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Document Name: ASTM D2986: Standard Method for Evaluation of Air,


Assay Media by the Monodisperse DOP (Dioctyl
Phthalate) Smoke Test
CFR Section(s):
40 CFR 86.1310-2007(b)(7)(i)(A)

Standards Body: American Society for Testing and Materials

Official Incorporator:
THE EXECUTIVE DIRECTOR
OFFICE OF THE FEDERAL REGISTER
WASHINGTON, D.C.
ASTM Logo
Removed

Designation: D 2986 - 95a (Reapproved 1999) An American National Standard

Standard Practice for


Evaluation of Air Assay Media by the Monodisperse DOP
(Dioctyl Phthalate) Smoke Test1 .
T~is.standard .is issu~d under the fixe~ ?esignation D 2986; the number immediately following the designation indicates the year of
ongmal adoption or, m the case of reVlSlOn, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (E) indica!es an editorial change s!nce the last revision or reapproval. .

1. Scope 3.2 Other terms are defined as follows:


1.1 The dioctyl phthalate (DOP) smoke test is a highly 3.3 optical owl, n-an optic~l instrument for visual estima-
sensitive and reliable technique for measuring the fine particle tion of the particle I;iiameter of the monodispetse aerosol by the
arresting efficiency of an air or gas cleaning system or device. angular dependence of light scattering, in accordance with the
It is especially useful for evaluating the efficiency d depth Mie theory. ..
filters, membrane filters, and other particle-collecting devices
4. Summary ·of Practice
used in air assay work. .
·1.2 The technique was developed by the U.S. Govemm~nt 4.1 A monodispersed aerosol of 0.3-1lffi diameter is continu-
during World War U. 2 Its validity for use in evaluation of air ously generated by condensation of DOP vapor under con-
sampling media has been well demonstrated. 3 · . trolled conditions. By selective value arrangement, a metered
1.3 Although a little latitude is pemiissiblein the associated P?rtion of thi~ aerosol is drawn through a specimen mount
equipment and in the operation method, experience has shown containing the item under test. Flowrate through the specimen
the desirability of operating within established design param- is adjustable and the corresponding flow resistance is noted as
~~~~.. .. .
eters and recognizeci test procedures. 4 . . .
1.4 This practice describes the present DOP te~t method, . 4.4With aerosol generation stabilized (constant particle size
typical equipment, calibnttioIl, procedures, and test particles. It and concentration), aerosol concentration is measured up-
is applicable for use with commercially available equipment. stream and downstream of the specimen under test by use of a
L~ This standard 'does not purport to address aU of the linear forward light-scattering photometer.
safety concerns, if any, associafed with its use. It is the 4.3 Results are expressed as percent of DOP penetration at
responsibility of the user of this standard to establish appro- the flow rate used.. .
priate safety· arid health practices and determine ·the applica- 5. Apparatus
bility of regulatory limitations prior to use. For specific safety
precaution, see 6.1. .. '.. . 5.~ EqUIpment for use with this technique consists of
several interoperationalparts. These ~e indicated in proper
2. Referenced Documents relative arrangement by the diagrapunatic sketch, Fig. 1. In
2.1 ASTM Standards: Fig: 1, the lette.r designations. refer to' the same parts as
D 1356 Terminology ~elating to Sampling and Analysis of ~escribed in: ~e immediately following subs(;lctions: .
Atmospheres 5 . . . ·5.2 'Air Supply Sourc~ (a)-This can be a blower as shown
diagratp.matically or a. compressed air source with stepdown
3. Ter~inology regulator. In any case, the air supply sOurce must be clean, free
3.1 Definitions-For other definitions of terms used in this of entrainment, and sufficient to provide fuil flow against the
practice, refer to Terminology D 1356. total resistance of aerosol generator and aerosol conductor lines
to the excess aerosol exhaust pqint. . .
5.3 DOPAerosol Generator (b)-The generator is designed
1 This practice is under the jurisdiction of ASTM COmJpittee D-22 on Sampling
and Analysis of Atmospheresand is the direct responsibility of Stlbcommittee to produce uniform size. liquid droplet particles of 0.3-1lffi
D22.010n Quality Control. . ... diameter at a concentration of about 100 ±. 20 IlglL of air.
Current edition approved Sept. 10, 1995. Published February 1996. Originally Further description of the generator IS given in 8.3.
published as D 2986-71. Last previous edition D 2986 - 95. .
2 Knudson, H. W., and White, Locke, Ens. USNR, "Development of Smoke
5.4 Aging Chamber ~c)-This is simpiy a large vessel
Penetration Meters," Naval Research Laboratory Report No. P-2642, P.B. No. (usually about 20 L in volume) wherein some dwell time is
119781, September 1945. provided to permit stabilization of the aerosol.
3 Smith, Walter, J., and Surprenant, N. E, "Properties of Various Filtering Media
5.5 .Sample Holder (d)":"'Si~e and design pf the sample
for Atmospheric Dust· Sampling,'! Proceedings, ASTM, Vol ~3, 1953, pp.
holder can be accommodated· to the item under test. However
1122-1135. .
4 Insiruction Mallual-Penetrometer. :£lilter Testing, DOP, Q127 136-30D-138B,
.;
for evaluation of filter media, ~ circular test area of 100 cm2 · ±
Edgewood Arsenal, MD, July 1963. . . 2 % is specified. Provision
. i~ ~acie
. . to measure flow resistance
5 AnnualBook of ASTM Standards. Vol 11.03.

Copyright © ASTM, 100 Barr Harbor Drive. West Conshohocken, PA 19428-2959, United States.

65
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D 2986
Excess Aerosol Vent
Particle Size Meter
Mechanical Analyzer
e

g ng
Chamber er

Exhaus t Pump
or Blower

Air Cleanup
Su~ply
Filter
(IIEPA)

Scattering
Chamber

Absolute Filter
(IIEPA)

FIG. 1 Simplified Diagram Showing Relation of Principal Parts of DOP Aerosol Test Apparatus

across the test piece. A wire screen may be used to support the NOTE I-DOP is under investigation as a possible carcinogen. Use only

sample. by trained persounel wearing appropriate safety equipment to avoid skin


contact and inhalation.
5.6 Particle Size Analyzer (e)-Particle size in the aerosol is
indicated by the particle size analyzer. The visual owl may be 7. Procedure
used to verify the aerosol particle size. The electronic owl is an
adaption designed to remove the human factor; it has proven to 7.1 It is necessary to have the equipment prepared and
be highly successful. Both instruments operate by optical calibrated in advance of any test work. Once prepared and in
rotation bf light scattered at a 90° angle. Paragraph 8.4 gives adjustment, the equipment can be turned on at any time and
further detail for the optical owl. operated as long as desired with only occasional minor
5.7 Scattering Chamber (f)-The scattering chamber is readjustment. Instruction for preparation and operation of each
used to determine concentration of aerosol either upstream or item of equipment is given below.
downstream of the item under test. Further detail for a typical 7.2 Aerosol Generator-Tum on the air supply and heating
chamber is given in 8.5. units of the DOP aerosol generator. Wait until the aerosol
5.8 Photometer (g)-This is a combination of sensitive output has been stabilized; usually this will require V2 h or
multiplier phototube and meter. The multiplier phototube more from a cold start. Draw a portion of the aerosol through
mounts on. the scattering chamber and detects light forward the particle size analyzer, verify the aerosol particle size, and
scattered by any particles in the chamber. Further description adjust generator conditions until particle diameter is 0.30 /lffi
of the photometeris given in 8.6. (by adjustment of quench air temperature).
5.9 Flowmeter (h)-A float-type flowmeter (rotameter) is 7.3 Adjustment of Photometer-Using the same flow rate
used, capable of reading a flow rate well in excess of the that will be used for the test specimen (usually 32 Llmin± 2 %
maximum test rate to be used. A meter reading somewhat through 100 cm2 of area ± 2 % when testing filter media),
above 100 Llmin is the common size. It must be protected aerosol from the generator is passed directly through the
against fouling by any DOP accumulation. scattering chamber. Adjust the Gain potentiometer of the
5.10 Exhaust Pump or Blower (i)-This qm be either a galvanometer circuit in the photometer until the meter reads
positive displacement pump or blower or a multistage turbine- 100.0.
type blower. In any case, there must be more than sufficient 7.3.1 Draw clean filtered air through the scattering chamber.
capacity to draw air through the total resistance of test Adjust for stray light so that the photometer meter reads zero
specimen, scattering chamber, flowmeter, and all of the related on the most sensitive scale.
lines, valves, filters, etc., at the maximum test,rate (usually 85 7.4 Penetration Measurement-Mount the, sample to be
Llmin). tested in the sample holder, making certain that all seals are
5.11 Cleanup Filter G)-;;This should be, a filter of suffi-, tight. Draw aerosol through the test specimen. Adjust flow rate
ciently high capacity and efficiency to remove smoke from the to the desired level, for example, 32 Llmin. Starting with the
airstream before it passes through the flowmeter. Aerosol least sensitive range, use progressively higher sensitivity until
particles would ultimately affect the accuracy of the meter. a reading can be obtained.
7.4.1 Read the photometer. Report the value as percent DOP
6. Reagents and Materials penetration.
6.1 dioctyl phthalate, (DOP)-Technical grade. 7.5 Flow Resistance-At the beginning of the penetration

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D 2986

A-Smoke chamber and light-scattering tube J-Polaroid analyzer tube


B-Smoke inlet port K-Light collecting lens
C-Smoke outlet port L-Bipartite disc (split field polaroid)
D-Light source M-Polaroid disc mounted in movable collar
E-Lens to form parallel beam of light through smoke chamber N-Indicator on polaroid holder to show angle of displacement from verticle axis
F-Baffle to reduce stray light scattered from walls of chamber O-Degree scale for indicator (N)
G-Velvet-lined cap on chamber . P-Green filter for obtaining monochromatic light
H-Side arm to light scattering tube Q-Adjustable eyepiece
I-Smoke-retaining window R-Lens in eyepiece
FIG. 2 "Owl" Particle Size Meter

test and after the desired flow rate has been established, the 8.2 Air Supply-Any reliable air source may be used that is
manometer is read, showing the resulting pressure drop across capable of supplying 120 Llmin. If taken from a compressed
the test specimen. This may change after a short time due to air system, a stepdown regulator should be used, followed by
accumulation of DOP in the test piece. Ordinarily, the reading a control value, and a good commercial air-line filter ahead of
is reported in millimetres of water pressure. the high-efficiency (HEPA) filter.
7.6 Other Data-Line temperature and manometer readings 8.2.1 For a mobile unit or where a compressed air line is not
at the flowmeter should be noted along with the current available, a blower can be used. A multistage blower, turbine-
barometer reading so that airflow rates may be reduced to type, is effective and will run continuously with very little
standard conditions if this is required at some later time. maintenance. An absolute (HEPA) type filter is used custom-
7.7 Q Value-When comparing the filter efficiency of vari- arily in the supply line to ensure that the air is entirely clean.
ous media, it is often useful to report filter performance in 8.2.2 In any case, provision must be made to either cool or
terms of the Q value. Calculate Q value as follows: heat the air as conditions may require. Commercial heat
Q = [-100 log (P/lOO)J/~p (1) exchange equipment is satisfactory.
8.3 Aerosol Generator-The aerosol generator consists of a
where:
pot containing about 500 mL of DOP at about 170°C. DOP
P = DOP penetration, %, and
Ap = airflow resistance, mm of water. vapor is carried from the container by a small heated airstream
(about 215°C) and mixed with a larger stream of quench air
S. Discussion of Equipment (about 25°C) to form the aerosol particles. The airstream
8.1 Availability-Although equipment for the DOP test is temperatures determine particle size and, once established
commercially available, some care must be exercised in its must be precisely controlled. The aerosol is generated continu-
procurement. While the test is well developed and very ously; excess aerosol is disposed of away from the test area.
reliable, the equipment is complex. It must be within certain 8.4 Owl-A typical "Owl" is shown in Fig. 2. A reading of
design parameters and must be carefully fabricated. Design 29 ± 1° corresponds toO.3-fllTI diameter DOP particles.
details are available4 but it is strongly recommended that 8.5 Light-Scattering Chamber-The light-scattering cham-
purchase be made of equipment from a professional fabrica- ber shown diagrammatically in Fig. 3 is an essential compo-
tor. 6 nent of the photometer system. Any airborne particles entering
the chamber are strongly illuminated and the forward-scattered
6 Equipment suitable for the DOP test may be obtained from Air Technology,
light intensity is detected by a multiplier phototube (H).
Inc., 1717 Whitehead Rd, Baltimore, MD 21207. 8.5.1 Light from the lamp bulb filament (A) is focused at the

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1 .T

A-Light source F-Backlens


B-Front lenses G-Rear light baffle
C-Optical filter or light screen H-Multiplier protCltube
D-Opaque disk I-Filament image'
E-Center light baffle J-Inlet port
K-Outlet port, '.
FIG. 3 Light-Scattering Chamber-Schematic Section Showi'ng .optical System

center of the light tube (E) by means of condensing lenses (B). 9.2.2 See that all temperatures are correct and that controls
An opaque patch (D) cemented to the inside facing of the are functioning properly. I
condensing lens intercepts any direct light from the filament to 9.2.3 If supply air or quench air must be cooled, see that the
the phototube. i' , cooling water is turned on. . . .,' .
8:5.2 The stop opening at (E) has a, beveled edge, thus 9.2.4 Check aerosol particle' size and make any adjustments
providing a knife edge periphery to the opening. This 'is- needed to maiiifhlIi O.3-I.mf diameter.' , , 'l

important in keeping the amount of 'light scatter from this , 9.3 No Aerosol Generation:
illuminated edge at a bare minimum. 9.3.1 Make sure that air supply is working properly.
8.5.3 Take every care to ensure that only lighL forw.ard-,. 9.3'.2 See that all heaters are on and working.
scattered by the test aerosol is seen by the phototube. Follow- 9.3.3 Check DOP level or supply.
ing, are points requiring speciaL attention: :9.3.4 See: that" both heatedaii; and quench air are being
.K5;3.1 Optics,. must he aCC,urately aligned with theoptipal suppliedilnd at,theiptopet 'rates. '
ax:is,. The ,light bulb filament, image should be focused at the , 914' Partidle) Size Analyzer!'
center of the 'light stop opening. ; . , .. ' ! , 9A.1 See\lftat'the analyzer'lamp is lighted.
8.5.3.2 All lens surfaces mu.Stbe perfe,ctly clean; otherw~e, 9.4.2 Make sure that aerosol is flbwihg tht6ugh the instru-
light scatter will result. ,\. . " I, fuent(exha:usFo16We{orpuilipfutri'~d on and the analyzer line
" 8I p.3.3; AJllel1s'?4ge~, especially if tht1yare ground sur- \ralve open,). " '.'
fa~es, s~ouJd pe painted, with flat black, , , '. 9A.3 See '~at connection tUbes' t9 'the ailalYZer are not
.8. 5.;3.4~9 frostecl or etched d~sign Of;, figurl1 can be permit, pinched. " , " ' , ' i ,," I'i' .i,' " "
~crP op. theJight,buJp envelop facing the .condensing lenses.
9:4.4 Adjiist'quepbiI air tenipetatfue toattiiiil cbrre~+particle
8.~.3.5,:rl;1esl;1aw
,I ',1,. ",
edge
'.
,,~
of
,
th~ ligpt stop mJ,lst be fre~ of
'j • ,: • .' I . ~
size.,;I, ,~';.~ ~q' '(','" ~ _t, ·r l' ''"' . .,; " .: ,
nicks,butrs, .9r even !l~~ached part;ICles. , , 'J 9.5 Phdtofti~t~'r Not Re'a'aing:" ,". I'
'8'.5.3.6 Light bulbcu'rreIlt,~ust be sUPI?,~redfroIll, a '~9ltage~
stabilized circuit. '"' : ' .9.5.1 See that the lamp is' lighted in the scattering chamber.
9.5.2 See that the amplifier is plugged in and operating,
~.?PhqtqrJ(~ter~Vanqu~ rypes ,of' photometers ar~, i~ use:
ltl'moSt, a Type 931A multiplier phototube is' bnerated 'at output 9.5.3 Make sure that aerosol is,:(lo,wmg Jhrpugh the scatter-
dnfei1ts b~i6W 30 !1A td lbkllre'stable dperaHon. f,. sc~e switch in
ing chamber (selector valve. rn~ POS:i#9II and not purge).
pertOiis The'nieasurethents do~n tit 0.001 % OJ 0.0001 % 9.5.4 See that multipler phototube is mounted on the scat-
pehddUonOf DOP'·strtoke." ' , i " h' , tering chamber and that lead wires' : tire; conne6ted in: the
"i.,i" ;," ,', • (" l:il, amplifier.,. 'l.· " ,
9. 'Maintenance' and Troubleshooting· , 9.;6 Photometer :Cannot .be Adjustedfor, 100. % Reading:
i 9,;6.1 Make sure' that aerosol generator is ,Q'peratingr prolD~rly.
,.', " .: ".". .' ," '.'''' "1.,'. r
9.'1 When used tdutinely, the DOPtest" 'is rehable and
seldom' ptesents"any ;serious' proolei:ris. Expenencewill' s60n ,:9.6.2 ,Make sUre' that,;multiplier phototube;~s, properly ad-
show,the';operatoi what steps' iritistb~ followed to'rrtaintrun ju~ted. .:,<) ,d, ,i;, " ',:. ~) "

fully sa,tisfabtory, equipment perfonhimce~ However, t'oassist ':,9.7 Rhotometer Canrzot,be.AdjustedJorrStray!Light:, :;gJ.
the; neophyte"especially, tlte, following' basic suggestions are ,9 :h1 The usu'al fl:J.ult is' excessi;ve:stray ligHtlin the scattering
offered: ' j .,. ;1' '
'; " " , (, chamber. Adjust position of the light source (instruIi1ent
9.2, Ddily, Care: manual) to attain minimum reading on clean air.
9.2.1 Asc'ertain"that the, DOP'liquid',level or supply: is .'\.'. 9.7.2
~ \: 11
i
A~certajn. that the amplifier
: • ,'" , y,;. _ .
~s:', perforp:ring
', ".' .f"
correct;ly.
I, .• <1 1'1'
"!' . •

adequate., , ,i' '9.7.3 Have the phototube an~:lc9.n.nec;ti,ngde~ds ,ghecked..

68
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02986
9.7.4 Make sure there are no leaks into the filtered air supply regarding calibrated plates, inquire of the manufacturer. 7
line. Leaks will introduce particulate matter and cause a meter 10.1.2 Leaks in the system can be serious since they will
reading. impair the accuracy of flow rate ~eadings. Every precaution
must be taken to ensure tightness in lines, instrument filters,
9.7.5 If the problem persists, the source of stray light
and fittings. ,
sometimes can be detected by removing the multiplier photo-
10.1.3 Reference Filter Paper-It is convenient to have on
tube and looking into the scattering chamber. This approach hand a supply of high-efficiency filter paper that has been
should be taken only by someone thoroughly familiar with the pretested and preferably cross-checked by at least one other
equipment. laboratory. Ail occasional test run on one of these filter samples
will be reassuring and indicative that all is well. Results may be
10. Quality Control plotted on a control chart to demonstrate attainment of statis-
tical control of the measurement process. 7
10.1 Following are steps thilt can be taken to help ensure a
11. Keywords
reliable bias and agreement between laboratories:
11.1 atmospheric analysis; air assay media; collection effi-
10.1.1 Calibrated Orifice Plate-Orifice plates are avail- ciency evaluation of filters; dioctyl phthiLlate, use for filter
able ,·with:· calibrations traceable to the National Institute of evaluation; high efficiency filters; membrane filters; particle
Standards ,and Technology (formerly NBS). The, plate is collecting devices; smoke test for filter evaluation
inserted in the sample holder and used as aflowmeter against
which the instrument flowmeter is compare.d. For information 7 Taylor, John K., "Quality Assurance of Chemical Measurements," Lewis
Publishers, Inc., Chelsea, MI (1987).

, , The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned iri this standard. Users of this standard are expressiy advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility. ,
,
This standard is subject to revision at any time by the responsible technical committee and must be reviewed evel}' five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
. 1.' and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible
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