Method 316 EPA
Method 316 EPA
Method 316 EPA
* * * * *
Method 316 - Sampling and Analysis for Formaldehyde Emissions
from Stationary Sources in the Mineral Wool and Wool Fiberglass
Industries
1.0 Introduction.
This method is applicable to the determination of
formaldehyde, CAS Registry number 50-00-0, from stationary
sources in the mineral wool and wool fiber glass industries.
High purity water is used to collect the formaldehyde. The
formaldehyde concentrations in the stack samples are determined
using the modified pararosaniline method. Formaldehyde can be
detected as low as 8.8 x 10-10 lbs/cu ft (11.3 ppbv) or as high as
1.8 x 10-3 lbs/cu ft (23,000,000 ppbv), at standard conditions
over a 1 hour sampling period, sampling approximately 30 cu ft.
2.0 Summary of Method.
Gaseous and particulate pollutants are withdrawn
isokinetically from an emission source and are collected in high
purity water. Formaldehyde present in the emissions is highly
soluble in high purity water. The high purity water containing
formaldehyde is then analyzed using the modified pararosaniline
method. Formaldehyde in the sample reacts with acidic
pararosaniline, and the sodium sulfite, forming a purple
chromophore. The intensity of the purple color, measured
spectrophotometrically, provides an accurate and precise measure
of the formaldehyde concentration in the sample.
3.0 Definitions.
See the definitions in the General Provisions of this
Subpart.
4.0 Interferences.
Sulfite and cyanide in solution interfere with the
pararosaniline method. A procedure to overcome the interference
by each compound has been described by Miksch,
et al.
5.0 Safety. (Reserved)
6.0 Apparatus and Materials.
6.1 A schematic of the sampling train is shown in
Figure 1. This sampling train configuration is adapted from EPA
Method 5, 40 CFR part 60, appendix A, procedures.
FL or 100
Fg/mL Solution
0.250
250
100
0.500
500
100
1.00
1000
100
2.00
2000
100
3.00
1500
50
If the laboratory
that the working standards are stable - DO NOT assume that your
working standards are stable for more than a day unless you have
verified this by actual testing for several series of working
standards.
8.0
Sample Collection.
8.1
Laboratory Preparation:
All the components shall be maintained and
Record on each
As
8.3
content using EPA Approximation Method 4,40 CFR part 60, appendix
A, or its alternatives to establish estimates of isokinetic
sampling rate settings.
Section 3.6.
For large
To avoid timekeeping
In these cases,
Place 100 mR of
If additional
to ensure that the silica gel is not entrained and carried out
from the impinger during sampling.
Other
potentiometer/display unit.
ambient temperatures.
8.4.5
8.4.6
temperature to stabilize.
8.5
8.5.1
Leak-Check Procedures.
Pre-test Leak-check:
required.
If a
Instead, leak-
helpful.
adjust valve and slowly close the fine-adjust valve until the
desired vacuum is reached.
If the
When the
8.5.2.1
If the
Post-test Leak-check:
8.5.3.1
If the
rate is obtained, the tester shall record the leakage rate and
void the sampling run.
8.6
8.6.1
8.6.2
Plant . . . . . . . . . . .
Ambient temperature . . . . . . .
Location
. . . . . . . . .
Barometric pressure . . . . . . .
Operator
. . . . . . . . .
Date
. . . . . . . . . . .
Run No
. . . . . . . . . .
. . . . . .
Nozzle Identification No
Sample box No . . . . . . .
Meter box No
diameter, cm (in.)
. . . . . . .
. . . .
. . . . . . .
Meter )H
. . . . . . . . .
C Factor
. . . . . . . . .
. . . . . .
. . . . . .
. . . . . . . . . . .
Sampling
time
Vacuum
Stack
temperature
(T )
Velocity
head
EC (EF)
()P) mm
(in) H2O
Pressure
differential
across
orifice
meter
mm H2O
(in. H2O)
Gas
sample
volume
Gas sample
temperature
at dry gas
meter
Inlet
EC
(EF)
Outlet
EC
(EF)
Total
Avg.
Avg.
Average
Avg.
Traverse
point
number
(e) min.
mm Hg
(in. Hg)
m3
(ft3)
Filter
holder
temperature
Temperature
of gas
leaving
condenser
or last
impinger
EC (EF)
EC (EF)
Take
traverse point, with the tip pointing directly into the gas
stream.
isokinetic conditions.
and the pitot tube coefficient are outside the above ranges,
do not use the nomographs unless appropriate steps are taken
to compensate for the deviations.
8.6.4
If necessary, a
8.6.8
Also, check
However, forming
For these
Samples should be
Samples must be
Sample Recovery.
8.8.1
Preparation:
8.8.1.1
Do
cleanup site, remove the probe from the sampling train and
cap the open outlet, being careful not to lose any
condensate that might be present.
If a flexible
Catches.
8.8.2
Sample Containers:
8.8.2.1
Container 1:
ml, and record the volume of the solution in the first three
impingers.
While
squirting the water into the upper end of the probe, tilt
and rotate the probe so that all inside surfaces will be
wetted with water.
water into the upper end as the probe brush is being pushed
with a twisting action through the probe.
Any physical
Container 2:
Sample Blank.
Prepare a
Process
Container 3:
Silica Gel.
Note the
Ground-glass stoppers
If a
Sample
It is
If the color-developed
Quality Control.
9.1
Sampling:
Analysis:
The positive
9.2.1
Field Blanks:
At a
Blank Correction:
Blank
Method Blanks:
Calibration.
10.1 Probe Nozzle:
Using a
When the
Instead of physically
For metering
For these
make
To adjust the
The
Probes constructed
Alternately, if a
The weights
The standards
In
Record
the time of addition of the sodium sulfite and let the color
develop at room temperature for 60 minutes.
Set the
Place cuvette(s)
Record the
The procedure is
0.9999
Slope:
0.50
Y-Intercept:
0.090
For
example, the TI-55 calculators use the "X" key (this gives
the predicted formaldehyde concentration for the value of
the absorbance you key in for the sample).
Multiply the
temperature-sensitive.
It is
is being used.
operation.
11.1.5
This allows
C d V DF x 0.001 mg/g
where:
Cd
DF
dilution factor
12.1.2
Cd V
(V&B) DF 0.001 mg/g
Where:
Cd
DF
dilution factor
gas.
K [total formaldehyde,mg]
Vm(std)
where:
K
or
Vm(std)
15.0
16.0
References.