I I
I

>GAS
INLET

ALUMINA =

7
SUPPORT
I I I w TO NEGATIVE
HV POWER

U U \I Y
SUPPLY

Fig 3
Stainless Steel EnvironmentalResistivity Chamber

ash agglomerates by gently brushing with a camel
hair brush any material retained on the screen.
The test sample shall be bottled and identified.
6.3.2 Resistivity Test Cell Preparation. Each
test cell shall be numbered, and the weight and ash
layer volume recorded. The ash layer thickness in
the test cell shall be 0.5 cm f0.05 em.
The ash sample shall be poured into the cup or
dish electrode of the test cell until the ash over-
flows the edge. A metal straight edge shall be used
to tap the sides and base of the dish electrode to
settle the ash. The straight edge shall be used to
strike the ash level with the upper edge of the dish
electrode. The filled dish electrode shall be tapped
again to determine whether noticeable settling
occurs. If so, additional ash is added, and the tap-
ping and leveling is repeated. These steps shall be
repeated until no more ash can be added.
The loaded cup portion of the resistivity cell
shall be weighed, and bulk density calculated. Ash
layer porosity can also be calculated if the true
density of the fly ash is known.
The lower cup electrode filled with fly ash shall
be placed in a grounded environmental chamber
(see Fig 3) on an alumina (>99%Al,O,) support,
and the negative, high-voltage lead shall be at-
tached. The upper electrode shall be gently placed
on top of the ash exerting a pressure of about
10 g/cm2. The guard electrode shall be attached
directly to ground, while the center, current-
measuring electrode shall be attached to the elec-
trometer. The environmental chamber in which
the cell is placed shall then be sufficientlysealed to
maintain about one inch of positive water pressure
when the controlled environmental gas is intro-
duced.

12

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MEASUREMENT AND REPORTING OF FLY ASH RESISTIVITY
-CELL 3 :Fc:tR 6
-
' RG - 58iU
-CELL 2 F:F:tR 6
- RG . 58iU
-CELL1 $E&,: -[I
6- RG - 5 8 i U
RG - 58iU
Fig 4
Schematic W d g Diagram for Four Guarded Parallel Plate
Resistivity Cells Housed in a Thermally and
Environmentally Controlled Chamber
6.3.3 Procedures for Taking Resistivity Data
The procedure shall be to conduct a "round trip"
test program, starting with the ascending phase at
a temperature level of 95 "C and proceeding in
defined temperature increments to approximately
450 "C.After holding a temperature of 460 "C to
480 "C overnight (16 h), the descending phase shall
be started.
(1) Ascending TemperaturePhase. The resistiv-
itytest cells shall be heated to 95 "Cf 1 "Cin an envi-
ronment of dried air or dried nitrogen. Within
30 min of achieving this temperature, the resistiv-
ity test environment shall be introduced. After 99%
environmental dilution has occurred, resistivity
data shall be taken. The 99%dilution will require
approximately 60 min using a flow rate of five
volume changes of the test chamber or cell per
hour. The time required is directly proportional to
the total flow rate for a given experimental setup.
The negative high voltage shall be impressed on
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IEEE
Std 548-1984
c< ---/
0
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/
-
I
0 - --
//
HIGH-VOLTAG E
POWER SUPPLY
one resistivity test cell at a time, and 60 s later, the
current being passed through the ash layer, the
time, and the temperature of the ash layer shall be
recorded. The high voltage shall be removed until
the next data point is to be obtained. It is
important that the temperature of the ash be
known at the moment the resistivity data point is
being established. This shall be accomplished by
determining the test cell temperature with a
thermocouple. A temperature correlation shall be
established between one dummy cell (not electri-
fied) with thermocouple and the other test cells in
the chamber without thermocouples.
The oven temperature shall be increased in
increments of about 30 "C,and the resistivity mea-
surements shall be repeated until a temperature of
about 215 "C is reached. Resistivity measurements
shall also be made at about 315 "C and 425 "C. At
each test temperature, resistivity data shall not be
taken until the ash temperature has stabilized to
13
 ~
IEEE
Std 548-1984
less than 1"Cchange in 10 min. Total elapsed time
between successive test temperatures shall be less
than one h.
(2) Descending Temperature Phase. Without
interruption of the ongoing procedure, dried air or
dried nitrogen shall be passed through the sealed
environmental chamber or appropriately con-
nected test cell at a rate of about one chamber or
cell volume per hour while the ash is heated to and
maintained at 460 "C to 480 "Cfor approximately
16 h (overnight). The environment shall be con-
verted to that desired for the resistivity test and
allowed to flow until approximately a 99%dilution
of the test environment has occurred. This will
require approximately 60 min using a flow rate of
five volume changes of the chamber or cell per
hour. The time required is directly proportional to
the total flow rate for a given experimental setup.
After achieving the 99% dilution of the environ-
ment, the oven shall be turned off allowing the test
cells to cool by convection at a rate that will pro-
duce a resistivity test cell temperature of 95 "C in
4 to 6 h.
Resistivity is determined as the temperature
decreases. For approximately each 30 "C decrease
in temperature a resistivity data point is estab-
lished.The negative high voltage shall be impressed
on one resistivity test cell at a time, and 60 s later,
the current being passed through the ash layer, the
time, and the temperature of the ash layer shall be
recorded. The high voltage shall be removed until
the next data point is to be obtained. It is
important that the temperature of the ash be
known at the moment the resistivity data point is
being established. This shall be accomplished by
determining the test cell temperature with a
thermocouple. A temperature correlation shall be
established between one dummy cell (not electri-
fied) with thermocouple and the other test cells in
the chamber without thermocouples.
(3) Resisti~tyvs Electric Field. After the de-
scending temperature phase has been completed,
the oven is turned on with the set-point adjusted
to give a temperature of 150 O C , 350 "C,or any other
temperature of interest to the user. After the
temperature of the ash has stabilized at the
desired temperature (temperature change of less
than 1 "C in 10 min), data shall be taken. The
negative high-voltage source shall be set to pro-
duce an ash layer electric field strength of 2 kV/cm.
After the voltage has been impressed for 60 s, the
current shall be read. The voltage shall imme-
14
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IEEE STANDARD CRITERIA FOR THE LABORATORY
diately be increased an increment equivalent to
2 kV/cm, impressed for 60 s, and the current shall
be again determined. This shall be repeated until
the desired maximum electricfield strengthis attained
or dielectric failure occurs. It is not recommended
that resistMty/temperature data be taken after
resistivity/electric field strength data are acquired
with a given ash sample.
After the resistivitytest has been completed, the
test cells are removed and the thickness of the ash
layer at the current measuring electrode shall be
determined. This value is used to calculate the
geometric factor by which the resistance is multi-
plied to obtain the resistivity value. If a 0.5 mm or
greater decrease in ash layer thickness occurs dur-
ing the test, the porosity and electric field strength
shall be recalculated based on the final ash layer
thickness. The electrodes shall be cleaned with a
commercial, ultrasonic cleaning agent, rinsed in
distilled water, and dried.
7. Reporting Procedure with Example
There are two parts to the report: (1) the rela-
tionship of resistivity to temperature and moisture
content (Standard Resistivity Report, 7.1) and (2)
the effect of electric field strength on resistivity at a
characteristic temperature and moisture level
(Resistivity-Electric Field Report, 7.3).
7.1 Standard Resistivity Report (Part 1). The
report paper is shown as Fig 5 . AU available perti-
nent information shall be entered in the upper
right-hand box on this form, as shown in Fig 6. If
the information is not available, it should be indi-
cated by NA. In addition, a space is provided,
under description, for an identlfylng number or
code and a description of the material such as
isokinetically collected fly ash, hopper ash, etc.
The information in this example, Fig 6, repres-
ents typical data. The sample was collected isoki-
netically through port No 6 on Dec 8,1974, at Big
Marie Station, Unit No 5. The data to be entered in
the upper right-hand box are discussed below.
7.1.1 Test Gas Phase. The composition of the
resistivity test environment shall be reported. In
the example, moisture levels of 0,6,9,and 15%by
volume were used. The ranges of the other constit-
uents reflect the variation due to changes in mois-
ture content.
 IEEE
MEASUREMENT AND REPORTING OF FLY ASH RESISTIVITY Std 548-1984

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 IEEE
Std 548-1984 IEEE STANDARD CRITERIA FOR THE LABORATORY

16

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 ~

IEEE
MEASUREMENT AND REPORTING OF FLY ASH RESISTIVITY Std 548-1984

7.1.2 Expected Gas Phase. The coimposition of

the plant flue gas, as measured or calculated based
on stoichiometry, shall be reported in volume
percent.
Based on the fuel ultimate analysis and an
excess air level of 28%, calculation indicated the
followingflue gas composition, assuming complete
combustion: 13.2%CO,, 0.033%SO, 4.4% 0,,76.8%
N,, and 6.6% H,O.
7.1.3 Electric Field. In accordance with the
recommended procedure, the standard value, 4 kV/
cm, of electric field strength for determining the
effect of temperature and moisture content on
resistivity is reported (as shown in Fig 6).
7.1.4 Bulk Density. In this case the resistivity
cell (diameter) 3.0 cm has avolume of ash equal to
-
(7r/4) * (3.02 0.5) = 3.53 cm3. The ash in the cell
weighed 4.271 g, leading t o a bulk density of
4.27U3.53 or 1.21 g/cm3.
7.1.5 True Density. This is usually determined
by pycnometry. Helium is the preferred pycnomet-
ric fluid but, in practice, liquids in which the par-
ticulate is insoluble are often used. In this example
the helium pycnometer density was found to be
2.52 g/cm3.
7.1.6 Porosity. Ash layer porosity of the sample
is expressed as the volume of the ash layer voids
divided by the test cell volume. Percent porosity is
conveniently calculated as:
bulk density
100 * (1-
true density
Hence the porosity was
Particle Diameter % by Weight Less than
Ctm Indicated Size
1.4 3.3
2.2 8.1
4.4 31.1
8.2 64.4
13.0 81.1
22.7 94.6
30.1 97.0
Based on the use of log normal probability
paper, this distribution was found to correspond
to a mass-median diameter of 6.2pm. The geomet-
ric standard deviation was calculated from the
ratio of the mass-median diameter to the 15.9%
weight diameter (2.8pm). This value of 15.9%cor-
responds to one standard deviation. Thus, the
geometric standard deviation is 6.2/2.8, or 2.2.
7.1.8 Remarks. Provide here any further des-
cription of the ash or the procedure used, espe-
cially relative to temperature cycle. Describe pro-
cedure in detail when it deviates from the standard
method. In the example case, the geometric stan-
dard deviation of the ash is indicated. Also noted is
that measurements were made using the ascend-
ing temperature approach.
7.1.9 Chemical Composition. The fly ash ele-
mental chemical composition shall be reported on
an oxide basis in accordance with ANSI/ASTM D
3682-78 [3].
7.1.10 Loss on Ignition (LOI). This value is
usually determined by the difference between the
weight of a 100 "C dried sample and a 750 "C
ignited sample, expressed as a percentage of the
as-received sample weight.
In this example, the as-received sample weighed
1.191 g, and when dried at 100 "C, was found to
weigh 1.062 g. After ignition at 750 "C, the sample
weight was found to be 1.012 g. The loss on ignition
was therefore

7.1.7 Mean Particle Size. The mean particle

size or the size distribution parameters should be
indicated. The latter is preferred. The method of
analysis (for example, BAHCO, Impactor, Coulter 7.2 Calculation of Resistivity Values. Resistivity
Counter) should be identifed. values are calculated from:
In this case the following data were obtained by
use of the BAHCO centrifugal classi&!r: -
p = ( V / I ) (A/1)

17

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 IEEE
Std 548-1984 IEEE STANDARD CRITERIA FOR THE LABORATORY

where: At the 6%moisture level, and 232 "C, the mea-

sured current was 11.3 PA. Hence the calculated
p = the resistivity, fl * cm resistivity value is:
V the applied
= _ _ dc potential, volts
I the measured current, amperes
=
2*03 = 1.8 (10)2 cm
I = the ash layer thickness, cm
11.3
A = the current-measuring electrode face
area, cm2 In the example given, the resistivity was deter-
mined using the standard guarded, parallel plate
For the cell used cell shown in FIg 1.
(7r/4)(2.54)2 7.3 Resistivity-Electric Field Report (Part 2).
AA =
0.5 Values of resistivity measured at increasing elec-
tric field strength at a characteristic temperature
= 10.13 cm (150 "C or 350 "C)and at least one moisture level
shall be reported. Figure 7 shows such data, nor-
Measurements made at the standard 4 kV/cm
malized to a 4 kV/cm electric field, for a moisture
requiredthe application Of 2ooo v.
level closely a p p r o x ~ a t ~the
g expected level.
At this electric field strength, resistivityvalues are
The breakdown electric field strength also shall be
calculated directly from
reported. Figure 8 represents a reporting form.
p = (2000/1) 10.13 - 7.4 Interpretation of Test Results. The justifi-
= 2.03 (10)4/1 cation for the basis of the following interpretation

I-
a

E, ELECTRIC F I E L D STRENGTH, kV/cm

Fig 7
Resistivity-Electric Field Report

18

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 IEEE
MEASUREMENT AND REPORTING OF FLY ASH RESISTMTY Std 548-1984

10.0

6
5
4

-
L
L
5
v) 1.0
w
K
W
0.8
>
-
c 0.6
4w 0.5
K
0.4

0.3

0.2

0.1
0 2 4 6 8 10 12 14

E, ELECTRIC FIELD STRENGTH, kV/crn

Fig 8
Resistivity - Electric Field Report Form

of results obtained from the test described in 6.3.3
is given in Appendixes C and D.
7.4.1 Choice of Data from Ascending or De-
scending Mode. The design resistivity value at
any temperature of interest shall be the higher
value obtained byeither the ascending or descend-
ing technique, adjusted to take into account any
change in resistivity produced by the increased
electric field immediately prior to dielectric failure.
If there is a difference greater than one order of
magnitude between the descending and ascending
test results, the cause shall be investigated (par-
ticularly with respect to conformance with para-
graphs 6.2.3,6.3.3and 7.4.2) and, as a minimum,
the tests shall be repeated - preferablywith a new
sample of ash.
7.4.2 Precision (within-LaboratoryRepeata-
bility). (subjective evaluation - see Appendix
C) The results of resistivity determinations car-
ried out by the same mode of measurement (that
is, ascending or descending) should not differ by
more than a ratio of two (higherhower). Analyses
with a greater ratio may be considered suspect;
conformance with paragraphs 6.2.3 and 6.3.3

19

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 IEEE
Std 548-1984
shall be reviewed, and if necessary, additional
measurements should be made - preferablywith
a new sample of ash.
7.4.3 Precision (Between-Laboratory Repro-
ducibility). (statistical evalution - see Appen-
dix D) The results of resistivity determinations
carried out by different laboratories on represen-
tative portions taken from the same sample and
using the same temperature, atmosphere, and the
same mode of measurement (that is, both labora-
tories using the ascending mode or both laborato-
ries using the descending modej should not differ
by more than a ratio of 2.7 (higherhower), 95%of
the time. Results with a ratio greater than 2.7 may
be considered suspect, and additional measure-
ments are indicated to resolve the issue.
8. Bibliography
The following standards, technical journals, and
reports have been reviewed and considered during
the writing of IEEE Std 548
ANSI/ASTM D257-78 Standard Test Methods for
DC Resistance or Conductance of Insulating Mate-
rials, American Society for Testing and Materials,
Part 39,1979, pp 152-71
BAKER, J. W. and SULLIVAN,K. M. Reproducibility
of Ash Resistivity Determinations, IEEE Paper No
78 303-0, IEE Power Engineering Society Winter
Meeting New York, NY, Jan 29-Feb 3,1978
BICKELHAUPT, R. E. Surface Resistivity and the
Chemical Composition of Fly Ash, APCA Journal,
vol25, no 2, February 1975, pp 148-52
BICKELHAUPT, R. E. Volume Resistivity - Fly
Ash Composition Relationship, Environmental
Science and Technology, vol9, no 4, April 1975, pp
336-342
IEC PUBLICATION 93, Recommended Methods of
Test for Volume and Surface Resistivities of Elec-
trical Insulating Materials, International Electro-
technical Commission 195fi4
MAARTMA”, S. The Effect of Gas Temperature
and Dew Point on Dust Resistivity and Thus the
41EC documents are available from the American National
Standards Institute, 1430 Broadway, New York, NY 10018.
20
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IEEE STANDARD CRITERIA FOR THE LABORATORY
Collecting Efficiency of Electrostatic Precipitators,
Proceedings of Second International Clean Air
Congress,Washington, DC, December 6-1 1,1970,
Paper EN 34F, pp 900-905
MASUDA, S. Effects of Temperature and Humidity
on the Apparent Conductivity of High Resistivity
Dusts, Electro-TechnicalJournal, Japan (English),
vol7, no 3,1962, pp 108-113
McLEAN, K. J. Factors Affecting the Resistivity of a
Particulate Layer in Electrostatic Precipitators,
APCA Journal, vol26, no 9, September 1976, pp
866-70
NEVENS, T. D. A Comparative Evaluation of Cells
for Ash Resistivity Measurement, IEEE Paper No
A 78-304-8, IEEE Power Engineering Society
Winter Meeting New York, NY, Jan 29-Feb 3,
1978
NICHOLS, G. B. Theoretical and Practical Aspects
of Fine Particle Collection by Electrostatic Precip-
itators. Proceedings, Symposium on Control of
fie-Particulate Emissions from Industrial Sour-
ces, San Francisco, California, January 15-18,
1974, pp 137-168
SELLE, S. J. Western Fly Ash Composition as an
Indicator of Resistivity and Pilot ESP Removal Effi-
ciency, presented at the 68th Annual Meeting of
the Air Pollution Control Association,APCA Paper
No 75-02.5, Boston, Mass., June 15-20, 1975
SMITH,W. B. Procedures Manual for Electrostatic
Precipitator Evaluation, EPA-600/7-77-059, June
1977
SULLIVAN,K. M. The Laboratory Examination of
Low Sulfur Coals in Relation to Their Electrostatic
Precipitability, Australian Coal Industry Research
Laboratories Ltd, Paper PR 73-5, June 1973,
PP 7-8
TASSICKER, 0.J. and SULLIVAN,K. M. Estimation
of Precipitator Performance for Collection of Fly
Ash by Examination of Low-Sulfur Coal Bore
Cores, Paper No 73-311, presented at the 66th
Annual Meeting of the Air Pollution Control Asso-
ciation, Chicago, Illinois, June 24-28, 1973
WAGONER, C. L. Fuel and Ash Evaluation to Pre-
dict Electrostatic Precipitator Performance. A
Progress Report, IEEEPaperNoA 78 305-5, IEEE
Power Engineering Society Winter Meeting New
York, NY Jan 29-Feb 3,1978

MEASUREMENT AND REPORTING OF FLY ASH RESISTMTY
Appendixes
(These Appendixes are not a part of IEE Std 548-1984,IEEE Standard Criteria and Guidelinesfor the Laboratory Measurement and
Reporting of Fly Ash Resistivity.)
Appendix A
History, Present Status,and Objectives of the
Round Robin Laboratory Tests of Fly Ash Resistivily
Al. History and Present Status. It is generally
agreed that a given laboratory conducting resis-
tivity measurements in a professionally acceptable
manner will not have problems with data repeat-
ability. However, several laboratories testing
identical ash samples, using similar equipment
and test variables but different procedures,
produced resistivity/ temperature data that were
judged to be too divergent for acceptable precision.
This point was demonstrated by the results of
Round Robin I conducted by the subject committee.
The need for a precise resistivity test procedure,
which will allow laboratories to produce data
showing little scatter for a specific ash, is compli-
cated by a major difference in test logic. Without
discussing the reasoning or the specific details of
differences, one can simply say that some investi-
gators prefer obtaining resistivityhemperature
data using an ascending test temperature, while
others prefer to obtain these data using a descend-
ing test temperature. For specific ash composi-
tions and test temperatures, these two test proce-
dures can produce data having excessive differ-
ence.
In the first Round Robin all laboratories used
test cells and test procedures of their preference.
Depending upon each combination and sequence
of events selected, a large variation in resistivity
was reported. For a given ash in an environment of
air and 9%byvolume water at 148.9"C(300 T),the
resistivity was reported as:
Resistivity
Test Number S l - cm
4 -
3 10'0
2 -
4 10'0
1 1* 10"
7 3 * 1011
6 -
5 10"
Not all ashes are as sensitive to test procedure as
the one illustrated above; however, it was selected
21
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IEEE
Std 548-1984
to satisfy the objective of demonstrating that a
significant variation in resistivity can be expe-
rienced using test procedures differing no more
than those shown in Table Al.
In a second Round Robin test program, an
attempt was made to show less data divergency
among laboratires if the same ash, similar equip-
ment, identical test variables, and identical test
procedures were used. Although tending to con-
firm the reduction of divergency, the results were
in reality somewhat inconclusive.The data scatter
was improved over the first Round Robin effort,
but the divergency was still greater than antici-
pated.
A careful review of the results from the second
Round Robin effort indicated that the various
laboratories did not use exactly the same test
procedure with respect to all details. Also thevari-
ation in ash layer porosity between the different
laboratories was suggested as a contributing factor
to data scatter.
In summary, the achievement of a precise resis-
tivity test procedure, which will allow laboratories
to produce data showing minimal scatter for a
specific ash,is complicated by a major differencein
test logic as cited above. In addition to such pre-
ferred differences in test logic (ascendingversus
descending test temperatures), the most signifi-
cant variations among laboratory procedures are
related to the treatment of the ash from the time
it is placed in the test cell to the completion of
the test with respect to time, temperature, and
environment.
A2. Objectives of Round Robin 111. As a result
of the observations regarding the first two Round
Robin efforts, a third program is in progress. This
program is known as Round Robin 111. The expe-
rience gained in the first two Round Robin efforts
will be helpful in setting up a test procedure and
test variables to be exactly followed by the partici-
pants in this program.
 IEEE
Std 548-1984 IEEE STANDARD CRITERIA FOR THE LABORATORY

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MEASUREMENT AND REPORTING OF FLY ASH RESISTIVITY
Specifically, the principal objectives of Round
Robin I11 are:
(1) Overcome the problems experienced during
Round Robin I1 and determine the range of resis-
tivity data to be expected when laboratories test
identical ash samples using exaetlythe same test
procedure and test variables.
(2 j Determine the difference in resistivity data
produced by laboratories using identical ash sam-
ples and test variables but two different test
procedures that are followed exactly by each
laboratory.
The two procedures that are being considered
can be identified by ascending and descendingtest
temperature. The resistivity test procedures are
described in detail respectively in Appendixes B
and C of this standard.
A3. General Requirements of Round Robin
111. The principal requirements for conducting
Round Robin I11 are given below. All details will be
included as part of the final report of this test
program.
Approximately ten fly ash samples are to be
used in these tests. The samples shall represent
commercially or scientifically important ashes,
some of which can be classified as difficult to col-
lect. An effort will be made to obtain a variety of
ash types by nation, region, and ash composition.
The participants in the test program shall furnish
the ash samples, with the subcommittee on Test
Procedure of IEEE Std 548-1981, IEEE Standard
Criteria and Guidelines for the Laboratory Mea-
surement and Reporting of Fly Ash Resistivityhav-
ing the privilege to refuse a sample. If possible, the
ashes selected for Round Robin I11 will be chemi-
cally and physically characterized. The ash sam-
ples must come from installations that are not
using some form of gas conditioning, and the ash
must contain less than 5% combustibles.
Prior to acceptance for use in this study, data
describing the potential ash samples shall be sub-
mitted to the subcommittee on Test F’rocedure for
review. This is being done principally to avoid ash
type duplication and to assure that the ashes being
used have been previously characterized to some
extent.
23
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IEEE
Std 548-1984
The following guide list describes potential
candidate ash samples with respect to origin,
principal coal characteristics, and principal ash
compositional features. It is assumed that each
type described below will be included in the study
and that important ashes omitted from this list
will be welcomed for approval by the subcommittee.
(1) USA Eastern bituminous - Coal char-
acterized by high sulfur and ash by high iron
concentration.
(2) USA Eastern bituminous - Coal char-
acterized by low sulfur and ash by low iron
concentration.
(3) USA or Canada: Western sub-bituminous
- Coal characterized by low sulfur and ash by
(a) High alkaline earth (>20%) and low
sodium (0.1 - 0.5%)
(b) High alkaline earth (>20%) and moderate
to high sodium (>l.O%)
(c) Low to moderate alkaline earth (5 - 15%)
and moderate to high sodium (0.1 - 0.5%)
(dj Low to moderate alkaline earth (5 -
15%)and moderate to high sodium (>l.O%j
(4) USA Texas lignite - Coal characterized by
high moisture and high ash with low to high sulfur
and ash generally characterized as similar to (3)
(a) above.
( 5 ) Australian: bituminous - Coal character-
ized by low sulfur and ash by low alkaline earth,
low sodium, and low iron.
(6) Australian: brown coal - Coal character-
ized by high moisture and ash by moderate iron,
moderate alkaline earth, and high sodium.
(7) Indian: bituminous - Coal characterized
by high ash content and ash by low iron, alkaline
earth, and sodium concentration.
(8) South African: Transvaal - Coal charac-
terized by low sulfur and ash composition similar
to (3) (cj above.
The participant shall supply an ash sample, if
approved by the subcommittee on Test Procedure,
and be willing to test at least 50%of the 10 to 12
ashes collected using one of the two procedures
described. All participants are encouraged to test
all the ashes using both procedures if the labora-
tory can follow the procedures exactly.
 IEEE
Std 548-1984
Appendix B
Imuence of Sulfuric Acid on
Laboratory Measurement of Fly Ash Resistivity
In Appendix E of the 1981edition, reference was
made to the EPA document Measurement of Fly
Ash Resistivity Using Simulated Flue Gas Environ-
ments [6].Additional discussion of this subject has
recently appeared [ 5 ] . Some of the difficulties
involved when testing in an environment contair-
ing sulfur trioxide (sulfuric acid vapor) were
described. Using the resistivity cell suggested in
ASME F'TC-28 [ 1] and subsequently adopted by
this standard, the investigator attempted several
experimental variations to demonstrate the very
significant effect of sulfuric acid vapor on resistiv-
ity. In the end, it was learned that to obtain
laboratory-measured resistivitydata in reasonable
agreement with in situ resistivity data (obtained in
a flue gas containing a measurable concentration
of sulfuric acid vapor) one must utilize a labora-
tory test environment containing the requisite
concentration of sulfuric acid vapor. Regardless of
apparatus used or techniques employed, the dra-
matic effect of sulfuric acid vapor observed in situ
24
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IEEE STANDARD CRITERIA FOR THE MORATORY
could not be reproduced in the laboratory with
test environments devoid of sulfuric acidvapor. Of
equal importance was the observation that the
test cell shown in this standard was unsuitable. A
cell consisting of concentric electrodes in which a
layer of ash 1 mm thick is evaluated was success-
ful. Also in contrast to this standard, the gas test
phase delivery system required alteration with
respect to materials, flow rates, and precision of
thermal tracing. A means of supplying and deter-
mining the concentration of sulfuric acid vapor
are additional requisites. Finally, it was learned
that a long-time isothermal test procedure was
required in contrast to the procedure described in
this standard.
The dissimilarity between the apparatus and
procedures recommended in this standard and
those required for a resistivity determination in
the presence of sulfuric acid vapor places the lat-
ter beyond the scope of this standard.

MEASUREMENT AND REPORTING OF FLY ASH RESISTIVITY
Appendix C
Background in Support of Resistivity Test Procedure (6.3.3)
and Interpretation of Results (7.4)
C.l VariabilityBetween Test Modes. In spite of
in-depth research that has been published in con-
nection with resistivity test procedures during the
past ten years, the paragraphs describing specific
tests (6.3.3), and their interpretation (7.4), still
suggest areas of uncertainty that require the
application of subjective decisions. The problem
can be illustrated with the results from three tests
generdy conducted in accordance with the instruc-
tions in 6.3.3.Although it is noted that there were
some deviations from the test apparatus and pro-
cedures required in 6.2.4 and 6.3.3,the resistivity
curves shown in Figs C1, C2, and C3 are satisfac-
tory for the intended purpose. For discussion, the
data acquired at 150 “C are tabulated as:
Resistivity, Q cm (150 “C)
Sample Descending (D) Ascending (A)
J-1 (FigC1) 2.OE12 4.OE12
1-2 (FigC2) 7.5E10 5.OE11
6-2 (FigC3) 3.6E10 5.OE9
It is apparent that either the descending or
ascending resistivity value can be greater than the
other by a factor of 7. The importance of this
difference can be compounded bythe level of resis-
tivity being measured. The size of a precipitator is
in part dependent upon the allowable electrical
operating conditions, which in turn are dependent
on the electrical properties of the ash layer.
According to White [ 111: “The severity of spark-
over and back corona increases with the resistivity
of the particles. There is no significant effect below
about 1Olo n-cm.’ Sparkover voltages are reduced
for resistivities between loloand 10llQ-cm, but
little or no back corona occurs. Above 10llQ-cm
back corona begins and becomes increasingly
severe as resistivity rises.”
With this in mind, the interpretation of data
becomes very critical for an ash such as sample 1-2
above, wherein the ascending values are not only
higher than the descending values but also are
’These resistivity values apply to flue gas pressures at sea
level. Appropriate adjustments should be made for other pres-
sure conditions.
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IEEE
Std 548-1984
above the critical corona onset value of 10” n-cm
(in contrast to the descending value, which is
below this criticalvalue). Rational speculation can
be given to explain why one value is greater than
another. However, no unequivocal evidence is
available to identlfy the cause.
One can reason that the freshly formed fly ash
surface is chemically attacked by adsorbed acid
vapor and adsorbed water vapor as it cools in the
flue gas and is collected. Often this hostile action
continues in storage where this ash can be exposed
to relative humidity much greater than that in a
precipitator. It has been shown [5]that “thermal
annealing” of the fly ash at 45 “C or higher after
severe surface abuse tends to restore the fly ash
surface to its original condition. Since the effect of
sulfuric acid adsorbed from the flue gas during the
-
D/A collection of the fly ash cannot be monitored in the
0.50 laboratory (see Appendix B), one is not concerned
0.15 about destroying this effect during the anneal. The
7.2 thermal anneal is the preliminary step to the de-
scendingtechnique for the resistivity measurement.
In an unpublished communication6, a labora-
tory has supplied information supporting the des-
cending technique. Two cases were cited in which
point-plane in situ resistivity measurements and
the precipitator electrical characteristics were in
agreement with descending laboratory resistivity
measurements and in disagreementwith the ascend-
ing values. In one case, the ascending data was an
order of magnitude less than the descending data,
and in the other, the ascending data was an order
of magnitude greater than the descending value.
No second laboratory has corroborated this obser-
vation; however, no laboratory has presented this
type of data to favor the ascending technique.
In another unpublished communication7,a labo-
ratory that has regularly run a “round trip” resis-
tivity test reports that the descending resistivity
values can be greater than but are never signif-
cantly less than the ascending values.
‘BICKELHAUPT, R. E., Southern Research Institute, Personal
letter to V. F. Estcourt, July 12, 1983.
7RAY,AB.,Research-Cottrell,Telephone conference with V. F.
Estcourt, June 9,1983.
25
 IEEE
Std 548-1984
C2. Variability Between Laboratories.As a result
of four Round Robins, the test procedure was pro-
gressively refined until, in Round Robin IV,the final
test procedure (6.3.3)yielded an acceptable agree-
ment in test results among the participatinglabora-
tories. This conclusion was supported by a statisti-
cal analysis of Round Robin IV data made by Mr.
Charles D. Rose of ASTM Committee E-11 on Sta-
tistical Methods. A quantitative precision state-
ment of the test method with respect to between-
laboratory variability was developed by Mr. Rose
from 137 individual resistivity measurements. Mr.
Rose found that the results of resistivity determi-
nations carried out by different laboratories on
representative portions taken from the same sam-
ple and using the same temperature, atmosphere,
and mode of measurement (ascending or descend-
ing mode) should not differ by more than a ratio of
2.7 (higherhower), 95%of the time (see 7.4.3).
C3. Within-Laboratory Repeatability. A subjec-
tive estimate can be made for repeatability (see
7.4.2),although replicate data were not obtained
in Round Robin IV that would have permitted
direct calculation of within-laboratory variability.
This estimate can be based on the statistical eval-
uation (see Appendix D) of between-laboratory
variability (reproducibility).
The ratio of 2.7 calculated for reproducibility
contains both within- and between-laboratory
components of variance. A subjective estimate for
the portion of the ratio only due to within-
laboratory variance is a ratio of ”two”for repeata-
bility as shown in 7.4.2.This estimate is based on a
typical ratio of repeatability to reproducibility
reported for ASTM standard procedures. The
IEEE subjective ratio of two provides a value
expected in a typical laboratory and should be
used as a general guide until a laboratory uses this
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IEEE STANDARD CRITERIA FOR THE LABORATORY
IEEE procedure for a large number of analyses
and develops a specific repeatability value using
their own data base.
C4. Preference for Test Mode (Descen
Ascending). Based on the available information,
the committee favors the descending technique for
the determination of resistivity in test environ-
ments, excluding sulfur oxides for fly ash pro-
duced from coal combustion. However, with an
effort to be prudent and conservative, the commit-
tee has selected the “round trip” technique. It is
hoped that with time, sufficient evidence will be
developed to confwm or refute the committee’s
opinion regarding the descending technique. The
round trip procedure will allow the user to have
available the preferred descending data without
sacrificing the ability to evaluate ashes containing
large amounts of combustibles, coprecipitated
thermally degradable conditioning agents, or ashes
involving other (as yet) undetermined factors of
influence with respect to the laboratory measure-
ment of resistivity.
The committee suggests that the data acquired
using the round trip technique should be inter-
preted by selecting the higher resistivity value at
the temperature of interest to be used for precipi-
tator design purposes. This will provide additional
assurance for a precipitator design with minimal
risk of undersizing, but, of course, with added risk
of oversizing. The committee realizes that there are
laboratories where superior judgment has been
developed as a result of unusually long and de-
tailed experience in this field of measurement. It is
assumed that subjective decisions with respect to
the interpretation of test results can be made
safely by these individuals.
 IEEE
MEASUREMENT AND REPORTING OF FLY ASH RESISTIVITY Std 548-1984

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 IEEE
Std 548-1984 IEEE STANDARD CRITERIA FOR THE M O R A T O R Y

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 IEEE
MEASUREMENTAND REPORTING OF FLY ASH RESISTIVITY Std 548-1984

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 IEEE
Std 548-1984
Appendix D
Background in Support of Precision
Statements (7.4.2 and 7.4.3)
The following statistical analysis of data from
Round Robin IVwas made for IEEE by Mr. Charles
D. Rose, a member of ASTM Committee E-11 on
Statistical Methods. The purpose of this work
was to develop a quantitative statement about
the precision of the test method with respect
to between-laboratory variability (reproduci-
bility).
D1. Calculation of Between-Laboratory Preci-
sion
D1.l Round Robin IV Data Reproducibility
was quantified statistically using 137 resistivity
measurements selected from Round Robin IVdata.
Four laboratories generated these data. Two of the
four laboratories used both ascending and de-
scending modes and accounted for 100 of the 137
measurements. Five ash samples were tested, and
data was taken from resistivity-temperature
curves at five common temperatures of interest
(110,150,190,300and 400 "C).
The participating laboratories had been given
instructions to explicitly follow the test standard
IEEE Std 548-1981except for two changes,result-
ing from Round Robin I11 data, which produced
additional specifications designed to reduce scat-
ter due to potential differences in ash-layer poros-
ity and starting conditions. The Round Robin data
provide a realistic and useful basis for evaluation
of between-laboratory variability that depicts typ-
ical laboratory performance. The initial report of
Round Robin IV to P-548 working group members
indicated success in achieving improved repro-
ducibility. The report further stated that the
reduced level of scatter among laboratories was
excellent.
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D1.2. Statistical Analysis, Data Transforma-
tion. In order to gain the considerable advantage
of working with normally distributed data, all raw
data were immediately given the transformation
x = lny
With temperature, mode of measurement, and ash
type each constant, the xis appeared to be normal-
ly distributed and suitable for statistical analysis.
Data from the two laboratories that used both
ascending and descending modes (100 measure-
ments) were examined. The average variances in
terms of x for given temperature, ash, and mode
came to ascending: 0.1041; descending: 0.1391.
Utilizing the F ratio test, these variances were
not found to be significantlydifferent on a statisti-
cal basis. Therefore, ascending and descending
data from all four laboratories were combined
(137 measurements) for a single statistical evalua-
tion to yield a standard deviation of 0.35.Because
the standard deviation of differences is f l u , the
following statement can be made to describe the
data from Round Robin Tv:Using the same temper-
ature, atmosphere, and mode of measurement, the
ratio (higherhower) of two measurements of
resistivity obtained by different laboratories on the
same ash will be expected to exceed 2.7 only 5%of
the time.
D1.3 Adequacy of Size of Round Robin Pro-
gram. Round Robin IV represents a good balance
between the ability to achieve accuracy in statisti-
cal analysis and a realistic degree of laboratory
participation. It qualifies as the basis for develop-
ing a standard precision statement using ASTM
practices.