Professional Documents
Culture Documents
Model 900
BGI 900
HIGH VOLUME CASCADE IMPACTOR
BGI Incorporated
58 Guinan Street
Waltham, MA 02451 USA
Tel : 781 891-9380
Fax: 781 891-8151
www.bgiusa.com
info@bgiusa.com
This Guidance Manual may contain trade secrets and confidential information
proprietary to BGI and HSPH. The documentation and information contained
therein may not be used, duplicated or disclosed to anyone, in whole or in part,
other than as authorized by Agreement and with the express written permission
of BGI.
1
Safety Notice
BGI and its licensed distributors can not foresee all possible modes of
operation in which the user may attempt to utilize this instrument. The user
assumes all liability associated with the use of the instrument. BGI and its
distributors further disclaim any responsibility for consequential damages. Use
of this product in any manner not intended by BGI, the manufacturer, will void
the safety protection provided by the equipment, and may damage the equipment
and subject the user to injury.
2
Warranty (U.S.)
BGI warrants equipment of its manufacture and bearing its nameplate to be free from defects in
workmanship and material. We make no warranty, express or implied, except as set forth herein.
BGI's liability under this warranty extends for a period of one (1) year from the date of BGI's
shipment. It is expressly limited to repairing or replacing at the factory during this period and at
BGI's option, any device or part which shall within one year of delivery to the original purchaser,
be returned to the factory, transportation prepaid and which on examination shall in fact be proved
defective.
BGI assumes no liability for consequential damages of any kind. The purchaser, by acceptance of
this equipment, shall assume all liability for consequences of its misuse by the purchaser, his
employees or others. No information derived from the use of this equipment is warranted for any
purpose whatsoever. This warranty will be void if the equipment is not handled, installed, or
operated in accordance with our instructions. If damage occurs during transportation to the
purchaser, BGI must be notified immediately upon arrival of the equipment. The Equipment will be
returned via collect shipment.
A defective part in the meaning of this warranty shall not, when such part is capable of being
repaired or replaced, constitute a reason for considering the complete equipment defective.
Acknowledgment and approval must be received from BGI prior to returning parts or equipment
for credit. BGI makes engineering changes and improvements from time to time on instruments of
its manufacture. We are under no obligation to retrofit these improvements and/or changes into
instruments which have already been purchased.
No representative of ours has the authority to change or modify this warranty in any respect.
3
Operation Manual Revision List
The latest versions of any BGI manual may be found on our website:
http://www.bgiusa.com/cau/manuals_2005.htm
To assist users of the High Volume Cascade Impactor track the future
changes, the following list of manual sections with its respective revision
number are listed:
(Replaced With)
Model 900 High Volume Cascade Impactor December 2008
4
Section 1. INTRODUCTION
Figure 1-1. High Volume Cascade Impactor System with Mounting Tripod
5
The amount of particulate mass that must be collected on each stage for
certain types of toxicological and chemical speciation sampling ranges from a
milligram (mg) to a gram (g). To collect the amount of mass needed over a short
period of sample event, the High Volume Cascade Impactor is operated at a
designed high sample flow rate of 900.0 Liters/Minute.
Historical filter and impaction methods were not suitable for classifying
particulate matter at high flow rates. For example, filtration methods such as the
Hi Volume Sampler (Hi-Vol), which operates at a flow rate of 1,000
Liters/Minute, require large glass or quartz fiber filters (8x10inches,
20.3x25.4cm). As a result, these collection media also require large quantities of
solvents to recover the collected particulate matter and the weighing analysis is
conducted on an analytical balance rather than a microbalance. This severely
limits the Hi-Vol usefulness for both toxicological and chemical speciation
characterization studies.
In contrast, conventional inertial impactor designs, like the HVCI have the
ability to focus the collected particulate matter onto relatively small surfaces.
These small collection surfaces allow the operator to recover particulate matter
from the impaction substrate surface using relatively small extract volumes of
solvents.
6
The large pores and relatively low overall density characteristic of PUF allows
particles to be collected using the conventional impaction process. Polyurethane
foams produce impaction processes with negligible particulate matter bounce-off
losses because particulate matter can impinge onto the substrate with a possible
gradual decrease of particle velocity. Because of their highly specific surface area,
these substrates present a high-collection capacity and can be used to collect
milligram to gram quantities of particulate matter materials.
The High Volume Cascade Impactor can be used to collect ambient particulate
matter samples for one week or longer (depending on how much particulate matter
pollution exists in the ambient atmosphere) at a design flow rate of 900 l/min,
(31.8 CFM). The impactor cut-points range from 0.17 to 10 µm. Smaller (ultrafine)
particulate matter can be collected on a disk of absolute filter material located
downstream of the final impactor stage.
Figure 1-2. Rain cap, four impactor stages and Polyurethane (PUF) foam
collection substrates.
7
Section 2: Hardware Installation
This section describes the installation of the Model 900 High Volume Cascade
Impactor. This section also covers a number of operational considerations.
Figure 2-1 displays a schematic diagram of the sampler. This figure shows a
configuration of all possible impactor stages followed by an ultrafilter. The key
feature of the High Volume Cascade Impactor (HVCI) sampler is the ability to collect a
large quantity of particulate matter and to classify the material according to particle
size. The available selection of stages have cut points of 10 µm (PUF and grease), 2.5
µm (PUF), 1 µm (PUF), 0.5 µm (PUF), 0.17 µm (PUF). The sampler also has an
optional final-stage ultrafine filter (“ultrafilter”) that collects ultrafine particulate
matter that measure less than 0.1 micrometers.
Figure 2-1. Schematic
drawing of an installation of
the Model 900 sampler.
TOP
COLLECTION
STAGE
PM-10
PM-2.5
PM-1.0 INTERMEDIATE
COLLECTION
PM-0.5 STAGES
PM-0.1
EFFLUENT
BOTTOM AIR
FILTER
COLLECTION
STAGES
BYPASS
TRIPOD AIR
FILTER
PUMP
8
Figure 2-2 lists the actual D50 cut points for each of the HVCI stages. The ultrafine PTFE
coated glass fiber filter stage has > 99% collection efficiency for particulate matter
below 0.1 micron.
PM-2.5 2.5
PM-1.0 1.0
PM-0.5 0.6
PM-0.1 0.17
The HVCI sampler’s design features a circular slit (sectioned into 3 equal arcs)
acceleration platform, with corresponding PUF rings for impaction substrates (Figure 2-
3). The acceleration platforms are mounted in modular cylindrical housings called
“collection stages” (Figure 2-3). The collection stages are stacked in sequence, with
the selected stages in proper order (by descending cut-point sizes) (Figure 2-1). A
removable rain cover is attached to the top stage (Figure 2-4), which always is PM-
10 grease or PM- 10 PUF substrate.
PM-2.5 PUF
Collection
stage
Substrate
holder
9
Figure 2-4. HVCI
Sampler.
• A top collection stage for the PM-10 cut point that has the appropriate
fittings for attaching the rain cover to the system. This stage must contain
the PM-10 (PUF or Silicone Grease) stage.
• A final, bottom collection stage which can be PM- 2.5, 1.0, 0.5, 0.17, or
ultrafine.
10
2.2. D ESCRIPTION OF THE S AMPLING P UMP (Not Supplied by BGI)
The pump for the HVCI system is designed to accommodate a variety of different HVCI
sampler configurations. The pump will pull as much air as mechanically possible. If the
pump draws in excess of the specified 900 l/min, a bypass valve must be mounted on
the pump inlet to increase the pressure drop (Figure 2-6), to maintain the flow at the
desired rate of 900 l/min. The pump should give the user a free air flow amount
capacity above the demand of the system.
11
Figure 2-6. A Typical
bypass valve on the
pump that allows
adjustment of flow rate
to the pump.
When you select a pump, you must choose a system that produces a minimum of 900
Liters/Minute with the final filter in place. The TX40 PTFE coated filter media alone
produces a differential pressure of 24 inches of water (1.8inches of Mercury) at 900
l/min. When choosing a new system, be sure to specify sufficient extra blower pressure
drop for contingencies.
Two different blowers that are recommended by BGI that produce 50 and 150 inches
H2O of column vacuum at 900 l/min. The Gast Pump is recommended for 240 Volt AC
North American operation. The Ritchle Thomas Model SAH95 is recommended for
240Volt use in Europe. The desired flow through the system is 900 l/min ± 5%. Refer to
Section 2.4.5 for further information regarding the pump setup and operation.
Additional hardware will be necessary to make a pump assembly. These include a 1”
heavy wall vacuum hose with connectors to fit the Model 900 1” male pipe thread
and the 2” female Gast pump. The pump manufacturer or industrial supplier should
be able to outfit the pump assembly, including vacuum hose, check filter, bleed
valve, exhaust muffler and electrical switches and breakers to meet local codes.
12
2.3. D ESCRIPTION OF THE PUF S UBSTRATES AND F ILTER M ATERIAL
The HVCI sampler uses polyurethane foam (PUF) as the impaction substrate (Figure
2-7). The PUF substrates use ether-based foam, which is more chemical- and
temperature-resistant than other types of foam. The substrates come in three different
sizes for the PM- 10, PM-2.5, and PM-1 to 0.1 stages. PUF volume and dimensions are
explained in Figure 2-8.
PM- 1.0
PM-0.5 PUF3 4.75 inches 5.25 inches 1
PM-0. 1
13
The ultrafine stage (ultrafilter) (Figure 2-9) uses a PTFE coated Glass Micro-Fiber
filter that traps particulate matter, essentially an absolute filter. These substrates and
filters are available through BGI and are packaged in quantities of 10 (Figure 2-10).
14
2.4. S YS TE M S E TUP
When the sampler is assembled and the clamps are securely tightened, there are no
moving parts to manipulate. With an actual experiment in a specific location, you can
gradually extend the sampling period from one day to multiple days. Be sure to closely
monitor the PUF substrate(s) to prevent too much particulate matter from collecting
on the substrate(s) and ultrafilter. If you allow too much particulate matter to collect on
the substrate(s) and ultrafilter, it may change the cut point of the stage or cause
bounce-off losses (Section 1).
To set up the HVCI sampler, you must determine the number of stages that you want
to use, clean the glassware and other instruments used to prepare the PUF substrates
(Section 2.4.1), prepare the PUF substrates (Section 2.4.2), assemble the collection
stages (Section 2.4.3), install the entire system onto the tripod (Section 2.4.4), and turn
on the pump and adjust its bypass valve (Section 2.4.5).
15
2.4.1. C LEANING THE G LASSWARE AND T OOLS
There are two methods of cleaning the glassware and other instruments that are used
for loading the HVCI sampler and performing the subsequent analysis on the PUF
substrates and ultrafilter. The two methods are thermal cleaning and solvent cleaning.
If you are using Teflon labware, do not use the thermal cleaning technique. The thermal
cleaning technique uses high temperatures that will damage Teflon labware and release
toxic fumes, such as carbonyl fluoride.
2.4.1.1. T H E R M A L C L E A N I N G
You will need two ovens for this procedure: a conventional oven that can reach
temperatures of up to 100° C, and a high-temperature oven that can reach temperatures
of up to 600° C.
NOTE: It is important to wear powder-free gloves at all times. Rinse the gloves
with Milli-Q water and dry the gloves by wiping them with Kimwipes.
1) Wash all glassware and other necessary tools with detergent.
2) Rinse the glassware and tools with distilled water.
3) Rinse the glassware and tools three times with Milli-Q water.
4) Place the glassware and tools in a conventional oven at 100° C
until they are dry.
5) After the glassware and tools are dry, remove from them from the oven
and wrap them with aluminum foil.
6) Place the glassware and tools that are wrapped in aluminum foil into
the high-temperature oven.
7) Set the oven temperature to 450° C.
8) Turn on the high-temperature oven.
9) Bake the glassware and tools in the high-temperature oven for four
hours.
10) Turn off the oven but DO NOT OPEN THE OVEN DOOR.
11) Allow the temperature of the high-temperature oven to drop to
ambient temperature.
12) Open the oven door and remove the glassware and tools.
16
2.4.1.2. S O L V E N T C L E A N I N G
NOTE: It is important to wear powder-free gloves at all times. Rinse the gloves
with Milli-Q water and dry the gloves by wiping them with Kimwipes.
1) Wash all glassware and other necessary tools with detergent.
2) Rinse the glassware and tools with distilled water.
3) Rinse the glassware and tools three times with Milli-Q water.
4) Place the glassware and tools in a conventional oven at 100° C until
they are dry.
5) After the glassware and tools are dry, remove from them from the oven.
6) Place the glassware and tools into a 4000 ml beaker.
7) Add Milli-Q water into the beaker until the water covers the glassware and
tools.
8) Place the beaker into an ultrasonic bath.
9) Place the ultrasonic bath into a positive-flow clean-air hood.
10) Sonicate for 1 hour.
11) Repeat steps 6-10 using hexane instead of Milli-Q water.
12) Repeat steps 6-10 using methanol instead of hexane.
13) Repeat steps 6-10 using dichloromethane instead of methanol.
14) After you have sonicated the glassware and tools using
dichloromethane, place the glassware and tools into a stainless steel
basket.
15) Place the stainless steel basket into the clean air hood until the
glassware and tools are dry.
16) After the glassware and tools are dry, wrap them with clean aluminum foil
to protect them from dust and other contamination during storage.
17
2.4.2. P REPARI NG THE PUF S UBSTR ATES
Prepare the PUF substrates and substrate holders in a laboratory. Be sure to fill the PM-10
grease platform until the grease is level with the top of the rim of the substrate holder.
The PUF platforms only need to have the foam placed into the groove of the substrate
holders. Be sure to line up the holes in the PUF substrates with the holes in the
substrate holders. The PM- 10, PM-2.5, PM-1, PM-0.5 and PM-0. 1 PUF substrates and
their substrate holders (collection platforms) will fit onto the standoffs located on the
acceleration platforms.
18
2.4.2.1. CLEANING THE PUF SUBSTRATES
You must clean the PUF substrates before sampling to remove any trace quantities of
materials that may have collected on the foam during the fabrication process. The
cleaning procedure uses a series of four different solvents (purified water, methanol
(CH3OH), dichloromethane (CH2Cl2), and hexane (C6H14) to ensure that the
extraction process removes materials that are highly polar, slightly polar, and
completely nonpolar. Be sure to use high-grade solvents for the cleaning procedure, and
exercise great care while handling the solvents. Use a fume hood to minimize personal
exposure to the solvents.
Be sure to sonicate only in glassware, because plastic tends to damp the ultrasonic
energy too much. Organic solvents will cause the PUF substrates to swell. This
swelling process will reverse as the PUF substrates dry. When the PUF substrates are
in a swollen condition, they are more fragile than when they are dry.
NOTE: It is important to wear powder-free gloves at all times. Rinse the gloves
with Milli-Q water and dry the gloves by wiping them with Kimwipes.
1) Place the P2 and P3 (Figures 2-8 and 2-9) PUF substrates into the 1000
ml glass beaker. Place the P1 PUF substrate into the 4000 ml
beaker.
2) Add the Milli-Q water to the beaker until it covers the PUF substrates.
3) Place the beaker in the ultrasonic bath.
4) Place the ultrasonic bath in the clean air hood.
5) Son icate for 1 hour.
6) Repeat steps 2-5 using hexane instead of Milli-Q water.
19
11) Leave the stainless steel basket in the clean air hood for 24 hours, or
until the PUF substrates are dry.
12) After the PUF substrates are dry, go to Section 2.4.2.2 (Storing the Clean,
Dry PUF Substrates).
20
2.4.2.2. STORING THE CLEAN, DRY PUF SUBSTRATES
The most important aspect of storing the PUF substrates is to prevent ambient
contamination before the foam is used. Protection from particulate matter contami-
nation is straightforward, but gas-phase contamination requires a container that
prevents diffusion of contaminants. Foil bags prevent both particulate-matter and gas-
phase contamination. Also, the foil bags keep the PUF substrates flat for use. Be sure
to keep the PUF substrates from distorting during the storage process. Estimated shelf
life for cleaned PUF substrates is six months.
NOTE: It is important to wear powder-free gloves at all times. Rinse the gloves
with Milli-Q water and dry the gloves by wiping them with Kimwipes.
1) Clean and dry the PUF substrates (Section 2.4.2.1).
2) While the PUF substrates are still inside the clean-air hood, transfer the
dry PUF substrates to the glass jar(s).
3) Tightly cap each jar.
4) Wrap each jar with aluminum foil (this is necessary to keep out light).
5) Store the wrapped jars in a refrigerator at 4° C.
21
2.4.2.3. CLEANING THE SUBSTRATE HOLDERS
NOTE: It is important to wear powder-free gloves at all times. Rinse the gloves
with Milli-Q water and dry the gloves by wiping them with Kimwipes.
1) Locate the empty substrate holder(s) (Figure 2-11).
2) If you are cleaning new, unused substrate holders, go to step 3. If you are
cleaning previously used substrate holders, go to step 6. If you are
cleaning a previously used PM-10 grease substrate holder, go to step
7.
3) Clean all surfaces of the new, unused substrate holders with
detergent, water and a brush. Go to step 4.
4) Rinse all surfaces of the new, unused substrate holders with
distilled water. Go to step 5.
5) Dry all surfaces of the new, unused substrate holders with
Kimwipes, or other other laboratory tissues. Go to step 10.
6) Clean all surfaces (that come in contact with the PUF substrates) of the
previously used substrate holders using cotton swabs moistened with
Milli-Q water. Go to step 10.
7) Remove the used grease with a Kimwipe. Go to step 8.
8) Wash the PM-10 grease substrate holder with detergent and water.
Go to step 9.
9) Dry all surfaces of the PM-10 grease substrate holder with
Kimwipes, or other other laboratory tissues. Go to step 10.
10) Store the substrate holders in plastic bags to keep them free from dust or
other contamination.
22
2.4.2.4. CLEANING THE ULTRAFINE FILTER HOLDERS
NOTE: It is important to wear powder-free gloves at all times. Rinse the gloves
with Milli-Q water and dry the gloves by wiping them with Kimwipes.
1) Locate the circular plate w/ bar and the screen (Figures 2-12, 2-13 and 2-
14).
23
Figure 2-14. Ultrafine
collection stage with
Ultrafilter highlighted.
2) If you are cleaning a new, unused circular plate w/ bar and screen, go to step 3.
If you are cleaning a previously used bar, circular plate and screen, go to
step 6.
3) Clean all surfaces of the new, unused circular plate w/ bar and screen with
detergent, water and a brush. Go to step 4.
4) Rinse all surfaces of the new, unused circular plate w/ bar and screen with
distilled water. Go to step 5.
5) Dry all surfaces of the new, unused circular plate w/ bar and screen with
Kimwipes, or other other laboratory tissues. Go to step 7.
6) Clean all surfaces (that come in contact with the ultrafine filter) of the previously
used circular plate w/ bar and screen using cotton swabs moistened with
Milli-Q water. Go to step 7.
7) Store the circular plate w/ bar and screen in a plastic bag to keep them
free from dust or other contamination.
24
2.4.2.5. PREPARING THE PM-10 GREASE COLLECTION PLATFORM
NOTE: It is important to wear powder-free gloves at all times. Rinse the gloves
with Milli-Q water and dry the gloves by wiping them with Kimwipes.
1) Clean the PM-10 grease substrate holder (Section 2.4.2.3).
2) Fill the clean substrate holder with fresh grease (Dow Corning silicone
high-vacuum grease).
3) Ensure that the entire volume (except for 0.25 cm at each end of the
cavity) is filled with grease.
4) Using a metal straightedge, ensure that the height of grease is level
with the height of substrate holder. When you fill the substrate holder
with grease, it becomes the “PM-10 grease collection platform.”
5) Place the PM-1 0 grease collection platform into a glass container
(crystallizing dish without a cover, 170 mm [ID] x 90-mm [H]).
6) Wrap the glass container with aluminum foil.
After you have cleaned the PUF substrates and the substrate holders (Section 2.3.2),
you must install the PUF substrates into the substrate holders. When you install a PUF
substrate into a substrate holder, or install grease into the PM- 10 grease substrate
holder (Section 2.4.2.5), the combined assembly becomes a “collection platform.”
After you have prepared the collection platforms, you must install them into the
collection stages. When the collection stages are assembled, you must then assemble
the sampler (Section 2.4.3.2).
25
Figure 2-15. PM-2.5 PUF
collection platform.
6) Ensure that the holes in the PUF substrate line up with the holes in
the substrate holder (Figure 2-16). If you will be using the ultrafine filter
(ultrafilter), go to step 7. If you will not be using the ultrafine filter
(ultrafilter), go to step 12.
26
7) Remove the (4) four screws from the circular plate and remove plate
(Figure 2-17). Go to step 8.
Bar
8) Insert the Ultrafine Filter onto the screen in the circular plate w/ bar. Be
sure to handle the ultrafine filter with the unserrated stainless-steel
forceps (Figure 2-18). Go to step 9.
27
9) Install the circular plate onto the screen (Figure 2-20). Go to step 10
Figure 2-20. Install the
Circular plate onto the
ultrafine filter. Circular
plate
Screen
28
10) Secure the circular plate with the round screws (Figure 2-21). Go to
step 12.
11) Locate the top collection stage with the rain cover (Figure 2-22).
PM-10 PUF
collection platform
Rain
cover
29
12) Install the PM-10 PUF substrate or PM-10 grease collection platform into
the top collection stage (Figures 2-23, 2-24 and 2-25).
30
Figure 2-25. Securing
the PM-10 PUF
collection platform onto
the three standoffs.
(HVCI is inverted)
13) Install the remaining PUF substrate collection platforms into the other
collection stages. Be sure to match the correct size PUF substrate
collection platform with the correct cut-point size impaction platform.
For example, you should install the PM-2.5 PUF collection platform into
a PM-2.5 cut-point size impaction platform.
14) Assemble the individual stages so that the largest cutpoint collection stage
(PM-10 PUF or grease) is installed in the top collection stage, with the
subsequent collection stages possessing smaller cut points installed
underneath each other. For example, if you want to use all six possible
cut point sizes (PM-10, PM-2.5, PM-1.0, PM-0.5, PM-0.1 and the
ultrafilter) the PM-10 collection stage would be the top collection stage,
the PM-2.5 collection stage should be installed below the PM-10 collection
stage, the PM-1.0 collection stage should be installed below the PM-2.5
collection stage, the PM-0.5 collection stage should be installed below
the PM-1.0 collection stage, the PM-0.1 collection stage should be
installed below the PM-0.5 collection stage, and the ultrafilter collection
stage should be installed below the PM-0.1 collection stage (Figure 2-
26).
31
Figure 2-26.
Sampler
assembled.
32
17) Install the sampler base plate onto the bottom collection stage (Figure 2-
28). Go to Section 2.4.4 (Installing the Sampler Onto the Tripod).
33
2.4.4. I NSTALLING THE S AMPLER O NTO THE T RIPOD
1) Determine an appropriate location for the sampler and pump. The HVCI
sampler should be located as far away from the pump’s exhaust as
possible to ensure that the instrument samples a representative sample of air,
and to minimize the potential for contamination.
2) Secure the tripod’s feet with spikes or screws. Spiked feet or
flat feet may be used. The flat feet have 2 holes with knock-outs that
can be used to secure the tripod.
34
4) Install the Model 900 Magnehelic Gage system onto the sampler base
plate. (Figure 2-30).
Figure 2-30. Magnehelic
Gage installed onto the
base plate of the BGI900
35
2.4.5. S ETTING U p THE P UMP
The pump should have a protective filter installed upstream of the blower itself. The
filter will prevent soil and other foreign matter from being drawn into the system if a
hose fitting detaches from the pump during sampling. The pump system (see Figure 2-
1 in section 2.1) must have an adjustable flow valve in-line that allows the operator to
set the flow rate.
The flow rate is set by using a BGI High Volume Calibrator. (The latest manual can
be found here: http://www.bgiusa.com/cau/manuals_2005.htm) A top inlet adaptor
connects to the Model 900 and when the pump is energized the flow rate in CFM is
displayed on the calibrator. The target flow rate is 31.8 CFM (900 Liters/Minute).
Manually adjust the flow valve located just before the pump to set the sample flow
rate at 31.8CFM. The Magnehelic Gauge is a reference of the differential pressure
across the impactor. The gauge will display a number which should be recorded on
the field data sheet as the calibration reference point. You should periodically check
the volumetric flow through the sampler during the pump’s “break-in” period to see
if this calibration reference point changes. Adjust the flow rate valve.
HiVolCal
Calibrator
TOP
PM-10 COLLECTION
STAGE
PM-2.5
PM-1.0 INTERMEDIATE
COLLECTION
PM-0.5 STAGES
PM-0.1
EFFLUENT
BOTTOM AIR
FILTER
COLLECTION
STAGES
BYPASS
TRIPOD AIR
FILTER
PUMP
36
Adjust the bypass valve (Figure 2-31) on the pump to match the
Volumetric Flow Rate reading on the BGI Hi Vol Calibrator
37
Section 3: Post-Sampling Analysis
This section explains how to remove the PUF substrates from the sampler, and
describes the substrate extraction procedures for analysis of water-soluble components
and toxicological testing and the analysis procedures.
After sampling is complete, you must remove the collection platforms from the
collection stages. The collection platform consists of the PUF substrate installed inside
the substrate holder.
38
4) Place the used collection platforms (Figure 3-2) into individual containers
to prevent cross contamination. Label the containers.
5) If you have used an ultrafilter (Figure 3-3), remove it from its retainer
and place it into a suitable container that is labeled. Be sure to handle
the ultrafine filter with the unserrated stainless-steel forceps (Figure
3-4).
39
Figure 3-3. Ultrafilter
installed inside a
collection stage with a
spare ultrafilter.
Ultrafilter installed
in collection stage
Ultrafilter
40
6) Wrap the containers with aluminum foils.
7) Label the outside of the aluminum foil of each container.
8) Store the containers (Section 2) until you are ready to analyze them.
9) Install an unused collection platform into each collection stage.
10) Assemble the sampler and install it onto the tripod (Section 2).
11) Turn on the pump.
41
3.2. SUBSTRATE EXTRACTION FOR ANALYSIS OF W-SATEROLUBLE
COMPONENTS
These extraction procedures are for aqueous extraction of polyurethane foam (PUF)
P1, P2, and P3 substrates and ultrafine filter (ultrafilter). These extracts are suitable for
analysis of water-soluble components. Note that the volumes of the substrate sizes are
not the same and the extraction solvent volume is proportional to each substrate and
filter size (Figure 3-5). Because these materials cannot be wetted directly with water,
methanol is used to wet the surfaces prior to aqueous extraction.
Ultrafilter( 600 ml
ultrafine)
T
Tools and materials required for PUF substrates only:
Ultrasonic bath (large enough to hold racks with culture tubes)
25 ml culture tubes with PTFE-face rubber-lined cap
50 ml culture tubes with PTFE-face rubber-lined cap
240 ml bottle beakers, medium-rounds, wide-mouth with
Teflon PTFE-lined caps
Disposable 1 ml plastic pipettes individually wrapped in paper/plastic
Disposable 10 ml plastic pipettes individually wrapped in paper/plastic
Automated pipette
Tube rack(s) to hold culture tubes (must be plastic-coated or
uncoated metal wire)
Labels for culture tubes
Glass rods
Nonserrated stainless-steel forceps
Stainless-steel scissors
Thermometer
Timer
Watch glass (~ 10 cm diameter)
Milli-Q grade water or equivalent Methanol
42
Tools and materials required for ultrafilters only:
Crystallizing dish (190 mm (diameter) x 100 mm [H])
Straight-sided, round, wide-mouth flasks
1000 ml graduated cylinder
Aluminum foil
Parafilm
3.2.1. L A B W A R E W A S H I N G
43
3.2.2. E XTRACTING PUF S UBSTRATES WITH ILLI M-Q W ATER
NOTE: It is important to wear powder-free gloves at all times. Rinse the gloves
with Milli-Q water and dry the gloves by wiping them with Kimwipes.
1) Hold the P1 PUF substrate with the stainless-steel forceps.
2) Using the stainless-steel scissors, cut off 1/3 piece of the P1 PUF
substrate.
3) Hold the 1/3 piece of the P1 PUF substrate with the stainless-steel
forceps.
4) Using the stainless-steel scissors, cut this 1/3 piece of PUF into 32
pieces. Allow the small pieces to fall onto a watch glass. All of the pieces
should be about the same size. For example, first cut the 1/3 piece in
half, then in quarters, then in eighths, then in sixteenths and finally in
thirty-seconds.
5) Using the stainless-steel forceps, place the 32 PUF pieces into a labeled
culture tube or other suitable glass laboratory vessel. If necessary, use a
glass rod to push the PUF pieces down to the bottom of the extraction
flask.
6) Clean the rod, forceps, scissors and watch glass with Milli-Q grade
water between samples.
7) Add 6 ml of methanol to one flask using the pipette.
8) Place a cap on the flask, then gently shake to evenly wet the PUF pieces
with methanol.
9) Remove the cap and, without delay (to minimize evaporation of
methanol), pipette 120 ml of Milli-Q water into the culture tube (twelve
10 ml aliquots with the 10 ml pipette).
10) Use a clean, dry glass rod to disperse any small air bubbles in the PUF
pieces that float near the top of the aqueous solution.
11) Replace the cap onto the top of the flask.
12) Place the flask (with the PUF pieces) in a rack.
13) Return to the original P1 PUF substrate (that has a 1/3 piece cut out)
and hold it with the stainless-steel forceps.
14) Using the stainless-steel scissors, cut off another 1/3 piece of the P1
PUF substrate.
15) Repeat steps 3-12 for the second 1/3 piece of the P1 PUF substrate.
16) Hold the last remaining 1/3 piece of the original P1 PUF substrate with
the stainless-steel forceps.
17) Repeat steps 2-12 for the remaining 1/3 piece of the P1 PUF substrate.
44
18) Place the rack in the ultrasonic bath.
19) Begin to sonicate the flasks starting with room temperature water.
20) Measure and record the temperature of the water in the ultrasonic bath.
21) Sonicate the flasks for 60 minutes.
22) Check the temperature of the water in the ultrasonic bath periodically. If
the water temperature rises above 30º C, change the water in the
bath to keep the water temperature below 30ºC.
23) C o v e r t h e f l a s k s w i t h P a r a f i l m .
24) Store the covered flasks in a dark refrigerator, prior to analysis.
45
3.2.2.2. PM-2.5 PUF S UBSTRATE (P2 S IZE)
NOTE: It is important to wear powder-free gloves at all times. Rinse the gloves
with Milli-Q water and dry the gloves by wiping them with Kimwipes.
1) Hold the P2 PUF substrate with the stainless-steel forceps.
2) Using the stainless-steel scissors, cut off 1/3 piece of the P2 PUF
substrate.
3) Hold the 1/3 piece of the P2 PUF substrate with the stainless-steel
forceps.
4) Using the stainless-steel scissors, cut this 1/3 piece of PUF into 16
pieces. Allow the small pieces to fall onto a watch glass. All of the pieces
should be about the same size. For example, first cut the 1/3 piece in
half, then in quarters, then in eighths, and finally in sixteenths.
5) Using the stainless-steel forceps, place the 16 PUF pieces into a labeled,
50 ml culture tube or other suitable glass laboratory vessel. If
necessary, use a glass rod to push the PUF pieces down to the
bottom of the extraction flask.
6) Clean the rod, forceps, scissors and watch glass with Milli-Q grade
water between samples.
7) Add 2 ml of methanol to one flask using two 1 ml pipettes.
8) Place a cap on the flask, then gently shake to evenly wet the PUF pieces
with methanol.
9) Remove the cap and, without delay (to minimize evaporation of
methanol), pipette 40 ml of Milli-Q water into the culture tube (four
10 ml aliquots with the 10 ml pipette).
10) Use a clean, dry glass rod to disperse any small air bubbles in the PUF
pieces that float near the top of the aqueous solution.
11) Replace the cap onto the top of the flask.
12) Place the flask (with the PUF pieces) in a rack.
13) Return to the original P2 PUF substrate (that has a 1/3 piece cut out)
and hold it with the stainless-steel forceps.
14) Using the stainless-steel scissors, cut off another 1/3 piece of the P2
PUF substrate.
15) Repeat steps 3-12 for the second 1/3 piece of the P2 PUF substrate.
16) Hold the last remaining 1/3 piece of the original P2 PUF substrate with
the stainless-steel forceps.
17) Repeat steps 2-12 for the remaining 1/3 piece of the P2 PUF substrate.
18) Place the rack in the ultrasonic bath.
19) Begin to sonicate the flasks starting with room temperature water.
20) Measure and record the temperature of the water in the ultrasonic bath.
46
21) Sonicate the flasks for 60 minutes.
22) Check the temperature of the water in the ultrasonic bath periodically. If
the water temperature rises above 30º C, change the water in the
bath to keep the water temperature below 30ºC.
23) Cover the flasks with Parafilm.
24) Store the covered flasks in a dark refrigerator, prior to analysis.
47
3.2.2.3. PM-1.0, PM-0.5 AND PM-0.1 PUF S UBSTRATE (P3 S IZE)
NOTE: It is important to wear powder-free gloves at all times. Rinse the gloves
with Milli-Q water and dry the gloves by wiping them with Kimwipes.
1) Hold the P3 PUF substrate with the stainless-steel forceps.
2) Using the stainless-steel scissors, cut off 1/3 piece of the P3 PUF
substrate.
3) Hold the 1/3 piece of the P3 PUF substrate with the stainless-steel
forceps.
4) Using the stainless-steel scissors, cut this 1/3 piece of PUF into 8 pieces.
Allow the small pieces to fall onto a watch glass. All of the pieces
should be about the same size. For example, first cut the 1/3 piece in
half, then in quarters, and finally in eighths.
5) Using the stainless-steel forceps, place the 16 PUF pieces into a labeled,
25 ml culture tube or other suitable glass laboratory vessel. If
necessary, use a glass rod to push the PUF pieces down to the
bottom of the extraction flask.
6) Clean the rod, forceps, scissors and watch glass with Milli-Q grade
water between samples.
7) Add 1 ml of methanol to one flask using a 1 ml pipette.
8) Place a cap on the flask, then gently shake to evenly wet the PUF pieces
with methanol.
9) Remove the cap and, without delay (to minimize evaporation of methanol),
pipette 20 ml of Milli-Q water into the culture tube (two 10 ml aliquots
with the 10 ml pipette).
10) Use a clean, dry glass rod to disperse any small air bubbles in the PUF
pieces that float near the top of the aqueous solution.
11) Replace the cap onto the top of the flask.
12) Place the flask (with the PUF pieces) in a rack.
13) Return to the original P3 PUF substrate (that has a 1/3 piece cut out)
and hold it with the stainless-steel forceps.
14) Using the stainless-steel scissors, cut off another 1/3 piece of the P3
PUF substrate.
15) Repeat steps 3-12 for the second 1/3 piece of the P3 PUF substrate.
48
16) Hold the last remaining 1/3 piece of the original P3 PUF substrate with
the stainless-steel forceps.
17) Repeat steps 2-12 for the remaining 1/3 piece of the P3 PUF substrate.
18) Place the rack in the ultrasonic bath.
19) Begin to sonicate the flasks starting with room temperature water.
20) Measure and record the temperature of the water in the ultrasonic bath.
21) Sonicate the flasks for 60 minutes.
22) Check the temperature of the water in the ultrasonic bath periodically. If
the water temperature rises above 30º C, change the water in the
bath to keep the water temperature below 30ºC.
23) C o v e r t h e f l a s k s w i t h P a r a f i l m .
24) Store the covered flasks in a dark refrigerator, prior to analysis.
49
3.2.2.4. ULTRAFINE FILTER (ULTRAFILTER)
NOTE: It is important to wear powder-free gloves at all times. Rinse the gloves
with Milli-Q water and dry the gloves by wiping them with Kimwipes.
1) Place the ultrafine filter inside the 190 mm crystallizing dish.
2) Hold the ultrafine filter with the stainless-steel forceps.
3) Using the stainless-steel scissors, cut the entire ultrafine filter into
small pieces (about 2 cm square).
4) Place the small pieces of cut-up ultrafine filter into a straight-sided
round flask.
5) Pipette 30 ml of methanol into the flask.
6) Without delay, to minimize evaporation of methanol, gently shake the
flask to evenly wet the filter pieces with methanol.
7) Using the 1000 ml-graduated cylinder, immediately add 600 ml of Milli-Q
water to the flask.
8) Cover the flask with a small piece of aluminum foil.
9) Place the flask directly into the water of the ultrasonic bath.
10) Begin to sonicate the flask starting with room temperature water.
11) Measure and record the temperature of the water in the ultrasonic bath.
21) Sonicate the flask for 60 minutes.
22) Check the temperature of the water in the ultrasonic bath periodically. If
the water temperature rises above 30º C, change the water in the
bath to keep the water temperature below 30ºC.
23) Cover the flask with Parafilm.
24) Store the covered flask in a dark refrigerator, prior to analysis.
50
3.3. S UBSTRATE E XTRACTION FOR T OXICOLOGICAL T ESTING
These extraction procedures are for solvent extraction of polyurethane foam (PUF)
P1, P2, and P3 substrates and ultrafine filters (ultrafilter). These extracts are suitable
for analysis of water-soluble components. Note that the volumes of the substrate sizes
are not the same and the extraction solvent volume is proportional to each substrate
and filter size (Figure 3-4).
51
3.3.1. L A B W A R E W A S H I N G
52
3.3.2. E XTRACTING PUF S UBSTRATES WITH M ETHANOL
NOTE: It is important to wear powder-free gloves at all times. Rinse the gloves
with Milli-Q water and dry the gloves by wiping them with Kimwipes.
1) Hold the P1 PUF substrate with the stainless-steel forceps.
2) Using the stainless-steel scissors, cut off 1/3 piece of the P1 PUF
substrate.
3) Hold the 1/3 piece of the P1 PUF substrate with the stainless-steel
forceps.
4) Using the stainless-steel scissors, cut this 1/3 piece of PUF into 32
pieces. Allow the small pieces to fall onto a watch glass. All of the pieces
should be about the same size. For example, first cut the 1/3 piece in
half, then in quarters, then in eighths, then in sixteenths and finally in
thirty-seconds.
5) Using the stainless-steel forceps, place the 32 PUF pieces into a 250
ml extraction flask. If necessary, use a glass rod to push the PUF pieces
down to the bottom of the extraction flask.
6) Clean the rod, forceps, scissors and watch glass with Milli-Q grade
water between samples.
7) Add 15 ml of methanol to the flask using the automatic pipette and a
10 ml pipette.
8) Place a cap on the flask, then gently shake to evenly wet the PUF pieces
with methanol.
9) Place the flask (with the PUF pieces) in a rack.
10) Return to the original P1 PUF substrate (that has a 1/3 piece cut out)
and hold it with the stainless-steel forceps.
11) Using the stainless-steel scissors, cut off another 1/3 piece of the P3
PUF substrate.
12) Repeat steps 3-9 for the second 1/3 piece of the P3 PUF substrate.
13) Hold the last remaining 1/3 piece of the original P3 PUF substrate with
the stainless-steel forceps.
14) Repeat steps 2-9 for the remaining 1/3 piece of the P3 PUF substrate.
15) Place the rack in the ultrasonic bath.
16) Begin to sonicate the flasks starting with room temperature water.
17) Measure and record the temperature of the water in the ultrasonic bath.
18) Sonicate the flasks for 60 minutes.
19) Check the temperature of the water in the ultrasonic bath periodically. If
the water temperature rises above 30º C, change the water in the
53
20) Use a 10 ml pipette to transfer the methanol extracts from the
extraction tubes to labeled 40 ml evaporation tubes.
21) Cap the extraction tubes and evaporation tubes except during
transfers.
22) Transfer as much extract from each tube as is conveniently possible.
23) Record the approximate amount of solvent transferred using the 10
ml pipette.
24) Add 10 ml of fresh methanol to each extraction tube.
25) Place the extraction tubes in a rack.
26) Repeat steps 15-19.
27) Repeat steps 20-23.
28) Add 10 ml of fresh methanol to each extraction tube.
29) Place the extraction tubes in a rack.
30) Repeat steps 15-19.
31) Repeat steps 20-23. The approximate overall efficiency of extraction
can be calculated using measured amounts of methanol added and
approximate amounts of extract transferred for each of the three
extractions. For example, you started with 15 ml for original extraction,
transferred most to evaporation tube, added 10 ml to the extraction
tubes, sonicated, and transferred most to the evaporation tubes,
added second 10 ml to extraction tubes, son icated, and transferred
most of the extract to the evaporation tube.
54
3.3.2.2. PM-2.5 PUF S UBSTRATE (P2 S IZE)
NOTE: It is important to wear powder-free gloves at all times. Rinse the gloves
with Milli-Q water and dry the gloves by wiping them with Kimwipes.
1) Hold the P2 PUF substrate with the stainless-steel forceps.
2) Using the stainless-steel scissors, cut off 1/3 piece of the P2 PUF
substrate.
3) Hold the 1/3 piece of the P2 PUF substrate with the stainless-steel
forceps.
4) Using the stainless-steel scissors, cut this 1/3 piece of PUF into 16
pieces. Allow the small pieces to fall onto a watch glass. All of the pieces
should be about the same size. For example, first cut the 1/3 piece in
half, then in quarters, then in eighths, and finally in sixteenths.
5) Using the stainless-steel forceps, place the 16 PUF pieces into a
labeled, 50 ml culture tube or other suitable glass laboratory vessel. If
necessary, use a glass rod to push the PUF pieces down to the
bottom of the extraction flask.
5) Using the stainless-steel forceps, place the 16 PUF pieces into a 250
ml extraction flask. If necessary, use a glass rod to push the PUF pieces
down to the bottom of the extraction flask.
6) Clean the rod, forceps, scissors and watch glass with Milli-Q grade
water between samples.
7) Add 15 ml of methanol to the flask using the automatic pipette and a
10 ml pipette.
8) Place a cap on the flask, then gently shake to evenly wet the PUF pieces
with methanol.
9) Place the flask (with the PUF pieces) in a rack.
10) Return to the original P2 PUF substrate (that has a 1/3 piece cut out)
and hold it with the stainless-steel forceps.
11) Using the stainless-steel scissors, cut off another 1/3 piece of the P3
PUF substrate.
12) Repeat steps 3-9 for the second 1/3 piece of the P3 PUF substrate.
13) Hold the last remaining 1/3 piece of the original P3 PUF substrate with
the stainless-steel forceps.
14) Repeat steps 2-9 for the remaining 1/3 piece of the P3 PUF substrate.
15) Place the rack in the ultrasonic bath.
16) Begin to sonicate the flasks starting with room temperature water.
17) Measure and record the temperature of the water in the ultrasonic bath.
18) Sonicate the flasks for 60 minutes.
19) Check the temperature of the water in the ultrasonic bath periodically. If
55
the water temperature rises above 30º C, change the water in the
bath to keep the water temperature below 30ºC.
20) Use a 10 ml pipette to transfer the methanol extracts from the
extraction tubes to labeled 40 ml evaporation tubes.
21) Cap the extraction tubes and evaporation tubes except during
transfers.
22) Transfer as much extract from each tube as is conveniently possible.
23) Record the approximate amount of solvent transferred using the 10
ml pipette.
24) Add 10 ml of fresh methanol to each extraction tube.
25) Place the extraction tubes in a rack.
26) Repeat steps 15-19.
27) Repeat steps 20-23.
28) Add 10 ml of fresh methanol to each extraction tube.
29) Place the extraction tubes in a rack.
30) Repeat steps 15-19.
31) Repeat steps 20-23. The approximate overall efficiency of extraction can
be calculated using measured amounts of methanol added and
approximate amounts of extract transferred for each of the three
extractions. For example, you started with 15 ml for original extraction,
transferred most to evaporation tube, added 10 ml to the extraction
tubes, sonicated, and transferred most to the evaporation tubes,
added second 10 ml to extraction tubes, son icated, and transferred
most of the extract to the evaporation tube.
56
3.3.2.3. PM-1.0, PM-0.5 AND PM-0.1 PUF S UBSTRATE (P3 S IZE)
NOTE: It is important to wear powder-free gloves at all times. Rinse the gloves
with Milli-Q water and dry the gloves by wiping them with Kimwipes.
1) Hold the P3 PUF substrate with the stainless-steel forceps.
2) Using the stainless-steel scissors, cut off 1/3 piece of the P3 PUF
substrate.
3) Hold the 1/3 piece of the P3 PUF substrate with the stainless-steel
forceps.
4) Using the stainless-steel scissors, cut this 1/3 piece of PUF into 8 pieces.
Allow the small pieces to fall onto a watch glass. All of the pieces
should be about the same size. For example, first cut the 1/3 piece in
half, then in quarters, and finally in eighths.
5) Using the stainless-steel forceps, place the 8 PUF pieces into a
labeled, 50 ml culture tube or other suitable glass laboratory vessel.
If necessary, use a glass rod to push the PUF pieces down to the
bottom of the extraction flask.
5) Using the stainless-steel forceps, place the 8 PUF pieces into a 250 ml
extraction flask. If necessary, use a glass rod to push the PUF pieces
down to the bottom of the extraction flask.
6) Clean the rod, forceps, scissors and watch glass with Milli-Q grade
water between samples.
7) Add 15 ml of methanol to the flask using the automatic pipette and a
10 ml pipette.
8) Place a cap on the flask, then gently shake to evenly wet the PUF pieces
with methanol.
9) Place the flask (with the PUF pieces) in a rack.
10) Return to the original P3 PUF substrate (that has a 1/3 piece cut out)
and hold it with the stainless-steel forceps.
11) Using the stainless-steel scissors, cut off another 1/3 piece of the P3
PUF substrate.
12) Repeat steps 3-9 for the second 1/3 piece of the P3 PUF substrate.
13) Hold the last remaining 1/3 piece of the original P3 PUF substrate with
the stainless-steel forceps.
14) Repeat steps 2-9 for the remaining 1/3 piece of the P3 PUF substrate.
15) Place the rack in the ultrasonic bath.
16) Begin to sonicate the flasks starting with room temperature water.
17) Measure and record the temperature of the water in the ultrasonic bath.
18) Sonicate the flasks for 60 minutes.
19) Check the temperature of the water in the ultrasonic bath periodically. If
57
the water temperature rises above 30º C, change the water in the
bath to keep the water temperature below 30ºC.
20) Use a 10 ml pipette to transfer the methanol extracts from the
extraction tubes to labeled 40 ml evaporation tubes.
21) Cap the extraction tubes and evaporation tubes except during
transfers.
22) Transfer as much extract from each tube as is conveniently possible.
23) Record the approximate amount of solvent transferred using the 10
ml pipette.
24) Add 10 ml of fresh methanol to each extraction tube.
25) Place the extraction tubes in a rack.
26) Repeat steps 15-19.
27) Repeat steps 20-23.
28) Add 10 ml of fresh methanol to each extraction tube.
29) Place the extraction tubes in a rack.
30) Repeat steps 15-19.
31) Repeat steps 20-23. The approximate overall efficiency of extraction can
be calculated using measured amounts of methanol added and
approximate amounts of extract transferred for each of the three
extractions. For example, you started with 15 ml for original extraction,
transferred most to evaporation tube, added 10 ml to the extraction
tubes, sonicated, and transferred most to the evaporation tubes,
added second 10 ml to extraction tubes, son icated, and transferred
most of the extract to the evaporation tube.
58
3.3.3. E VAPORATION OF S OLVENT FROM PUF E XTRACTS
NOTE: It is important to wear powder-free gloves at all times. Rinse the gloves
with Milli-Q water and dry the gloves by wiping them with Kimwipes.
1) Remove the caps from as many evaporation tubes as will fit into the
evaporator.
2) Place the evaporation tubes into the evaporator. If the evaporator has a
provision for the use of a water bath, maintain the bath temperature at
30° C.
3) Place clean Pasteur pipettes in the evaporator.
4) Cover the opening of each evaporation tube with a piece of aluminum foil.
5) Open the valves of the pipettes and bring the tip of each pipette close to
the solvent surface (inside the evaporation tubes) until there is a very
slight indenture in the surface due to the gas flow.
6) As the methanol evaporates, add fresh methanol to wash the walls
of the evaporation tubes.
7) Evaporate until the volume in the evaporation tubes is less than 3 ml.
8) Remove the evaporation tubes from the evaporator.
9) Cap each evaporation tube until you are ready to transfer the
concentrated extract to the storage tubes.
Transfer of extract to the storage tubes
10) Use a clean Pasteur pipette to transfer the concentrated extract from
the evaporation tubes to preweighed, labeled storage tubes. Be sure to
weigh the storage tubes with their caps on. The cap used for weighing
must be identifiable to make sure that the same cap is used for
post-weighing of each tube.
11) Replace the caps on the evaporation tubes until you are ready to rinse
them into the storage tubes.
12) Replace the caps on the storage tubes until you are ready to
evaporate the concentrated extract.
13) Remove the caps from as many storage tubes as will fit into the
evaporator.
59
14) Place the storage tubes in the evaporator.
15) Evaporate most of the concentrated extract in the storage tubes. First
rinse of the evaporation tubes
16) Using a 1 ml pipette, add 0.5 ml of fresh methanol to rinse the
evaporation tubes.
17) Transfer this first 0.5 ml rinse of the evaporation tubes to the storage
tubes.
18) Repeat steps 4-8.
19) Evaporate most of the concentrated extract in the storage tubes.
Second rinse of the evaporation tubes
20) Using a 1 ml pipette, add another 0.5 ml of fresh methanol to rinse the
evaporation tubes a second time.
21) Transfer this second 0.5 ml rinse of the evaporation tubes to the storage
tubes.
22) Repeat steps 4-8.
23) Evaporate most of the concentrated extract in the storage tube. Third
rinse of the evaporation tubes
24) Using a 1 ml pipette, add another 0.5 ml of fresh methanol to rinse the
evaporation tubes a third time.
25) Transfer this third 0.5 ml rinse of the evaporation tubes to the storage
tubes.
26) Repeat steps 4-8.
27) Evaporate the concentrated extract until it is dry.
28) Replace the caps on the storage tubes. Ensure that each cap corresponds
to the original pre-weighing of each storage tube.
29) Weigh each storage tube and record its weight.
30) Calculate the weight of the extract by subtracting the original weight of
the storage tube from the final weight of the storage tube. Repeat this
for each storage tube and record all values.
31) Place the storage tubes in a freezer at -20° C until you are ready to begin
the toxicological analysis (Section 3.4).
60
3.3.4. E XTRACTING U LTRAFILTER F ILTERS WITH M ETHANOL
NOTE: It is important to wear powder-free gloves at all times. Rinse the gloves
with Milli-Q water and dry the gloves by wiping them with Kimwipes.
1) Place the ultrafine filter inside the 190 mm crystallizing dish.
2) Hold the ultrafine filter with the stainless-steel forceps.
3) Using the stainless-steel scissors, cut the entire ultrafine filter into
small pieces (about 2 cm square).
4) Place the small pieces of cut-up ultrafine filter into a 250 ml Erlenmeyer
(“extraction”) flask.
5) Using the graduated cylinder, add 120 ml of methanol into the
extraction flask.
6) Use a small piece of aluminum foil to cover the flask.
7) Place the flask directly into the water of the ultrasonic bath.
8) Begin to sonicate the flask starting with room temperature water.
9) Measure and record the temperature of the water in the ultrasonic bath.
10) Sonicate the flask for 60 minutes.
11) Check the temperature of the water in the ultrasonic bath periodically. If
the water temperature rises above 30º C, change the water in the
bath to keep the water temperature below 30ºC.
12) Pour this first methanol extract from the original extraction flask into
another clean 500 ml Erlenmeyer (“storage”) flask.
13) Add an additional 120 ml of fresh methanol to the original extraction
flask.
14) Use a small piece of aluminum foil to cover the original extraction flask.
15) Place the original extraction flask directly into the water of the
ultrasonic bath.
16) Repeat steps 8-11.
17) Pour the second methanol extract into the same storage flask used in
step 12.
61
18) Add an additional 120 ml of fresh methanol to the original extraction
flask.
19) Use a small piece of aluminum foil to cover the original extraction flask.
20) Place the original extraction flask directly into the water of the
ultrasonic bath.
21) Repeat steps 8-11.
22) Pour the third methanol extract into the same storage flask used in
step 12.
23) Cap the 500 ml Erlenmeyer storage flasks containing the extracts until
you are ready to begin the evaporation procedure (Section 3.3.5).
Note that the total amount of methanol retained by the ultrafine filter is about 30 ml.
Thus the first aliquot of methanol transferred from the extraction flask contains about
75% (90/120) of the material dissolved in the solvent. The second aliquot of methanol
transferred from the extraction flask contains about 80% (120/150) of the remaining
material (25%). The third aliquot transferred contains about 80% (120/150) of the
remaining material (5%). Therefore, the total fraction transferred from the extraction
flask is about (75 + 0.8(25) + 0.8(5))% = 99%.
62
3.3.5. E VAPORATION OF S OLVENT FROM U LTRAFINE E XTRACTS
NOTE: It is important to wear powder-free gloves at all times. Rinse the gloves
with Milli-Q water and dry the gloves by wiping them with Kimwipes.
1) Determine the maximum number (N) of evaporation tubes that can be
used simultaneously with the evaporator.
2) Remove the caps of the evaporation tubes. Transfer
of extract to each of the “N” evaporation tubes
3) Using a pipette, transfer 35 ml of extract from the storage flask to each of
the “N” evaporation tubes.
4) Place the evaporation tubes into the evaporator. If the evaporator has a
provision for the use of a water bath, maintain the bath temperature at
30° C.
5) Place clean Pasteur pipettes in the evaporator.
6) Cover the opening of each evaporation tube with a piece of aluminum foil.
7) Open the valves of the pipettes and bring the tip of each pipette close to
the solvent surface (inside the evaporation tubes) until there is a very
slight indenture in the surface due to the gas flow.
8) As the methanol evaporates, add fresh methanol to wash the walls
of the evaporation tubes.
9) Continue transferring until all the extract has been removed from the
storage flask (step 3).
First rinse of the storage flask
10) After all of the extract has been removed from the storage flask, add 25
ml of fresh methanol to rinse the storage flask.
11) Transfer 35 ml of the first rinse (using a pipette) from the storage flask to
each of the “N” evaporation tubes.
12) Repeat steps 4-8.
13) Continue transferring until all the first rinse has been removed from the
storage flask (step 3).
63
Second rinse of the storage flask
14) After all of the first rinse has been removed from the storage flask,
add 25 ml of fresh methanol to rinse the storage flask a second time.
15) Transfer 35 ml of the second rinse (using a pipette) from the
storage flask to each of the “N” evaporation tubes.
16) Repeat steps 4-8.
17) Continue transferring until all the second rinse has been removed from
the storage flask (step 3).
18) Evaporate until volume is less than 3 ml.
Transfer of extract to “Tube A” and “Tube B”
19) Using a pipette, transfer all of the remaining extract from the “N”
evaporation tubes to only two of the evaporation tubes (“Tube A” and
“Tube B”).
20) Repeat steps 4-8.
21) Evaporate the extract in Tube A and Tube B until the volume is less
than 3 ml in each tube.
First rinse of the “N” evaporation tubes
22) Using a 1 ml pipette, add 1 ml of fresh methanol to rinse the other “N”
evaporation tubes.
23) Transfer this first 1 ml rinse of the other “N” evaporation tubes to Tube A
and Tube B (step 19).
24) Repeat steps 4-8.
25) Evaporate the first 1 ml rinse until the volume is less than 3 ml in each
tube.
Second rinse of the “N” evaporation tubes
26) Using a 1 ml pipette, add another 1 ml of fresh methanol to rinse the
other “N”evaporation tubes a second time.
27) Transfer this second 1 ml rinse of the other “N” evaporation tubes to
Tube A and Tube B (step 19).
28) Repeat steps 4-8.
29) Evaporate the second 1 ml rinse until the volume is less than 3 ml in
each tube.
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Third rinse of the “N” evaporation tubes
30) Using a 1 ml pipette, add another 1 ml of fresh methanol to rinse the
other “N” evaporation tubes a third time.
31) Transfer this third 1 ml rinse of the other “N” evaporation tubes to Tube A
and Tube B (step 19).
32) Repeat steps 4-8.
33) Evaporate the third 1 ml rinse until the volume is less than 3 ml in each
tube.
Transfer of extract to “Tube B”
34) Using a pipette, transfer the extract from one of the two remaining
evaporation tubes (Tube A) to the other evaporation tube (Tube B).
35) Repeat steps 4-8.
36) Evaporate the extract in Tube B until the volume is less than 3 ml. First
rinse of “Tube A”
37) Using a 1 ml pipette, add 1 ml of fresh methanol to rinse Tube A.
38) Transfer this first 1 ml rinse of Tube A to Tube B.
39) Repeat steps 4-8.
40) Evaporate the first 1 ml rinse until the volume is less than 3 ml in Tube B.
Second rinse of “Tube A”
41) Using a 1 ml pipette, add another 1 ml of fresh methanol to rinse Tube A
a second time.
42) Transfer this second 1 ml rinse of Tube A to Tube B.
43) Repeat steps 4-8.
44) Evaporate the second 1 ml rinse until the volume is less than 3 ml in
Tube B.
Third rinse of “Tube A”
45) Using a 1 ml pipette, add another 1 ml of fresh methanol to rinse Tube A
a third time.
46) Transfer this third 1 ml rinse of Tube A to Tube B.
47) Repeat steps 4-8.
48) Evaporate the third 1 ml rinse until the volume is less than 3 ml in Tube B.
49) Remove Tube B from the evaporator.
50) Cap Tube B until you are ready to transfer the concentrated extract to
the storage tube.
Transfer of extract to the storage tube
51) Use a clean Pasteur pipette to transfer the concentrated extract from
Tube B to a preweighed, labeled storage tube. Be sure to weigh the
storage tube with its cap on. The cap used for weighing must be
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identifiable to make sure that the same cap is used for post-weighing
of the storage tube.
52) Replace the cap on Tube B until you are ready to rinse it into the
storage tube.
53) Replace the cap on the storage tube until you are ready to evaporate the
concentrated extract.
54) Remove the cap from the storage tube.
55) Place the storage tube in the evaporator.
56) Evaporate most of the concentrated extract in the storage tube. First
rinse of the storage tube
57) Using a 1 ml pipette, add 0.5 ml of fresh methanol to rinse Tube B.
58) Transfer this first 0.5 ml rinse of Tube B to the storage tube.
59) Repeat steps 4-8.
60) Evaporate most of the concentrated extract in the storage tube.
Second rinse of the storage tube
61) Using a 1 ml pipette, add another 0.5 ml of fresh methanol to rinse Tube
B a second time.
62) Transfer this second 0.5 ml rinse of Tube B to the storage tube.
63) Repeat steps 4-8.
64) Evaporate most of the concentrated extract in the storage tube. Third
rinse of the storage tube
65) Using a 1 ml pipette, add another 0.5 ml of fresh methanol to rinse Tube
B a third time.
66) Transfer this third 0.5 ml rinse of Tube B to the storage tube.
67) Replace the cap on the storage tube. Ensure that the cap corresponds
to the original pre-weighing of the storage tube.
68) Weigh the storage tube and record its weight.
72) Calculate the weight of the extract by subtracting the original weight of
the storage tube from the final weight of the storage tube.
73) Place the storage tube in a freezer at -20° C until you are ready to begin
the toxicological analysis (Section 3.4).
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3.4. A N AL Y S IS OF S AM P LES
The Model 900 HVCI samples can be analyzed for Toxicological, Biological,
Chemical Speciation and Radionuclide Analysis:
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Reference Publications:
Impaction substrate and methods of use. The present disclosure relates to a method of
collecting particles in a gas sample comprising impacting particles in the gas sample on a porous
material, as well as to impactors wherein an inertial impactor includes a porous substrate.
Inventors: Ferguson; Stephen T. (N. Billerica, MA), Kavouras; Ilias G. (Boston, MA), Wolfson;
Jack M. (Jamaica Plain, MA), Koutrakis; Petros (Wellesley, MA)
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