&EPA
United States
Environmental
Protection Agency
Office of
Pollution Prevention
and Toxics
EPA 747-R-94-004B
March 1995
Laboratory Evaluation of Dust
and Dust Lead Recoveries for
Samplers and Vacuum Cleaners
Volume II:
Appendices from the
Quality Assurance Project Plan
-------
March 1995
EPA 747-R-94-004B
LABORATORY EVALUATION OF DUST
AND DUST LEAD RECOVERIES FOR
SAMPLERS AND VACUUM CLEANERS
VOLUME II: APPENDICES FROM THE
QUALITY ASSURANCE PROJECT PLAN
Technical Program Branch
Chemical Management Division
Office of Pollution Prevention and Toxics
Office of Prevention, Pesticides, and Toxic Substances
U.S. Environmental Protection Agency
Washington DC 20460
Recycled/Recyclable • Printed with Vegetable Based Inks on Recycled Paper (20% Postconsumer)
-------
The material in this document has been subject to Agency technical and
policy review and approved for publication as an EPA report. Mention of
trade names, products, or services does not convey, and should not be
interpreted as conveying, official EPA approval, endorsement, or
recommendation.
u
-------
CONTENTS
Introduction 1
LIST OF APPENDICES
A PROTOCOL FOR COLLECTING AND HANDLING USED HOUSEHOLD
VACUUM CLEANER BAGS A-l
B PROTOCOL FOR SIEVING HOUSEHOLD DUST B-l
C PROTOCOL FOR GRINDING DUST INTO CARPET C-l
D PROTOCOL FOR CONDITIONING CARPET AND OTHER
SUBSTRATES D-l
E PROTOCOL FOR WIPE SAMPLING OF DUST E-l
F PROTOCOL FOR VACUUM SAMPLING OF DUST WITH THE
MODIFIED R&M HVS3 CYCLONE SAMPLER VAC F-l
G PROTOCOL FOR VACUUM SAMPLING OF DUST WITH THE CAPS
CYCLONE SAMPLER VAC G-l
H PROTOCOL FOR VACUUM SAMPLING OF DUST WITH THE BLUE
NOZZLE SAMPLER VAC H-l
I PROTOCOL FOR VACUUMING AND SAMPLING OF DUST WITH
HOUSEVACS 1-1
J DIGESTION PROCEDURE - MODIFIED METHOD 3050 FOR ANALYSIS
OF LEAD (Pb) IN WIPE DUST SAMPLES J-l
K DIGESTION PROCEDURE-MODIFIED METHOD 3050 FOR ANALYSIS
OF LEAD (Pb) IN VACUUM DUST SAMPLES (CASSETTES OR
BOTTLES) COLLECTED WITH A SAMPLER OR HOUSEVAC K-l
111
-------
L ANALYTICAL PROCEDURE-MODIFIED 6010A FOR THE ANALYSIS
OF DIGESTED SAMPLES FOR LEAD(Pb) BY INDUCTIVELY COUPLED
PLASMA (ICP-AES) PLUS MODIFIED METHODS FOR FLAME ATOMIC
ABSORPTION (FAAS) AND GRAPHITE FURNACE ATOMIC
ABSORPTION (GFAAS) TECHNIQUES L-l
M GLASSWARE/PLASTICWARE CLEANING PROCEDURE M-l
N ACID BATH MAINTENANCE PROCEDURE N-l
O PROTOCOL FOR SAMPLING HOUSEVAC EXHAUST EMISSIONS O-l
P TEST PATTERN, HOUSEVACS P-l
Q TEST PATTERN, SAMPLERS Q-l
R PROTOCOL FOR CONDUCTING TESTS WITH SAMPLERS R-l
IV
-------
1 INTRODUCTION
This project to expand the knowledge on household dust testing methods was
undertaken by the U.S. Environmental Protection Agency (EPA) as part of a major
national effort to address the public health issue of childhood lead poisoning. The effort
was given impetus by the CDC's statement on lead poisoning, which reduced the level
of concern for blood lead levels from 25 micrograms/deciliter (jig/dl) to 10 M-g/dl. It
has also been given impetus by the passage of the "Residential Lead-Based Paint Hazard
Reduction Act of 1992," also known as "Title X." In response to Title X, EPA is
proceeding towards the development of health-based standards for house dust lead
levels. To do this, appropriate methods for sampling house dust are needed. As part of
this effort, numerous questions about house dust sampling have risen. This study was
designed to address some of these questions.
This project was undertaken by the EPA Office of Pollution Prevention and Toxics
(OPPT) to evaluate house dust sampling methods and to assess the efficacy of typical
household vacuuming on removing leaded dust from residential surfaces. Dust-lead
sampling results from the National Survey of Lead-Based Paint in Housing (HUD
National Survey) are reexamined, based on new information collected in this study
about the performance of the dust sampler used during that survey.
Two standardized laboratory testing procedures were developed for this study. The
first procedure was designed to characterize the performance of house dust samplers.
The second was designed to evaluate how well commercially available vacuum cleaners
collect dust from various surface types. Three vacuum sampling methods and one wipe
sampling method were tested by the first procedure. These methods included the
"Farfel modified" High Volume Small Surface Sampler used in the Baltimore Repair and
Maintenance study (called the BRM sampler is this report), the Comprehensive
Abatement Performance Study (CAPS) cyclone sampler, the Blue Nozzle sampler, and
the Department of Housing and Urban Development's (HUD) wipe sampling method.
All of these sampling methods have been used in previous EPA/OPPT studies. The
second procedure was used to characterize four commercially available household
vacuum cleaners ranging in price from $120 to $800. The most expensive vacuum
cleaner was equipped with a high efficiency particulate air (HEPA) filter. The protocols
for both testing procedures included using real house dust sieved into six particle size
classes ranging from 0 to 2,000 microns in size. The dust was applied to five substrates
commonly encountered inside a residence: tile, wood flooring, linoleum (sheet vinyl),
upholstery, and carpet.
A secondary purpose of the project was to assess the amount of dust exhausted into the
air while dust is being vacuumed. The Federal government has concerns that routine
vacuuming of highly lead-contaminated dust may create unseen health hazards by
polluting the air with lead particles. Lead abatement specialists use vacuum cleaners
equipped with a HEPA filter to clean up lead-contaminated dust. The HEPA filters
prevent fine lead particles from escaping the vacuum cleaner through the exhaust and,
thus, prevent a potential airborne lead hazard. While vacuum cleaners fitted with
-------
HEPA filters are available, they usually are expensive and not readily accessible to the
general public, although the situation is improving. This project measured the recovery
and exhaust emissions of lead dust in a laboratory setting by four different vacuum
cleaners currently available for household use. One of these vacuum cleaners was
equipped with a HEPA filter.
The sampling and analysis procedures and the project organization are described in the
Quality Assurance Project Plan for the Wipe and Vacuum Study (QAPjP), Revision 1
dated September 24, 1993. The protocols for collecting and handling household dust
used in the tests, preparing the substrate sections for the tests, operating the samplers
and vacuum cleaners, and performing various steps for the analysis of lead are
contained the QAPjP appendices.
The study report is divided into two volumes. Volume I presents the background,
methods, and study results. For readers interested in the specific sampling and analysis
procedures or those interested in replicating the procedures, Volume II contains the
appendices from the QAPjP which describe the sampling and analysis procedures. The
Table of Contents lists the various appendices. In the original QAPjP, the BRM sampler
was referred to as the HVS3 sampler. The terminology was changed for this report to
better describe the sampler. In these appendices the term HVS3 has been changed to
BRM except on copies of the data collection sheets used during the study. Any such
reference to HVS3 refers to the BRM sampler, the sampler used in the Baltimore Repair
and Maintenance study.
-------
APPENDIX A
PROTOCOL FOR COLLECTING AND HANDLING USED
HOUSEHOLD VACUUM CLEANER BAGS
M»-OPPT\R55-90.APA
-------
Protocol: Collecting Household Dust
Revision No. 1
September 24, 1993
Page 1 of 2
PROTOCOL FOR COLLECTING AND HANDLING USED
HOUSEHOLD VACUUM CLEANER BAGS
1.0 INTRODUCTION
This protocol provides instructions on how to obtain and prepare household
dust to perform the tests according to the QAPjP. Based on the results from the
National Survey, the assumption is made that lead levels in household dust correlate
with the age of the dwelling. Thus, household dust vacuum bags will be collected
from homes built in or after 1983 (newer homes) and in or before 1962 (older homes).
All three organizations involved in this task participate in the collection.
2.0 COLLECTION PROCEDURE
• Within each organization (EPA, MRI, and Westat), distribute kitchen trash bags with
the following instructions to volunteer staff in their organizations:
• Put (preferably full) used household vacuum bag (bag and dust) in trash bag. Do
this carefully so that the dust from the vac bag does not blow out into the trash
bag.
* Close trash bag with twist tie.
« Indicate on enclosed label whether home was old (1962 or earlier) or new (1983
or later). Attach label to trash bag.
• Bring bag to designated area.
• Collect the vacuum bags with their dust content at each organization. Each vacuum
bag will be in a separate kitchen bag and tagged as to the age of the home (older
or newer).
3.0 STERILIZATION PROCEDURE
• After collection, package the bags in cartons at each organization and ship via
Federal Express to the following address:
MRI-OPPT\R3MO.APA
A-1
-------
Protocol: Collecting Household Dust
Revision No. 1
September 24, 1993
Page 2 of 2
Neutron Products
Attn: Ms. Geraldine Barrett
22301 Mount Ethraim Road
P.O. Box 68
Dickerson, MD 20842
Telephone: (301)349-5001
At Neutron Products, have the bags sterilized by radiation, according to the proce-
dure developed by RTI and followed by ORD and NIST.
After sterilization, have Neutron Products ship the cartons from all three
organizations back to MRI by Federal Express.
A-2
MRI-OPPTAR55-90.APA " *•
-------
APPENDIX B
PROTOCOL FOR SIEVING HOUSEHOLD DUST
MFH-OPPT\R35-90.AP8
-------
Protocol: Sieving Household Dust
Revision No. 1
September 24, 1993
Page 1 of 9
PROTOCOL FOR SIEVING HOUSEHOLD DUST
1.0 INTRODUCTION
The household dust is contained in the original vacuum bags collected by EPA,
MRI, and Westat volunteers. Each bag has been sterilized by radiation and shipped
back to MRI (see Appendix A). The bags will each be tagged as to the two categories
of homes: built in or before 1962 (older homes), or built in or later than 1983 (newer
homes). This protocol provides instructions to sieve the dust in both categories into
six particle size classes. The sieved fractions from each category will be composited
and used as the test dust for the laboratory testing under this project.
2.0 EQUIPMENT AND SUPPLIES
• Vacuum dust bags
• Six 8-in stainless steel sieves, soldered with 100% tin, lead-free, as follows:
t
« Less than 2,000//m: Sieve No. 10
4 Less than 250 /ym: Sieve No. 60
« Less than 212 //m: Sieve No. 70
* Less than 150//m: Sieve No. 100
* Less than 106/ym: Sieve No. 140
* Less than 53 jjm: Sieve No. 270
• 8-in pan with lid
• Mechanical shaker sieving device
• Plastic containers for sieved dust (minimum of 12)
• Balance to weigh full bags and to weigh sieved dust in containers
• Balance to weigh samples of sieved dust
• Soft brush
• Plastic trash bags
B-1
-------
Protocol: Sieving Household Dust
Revision No. 1
September 24, 1993
Page 2 of 9
• Small plastic bottles for samples of sieved dust (24)
• Ziplock plastic bags
3.0 PREPARATION PROCEDURES
• Weigh the dust bags separately in each of the two categories and record total
weight for each category on data entry forms at the end of this Appendix B.
• Label containers as follows, where "high" corresponds to dust samples from older
homes and "low" corresponds to dust samples from newer homes:
1. High: 250-2,000 //m
2. High: 212-250//m
3. High: 150-212//m
4. High: 106-150//m
5. High: 53-106//m
6. High: less than 53 //m
7. Low: 250-2,000 //m
8. Low: 212-250 /vm
9. Low: 150-212//m
10. Low: 106-150//m
11. Low: 53-106//m
12. Low: less than 53//m
• Weigh at least 12 empty plastic containers (tare weight) in which sieved dust
composites will be stored, and record weights on data entry forms at the end of this
Appendix B.
4.0 SIEVING PROCEDURE
NOTE: Always keep the two categories of dust bags (older homes and newer
homes) separated. Start with the bags collected in the newer homes to
minimize lead contamination.
• Clean the sieves with compressed air and/or a soft brush. Material lodged in the
sieve openings or adhering to the sides of the sieves should be removed (if possible)
without handling the screen roughly.
B-2
-------
Protocol: Sieving Household Dust
Revision No. 1
September 24, 1993
Page 3 of 9
• Nest the sieves in decreasing order in the sieving device, with pan at the bottom.
(Sieving device to be located in a hood.)
• Empty dust bag(s) from one category homes onto top sieve. Empty as many bags
as necessary to have sufficient dust sample on top sieve. Discard empty vacuum
bags in trash bag.
• Sieve for 5 minutes. Redistribute material on top of sieve and sieve for 5 more
minutes.
• Discard material from top sieve in trash bag.
• Collect the dust samples from all but the top sieve and from the pan and transfer
to appropriate labelled containers.
• Repeat sieving procedure with additional bags from one home category until enough
dust is obtained in each size category are exhausted. Use additional containers if
necessary.
• Weigh containers when full or when sieving is completed and record total weight
of each container on weighing form (see Section 3.1 of QAPjP).
• Clean the sieves with compressed air and/or a soft brush, whenever necessary
during sieving operations.
• Repeat dust sieving, dust collection, weighing and recording for the second
category of dust bags (older homes).
• For each category of dust bags, sieve additional bags until enough dust has
been obtained for the tests. For dust from older homes, start with those bags
which can be identified as coming from the oldest homes, if possible.
5.0 PREPARE SAMPLES FOR ANALYSIS
• Obtain 24 small, clean plastic bottles for samples to be analyzed. Place a bar code
label on each bottle and an identical label on the weighing form. Also, place a
handwritten label on each bottle that identifies the test category and class (new
homes/old homes, size class).
B-3
-------
Protocol: Sieving Household Dust
Revision No. 1
September 24, 1993
Page 4 of 9
Weigh the empty bottles (with lid and labels). Record weight on data form.
• Thoroughly mix the contents of each container of dust.
• Take 10 small subsamples (approx. 70 mg each) from each container of dust (or
from all containers in which that dust category is stored). Composite these
subsamples into the sample bottle for that category. Repeat this subsampling once
to obtain duplicate samples.
• Reweigh the sample bottles containing the composite samples (total of 24 samples,
including duplicates). Record weight on data form, and test number per attached
test sequence.
• Place each sample bottle in a ziplock plastic bag. Submit samples for Pb analysis.
The Data Entry Sheet for Initial Analysis of Sieved Dust is shown following paragraph
6.0
6.0 COLLECTION OF SIEVED DUST SAMPLES BEFORE TESTS, AND WEEKLY
Samples of sieved dust will be taken for Pb analysis just prior to the tests and weekly
thereafter (total of 12 samples each week). These will be taken in a manner that
duplicates the application of dust onto substrates. Approximately 0.678g of each
category of dust (size and Pb concentration) will be taken, and using the dust
application device, the dust will be collected on a plastic sheet. Dust on the plastic
sheet will then be transferred into a weighted sample bottle and analyzed for Pb. Data
forms for these samples, and the test number sequences are found following this
paragraph.
B-4
-------
Data Form for
Sieving of Dust Bags
Date
Operator
Dust Bags from
Number of Dust Bags Sieved
Total Weight of Bags Sieved
(in grams)
(old or newer homes)
Weight of Dust Recovered fbv size):
Final Wt (g)
Tare Wt (g)
Net
< 53 um
53-106 urn
106-150 um
150-212 um
212-250 um
250-2.000 um
Reviewed by
B-5
-------
Data Entry Sh««t
for
Initial Analytic of Sfovad Dust
Procedure
Test No.
Thoroughly mix each container of dust from new homes
Tare weigh 1 2 sample bottles, with bar code labels
Take 10 random subsamples of about 70 mg each from one container, and
combine in first sample bottle
Re weigh sample bottle after taking 10 subsamples
Repeat preceding step (i.e., duplicate sample)
Repeat the above steps for each size of dust (total of 1 2 samples including duplicates)
Using new data sheet, repeat all the above for dust from the older age of homes
Date
Operator
Dust Type
(old or new homes)
Sample Weight (Balance No.
Sample Weight (Balance No.
< 53 um
Final Wt
Tare Wt
Net
< 53 um (dup)
Bar Code
Label
Final Wt
Tare Wt
Net
Bar Code
Label
53-106 um
53-106 i/m (dup)
Final Wt
Tare Wt
Net
Bar Code
Label
Final Wt
Tare Wt
Net
Bar Code
Label
106-150 um
106-1 SO um
Final Wt
Tare Wt
Net
Bar Code
Label
Final Wt
Tare Wt.
Net
Bar Code
Label
150-212 um
150-212 um
Final Wt
Tare Wt
Net
Bar Code
Label
Final Wt
Tare Wt
Net
Bar Code
Label
212-250 um
212-250 um
Final Wt
Tare Wt
Net
Bar Code
Label
Rnal Wt
Tare Wt
Net
Bar Code
Label
250-20OO um
250-2000 um
Final Wt
Tare Wt
Net
Bar Code
Label
Final Wt
Tare Wt
Net
Bar Code
Label
Date
Samples Relinquished by:
Samples Received by:
Reviewed by:
B-6
-------
Data Entry Sheet
for
Pretest and Weekly Analysis of Sieved Dust
Procedure
Collect sample of each dust size, from new homes, as follows:
Take approximately 0.678 g from dust container
Deposit dust through sieve, onto plastic sheet, to simulate depositing of
dust on substrate
Determine weight of dust deposited
Transfer dust on plastic sheet into labeled and weighed sample bottle
Determine weight of dust sample in sample bottle
Repeat all the above for each particle size
Using new data sheet, repeat all the above for dust from older homes
Test No. _
Date _
Operator _
Dust Type
(old or new homes)
Dust Applied (gm)
(Balance No. )
Total Wi Final Wt
Total Wt
Dust Sample (gm)
(Balance No. )
Tare Wt
Net Wt
> 53 um
Bar Code
Label
53-106tfm
Bar Code
Label
106-150 um
Bar Code
Label
150-212 um
Bar Code
Label
212-250 um
Bar Code
Label
250-2000 um
Bar Code
Label
Samples Relinquished by:
Samples Received by:
Date:
Reviewed by
Date
B-7
-------
Lead concentration in the source dust
Table shows each sample of dust collected tot analysis
Test Sequence for Samples of Dust
. Test
number
Substrate sample
Lead
Substrate Dust Loading Cone
Particle size
New
bag
Dust
deposited
(n»g)
Vacuum
Team
time
vacuumed
dust
collected
(m$
dust sent for
analysis (mg)
lead
amount
(ug)
Date
Collected
Time
collected
Target
Dust
deposited
(K)
Sample of dust for analysis
CD
CO
Sample of dust for analysis
601
602
603
604
605
606
607
608
609
610
611
612
621 Sample of dust for analysis
622
623
624
625
626
627 Sample of dust for analysis
628
629
630
631
632
641 Sample of dust for analysis
642
643
644 „
645
646
647 Sample of dust for analysis
648
649
650
651
652
Low
Low
Low
Low
Low
Low
High
High
High
High
High
High
Low
Low
Low
Low
Low
Low
High
High
High
High
High
High
Low
Low
Low
Low
Low
Low
High
High
'High
High
High
High
<53
53-106 ;';• '
106-150 ', ;-.%
150-212 <"~\
212-250 *>'-'-,*
250-2000 vV-;'
<53 ;,;>
53-106 £v',, '
106-150 ';<,
150-212 ?;,"•,'
212-250 f;i:t
<53 r-::;:f-
53-106 :-/;';'',i
106-150 \;:V, .'
150-212 ^; "'-,
212-250 ! '•'>.:>
250-2000 't^'\'
150-212 ~g%
212-250 °,s<'.\ i
250-2000 r;;,,;;'
<53 )'-',j;7^
53-106 |;,v;|;1
106-150 ;; ;V;;'
150-212 i|fjiH
212-250 j',;,;;./, 5
250-2000 |;v»a*'i
<53 ?/;^f!;i
53-106 i.*f^
106-150 p^%
150-212 |CTf/^
212-250 i'",$\\
250-2000 i'j/l'
Prior to testing
> «* •~"v
:;- - v'}«£5,, ?••'' i' f I| i I •
'•''3'~J•.'' i '< xf ^** ft <' /'-,'-^ <'
Prior to testing (duplicate)
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
-------
Lead concentration in the source dust (continued)
Table shows each sample of dust collected for analysis
Test
number
Substrate sample
Substrate
Dust Loading
Lead
Cone
Particle sizel
New
bag
Dust
deposited
00
(b
661 Sample of dust for analysis
662
663
664
665
666
667 Sample of dust for analysis
668
669
670
671
672
681
682
683
684
685
686
687
688
689
690
691
692
701
Sample of dust for analysis
Sample of dust for analysis
Low
Low
Low
Low
Low
Low
High
High
High
High
High
High
Low
Low
Low
Low
Low
Low
High
High
High
High
High
High
53-106
150-212
212-250
250-2000
53-106
•* r\f * c« |N^^§w«Nf
106-150
1 50-71") ifellli
fepKl^t"*
212-250
250-2000
<53
53-106
106-150
150-212
212-250
250-2000
<53
53-106
106-150
150-212
212-250
250-2000
With second weeks batch of samples
Continue until the tests are complete ...
\
IF there are 10 batches of samples where will be 156 dust analyses on these dust samples, with 9 grams of dust required for each size and lead level class
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0,678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
-------
APPENDIX C
PROTOCOL FOR GRINDING DUST INTO CARPET
MFS-OPPT\H33-eO.APC
-------
Protocol: Grinding Dust Into Carpet
Revision No. 1
September 24, 1993
Page 1 of 3
PROTOCOL FOR GRINDING DUST INTO CARPET
1.0 INTRODUCTION
Some tests on this study require grind-in of test dust into the carpet substrate.
Further, the area of the substrate on which the test dust is to be applied and ground-
in will depend on whether the test is to be done using a research vac (1 ft2) or a
Housevac (6.78 ft2). In either case, the grind-in will be done using the same grind-in
tool as listed below, which was built in accordance with that in ASTM F 608-89.
2.0 EQUIPMENT AND SUPPLIES
Grind-in tool
Small paintbrush
Templates (1 and 6.78 ft2)
Wide masking tape
Stopwatch
Carpet
3.0 PROCEDURE
This procedure is to be used in part of the dust preconditioning of
carpet/upholstery substrates and as part of housevac and sampler tests. Refer to
those appendices (App D, I, P, Q, and R) for test sequences and data forms.
3.1 Preparation for Grind-in
• Weigh out the amount of test dust to be used, depending on the test to be
conducted:
Test of research vac: 100 mg or 400 mg (±10 mg)
Test of Housevac: 678 mg or 2,712 mg (±10 mg)
• Be sure the test dust used corresponds with that specified for the tests [correct
particle size range and correct Pb content (high or low Pb)]. Transfer the weighed
MRI-OPPT\R5S-BO.APC
C-1
-------
Protocol: Grinding Dust Into Carpet
Revision No. 1
September 24, 1993
Page 2 of 3
amount of dust into a shaker or other suitable device for distributing dust onto the
carpet. Weigh the device and dust together, and record as total weight.
• Place the template on the carpet. Use masking tape to mark the test area.
Distribute the dust as evenly as possible over the test area, inside the template.
Remove the template, being careful to tap and brush the template so that any dust
adhering to the template falls back onto the test area.
• Distribute dust onto substrate.
• Reweigh device with any remaining dust. Calculate net weight of dust deposited.
3.2 Grind-in
• Embed the test dust into the carpet using the grind-in tool. Perform the grind-in by
using a dragging motion in both directions, alternating directions forward and back.
Do not drag the tool in one direction and push it back the other direction (even
though this would be more convenient). Hold the handle near a 45-degree angle
when dragging the tool across the test section.
• Drag the tool over the test area, exactly 30 strokes, using a uniform movement and
stroke time of 2.5 sec per stroke (i.e., 30 strokes over a total time of 75 sec.) (A
movement in one direction is one "stroke.") Be sure the tool covers the entire test
area on every stroke (i.e., ends of the tool extend over both sides of the test area
at all times).
• After completing the grind-in, use the small paintbrush to brush any material
adhering to the tool back onto the test area. Remove the grind-in tool from the test
locale, and clean it off with compressed air, if necessary, prior to the next use.
• Clean the template with compressed air.
P-2
MRI-OPPT\R55-90.APC ^ *-
-------
Protocol: Grinding Dust Into Carpet
Revision No. 1
September 24, 1993
Page 3 of 3
4.0 DEVIATIONS FROM PROTOCOL
Every attempt shall be made to follow this protocol. Deviations from the
protocol may compromise the data quality and completeness objectives of the project.
Deviations from the protocols will generally fall into two categories: inadvertent
deviations (procedural errors) and deliberate deviations (modifications to the protocol
in response to unusual (or unanticipated conditions).
In the case of inadvertent deviations from the protocol, the sampling team shall
fully document the deviation on the sampling data form and immediately notify the
team leader and the MRI Work Assignment Leader. Corrective action(s) shall be taken
to ensure that the situation is not repeated. If possible, samples affected by the
inadvertent deviation shall be recollected in accordance with the specified protocol.
Deliberate deviations from the sampling protocol should be approved in advance
with a signed modification to the QAPjP. If time is critical, preliminary verbal approval
may be granted by EPA. These verbal approvals will be followed up with a signed
modification to the QAPjP. In either case, the sampling team should notify all parties
concerned in a timely manner so that the approval mechanism can be expedited. The
MRI Work Assignment Leader is responsible for initiation of the QAPjP modification
and acquiring the necessary approvals.
MW-OPPT\R55-80J«»C
C-3
-------
APPENDIX D
PROTOCOL FOR CONDITIONING CARPET
AND OTHER SUBSTRATES
MRK)PPT\BSMO.APO
-------
Protocol: Conditioning Carpet and Other Substrates
Revision No. 1
September 24, 1993
Page 1 of 13
PROTOCOL FOR CONDITIONING CARPET
AND OTHER SUBSTRATES
1.0 INTRODUCTION
Tests on this study involve several different substrates (e.g., carpet, upholstery,
wood). Some preconditioning of each of these substrates is necessary prior to their
use in the tests, especially carpets. For example, carpet must be vacuumed several
times before use in any tests, because a substantial amount of carpet fibers are
collected when a new carpet is first vacuumed, which would interfere with
determination of recovery of dust applied to the carpet.
After preconditioning, one section of each substrate will be used in all tests, so
long as those tests involve the same dust loading (i.e., 100 or 400 mg/ft2) and the
same concentration of Pb in the dust (i.e., low Pb or high Pb). Therefore, four
separate sections of each substrate will be required, identified for use in the following
tests:
Low loading/low lead
Low loading/high lead
High loading/low lead
High loading/high lead
Preconditioning procedures for each substrate are described below.
2.0 EQUIPMENT AND SUPPLIES
Four sections of each substrate (72 x 27 in.)
Grind-in tool
Template (18 x 54 in.)
Duct tape
Dust to be applied
Housevacs with attachments for each substrate
Stopwatch
MRM3PPT\R5B40APD
-------
Protocol: Conditioning Carpet and Other Substrates
Revision No. 1
September 24, 1993
Page 2 of 13
3.0 PROCEDURES
Procedures are described below for each of the substrates to be tested:
Carpet
Carpet with grind-in
Upholstery
Wood
Tile
Linoleum
3.1 FIBER PRECONDITIONING OF CARPET AND UPHOLSTERY SUBSTRATES
Fiber preconditioning of carpet and upholstery substrates will be carried out in
accordance with the test sequence and data form attached at the end of this
appendix. For each section of substrate, this involves vacuuming for 5 min. with each
of the four Housevacs in sequence (starting with a specific Housevac for each section
of substrate as specified in the test sequence). Vacuuming with each Housevac in
sequence, continue as many times as is necessary to achieve the criteria given below.
The procedure for this fiber preconditioning of each section of substrate is as follows:
a. Record data using data entry forms attached at the end of this appendix.
b. Use a new bag for each Housevac each morning.
c. Tare weigh bag prior to first use:
Run free for 5 min, cool 2 min, brush* and record weight after 1 more
min
*(refers to brush of bag with anti-static brush)
d. Vacuum substrate section for 5 min, starting with the Housevac identified in
test sequence.
e. Reweigh bag after vacuuming for 5 min: (Cool 2 min, brush and record weight
after 1 more min)
f. Proceed with 5 min vacuuming with each Housevac per test sequence.
M»-OPPT\f»MO.APO
D-2
-------
Protocol: Conditioning Carpet and Other Substrates
Revision No. 1
September 24, 1993
Page 3 of 13
g. Continue 5 min vacuumings until substrate has been vacuumed a total of 20
times, or until weight gain reaches 20 mg or less for 4 consecutive
vacuumings.
3.2 DUST PRECONDITIONING OF ALL SUBSTRATES
Dust preconditioning of all substrates will be carried out in accordance with the test
sequence and data form attached at the end of this appendix. For each section of
substrate, this involves several applications of dust of different sizes, and vacuuming
for 40 sec using a different Housevac each time. The procedure for the dust
preconditioning of each substrate is as follows:
a. Mark test area on carpet using template and duct tape.
b. Use a new bag in each Housevac at beginning of each day.
c. Perform the tests according to the test sequence. Be sure the substrate is
properly identified for the specific dust loading (100 or 400 mg/ft2) and specific
Pb concentration (low or high), for which it will be used in all subsequent
testing of Housevacs and samplers.
d. Deposit required amount of dust having the particle size specified in test
sequence. Determine actual weight of dust deposited.
e. Grind in dust, if applicable (per Appendix C).
f. Determine tare weight of each bag before each use:
Run free for 40 sec, cool 2 min, brush and record weight after 1 more
min
g. Vacuum for 40 sec with the Housevac specified in the test sequence.
h. Record time of the vacuuming.
i. Reweigh bag (cool 2 min, brush, and record weight ater 1 more min).
j. Repeat tare-vac-reweigh (steps d-i above) using the next Housevac and particle
size designated in the test sequence. Continue until all tests shown in the test
sequence are completed for that substrate section.
k. Vacuum wand and brush on all Housevacs after completing all substrate tests
(no weighing).
MHK>PPT\RSMO.APO D'3
-------
Protocol: Conditioning Carpet and Other Substrates
Revision No. 1
September 24, 1993
Page 4 of 13
4.0 DEVIATIONS FROM PROTOCOL
Every attempt shall be made to follow this protocol. Deviations from the protocol may
compromise the data quality and completeness objectives of the project. Deviations
from the protocols will generally fall into two categories: inadvertent deviations
(procedural errors) and deliberate deviations (modifications to the protocol in response
to unusual or unanticipated conditions.
In the case of inadvertent deviations from the protocol, the sampling team shall fully
document the deviation on the sampling data form and immediately notify the team
leader and the MRI Work Assignment Leader. Corrective action(s) shall be taken to
ensure that the situation is not repeated. If possible, samples affected by the
inadvertent deviation shall be recollected in accordance with the specified protocol.
Deliberate deviations from the sampling protocol should be approved in advance with
a signed modification to the QAPjP. If time is critical, preliminary verbal approval may
be granted by EPA. These verbal approvals will be followed up with a signed
modification to the QAPjP- In either case, the sampling team should notify all parties
concerned in a timely manner so that the approval mechanism can be expedited. The
MRI Work Assignment Leader is responsible for initiation of the QAPjP modification
and acquiring the necessary approvals.
D-4
-------
Test Sequence for Fiber Preconditioning of Carpets and Upholstery
Table shows vacuumings within tests
Cycle through the vacuums until two successive vacuums collect less than 20 mg. of dust per 5 minutes of vacuuming
The order of the substrates and the choice of teams is not important
Put a new bag in each vacuum each morning
Test
number
Substrate sample
Lead
Substrate Dust Loading Cone
Particle size
New
bafi
Dust
deposited
(mg)
Vacuum
Team
time
vacuumed
weight
increase
(mg)
dust sent for
analysis (me)
lead
amount
W
Date
Vacuumed
Time
vacuumed
D
CJ1
1.01
1.02
1.03
1.04
1.05
2.01
2.02
2.03
2.04
2.05
3.01
3.02
3.03
3.04
3.05
4.01
4.02
4.03
4.04
4.05
5.01
5.02
5.03
5.04
5.05
6.01
6.02
6.03
6.04
6.05
Carpet
400 mg/sq ft High
Carpet 400 mg/sq ft Low
Carpet 100 mg/sq ft Low
Carpet 100 mg/sq ft High
Carpet with Grind-in 100 mg/sq ft Low
Carpet with Grind-in 100 mg/sq ft High
';' --,.:•',:•', no? ^;,-,.
•' "- ;,' , ,"'< • - no7 T-Vi
i . ;.'" no? "-"v'
<', f - ~ v' s,' ^ ^
C- ,-- : -• s -no? ;:-' ,
! -' •> 'f
i. -,1 '.*i , -no? sf"' -;
'.,' ,'l"' -r s't no? ,.,\..
',- ,V,'"•'','? "> no? ,",. •
_
( no? •;„
no? ,i
no? :
no?
,- no? *-
'v; no? >^
'. no? ",,
-"" no? <'
no? \
no? :'
- no? ',,
. no? ,
' no? ^
'; no? -•
>. no? "
no?
no; tfv,,,,,
no? |JiK*)/T* ,'"'•V" •''"!
no? |;'K'V' i
no? * •'•<•!'„- •>'•> '••«'
no? '"'= ''• -
, ?:•*-, ' --
no? '" /-.-! ,,/ .,
A
B
C
vD
B
C
D
A
C
D
A
B
D
A
B
C
B
C
D
A
C
D
A
B
Smin
Smin
Smin
Smin
Smin
Smin
Smin
Smin
Smin
Smin
Smin
Smin
5 min
Smin
Smin
Smin
Smin
Smin
Smin
Smin
5 min
Smin
Smin
Smin
TJ
O
8
O
o
o
o
u
Q.
(O
O
Q>
•3
CD
0)
D
Q.
CO
v>
CD
•o
CD O
3i-f
3) 3-
I CT (D CD
C/)
•£§!
o -»z^
~*> CO O 0>
-» co • ro
CO CA) -» W
-------
Fiber preconditioning (continued)
Table shows vacuumings within tests
Test Sequence for Fiber Preconditioning of Carpets and Upholstery (continued)
Test
number
Substrate sample
Substrate
Dust Loading
Lead
Cone
Particle size
New
bag
7.01
7.02
7.03
7.04
7.05
8.01
8.02
8.03
8.04
8.05
9.01
9.02
9.03,
9.04
9.05
10.01
10.02
10.03
10.04
10.05
11.01
11.02
11.03
11.04
11.05
12.01
12.02
12.03
12.04
12.05
Carpet with Grind-in 400 mg/sq ft Low
Carpet with Grind-in 400 mg/sq ft High
Dust
deposited
Vacuum
Upholstery
100 mg/sq ft Low
Upholstery 100 mg/sq ft High
Upholstery 400 mg/sq ft High
Upholstery 400 mg/sq ft Low
D
A
B
C
A
B
C
D
C
D
A
B
D
A
B
C
A
B
C
D
B
C
D
A
Team
time
vacuumed
weight
increase
5 min
5 min
5 min
5 min
5 min
5 min
5 min
V)
CO
T3
r-t
CD
(Q
O
o
o
o
o
(Q
O
Q>
CD
Q)
Q.
O
r+
CO (D
(/)
iKs&
0>- D «
o -> zg
-» CO ' CD
CiJ CO -» C/>
-------
Protocol: Conditioning Carpet and Other Substrates
Revision No. 1
September 24, 1993
Page 7 of 13
Data Entry Sheet
for
Fiber Preconditioning:
First Vacuum—A
Test Identification Test number
Date
Substrate (upholstery/ carpet) Operator
Substrate to be used for: Time
Grind-in (Yes or No)
Dust Amount (100, 400 mg/sq ft)
Pb Cone (Low, High)
Procedure
Use a new bag for each vac each morning
Tare weigh each new bag prior to first use:
Run free for 5 min, cool 2 min, brush, place in plastic bag and record weight after 1 more min
Vac carpet for 5 min, starting with vac identified in above heading
Reweigh after vac carpet for 5 min (cool 2 min, brush, place back in plastic bag and record weight after 1 more min)
Proceed with 5 min vacuumings with each vac. For tare weight use previous final weight from other sheet
Continue 5 min vacuumings until weight change is <20 mg for 4 vacs consecutively, or <40 mg for 8 vacs
consecutively
A B c D
(Balance No. ) (Balance No. ) (Balance No. ) (Balance No. )
TareWt Weight Rnal Tare Wt Weight Final Tare Wt Weight Final Tare Wt Weight
Chg om Wt. am gm Cha gm Wt. am gm Chg am Wt. am am Chg am
01
.02
.03
.04
.05
.06
.07
.08
.09
.10
.11
.12
.13
.14
.15
.16
.17
.18
.19
.20
Reviewed by
Date reviewed
MRtOPPT\R3MO.APD
D-7
-------
Protocol: Conditioning Carpet and Other Substrates
Revision No. 1
September 24, 1993
Page 8 of 13
Data Entry Sheet
for
Fiber Preconditioning:
Firet Vacuum—B
Test Identification Test number
Date
Substrate (upholstery, carpet) Operator
Substrate to be used for: Time
Grind-in (Yes or No)
Dust Amount (100, 400 mg/sq ft)
Pb Cone (Low, High)
Procedure
Use a new bag for each vac each morning
Tare weigh each new bag prior to first use:
Run free for 5 min, cool 2 min, brush, place in plastic bag and record weight after 1 more min
Vac carpet for 5 min, starting with vac identified in above heading
Reweigh after vac carpet for 5 min (cool 2 min, brush, place back in plastic bag and record weight after 1 more min)
Proceed with 5 min vacuumings with each vac. For tare weight use previous final weight from other sheet
Continue 5 min vacuumings until weight change is <20 mg for 4 vacs consecutively, or <40 mg for 8 vacs
consecutively
B
(Balance No. ) (Balance No. ) (Balance No. ) (Balance No.
Weight Final Tare Wt Weight Final Tare Wt
Cho am Wt. gm am Chg am
01
.02
.03
.04
.05
.06
.07
.08
.09
.10
.11
.12
.13
.14
.15
.16
.17
.18
.19
.20
Reviewed by
Date reviewed
MflMDPPT\FBMO.APD
D-8
-------
Protocol: Conditioning Carpet and Other Substrates
Revision No. 1
September 24, 1993
Page 9 of 13
Data Entry Sheet
for
Fiber Preconditioning:
Firct Vacuum—C
Test Identification Test number
Date
Substrate (upholstery, carpet) Operator
Substrate to be used for: Time
Grind-in (Yes or No)
Dust Amount (100, 400 mg/sq ft)
Pb Cone (Low, High)
Procedure
Use a new bag for each vac each morning
Tare weigh each new bag prior to first use:
Run free for 5 min, cool 2 min, brush, place in plastic bag and record weight after 1 more min
Vac carpet for 5 min, starting with vac identified in above heading
Reweigh after vac carpet for 5 min (cool 2 min, brush, place back in plastic bag and record weight after 1 more min)
Proceed with 5 min vacuumings with each vac. For tare weight use previous final weight from other sheet
Continue 5 min vacuumings until weight change is <20 mg for 4 vacs consecutively, or <40 mg for 8 vacs
consecutively
B
(Balance No. ) (Balance No. ) (Balance No. ) (Balance No. )
Tare Wt Weight Rnal Tare Wt Weight Rnal Tare Wt Weight
Cho am Wt. am am Cha am Wt. am am Cha am
01
.02
.03
.04
.05
.06
.07
.08
.09
.10
.11
.12
.13
.14
.15
.16
.17
.18
.19
.20
Reviewed by
Date reviewed
MRI-OPPT\RS3-90.APD
D-9
-------
Protocol: Conditioning Carpet and Other Substrates
Revision No. 1
September 24, 1993
Page 10 of 13
Data Entry Sheet
for
Fiber Preconditioning:
First Vacuum—D
Test Identification Test number
Date
Substrate (upholstery, carpet) Operator
Substrate to be used for: Time
Grind-in (Yes or No)
Dust Amount (100, 400 mg/sq ft)
Pb Cone (Low, High)
Procedure
Use a new bag for each vac each morning
Tare weigh each new bag prior to first use:
Run free for 5 min, cool 2 min, brush, place in plastic bag and record weight after 1 more min
Vac carpet for 5 min, starting with vac identified in above heading
Reweigh after vac carpet for 5 min (cool 2 min, brush, place back in plastic bag and record weight after 1 more min)
Proceed with 5 min vacuumings with each vac. For tare weight use previous final weight from other sheet
Continue 5 min vacuumings until weight change is <20 mg for 4 vacs consecutively, or <40 mg for 8 vacs
consecutively
D A B C
(Balance No. ) (Balance No. ) (Balance No. ) (Balance No. )
Final Tare Wt Weight Final Tare Wt Weight Final Tare Wt Weight Final Tare Wt Weight
Wt. om gm Chg qm Wt. gm gm Cha gm Wt. gm gm Chg gm Wt. gm gm Cha gm
01
.02
.03
.04
.05
.06
.07
.08
.09
.10
.11
.12
.13
.14
.15
.16
.17
.18
.19
.20
Reviewed by
Date reviewed
MFU-OPFT\R35-90.APD
D-10
-------
Dust preconditioning. Team 1
Table shows sequence of tests by team
Test Sequence for Dust Preconditioning (Team 1)
Test
number
Substrate sample
Substrate
Dust Loading
Lead
Cone
Particle size
New
_bag_
Dust
deposited
Vacuum
Team
time
vacuumed
Date
Vacuumed
Time
vacuumed
Target
Dust
deposited
SSL
101 Carpet 400 mg/sq ft Low 150-212
102 Carpet 400mg/sqft Low 250-2000
103 Carpet 400mg/sqft Low 53-106
104 Carpet 400 mg/sq ft Low 106-150
105 Carpet - 400 mg/sq ft Low 212-250
106 Carpet 400 mg/sqft Low <53
107 Upholstery 400 mg/sq ft Low 106-150
108 Upholstery 400 mg/sq ft Low <53
109 Upholstery 400 mg/sq ft Low 250-2000
110 Upholstery 400 mg/sq ft Low 212-250
111 Upholstery 400 mg/sq ft Low 150-212
112 Upholstery 400 mg/sq ft Low 53-106
113 Upholstery 100 mg/sq ft High 106-150
114 *" Upholstery 100 mg/sq ft High <53
115 Upholstery 100 mg/sq ft High 150-212
116 Upholstery 100 mg/sq ft High 212-250
117 Upholstery 100 mg/sq ft High 53-106
118 Upholstery 100mg/sq ft High. 250-2000
119 Carpet' 100 mg/sq ft High 150-212
120 Carpet 100 mg/sq ft High 106-150
121 Carpet 100 mg/sq ft High 53-106
122 Carpet 100 mg/sq ft High 250-2000
123 Carpet 100 mg/sq ft High <53
124 Carpet 100 mg/sq ft High 212-250
125 Carpet with Grind-in 100 mg/sq ft Low- <53
126 Carpet with Grind-in 100 mg/sq ft Low 106-150
127 Carpet with Grind-in 100 mg/sq ft Low 250-2000
128. Carpet with Grind-in 100 mg/sq ft Low 212-250
129* Carpet with Grind-in 100 mg/sq ft Low 150-212
130 Carpet with Grind-in 100 mg/sq ft Low 53-106
131 aSheet vinyl 400 mg/sq ft Low 106-150
132 aSheet vinyl 100 mg/sq ft Low 106-150
133 aSheet vinyl 100 mg/sq ft High 106-150
134 aSheet vinyl 400 mg/sq ft High 106-150
135 aWood 100 mg/sq ft Low 106-150
136 aWood 100 mg/sq ft High 106-150
137 Carpet with Grind-in 400 mg/sq ft High 150-212
138 Carpet with Grind-in 400 mg/sq ft High 106-150
139 Carpet with Grind-in 400 mg/sq ft High 212-250
140 Carpet with Grind-in 400 mg/sq ft High 53-106
141 Carpet with Grind-in 400 mg/sq ft High <53
142 Carpet with Grind-in 400 mg/sq ft High 250-2000
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
D
B
B
C
A
C
A
B
D
C
A
D
D
D
A
B
C
C
C
D
A
A
B
D
D.
B
A
D
C
A
B
D
A
C
B
C
B
A
C
D
A
D
2.712
2.712
2.712
2.712
2.712
2.712
2.712
2.712
2.712
2.712
2.712
2.712
0.678 .
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
2.712
0.678
0.678
2.712
0.678
0.678
2.712
2.712
2.712
2.712
2.712
2.712
O
O
o
o
o
D
Q.
5'
D
CO
O
Q)
—t
T3
CD
i-f
CO §
•o °-
CD O
13 *"*
Q) O" CD CD
(Q CD < ~»
<" ~* 55' (/)
i8§&
-» , 3 w
O _> Z =?
•* CD o 9>
-» CD • CD
00 W -» M
-------
Dust preconditioning, Team 2
Table shows sequence of tests by team
Test Sequence (or Dust Preconditioning (Team 2)
O
fo
Test
number
Substrate sample
Lead
Substrate Dust Loading Cone
Particle size
New
bag
Dust
deposited
(mg)
Vacuum
Team
time
vacuumed
dust
collected
(mg)
dust sent for
analysis (mg)
lead
amount
H>
Date
Vacuumed
Time
vacuumed
Target
Dust
deposited
(g)
201
202
203
204
205
206
207
208
209
210
211
212
213
214
215
216
217
218
219
220
221
222
223
224
225
226
227
228
229
230
231
232
233
234
235
236
237
238
239
240
241
242
Tile
Tile
Tile
Tile
Wood
Wood
Carpet
Carpet
Carpet
Carpet
Carpet
Carpet
Carpet
Carpet
Carpet
Carpet
Carpet
100 mg/sq ft Low
400 mg/sq ft High
400 mg/sq ft Low
100 mg/sq ft High
400 mg/sq ft Low
400 mg/sq ft High
400 mg/sq ft High
106-150
106-150
106-150
106-150
106-150
106-150
212-250
400 mg/sq ft High 250-2000
400 mg/sq ft High 53-106
400 mg/sq ft High
400 mg/sq ft .High
400 mg/sq ft High
100 mg/sq ft Low
100 mg/sq ft Low
100 mg/sq ft Low
100 mg/sq ft Low
100 mg/sq ft Low
100 mg/sq ft Low
Carpet
Carpet with Grind-in 400 mg/sq ft Low
Carpet with Grind-in 400 mg/sq ft Low
Carpet with Grind-in 400 mg/sq ft Low
Carpet with Grind-in 400 mg/sq ft Low
Carpet with Grind-in 400 mg/sq ft Low
Carpet with Grind-in 400 mg/sq ft Low
Upholstery 100 mg/sq ft Low
Upholstery
Upholstery
Upholstery
Upholstery
Upholstery
Carpet with Grind-in 100 mg/sq ft High
Carpet with Grind-in 100 mg/sq ft High
Carpet with Grind-in 100 mg/sq ft High
Carpet with Grind-in 100 mg/sq ft High
Carpet with Grind-in 100 mg/sq ft High
Carpet with Grind-in 100 mg/sq ft High
Upholstery 400 mg/sq ft High
Upholstery
Upholstery
Upholstery
Upholstery
Upholstery
106-150
<53
150-212
212-250
106-150
53-106
250-2000
<53
150-212
106-150
<53
250-2000
150-212
53-106
212-250
250-2000
106-150
150-212
53-106
212-250
<53
<53
106-150
53-106
212-250
150-212
250-2000
212-250
106-150
400 mg/sq ft High 250-2000
400 mg/sq ft" High 53-106
400 mg/sq ft High 150-212
400 mg/sq ft High <53
100 mg/sq ft Low
100 mg/sq ft Low
100 mg/sq ft Low
100 mg/sq ft Low
100 mg/sq ft Low
400 mg/sq ft High
A
D
C
B
D
A
B
C
C
B
D
A
C
A
D
D
A
B
D
A
C
B
C
B
B
C
D
B
A
C
C
C
B
A
D
B
D
B
A
A
C
B
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
0.678
2.712
2.712
0.678
2.712
2.712
2.712
2.712
2.712
2.712
2.712
2.712
0.678
0.678
0.678
0.678
0.678
0.678
2.712
2.712
2.712
2.712
2.712
2.712
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
0.678
2.712
2.712
2.712
2.712
2.712
2.712
CD
TJ
O
c-t
O
O
O
O
O
Q.
rt.'
o'
D
D'
CO
O
Q>
•5
CD
i-+
to
D
Q.
Dust preconditioning will require 21 grams of dust for each particle size and lead level, except 42 grams of size 106-150 um
CD O
3 <~f
Q) O" CD CD
(Q CD < ""*
» ~" M CO
s?s|
2, "* z ^
rt H? ' «
CO W -» en
-------
Protocol: Conditioning Carpet and Other Substrates
Revision No. 1
September 24, 1993
Page 13 of 13
Dust Entry Sheets
For
Dust Preconditioning
Test Sequence Numbers
Data
Operator
Test Identification
Substrate
Grind-in
Dust Amount
Pb Cone
Dust Size
Team
(see below)
(TILE, LINOteum, WOOD, UPHOLstery, CaPReT)
(Yes, No)
(100,400 mg/sq ft)
(Low, High)
(number 1 or 2)
Procedure
Use a new bag in each vacuum at the beginning of the day
Perform the tests according to the test sequence for dust preconditioning
Deposit dust. Determine the actual weight of dust deposited
Grind-in if applicable
Determine tare weight of bag before each use:
Run free for 40 sec, cool 2 min, brush and record weight after 1 more min
Vacuum for 40 sec with the vacuum indicated in the test sequence for dust preconditioning
Record the time of the vacuuming
Reweigh bag after 40 sec vac (cool 2 min, brush and record weight after 1 more min)
Repeat tare-vac-reweigh using the housevac and particle size designated in test sequence, which utilizes the
same substrate with the same dust loading and lead cone.
Vacuum the wand and brush all housevacs after completing all tests on the substrate (no weighing)
Weight of Dust Applied (g)
(Balance No. )
Weight of Bag (g)
(Balance No. )
Test
Number
(Time)
House
Vac
Particle
Size
Total
Wt
Tare
Wt
Net
Wt
Final
Wt
Tare
Wt
Net
Wt
D-13
-------
APPENDIX E
PROTOCOL FOR WIPE SAMPLING OF DUST
MH«JPPT\RSWO.APE
-------
Protocol: Wipe Sampling of Dust
Revision No. 1
September 24, 1993
Page 1 of 4
PROTOCOL FOR WIPE SAMPLING OF DUST
1.0 INTRODUCTION
Wipe samples of dust will be collected from substrates (except carpet and
upholstery) using commercially available moistened disposable wipes (Wash-a-bye
Baby" brand). The surfaces will be wiped using a sampling method developed by
Dr. Farfel for his doctoral thesis at Johns Hopkins University, School of Hygiene and
Public Health (Farfel, 1987). This sampling method is also found in the National
Institute of Building Sciences "Guidelines for Testing, Abatement, Clean Up, and
Disposal of Lead-Based Paint in Housing."
2.0 SAMPLING EQUIPMENT AND SUPPLIES
The following materials will be used to collect wipe samples:
• Wash-a-bye Baby" wipes
• Washable template (Inside dimensions, 1 ft by 1 ft)
• Steel measuring tape
• Marking pen
• 1 -quart plastic bags
• Disposable vinyl gloves (powderless)
• Substrates (tile, linoleum, wood)
c.1
-------
Protocol: Wipe Sampling of Dust
Revision No. 1
September 24, 1993
Page 2 of 4
3.0 WIPE SAMPLING PROTOCOL
The following procedure will be used to wipe sample substrate surfaces:
• Don a pair of clean, powderless, vinyl gloves.
• Remove the seal on a package containing the wipes (if not already removed during
previous sampling efforts), open the lid, start the lid dispenser, replace the lid,
remove several wipes, and discard them in the black trash bag. Use the next wipe
from the container to collect the sample.
• Position a clean 1-ft2 template on the surface to be sampled.
• Place the wipe flat on the surface within the sample area as defined by the
template. Using an open flat hand with the fingers together wipe the marked
surface in an overlapping "S" pattern, first side to side and then front to back so
that the entire 1-ft2 area is covered.
• Fold the wipe in half with the sample side folded in and repeat the wiping procedure
within the marked surface area on one side of the folded wipe.
• Fold the wipe again with the sample side folded in.
• Insert the folded wipe into the inner ziplock plastic bag and seal. Attach barcode
label to the bag and a duplicate barcode label on the sampling form. Place the
plastic bag inside another plastic bag along with extra duplicate barcode labels.
• Remove the vinyl gloves and dispose of them in the black trash bag.
• Record test number, date, time, etc., on the sampling data form.
4.0 PREPARATION OF SAMPLING BLANK SAMPLE
The sampling blank will consist of a Wash-a-bye Baby" wipe that is handled
using the identical procedure used for the dust samples except that no sample is
collected. Provide a blank sample with each batch of samples, or once each week as
a minimum.
-------
Protocol: Wipe Sampling of Dust
Revision No. 1
September 24, 1993
Page 3 of 4
5.0 CONTAMINATION AVOIDANCE
The following work practices will be instituted to prevent cross-contamination
between samples collected:
• Clean vinyl gloves (powderless) will be donned prior to collecting each wipe sample
and will be disposed of after each sample is collected.
• The templates will be cleaned with a Wash-a-bye Baby" disposable wet wipe
between each use. After cleaning the template, remove the vinyl gloves and
dispose of them.
6.0 DEVIATIONS FROM THE WIPE SAMPLING PROTOCOL
Every attempt shall be made to follow this sampling protocol. Deviations from the
sampling protocols may compromise the data quality and completeness objectives of
the project. Deviations from the protocols will generally fall into two categories:
inadvertent deviations (procedural errors) and deliberate deviations (modifications to
the protocol in response to unusual conditions encountered in the laboratory).
In the case of inadvertent deviations from the protocol, the sampling team shall fully
document the deviation on the sampling data form and immediately notify the MRI
work assignment leader. Corrective action(s) shall be taken to ensure that the situa-
tion is not repeated. If possible, samples affected by the inadvertent deviation should
be recollected in accordance with the specified protocol prior to leaving the site.
Deliberate deviations from the sampling protocol must be approved in advance with
a signed modification to the QAPjP. If time is critical, preliminary verbal approval may
be granted by EPA and MRI. These verbal approvals will be followed by a signed
modification to the QAPjP- In either case, the sampling team should notify all parties
concerned in a timely manner so that the approval mechanism can by expedited. The
MRI work assignment leader is responsible for initiation of the QAPjP modification and
for acquiring the necessary approvals from EPA and MRI.
The work assignment leader shall be notified by the sampling team when conditions
found in the laboratory do not allow full compliance with the protocol or when the
protocol does not appear to apply to the situation. The condition/situation shall be
fully documented in a laboratory notebook.
M»-OPPT\HSMO.APE
E-3
-------
Project 9802
WA#55
Data Entry Sheets
for
Sampler Teats
Test Identification
Sampler
Substrate "
Grind-in
Dust Amount
Pb Cone
Dust Size
Team
Square number
Test Sequence Number
Date
Operator
(Blue Nozzle, CAPS, HVS3 or WIPE)
(TILE, UNOIeum, WOOD, UPHOIstery, CaRPeT)
(Yes, No)
(100, 400 mg/ft2)
(Low, High)
(>53, 53-106. 106-150, 150-212, 212-250, 250-2000)
(Number 1 or 2)
(1, 2, 3 or 4) 1 = first, 3=last for carpet and upholstery, else 4-last)
Procedure
Perform the tests according to the sampler test sequence in Appendix Q, and procedures in Appendix E, F, G or H.
Housevac A will be used to vacuum the first square before sampler tests, or to vacuum the last square after sampler
tests.
If first square:
Tare weigh bag (run free for 40 seconds, cool 2 minutes, brush and record weight after 1 more minute)
Vac square for 40 seconds with Housevac A
Reweigh bag (cool 2 minutes, brush and record weight after 1 more minute)
Deposit dust in specified square and weigh the amount deposited (Grind-in dust if applicable)
Sample dust according to the appropriate protocol, weigh the dust collected (except for wipes)
Prepare the dust sample for analysis
If last square:
Tare weigh bag (run free for 120 seconds, cool 2 minutes, brush and record weight after 1 more minute)
Vac square for 120 seconds with Housevac A
Reweigh bag (cool 2 minutes, brush and record weight after 1 more minute)
Vacuum dust from wand and brush (no weighing)
Weight of Dust
(Balance # )
Weight of Bag
(Balance # )
Initial weight of bag
(if first or last square)
Vacuum and reweigh
bag (if first square)
Dust deposited
Dust collected by
sampler (exclu wipes)
Total Wt.
am.
.0
.1
.2
Final Wt.
gm.
NetWt.
am.
Time
Weight
gm.
Increase
gm.
.3
Vacuum & reweigh bag 4.
(if last square)
Bar Code
for Sample
Bar Code
for Blank
NOTE: Submit one blank for each sampler, once each week
Sample relinquished by Reviewed by
Sample received by Date reviewed _
Date of transfer
E-4
-------
APPENDIX F
PROTOCOL FOR VACUUM SAMPLING OF DUST
WITH THE BRM CYCLONE SAMPLER VAC
-------
Protocol: Vacuum Sampling of Dust
With BRM Cyclone
Revision No. 1
Date: September 24, 1993
Page 1 of 14
PROTOCOL FOR VACUUM SAMPLING OF DUST
WITH THE BRM CYCLONE SAMPLER VAC
1.0 INTRODUCTION
Vacuum samples of dust will be collected from floors (carpeted and uncarpeted)
and upholstery material as specified by the QAPjP. The vacuum sampling device is
a BRM cyclone dust collector shown in Figure F-1.
Each 1 -ft2 section of the surface to be sampled will be vacuumed in overlapping
passes (Figure F-2). A 1-ft2 template will be used to define and measure the areas to
be vacuumed.
2.0 SAMPLING EQUIPMENT AND SUPPLIES
• Modified BRM cyclone dust collectors
• 12-in Remote switch
• Vinyl tubing (3A-in ID)
• Dust catch containers (for the modified BRM cyclone)
• Plastic bottles for collection of dust samples
• 1-ft2 templates (full square)
• Stainless steel dust collector
• Steel measuring tape
• Screwdriver (tapping cyclone dust samples, If necessary)
-------
Protocol: Vacuum Sampling of Dust
With BRM Cyclone
Revision No. 1
Date: September 24, 1993
Page 2 of 14
o
4-1
O
o
u
+rf
(0
•o
o
oc
£0
u.
I
O)
QZ
F-2
-------
Pick-Up Nozzle
Protocol: Vacuum Sampling of Dust
With BRM Cyclone
Revision No. 1
Date: September 24, 1993
Page 3 of 14
Template
T
1'ft
! '
-1ft
«M3 SEV mctiugh actom 2 092590
Figure F-2. Vacuuming sampling pattern.
F-3
-------
Protocol: Vacuum Sampling of Dust
With BRM Cyclone
Revision No. 1
Date: September 24, 1993
Page 4 of 14
• Tweezers (long 12-in).
• Timing device (stopwatch, timer, or watch with second hand).
• Barcode labels (12 identical labels per sample with a unique sample number).
• 1-qt and 1-gal ziplock plastic bags
• Sample data sheets
• Vinyl gloves (powderless)
• Wash-a-bye Baby" premoistened disposable wipes to clean equipment
• Large Kimwipes"
3.0 VACUUM SAMPLING PROTOCOL
The following protocol will be used to collect vacuum samples of dust.
3.1 Sampling Preparations
• Use a clean 1-ft2 template to define the surface area to be vacuumed.
• Record test number, date, time, etc., on the sampling data form.
3.2 Cyclone Vacuum Assembly
• The cyclone vacuum consists of four major parts (see Figure F-3).
• Head
• Case
4 Teflon ring
• Clamp
F-4
M»-OPPr\RSMQAJVF « "*
-------
Protocol: Vacuum Sampling of Dust
__ With BRM Cyclone
Revision No. 1
Date: September 24, 1993
Page 5 of 14
Head
Clamp
Teflon Sealing Ring
Case
93-11 BALbaldrw 2 042993
Figure F-3. BRM cyclone vacuum assembly.
F-5
-------
Protocol: Vacuum Sampling of Dust
Wrth BRM Cyclone
Revision No. 1
Date: September 24, 1993
Page 6 of 14
The head of the cyclone has an output nozzle located on the top that would be
connected to a vacuum source and an inlet located tangentially on the side that would
be connected to a pick-up tube.
The conical shaped bottom half of the cyclone vacuum is the case. Internal
threads are located at the narrow end of the case. The dust catch container will be
screwed tightly into these threads.
A Teflon sealing ring is located between the head and case of the cyclone. The
clamp holds the head and case together.
3.3 Cyclone Dust Collector Preparation
• Property support the cyclone dust collector for disassembly.
• Disengage the clamping device used to hold the head and case together.
• Remove the clamp and separate the head and case.
• Wipe the inside surfaces of the cyclone's head and case with a Wash-A-Bye Baby"
wipe. Long tweezers or other devices may be required to reach all areas to wipe.
Use more than one wipe if necessary.
• Rewipe the inside surfaces of the cyclone head and case with a dean, dry
Kimwipe".
• Place the used wipes in a waste container.
• Reassemble cyclone head and case. Be sure Teflon sealing ring is in its proper
position (Rgure F-3). Before engaging clamp, make sure head and case are lined
up correctly. If the clamp appears to be more difficult than normal to engage,
check for misalignment,
• Affix the hand vacuum to the cyclone sampler case as shown in Rgure F-1.
• Don a pair of powdertess vinyl gloves prior to handling the sampling dust catch
container.
F-6
-------
Protocol: Vacuum Sampling of Dust
Wrth BRM Cyclone
Revision No, 1
Date: September 24, 1993
Page 7 of 14
• Obtain a sampling dust container (plastic bottle with lid). Affix a barcode label to
the container and an identical barcode label on the associated sampling data form.
• Weigh the sample container (with label and lid) and record weighings on test form.
Weigh the container twice or as many times as necessary until two weighings agree
within ±2 mg.
• Place a clean grey PVC transition piece onto the tangential inlet of the cyclone
head. This piece has two different IDs, The proper end of the transition piece
should fit snugly onto the inlet tube,
• Position the cyclone in a vertical position.
• Securely screw the sampling container into the lower threaded end of the cyclone
case (see Rgure F-4).
• Insert the proper end of the pick-up tube into the grey transition piece mentioned
above.
• Attach the vinyl tubing (Figure F-5) to the sampler case's Vin inlet.
3.4 Vacuuming Procedures for the BRM Cyclone
• Plug the hand vacuum in a 110-V AC outlet.
NOTE: The vacuum unit comes with a 12-ft vacuum extension hose and a
remote switch. This allows the vacuum unit to be located away from the
samping area while on/off control is maintained at the sampling location.
F-7
-------
Protocol: Vacuum Sampling of Dust
With BRM Cyclone
Revision No. 1
Date: September 24, 1993
Page 8 of 14
93-11 BALDUCkw 3 042993
Figure F-4. Sample collection bottle with cyclone assembly.
F-8
-------
ID
n
o
(D
Figure F-5. Attachment of vinyl tubing.
n
c
5 ^W
3 aw
i. 30 3
-D £T * CD-o
0) SJ <. 3D =:
(O co ? 3
TIT ^ % ;?? ^^ ^Jr
-------
Protocol: Vacuum Sampling of Dust
With BRM Cyclone
Revision No. 1
Date: September 24, 1993
Page 10 of 14
• Turn on the pump and vacuum the area of interest evenly in overlapping passes (at
least 50% overlap), first left to right, then front to back over the entire designated
area (Figure F-2). Vacuum the area again using this same pattern. For a 1-ft2 area,
vacuuming should not exceed 2 min.
NOTE: The cyclone sampler case must be held vertically throughout the
vacuuming process through the removal of the sampling container.
NOTE: The template used to define a surface area to be vacuumed is the
potential source of cross-contamination between samples. The template must
be thoroughly cleaned with disposable wipes between each sample.
• When the vacuuming is complete, turn off the hand vacuum, keeping the sampler
case vertical.
3.5 Sample Recovery
• Raise the humidity in the sampler case (body) by slowly blowing three breaths into
the nozzle using the separator as shown in Figure F-6. (Each sampling team
member performing the sampling job should have his or her own personal
separator.) Tap the sampler case three times with a small rod such as a
screwdriver.
• Carefully unscrew the sampling container, while keeping the sampler case vertical,
and carefully remove the container.
• Screw the sample catch container cap onto the container.
• Reweigh the container and record data on test data form. Again, weigh the
container twice or as many times as necessary until weighings agree within
±2 mg.
• Place the sampling container in a ziplock plastic bag, along with extra duplicate
barcode labels for use by analyst.
• Remove the vinyl gloves and dispose of them in the black trash bag.
F-1O
-------
Data Entry Sheets
for
Sampler Tests
Project 9802
WA#55
Test Identification
Sampler
Substrate
Grind-in
Oust Amount
Pb Cone
Dust Size
Team
Square number
Test Sequence Number
Date '_
Operator
(Blue Nozzle, CAPS, HVS3 or WIPE)
(TILE, UNOIeum, WOOD, UPHOIstery, CaRPeT)
(Yes, No)
(100, 400 mg/ft2)
(Low, High)
(>53, 53-106, 106-150, 150-212, 212-250, 250-2000)
(Number 1 or 2)
(1, 2, 3 or 4) 1 = first, 3=last for carpet and upholstery, else 4=
last)
Procedure
Perform the tests according to the sampler test sequence in Appendix 0, and procedures in Appendix E, F, G or H.
Housevac A will be used to vacuum the first square before sampler tests, or to vacuum the last square after sampler
tests.
If first square:
Tare weigh bag (run free for 40 seconds, cool 2 minutes, brush and record weight after 1 more minute)
Vac square for 40 seconds with Housevac A
Reweigh bag (cool 2 minutes, brush and record weight after 1 more minute)
Deposit dust in specified square and weigh the amount deposited (Grind-in dust if applicable)
Sample dust according to the appropriate protocol, weigh the dust collected (except for wipes)
Prepare the dust sample for analysis
If last square:
Tare weigh bag (run free for 120 seconds, cool 2 minutes, brush and record weight after 1 more minute)
Vac square for 120 seconds with Housevac A
Reweigh bag (cool 2 minutes, brush and record weight after 1 more minute)
Vacuum dust from wand and brush (no weighing)
Weight of Dust
(Balance # )
Weight of Bag
(Balance #
J
Initial weight of bag
(if first or last square)
Vacuum and reweigh
bag (if first square)
Dust deposited
Dust collected by
sampler (exclu wipes)
Vacuum & reweigh bag 4.
(if last square)
Total Wt.
om.
.0
.1
.2
Final Wt.
gm.
NetWt.
gm.
Time
Weight
gm.
Increase
gm.
Bar Code
for Sample
Bar Code
for Blank
NOTE: Submit one blank for each sampler, once each week
Sample relinquished by
Sample received by
Date of transfer
Reviewed by _
Date reviewed
F-11
-------
10
• Separator
1 11 DAL bal drw 4 O43093
7
s
O)
CD
•a
ff
-oi
TJ
I
O
O.
• •
£
O
c
D)
Figure F-6. Illustration of method used to raise humidity in the sampler case.
O -»
§.23
= 5a
O) -» (D S
-------
Protocol: Vacuum Sampling of Dust
With BRM Cyclone
Revision No. 1
Date: September 24, 1993
Page 13 of 14
4.0 CONTAMINATION AVOIDANCE
The following work practices will be instituted to prevent cross-contamination
between samples.
• Clean vinyl gloves (powderless) will be donned prior to collecting each vacuum
sample and will be disposed of after each sample is collected.
• The vacuum nozzle will be cleaned with soapy water or Wash-a-bye Baby" brand
disposable wet wipes between each sampling. Vinyl gloves will be used when
cleaning nozzles and changed to a clean pair prior to collecting samples. There
should be an adequate supply of clean nozzles to accommodate all the vacuum
samples collected in one day.
• The templates will be cleaned with a Wash-a-bye Baby" brand disposable wet wipe
between each sample.
5.0 DEVIATIONS FROM SAMPLING PROTOCOLS
Every attempt shall be made to follow this sampling protocol. Deviations from
the sampling protocols may compromise the data quality and completeness objectives
of the project. Deviations from the protocols will generally fall into two categories:
inadvertent deviations (procedural errors) and deliberate deviations (modifications to
the protocol in response to unusual conditions encountered in the laboratory).
In the case of inadvertent deviations from the protocol, the sampling team shall
fully document the deviation on the sampling data form and immediately notify the
MRI work assignment leader. Corrective action(s) shall be taken to ensure that the
situation is not repeated. If possible, samples affected by the inadvertent deviation
should be recollected in accordance with the specified protocol prior to leaving the
site.
Deliberate deviations from the sampling protocol must be approved in advance
with a signed modification to the QAPjP. If time is critical, preliminary verbal approval
may be granted by EPA and MRI. These verbal approvals will be followed up with a
signed modification to the QAPjP. In either case, the sampling team should notify all
parties concerned in a timely manner so that the approval mechanism can be
MBWPPTVWMO/LAPF
-------
Protocol: Vacuum Sampling of Dust
With BRM Cyclone
Revision No. 1
Date: September 24, 1993
Page 14 of 14
expedited. The MRI work assignment leader is responsible for initiation of the QAPjP
modification and acquiring the necessary approvals from EPA and MRI.
The work assignment leader shall be notified by the sampling team when
conditions found in the laboratory do not allow full compliance with the protocol or
when the protocol does not appear to apply to the situation. The condition/situation
shall be fully documented in a laboratory notebook. The sampling team leader will in
turn notify the MRI work assignment leader.
F.I 4
' ' ^
-------
APPENDIX G
PROTOCOL FOR VACUUM SAMPLING OF DUST
WITH THE CAPS CYCLONE SAMPLER VAC
MH-OPfT\HSWO.APa
-------
Protocol: Vacuum Sampling of Dust
With CAPS Cyclone Sampler
Revision No. 1
September 24, 1993
Page 1 of 12
PROTOCOL FOR VACUUM SAMPLING OF DUST
WITH THE CAPS CYCLONE SAMPLER VAC
1.0 INTRODUCTION
Vacuum samples of dust will be collected from floors (carpeted or uncarpeted)
and upholstery, using different research sampling vacuums, one of which is the CAPS
cyclone described in this protocol and shown in Figure G-1.
Each 1-ft2 section to be sampled will be vacuumed in overlapping passes
(Figure G-2). A 1-ft2 template will be used to define the areas to be vacuumed.
2.0 SAMPLING EQUIPMENT AND SUPPLIES
• Cyclone dust collectors
• PVC tubing
• Plastic bottles for collection of dust samples
• PVC nozzles (1 in. in diameter)
• 1-ft2 templates (full square)
• Steel measuring tape
• Tweezers
-------
Dirt Devil® Accessory Hose
Model #192
Q
Dirt Devil® Hand Vacuum
Model #103
7
Cyclone Sampler Case
Cyclone Sampler System
no
Vacuum Nozzle
en
CD
TJ
o
o
0)
02
^; =
TJ 3
en =»
A r^ **»
b*5
Jli.fl
-------
Protocol: Vacuum Sampling of Dust
With CAPS Cyclone Sampler
Revision No. 1
September 24, 1993
Page 3 of 12
Pick-Up Nozzle
Template
c
i^rnnrjcqzn^rjr,
4
)
T
1ft
90-43 SEV mchughKhtma 002590
MW-OPPTVW5-90.APQ
Figure G-2. Vacuum sampling pattern.
G-3
-------
Protocol: Vacuum Sampling of Dust
With CAPS Cyclone Sampler
Revision No. 1
September 24, 1993
Page 4 of 12
• Timing device (stopwatch, timer, or watch with second hand)
• Barcode labels
• 1-qt and 1-gal ziplock plastic bags
• Sample logs (test forms)
• Vinyl gloves (powderless)
• Wash-a-bye Baby premoistened, disposable wipes to clean equipment
• Spatula
3.0 VACUUM SAMPLING PROTOCOL
The following protocol will be used to collect vacuum samples of dust:
3.1 Sampling Preparations
• A clean, 1-ft2 template will be used to define and measure the surface area to be
vacuumed. Measurements will be made after the sample has been collected.
• Record test number, date, time, etc., on the sampling data form.
• Prepare the cyclone dust collector (Figure G-3 as follows):
• Remove the plug (at bottom of cyclone sampler case) by unscrewing it. Set the
holder plug aside.
• Remove the three O-rings that hold the dust collector case's top and body together.
Set these aside with the holder plug.
• Separate the dust collector's top from its case.
M«-OPPT\R55-90.APG
-------
Protocol: Vacuum Sampling of Dust
With CAPS Cyclone Sampler
Revision No. 1
September 24, 1993
Page 5 of 12
•o
0
25
CD
CO
CO
CO
_co
T3
•o
c
CO
•o
o
A
o
CO
CO
a
o
o
o
a
•o
o
o
o
CO
a.
<
o
o
S
O)
G-5
-------
Protocol: Vacuum Sampling of Dust
With CAPS Cyclone Sampler
Revision No. 1
September 24, 1993
Page 6 of 12
• Wipe the inside surfaces of the dust collector's top and case with Wash-a-bye Baby
wipes. Use more than one, if necessary.
• Place the used wipes in a waste container.
• Reassemble cyclone top and sampler case by placing the top onto the sampler case
and affixing the three O-rings. Be sure the O-ring holders on the top are aligned
with those on the sampler case.
• Affix the hand vacuum to the cyclone sampler case as shown in Figure G-3.
• Don a pair of powderless vinyl gloves prior to handling sample bottles.
• Obtain a sampling dust container (plastic bottle with lid). Affix a barcode label to
the container and an identical label on the associated sampling data form.
• Weigh the sample container (with label and lid) and record weighings on test form.
Weigh the container twice or as many times as necessary until two weighings agree
within ±2 mg.
• Screw sample container into the bottom of the cyclone. (Store lid in plastic bag.)
• Retrieve a clean 90-degree elbow and a clean 1-in i.d. nozzle from their containers.
Attach the elbow (Figure G-4) to the sampler case's 1-in inlet.
• Place the 1-in i.d. nozzle into the open end of the 90-degree elbow (Figure G-4).
• Position the nozzle and the sample case vertically as shown in Figure G-4.
3.2 Conduct Sampling
• Plug the hand vacuum in a 110-V AC outlet.
• Turn on the pump and vacuum the 1-ft2 area evenly in overlapping passes (at least
50% overlap), first left to right, then front to back over the entire designated area
(Figure G-2). Vacuum the area again using this same pattern. For the 1-ft2 area,
vacuuming should not exceed 2 min.
M«-OPPT\R55-90J\PQ U~O
-------
9
93 ?•, SEV goc scm .1061893
Figure G-4. Affixing nozzle to cyclone dust collector.
CO
(D
•o
i-t
(D
3 J>
"D 5" ®
M 5 <
(O (A
o> M5-
XI ,*§
Q -» Z
O
o
o
>c
02.
81
CO o
I a
3 n
~^ «J O -Q _
wS-« 5
N> CO -* -, r->
-------
Protocol: Vacuum Sampling of Dust
With CAPS Cyclone Sampler
Revision No. 1
September 24, 1993
Page 8 of 12
NOTE: The cyclone sampler case must be held vertically throughout the vacuuming
process through the removal of the sample container.
NOTE: The template that is used to define a surface area to be vacuumed is the
potential source of cross-contamination between samples. The template must be
thoroughly cleaned with disposable wipes between each sample.
• When the vacuuming is complete, turn off the hand vacuum, keeping the sampler
case vertical.
3.3 Sample Recovery
• Raise the humidity in the sampler case (body) by slowly blowing three breaths into
the nozzle using the separator as shown in Figure G-5. (Each sampling team
member performing the sampling job should have his own personal separator.) Tap
the sampler case three times with a small rod (a screwdriver is an example).
• Carefully unscrew the sample bottle while keeping the sampler case vertical.
Replace the lid.
• Reweigh the sample bottle and record on test data form. Again, weigh the bottle
twice or as many times as necessary until weighings agree within ±2 mg.
• Place the sample bottle in a ziplock plastic bag with extra duplicate barcode labels.
• Remove the vinyl gloves and dispose in the black trash bag.
4.0 CONTAMINATION AVOIDANCE
The following work practices will be instituted to prevent cross contamination
between samples.
• Clean vinyl gloves (powderless) will be donned prior to collecting each vacuum
sample and will be disposed of after each sample is collected.
fc«WDPPT\RSS-90JU=G
-------
9
to
CO
(D
B
(D
TJ
!
o
o
3" Q)
og
-I
CO 3
D 0)
' o 3
»<5 SCV got Km 081W3
o is> «
o -»
Figure G-5. Separator and its use.
foS-? 21
-------
Protocol: Vacuum Sampling of Dust
With CAPS Cyclone Sampler
Revision No. 1
September 24, 1993
Page 10 of 12
Sample containers will not be handled without the use of vinyl gloves to prevent the
deposition of residues that may interfere with gravimetric analysis of the sample.
• The vacuum nozzle is cleaned with soapy water or "Wash-a-bye Baby" brand
disposable wet wipes between each sample. Vinyl gloves will be used when
cleaning nozzles and changed to a clean pair prior to collecting samples. There
should be an adequate supply of clean nozzles to accommodate all the vacuum
samples collected.
• The templates will be cleaned with a "Wash-a-bye Baby" brand disposable wet wipe
between each sample.
5.0 DEVIATIONS FROM SAMPLING PROTOCOLS
Every attempt shall be made to follow this sampling protocol. Deviations from
the sampling protocols may compromise the data quality and completeness objectives
of the project. Deviations from the protocols will generally fall into two categories;
inadvertent deviations (procedural errors), and deliberate deviations (modifications to
the protocol in response to unusual conditions encountered in the laboratory).
In the case of inadvertent deviations from the protocol, the sampling team shall
fully document the deviation on the sampling data form and immediately notify the
MRI work assignment leader. Corrective action(s) shall be taken to ensure that the
situation is not repeated. If possible, samples affected by the inadvertent deviation
should be recollected in accordance with the specified protocol prior to leaving the
site.
Deliberate deviations from the sampling protocol should be approved in advance
with a signed modification to the QAPjP. If time is critical, preliminary verbal approval
may be granted by EPA and MRI. These verbal approvals will be followed up with a
signed modification to the QAPjP. In either case, the sampling team should notify all
parties concerned in a timely manner so that the approval mechanism can by
expedited. The MRI work assignment leader is responsible for initiation of the QAPjP
modification and acquiring the necessary approvals from EPA and MRI.
MHI-OPPT\R55-90.APG
-------
Protocol: Vacuum Sampling of Dust
With CAPS Cyclone Sampler
Revision No. 1
September 24, 1993
Page 11 of 12
The work assignment leader shall be notified by the sampling team when
conditions found in the laboratory do not allow full compliance with the protocol or
when the protocol does not appear to apply to the situation. The condition/situation
shall be fully documented in a laboratory notebook. The team leader will in turn notify
the MRI work assignment leader.
M«-Of>PT\H58-BO.APG
G-11
-------
Data Entry Sheets
for
Sampler Tests
Project 9802
WA#55
Test Identification
Sampler
Substrate
Grind-in
Dust Amount
Pb Cone
Dust Size '
Team
Square number
Test Sequence Number
Date
Operator
(Blue Nozzle, CAPS, HVS3 or WIPE)
(TILE, UNOIeum, WOOD, UPHOIstery, CaRPeT)
(Yes, No)
(100, 400 mg/ft2)
(Low, High)
(>53, 53-106, 106-150. 150-212, 212-250, 250-2000)
(Number 1 or 2)
(1, 2, 3 or 4) 1 = first, 3 = last for carpet and upholstery, else 4=
last)
Procedure
Perform the tests according to the sampler test sequence in Appendix Q, and procedures in Appendix E, F, G or H.
Housevac A will be used to vacuum the first square before sampler tests, or to vacuum the last square after sampler
tests.
If first square:
Tare weigh bag (run free for 40 seconds, cool 2 minutes, brush and record weight after 1 more minute)
Vac square for 40 seconds with Housevac A
Reweigh bag (cool 2 minutes, brush and record weight after 1 more minute)
Deposit dust in specified square and weigh the amount deposited (Grind-in dust if applicable)
Sample dust according to the appropriate protocol, weigh the dust collected (except for wipes)
Prepare the dust sample for analysis
If last square:
Tare weigh bag (run free for 120 seconds, cool 2 minutes, brush and record weight after 1 more minute)
Vac square for 120 seconds with Housevac A
Reweigh bag (cool 2 minutes, brush and record weight after 1 more minute)
Vacuum dust from wand and brush (no weighing)
Weight of Dust
(Balance # )
Weight of Bag
(Balance # )
Initial weight of bag
(if first or last square)
Vacuum and reweigh
bag (if first square)
Dust deposited
Dust collected by
sampler (exdu wipes)
Total Wt.
flm.
.0
.1
.2
Final Wt.
am.
NetWt.
am.
Time
Weight
am.
Increase
flm.
.3
Vacuum & reweigh bag 4.
(if last square)
Bar Code
for Sample
Bar Code
for Blank
NOTE: Submit one blank for each sampler, once each week
Sample relinquished by Reviewed by
Sample received by Date reviewed _
Date of transfer
G-12
-------
APPENDIX H
PROTOCOL FOR VACUUM SAMPLING OF DUST
WITH THE BLUE NOZZLE SAMPLER VAC
MHK>PPT\HBWO.APH
-------
Protocol: Vacuum Sampling of Dust
with Blue Nozzle Sampler
Revision No. 1
September 24, 1993
Page 1 of 9
PROTOCOL FOR VACUUM SAMPLING OF DUST
WITH THE BLUE NOZZLE SAMPLER VAC
1.0 INTRODUCTION
Vacuum samples of dust will be collected from floors (carpeted and uncarpeted)
and upholstery material using different sampling vacs, one of which is the Blue Nozzle
Sampler described in this protocol and shown in Figure H-1. This vacuum sampling
device consists of a Teflon pickup nozzle mounted on a preweighed 37-mm, mixed
cellulose ester filter cassette (0.8-//m pore size). This collection device is coupled to
a Gast rotary-vane vacuum pump with Tygon tubing (Figure H-1).
Each 1-ft2 section of the surface to be sampled will be vacuumed in overlapping
passes (Figure H-2). A 1-ft2 template will be used to define the area to be vacuumed.
2.0 SAMPLING EQUIPMENT AND SUPPLIES
• Gast rotary-vane vacuum pumps
• Tygon tubing
• Gelman GN-4, 37-mm, mixed cellulose ester (MCE) filter cassettes (0.8-//m pore
size)
• Teflon pickup nozzles
• 1 -ft2 templates
• Steel measuring tape
• Screwdriver
• Barcode labels
• 1-qt and 1-gal ziplock plastic bags
• Plastic trash bag
• Sample data sheets
• Vinyl gloves (powderless)
MRK3PPT\R»go.APH
H-1
-------
3D
6
TJ
Tygon Tubing
I
rb
Ptek-Up Nozzle
Plastic Lure /
Gast Vacuum Pump
Open-Face
37-mm Gelman MCEF
Rlter Cassette wilh Retaining Ring
O
O
Figure H-1. Schematic of rotary vacuum pump with blue nozzle.
(D
*
(D
^' o
3- C
M
(D CO
_ Q)
o 3
® < K=:
NJ Q* (D
,*§ S?0
S,g?f ?
co co -» 5 S
-------
Protocol: Vacuum Sampling of Dust
with Blue Nozzle Sampler
Revision No. 1
September 24, 1993
Page 3 of 9
Pick-Up Nozzle
Template
1ft
-1ft
9O-43 SEV mchugh tditm 2 092590
Figure H-2. Vacuum sampling pattern.
MRI-OPPT\RS5-flO.APH
H-3
-------
Protocol: Vacuum Sampling of Dust
with Blue Nozzle Sampler
Revision No. 1
September 24, 1993
Page 4 of 9
3.0 VACUUM SAMPLING PROTOCOL
The following protocol will be used to collect vacuum samples of dust using the
blue nozzle sampler.
3.1 Sampling Preparations
• A clean, 1-ft2 template will be used to define the surface area to be vacuumed.
NOTE: The template that is used to define a surface area to be vacuumed is a
potential source of cross contamination between samples. The template must be
thoroughly cleaned with disposable wipes between each sample.
• Record test number, date, time, etc., on the sampling data form.
• Don a pair of powderless vinyl gloves prior to handling filter cassettes. Do not
touch the cassettes with bare hands.
• Obtain one of the filter cassettes from the box in the laboratory so that the cassette
will have equilibrated with conditions in the test laboratory.
• Weigh the cassette and record weighings on data form. Weigh the cassettes twice
or as many times as necessary until two weighings agree within ±2 mg.
• Pry open the top section of the filter cassette with a clean flat-edged screwdriver
or equivalent tool. Carefully remove the top section. (See Figure H-3)
NOTE: The middle retaining ring holds the filter and support pad in place against
the bottom section of the cassette (Figure H-3). The retaining ring should be
inspected to ensure that it is seated tightly against the bottom section. If the
middle ring is not secure, the filter may tear during the sampling procedure. The
seal between the bottom section of the cassette and the middle ring can be secured
by squeezing the two sections firmly between the index fingers and the thumbs of
both hands.
M«-OPPT\HS5-90.APH
-------
Protocol: Vacuum Sampling of Dust
with Blue Nozzle Sampler
Revision No. 1
September 24, 1993
Page 5 of 9
ASSEMBLY
ORDER
First Clear Plastic Cap
Second Level of Plastic Cassette
•Filter
Filter Backup Support Pad
ASSEMBLED
CASSETTE
Sl-ie SEV bmltieml MIBft
First Clear Plastic Cap
Second Level of Plastic Cassette
Filter
Filter Backup Support Pad
Figure H-3. Unassembled and assembled dust sample cassette.
MRI-OPPTVISS.90.APH
H-5
-------
Protocol: Vacuum Sampling of Dust
with Blue Nozzle Sampler
Revision No. 1
September 24, 1993
Page 6 of 9
• Store the top section of the cassette inside a ziplock bag during sampling to avoid
contamination.
• Attach Tygon tubing between the inlet of the pump and the outlet of the filter
cassette.
• Insert the open side of the filter cassette into a pickup nozzle. The nozzle must fit
snugly around the rim of the retaining ring. If it does not fit snugly, replace the
nozzle or discard the filter cassette.
3.2 Conduct Vacuuming
• Turn on the pump and vacuum the 1-ft2 area in overlapping passes (at least 50
percent overlap), first left to right and then front to back over the entire designated
area (see Figure H-2). Vacuum the designated area again using this same pattern.
For the 1-ft2 area, vacuuming should not exceed 2 min.
• When the vacuuming is complete, hold the open end of the nozzle upright, and turn
off the pump.
3.3 Sample Recovery
• While maintaining the filter cassette in an upright position, carefully remove the
nozzle and disconnect the Tygon tubing.
• Replace the top section of the cassette.
• Reweigh the cassette and record weight on test data form. Again, weigh the
cassette twice or as many times as necessary until weighings agree within ±2 mg.
• Place the filter cassette in a ziplock plastic bag. Attach barcode label to plastic bag
and duplicate barcode label on the sampling data form.
• Place the plastic bag containing the cassette inside a second plastic bag along with
extra duplicate barcode labels for use by analyst.
M»-OPPT\H»-OO.APH M-D
-------
Protocol: Vacuum Sampling of Dust
with Blue Nozzle Sampler
Revision No. 1
September 24, 1993
Page 7 of 9
• Remove the vinyl gloves and dispose in the trash bag.
• Store samples in a clean container until ready for analysis.
4.0 PREPARATION OF SAMPLING BLANK SAMPLES
Sampling blank samples will consist of a filter cassette that is handled in the
same manner as the regular vacuum samples, except that no sample is collected.
Provide a blank sample with each batch of samples, or once a week at minimum.
5.0 CONTAMINATION AVOIDANCE
The following work practices will be utilized to prevent contamination of
samples.
• Clean vinyl gloves (powderless) will be donned prior to collecting each vacuum
sample and will be disposed of after each sample is collected.
• Filter cassettes must not be handled without the use of vinyl gloves to prevent the
disposition of residues that may interfere with gravimetric analysis of the sample.
If the filter cassette is inadvertently touched prior to collecting the sample, the filter
cassette will be discarded.
• The vacuum nozzle will be cleaned with soapy water or "Wash-a-bye Baby" brand
disposable wet wipes between each sample. There should be an adequate supply
of clean nozzles to accommodate all the vacuum samples collected.
• The templates will be cleaned with a "Wash-a-bye Baby" brand disposable wet wipe
between each sample.
MRK)PPT\R5MO.APH
H-7
-------
Protocol: Vacuum Sampling of Dust
with Blue Nozzle Sampler
Revision No. 1
September 24, 1993
Page 8 of 9
6.0 DEVIATIONS FROM SAMPLING PROTOCOLS
Every attempt shall be made to follow this sampling protocol. Deviations from
the sampling protocols may compromise the data quality and completeness objectives
of the project. Deviations from the protocols will generally fall into two categories:
inadvertent deviations (procedural errors), and deliberate deviations (modifications to
the protocol in response to unusual conditions encountered in the laboratory).
In the case of inadvertent deviations from the protocol, the sampling team shall
fully document the deviation on the sample log and immediately notify the MRI work
assignment leader. Corrective action(s) shall be taken to ensure that the situation is
not repeated. If possible, samples affected by the inadvertent deviation should be
recollected in accordance with the specified protocol.
Deliberate deviations from the sampling protocol should be approved in advance
with a signed modification to the QAPjP. If time is critical, preliminary verbal approval
may be granted by EPA and MRI. These verbal approvals will be followed up with a
signed modification to the QAPjP. In either case, the sampling team should notify all
parties concerned in a timely manner so that the approval mechanism can be
expedited. The MRI work assignment leader is responsible for initiation of the QAPjP
modification and acquiring the necessary approvals from EPA and MRI.
The work assignment leader shall be notified by the sampling team when
conditions found in the laboratory do not allow full compliance with the protocol or
when the protocol does not appear to apply to the situation. The condition/situation
shall be fully documented in a laboratory notebook.
|_| O
MRI-OPPT\R55-90.APH ITU
-------
Project 9802
WA#55
Data Entry Sheets
for
Sampler Tests
Test Identification
Sampler
Substrate
Grind-in
Dust Amount
Pb Cone
Dust Size '
Team
Square number
Test Sequence Number
Date
Operator
(Blue Nozzle, CAPS, HVS3 or WIPE)
(TILE, LINOIeum, WOOD, UPHOIstery, CaRPeT)
(Yes, No)
(100, 400 mg/ft2)
(Low, High)
(>53, 53-106, 106-150, 150-212, 212-250, 250-2000)
(Number 1 or 2)
(1, 2, 3 or 4) 1 = first, 3=last for carpet and upholstery, else 4 = last)
Procedure
Perform the tests according to the sampler test sequence in Appendix Q, and procedures in Appendix E, F, G or H.
Housevac A will be used to vacuum the first square before sampler tests, or to vacuum the last square after sampler
tests.
If first square:
Tare weigh bag (run free for 40 seconds, cool 2 minutes, brush and record weight after 1 more minute)
Vac square for 40 seconds with Housevac A
Reweigh bag (cool 2 minutes, brush and record weight after 1 more minute)
Deposit dust in specified square and weigh the amount deposited (Grind-in dust if applicable)
Sample dust according to the appropriate protocol, weigh the dust collected (except for wipes)
Prepare the dust sample for analysis
If last square:
Tare weigh bag (run free for 120 seconds, cool 2 minutes, brush and record weight after 1 more minute)
Vac square for 120 seconds with Housevac A
Reweigh bag (cool 2 minutes, brush and record weight after 1 more minute)
Vacuum dust from wand and brush (no weighing)
Weight of Dust
(Balance # )
Weight of Bag
(Balance # )
Initial weight of bag
(if first or last square)
Vacuum and reweigh
bag (if first square)
Dust deposited
Dust collected by
sampler (exclu wipes)
Total Wt.
am.
.0
.1
.2
.3
Final Wt.
qm.
NetWt.
gm.
Time
Weight
gm.
Increase
gm.
Vacuum & reweigh bag 4.
(if last square)
Bar Code
for Sample
NOTE: Submit one blanl
Sample relinquished by
Sample received by
Date of transfer
Bar Code
for Blank
t for each sampler, once each week
Reviewed by
Date reviewed
H-9
-------
APPENDIX I
PROTOCOL FOR VACUUMING AND SAMPLING
OF DUST WITH HOUSEVACS
-------
Protocol: Vacuuming and Sampling of
Dust with Housevacs
Revision No. 1
September 24, 1993
Page 1 of 7
PROTOCOL FOR VACUUMING AND SAMPLING
OF DUST WITH HOUSEVACS
1.0 INTRODUCTION
Many of the tests to be done for this study require sampling with Housevacs
(four different brands) as specified in Appendix P. This protocol describes the
procedure to be used in carrying out the vacuuming operations and sampling of
collected dust after the final vacuuming. It is applicable to all substrates: carpeted
and uncarpeted floors and upholstery material. For all substrates, the area to be
vacuumed will be 6.78 ft2 (18 x 54 in).
2.0 EQUIPMENT AND SUPPLIES
Tape measure or ruler
Template (18 x 54 in)
Wide masking tape
Stopwatch
Dust sample bottles
Barcode labels
Test data forms
Substrates
3.0 PROCEDURE
3.1 Preparations
• Use data entry forms (attached at the end of this appendix).
• Use preconditioned substrates per Appendix D.
• Place template on substrate and mark test area with masking tape.
1-1
-------
Protocol: Vacuuming and Sampling of
Dust with Housevacs
Revision No. 1
September 24, 1993
Page 2 of 7
• Select Housevac to be tested (per test design) and proper cleaning attachment
depending on substrate to be tested. (Note: for carpet, always use the power
nozzle attachment.)
• Measure the outside width of the nozzle housing, in inches.
• Calculate the number of vacuuming "strips" (N) to be used, as follows:
1 R in
N = Number of strips = (Round to nearest whole number.)
nozzle width
Example: If nozzle width is 7 in, the number of "strips" would be 3. Thus, each
strip would be 6 in wide.
• Use duct tape to mark the test strips at both ends of the test area (see Figure 1-1).
• Determine the stroke pattern to be used, per Figure 1-1. In all cases, the total
number of strokes used must be 16 (a movement in one direction is one stroke).
3.2 Vacuuming Procedure
• Cleaner nozzle is to be placed on the test carpet so that the front of the nozzle is
coincident with the line defining the beginning of the test area and with the right
side of the nozzle at the right side boundary shown in the applicable illustration in
Figure 1-1.
• Carry out vacuuming per the stroke pattern determined above. Each stroke pattern
utilizes a total of 16 strokes. Length of time for each stroke should be near
2.5 sec, for a total vacuuming time of 40 sec.
I-2
-------
Protocol: Vacuuming and Sampling of
Dust with Housevacs
Revision No. 1
September 24, 1993
Page 3 of 7
N = 2
10.12.14,161 2.4.6.8
I : I
I
I
11.13.15 | 1.3.5.7
12, 14.161 8.10 I 2.4
1 ' I '
till
I I
,6,
13. 15 | 7.9 | 1.3.5
• Stroke Numbers
14 F 10 I 6 I 2
I I I I
16
I I I
I 12 I 8 I
I I • I
I I I I I
13.15| 9.11 | 5.7 | 1.3
N = 6
16 I 14 | 10T 8 I 4 I 2
I
I I
15\12/ 9\ 6/ \3
M rvf r
I
'MI
M3 | 11 | 7 | 5
Figure 1-1. Test cleaning patterns.
I-3
-------
Protocol: Vacuuming and Sampling of
Dust with Housevacs
Revision No. 1
September 24, 1993
Page 4 of 7
Ensure that each forward stroke ends with the cleaner nozzle coincident with the
end of the test area. When the cleaner reaches the extreme left strip, align the left
side of the nozzle with the left side boundary of the test area. Take care to ensure
that during each stroke the side of the nozzle, right side or left side as applicable,
is kept aligned with the side boundary of the test strip being cleaned, except for
cross-over strokes.
At the end of the last stroke, smoothly tilt or lift the nozzle off the substrate and
allow Housevac to run 10 sec to clear the system.
During this 10-sec period, the hose used on some Housevacs should be flexed to
help clear it of any dust.
3.3 Conduct Test
The procedure to be used in conducting each Housevac test is as follows:
• Tare weigh new bag:
Run free for 40 sec, cool 2 min, brush and record weight after 1 more min.
• Vacuum for 40 sec, before any dust is deposited.
• Reweigh bag (cool 2 min, brush and record weight after 1 more min)
• Deposit dust, vacuum for 40 sec, reweigh bag). Total of 3 times.
• Vacuum and reweigh bag 3 times (no dust deposit)
• Recover dust sample from bag per Section 4.0.
• Vacuum dust from wand and brush (no weighing).
1-4
-------
Protocol: Vacuuming and Sampling of
Dust with Housevacs
Revision No. 1
September 24, 1993
Page 5 of 7
4.0 SAMPLE COLLECTION
After the specified number of vacuumings and weighings, a sample of the dust
collected in the Housevac bag will need to be taken for analysis, as follows:
• Obtain one of the wide mouth plastic sample bottles. Place a barcode label on the
bottle and an identical label on the test form.
• Weigh the empty bottle (with lid and label). Record weight on test form. Weigh
the bottle twice or as many times as necessary until two weighings agree within
±2 mg.
• Carefully cut away any sealing flaps on the bag inlet hole.
• Place the bag over the top of the weighed plastic bottle, with the bag opening
facing down into the bottle. If the bag opening is larger than the top of the bottle,
use a suitable clean funnel for this operation.
• Tap the outside of the bag; this should cause some dust inside to fall into the
sample bottle.
• Place the lid back on the sample bottle and reweigh. Record weight on test form.
Again, weigh the bottle twice or as many times as necessary until two weighings
agree within ±2 mg.
5.0 CONTAMINATION AVOIDANCE
Contamination refers to both the inadvertent increase (or decrease) in the
weight of dust collected by the Housevac (other than that applied to the substrate)
and potential Pb contamination of that dust or dust sample.
To avoid such contamination, the Housevac must be run only as specified in the
protocol, to avoid "sucking in" any other dust in the vicinity. Care must especially be
taken in removing the bag from the Housevac for weighing, so that none of the
collected dust escapes or is allowed to fall out of the bag.
I-5
-------
Protocol: Vacuuming and Sampling of
Dust with Housevacs
Revision No. 1
September 24, 1993
Page 6 of 7
For sample collection, always use clean equipment. Collect the sample
carefully, and in an area that minimizes potential contamination from other sources or
test operations.
6.0 DEVIATIONS FROM PROTOCOL
Every attempt shall be made to follow this protocol. Deviations from the
protocol may compromise the data quality and completeness objectives of the project.
Deviations from the protocol will generally fall into two categories: inadvertent
deviations (procedural errors) and deliberate deviations (modifications to the protocol
in response to unusual (or unanticipated conditions).
In the case of inadvertent deviations from the protocol, the sampling team shall
fully document the deviation on the sampling data form and immediately notify the
MRI work assignment leader. Corrective action(s) shall be taken to ensure that the
situation is not repeated. If possible, any tests or samples affected by the inadvertent
deviation shall be redone in accordance with the specified protocol.
Deliberate deviations from the protocol should be approved in advance with a
signed modification to the QAPjP. If time is critical, preliminary verbal approval may
be granted by EPA. These verbal approvals will be followed up with a signed
modification to the QAPjP. In either case, the sampling team should notify all parties
concerned in a timely manner so that the approval mechanism can be expedited. The
MRI work assignment leader is responsible for initiation of the QAPjP modification and
acquiring the necessary approvals.
I-6
-------
Project 9802
WA No. 55
Test Identification
Housevac
Substrate
Grind-in
Dust Amount
Pb Cone
Dust Size
Team
Data Entry Sheets
for
Housevac Tests
Test Sequence Number
Date
Operator
(A, B, C or D)
(TILE, LINOIeum, WOOD, UPHOIstery, CaRPeT)
(Yes, No)
(100, 400 mg/ft2
(Low, High)
«53, 53-106, 106-150, 150-212, 212-250, 250-2000)
(number 1 or 2)
Procedure
Perform the tests according to the housevac test sequence in Appendix P, and vac procedure in Appendix I
Tare weigh new bag:
Run free 40 sec, cool 2 min, brush and record weight after 1 more min
Vacuum for 40 sec before any dust deposit
Reweigh bag (cool 2 min, brush and record weight after 1 more min)
Deposit dust, vacuum 40 sec, weigh the bag. Total of 3 times. (Grind-in after each dust deposit, if applicable)
Repeat vacuuming only (vacuum 40 sec, weigh the bag) 3 times
Shake dust from the bag, weigh, prepare for lead analysis
Vacuum dust from wand and brush (no weighing)
Tare weight of bag
Vacuum and weigh
Add dust, vac & weigh
Add dust, vac & weigh
Add dust, vac & weigh
Vacuum & weigh
Vacuum & weigh
Vacuum & weigh
Dust sent to lab
Weight of Dust
(Balance # )
Weight of Bag
(Balance # )
Total Wt
am.
.0
.1
.2
.3
Tare Wt
dm.
Net Wt
am.
Time
Weight
am.
Increase
gm.
.5
.6
.7
.8
Bar Code
for Sample
Bar Code
for Blank
Submit one blank for each week
Sample relinquished by
Sample received by
Date of transfer
Reviewed by _
Date reviewed
1-7
-------
APPENDIX J
DIGESTION PROCEDURE
MODIFIED METHOD 3050 FOR ANALYSIS OF LEAD (Pb)
IN WIPE DUST SAMPLES
-------
Modified Method 3050: Lead in Wipe Dust Samples
Revision No. 0
Date: June 18, 1993
Page 1 of 5
DIGESTION PROCEDURE
MODIFIED METHOD 3050 FOR ANALYSIS OF LEAD (Pb)
IN WIPE DUST SAMPLES
1.0 SUMMARY OF METHOD
This analytical method is a modified version of Method 3050 from the SW-846,
3rd Edition manual. It is written in a manner that provides ease of execution relative
to the published procedure. This method is used for the acid digestion of wipe dust
samples and associated quality control (QC) samples for ICP-AES analysis of lead (Pb).
It should be noted that this procedure for preparing dust wipe samples does not use
hydrochloric acid for digestion. The final reflux is nitric acid (HN03), and the sample
digestate will be approximately 10% (v/v) HN03 following digestion.
The entire wipe dust sample is digested in HNO3 and hydrogen peroxide (H202).
The digestates are diluted to final volume following a final reflux and cookdown using
nitric acid.
2.0 APPARATUS AND MATERIALS
• Beakers: Griffin 250-mL
• Watch glasses
• Forceps: polyethylene
• Volumetric flasks with stoppers: 100-mL
• Funnels: Plastic, porcelain, or glass fitted with fast filter paper suitable for lead
analysis. (Buchner type funnels are recommended due to potentially large amount
of undigested wipe materials commonly encountered using this method.)
• Thermometers: red alcohol and covers range of 0° to 110°C
• Hot plates: capable of maintaining a temperature of 80° to 100°C
• Centrifuge
• Centrifuge tubes: polyethylene with screw caps, 50-mL capacity
J-1
-------
Modified Method 3050: Lead in Wipe Dust Samples
Revision No. 0
Date: June 18, 1993
Page 2 of 5
• Kimwipes"
• Disposable plastic 10-mL syringes with Luer-lok fittings
• Gelman Acrodisc filters, female Luer-lok, 0.45-//m pore size
3.0 REAGENTS
• ASTM Type I water: Minimum resistance of 16.67 megaohm-cm, or equivalent
• Concentrated (70 to 71%) HNO3: Baker instra-analyzed, or equivalent
• Hydrogen peroxide (30%), reagent grade
4.0 QUALITY CONTROL
For each group of samples processed, sample preparation quality control
samples (SP QCs) should be carried throughout the entire sample preparation and
analytical process. The SP QCs to include in each batch of samples are summarized
in Table J-1.
TABLE J-1. SUMMARY OF SAMPLE PREPARATION QC SAMPLES-WIPES
Sample Type
Method Blank
Reference Material
(2 different lead
levels)
No-Spiked Sample
Spiked Sample and
spiked duplicate
Description
Empty beaker,
equivalent to a reagent
blank
1 g ± 0.1 g of
reference material plus
a blank wipe
Blank wipe
1 mL of 100^/g/mL
lead stock solution plus
a blank wipe
Frequency
1 per 20 samples;
minimum of 1 per
batch
1 of NIST SRM 1646
and 1 NIST SRM 2704
per batch
1 per 20 samples;
minimum of 1 per
batch
1 per 20 samples;
minimum of 1 per
batch
Data Quality Objective
Measured value less
than 10 times the
Instrumental Detection
Limit
Accuracy of ± 25%
from average known
value
Not applicable— used to
calculate spiked sample
recovery
Accuracy of ± 20%
from average known
value
J-2
-------
Modified Method 3050: Lead in Wipe Dust Samples
Revision No. 0
Date: June 18, 1993
Page 3 of 5
5.0 PROCEDURE
5.1 Care should be taken during the execution of each step of the following
procedure to ensure the sample losses do not occur due to spillage and the
gains do not occur due to contamination (See Note 1).
NOTE 1: All reagent sources (lot numbers) used for sample preparation must
be recorded in a laboratory notebook. In addition, any inadvertent deviations
to this procedure, unusual occurrences or observations must also be recorded
on a real-time basis as samples are processed. The laboratory task leader
must be informed in a manner which permits as close to real-time action as
possible if any deviations or unusual happenings occur in order to take any
needed corrective actions.
All samples in a processing batch must be treated equally. For example, if one
sample requires additional hydrogen peroxide, then all samples in that batch
must be given additional peroxide.
5.2 Document the condition of samples received in a laboratory note.
5.3 Label 250-mL Griffin beakers for each wipe sample and associated quality
control sample to be processed.
5.4 The wipe samples do not require weighing by the LAB. Carefully open the
container containing the sample and transfer the contents into labeled Griffin
beakers using a new pair of plastic gloves and\or plastic forceps (see Note 2).
NOTE 2: For spikes and spike duplicates, transfer blank wipe to beakers
targeted for these samples and spike onto them according to details in Table J-
1.
5.5 SAMPLE DIGESTION
Perform digestion of each sample as follows:
Carefully, add 25 mL of 1:1 HN03 to each beaker, gently swirl to mix, and
cover with a watch glass. Gently heat the sample to 85° to 100°C and reflux
for 10 to 15 min without boiling.
J-3
-------
Modified Method 3050: Lead in Wipe Dust Samples
Revision No. 0
Date: June 18, 1993
Page 4 of 5
5.5.2 Allow the sample to cool.
5.5.3 Add 10 ml of concentrated HNO3, replace the watch glass, and reflux for 30
min without boiling.
5.5.4 Repeat this last step (5.5.3) to ensure complete oxidation.
5.5.5 Remove watch glass and allow the solution to evaporate to approximately 10
ml without boiling, while maintaining a covering of solution over the bottom
of the beaker (see Note 3).
NOTE 3: Because ribbed watch glasses are not available, the watch glasses
may be removed to accelerate volume reduction while ensuring minimal con-
tamination of the samples through careful observation. When removing these
watch glasses, care must be exercised to avoid losses by rinsing them with a
minimum amount of Type I water (rinsed into the sample beaker) and avoiding
contaminating them by placing them upside down on new clean Kimwipes".
5.5.6 Allow the sample to cool.
5.5.7 Add 5 mL Type I water and 5 ml_ of 30% hydrogen peroxide (H202). Cover
the beaker with a watch glass and return the covered beaker to the hot plate
for warming and to start the peroxide reaction. Care must be taken to ensure
that losses do not occur due to excessively vigorous effervescence. Heat until
effervescence subsides and cool the beaker.
5.5.8 Continue to add 30% H202 in 1-mL aliquots with warming until the
effervescence is minimal or until the general sample appearance is unchanged
(see Note 4).
NOTE 4: Do not add more than a total of 10 ml of 30% H2O2 even if
effervescence has not been reduced to a minimal level.
5.5.9 Remove the watch glass and continue heating the acid-peroxide digestate
carefully until the volume has been reduced to approximately 10 ml (see Note
3).
J-4
-------
Modified Method 3050: Lead in Wipe Dust Samples
Revision No. 0
Date: June 18, 1993
Page 5 of 5
5.5.10 Allow the digestates to cool, rinse the beaker walls and bottom of the
watch glass into the digestate, and quantitatively transfer to a 100-mL
volumetric flask (see Note 5). Dilute to volume with Type I water.
NOTE 5: It is recommended that a funnel be used to aid in quantitative
transfer due to the potential presence of large quantities of undissolved wipe
material. Use either a clean porcelain funnel or a glass or plastic funnel. If the
funnel contains small premade holes (Buchner type), then no filter needs to be
used. Otherwise fit the funnel with the fastest filter paper suitable for metals
analysis filtering.
5.6 Particulates in the digestate then should be removed by filtration, by
centrifugation, or by allowing the sample to settle prior to instrumental
measurement. A disposable syringe equipped with an Acrodisc filter can be
used to filter a portion of the sample digest prior to analysis.
5.7 The diluted digestate solution contains approximately 10% (v/v) HN03. Calibra-
tion standards used for instrumental measurement should be made with this
level of HN03.
J-5
-------
APPENDIX K
DIGESTION PROCEDURE
MODIFIED METHOD 3050 FOR ANALYSIS OF LEAD (Pb)
IN VACUUM DUST SAMPLES (CASSETTES OR BOTTLES)
COLLECTED WITH A SAMPLER OR HOUSEVAC
-------
Modified Method 3050: Lead in Vacuum Dust Samples
Revision No. 0
Date: June 18, 1993
Page 1 of 6
DIGESTION PROCEDURE
MODIFIED METHOD 3050 FOR ANALYSIS OF LEAD (Pb)
IN VACUUM DUST SAMPLES (CASSETTES OR BOTTLES)
COLLECTED WITH A SAMPLER OR HOUSEVAC
1.0 SUMMARY OF METHOD
This analytical method is a modified version of Method 3050 from the SW-846,3rd Edition
manual. It is written in a manner which provides ease of execution relative to the
published procedure. This method is used for the acid digestion of dust samples in
cassettes or bottles and associated quality control (QC) samples for ICP-AES analysis
of Pb. The primary focus of the modifications relative to the published procedure is a
change in amounts of reagents used and a change in final dilution volume to accom-
modate the sample size. In addition, the method has been modified for handling the
samples contained in filter cassettes and bottles. It should be noted that this procedure
does not use hydrochloric acid for digestion. The final reflux is nitric acid (HNO3) and the
sample digestate will be approximately 10% (v/v) HNO3 following digestion.
The samples are digested in HNO3 and hydrogen peroxide (H2Oj). The digestates are
diluted to final volume following a final reflux and cookdown using nitric acid.
2.0 APPARATUS AND MATERIALS
• Beakers: Griffin 100-mL
• Watch glasses
• Forceps: polyethylene
• Volumetric flasks with stoppers: 25-mL
• Thermometers: red alcohol and covers range of 0° to 110°C
• Hot plates: capable of maintaining a temperature of 80° to 100° C
• Centrifuge
• Centrifuge tubes: polyethylene with screw caps, 50-mL capacity
• Kimwipes™
• Disposable plastic 10-L syringes with Luer-lok fittings
K-1
-------
Modified Method 3050: Lead in Vacuum Dust Samples
Revision No. 0
Date: June 18, 1993
Page 2 of 6
• Gelman Acrodisc filters, female Luer lok, 0.45-//m pore size
• Screwdriver
3.0 REAGENTS
• ASTM Type I water: Minimum resistance of 16.67 megaohm-cm, or equivalent
• Concentrated (70 to 71%) HNO3: Baker instra-analyzed, or equivalent
• Hydrogen peroxide (30%), reagent grade
4.0 QUALITY CONTROL
For each group of samples processed, sample preparation quality control samples (SP
QCs) should be carried throughout the entire sample preparation and analytical process.
The SP QCs to include in each batch of samples are summarized in Table K-1.
5.0 PROCEDURE
5.1 Care should be taken during the execution of each step of the following procedure to
ensure that sample losses do not occur due to spillage and that gains do not occur due
to contamination (see NOTE 1).
K-2
-------
Modified Method 3050:
Lead in Vacuum Dust Samples
Revision No. 0
Date: June 18, 1993
Page 3 of 6
NOTE 1: All reagent sources (lot numbers) used for sample preparation must be
recorded In a laboratory notebook. In addition, any inadvertent deviations to this
procedure, unusual occurrences or observations must also be recorded on a real-
time basis as samples are processed. The laboratory task leader must be informed
In a manner which permits as close to real-time action as possible if any deviations
or unusual happenings occur in order to take any needed corrective actions.
All samples in a processing batch must be treated equally. For example, if one
sample requires additional hydrogen peroxide, then all samples in that batch must
be given additional peroxide.
TABLE K-1. SAMPLE PREPARATION QC SAMPLES-
CASSETTES AND DUST IN BOTTLES
Sample Type
Method Blank
Reference Material
(2 different lead
levels)
No-Spiked Sample,
cassette
Spiked Sample, and
duplicate spike
cassette
Spiked Sample, and
duplicate spike dust
bottle
Description
Empty beaker,
equivalent to a reagent
blank and a no-spiked
sample for dust in
bottles.
1 g ± 0.1 g of
reference material into
an empty beaker
Blank cassette
1 mLof 100^g/mL
lead stock solution plus
a blank cassette
1 mLof 100//g/mL
lead stock solution into
an empty beaker,
equivalent to a spiked
method blank
Frequency
1 per 20 cassette plus
dust bottle samples;
minimum of 1 per
batch
1 NISTSRM 1646 and
1 NIST SRM 2704 per
batch
1 per 20 cassette
samples; minimum of
1 per batch
1 per 20 cassette
samples; minimum of
1 per batch
1 per 20 dust bottle
samples; minimum of
1 per batch
Data Quality Objective
Measured value less than
10 times the Instrumental
Detection Limit
Accuracy of ± 25% from
average known value
Not applicable— used to
calculate spiked sample
recovery
Accuracy of ± 20% from
average known value
Accuracy of ± 20% from
average known value
5.2 Document the condition of samples received in the laboratory notebook.
5.3 Label 100-mL Griffin beakers for each sample and associated quality control sample to
be processed.
K-3
-------
Modified Method 3050: Lead in Vacuum Dust Samples
Revision No. 0
Date: June 18, 1993
Page 4 of 6
5.4 TRANSFER OF CASSETTE SAMPLES TO DIGESTION VESSELS
The cassette dust samples do not require weighing. Transfer each entire cassette dust
sample into labeled Griffin beakers using the following procedure (see NOTE 2).
NOTE 2: For spikes and spike duplicates, transfer blank cassettes to beakers
targeted for these samples and spike onto them according to details in Table K-1.
5.4.1 For cassette samples, carefully pry open and remove the top section of the filter cassette
using a clean flat-edged screw driver, or equivalent tool. Place the top section upside
down (in a manner which will not cause sample loss) on a clean Kimwipe™.
5.4.2 Gently empty the loose dust from the cassette into a labeled beaker. Care should be
taken to prevent sample losses due to blowing or scattering of the dust.
5.4.3 Carefully rinse the inside of both the top section and remaining cassette assembly with
5 to 10 mL of 10% (v/v) HNO3 transferring the rinse solution to the digestion beaker.
5.4.4 Carefully pry open and remove the retaining ring (placing it on a clean Kimwipe™) using
a clean flat-edged screw driver, or equivalent tool.
5.4.5 Using acid cleaned polypropylene forceps carefully remove and transfer the filter to the
digestion beaker.
5.4.6 Using the same forceps grasp the backup support pad and using the forceps and
support pad, carefully swab the inside of the top section, retaining ring, and bottom
section of the filter cassette. Then transfer the pad to the digestion beaker. This step is
performed the help ensure that a quantitative sample transfer is achieved.
5.5 TRANSFER OF BOTTLED DUST SAMPLES TO DIGESTION VESSELS
The dust samples in bottles do not require weighing. Transfer each entire dust sample
into labeled Griffin beakers using the following procedure (see NOTE 3). If the amount
of dust contained in a bottle is too large, take a weighed aliquot for digestion.
NOTE 3: For spikes and spike duplicates, add 5 mL of 1:1 HNO3 to each beaker and
spike into empty beakers according to details in Table K-1.
5.5.1 Wipe off the outside of the bottle with a laboratory wipe (particularly the cap). Hold the
top of the bottle over the beaker and carefully remove the top allowing any dust trapped
in the cap to the fall into the beaker. While holding the cap over the beaker, rinse off the
K-4
-------
Modified Method 3050: Lead in Vacuum Dust Samples
Revision No. 0
Date: June 18, 1993
Page 5 of 6
inside surface into the beaker using about 1 to 2 ml of water from a squirt bottle filled
with ASTM Type I water. Set the cap down (inside surface up) on a clean laboratory wipe.
5.5.2 Carefully tap the contents of the bottle into the beaker.
5.5.3 Place approximately 2 ml of 1:1 HNO3 into the bottle, and recap. Gently turn the bottle
to allow the solution to come into contact with all inside surfaces of the bottle. Uncap
the bottle and pour the contents into the beaker.
5.5.4 Place approximately 2 mL of 1:1 HNO3 into the bottle, and recap. Gently turn the bottle
to allow the solution to come into contact with all inside surfaces of the bottle. Uncap
the bottle and pour the contents into the beaker. (This is a repeat of step 5.5.3).
5.5.5 Place approximately 2 mL of 1:1 HNO3 into the bottle, and recap. Gently turn the bottle
to allow the solution to come into contact with all inside surfaces of the bottle. Uncap
the bottle and pour the contents into the beaker. (This is a second repeat of step 5.5.3
for a total of three rinses of the bottle).
5.6 DIGESTION OF SAMPLES
Perform digestion of each sample as follows (see NOTE 4).
NOTE 4: For dust samples from bottles, skip to step 5.6.2 since acid was already
used to quantitatively transfer the sample from the bottle to the beaker.
5.6.1 Add 5 mL of 1:1 HNO3 to each beaker.
5.6.2 Gently swirl to mix, and cover with a watch glass. Gently heat the sample to 85° to
100°C and reflux for 10 to 15 min without boiling.
5.6.2 Allow the sample to cool.
5.6.3 Add 2.5 mL of concentrated HNO3, cover with watch glass and reflux for 30 min without
boiling.
5.6.4 Repeat this last step (5.6.3) to ensure complete oxidation.
5.6.5 Remove watch glass and allow the solution to evaporate to approximately 5 mL without
boiling, while maintaining a covering of solution over the bottom of the beaker (see NOTE
5).
K-5
-------
Modified Method 3050: Lead in Vacuum Dust Samples
Revision No. 0
Date: June 18, 1993
Page 6 of 6
NOTE 5: Because ribbed watch glasses are not available, the watch glasses may be
removed to accelerate volume reduction while assuring minimal contamination of the
samples through careful observation. When removing these watch glasses, care
must be exercised to avoid losses by rinsing them with a minimum amount of Type
I water (rinsed into the sample beaker) and avoiding contaminating them by placing
them upside down on new clean Kimwipe™.
5.6.6 Allow the sample to cool.
5.6.7 Add 2 mL Type I water and 2 mL of 30% hydrogen peroxide (H2OJ. Cover the beaker
with a watch glass and return the covered beaker to the hot plate for warming and to start
the peroxide reaction. Care must be taken to ensure that losses do not occur due to
excessively vigorous effervescence. Heat until effervescence subsides and cool the
beaker.
5.6.8 Continue to add 30% H2O2 in 1-mL aliquots with warming until the effervescence is
minimal or until the general sample appearance is unchanged (see NOTE 6).
NOTE 6: Do not add more than a total of 5 mL of 30% H2O2 even if effervescence
has not been reduced to a minimal level.
5.6.9 Remove the watch glass and continue heating the acid-peroxide digestate carefully until
the volume has been reduced to approximately 2.5 mL (see NOTE 5).
5.6.10 Allow the digestates to cool, rinse the beaker walls and bottom of the watch glass into
the digestate, and quantitatively transfer to a 25-mL volumetric flask. Dilute to volume
with Type I water.
5.7 Particulates in the digestate should then be removed by filtration, by centrifugation, or by
allowing the sample to settle prior to instrumental measurement. A disposable syringe
equipped with an Acrodisc filter can be used to filter a portion of the sample digest prior
to analysis.
5.8 The diluted digestate solution contains approximately 10% (v/v) HNO3. Calibration
standards used for instrumental measurement should be made with this level of HNO3.
K-6
-------
APPENDIX L
ANALYTICAL PROCEDURE
MODIFIED METHOD 601OA FOR THE ANALYSIS OF DIGESTED SAMPLES
FOR LEAD (Pb) BY
INDUCTIVELY COUPLED PLASMA (ICP-AES)
PLUS MODIFIED METHODS FOR FLAME ATOMIC ABSORPTION (FAAS)
AND GRAPHITE FURNACE ATOMIC ABSORPTION (GFAAS) TECHNIQUES
-------
Modified Method 601OA: Lead
Revision No. 0
Date: June 18, 1993
Page 1 of 12
MODIFIED METHOD 6010A FOR THE ANALYSIS OF DIGESTED SAMPLES
FOR LEAD (Pb) BY
INDUCTIVELY COUPLED PLASMA (ICP-AES)
PLUS MODIFIED METHODS FOR FLAME ATOMIC ABSORPTION (FAAS)
AND GRAPHITE FURNACE ATOMIC ABSORPTION (GFAAS) TECHNIQUES
1.0 SUMMARY
A sample digestate is analyzed for lead content using ICP-AES, Flame-AAS, or
Graphite Furnace-AAS techniques. Instrumental Quality Control samples are analyzed
along with sample digestates to assure adequate instrumental performance. This
procedure is a modification of the SW-846 Method 601 OA.
2.0 DEFINITIONS
2.1 Digestion - The sample preparation process that will solubilize targeted analytes
present in the sample and results in an acidified aqueous solution called the
digestate.
2.2 Digestate - An acidified aqueous solution that results from performing sample
preparation (digestion) activities. Lead measurements are made using this
solution.
2.3 Batch A group of QC samples that are processed together using the same
reagents and equipment.
2.4 Serial Dilution - A method of producing a less concentrated solution through
one or more consecutive dilution steps. The dilution step for a standard or
sample is performed by volumetrically placing a small aliquot of a higher
concentrated solution into a volumetric flask and diluting to volume with water
containing the same acid levels as found in original sample digestates.
2.5 Method Blank - A digestate that reflects the maximum treatment given any one
sample within a sample batch except that it has no sample initially placed into
the digestion vessel. (The same reagents and processing conditions that are
applied to samples within a batch also are applied to the method blank.)
L-1
-------
Modified Method 601OA: Lead
Revision No. 0
Date: June 18, 1993
Page 2 of 12
Analytical results from method blanks provide information on the level of
potential contamination experienced by samples processed within the batch.
2.6 No-Spiked Sample A portion of a homogenized sample that is targeted for
addition of analyte but that was not fortified with all the target analytes before
sample preparation. A method blank serves as a no-spike sample in cases
where samples can not be uniformly split, as described in section 2.7. Analysis
results for this sample are used to correct for native analyte levels in the spiked
and spiked duplicate samples.
2.7 Spiked Sample and Spiked Duplicate Sample - Two portions of a homogenized
sample that are targeted for addition of analyte and are fortified with all the
target analytes before preparation. In cases where samples can not be
uniformly split (such as paint chip samples taken for lead per area
determinations), a method blank can be used in place of the homogenized
sample split. Use of a method blank for a spiked sample should be referred to
as a "spiked method blank" or "spiked method blank duplicate." Analysis
results for these samples are used to provide information on accuracy and
precision of the overall analysis process.
2.8 Analysis Run - A period of measurement time on a given instrument during
which data is calculated from a single calibration curve (or single set of curves).
Re-calibration of a given instrument produces a new analysis run.
2.9 Instrumental QC Standards - Solutions analyzed during an instrumental analysis
run that provide information on measurement performance during the
instrumental analysis portion of the overall lead measurement process.
2.10 Semi-quantitative Screen - An analysis run that is performed on highly diluted
sample digestates for the purpose of determining the approximate analyte level
in the digest. This analysis run is generally performed without inserting
Instrumental QC standards except for calibration standards. Data from this run
are used for determining serial dilution requirements for sample digestates to
keep them within the linear range of the instrument.
2.11 Quantitative Analysis - An analysis run on sample digestates (or serial dilutions
of sample digestates) that includes Instrumental QC standards. Data from this
run are used to calculate and report final lead analysis results.
L-2
-------
Modified Method 601OA: Lead
Revision No. 0
Date: June 18, 1993
Page 3 of 12
2.12 Initial Calibration Blank (ICB) A standard solution which contains no analyte
and is used for initial calibration and zeroing instrument response. The ICB
must be matrix matched to acid content present in sample digestates. The ICB
must be measured during calibration and after calibration. The measured value
is to be less than 5 times the instrumental detection limit.
2.13 Calibration Standards Standard solutions used to calibrate instrument.
Calibration standards must be matrix matched to acid content present in sample
digestates and must be measured prior to measuring any sample digestates.
2.14 Initial Calibration Verification (ICV) A standard solution (or set of solutions)
used to verify calibration standard levels. Concentration of analyte near
mid-range of linear curve that is made from a stock solution having a different
manufacturer or manufacturer lot identification than the calibration standards.
The ICV must be matrix matched to acid content present in sample digestates.
The ICV must be measured after calibration and before measuring any sample
digestates. The measured value to fall within _±10% of known value.
2.15 Interference Check Standard (ICS) - A standard solution (or set of solutions)
used for ICP-AES to verify accurate analyte response in the presence of
possible spectral interferences from other analytes present in samples. The
concentration of analyte is to be less than 25% of the highest calibration
standard, concentrations of interferant will be 200//g/MI of Al, Ca, Fe, and Mg.
The ICS must be matrix matched to acid content present in sample digestates.
The ICS must be analyzed at least twice, once before and once after all sample
digestates. The measured analyte value is expected to be within ±20% of
known value.
2.16 Continuing Calibration Verification (CCVJ - A standard solution (or set of
solutions) used to verify freedom from excessive instrumental drift. The
concentration is to be near mid-range of linear curve. The CCV must be matrix
matched to acid content present in sample digestates. The CCV must be
analyzed before and after all sample digestates and at a frequency not less than
every 10 sample digestates. The measured value to fall within ±10% of
known value for ICP-AES or FAAS (±20% for GFAA), run once for every 10
samples.
2.17 Continuing Calibration Blank (CCB) - A standard solution that has no analyte
and is used to verify blank response and freedom from carryover. The CCB
L-3
-------
Modified Method 601OA: Lead
Revision No. 0
Date: June 18, 1993
Page 4 of 12
must be analyzed after the CCV and after the ICS. The measured value is to
be less than 5 times the instrumental detection limit.
3.0 APPARATUS AND MATERIALS
3.1 Analytical Instrumentation
3.1.1 Inductively Coupled Plasma Atomic Emission Spectrometer (ICP-AES).
The ICP-AES, either sequential or simultaneous, must be capable of measuring at least
one of the primary ICP lead emission lines. Emission line used must be demonstrated
to have freedom from common major interferants such as Al, Ca, Fe and Mg or the
ability to correct for these interferants.
3.1.2 Flame Atomic Absorption Spectrometer (FAAS) - Equipped with an air-
acetylene burner head, lead hollow cathode lamp or equivalent and capable of making
lead absorption measurements at the 283.3-nm absorption line.
NOTE: The 283.3-nm line is preferred over the 217-nm line because of the
increased noise levels commonly observed at the 217-nm line for FAAS and
GFAAS.
3.1.3 Graphite Furnace Atomic Absorption Spectrometer (GFAAS) Equipped
with background correction and lead hollow cathode lamp or equivalent and capable
of making lead absorption measurements at the 283.3-nm absorption line.
3.2 Gases
Grades specified by manufacturer of the instrument employed.
3.2.1 Compressed air and acetylene for FAAS.
3.2.2 Compressed or liquid argon for ICP-AES and GFAAS.
3.2.3 Minimum of two stage regulation of all gases.
3.3 Vinyl Gloves: Powderless
L-4
-------
Modified Method 601OA: Lead
Revision No. 0
Date: June 18, 1993
Page 5 of 12
3.4 Micropipettors with Disposable Plastic Tips
Sizes needed to make reagent additions, and spiking standards. In general, the
following sizes should be readily available: 1-5 ml adjustable, 1000^/L, 500 pL,
250 fjl, and 100//L.
3.5 Volumetric Flasks
Sizes needed to make calibration standards, serial dilutions, and Instrumental
QC standards.
4.0 REAGENTS
4.1 Nitric acid, concentrated and reagent grade
4.2 Wafer—Unless otherwise indicated, references to water shall be
understood to mean reagent water as defined by Type 1 of Specification D1193.
(ASTM Type I water: Minimum resistance of 16.67 megohm-cm, or equivalent.)
4.3 Calibration stock solution, 100//g/mL of Pb in dilute nitric acid or
equivalent (such as a multielement stock containing Pb).
4.4 Check standard stock solution (for ICV), 100 jjg/mL of Pb in dilute nitric
acid or equivalent. Must be sourced from a different lot number (or manufacturer)
than the calibration stock solution (7.3).
4.5 Interferant stock solution (for ICS; ICP-AES only), 10000 //g/mL of Al, Ca,
Fe, and Mg in dilute nitric acid or equivalent.
5.0 PROCEDURE
5.1 Laboratory Records—Record all reagent sources (lot numbers) used for
sample preparation in a laboratory notebook. Record any inadvertent deviations,
unusual happenings, or observations on a real-time basis as samples are processed.
Use these records to add supplement lead data when reporting results.
L-5
-------
Modified Method 601OA: Lead
Revision No. 0
Date: June 18, 1993
Page 6 of 12
5.2 Instrumental Setup
5.2.1 FAAS/GFAAS - Set the FAAS or GFAAS spectrometer up for the
analysis of lead at 283.3 nm according to the instructions given by the manufacturer.
Be sure to allow at least a 30-min warmup of the hollow cathode lamp prior to
starting calibration and analysis.
5.2.2 ICP-AES Set the ICP spectrometer up for the analysis of lead at a
primary lead emission line (such as 220.2 nm) according to the instructions given by
the manufacturer. Be sure to allow at least a 30-min warmup of the system prior to
starting calibration and analysis.
5.3 Preparation of Calibration and Instrumental QC Standards
5.3.1 Calibration Standards - Prepare a series of calibration standards covering
the linear range of the instrumentation. Prepare these standards using serial dilution
from the calibration stock solutions. Prepare these standards using the same final
nitric acid concentration present in the sample digestates. Also prepare an Initial
Calibration Blank (ICB) as defined in Section 3 and Table L-1.
NOTE: For FAAS/GFAAS prepare a minimum of 3 calibration standards plus
the ICB for performing calibration of the instrument. ICP-AES can be performed
using one high calibration standard and an ICB. However, more are generally
preferred.
5.3.2 Instrumental QC Standards Prepare Instrumental QC standards as
summarized in Table L-1 using serial dilution from the required stock solutions.
Prepare these standards using the same final nitric acid concentration present in the
sample digestates.
NOTE: The ICV is used to assess the accuracy of the calibration standards.
Therefore, it must be made from a different original source of stock solution
than the stock used to make the calibration standards. Use of a different serial
dilution of the same original stock is not acceptable.
5.4 Calibration and Instrumental Measurement Perform calibration and
quantitative lead measurement of sample digestates and instrumental QC samples in
the sequential order outlined in Table L-2.
L-6
-------
Modified Method 601OA: Lead
Revision No. 0
Date: June 18, 1993
Page 7 of 12
NOTE: Performance of a semi-quantitative screen prior to quantitative analysis
for sample digests containing unknown levels of lead is generally
recommended. The purpose of this screen is to determine serial dilution
requirements of each digestate needed to keep the instrumental response within
the calibration curve. During a semi-quantitative screen, all digestates are
diluted to a constant large value (1-to-100 for ICP/FAAS and 1-to-1000 for
GFAAS). The instrument is calibrated and diluted digestates are analyzed
without inserting the instrumental QC used for a quantitative analysis run.
Data from this screen are reviewed to calculate the optimum serial dilution
needed for each digestate. No sample data can be reported for any analyte
value not falling within the calibration range. Therefore, the optimum dilution
is one that achieves the maximum lead response still within the calibration
curve. For ICP-AES, levels of possible interferants (Al, Ca, Fe and Mg) also
may have to be considered in order to make interference corrections. For ICP-
AES, digestates must be sufficiently diluted to assure that levels of possible
interferants, such as Al, Ca, Fe and Mg, are at or below the levels present in
the ICS.
5.5 Instrumental QC Evaluation and Corrective Action Examine the data
generated from the analysis of calibration standards and Instrumental QC standards.
Evaluate the analysis run using the criteria shown in Table L-1. Failure to achieve the
specifications shown in Table L-1 will require corrective action to be performed as
described below:
5.5.1 ICB, Calibration standards, or ICV Failure to meet specifications for
these Instrumental QC standards requires complete re-calibration. Sample digestates
can not be measured under these conditions. It is recommended that standards be re-
prepared prior to re-calibration.
5.5.2 High Calibration Standard Re-run - Failure to meet specifications for this
Instrumental QC standard requires complete re-calibration. Sample digestates can not
be measured under these conditions. It is recommended that standard range be
reduced prior to re-calibration.
5.5.3 ICS- Failure to meet specifications for these Instrumental QC standards
requires re-analysis of the standard until specifications are met. Sample digestates
can not be measured under these conditions. Re-preparation of the standard prior to
re-analysis is recommended under these conditions. Continued failure of the ICS may
require interference correction investigation or changing of instrument parameters.
L-7
-------
Modified Method 601OA: Lead
Revision No. 0
Date: June 18, 1993
Page 8 of 12
Consult the manufacturer's recommendations under these conditions. Any change
in instrument parameters must be accompanied by recalibration. If measured aliquots
of sample digestates can be shown to contain interferants less than those
recommended for the ICS, then the interference levels in the ICS can be lowered.
Such changes must be documented in laboratory records with data supporting the
justification for the change. All measurements on sample digests must be bracketed
by an ICS that meets specifications (called a "passing" ICS). Failure to meet
specifications on the ICS run after the sample digestates requires re-running all sample
digestates since the last passing ICS was measured. Since only the ICS is required
to be analyzed twice, much data could be lost if the analytical run were long and the
second ICS failed specifications. This is a good reason for including periodic analysis
of the ICS as shown in Table L-2.
5.5.4 CCV- Failure to meet specifications for these Instrumental QC standards
indicates excessive instrumental drift. Sample digestates can not be measured under
these conditions and any sample digestates measured since the last passing CCV
must be reanalyzed. This situation requires either re-analysis of the standard until
specifications are met or re-calibration. All measurements on sample digests must be
bracketed by an CCV which meets specifications.
5.5.5 CCB - Failure to meet specifications for these Instrumental QC standards
indicates the presence of possible instrumental carryover or baseline shift. Such a
failure will have the most impact on sample digestates at the lower end of the
calibration curve. The first corrective action is to re-analyze the CCB. If the CCB
passes, then the rinse time between the samples should be increased and the analysis
continued. If the instrument response is still elevated and has not significantly
changed, then the instrument can be re-zeroed followed by a CCV-CCB and re-analysis
of all samples since the last passing CCB that are within 5 times the response of the
failed CCB.
6.0 CALCULATIONS
For FAAS/GFAAS : Prepare a calibration curve to convert instrument response
(absorbance) to concentration (jjQ/mL) using a linear regression fit. Convert all
instrumental measurements on instrumental QC standards and sample digests to lead
concentration (//g/mL) using the calibration curve.
L-8
-------
Modified Method 601OA: Lead
Revision No. 0
Date: June 18, 1993
Page 9 of 12
NOTE: Some instruments will automatically prepare a calibration curve based
on a linear regression fit.
For ICP-AES: All modern ICPs automatically prepare a calibration curve to convert
instrumental responses (emission intensity) to concentration (//g/ml).
Based on the volume of the solution analyzed (and considering any necessary
dilutions), use the concentration results to calculate the total //g of Pb in the original
sample that was digested, if the original sample was dust in a bottle and the sample
amount was too large so that a weighed aliquot was taken, divide the analysis result
(//g) by the weight of the aliquot and report the result as /jg/g of dust.
L-9
-------
Modified Method 601OA: Lead
Revision No. 0
Date: June 18, 1993
Page 10 of 12
Table L-1. SUMMARY OF LABORATORY INSTRUMENTAL MEASUREMENT
QC STANDARDS
Name
Use
Specification
Frequency
ICB-
Initial
calibration
blank
Used for initial
calibration and
zeroing instrument
response.
Calibration standard which
contains no analyte.
Measured value to be less than
5 times the instrumental
detection limit.
Must be measured during
calibration and after
calibration.
Calibration
standards
Used to calibrate
instrument.
The high standard
rerun is used to
check for high
response rollover.
Must be matrix matched to acid
content present in sample
digestates.
Correlation coefficient of
>.0.995, as measured using
linear regression on instrument
response (y) versus
concentration (x).
Measured value of highest level
calibration standard to fall within
+ 10% of known value.
Must be measured prior to
measuring any sample
digestates.
The highest level
calibration standard must
be measured after
calibration.
ICV-
Initial
calibration
verification
Used to verify
calibration
standard levels.
Concentration of analyte to be
near mid-range of linear curve,
which is made from a stock
solution having a different
manufacturer or manufacturer
lot identification than the
calibration standards.
Measured value to fall within
+ 10% of known value.
Must be measured after
calibration and before
measuring any sample
digestates.
L-10
-------
Modified Method 601OA: Lead
Revision No. 0
Date: June 18, 1993
Page 11 of 12
Table L-1. SUMMARY OF LABORATORY INSTRUMENTAL MEASUREMENT
QC STANDARDS (continued)
Name
Use
Specification
Frequency
ICS-
Interference
check
standard
(for ICP-AES
only)
Used to verify
accurate analyte
response in the
presence of
possible spectral
interferences from
other analytes
present in
samples.
Concentration of analyte to be
less than 25% of the highest
calibration standard.
concentrations of interferant will
be 200 fjg/mL of Al, Ca, Fe,
and Mg.
Measured analyte value to fall
within ±20% of known value.
Must be analyzed at least
twice, once before and
once after all sample
digestates.
CCV-
Continuing
calibration
Verification
Used to verify
freedom from
excessive
instrumental drift.
Concentration to be near
mid-range of linear curve.
Measured value to fall within
± 10% of known value for ICP-
AES or FAAS (±20% for
GFAA).
Must be analyzed before
and after all sample
digestates and at a
frequency not less than
every 10 sample
digestates.
CCB-
Continuing
calibration
blank
Used to verify
blank response
and freedom from
carryover.
Calibration standard which
contains no analyte.
Measured value to be less than
5 times the instrumental
detection limit.
Must be analyzed after the
CCV and after the ICS.
L-11
-------
Modified Method 601OA: Lead
Revision No. 0
Date: June 18, 1993
Page 12 of 12
TABLE L-2. EXAMPLE OF A TYPICAL ANALYSIS ORDER
FOR MEASUREMENT
Run Order No.
(relative)
1
2-4
5
6
7
8
9
10
11
12
Sample ID
ICB
tow, med,
high
ICB
ICV
high
standard
CCB
ICS
CCB
CCV
CCB
Comments
Calibration blank
Calibration standards
Calibration blank
Made from different stock, level
is near mid-point of curve
Calibration standard
Same as calibration blank
Interference check standard
Carryover check
Drift check, same as near
midpoint calibration standard
Carryover check
Instrument
calibration
Calibration
verification
Linearity
check
Interferant
check for ICP
only
Continuing
calibration
verification
*** start repeating cyde of samples-Instrumental QC here ***
13-22
23-24
25-34
35-36
37-38
Sample IDs
CCV
CCB
Sample IDs
ICS
CCB
CCV
CCB
Sample digestates
Drift check +
Carryover check
Sample digestates
Interferant check +
Carryover check
Drift check +
Carryover check
Max. of 10
samples
See run
# 11-12
Max. of 10
samples
See run
#9-10
See run
#11-12
*** end repeating cyde of samples-QC standards here ***
L-12
-------
APPENDIX M
GLASS WARE/PLASTIC WARE CLEANING PROCEDURE
-------
ATOMIC SPECTROMETRY FACILITY
STANDARD OPERATING PROCEDURE
Code: ASF-201
Revision: 1
Date: 02/9/93
Page: 1 of 8
Title:
Author:
Approved:
Glassware/Plasticware Cleaning Procedure
N. Friederich, G. Dewalt
Atoft
(~~y
Chemical Sciences Department Director
~f.^L* ^j^tt^uJkou.
Quality Assurance Unit
1.0 SUMMARY
This standard operating procedure is used to clean laboratory glassware
and plasticware (labware) in the Atomic Spectrometry Facility's Sample
Preparation Laboratory. Labware is cleaned with detergent and nitric acid
solution. Labware prepared by this procedure can be used for field
sample collection and routine sample preparation and analysis work.
The following items are exempt from this procedure because screening
analyses have been performed and these items do not contribute to posi-
tive method blanks: disposable pipette tips, disposable polystyrene
beakers, disposable autosampler tubes/cups, centrifuge tubes, and
disposable Falcon tubes. Additional items may also be exempt from this
procedure if screening analysis determines that these items are free from
contamination of the target analytes, at the levels of interest.
2.0 REQUIRED PRELIMINARY INFORMATION
The following information must be provided before this procedure may be
conducted:
• Charge number.
Total amount of glassware to be processed.
Material Safety Data Sheet for Nitric Acid (HNO3). This must be
read before using nitric acid.
M-1
-------
Code: ASF-201
Revision: 1
Date: 02/9/93
Page: 2 of 8
3.0 APPARATUS AND MATERIALS
3.1 Glassware tubs labeled as: For Clean Glassware and only used
for clean glassware.
3.2 Glassware tubs labeled as: For Dirty Glassware and only used for
dirty glassware.
3.3 Pipette cylinder: for Dl water rinsing
3.4 Pipette cylinder: for Milli-Q water rinsing
3.5 Pipette cylinder: for acid cleaning
3.6 Pipette basket: for acid cleaning and rinsing
3.7 Large acid tank: for acid cleaning
3.8 Brushes: plastic bristle, assorted sizes
3.9 Face shield
3.10 Gloves: heavy duty neoprene or nitrile (green), acid resistant
3.11 Gloves: disposable, powderless, vinyl or latex
3.12 Acid resistant protective clothing: rubber or poly-laminated, tyvek
apron
3.13 Filtering flask
3.14 Aspirator pump
3.15 Labware drainer
3.16 Pipette drying racks
3.17 Labware drying racks
3.18 Paper towels
3.19 Food service towels, or equivalent
3.20 Plastic bags: assorted sizes, for storage of clean, dry pipettes and
labware
3.21 Plastic squirt bottle: 500 mL, for baking soda slurry
MRl-QAWSF-201 . .
-------
Code: ASF-201
Revision: 1
Date: 02/9/93
Page: 3 of 8
4.0 REAGENTS
4.1 Acetone: ACS reagent grade, or equivalent
4.2 Deionized (Dl) water
4.3 Alconox detergent
4.4 Acationox detergent
4.5 Concentrated nitric acid (HNO3): ACS reagent grade
4.6 Approximately 20% to 30% (v/v) nitric acid (HNO3): for acid
cleaning (prepare by adding 1 part concentrated HNO3 to 3 parts Dl
water, as described in AS-201, Acid Bath Maintenance Procedure)
4.7 Milli-Q water (Type I Water): 16.67 megohm-cm minimum
resistance, or equivalent
4.8 Baking soda (sodium bicarbonate): for large acid spills
4.9 Baking soda slurry: for small acid spills (prepare by adding about
50 g baking soda to a 500-mL plastic squirt bottle, then diluting to
volume with Dl water)
5.0 SAFETY REQUIREMENTS
The use of large amounts fo nitric acid requires vigilance to avoid
splashes and spills. Before utilizing this procedure, an individual must
observe and be instructed in the proper technique for using the acid bath.
5.1 A Class A fume hood, verified to be in operating condition, must be
used for the acid bath solutions.
5.2 Safety glasses with side shields must be worn at all times in the
laboratory. A face shield should be used when handling large
pieces of glassware (e.g., 1-L beakers).
MRI-QA\ASF-201
M-3
-------
Code: ASF-201
Revision: 1
Date: 02/9/93
Page: 4 of 8
5.3 Neoprene gloves with vinyl or latex glove liners are required when
working with the acid bath or transferring large volumes of acid
solutions.
5.4 Lab coats are required for working with the acid bath. Acid-
resistant protective clothing, such as a rubber apron, is also
recommended.
5.5 An extra person must be present in the laboratory area when
concentrated acid transfers are being performed, in order to help
handle problems in case of inadvertent spills or exposure.
5.6 The closest shower and eye wash station must be noted before
beginning this procedure. It is located immediately before the
washing area.
5.7 A squirt bottle containing the baking soda (sodium bicarbonate)
slurry and an open box of baking soda must be in the work area for
neutralizing any spills. Use the slurry for neutralizing small acid
spills, including those on clothing. Use the bulk material for
neutralizing larger spills.
5.8 When mixing acid solutions, ALWAYS add the acid to the water to
prevent potentially violent reactions. NEVER add water to acid.
6.0 QUALITY CONTROL
The acid cleaning tanks containing approximately 20% to 30% (v/v) HNO3
are routinely monitored for contamination as described in ASF-202, Acid
Bath Maintenance Procedure.
7.0 GLASS VOLUMETRIC PIPETTE CLEANING PROCEDURE
NOTE: Aspiration is conducted using an aspirator pump attached to a
filtering flask. Do not aspirate from the delivery tip of a pipette.
MRI-OA\ASF-201
M-4
-------
Code: ASF-201
Revision: 1
Date: 02/9/93
Page: 5 of 8
7.1 Preclean with Alconox solution if pipettes are contaminated
with organic compounds. Pipettes are contaminated with organic
compounds when used with solid organic waste, municipal
wastewater, etc. If organic contamination is in doubt, ask the
project leader.
7.1.1 Scrub the outside of the pipettes using Alconox solution and
a food service towel.
7.1.2 Aspirate 2 pipette volumes of Alconox solution (prepared with
Dl water according to container's instructions) through each
pipette.
7.1.3 Rinse off the outside of the pipette with Dl water until suds
are gone.
7.1.4 Aspirate Dl water through each pipette until the suds are
gone.
7.2 Clean with Acationox solution.
7.2.1 Aspirate 2 aliquots Acationox solution (prepared with Dl
water according to container's instructions) through each
pipette.
7.2.2 Aspirate Dl water through each pipette until the suds are
gone.
7.2.3 Rinse the outside of the pipettes with Dl water.
7.3 Clean with nitric acid solution.
7.3.1 Place pipettes tip-up in the pipette basket. If the basket is
not already in the acid cylinder containing approximately 20%
to 30% (v/v) HNO3, carefully transfer the basket to the
cylinder.
7.3.2 Allow pipettes to soak for at least 15 min.
7.3.3 Slowly lift the basket, hook basket on hook inside hood, and
allow the acid solution to drain back into the acid bath.
MRI-QAVASF-201
M-5
-------
Code: ASF-201
Revision: 1
Date: 02/9/93
Page: 6 of 8
7.3.4 Transfer pipettes in the basket into the pipette Dl rinsing
tank. If needed, connect the Dl waterline to the rinsing tank.
Turn on the Dl water. Allow the Dl water to flow into the
rinsing tank until a minimum of 2 tank volumes have passed
through the tank. Lift the basket and allow any excess Dl
water to drain back into the rinsing tank.
7.3.5 Transfer pipettes in the basket to a Milli-Q cylinder. If the
cylinder is not already filled, fill with Milli-Q water. Slowly lift
the basket and allow the water to drain from the pipettes
back into the bath. Submerge the basket and pipettes into
the cylinder, allow the pipettes to fill with water. Lift the
basket and drain the pipettes again.
7.3.6 Carefully and slowly transfer pipettes to a Clean Glassware
tub for movement to a clean drying area or transfer directly
into a glassware cart drying rack lined with food towels.
7.3.7 If a clean glassware tub was used for transfer, stack pipettes
tip-up in a pipette drying rack or glassware cart drying rack
and cover with a clean food service towel.
7.3.8 Allow pipettes to dry completely at ambient temperature.
7.3.9 Store the clean dry pipettes in a clean drying area until use.
8.0 GENERAL LABWARE CLEANING PROCEDURE
8.1 Prepare labware for cleaning.
8.1.1 Place dirty labware in Dirty Glassware tubs.
8.1.2 Remove all identifying marks from the labware such as
labeling, barcodes, and tape. Remove indelible marking pen
labels by wiping with a paper towel saturated with acetone
(perform inside or immediately in front of a fume hood).
CAUTION: Acetone will react with and dissolve vinyl gloves,
therefore wear latex or nrtrile gloves when using acetone. In
addition, acetone may react with some plasticware.
MRI-QA\ASF-201
M-6
-------
Code: ASF-201
Revision: 1
Date: 02/9/93
Page: 7 of 8
8.2 Preclean with Alconox solution if labware is contaminated with
organics.
8.2.1 Fill a Dirty Glassware tub with Alconox solution (prepared
with hot tap water according to container's instructions).
8.2.2 Allow labware to soak for a sufficient amount of time
(approximately 2 to 4 hr) to remove organic residues from
the surface of the labware (see NOTE 1).
NOTE 1: CAUTION: Do not soak for more than 8 hr.
Alconox will remove the white permanent label
areas from glassware.
8.2.3 Scrub labware inside and out with an appropriate plastic
bristle brush or food service towel until they are clean.
8.2.4 Rinse labware inside and out a minimum of 3 times with Dl
water, then drain. Label if not proceeding as Labware Ready
for Acationox Cleaning.
8.3 Clean with Acationox solution.
8.3.1 Fill a Dirty Glassware tub with Acationox solution (prepared
with Dl water according to directions on the container).
8.3.2 Transfer labware to the tub. Scrub labware inside and out
with an appropriate plastic bristle brush or food service towel
until they are clean. Some labware, such as volumetric
flasks, cannot be easily cleaned inside using a brush or
towel. For these types of labware vigorously shake an
aliquot of Acationox solution within the vessel to help with
cleaning.
8.3.3 Rinse labware inside and out 3 or 4 times with Dl water.
8.3.4 Allow labware to drain for several minutes, by inverting them
in a drainer marked with a sign that identifies them as "ready
for acid bath.' In general, use of drainers in glassware carts
is recommended.
8.3.5 If labware will not be immediately cleaned in the acid bath,
cover labware with food service towels (to prevent
contamination from airborne dust) and label as Labware
Ready for Acid Bath.
MRI-QASASF-201
-------
Code: ASF-201
Revision: 1
Date: 02/9/93
Page: 8 of 8
8.4 Clean with nitric acid solution.
8.4.1 Carefully submerge labware into the acid bath tanks
containing approximately 20% to 30% (v/v) HNO3.
8.4.2 Allow labware to soak at least 15 min.
CAUTION: Avoid soaking plasticware longer than 8 h (to
prevent damage from long term exposure to the acid
solution).
8.4.3 Carefully remove labware from the tank, drain any acid back
into the tank (see NOTE 2).
NOTE 2: If gloves come into contact with acid, minimize
spillage caused by acid drips from gloves by
limiting movement of gloves outside the hood.
One method is the use of a separate plastic tub
or other equivalent container inside the hood for
placement of acid containing gloves. Other
methods which will minimize spillage can be
used. If spillage occurs, neutralize with baking
soda as described in Section 5.7.
8.4.4 If the labware is to be rinsed within the acid bath hood using
a rinse tank, then transfer labware to a clean glassware tub
containing Milli-Q water to transfer the glassware, then rinse
labware a minimum of 3 times with Milli-Q water.
If the labware is to be rinsed outside of the acid bath hood,
then transfer the labware to a clean glassware tub containing
Milli-Q water to eliminate the presence of acid fumes. Rinse
labware a minimum of 3 times with Milli-Q water.
8.4.5 Stack labware on drying racks lined with clean food service
towels. Cover labware with additional clean food service
towels (to prevent contamination from airborne dust). Label
as Clean Labware and place into a clean drying area.
8.4.6 Allow labware to dry completely at ambient temperature.
8.4.7 Store labware in sealed plastic bags until use.
MRI-QA\ASF-201
-------
APPENDIX N
ACID BATH MAINTENANCE PROCEDURE
-------
Code: ASF-202
ATOMIC SPECTROMETRY FACILITY Revision. 1
STANDARD OPERATING PROCEDURE Date: 02/9/93
Page: 1 of 9
Title:
Author:
Approved:
Acid Bath Maintenance Procedure
N. Friederich, G. Dewalt
CfTemical Sciences Department Director
Quality Assurance Unit
1.0 SUMMARY
Glassware and plasticware cleaning for the Atomic Spectrometry Facility is
performed in the sample preparation laboratory, using acid cleaning baths
containing approximately 20% to 30% (v/v) nitric acid (HNO3). This
standard operating procedure describes the set-up, routine screening (for
metals contamination), and replenishing of pipette and general labware
acid cleaning baths.
2.0 REQUIRED PRELIMINARY INFORMATION
The following information must be provided before this procedure may be
conducted:
• Charge number.
• Material Safety Data Sheet for Nitric Acid (HNO3) is available for
review in the MSDS notebook, located in the ASF data reduction
room.
3.0 ACID BATH MAINTENANCE LOGBOOK
All activities related to acid bath maintenance are recorded in a laboratory
notebook dedicated to the acid bath. Logbook entries must be made each
time a bath is filled, volume adjusted, or screened. It is the acid bath
maintenance staffs responsibility to assure that the log is completed as
required.
N-1
MRI-QA\ASF-202
-------
Code: ASF-202
Revision: 1
Date: 02/9/93
Page: 2 of 9
4.0 APPARATUS AND MATERIALS
4.1 Tygon tubing
4.2 Pipette cylinder: for acid bath cleaning
4.3 Large acid tank: for acid bath cleaning
4.4 Large acid tank: for neutralization
4.4 Large stirring rods
4.6 Large plastic drum: for acid waste disposal storage
4.7 Eppendorf pipettes with disposable tips
4.8 Inductively Coupled Plasma-Atomic Emission Spectrometer (ICP-
AES)
4.9 Face shield
4.10 Gloves: heavy duty, neoprene or nit rile (green), acid resistant
4.11 Gloves: disposable, powderless, vinyl, and latex
4.12 Acid-resistant protective clothing: rubber or poly-laminated tyvek
apron
4.13 Food service towels, or equivalent
4.14 Plastic squirt bottle: 400 ml, for baking soda slurry
4.15 Plastic baskets
4.16 Plastic hand pump suitable for nitric acid
5.0 REAGENTS
5.1 Deionized (Dl) water: used to prepare the acid bath solution
5.2 Concentrated nitric acid (HNO3): ACS reagent grade
5.3 Milli-Q water (Type I water): minimum resistance of
16.67 megohm-cm, or equivalent, used to dilute test samples for
analysis
5.4 Baking soda (sodium bicarbonate): bulk (without any of the
potential target metal analytes as a major contaminant (except
sodium)
5.5 Baking soda slurry: prepare by adding about 50 mL baking soda
(use a 50 mL disposal beaker) to a 500 mL plastic squirt bottle,
then diluting to volume with Dl water
N-2
MRI-QA\ASF-202
-------
Code: ASF-202
Revision: 1
Date: 02/9/93
Page: 3 of 9
5.6 Full range pH paper
5.7 Acationox detergent
6.0 SAFETY REQUIREMENTS
6.1 A Class A fume hood, verified to be in operating condition, must be
used when preparing and using acid bath solutions.
6.2 Safety glasses are required for all work and a face shield is
recommended. Face shields are required for any work involving
transfers of concentrated acid or large volumes (> 4 L) of acid
solutions.
6.3 Neoprene or nrtrile gloves with vinyl or latex glove liners are
required when working with the acid bath or transferring large
volumes of acid solutions.
6.4 Labcoats are required for working with the acid bath. Acid-resistant
protective clothing is required when transferring large volumes of
acid solutions.
6.5 An extra person is required to be present in the laboratory area
when concentrated acid transfers are being performed, in order to
help handle problems in case of inadvertent spills or exposure.
6.6 The closest shower and eye wash station must be noted before
beginning this procedure. They are located in front of the acid bath
hoods.
6.7 A squirt bottle containing'the baking soda slurry and an open box of
baking soda must be in the work area to neutralize spills. The
baking soda slurry is used to neutralize any small spills in the hood
or on clothing. The baking soda in the box is used to neutralize
larger spills.
6.8 When mixing acid solutions, ALWAYS add the acid to the water to
prevent potentially violent reactions. NEVER add water to acid.
6.9 Avoid putting your head and face inside the hood.
N-3
MRI-OA\ASF-202
-------
Code: ASF-202
Revision: 1
Date: 02/9/93
Page: 4 of 9
7.0 ACID BATH PREPARATION PROCEDURE: TANKS AND PIPETTE
CYLINDERS
7.1 Attach a piece of tygon tubing to the Dl water tap and place the
outlet in the bath.
7.2 Fill the acid bath tank with Dl water to the Dl water mark on the
side of the bath (or cylinder).
7.3 Carefully add ACS reagent grade HNO3 to the fill mark on the side
of the tank (or cylinder).
7.4 Stir the clean acid bath mixture with a large stirring rod. NOTE:
The resulting solution is approximately 20% to 30% (v/v) HNO3.
7.5 Record the fill date in the Logbook.
7.6 Screen the contents as described in Section 8.0.
8.0 ACID BATH SCREENING PROCEDURE
Acid baths for glassware preparation are used for cleaning glassware until
the concentration of metallic compounds in the baths rise above specified
levels. The acceptable contamination levels, shown in Table 1, have
been established based on experimental data. These levels are not
expected to result in addition of significant levels of contaminates to
samples prepared using glassware cleaned in the acid baths. This
screening procedure must be performed when the bath is first set up,
whenever it is replenished, approximately once per month with normal
sample preparation and analysis activities, and on an as-needed basis
when sample preparation and analysis activities are reduced.
A given acid bath is screened by performing ICP-AES analysis of a one to
one dilution of an aliquot from the bath followed by comparison to Table 1
levels. The procedure is detailed below.
8.1 Remove a 3-mL to 5-mL aliquot from each acid bath.
8.2 Dilute each aliquot with an equal amount of Milli-Q water for
analysis.
N-4
MRI-OAVASF-202
-------
Code: ASF-202
Revision: 1
Date: 02/9/93
Page: 5 of 9
Table 1. ACCEPTABLE LEVELS OF SELECTED
ANALYTES IN ACID BATHS
Analytes
Hg
Cd, Se, Ag, As, Ba, Cr, Pb, Mn, Sn Zn
Al, Ca, Fe, and Mg
Acceptable level
< 10 u.g/mL
< 25 u.g/mL
< 100 jig/mL
8.3 Analyze the above dilution for the analytes shown in Table 1 by
ICP-AES. NOTE: The acid concentration of the test sample is now
about approximately 10% to 15% (v/v) HNO3.
8.4 Multiply the analysis results by a dilution factor of 2.
8.5 Record the analytical results in the Logbook.
8.6 Compare the results to the criteria shown above in Table 1.
8.7 If the concentration of any analyte is greater than its acceptable
level, label the acid bath: DO NOT USE—ACID MUST BE
CHANGED, discard the bath contents, clean the bath and lids as
described in Section 9.0, and replenish as described in Section 7.0.
If the concentrations are close to but still beneath the acceptable
level, contact the facility manager.
8.8 If the results are exceedingly high, contact the facility manager and
investigate the probable cause, documenting the results of the
investigation in the Logbook.
8.9 If the results are within the acceptable levels and the total volume
levels in the bath are too low for use, add three parts Dl water and
one part concentrated HNO3 until the acid baths are filled to the
original fill mark. Document the addition in the Logbook.
9.0 DISPOSAL
Acid baths which fail to meet acceptable contaminate levels must be
emptied, rinsed and refilled. The acid bath contents are transferred to a
plastic drum identified for acid waste prior to disposal. Two options-
Indirect Pumping and Siphoning—are available for bulk transfer of the acid
to the drum. Direct Pumping is only used for transferring the acid tank
rinsate to the holding tank. Siphoning is presented as an option; however it
N-5
MRI-QA\ASF-202
-------
Code: ASF-202
Revision: 1
Date: 02/9/93
Page: 6 of 9
should be used only when Direct and Indirect Pumping are not possible.
Handling large quantities of acid require the use of a face shield and acid
resistant protective clothing.
9.1 Direct Pumping
Direct pumping of liquid from acid baths is the process of using a plastic
hand pump to transfer the liquid from the bath directly into the plastic drum
identified for acid waste (referred to as "Acid Waste Bulk" drum). A hand
pump is used as opposed to a mechanized pump to increase the operator
control of this transfer and reduce the chances of a spill involving large
volumes. Direct pumping should be used only for transfer of liquid out of
the narrow acid waste tanks located in the ASF acid bath hoods. This is to
reduce the risks of inadvertent contamination of a given acid bath system
caused by insertion of a contaminated plastic hand pump. However, if
required, direct pumping can be used to remove acid from any acid bath.
Under such circumstances, the hand pump should be thoroughly cleaned
and rinsed prior to use. Perform direct pumping as listed below.
9.1.1 Remove the plastic pump from storage and check the pump shaft for
cleanliness using visual inspection. Rinse off any observed
materials which may result in further contamination of the bath using
Dl water.
9.1.2 Place "Acid Waste Bulk" drum within easy reach of the pump tubing.
If the drum is not already connected to venting, remove the venting
bung and secure a venting tube to the drum.
9.1.3 Remove the fill bung of the "Acid Waste Bulk" drum and secure the
plastic flex hose from the plastic pump to the drum. Place the
plastic pump shaft into the tank targeted for emptying and pump the
liquid waste into the drum (see NOTE 1).
NOTE 1: The "Acid Waste Bulk" drum must not be filled
completely full to allow for expansion and contraction during
transport to the disposal site. Prior to pumping acid into the
drum, examine the drum for sufficient space to accommodate
the contents of the acid bath. A dip stick can be used to
check the drum volume level. The "Acid Waste Bulk" drum
final volume should not exceed 90% of the total drum volume.
9.1.4 Upon completion of transfer, pump several volumes of air to assure
no significant volumes of liquid remain in the pump. Remove the
plastic flex hose from the "Acid Waste Bulk" drum and replace the fill
bung. Remove the plastic pump from the acid tank, rinse it, place it
N-6
MHJ-OAVASF-202
-------
Code: ASF-202
Revision: 1
Date: 02/9/93
Page: 7 of 9
in a plastic bag or other suitable plastic container, and store for later
use.
9.1.5 If desired, remove the venting tube from the "Acid Waste Bulk" drum
and replace the bung. Store the "Acid Waste Bulk" drum out of the
way in a area with good ventilation.
9.2 Indirect Pumping
Indirect pumping is the process of using the air-driven pumping system
built into the acid bath hoods to transfer liquids from the acid baths into the
narrow acid waste tank mounted in the hoods. Perform indirect pumping
as described below.
9.2.1 Verify that the pump source piping or tubing is placed into the acid
tank targeted for transfer. If it is not, then affix the pipe or tubing as
needed.
9.2.2 Identify which acid tank number is to be emptied (1, 2, or 3). Use
this number to identify the correct "source valve" located under the
diaphragm pump assembly on the side on the hood.
9.2.3 Open the "water feed" valve for approximately 3 sec to initiate
priming of the diaphragm pump then shut it off.
9.2.4 Open the "source valve" corresponding to the acid tank targeted for
transfer.
9.2.5 Open the "on/off" pump valve (air feed) to start pumping (See Notes
2 and 3).
Open the "water feed" valve again for approximately 3 sec to
complete priming of the diaphragm pump (while the pump is
running) then shut it off.
Monitor the pumping of the acid bath contents into the narrow
acid tank. Take care not to overflow the narrow acid tank by
stopping the pump when the volume reaches about 3/4 of the
total tank volume. Stop the pumping by closing the "on/off"
pump valve (air feed).
NOTE 2: Check the air pressure feeding the "on/off" pump
valve when the pump is running. It should be set to between
10 psi and 25 psi. It is best to operate the pump as slow as
possible to reduce splashing: the lower the pressure, the
N-7
MR1-OA\ASF-202
-------
Code: ASF-202
Revision: 1
Date: 02/9/93
Page: 8 of 9
slower the pumping rate. If the pressure is too low, the pump
will not function.
NOTE 3: If the pump does not operate and the pressure
appears to be sufficiently high, then close the "on/off" pump
valve (air feed), push in the reset button located on the
diaphragm pump, and restart the procedure from the
beginning of Section 9.2.5.
9.2.6 Upon completion of the transfer of liquid from the acid baths to the
narrow acid tank, close the "source valve" corresponding to the acid
bath targeted for transfer.
9.3 Siphoning
Siphoning is the process of transferring acid bath contents using a hose
filled with liquid. This method should only be used when direct or indirect
pumping is not possible. Extra care must be taken when using this method
for liquid transfer to avoid exposure to acid solutions and fumes. Any
siphoning of acid bath contents must be performed with two people to help
reduce the hazards of this type of acid transfer.
An - 1/2-in inner diameter (i.d.) rubber hose of sufficient length is filled with
water, keeping both ends fo the hose at the same level. Close one end
with a clamp (while both ends are level) and place the other end in the
bath. Place the end with the clamp in the narrow acid tank and open the
clamp.
10.0 CLEANING
10.1 Previously used Acid Baths
Acid baths which have been emptied of acidic contents are cleaned prior to
refilling by rinsing with Dl water as described below.
10.1.1 Using a clean food service towel dampened with Dl water,
wipe off the top surface of the acid bath lid (if present) to
remove any foreign materials. Connect a clean tygon hose to
the Dl water tap and spray down the inside walls of the tank
lid into the tank. Rinse a minimum of 3 times using sufficient
Dl water to cover the entire surface area of the lid.
10.1.2 Using the clean tygon hose connected to the Dl water tap,
thoroughly rinse the inside walls of the tank. Use sufficient Dl
water to cover the entire surface area of the walls a minimum
N-8
MHJ-QAVASF-202
-------
Code: ASF-202
Revision: 1
Date: 02/9/93
Page: 9 of 9
of 2 times. Transfer the rinse water into the narrow acid tank
using the procedures described in Section 9 (see NOTE 4).
Indirect pumping with the diaphragm pump should be used as
a first choice.
NOTE 4: Since rinse water from acid baths is not to be
placed into the "Acid Waste Bulk" drum, no liquid other than
rinses must be present in the narrow acid tank. If acid waste
liquid other than rinses are present in the narrow acid tank,
then transfer this liquid into the "Acid Waste Bulk" drum prior
to initiating acid bath cleaning procedures as described in
Section 9.
10.1.3 Repeat the procedure described in 10.1.2 one more time (for
a total of two times).
10.1.4 Prior to disposal, neutralize the acid tank rinse water in the
narrow acid waste tank by adding a slurry of baking soda in
water to the tank combined with mixing using a section PVC
pipe (See Note 5). Use pH paper to monitor the pH during
this neutralization process. Avoid adding excessive quantities
of baking soda. After the pH has been raised to 6 or greater,
empty the contents of the tank by opening the drain valve at
the bottom of the narrow acid tank. Using the clean tygon
hose connected to the Dl water tap, rinse down the inside
walls of the narrow acid tank to remove any nonreacted
baking soda from the tank. Close the drain valve after rinsing
the tank.
NOTE 5: Use of a slurry of baking soda is preferred over use
of powder to avoid excessive sodium contamination of the
acid bath hood areas. Make a slurry in a bucket well
removed from glassware prep areas by mixing approximately
equal amounts of baking soda and Dl water. Use a plastic or
glass stirring rod to mix the slurry.
10.2 New Acid Baths
Acid baths which have never been used for glassware preparation must be
initially cleaned and scrubbed using soap and Dl water. Follow the
General Labware Cleaning Procedure in ASF-201 SOP as close as
possible to prepare new acid baths. After initial cleaning, execute the
rinsing procedures described in Section 10.1 prior to use.
N-9
MHI-QAVASF-202
-------
APPENDIX O
PROTOCOL FOR SAMPLING HOUSEVAC EXHAUST EMISSIONS
Mn-OPFT\R5S-eO.APO
-------
Protocol: Sampling Housevac Exhaust Emissions
Revision No. 1
September 24, 1993
Page 1 of 10
PROTOCOL FOR SAMPLING Housevac EXHAUST EMISSIONS
1.0 INTRODUCTION
Part of the work on this study is directed to testing dust emissions in the air
exhausted from each of the four brands of Housevacs. Dust concentrations and air
flow rates will be determined in each test. There are a total of 12 tests, since each
Housevac will be tested 3 times. One size class « 53 /ym) of test dust will be used
in all tests.
2.O EQUIPMENT AND SUPPLIES
• Turntable for dust feed
• Housevac enclosure and exhaust piping, etc., as shown in Figure O-1.
• Pitot tubes and inclined manometer or magnehelic gauge
• Paniculate concentration monitor
• Strip chart recorder
3.0 PROCEDURE
3.1 Preparations for Testing Each Housevac
• Install new bag in Housevac and run 5 min.
• Remove bag; wait 5 min. then record tare weight of bag. Reinstall tared bag in
Housevac.
• Place Housevac in enclosure. Push suction hose through opening in enclosure.
Seal with duct tape if necessary.
• Insert pitot tube (and T/C) in 2 in. diameter exhaust duct.
• Turn on Housevac, with nozzle positioned well above turntable, and note AP reading
for pitot tube in 2 in. diameter exhaust duct.
MRKJPPT\R3WO-APO
-------
Protocol: Sampling Housevac Exhaust Emissions
Revision No. 1
September 24, 1993
Page 2 of 10
• Lower nozzle toward turntable to determine how close nozzle can be positioned
without affecting pitot reading. Mark this position, and use it in conducting the
tests described below.
• Record temperature and &P reading for pitot tube.
• Shut off Housevac. Calculate total flow rate in duct (see Table O-1).
• Select diameter of sampling nozzle, and/or required sampling rate, to provide
isokinetic sampling for the paniculate concentration monitor (see attached
Table O-2). Adjust sampling rate, then install nozzle at center point of 8 in duct.
• Connect output signal from particulate concentration monitor to strip chart recorder.
• Weigh out 5 g. of sieved dust (<53 jjm size). Distribute dust into shallow trough
on turntable, as evenly as possible over the entire length of the trough circle, except
for 6 inches on each side of the nozzle.
• Position nozzle of Housevac in marked position just above turntable and in the
middle of the section of trough that does not contain dust.
3.2 Conduct Test
3.2.1 Initial Test
• Turn on particulate monitor and strip chart recorder. Mark date, time, and run
number on strip chart. Also, identify each of the following steps on the strip chart,
and times. Record data on data form (Table O-3).
• Turn on Housevac. Run for 1 min.
• Turn on the turntable, mark time when dust pickup begins.
• Continue running for 5 min., which should remove all dust from the turntable
(i.e., one revolution).
• Continue running for 1 min., then stop test.
• Remove bag from Housevac; wait 5 min., then record weight of bag,
M»-OPPT\RS6-90JVPO
-------
Protocol: Sampling Housevac Exhaust Emissions
Revision No. 1
September 24, 1993
Page 3 of 10
3.2.2 Repeat Test
• Install new bag in Housevac and run 5 min.
• Remove bag; wait 5 min. then record tare weight of bag. Reinstall tared bag in
Housevac.
• Weigh out 5 g. of sieved dust « 53 //m), and distribute evenly in trough, as
before.
• Position nozzle above turntable.
• Conduct test as in Section 3.2.1.
• Repeat test a total of 3 times (total of 3 tests using the same Housevac).
MHKJWT\HBWaAPO
-------
Protocol: Sampling Housevac Exhaust Emissions
Revision No. 1
September 24, 1993
Page 4 of 10
Pitot Tube Connected
to Inclined Monometer
Sample Nozzle
4^. Sample to
Continuous
Paniculate
Concentration
Monitor
Support for
Housevac Nozzle
36' Dia Wheel with —,
Shallow Trough
(1/2'Wide)
Near Outer Edge
110V Power
Motor
93-17 SEV QOf son 060893
Figure 0-1. Schematic diagram of test system for dust emissions testing.
M«-OPPT\«»«O.APO
0-4
-------
Protocol: Sampling Housevac Exhaust Emissions
Revision No. 1
September 24, 1993
Page 5 of 10
4.0 COLLECTION OF SAMPLE
It would be desirable to use a research sampling vacuum to sample the exhaust
dust emissions, for Pb analysis. However, it is expected that the dust concentration
will be quite low, precluding this sampling. If preliminary testing indicates that
sampling is feasible (and can be done isokinetically) it will be carried out using the
most appropriate sampler and this protocol will be revised to include that sampling.
5.0 CONTAMINATION AVOIDANCE
For this protocol, contamination refers to the inadvertent increase (or decrease)
in the weight of dust collected in the Housevac bag (other than that applied onto the
turntable). To avoid this, the Housevac must be run only as specified in the protocol,
to avoid "sucking in" any other dust in the vicinity. Care must especially be taken in
removing the bag from the Housevac for weighing, so that none of the collected dust
escapes or is allowed to fall out of the bag.
6.0 DEVIATIONS FROM PROTOCOL
Every attempt shall be made to follow this protocol. Deviations from the
protocol may compromise the data quality and completeness objectives of the project.
Deviations from the protocol will generally fall into two categories: inadvertent
deviations (procedural errors) and deliberate deviations (modifications to the protocol
in response to unusual (or unanticipated conditions).
In the case of inadvertent deviations from the protocol, the sampling team shall
fully document the deviation on the testing data form and immediately notify the team
leader and the MRI work assignment leader. Corrective action(s) shall be taken to
ensure that the situation is not repeated. If possible, any tests affected by the
inadvertent deviation shall be redone in accordance with the specified protocol.
Deliberate deviations from the protocol should be approved in advance with a
signed modification to the QAPjP. If time is critical, preliminary verbal approval may
be granted by EPA. These verbal approvals will be followed up with a signed
modification to the QAPjP. In either case, the sampling team should notify all parties
concerned in a timely manner so that the approval mechanism can be expedited. The
MRI work assignment leader or the task leader is responsible for initiation of the
QAPjP modification and acquiring the necessary approvals.
M«-OPPT\R8MO.APO
-------
L:\9011\901107\rev-1 \tab-o-l .WFW 9/29/93 5:12 PM dr
Protocol: Sampling Housevac Exhaust Emissions
Revision No. 1
Date: September 24, 1993
Page 6 of 10
TABLE O-1
CALCULATION OF AIRFLOW RATE IN 2 IN. DUCT
Step 1 - Measurements
Measure pitot reading at center point, in inches of H20 = A?
Measure temperature in duct in °F = t
Record barometric pressure, in inches of Hg = PJ
Step 2- Calculations
a. Calculate air density in Ib/ft3 = p
P = 1 .325 f ** } Ib/ft3
V460 + t;
b. Calculate velocity in ft/min (at center point)
V = 1,096 — ft/min
V P
c. Calculate average velocity in ft/min
Vavg = (VM0.9) ft/min
d. Calculate airflow rate in acfm =
QE = (Vavg)(0.0218ft2) acfm
Convert airflow rate to acm/min
= Qe(0.0283 m3/ft3) m3/min
Note: Airflow rate in m3/min can be used to calculate dust emission
in mg/min, based on dust concentration measured in mg/m3. This
assumes that dust concentration is measured at the same conditions
of t and PB as gas flow.
0-6
-------
Protocol: Sampling Housevac Exhaust Emissions
Revision No. 1
Date: September 24, 1993
Page 7 of 10
TABLE 0-2
CALCULATION OF NOZZLE SIZE AND SAMPLING RATE NEEDED FOR
ISOKINETIC SAMPLING OF DUST CONCENTRATION
Step 1 - Measurements
Measure pitot reading at center point of 2 in duct, in inches of H20
Measure temperature in duct in °F
Record barometric pressure, in inches of Hg
= t
Step 2 - Calculate velocity in 2 inch duct
density of air in Ib/ft3 = p= 1.325|—^—]
U60 + t;
Should be
about 0.070 Ib/ft3
Ap
velocity in ft/min = \/2 = 1,096 I—
V P
Should be
about 2,800 ft/min
Step 3 - Estimate velocity in 8 inch duct
V8 =
-------
Protocol: Sampling Housevac Exhaust Emissions
Revision No. 1
Date: September 24, 1993
Page 8 of 10
TABLE O-2 (continued)
Step 5 - Determine sampling rate to be used
Determine Vg per Step 3, in ft/min
Record dact (i.e., actual nozzle size in inches)
Let S = sampling rate required in L/min
Vd2
s = _§lVt Should be in the
6-47 range of 2 to 3 L/min
Step 6 - Adjust sampling rate
Adjust the RAM-1 sampling rate to correspond to that determined
above
Adjust the RAM-1 purge rate to 10% of the sampling rate
Shut off the RAM-1, and install sampling nozzle at center point of the
8 in. duct
0-8
-------
Protocol: Sampling Housevac Exhaust Emissions
Revision No. 1
Date: September 24, 1993
Page 9 of 10
TABLE 0-3
DATA FORM FOR HOUSEVAC EMISSION TESTS
Procedures
See attached pages
a. Preparations
Time
Date
Operator _
Housevac
Replicate
Bag tare
weight
(a)
RH
Temp.
(A, B, C, or D)
(Rep 1, 2, or 3)
Bar. Press.
(in. Ha)
2-in. duct pitot reading _
Calculated gas flow rate
Nozzle size selected
Sample rate selected
in. of H20, and temp
acfm
inches
L/min
Dust applied to turntable
Total wt.
(g)
Tare wt.
(g)
Net wt. of
dust (g)
b. Conduct Test (mark times on strip chart)
Operation
Time
Start housevac (run 1 min)
Start turntable and lower
the nozzle to near turntable
1 min
2 min
3 min
4 min
5 min
Stop housevac (run 1 min)
Weioh Baa
Time
Bag final
wt. (a)
2 in. duct
AP rdg.
(in H20)
Paniculate
cone.
(mg/m3)
RH
Temp.
0-9
-------
Protocol: Sampling Housevac Exhaust Emissions
Revision No. 1
Date: September 24, 1993
Page 10 of 10
Project 9802
WA No. 55
Test Identification
Housevac
Substrate
Grind-in
Dust Amount
Pb Cone
Dust Size
Team
Data Entry Sheets
for
Housevac Tests
Test Sequence Number
Date
Operator
(A, B, C or D)
(TILE, LINOIeum, WOOD, UPHOIstery, CaRPeT)
(Yes, No)
(100, 400 mg/ft2
(Low, High)
«53, 53-106, 106-150, 150-212, 212-250. 250-2000)
(number 1 or 2)
Procedure
Perform the tests according to the housevac test sequence in Appendix P, and vac procedure in Appendix I
Tare weigh new bag:
Run free 40 sec, cool 2 min. brush and record weight after 1 more min
Vacuum for 40 sec before any dust deposit
Reweigh bag (cool 2 min, brush and record weight after 1 more min)
Deposit dust, vacuum 40 sec, weigh the bag. Total of 3 times. (Grind-in after each dust deposit, if applicable)
Repeat vacuuming only (vacuum 40 sec, weigh the bag) 3 times
Shake dust from the bag, weigh, prepare for lead analysis
Vacuum dust from wand and brush (no weighing)
Weight of Dust
(Balance # )
Weight of Bag
(Balance #
Tare weight of bag
Vacuum and weigh
Add dust, vac & weigh .2_
Add dust, vac & weigh .3_
Add dust, vac & weigh .4_
Vacuum & weigh .5
Vacuum & weigh .6
Vacuum & weigh .7
Dust sent to lab .8
Total Wt
om.
.0
.1
Tare Wt
om.
NetWt
dm.
Time
Weight
om.
Increase
am.
Bar Code
for Sample
Bar Code
for Blank
Submit one blank for each week
Sample relinquished by
Sample received by
Date of transfer
Reviewed by _
Date reviewed
0-10
-------
APPENDIX P
TEST PATTERNS, HOUSEVACS
-------
Test Pattern, Housevacs
Revision No. 1
Date: September 9,1993
Appendix?
Page 1 of 2
Substrate Particle Size
Linoleum
Linoleum
Linoleum
Linoleum
Wood
Wood
Wood
Wood
Carpet
Carpet
Carpet
Carpet
Carpet
Carpet
Upholstery
Upholstery
Upholstery
Carpet w Grind-in
Carpet w Grind-in
Carpet w Grind-in
Upholstery
Upholstery
Carpet
Linoleum
Linoleum
Linoleum
Carpet
Carpet
Carpet w Grind-in
Linoleum
Linoleum
Linoleum
Upholstery
Upholstery
Carpet
Carpet
Carpet w Grind-in
Wood
Wood
Wood
Wood
Wood
53-106
<53
212-250
106-150
150-212
106-150
150-212
<53
53-106
53-106
53-106
53-106
<53
212-250
<53
<53
212-250
212-250
212-250
<53
53-106
53-106
106-150
212-250
106-150
150-212
<53
212-250
53-106
<53
53-106
250-2000
150-212
150-212
250-2000
150-212
150-212
212-250
106-150
250-2000
53-106
<53
Dust Loading Lead Cone Team vacuum
400 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
100 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
400 mg/sqft
400 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
400 mg/sqft
100 mg/sqft
100 mg/sqft
400 mg/sqft
100 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
100 mg/sqft
400 mg/sqft
100 mg/sqft
400 mg/sqft
100 mg/sqft
High
High
High
Low
High
Low
High
Low
Low
Low
Low
Low
Low
Low
High
High
High
High
High
High
High
High
High
High
Low
Low
Low
Low
High
High
High
High
Low
Low
High
High
Low
Low
Low
High
Low
Low
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
A
D
C
B
A
B
C
D
D
A
C
B
C
D
B
C
B
A
B
D
D
A
A
D
C
B
A
A
C
B
C
' B
B
A
B
D
B
B
D
A
B
C
Original
Number
1001
1002
1003
1004
1005
1006
1007
1008
1009
1010
1011
1012
1013
1014
1020
1085
1088
1052
1101
1104
1030
1032
1046
1026
1027
1056
1015
1083
1069
1075
1076
1095
1042
1044
1065
1119
1038
1079
1080
1111
1058
1077
Revised
Number
1-28
1-10
1-1
1-2
1-3
1-4
1-5
1-6
1-7
1-8
1-9
1-11
1-12
1-13
1-14
1-15
1-16
1-17
1-18
1-19
1-20
1-21
1-22
1-23
1-24
1-25
1-26
1-27
1-29
1-30
p-1
-------
Test Pattern, Housevacs
Revision No. 1
Date: September 9,1993
Appendix?
Page 2 of 2
Substrate Particle Size
Tile
Tile
Tile
Tile
Carpet
Carpet
Carpet
Carpet
Carpet w Grind-in
Carpet w Grind-in
Carpet w Grind-in
Carpet w Grind-in
Linoleum
Linoleum
Carpet w Grind-in
Carpet w Grind-in
Linoleum
Linoleum
Linoleum
Carpet
Upholstery
Wood
Wood
Wood
Carpet w Grind-in
Carpet w Grind-in
Wood
Wood
Wood
Linoleum
Linoleum
Linoleum
Carpet w Grind-in
Carpet w Grind-in
Carpet
Carpet
Upholstery
Upholstery
Upholstery
Upholstery
Carpet
Carpet
Carpet
150-212
212-250
150-212
<53
212-250
<53
<53
212-250
212-250
212-250
<53
<53
53-106
150-212
212-250
<53
250-2000
<53
53-106
53-106
53-106
212-250
53-106
<53
150-212
150-212
106-150
150-212
250-2000
212-250
150-212
106-150
53-106
53-106
212-250
<53
<53
212-250
212-250
150-212
106-150
150-212
250-2000
Dust Loading Lead Cone Team vacuum
100 mg/sqft
400 mg/sqft
100 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
100 mg/sqft
100 mg/sqft
400 mg/sqft
400 mg/sqft
100 mg/sqft
400 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
400 mg/sqft
100 mg/sqft
400 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
400 mg/sqft
400 mg/sqft
100 mg/sqft
400 mg/sqft
100 mg/sqft
100 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
100 mg/sqft
400 mg/sqft
100 mg/sqft
100 mg/sqft
Low
High
Low
High
High
High
High
High
Low
Low
Low
Low
Low
High
Low
Low
Low
Low
Low
High
Low
High
High
High
High
High
High
Low
Low
Low
High
High
Low
Low
High
High
Low
Low ,
Low
High
Low
Low
Low
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
C
B
A
D
C
D
A
B
C
B
D
A
A
B
D
C
C
A
D
C
C
C
A
D
A
C
B
A
D
A
D
A
D
B
D
B
D
C
A
D
C
B
C
Original
Number
2001
2002
2003
2004
2005
2006
2007
2008
2009
2010
2011
2012
2013
2014
2098
2099
2033
2048
2061
2106
2025
2065
2068
2095
2109
2112
2018
2020
2052
2064
2085
2088
2043
2044
2058
2060
2089
2091
2101
2078
2071
2022
2074
Revised
Number
2-1
2-2
2-3
2-4
2-5
2-6
2-7
2-8
2-9
2-10
2-11
2-12
2-13
2-14
2-15
2-16
2-17
2-18
2-19
2-20
2-21
2-22
2-23
2-24
2-25
2-26
2-27
2-28
2-29
2-30
P-2
-------
APPENDIX Q
TEST PATTERN, SAMPLERS
-------
Test Pattern, Samplers
Revision No. 1
Date: September 9,1993
Appendix Q
Page 1 of 2
Substrate
Carpet
Upholstery
Upholstery
Upholstery
Upholstery
Wood
Wood
Carpet
Carpet
Carpet w Grind-in
Carpet w Grind-in
Wood
Linoleum
Wood
Wood
Upholstery
Linoleum
Linoleum
Carpet w Grind-in
Carpet w Grind-in
Linoleum
Linoleum
Linoleum
Wood
Particle
Size
53-106
<53
<53
212-250
150-212
106-150
53-106
150-212
250-2000
53-106
150-212
150-212
106-150
212-250
<53
53-106
250-2000
53-106
212-250
<53
<53
212-250
150-212
250-2000
Dust
Loading
400 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
400 mg/sqft
100 mg/sqft
Lead
Cone
Low
High
High
High
Low
Low
Low
High
High
High
Low
High
Low
Low
Low
High
High
High
High
High
High
High
Low
High
Team
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Teaml
Team 1
Teaml
Teaml
Vacuum
R&MHVS3
CAPS cyclone
Blue nozzle
Blue nozzle
Blue nozzle
R&MHVS3
Blue nozzle
R&MHVS3
Blue nozzle
CAPS cyclone
Blue nozzle
CAPS cyclone
CAPS cyclone
Blue nozzle
CAPS cyclone
R&MHVS3
Blue nozzle
CAPS cyclone
Blue nozzle
R&MHVS3
Blue nozzle
R&MHVS3
Blue nozzle
Baby Wipe
Square
4
2
3
4
3
2
3
1
2
3
1
4
2
1
2
3
1
2
2
3
3
4
4
4
Revised
Number
3-1
3-2
3-3
3-4
3-5
3-6
3-7
3-8
3-9
3-10
3-11
3-12
3-13
3-14
3-15
3-16
3-17
3-18
3-19
3-20
3-21
3-22
3-23
3-24
Q-l
-------
Test Pattern, Samplers
Revision No. 1
Date: September 9,1993
Appendix Q
Page 2 of 2
Substrate
Linoleum
Linoleum
Carpet
Carpet
Carpet
Carpet w Grind-in
Carpet w Grind-in
Linoleum
Upholstery
Upholstery
Upholstery
Carpet w Grind-in
Carpet w Grind-in
Wood
Linoleum
Carpet w Grind-in
Linoleum
Linoleum
Carpet
Carpet
Wood
Wood
Upholstery
Wood
Wood
Wood
Carpet
Particle
Size
212-250
<53
53-106
<53
212-250
<53
212-250
106-150
53-106
<53
212-250
53-106
53-106
150-212
150-212
150-212
250-2000
53-106
250-2000
150-212
<53
212-250
150-212
53-106
106-150
250-2000
106-150
Dust
Loading
400 mg/sqft
400 mg/sqft
100 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
400 mg/sqft
100 mg/sqft
400 mg/sqft
400 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
400 mg/sqft
400 mg/sqft
100 mg/sqft
100 mg/sqft
100 mg/sqft
400 mg/sqft
400 mg/sqft
Lead
Cone
Low
Low
High
High
High
Low
Low
High
Low
Low
Low
Low
Low
Low
High
High
Low
Low
Low
Low
High
High
High
High
High
Low
Low
Team
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Team 2
Vacuum
Baby Wipe
Baby Wipe
CAPS cyclone
Blue nozzle
R&MHVS3
CAPS cyclone
R&MHVS3
Baby Wipe
CAPS cyclone
R&MHVS3
CAPS cyclone
Blue nozzle
R&MHVS3
Baby Wipe
R&MHVS3
CAPS cyclone
CAPS cyclone
R&MHVS3
CAPS cyclone
Blue nozzle
R&MHVS3
CAPS cyclone
R&MHVS3
Baby Wipe
Blue nozzle
R&MHVS3
CAPS cyclone
Square
1
2
1
3
4
1
2
4
4
1
2
1
2
2
1
1
2
3
1
2
2
3
3
2
3
2
3
Revised
Number
4-1
4-2
4-3
4-4
4-5
4-6
4-7
4-8
4-9
4-10
4-11
4-12
4-13
4-14
4-15
4-16
4-17
4-18
4-19
4-20
4-21
4-22
4-23
4-24
4-25
4-26
4-27
0-2
-------
APPENDIX R
PROTOCOL FOR CONDUCTING
TESTS WITH SAMPLERS
-------
Protocol: Conducting Tests with Samplers
Revision No. 1
Date: September 24, 1993
Page 1 of 4
PROTOCOL FOR CONDUCTING
TESTS WITH SAMPLERS
1.0 INTRODUCTION
Many of the tests to be done for this study require sampling with different
types of samplers, each of which involves a specific protocol per Appendices E, F, G
or H. These tests are to be conducted in accordance with the test pattern specified
in Appendix Q, which includes designated "test squares" on each substrate, where
samplers are to be tested (i.e., square 1, 2, 3 or 4). Moreover, the test design
requires vacuuming with Housevac A before the first specified square or after the last
specified square, by either team. Thus, the purpose of this protocol is to define the
procedure that is to be utilized for all sampler tests, in conjunction with the specific
procedures for each sampler in Appendices E, F, G or H.
2.0 EQUIPMENT AND SUPPLIES
Housevac A
Template (1 ft3)
Other equipment listed for each sampler in Appendices E, F, G or H.
3.0 PROCEDURE
3.1 Preparations
• When substrate is first used, mark four 1 ft2 squares within the already marked
Housevac test area.
• Outside the test area, number each square as 1, 2, 3, and 4. (1, 2, and 3 on
carpet and upholstery).
MRK>PPT\FB5-80.APO
R-1
-------
Protocol: Conducting Tests with Samplers
Revision No. 1
Date: September 24, 1993
Page 2 of 4
3.2 CONDUCT TEST
• Record all test data on data entry sheet shown at the end of this appendix.
• Refer to Appendix Q to determine the parameters for the test to be performed,
which includes the sampler to be used and test square to be used.
• If first square:
Tare weigh Housevac bag (run free 40 seconds, cool 2 minutes, brush
and record weight after 1 more minute).
Vac the entire test area for 40 seconds with Housevac A.
Reweigh bag (cool 2 minutes, brush and record weight after 1 more
minute).
• Deposit specified dust within test square, and determine amount deposited.
• Grind in dust, if applicable.
• Sample dust according to protocol for sampler to be tested (Appendices E, F,
G, orH).
• Prepare dust sample for analysis per sampler protocol.
• If the square used for the sampler test was the last square, vacuum the entire
test area with Housevac A after the sampler test:
Tare weigh Housevac bag (run free for 120 seconds, cool 2 minutes,
brush and record weight after 1 more minute).
Vac the entire test area for 120 seconds with Housevac A.
Reweigh bag (cool 2 minutes, brush and record weight after 1 more
minute).
• Vacuum dust from wand and brush of Housevac A (no weighing)
MFB-OPPARM-BO.APD
R-2
-------
Protocol: Conducting Tests with Samplers
Revision No. 1
Date: September 24, 1993
Page 3 of 4
4.0 CONTAMINATION AVOIDANCE
Contamination refers to both the inadvertent increase (or decrease) in the
weight of dust collected by the Housevac or sampler (other than that applied to the
test square) and potential Pb concentration of the sampler dust sample.
Care must be taken to prevacuum only the test square. Also, great care will
be needed to distribute the dust only on the test square, and avoid transfer of dust
to or from other test squares when grind-in of the dust is required.
5.0 DEVIATIONS FROM PROTOCOL
Every attempt shall be made to follow this protocol. Deviations from the
protocol may compromise the data quality and completeness objectives of the project.
Deviations from the protocol will generally fall into two categories: inadvertent
deviations (procedural errors) and deliberate deviations (modifications to the protocol
in response to unusual or unanticipated conditions).
In the case of inadvertent deviations from the protocol, the sampling team shall
fully document the deviation on the sampling data form and immediately notify the
MRI work assignment leader. Corrective action(s) shall be given to ensure that the
situation is not repeated. If possible, any tests or samples affected by the inadvertent
deviation shall be redone in accordance with the specified protocol.
Deliberate deviations from the protocol should be approved in advance with a
signed modification to the QAPjP. If time is critical, preliminary verbal approval may
be granted by EPA. These verbal approvals will be followed up with a signed
modification to the QAPjP. In either case, the sampling team should notify all parties
concerned in a timely manner so that the approval mechanism can be expedited. The
MRI work assignment leader is responsible for initiation of the QAPjP modification and
acquiring the necessary approvals.
M«-OPPT\FBMO.APD
R-3
-------
Project 9802
WA#55
Data Entry Sheets
for
Sampler Tests
Test Identification
Sampler
Substrate
Grind-in
Dust Amount
Pb Cone
Dust Size
Team
Square number
Test Sequence Number
Date
Operator
(Blue Nozzle, CAPS, HVS3 or WIPE)
(TILE, LINOIeum, WOOD, UPHOIstery, CaRPeT)
(Yes. No)
(100, 400 mg/ft2)
(Low, High)
(>53, 53-106, 106-150, 150-212, 212-250, 250-2000)
(Number 1 or 2)
(1, 2, 3 or 4) 1 =first, 3=last for carpet and upholstery, else 4=last)
Procedure
Perform the tests according to the sampler test sequence in Appendix Q, and procedures in Appendix E, F, G or H.
Housevac A will be used to vacuum the first square before sampler tests, or to vacuum the last square after sampler
tests.
If first square:
Tare weigh bag (run free for 40 seconds, cool 2 minutes, brush and record weight after 1 more minute)
Vac square for 40 seconds with Housevac A
Reweigh bag (cool 2 minutes, brush and record weight after 1 more minute)
Deposit dust in specified square and weigh the amount deposited (Grind-in dust if applicable)
Sample dust according to the appropriate protocol, weigh the dust collected (except for wipes)
Prepare the dust sample for analysis
If last square:
Tare weigh bag (run free for 120 seconds, cool 2 minutes, brush and record weight after 1 more minute)
Vac square for 120 seconds with Housevac A
Reweigh bag (cool 2 minutes, brush and record weight after 1 more minute)
Vacuum dust from wand and brush (no weighing)
Weight of Dust
(Balance # )
Weight of Bag
(Balance # )
Initial weight of bag
(if first or last square)
Vacuum and reweigh
bag (if first square)
Dust deposited
Dust collected by
sampler (exclu wipes)
Total Wt.
gm.
.0
.1
.2
Final Wt.
am.
NetWt.
qm.
Time
Weight
qm.
Increase
gm.
.3
Vacuum & reweigh bag 4.
(if last square)
Bar Code
for Sample
Bar Code
for Blank
NOTE: Submit one blank for each sampler, once each week
Sample relinquished by Reviewed by
Sample received by Date reviewed _
Date of transfer
R-4
-------
50272-101
REPORT DOCUMENTATION
PAGE
1. REPORT NO.
EPA 747-R-94-004A
3. Recipients Accession No.
4. Title and subtitle
Laboratory Evaluation of Dust and Dust Lead Recoveries for Samplers and Vacuum
Cleaners; Volume I: Objectives, Methods, and Results
Volume II: Appendices from the Quality Assurance Project Plan
5. Report Date
March 1995
7. Author(s)
Westat, Inc.
8. Performing Organization Rept No.
9. Performing Organization Name and Address
Westat, Inc.
1650 Research Blvd.
Rockville, MD 20850
10. ProJect/TasK/Work Unit No.
11. Contract (C) or Grant (G) No.
(O 68-D3-0011
(C) 68-DO-0137
12. Sponsoring Organization Name and Address
U.S. Environmental Protection Agency
Office of Pollution Prevention and Toxics
Washington, DC 20460
13. Type of Report & Period Covered
Technical Report
14.
15. Supplementary Notes
16. Abstract (Umlt: 200 words)
This document reports the results of a laboratory study to evaluate dust and lead recovery of four house dust sampling
methods used in previous EPA studies and four commercially available household vacuums. The dust sampling methods
included those used in the Baltimore Repair and Maintenance study (BRM), the Comprehensive Abatement Performance
Study (CAPS), the HUD National Survey of Lead-Based Paint (Blue Nozzle sampler), and the HUD's wipe sampling
method. Tho testing protocols used house dust from homes built before 1963 and after 1982, sieved into six particle size
classes ranging from 0 to 2,000 microns and applied to five substrates. Dust from older dwellings had a higher lead
concentration than the dust from newer homes. The BRM and the CAPS samplers produced the highest dust recoveries
across all substrates and particle sizes. The Blue Nozzle sampler had the lowest recoveries. The pattern of lead recovery
across samplers was similar to dust recovery, with the wipe lead recovery similar to that for the CAPS cyclone. Exhaust tests
showed that 0.02% or less of the dust passed through the vacuum cleaner bag. Adjustments to the results from the HUD
National Survey of Lead-Based Paint are also discussed.
17. Document Analysis a. Descriptor*
Environmental Contaminants
b. MenWtore/Open-Ended Terms
Dust lead, regression analysis, National Survey of Lead-Based Paint, dust samplers, vacuum cleaners
c. COSATI Reid/Group
18. Availability Statement
Available to the public from NITS, Springfield, VA
19. Security Class (This Report)
Unclassified
20. Security Class OThls Page)
Unclassified
21. No. of Pages
429
22. Price
(SeeANSt-ZM.18)
OPTIONAL FORM 272 (4-77)
(Formerly NTIS-35)
Department of Commerce
------- |