(ii) The coating operation(s) must be in compliance with the
operating limits for emission capture systems and add-on control
devices required by Sec.  63.4692 at all times, except for solvent
recovery systems for which you conduct liquid-liquid material balances
according to Sec.  63.4761(j).
    (iii) The coating operation(s) must be in compliance with the work
practice standards in Sec.  63.4693 at all times.
    (b) For existing sources as of March 4, 2019, before September 3,
2019, you must always operate and maintain your affected source,
including all air pollution control and monitoring equipment you use
for purposes of complying with this subpart, according to the
provisions in Sec.  63.6(e)(1)(i). On and after September 3, 2019 for
such existing sources and after March 4, 2019 for new or reconstructed
sources, you must always operate and maintain your affected source,
including associated air pollution control equipment and monitoring
equipment, in a manner consistent with safety and good air pollution
control practices for minimizing emissions. The general duty to
minimize emissions does not require you to make any further efforts to
reduce emissions if levels required by the applicable standard have
been achieved. Determination of whether a source is operating in
compliance with operation and maintenance requirements will be based on
information available to the Administrator which may include, but is
not limited to, monitoring results, review of operation and maintenance
procedures, review of operation and maintenance records, and inspection
of the source.
* * * * *
    (d) For existing sources, before September 3, 2019, if your
affected source uses an emission capture system and add-on control
device, you must develop a written startup, shutdown, and malfunction
plan (SSMP) according to the provisions in Sec.  63.6(e)(3). The SSMP
must address startup, shutdown, and corrective actions in the event of
a malfunction of the emission capture system or the add-on control
device. The SSMP must also address any coating operation equipment that
may cause increased emissions or that would affect capture efficiency
if the process equipment malfunctions, such as conveyors that move
parts among enclosures.

0
7. Section 63.4710 is amended by revising paragraph (c)(8)(ii) to read
as follows:

Sec.  63.4710   What notifications must I submit?

* * * * *
    (c) * * *
    (8) * * *
    (ii) For the emission rate without add-on controls option, provide
the calculation of the total mass of organic HAP emissions for each
month; the calculation of the total volume of coating solids used each
month; and the calculation of the 12-month organic HAP emission rate,
using Equations 1 and 1A (or 1A-alt) through 1C, 2, and 3,
respectively, of Sec.  63.4751.
* * * * *

0
8. Section 63.4720 is amended by:
0
a. Revising paragraph (a)(6)(ii) and paragraph (a)(7) introductory
text;
0
b. Redesignating paragraphs (a)(7)(i) through (xiv) as paragraphs
(a)(7)(i)(A) through (N);
0
c. Adding paragraph (a)(7)(i) introductory text and paragraph
(a)(7)(ii);
0
d. Revising paragraph (c) introductory text; and
0
e. Adding paragraph (d).
    The revisions and additions read as follows:

Sec.  63.4720   What reports must I submit?

    (a) * * *
    (6) * * *
    (ii) The calculations used to determine the 12-month organic HAP
emission rate for the compliance period in which the deviation
occurred. You must provide the calculations for Equations 1, 1A (or 1A-
alt) through 1C, 2, and 3 in Sec.  63.4751; and if applicable, the
calculation used to determine mass of organic HAP in waste materials
according to Sec.  63.4751(e)(4). You do not need to submit background
data supporting these calculations (e.g., information provided by
materials suppliers or manufacturers, or test reports).
* * * * *
    (7) Deviations: Emission rate with add-on controls option. You must
be in compliance with the emission limitations in this subpart as
specified in paragraphs (a)(7)(i) and (ii) of this section.

    (i) For existing sources, before September 3, 2019, if you used the
emission rate with add-on controls option and there was a deviation
from an emission limitation (including any periods when emissions
bypassed the add-on control device and were diverted to the
atmosphere), the semiannual compliance report must contain the
information in paragraphs (a)(7)(i)(A) through (N) of this section.
This includes periods of SSM during which deviations occurred.
* * * * *
    (ii) After March 4, 2019 for new and reconstructed sources, and on
and after September 3, 2019 for existing sources, if you used the
emission rate with add-on controls option and there was a deviation
from an emission limitation (including any periods when emissions
bypassed the add-on control device and were diverted to the
atmosphere), the semiannual compliance report must contain the
information in paragraphs (a)(7)(ii)(A) through (M) of this section.
    (A) The beginning and ending dates of each compliance period during
which the 12-month organic HAP emission rate exceeded the applicable
emission limit in Sec.  63.4690.
    (B) The calculations used to determine the 12-month organic HAP
emission rate for each compliance period in which a deviation occurred.
You must provide the calculation of the total mass of organic HAP
emissions for the coatings, thinners, and cleaning materials used each
month, using Equations 1 and 1A through 1C of Sec.  63.4751; and, if
applicable, the calculation used to determine mass of organic HAP in
waste materials according to Sec.  63.4751(e)(4); the calculation of
the total volume of coating solids used each month, using Equation 2 of
Sec.  63.4751; the calculation of the mass of organic HAP emission
reduction each month by emission capture systems and add-on control
devices, using Equations 1 and 1A through 1D of Sec.  63.4761, and
Equations 2, 3, and 3A through 3C of Sec.  63.4761, as applicable; the
calculation of the total mass of organic HAP emissions each month,
using Equation 4 of Sec.  63.4761; and the calculation of the 12-month
organic HAP emission rate, using Equation 5 of Sec.  63.4761. You do
not need to submit the background data supporting these calculations
(e.g., information provided by materials suppliers or manufacturers, or
test reports).
    (C) A brief description of the CPMS.
    (D) The date of the latest CPMS certification or audit.
    (E) The date and time that each CPMS was inoperative, except for
zero (low-level) and high-level checks.
    (F) The date, time, and duration that each CPMS was out-of-control,
including the information in Sec.  63.8(c)(8).
    (G) The date and time period of each deviation from an operating
limit in Table 3 to this subpart, date and time period of any bypass of
the add-on control device.
    (H) A summary of the total duration of each deviation from an
operating limit in Table 3 to this subpart, each bypass of the add-on
control device during the semiannual reporting period, and the total
duration as a percent of the total source operating time during that
semiannual reporting period.
    (I) A breakdown of the total duration of the deviations from the
operating limits in Table 3 to this subpart and bypasses of the add-on
control device during the semiannual reporting period by identifying
deviations due to control equipment problems, process problems, other
known causes, and other unknown causes; a list of the affected source
or equipment, an estimate of the quantity of each regulated pollutant
emitted over any emission limit, and a description of the method used
to estimate the emissions.
    (J) A summary of the total duration of CPMS downtime during the
semiannual reporting period and the total duration of CPMS downtime as
a percent of the total source operating time during that semiannual
reporting period.
    (K) A description of any changes in the CPMS, coating operation,
emission capture system, or add-on control device since the last
semiannual reporting period.
    (L) For each deviation from the standard, including work practice
standards, a description of the deviation, the date and time period of
the deviation, and the actions you took to correct the deviation.
    (M) A statement of the cause of each deviation.
* * * * *
    (c) SSM reports. For existing sources, before September 3, 2019, if
you used the emission rate with add-on controls option and you had an
SSM during the semiannual reporting period, you must submit the reports
specified in paragraphs (c)(1) and (2) of this section.
* * * * *
    (d) Electronic reporting. (1) Within 60 days after the date of
completing each performance test required by this subpart, you must
submit the results of the performance test following the procedures
specified in paragraphs (d)(1)(i) through (iii) of this section.
    (i) Data collected using test methods supported by EPA's Electronic
Reporting Tool (ERT) as listed on EPA's ERT website (https://www.epa.gov/electronic-reporting-air-emissions/electronic-reporting-tool-ert) at the time of the test. Submit the results of the
performance test to the EPA via the Compliance and Emissions Data
Reporting Interface (CEDRI), which can be accessed through EPA's
Central Data Exchange (CDX) (https://cdx.epa.gov/). The data must be
submitted in a file format generated through the use of EPA's ERT.
Alternatively, you may submit an electronic file consistent with the
extensible markup language (XML) schema listed on EPA's ERT website.
    (ii) Data collected using test methods that are not supported by
EPA's ERT as listed on EPA's ERT website at the time of the test. The
results of the performance test must be included as an attachment in
the ERT or an alternate electronic file consistent with the XML schema
listed on EPA's ERT website. Submit the ERT generated package or
alternative file to the EPA via CEDRI.
    (iii) Confidential business information (CBI). If you claim some of
the information submitted under paragraph (a)(1) of this section is
CBI, you must submit a complete file, including information claimed to
be CBI, to the EPA. The file must be generated through the use of EPA's
ERT or an alternate electronic file consistent with the XML schema
listed on EPA's ERT website. Submit the file on a compact disc, flash
drive, or other commonly used electronic storage medium and clearly
mark the medium as CBI. Mail the electronic medium to U.S. EPA/OAQPS/
CORE CBI Office, Attention: Group Leader, Measurement Policy Group, MD
C404-02, 4930 Old Page Rd., Durham, NC 27703. The same file with the
CBI omitted must be submitted to the EPA via EPA's CDX as described in
paragraph (d)(1)(i) of this section.
    (2) You must submit the Notification of Compliance Status required
in Sec.  63.4710(c) and the semiannual compliance reports required in
paragraph (a) of this section to the EPA via the CEDRI. (CEDRI can be
accessed through the EPA's CDX (https://cdx.epa.gov/)). For semiannual
compliance reports, you must use the appropriate electronic report in
CEDRI for this subpart or an alternative electronic file format
consistent with the XML schema listed on the CEDRI website (https://www.epa.gov/electronic-reporting-air-emissions/compliance-and-emissions-data-reporting-interface-cedri). If the reporting form
specific to this subpart is not available in CEDRI at the time that

the report is due, you must submit the report to the Administrator at
all the appropriate addresses listed in Sec.  63.13. Once the reporting
template has been available in CEDRI for 1 year, you must begin
submitting all subsequent reports via CEDRI. For the Notification of
Compliance Status, you must submit a file in portable document format
(PDF) to CEDRI. The reports must be submitted by the deadlines
specified in this subpart, regardless of the method in which the
reports are submitted.
    (3) If you are required to electronically submit a report through
CEDRI in EPA's CDX, you may assert a claim of EPA system outage for
failure to timely comply with the reporting requirement. To assert a
claim of EPA system outage, you must meet the requirements outlined in
paragraphs (d)(3)(i) through (vii) of this section.
    (i) You must have been or will be precluded from accessing CEDRI
and submitting a required report within the time prescribed due to an
outage of either EPA's CEDRI or CDX systems.
    (ii) The outage must have occurred within the period of time
beginning five business days prior to the date that the submission is
due.
    (iii) The outage may be planned or unplanned.
    (iv) You must submit notification to the Administrator in writing
as soon as possible following the date you first knew, or through due
diligence should have known, that the event may cause or has caused a
delay in reporting.
    (v) You must provide to the Administrator a written description
identifying:
    (A) The date(s) and time(s) when CDX or CEDRI was accessed and the
system was unavailable;
    (B) A rationale for attributing the delay in reporting beyond the
regulatory deadline to EPA system outage;
    (C) Measures taken or to be taken to minimize the delay in
reporting; and
    (D) The date by which you propose to report, or if you have already
met the reporting requirement at the time of the notification, the date
you reported.
    (vi) The decision to accept the claim of EPA system outage and
allow an extension to the reporting deadline is solely within the
discretion of the Administrator.
    (vii) In any circumstance, the report must be submitted
electronically as soon as possible after the outage is resolved.
    (4) If you are required to electronically submit a report through
CEDRI in EPA's CDX, you may assert a claim of force majeure for failure
to timely comply with the reporting requirement. To assert a claim of
force majeure, you must meet the requirements outlined in paragraphs
(d)(4)(i) through (v) of this section.
    (i) You may submit a claim if a force majeure event is about to
occur, occurs, or has occurred or there are lingering effects from such
an event within the period of time beginning five business days prior
to the date the submission is due. For the purposes of this section, a
force majeure event is defined as an event that will be or has been
caused by circumstances beyond the control of the affected facility,
its contractors, or any entity controlled by the affected facility that
prevents you from complying with the requirement to submit a report
electronically within the time period prescribed. Examples of such
events are acts of nature (e.g., hurricanes, earthquakes, or floods),
acts of war or terrorism, or equipment failure or safety hazard beyond
the control of the affected facility (e.g., large scale power outage).
    (ii) You must submit the notification to the Administrator in
writing as soon as possible following the date you first knew, or
through due diligence should have known, that the event may cause or
has caused a delay in reporting.
    (iii) You must provide to the Administrator:
    (A) A written description of the force majeure event;
    (B) A rationale for attributing the delay in reporting beyond the
regulatory deadline to the force majeure event;
    (C) Measures taken or to be taken to minimize the delay in
reporting; and
    (D) The date by which you propose to report, or if you have already
met the reporting requirement at the time of the notification, the date
you reported.
    (iv) The decision to accept the claim of force majeure and allow an
extension to the reporting deadline is solely within the discretion of
the Administrator.
    (v) In any circumstance, the reporting must occur as soon as
possible after the force majeure event occurs.

0
9. Section 63.4730 is amended by:
0
a. Revising paragraph (c)(3) and paragraph (k) introductory text;
0
b. Redesignating paragraphs (k)(1) through (4) as paragraphs (k)(1)(i)
through (iv);
0
c. Adding paragraph (k)(1) introductory text and paragraph (k)(2);
0
d. Redesignating paragraphs (k)(5)(i) through (iii) as paragraphs
(k)(1)(v)(A) through (C);
0
e. Redesignating paragraph (k)(5) introductory text as paragraph
(k)(1)(v) introductory text and revising it;
0
f. Redesignating paragraphs (k)(6)(i) and (ii) as paragraphs
(k)(1)(vi)(A) and (B);
0
g. Redesignating paragraph (k)(6) introductory text as paragraph
(k)(1)(vi) introductory text and revising it; and
0
h. Redesignating paragraphs (k)(7) and (8) as paragraphs (k)(1)(vii)
and (viii).
    The revisions and additions read as follows:

Sec.  63.4730   What records must I keep?

* * * * *
    (c) * * *
    (3) For the emission rate without add-on controls option, a record
of the calculation of the total mass of organic HAP emissions for the
coatings, thinners, and cleaning materials used each month, using
Equations 1, 1A (or 1A-alt) through 1C, and 2 of Sec.  63.4751; and, if
applicable, the calculation used to determine mass of organic HAP in
waste materials according to Sec.  63.4751(e)(4); the calculation of
the total volume of coating solids used each month, using Equation 2 of
Sec.  63.4751; and the calculation of each 12-month organic HAP
emission rate, using Equation 3 of Sec.  63.4751.
* * * * *
    (k) If you use the emission rate with add-on controls option, you
must keep the records specified in paragraphs (k)(1) through (2) of
this section.
    (1) For existing sources, before September 3, 2019:
* * * * *
    (v) For each capture system that is not a PTE, the data and
documentation you used to determine capture efficiency according to the
requirements specified in Sec. Sec.  63.4764 and 63.4765(b) through
(e), including the records specified in paragraphs (k)(1)(v)(A) through
(C) of this section that apply to you.
* * * * *
    (vi) The records specified in paragraphs (k)(1)(vi)(A) and (B) of
this section for each add-on control device organic HAP destruction or
removal efficiency determination as specified in Sec.  63.4766.
* * * * *
    (2) After March 4, 2019 for new and reconstructed sources, and on
and after September 3, 2019 for existing sources:
    (i) The records required to show continuous compliance with each
operating limit specified in Table 3 to this subpart that applies to
you.
    (ii) For each capture system that is a PTE, the data and
documentation you used to support a determination that the capture
system meets the criteria in Method 204 of appendix M to 40 CFR part 51
for a PTE and has a capture efficiency of 100 percent, as specified in
Sec.  63.4765(a).
    (iii) For each capture system that is not a PTE, the data and
documentation

you used to determine capture efficiency according to the requirements
specified in Sec. Sec.  63.4764 and 63.4765(b) through (e), including
the records specified in paragraphs (k)(2)(iii)(A) through (C) of this
section that apply to you.
    (A) Records for a liquid-to-uncaptured-gas protocol using a
temporary total enclosure or building enclosure. Records of the mass of
total volatile hydrocarbon (TVH) as measured by Method 204A or F of
appendix M to 40 CFR part 51 for each material used in the coating
operation, and the total TVH for all materials used during each capture
efficiency test run, including a copy of the test report. Records of
the mass of TVH emissions not captured by the capture system that
exited the temporary total enclosure or building enclosure during each
capture efficiency test run as measured by Method 204D or E of appendix
M to 40 CFR part 51, including a copy of the test report. Records
documenting that the enclosure used for the capture efficiency test met
the criteria in Method 204 of appendix M to 40 CFR part 51 for either a
temporary total enclosure or a building enclosure.
    (B) Records for a gas-to-gas protocol using a temporary total
enclosure or a building enclosure. Records of the mass of TVH emissions
captured by the emission capture system as measured by Method 204B or C
of appendix M to 40 CFR part 51 at the inlet to the add-on control
device, including a copy of the test report. Records of the mass of TVH
emissions not captured by the capture system that exited the temporary
total enclosure or building enclosure during each capture efficiency
test run as measured by Method 204D or E of appendix M to 40 CFR part
51, including a copy of the test report. Records documenting that the
enclosure used for the capture efficiency test met the criteria in
Method 204 of appendix M to 40 CFR part 51 for either a temporary total
enclosure or a building enclosure.
    (C) Records for an alternative protocol. Records needed to document
a capture efficiency determination using an alternative method or
protocol as specified in Sec.  63.4765(e), if applicable.
    (iv) The records specified in paragraphs (k)(2)(iv)(A) and (B) of
this section for each add-on control device organic HAP destruction or
removal efficiency determination as specified in Sec.  63.4766.
    (A) Records of each add-on control device performance test
conducted according to Sec. Sec.  63.4764 and 63.4766.
    (B) Records of the coating operation conditions during the add-on
control device performance test showing that the performance test was
conducted under representative operating conditions.
    (v) Records of the data and calculations you used to establish the
emission capture and add-on control device operating limits as
specified in Sec.  63.4767 and to document compliance with the
operating limits as specified in Table 3 to this subpart.
    (vi) A record of the work practice plan required by Sec.  63.4693,
and documentation that you are implementing the plan on a continuous
basis.

0
10. Section 63.4741 is amended by revising:
0
a. Paragraph (a)(2);
0
b. The subject heading and first sentence of paragraph (b)(1);
0
 c. The defined terms ``mvolatiles'' and ``Davg''
in Equation 1 in paragraph (b)(3) introductory text; and
0
d. Paragraph (c).
    The revisions read as follows:

Sec.  63.4741   How do I demonstrate initial compliance with the
emission limitations?

* * * * *
    (a) * * *
    (2) Method 24 (appendix A-7 to 40 CFR part 60). For coatings, you
may use Method 24 to determine the mass fraction of nonaqueous volatile
matter and use that value as a substitute for mass fraction of organic
HAP. (Note: Method 24 is not appropriate for those coatings with a
water content that would result in an effective detection limit greater
than the applicable emission limit.) One of the voluntary consensus
standards in paragraphs (a)(2)(i) through (iv) may be used as an
alternative to using Method 24.
    (i) ASTM Method D2111-10 (Reapproved 2015), ``Standard Test Methods
for Specific Gravity and Density of Halogenated Organic Solvents and
Their Admixtures,'' (incorporated by reference, see Sec.  63.14);
    (ii) ASTM Method D2369-10 (Reapproved 2015)\e\, ``Standard Test
Method for Volatile Content of Coatings,'' (incorporated by reference,
see Sec.  63.14);
    (iii) ASTM Method D2697-03 (Reapproved 2014), ``Standard Test
Method for Volume Nonvolatile Matter in Clear or Pigmented Coatings,''
(incorporated by reference, see Sec.  63.14); and
    (iv) ASTM Method D6093-97 (Reapproved 2016), ``Standard Test Method
for Percent Volume Nonvolatile Matter in Clear or Pigmented Coatings
Using a Helium Gas Pycnometer,'' (incorporated by reference, see Sec.
63.14).
* * * * *
    (b) * * *
    (1) ASTM Method D2697-03 (Reapproved 2014) or D6093-97 (Reapproved
2016). You may use ASTM Method D2697-03 (Reapproved 2014), ``Standard
Test Method for Volume Nonvolatile Matter in Clear or Pigmented
Coatings'' (incorporated by reference, see Sec.  63.14), or D6093-97
(Reapproved 2016), ``Standard Test Method for Percent Volume
Nonvolatile Matter in Clear or Pigmented Coatings Using a Helium Gas
Pycnometer'' (incorporated by reference, see Sec.  63.14), to determine
the volume fraction of coating solids for each coating. * * *
* * * * *
    (3) * * *

mvolatiles = Total volatile matter content of the
coating, including HAP, volatile organic compounds (VOC), water, and
exempt compounds, determined according to Method 24 in appendix A-7
of 40 CFR part 60, grams volatile matter per liter coating.
Davg = Average density of volatile matter in the coating,
grams volatile matter per liter volatile matter, determined from
test results using ASTM Method D1475-13, ``Standard Test Method for
Density of Liquid Coatings, Inks, and Related Products,''
(incorporated by reference, see Sec.  63.14), information from the
supplier or manufacturer of the material, or reference sources
providing density or specific gravity data for pure materials. If
there is disagreement between ASTM Method D1475-13 test results and
other information sources, the test results will take precedence.

    (c) Determine the density of each coating. Determine the density of
each coating used during the compliance period from test results using
ASTM Method D1475-13, ``Standard Test Method for Density of Liquid
Coatings, Inks, and Related Products,'' (incorporated by reference, see
Sec.  63.14), or information from the supplier or manufacturer of the
material. If there is disagreement between ASTM Method D1475-13 test
results and the supplier's or manufacturer's information, the test
results will take precedence.
* * * * *

0
11. Section 63.4751 is amended by:
0
a. Revising paragraph (c);
0
b. Revising the defined term ``A'' in Equation 1 in of paragraph (e)
introductory text; and
0
c. Adding paragraph (i).
    The revisions and addition read as follows:

Sec.  63.4751  How do I demonstrate initial compliance with the
emission limitations?

* * * * *
    (c) Determine the density of each material. Determine the density
of each coating, thinner, and cleaning material

used during each month from test results using ASTM Method D1475-13
(incorporated by reference, see Sec.  63.14), information from the
supplier or manufacturer of the material, or reference sources
providing density or specific gravity data for pure materials. If there
is disagreement between ASTM Method D1475-13 test results and such
other information sources, the test results will take precedence.
* * * * *
    (e) * * *

A = Total mass of organic HAP in the coatings used during the month,
grams, as calculated in Equation 1A (or 1A-alt) of this section.
* * * * *
    (i) Alternative compliance demonstration. As an alternative to
paragraph (h) of this section, you may demonstrate initial compliance
by identifying each organic HAP component in the coating(s) and
conducting a performance test using Method 320 of appendix A to 40 CFR
part 63 or NCASI Method ISS/FP A105.01 (incorporated by reference in
Sec.  63.14) (for formaldehyde) or Method 326 of appendix A to 40 CFR
part 63 (for isocyanates) to obtain an organic HAP emission factor
(EF). The voluntary consensus standard ASTM D6348-03 (Reapproved 2010)
(incorporated by reference, see Sec.  63.14) may be used as an
alternative to using Method 320 under the conditions specified in
paragraphs (i)(4)(i) and (ii) of this section.
    (1) You must also calculate the mass of organic HAP emitted from
the coatings used during the month using Equation 1A-alt of this
section:
[GRAPHIC] [TIFF OMITTED] TR04MR19.010

Where:

A = Total mass of organic HAP in the coatings used during the month,
grams.
Volc,i = Total volume of coating, i, used during the
month, liters.
Dc,j = Density of coating, i, grams coating per liter of
coatings.
Wc,i = Mass fraction of organic HAP in coating, i, grams
organic HAP per gram coating.
EFc,i = Organic HAP emission factor (three-run average
from performance testing, evaluated as proportion of mass organic
HAP emitted to mass of organic HAP in the coatings used during the
performance test).
m = Number of different coatings used during the month.

    (2) Calculate the organic HAP emission rate for the 12-month
compliance period, grams organic HAP per liter coating solids used,
using Equation 3 of this section.
    (3) The organic HAP emission rate for the initial 12-month
compliance period, calculated using Equation 3 of this section, must be
less than or equal to the applicable emission limit in Sec.  63.4690.
You must keep all records as required by Sec. Sec.  63.4730 and
63.4731. As part of the Notification of Compliance Status required by
Sec.  63.4710, you must identify the coating operation(s) for which you
used the emission rate without add-on controls option and submit a
statement that the coating operation(s) was (were) in compliance with
the emission limitations during the initial compliance period because
the organic HAP emission rate was less than or equal to the applicable
emission limit in Sec.  63.4690, determined according to this section.
    (4) If ASTM D6348-03 (Reapproved 2010) is used, the conditions
specified in paragraphs (i)(4)(i) and (ii) must be met.
    (i) Test plan preparation and implementation in the Annexes to ASTM
D6348-03 (Reapproved 2010), sections A1 through A8 are mandatory.
    (ii) In ASTM D6348-03 (Reapproved 2010) Annex A5 (Analyte Spiking
Technique), the percent (%) R must be determined for each target
analyte (Equation A5.5 of ASTM D6348-03). In order for the test data to
be acceptable for a compound, %R must be between 70 and 130 percent. If
the %R value does not meet this criterion for a target compound, the
test data are not acceptable for that compound, and the test must be
repeated for that analyte following adjustment of the sampling and/or
analytical procedure before the retest. The %R value for each compound
must be reported in the test report, and all field measurements must be
corrected with the calculated %R value for that compound using the
following equation: Reported Result = (Measured Concentration in the
Stack x 100)/%R.

0
12. Section 63.4752 is amended by adding paragraph (e) to read as
follows:

Sec.  63.4752   How do I demonstrate continuous compliance with the
emission limitations?

* * * * *
    (e) If you use the alternative compliance demonstration described
in Sec.  63.4751(i), you must identify each organic HAP component in
the coating(s) and conduct a performance test every 5 years to obtain
an organic HAP emission factor (EF). You must use the following
methods, as appropriate: Method 320 of appendix A to 40 CFR part 63 or
NCASI Method ISS/FP A105.01 (incorporated by reference, see Sec.
63.14) (for formaldehyde) or Method 326 of appendix A to 40 CFR part 63
(for isocyanates). The voluntary consensus standard ASTM D6348-03
(Reapproved 2010) (incorporated by reference, see Sec.  63.14) may be
used as an alternative to using Method 320 under the conditions
specified in Sec.  63.4751(i)(4)(i) and (ii).

0
13. Section 63.4761 is amended by revising paragraph (j)(3) to read as
follows:

Sec.  63.4761   How do I demonstrate initial compliance?

* * * * *
    (j) * * *
    (3) Determine the mass fraction of volatile organic matter for each
coating, thinner, and cleaning material used in the coating operation
controlled by the solvent recovery system during the month, grams
volatile organic matter per gram coating. You may determine the
volatile organic matter mass fraction using Method 24 of 40 CFR part
60, appendix A-7, one of the voluntary consensus standards specified in
Sec.  63.4741(a)(2)(i) through (iv), or an EPA approved alternative
method, or you may use information provided by the manufacturer or
supplier of the coating. In the event of any inconsistency between
information provided by the manufacturer or supplier and the results of
Method 24 of 40 CFR part 60, appendix A-7, or an approved alternative
method, the test method results will take precedence unless after
consultation, a regulated source could demonstrate to the satisfaction
of the enforcement agency that the formulation data were correct.
* * * * *

0
14. Section 63.4763 is amended by revising paragraph (h) to read as
follows:

Sec.  63.4763   How do I demonstrate continuous compliance with the
emission limitations?

* * * * *
    (h) For existing sources, before September 3, 2019, consistent with
Sec. Sec.  63.6(e) and 63.7(e)(1), deviations that occur during a
period of SSM of the

emission capture system, add-on control device, or coating operation
that may affect emission capture or control device efficiency are not
violations if you demonstrate to the Administrator's satisfaction that
you were operating in accordance with Sec.  63.6(e)(1). The
Administrator will determine whether deviations that occur during a
period you identify as an SSM are violations, according to the
provisions in Sec.  63.6(e).
* * * * *

0
15. Section 63.4764 is amended by revising paragraphs (a)(1) and (2) to
read as follows:

Sec.  63.4764   What are the general requirements for performance
tests?

    (a) * * *
    (1) Representative coating operation operating conditions. You must
conduct the performance test under representative operating conditions
for the coating operation. Operations during periods of startup,
shutdown, and nonoperation do not constitute representative conditions.
You may not conduct performance tests during periods of malfunction.
You must record the process information that is necessary to document
operating conditions during the test and explain why the conditions
represent normal operation. Upon request, you shall make available to
the Administrator such records as may be necessary to determine the
conditions of performance tests.
    (2) Representative emission capture system and add-on control
device operating conditions. You must conduct the performance test when
the emission capture system and add-on control device are operating at
a representative flow rate, and the add-on control device is operating
at a representative inlet concentration. Representative conditions
exclude periods of startup and shutdown. You may not conduct
performance tests during periods of malfunction. You must record
information that is necessary to document emission capture system and
add-on control device operating conditions during the test and explain
why the conditions represent normal operation.
* * * * *

0
16. Section 63.4766 is amended by revising paragraphs (a)(1) through
(4), (b), (d), and (f) to read as follows:

Sec.  63.4766   How do I determine the add-on control device emission
destruction or removal efficiency?

* * * * *
    (a) * * *
    (1) Use Method 1 or 1A of appendix A-1 to 40 CFR part 60, as
appropriate, to select sampling sites and velocity traverse points.
    (2) Use Method 2, 2A, 2C, 2D, or 2F of appendix A-1 to 40 CFR part
60, or Method 2G of appendix A-2 to 40 CFR part 60, as appropriate, to
measure gas volumetric flow rate.
    (3) Use Method 3, 3A, or 3B of appendix A-2 to 40 CFR part 60, as
appropriate, for gas analysis to determine dry molecular weight. You
may also use as an alternative to Method 3B, the manual method for
measuring the oxygen, carbon dioxide, and carbon monoxide content of
exhaust gas in ANSI/ASME PTC 19.10-1981, ``Flue and Exhaust Gas
Analyses [Part 10, Instruments and Apparatus]'' (incorporated by
reference, see Sec.  63.14).
    (4) Use Method 4 of appendix A-3 to 40 CFR part 60 to determine
stack gas moisture.
* * * * *
    (b) Measure total gaseous organic mass emissions as carbon at the
inlet and outlet of the add-on control device simultaneously, using
Method 25 or 25A of appendix A-7 to 40 CFR part 60, and Method 320 or
326 of appendix A to 40 CFR part 63, as specified in paragraphs (b)(1)
through (5) of this section. The voluntary consensus standard ASTM
D6348-03 (Reapproved 2010) (incorporated by reference in Sec.  63.14)
may be used as an alternative to using Method 320 if the conditions
specified in Sec.  63.4751(i)(4)(i) and (ii) are met. You must use the
same method for both the inlet and outlet measurements.
    (1) Use Method 25 of appendix A-7 to 40 CFR part 60 if the add-on
control device is an oxidizer, and you expect the total gaseous organic
concentration as carbon to be more than 50 parts per million (ppm) at
the control device outlet.
    (2) Use Method 25A of appendix A-7 to 40 CFR part 60 if the add-on
control device is an oxidizer, and you expect the total gaseous organic
concentration as carbon to be 50 ppm or less at the control device
outlet.
    (3) Use Method 25A of appendix A-7 to 40 CFR part 60 if the add-on
control device is not an oxidizer.
    (4) If Method 25A is used, and if formaldehyde is a major organic
HAP component of the surface coating exhaust stream, use Method 320 of
appendix A to 40 CFR part 63 or NCASI Method ISS/FP A105.01
(incorporated by reference in Sec.  63.14) or ASTM D6348-03 (Reapproved
2010) (incorporated by reference in Sec.  63.14) to determine
formaldehyde concentration.
    (5) In addition to Method 25 or 25A, use Method 326 of appendix A
to 40 CFR part 63 if isocyanate is a major organic HAP component of the
surface coating exhaust stream.
* * * * *
    (d) For each test run, determine the total gaseous organic
emissions mass flow rates for the inlet and the outlet of the add-on
control device, using Equation 1 of this section. If there is more than
one inlet or outlet to the add-on control device, you must calculate
the total gaseous organic mass flow rate using Equation 1 of this
section for each inlet and each outlet and then total all of the inlet
emissions and total all of the outlet emissions. The mass emission
rates for formaldehyde and individual isocyanate must be determined
separately.
[GRAPHIC] [TIFF OMITTED] TR04MR19.000

Where:

Mf = Total gaseous organic emissions mass flow rate,
grams per hour (h).
MW = Molecular weight of analyte of interest (12 for Method 25 and
25A results).
Cc = Concentration of organic compounds in the vent gas
(as carbon if determined by Method 25 or Method 25A), parts per
million by volume (ppmv), dry basis.
Qsd = Volumetric flow rate of gases entering or exiting
the add-on control device, as determined by Method 2, 2A, 2C, 2D,
2F, or 2G, dry standard cubic meters/hour (dscm/h).
41.6 = Conversion factor for molar volume, gram-moles per cubic
meter (mol/m\3\) (@293 Kelvin (K) and 760 millimeters of mercury
(mmHg)).
* * * * *
    (f) Determine the emission destruction or removal efficiency of the
add-on control device as the average of the efficiencies determined in
the three test runs and calculated in Equation 2 of this section.
Destruction and removal efficiency must be determined independently for
formaldehyde and isocyanates.

0
17. Section 63.4781 is amended by revising paragraph (3) under the
definition of ``deviation'' and revising the definition of
``tileboard'' to read as follows:

Sec.  63.4781  What definitions apply to this subpart?

* * * * *
    Deviation * * *
    (3) On and after September 3, 2019, fails to meet any emission
limit, or operating limit, or work practice standard in this subpart
during SSM.
* * * * *
    Tileboard means hardboard that meets the specifications for Class I
given by the standard ANSI A135.4-2012 (incorporated by reference, see
Sec.  63.14) as approved by the American National Standards Institute.
The standard specifies requirements and test methods for water
absorption, thickness swelling, modulus of rupture, tensile strength,
surface finish, dimensions, squareness, edge straightness, and moisture
content for five classes of hardboard. Tileboard is also known as Class
I hardboard or tempered hardboard.
* * * * *

0
18. Table 4 to Subpart QQQQ is revised to read as follows:
    Table 4 to Subpart QQQQ of Part 63--Applicability of General
Provisions to Subpart QQQQ of Part 63
    You must comply with the applicable General Provisions requirements
according to the following table:

----------------------------------------------------------------------------------------------------------------
                                                                     Applicable to
              Citation                         Subject               subpart QQQQ             Explanation
----------------------------------------------------------------------------------------------------------------
Sec.   63.1(a)(1)-(14)..............  General Applicability....  Yes.................
Sec.   63.1(b)(1)-(3)...............  Initial Applicability      Yes.................  Applicability to subpart
                                       Determination.                                   QQQQ is also specified
                                                                                in Sec.   63.4681.
Sec.   63.1(c)(1)...................  Applicability After        Yes.................
                                       Standard Established.
Sec.   63.1(c)(2)...................  Applicability of Permit    No..................  Area sources are not
                                       Program for Area Sources.                        subject to subpart QQQQ.
Sec.   63.1(c)(3)...................  [Reserved]...............  No..................
Sec.   63.1(c)(4)-(5)...............  Extensions and             Yes.................
                                       Notifications.
Sec.   63.1(d)......................  [Reserved]...............  No..................
Sec.   63.1(e)......................  Applicability of Permit    Yes.................
                                       Program Before Relevant
                                       Standard is Set.
Sec.   63.2.........................  Definitions..............  Yes.................  Additional definitions
                                                                                are specified in Sec.
                                                                                63.4781.
Sec.   63.3(a)-(c)..................  Units and Abbreviations..  Yes.................
Sec.   63.4(a)(1)-(5)...............  Prohibited Activities....  Yes.................
Sec.   63.4(b)-(c)..................  Circumvention/             Yes.................
                                       Severability.
Sec.   63.5(a)......................  Construction/              Yes.................
                                       Reconstruction.
Sec.   63.5(b)(1)-(6)...............  Requirements for           Yes.................
                                       Existing, Newly
                                       Constructed, and
                                       Reconstructed Sources.
Sec.   63.5(c)......................  [Reserved]...............  No..................
Sec.   63.5(d)......................  Application for Approval   Yes.................
                                       of Construction/
                                       Reconstruction.
Sec.   63.5(e)......................  Approval of Construction/  Yes.................
                                       Reconstruction.
Sec.   63.5(f)......................  Approval of Construction/  Yes.................
                                       Reconstruction Based on
                                       Prior State Review.
Sec.   63.6(a)......................  Compliance With Standards  Yes.................
                                       and Maintenance
                                       Requirements--Applicabil
                                       ity.
Sec.   63.6(b)(1)-(7)...............  Compliance Dates for New   Yes.................  Sec.   63.4683 specifies
                                       and Reconstructed                                compliance dates.
                                       Sources.
Sec.   63.6(c)(1)-(5)...............  Compliance Dates for       Yes.................  Sec.   63.4683 specifies
                                       Existing Sources.                                compliance dates.
Sec.   63.6(d)......................  [Reserved]...............  No..................
Sec.   63.6(e)(1)(i)................  General Duty to Minimize   No..................  See Sec.   63.4700(b) for
                                       Emissions.                                       general duty
                                                                                requirement.
Sec.   63.6(e)(1)(ii)...............  Requirement to Correct     No..................
                                       Malfunctions ASAP.
Sec.   63.6(e)(1)(iii)..............  Operation and Maintenance  Yes.................
                                       Requirements Enforceable
                                       Independent of Emissions
                                       Limitations.
Sec.   63.6(e)(2)...................  [Reserved]...............  No..................
Sec.   63.6(e)(3)...................  SSMP.....................  No..................
Sec.   63.6(f)(1)...................  Compliance Except During   No..................
                                       SSM.
Sec.   63.6(f)(2)-(3)...............  Methods for Determining    Yes.................
                                       Compliance.
Sec.   63.6(g)(1)-(3)...............  Use of an Alternative      Yes.................
                                       Standard.
Sec.   63.6(h)......................  Compliance with Opacity/   No..................  Subpart QQQQ does not
                                       Visible Emissions                                establish opacity
                                       Standards.                                       standards and does not
                                                                                require continuous
                                                                                opacity monitoring
                                                                                systems (COMS).
Sec.   63.6(i)(1)-(16)..............  Extension of Compliance..  Yes.................
Sec.   63.6(j)......................  Presidential Compliance    Yes.................
                                       Exemption.
Sec.   63.7(a)(1)...................  Performance Test           Yes.................  Applies to all affected
                                       Requirements--Applicabil                         sources. Additional
                                       ity.                                             requirements for
                                                                                performance testing are
                                                                                specified in Sec.  Sec.
                                                                                63.4751, 63.4752,
                                                                                63.4764, 63.4765, and
                                                                                63.4766.
Sec.   63.7(a)(2)...................  Performance Test           Yes.................  Applies only to
                                       Requirements--Dates.                             performance tests for
                                                                                capture system and
                                                                                control device
                                                                                efficiency at sources
                                                                                using these to comply
                                                                                with the standard. Sec.
                                                                                63.4760 specifies the
                                                                                schedule for performance
                                                                                test requirements that
                                                                                are earlier than those
                                                                                specified in Sec.
                                                                                63.7(a)(2).
Sec.   63.7(a)(3)...................  Performance Tests          Yes.................
                                       Required By the
                                       Administrator.
Sec.   63.7(a)(4)...................  Notification of Delay in   Yes.................
                                       Performance Testing Due
                                       to Force Majeure.

Sec.   63.7(b)-(d)..................  Performance Test           Yes.................  Applies only to
                                       Requirements--Notificati                         performance tests for
                                       on, Quality Assurance,                           capture system and add-
                                       Facilities Necessary for                         on control device
                                       Safe Testing, Conditions                         efficiency at sources
                                       During Test.                                     using these to comply
                                                                                with the standard.
Sec.   63.7(e)(1)...................  Performance Testing......  Yes.................
Sec.   63.7(f)......................  Performance Test           Yes.................  Applies to all test
                                       Requirements--Use of                             methods except those
                                       Alternative Test Method.                         used to determine
                                                                                capture system
                                                                                efficiency.
Sec.   63.7(g)-(h)..................  Performance Test           Yes.................  Applies only to
                                       Requirements--Data                               performance tests for
                                       Analysis, Recordkeeping,                         capture system and add-
                                       Reporting, Waiver of                             on control device
                                       Test.                                            efficiency at sources
                                                                                using these to comply
                                                                                with the standard.
Sec.   63.8(a)(1)-(2)...............  Monitoring Requirements--  Yes.................  Applies only to
                                       Applicability.                                   monitoring of capture
                                                                                system and add-on
                                                                                control device
                                                                                efficiency at sources
                                                                                using these to comply
                                                                                with the standard.
                                                                                Additional requirements
                                                                                for monitoring are
                                                                                specified in Sec.
                                                                                63.4768.
Sec.   63.8(a)(3)...................  [Reserved]...............  No..................
Sec.   63.8(a)(4)...................  Additional Monitoring      No..................  Subpart QQQQ does not
                                       Requirements.                                    have monitoring
                                                                                requirements for flares.
Sec.   63.8(b)......................  Conduct of Monitoring....  Yes.................
Sec.   63.8(c)(1)...................  Continuous Monitoring      Yes.................  Applies only to
                                       System (CMS) Operation                           monitoring of capture
                                       and Maintenance.                                 system and add-on
                                                                                control device
                                                                                efficiency at sources
                                                                                using these to comply
                                                                                with the standard.
                                                                                Additional requirements
                                                                                for CMS operations and
                                                                                maintenance are
                                                                                specified in Sec.
                                                                                63.4768.
Sec.   63.8(c)(1)(i)................  General Duty to Minimize   No..................
                                       Emissions and CMS
                                       Operation.
Sec.   63.8(c)(1)(ii)...............  Operation and Maintenance  Yes.................
                                       of CMS.
Sec.   63.8(c)(1)(iii)..............  Requirement to Develop     No..................
                                       SSM Plan for CMS.
Sec.   63.8(c)(2)-(3)...............  Monitoring System          Yes.................
                                       Installation.
Sec.   63.8(c)(4)...................  CMSs.....................  No..................  Sec.   63.4768 specifies
                                                                                the requirements for the
                                                                                operation of CMS for
                                                                                capture systems and add-
                                                                                on control devices at
                                                                                sources using these to
                                                                                comply.
Sec.   63.8(c)(5)...................  COMS.....................  No..................  Subpart QQQQ does not
                                                                                have opacity for visible
                                                                                emission standards.
Sec.   63.8(c)(6)...................  CMS Requirements.........  Yes.................  Sec.   63.4768 specifies
                                                                                the requirements for
                                                                                monitoring systems for
                                                                                capture systems and add-
                                                                                on control devices at
                                                                                sources using these to
                                                                                comply.
Sec.   63.8(c)(7)...................  CMS Out-of-Control         Yes.................
                                       Periods.
Sec.   63.8(c)(8)...................  CMS Out-of-Control         No..................  Sec.   63.4720 requires
                                       Periods Reporting.                               reporting of CMS out-of-
                                                                                control periods.
Sec.   63.8(d)-(e)..................  Quality Control Program    No..................  Subpart QQQQ does not
                                       and CMS Performance                              require the use of
                                       Evaluation.                                      continuous emissions
                                                                                monitoring systems.
Sec.   63.8(f)(1)-(5)...............  Use of an Alternative      Yes.................
                                       Monitoring Method.
Sec.   63.8(f)(6)...................  Alternative to Relative    No..................  Subpart QQQQ does not
                                       Accuracy Test.                                   require the use of
                                                                                continuous emissions
                                                                                monitoring systems.
Sec.   63.8(g)(1)-(5)...............  Data Reduction...........  No..................  Sec.  Sec.   63.4767 and
                                                                                63.4768 specify
                                                                                monitoring data
                                                                                reduction.
Sec.   63.9(a)-(d)..................  Notification Requirements  Yes.................
Sec.   63.9(e)......................  Notification of            Yes.................  Applies only to capture
                                       Performance Test.                                system and add-on
                                                                                control device
                                                                                performance tests at
                                                                                sources using these to
                                                                                comply with the
                                                                                standard.
Sec.   63.9(f)......................  Notification of Visible    No..................  Subpart QQQQ does not
                                       Emissions/Opacity Test.                          have opacity or visible
                                                                                emission standards.
Sec.   63.9(g)(1)-(3)...............  Additional Notifications   No..................  Subpart QQQQ does not
                                       When Using CMS.                                  require the use of
                                                                                continuous emissions
                                                                                monitoring systems.
Sec.   63.9(h)......................  Notification of            Yes.................  Sec.   63.4710 specifies
                                       Compliance Status.                               the dates for submitting
                                                                                the Notification of
                                                                                Compliance Status.
Sec.   63.9(i)......................  Adjustment of Submittal    Yes.................
                                       Deadlines.
Sec.   63.9(j)......................  Change in Previous         Yes.................
                                       Information.
Sec.   63.10(a).....................  Recordkeeping/Reporting--  Yes.................
                                       Applicability and
                                       General Information.
Sec.   63.10(b)(1)..................  General Recordkeeping      Yes.................  Additional requirements
                                       Requirements.                                    are specified in Sec.
                                                                                Sec.   63.4730 and
                                                                                63.4731.
Sec.   63.10(b)(2)(i)-(ii)..........  Recordkeeping of           No..................
                                       Occurrence and Duration
                                       of Startups and
                                       Shutdowns.
Sec.   63.10(b)(2)(iii).............  Recordkeeping Relevant to  Yes.................
                                       CMS.
Sec.   63.10(b)(2)(iv)-(v)..........  Recordkeeping Relevant to  No..................
                                       SSM.
Sec.   63.10(b)(2)(vi)-(xi).........  Recordkeeping for CMS      Yes.................
                                       Malfunctions.
Sec.   63.10(b)(2)(xii).............  Records..................  Yes.................

Sec.   63.10(b)(2)(xiii)............  .........................  No..................  Subpart QQQQ does not
                                                                                require the use of
                                                                                continuous emissions
                                                                                monitoring systems.
Sec.   63.10(b)(2)(xiv).............  .........................  Yes.................
Sec.   63.10(b)(3)..................  Recordkeeping              Yes.................
                                       Requirements for
                                       Applicability
                                       Determinations.
Sec.   63.10(c)(1)-(6)..............  Additional Recordkeeping   Yes.................
                                       Requirements for Sources
                                       with CMS.
Sec.   63.10(c)(7)-(8)..............  .........................  No..................  The same records are
                                                                                required in Sec.
                                                                                63.4720(a)(7).
Sec.   63.10(c)(9)-(14).............  .........................  Yes.................
Sec.   63.10(c)(15).................  Use of SSM Plan..........  No..................
Sec.   63.10(d)(1)..................  General Reporting          Yes.................  Additional requirements
                                       Requirements.                                    are specified in Sec.
                                                                                63.4720.
Sec.   63.10(d)(2)..................  Report of Performance      Yes.................  Additional requirements
                                       Test Results.                                    are specified in Sec.
                                                                                63.4720(b).
Sec.   63.10(d)(3)..................  Reporting Opacity or       No..................  Subpart QQQQ does not
                                       Visible Emissions                                require opacity or
                                       Observations.                                    visible emissions
                                                                                observations.
Sec.   63.10(d)(4)..................  Progress Reports for       Yes.................
                                       Sources With Compliance
                                       Extensions.
Sec.   63.10(d)(5)..................  SSM Reports..............  No..................  Malfunctions shall be
                                                                                reported based on
                                                                                compliance option under
                                                                                Sec.   63.4720(a)(5-7).
Sec.   63.10(e)(1)-(2)..............  Additional CMS Reports...  No..................  Subpart QQQQ does not
                                                                                require the use of
                                                                                continuous emissions
                                                                                monitoring systems.
Sec.   63.10(e)(3)..................  Excess Emissions/CMS       No..................  Sec.   63.4720(b)
                                       Performance Reports.                             specifies the contents
                                                                                of periodic compliance
                                                                                reports.
Sec.   63.10(e)(4)..................  COMS Data Reports........  No..................  Subpart QQQQ does not
                                                                                specify requirements for
                                                                                opacity or COMS.
Sec.   63.10(f).....................  Recordkeeping/Reporting    Yes.................
                                       Waiver.
Sec.   63.11........................  Control Device             No..................  Subpart QQQQ does not
                                       Requirements/Flares.                             specify use of flares
                                                                                for compliance.
Sec.   63.12........................  State Authority and        Yes.................
                                       Delegations.
Sec.   63.13........................  Addresses................  Yes.................
Sec.   63.14........................  Incorporation by           Yes.................  Test Methods ANSI A135.4-
                                       Reference.                                       2012, ANSI/ASME PTC
                                                                                19.10-1981, Part 10,
                                                                                ASTM D1475-13, ASTM
                                                                                D2111-10 (Reapproved
                                                                                2015), ASTM D2369-10
                                                                                (Reapproved 2015) \e\,
                                                                                ASTM D2697-03
                                                                                (Reapproved 2014), ASTM
                                                                                D4840-99 (2018) \e\,
                                                                                ASTM D6093-97
                                                                                (Reapproved 2016), ASTM
                                                                                D6348-03 (Reapproved
                                                                                2010) and NCASI Method
                                                                                ISS/FP A105.01
                                                                                (incorporated by
                                                                                reference, see Sec.
                                                                                63.14).
Sec.   63.15........................  Availability of            Yes.................
                                       Information/
                                       Confidentiality.
Sec.   63.16........................  Requirements for           Yes.................
                                       Performance Track Member
                                       Facilities.
----------------------------------------------------------------------------------------------------------------

0
19. Appendix A to part 63 is amended by adding Method 326 in numerical
order to read as follows:

Appendix A to Part 63--Test Methods

* * * * *

Method 326--Method for Determination of Isocyanates in Stationary
Source Emissions

1.0 Scope and Application

    This method is applicable to the collection and analysis of
isocyanate compounds from the emissions associated with
manufacturing processes. This method is not inclusive with respect
to specifications (e.g., equipment and supplies) and sampling
procedures essential to its performance. Some material is
incorporated by reference from other EPA methods. Therefore, to
obtain reliable results, persons using this method should have a
thorough knowledge of at least Method 1, Method 2, Method 3, and
Method 5 found in Appendices A-1, A-2, and A-3 in Part 60 of this
title.
    1.1 Analytes. This method is designed to determine the mass
emission of isocyanates being emitted from manufacturing processes.
The following is a table (Table 1-1) of the isocyanates and the
manufacturing process at which the method has been evaluated:

                                              Table 326-1--Analytes
----------------------------------------------------------------------------------------------------------------
                                                                   Detection
                Compound's name                     CAS No.       limit (ng/          Manufacturing process
                                                                   m\3\) \a\
----------------------------------------------------------------------------------------------------------------
2,4-Toluene Diisocyanate (TDI)................        584-84-9             106  Flexible Foam Production.
1,6-Hexamethylene Diisocyanate (HDI)..........        822-06-0             396  Paint Spray Booth.
Methylene Diphenyl Diisocyanate (MDI).........        101-68-8             112  Pressed Board Production.
Methyl Isocyanate (MI)........................        624-83-0             228  Not used in production.
----------------------------------------------------------------------------------------------------------------
\a\ Estimated detection limits are based on a sample volume of 1 m\3\ and a 10-ml sample extraction volume.

    1.2 Applicability. Method 326 is a method designed for
determining compliance with National Emission Standards for
Hazardous Air Pollutants (NESHAP). Method 326 may also be specified
by New Source Performance Standards (NSPS), State Implementation
Plans (SIPs), and operating permits that require measurement of
isocyanates in stationary source emissions, to determine compliance
with an applicable emission standard or limit.
    1.3 Data Quality Objectives (DQO). The principal objective is to
ensure the accuracy of the data at the actual emissions levels and
in the actual emissions matrix encountered. To meet this objective,
method performance tests are required and NIST-traceable calibration
standards must be used.

2.0 Summary of Method

    2.1 Gaseous and/or aerosol isocyanates are withdrawn from an
emission source at an isokinetic sampling rate and are collected in
a multicomponent sampling train. The primary components of the train
include a heated probe, three impingers containing derivatizing
reagent in toluene, an empty impinger, an impinger containing
charcoal, and an impinger containing silica gel.
    2.2 The liquid impinger contents are recovered, concentrated to
dryness under vacuum, brought to volume with acetonitrile (ACN) and
analyzed with a high pressure liquid chromatograph (HPLC).

3.0 Definitions [Reserved]

4.0 Interferences

    4.1 The greatest potential for interference comes from an
impurity in the derivatizing reagent, 1-(2-pyridyl)piperazine (1,2-
PP). This compound may interfere with the resolution of MI from the
peak attributed to unreacted 1,2-PP.
    4.2 Other interferences that could result in positive or
negative bias are (1) alcohols that could compete with the 1,2-PP
for reaction with an isocyanate and (2) other compounds that may co-
elute with one or more of the derivatized isocyanates.
    4.3 Method interferences may be caused by contaminants in
solvents, reagents, glassware, and other sample processing hardware.
All these materials must be routinely shown to be free from
interferences under conditions of the analysis by preparing and
analyzing laboratory method (or reagent) blanks.
    4.3.1 Glassware must be cleaned thoroughly before using. The
glassware should be washed with laboratory detergent in hot water
followed by rinsing with tap water and distilled water. The
glassware may be dried by baking in a glassware oven at 400 [deg]C
for at least one hour. After the glassware has cooled, it should be
rinsed three times with methylene chloride and three times with
acetonitrile. Volumetric glassware should not be heated to 400
[deg]C. Instead, after washing and rinsing, volumetric glassware may
be rinsed with acetonitrile followed by methylene chloride and
allowed to dry in air.
    4.3.2 The use of high purity reagents and solvents helps to
reduce interference problems in sample analysis.

5.0 Safety

    5.1 Organizations performing this method are responsible for
maintaining a current awareness file of Occupational Safety and
Health Administration (OSHA) regulations regarding safe handling of
the chemicals specified in this method. A reference file of material
safety data sheets should also be made available to all personnel
involved in performing the method. Additional references to
laboratory safety are available.

6.0 Equipment and Supplies

    6.1 Sample Collection. A schematic of the sampling train used in
this method is shown in Figure 207-1. This sampling train
configuration is adapted from Method 5 procedures, and, as such,
most of the required equipment is identical to that used in Method 5
determinations. The only new component required is a condenser.
    6.1.1 Probe Nozzle. Borosilicate or quartz glass; constructed
and calibrated according to Method 5, sections <IP_ADDRESS> and 10.1, and
coupled to the probe liner using a Teflon union; a stainless steel
nut is recommended for this union. When the stack temperature
exceeds 210 [deg]C (410 [deg]F), a one-piece glass nozzle/liner
assembly must be used.
    6.1.2 Probe Liner. Same as Method 5, section <IP_ADDRESS>, except
metal liners shall not be used. Water-cooling of the stainless steel
sheath is recommended at temperatures exceeding 500 [deg]C (932
[deg]F). Teflon may be used in limited applications where the
minimum stack temperature exceeds 120 [deg]C (250 [deg]F) but never
exceeds the temperature where Teflon is estimated to become unstable
[approximately 210 [deg]C (410 [deg]F)].
    6.1.3 Pitot Tube, Differential Pressure Gauge, Filter Heating
System, Metering System, Barometer, Gas Density Determination
Equipment. Same as Method 5, sections <IP_ADDRESS>, <IP_ADDRESS>, <IP_ADDRESS>,
<IP_ADDRESS>, 6.1.2, and 6.1.3.
    6.1.4 Impinger Train. Glass impingers are connected in series
with leak-free ground-glass joints following immediately after the
heated probe. The first impinger shall be of the Greenburg-Smith
design with the standard tip. The remaining five impingers shall be
of the modified Greenburg-Smith design, modified by replacing the
tip with a 1.3-cm (\1/2\-in.) I.D. glass tube extending about 1.3 cm
(\1/2\ in.) from the bottom of the outer cylinder. A water-jacketed
condenser is placed between the outlet of the first impinger and the
inlet to the second impinger to reduce the evaporation of toluene
from the first impinger.
    6.1.5 Moisture Measurement. For the purpose of calculating
volumetric flow rate and isokinetic sampling, you must also collect
either Method 4 in Appendix A-3 to this part or other moisture
measurement methods approved by the Administrator concurrent with
each Method 326 test run.
    6.2 Sample Recovery
    6.2.1 Probe and Nozzle Brushes; Polytetrafluoroethylene (PTFE)
bristle brushes with stainless steel wire or PTFE handles are
required. The probe brush shall have extensions constructed of
stainless steel, PTFE, or inert material at least as long as the
probe. The brushes shall be properly sized and shaped to brush out
the probe liner and the probe nozzle.
    6.2.2 Wash Bottles. Three. PTFE or glass wash bottles are
recommended; polyethylene wash bottles must not be used because
organic contaminants may be extracted by exposure to organic
solvents used for sample recovery.
    6.2.3 Glass Sample Storage Containers. Chemically resistant,
borosilicate amber glass bottles, 500-mL or 1,000-mL. Bottles should
be tinted to prevent the action of light on the sample. Screw-cap
liners shall be either PTFE or constructed to be leak-free and
resistant to chemical attack by organic recovery solvents. Narrow-
mouth glass bottles have been found to leak less frequently.
    6.2.4 Graduated Cylinder. To measure impinger contents to the
nearest 1 ml or 1 g. Graduated cylinders shall have subdivisions not
>2 mL.
    6.2.5 Plastic Storage Containers. Screw-cap polypropylene or
polyethylene containers to store silica gel and charcoal.
    6.2.6 Funnel and Rubber Policeman. To aid in transfer of silica
gel or charcoal to container (not necessary if silica gel is weighed
in field).
    6.2.7 Funnels. Glass, to aid in sample recovery.
    6.3 Sample Preparation and Analysis.
    The following items are required for sample analysis.
    6.3.1 Rotary Evaporator. Buchii Model EL-130 or equivalent.
    6.3.2 1000 ml Round Bottom Flask for use with a rotary
evaporator.
    6.3.3 Separatory Funnel. 500-ml or larger, with PTFE stopcock.
    6.3.4 Glass Funnel. Short-stemmed or equivalent.
    6.3.5 Vials. 15-ml capacity with PTFE lined caps.
    6.3.6 Class A Volumetric Flasks. 10-ml for bringing samples to
volume after concentration.
    6.3.7 Filter Paper. Qualitative grade or equivalent.
    6.3.8 Buchner Funnel. Porcelain with 100 mm ID or equivalent.
    6.3.9 Erlenmeyer Flask. 500-ml with side arm and vacuum source.
    6.3.10 HPLC with at least a binary pumping system capable of a
programmed gradient.
    6.3.11 Column Systems Column systems used to measure isocyanates
must be capable of achieving separation of the target compounds from
the nearest eluting compound or interferents with no more than 10
percent peak overlap.
    6.3.12 Detector. UV detector at 254 nm. A fluorescence detector
(FD) with an excitation of 240 nm and an emission at 370 nm may be
also used to allow the detection of low concentrations of
isocyanates in samples.
    6.3.13 Data system for measuring peak areas and retention times.

7.0 Reagents and Standards

    7.1 Sample Collection Reagents.
    7.1.1 Charcoal. Activated, 6-16 mesh. Used to absorb toluene
vapors and prevent them from entering the metering device. Use once
with each train and discard.
    7.1.2 Silica Gel and Crushed Ice. Same as Method 5, sections
7.1.2 and 7.1.4 respectively

    7.1.3 Impinger Solution. The impinger solution is prepared by
mixing a known amount of 1-(2-pyridyl) piperazine (purity 99.5+%) in
toluene (HPLC grade or equivalent). The actual concentration of 1,2-
PP should be approximately four times the amount needed to ensure
that the capacity of the derivatizing solution is not exceeded. This
amount shall be calculated from the stoichiometric relationship
between 1,2-PP and the isocyanate of interest and preliminary
information about the concentration of the isocyanate in the stack
emissions. A concentration of 130 [micro]g/ml of 1,2-PP in toluene
can be used as a reference point. This solution shall be prepared,
stored in a refrigerated area away from light, and used within ten
days of preparation.
    7.2 Sample Recovery Reagents.
    7.2.1 Toluene. HPLC grade is required for sample recovery and
cleanup (see Note to 7.2.2 below).
    7.2.2 Acetonitrile. HPLC grade is required for sample recovery
and cleanup. Note: Organic solvents stored in metal containers may
have a high residue blank and should not be used. Sometimes
suppliers transfer solvents from metal to glass bottles; thus blanks
shall be run before field use and only solvents with a low blank
value should be used.
    7.3 Analysis Reagents. Reagent grade chemicals should be used in
all tests. All reagents shall conform to the specifications of the
Committee on Analytical Reagents of the American Chemical Society,
where such specifications are available.
    7.3.1 Toluene, C6H5CH3. HPLC
Grade or equivalent.
    7.3.2 Acetonitrile, CH3CN (ACN). HPLC Grade or
equivalent.
    7.3.3 Methylene Chloride, CH2Cl2. HPLC
Grade or equivalent.
    7.3.4 Hexane, C6H14. HPLC Grade or
equivalent.
    7.3.5 Water, H2O. HPLC Grade or equivalent.
    7.3.6 Ammonium Acetate,
CH3CO2NH4.
    7.3.7 Acetic Acid (glacial), CH3CO2H.
    7.3.8 1-(2-Pyridyl)piperazine, (1,2-PP), >=99.5% or equivalent.
    7.3.9 Absorption Solution. Prepare a solution of 1-(2-
pyridyl)piperazine in toluene at a concentration of 40 mg/300 ml.
This solution is used for method blanks and method spikes.
    7.3.10 Ammonium Acetate Buffer Solution (AAB). Prepare a
solution of ammonium acetate in water at a concentration of 0.1 M by
transferring 7.705 g of ammonium acetate to a 1,000 ml volumetric
flask and diluting to volume with HPLC Grade water. Adjust pH to 6.2
with glacial acetic acid.

8.0 Sample Collection, Storage and Transport

    Note:  Because of the complexity of this method, field personnel
should be trained in and experienced with the test procedures in
order to obtain reliable results.

    8.1 Sampling
    8.1.1 Preliminary Field Determinations. Same as Method 5,
section 8.2.
    8.1.2 Preparation of Sampling Train. Follow the general
procedure given in Method 5, section 8.3.1, except for the following
variations: Place 300 ml of the impinger absorbing solution in the
first impinger and 200 ml each in the second and third impingers.
The fourth impinger shall remain empty. The fifth and sixth
impingers shall have 400 g of charcoal and 200-300 g of silica gel,
respectively. Alternatively, the charcoal and silica gel may be
combined in the fifth impinger. Set-up the train as in Figure 326-1.
During assembly, do not use any silicone grease on ground-glass
joints.

    Note:  During preparation and assembly of the sampling train,
keep all openings where contamination can occur covered with PTFE
film or aluminum foil until just before assembly or until sampling
is about to begin.

    8.1.3 Leak-Check Procedures. Follow the leak-check procedures
given in Method 5, sections 8.4.2 (Pretest Leak-Check), 8.4.3 (Leak-
Checks During the Sample Run), and 8.4.4 (Post-Test Leak-Check),
with the exception that the pre-test leak-check is mandatory
    8.1.4 Sampling Train Operation. Follow the general procedures
given in Method 5, section 8.5. Turn on the condenser coil coolant
recirculating pump and monitor the gas entry temperature. Ensure
proper gas entry temperature before proceeding and again before any
sampling is initiated. It is important that the gas entry
temperature not exceed 50 [deg]C (122 [deg]F), thus reducing the
loss of toluene from the first impinger. For each run, record the
data required on a data sheet such as the one shown in Method 5,
Figure 5-3.
    8.2 Sample Recovery. Allow the probe to cool. When the probe can
be handled safely, wipe off all external particulate matter near the
tip of the probe nozzle and place a cap over the tip to prevent
losing or gaining particulate matter. Do not cap the probe tip
tightly while the sampling train is cooling down because this will
create a vacuum in the train. Before moving the sample train to the
cleanup site, remove the probe from the sample train and cap the
opening to the probe, being careful not to lose any condensate that
might be present. Cap the impingers and transfer the probe and the
impinger/condenser assembly to the cleanup area. This area should be
clean and protected from the weather to reduce sample contamination
or loss. Inspect the train prior to and during disassembly and
record any abnormal conditions. It is not necessary to measure the
volume of the impingers for the purpose of moisture determination as
the method is not validated for moisture determination. Treat
samples as follows:
    8.2.1 Container No. 1, Probe and Impinger Numbers 1 and 2. Rinse
and brush the probe/nozzle first with toluene twice and then twice
again with acetonitrile and place the wash into a glass container
labeled with the test run identification and ``Container No. 1.''
When using these solvents ensure that proper ventilation is
available. Quantitatively transfer the liquid from the first two
impingers and the condenser into Container No. 1. Rinse the
impingers and all connecting glassware twice with toluene and then
twice again with acetonitrile and transfer the rinses into Container
No. 1. After all components have been collected in the container,
seal the container, and mark the liquid level on the bottle.
    8.2.2 Container No. 2, Impingers 3 and 4. Quantitatively
transfer the liquid from each impinger into a glass container
labeled with the test run identification and ``Container No. 2.''
Rinse each impinger and all connecting glassware twice with toluene
and twice again with acetonitrile and transfer the rinses into
Container No. 2. After all components have been collected in the
container, seal the container, and mark the liquid level on the
bottle.

    Note:  The contents of the fifth and sixth impinger (silica gel)
can be discarded.

    8.2.3 Container No. 3, Reagent Blank. Save a portion of both
washing solutions (toluene/acetonitrile) used for the cleanup as a
blank. Transfer 200 ml of each solution directly from the wash
bottle being used and combine in a glass sample container with the
test identification and ``Container No. 3.'' Seal the container, and
mark the liquid level on the bottle and add the proper label.
    8.2.4 Field Train Proof Blanks. To demonstrate the cleanliness
of sampling train glassware, you must prepare a full sampling train
to serve as a field train proof blank just as it would be prepared
for sampling. At a minimum, one complete sampling train will be
assembled in the field staging area, taken to the sampling area, and
leak-checked. The probe of the blank train shall be heated during
and the train will be recovered as if it were an actual test sample.
No gaseous sample will be passed through the sampling train. Field
blanks are recovered in the same manner as described in sections
8.2.1 and 8.2.2 and must be submitted with the field samples
collected at each sampling site.
    8.2.5 Field Train Spike. To demonstrate the effectiveness of the
sampling train, field handling, and recovery procedures you must
prepare a full sampling train to serve as a field train spike just
as it would be prepared for sampling. The field spike is performed
in the same manner as the field train proof blank with the
additional step of adding the Field Spike Solution to the first
impinger after the initial leak check. The train will be recovered
as if it were an actual test sample. No gaseous sample will be
passed through the sampling train. Field train spikes are recovered
in the same manner as described in sections 8.2.1 and 8.2.2 and must
be submitted with the samples collected for each test program.
    8.3 Sample Transport Procedures. Containers must remain in an
upright position at all times during shipment. Samples must also be
stored at <4 [deg]C between the time of sampling and concentration.
Each sample should be extracted and concentrated within 30 days
after collection and analyzed within 30 days after extraction. The
extracted sample must be stored at 4 [deg]C.
    8.4 Sample Custody. Proper procedures and documentation for
sample chain of custody are critical to ensuring data integrity. The
chain of custody procedures in ASTM D4840-99 (Reapproved 2018) \e\
``Standard Guide for Sampling Chain-of-Custody Procedures''
(incorporated by reference, see Sec.  63.14) shall be followed for
all samples (including field samples and blanks).

9.0 Quality Control

    9.1 Sampling. Sampling Operations. The sampling quality control
procedures and acceptance criteria are listed in Table 326-2 below;
see also section 9.0 of Method 5.
    9.2 Analysis. The analytical quality control procedures required
for this method includes the analysis of the field train proof
blank, field train spike, and reagent and method blanks. Analytical
quality control procedures and acceptance criteria are listed in
Table 326-3 below.
    9.2.1 Check for Breakthrough. Recover and determine the
isocyanate(s) concentration of the last two impingers separately
from the first two impingers.
    9.2.2 Field Train Proof Blank. Field blanks must be submitted
with the samples collected at each sampling site.
    9.2.3 Reagent Blank and Field Train Spike. At least one reagent
blank and a field train spike must be submitted with the samples
collected for each test program.
    9.2.4 Determination of Method Detection Limit. Based on your
instrument's sensitivity and linearity, determine the calibration
concentrations or masses that make up a representative low level
calibration range. The MDL must be determined at least annually for
the analytical system using an MDL study such as that found in
section 15.0 to Method 301 of appendix A to part 63 of this chapter.

                           Table 326-2--Sampling Quality Assurance and Quality Control
----------------------------------------------------------------------------------------------------------------
          QA/QC criteria                Acceptance criteria           Frequency          Consequence if not met
----------------------------------------------------------------------------------------------------------------
Sampling Equipment Leak Checks....  <=0.00057 m3/min (0.020     Prior to, during       Prior to: Repair and
                                     cfm) or 4% of sampling      (optional) and at      repeat calibration.
                                     rate, whichever is less.    the completion to      During/Completion: None,
                                                                 sampling.              testing should be
                                                                                considered invalid.
Dry Gas Meter Calibration--Pre-     within 2% of    Pre-test.............  Repeat calibration point.
 Test (individual correction         average factor
 factor--Yi).                        (individual).
Dry Gas Meter Calibration--Pre-     1.00 1%.......  Pre-test.............  Adjust the dry gas meter
 Test (average correction factor--                                                      and recalibrate.
 Yc).
Dry Gas Meter Calibration--Post-    Average dry gas meter       Each Test............  Adjust sample volumes
 test.                               calibration factor agrees                          using the factor that
                                     with 5% Yc.                            gives the smallest
                                                                                volume.
Temperature sensor calibration....  Absolute temperature        Prior to initial use   Recalibrate; sensor may
                                     measures by sensor within   and before each test   not be used until
                                     1.5% of a       thereafter.            specification is met.
                                     reference sensor.
Barometer calibration.............  Absolute pressure measured  Prior to initial use   Recalibrate; instrument
                                     by instrument within        and before each test   may not be used until
                                     10 mm Hg of     thereafter.            specification is met.
                                     reading with a mercury
                                     barometer or NIST
                                     traceable barometer.
----------------------------------------------------------------------------------------------------------------

                          Table 326-3--Analytical Quality Assurance and Quality Control
----------------------------------------------------------------------------------------------------------------
          QA/QC criteria                Acceptance criteria           Frequency          Consequence if not met
----------------------------------------------------------------------------------------------------------------
Calibration--Method Blanks........  <5% level of expected       Each analytical        Locate source of
                                     analyte.                    method blank.          contamination;
                                                                                reanalyze.
Calibration--Calibration Points...  At least six calibration    Each analytical batch  Incorporate additional
                                     point bracketing the                               calibration points to
                                     expected range of                                  meet criteria.
                                     analysis.
Calibration--Linearity............  Correlation coefficient     Each analytical batch  Verify integration,
                                     >0.995.                                            reintegrate. If
                                                                                necessary, recalibrate.
Calibration--secondary standard     Within 10% of   After each             Repeat secondary standard
 verification.                       true value.                 calibration.           verification,
                                                                                recalibrate if
                                                                                necessary.
Calibration--continual calibration  Within 10% of   Daily and after every  Invalidate previous ten
 verification.                       true value.                 ten samples.           sample analysis,
                                                                                recalibrate and repeat
                                                                                calibration, reanalyze
                                                                                samples until
                                                                                successful.
Sample Analysis...................  Within the valid            Each sample..........  Invalidate the sample if
                                     calibration range.                                 greater than the
                                                                                calibration range and
                                                                                dilute the sample so
                                                                                that it is within the
                                                                                calibration range.
                                                                                Appropriately flag any
                                                                                value below the
                                                                                calibration range.
Replicate Samples.................  Within 10% of   Each sample..........  Evaluate integrations and
                                     RPD.                                               repeat sample analysis
                                                                                as necessary.
Field Train Proof Blank...........  <=10% level of expected     Each test program....  Evaluate source of
                                     analyte.                                           contamination.
Field Train Spike.................  Within 30% of   Each test program....  Evaluate performance of
                                     true value.                                        the method and consider
                                                                                invalidating results.
Breakthrough......................  Final two impingers Mass    Each test run........  Invalidate test run.
                                     collected is >5% of the
                                     total mass or >20% of the
                                     total mass when the
                                     measured results are 20%
                                     of the applicable
                                     standard. Alternatively,
                                     there is no breakthrough
                                     requirement when the
                                     measured results are 10%
                                     of the applicable
                                     standard.
----------------------------------------------------------------------------------------------------------------

10.0 Calibration and Standardization

    Note: Maintain a laboratory log of all calibrations.

    10.1 Probe Nozzle, Pitot Tube Assembly, Dry Gas Metering System,
Probe Heater, Temperature Sensors, Leak-Check of Metering System,
and Barometer. Same as Method 5, sections 10.1, 10.2, 10.3, 10.4,
10.5, 8.4.1, and 10.6, respectively.
    10.2 High Performance Liquid Chromatograph. Establish the
retention times for the isocyanates of interest; retention times
will depend on the chromatographic conditions. The retention times
provided in Table 10-1 are provided as a guide to relative retention
times when using a C18, 250 mm x 4.6 mm ID, 5[micro]m particle size
column, a 2 ml/min flow rate of a 1:9 to 6:4 Acetonitrile/Ammonium
Acetate Buffer, a 50 [micro]l sample loop, and a UV detector set at
254 nm.

                  Table 326-4--Example Retention Times
------------------------------------------------------------------------
                             Retention times
-------------------------------------------------------------------------
                                                          Retention time
                        Compound                             (minutes)
------------------------------------------------------------------------
MI......................................................            10.0
1,6-HDI.................................................            19.9
2,4-TDI.................................................            27.1
MDI.....................................................            27.3
------------------------------------------------------------------------

    10.3 Preparation of Isocyanate Derivatives.
    10.3.1 HDI, TDI, MDI. Dissolve 500 mg of each isocyanate in
individual 100 ml aliquots of methylene chloride (MeCl2),
except MDI which requires 250 ml of MeCl2. Transfer a 5-
ml aliquot of 1,2-PP (see section 7.3.8) to each solution, stir and
allow to stand overnight at room temperature. Transfer 150 ml
aliquots of hexane to each solution to precipitate the isocyanate-
urea derivative. Using a Buchner funnel, vacuum filter the solid-
isocyanate-urea derivative and rinse with 50 ml of hexane. Dissolve
the precipitate in a minimum aliquot of MeCl2. Repeat the
hexane precipitation and filtration twice. After the third
filtration, dry the crystals at 50 [deg]C and transfer to bottles
for storage. The crystals are stable for at least 21 months when
stored at room temperature in a closed container.
    10.3.2 MI. Prepare a 200 [mu]g/ml stock solution of methyl
isocyanate-urea, transfer 60 mg of 1,2-PP to a 100-ml volumetric
flask containing 50 ml of MeCl2. Carefully transfer 20 mg
of methyl isocyanate to the volumetric flask and shake for 2
minutes. Dilute the solution to volume with MeCl2 and
transfer to a bottle for storage. Methyl isocyanate does not produce
a solid derivative and standards must be prepared from this stock
solution.
    10.4 Preparation of calibration standards. Prepare a 100 [mu]g/
ml stock solution of the isocyanates of interest from the individual
isocyanate-urea derivative as prepared in sections 10.3.1 and
10.3.2. This is accomplished by dissolving 1 mg of each isocyanate-
urea derivative in 10 ml of Acetonitrile. Calibration standards are
prepared from this stock solution by making appropriate dilutions of
aliquots of the stock into Acetonitrile.
    10.5 Preparation of Method Blanks. Prepare a method blank for
each test program (up to twenty samples) by transferring 300 ml of
the absorption solution to a 1,000-ml round bottom flask and
concentrate as outlined in section 11.2.
    10.6 Preparation of Field Spike Solution. Prepare a field spike
solution for every test program in the same manner as calibration
standards (see Section 10.4). The mass of the target isocyanate in
the volume of the spike solution for the field spike train shall be
equivalent to that estimated to be captured from the source
concentration for each compound; alternatively, you may also prepare
a solution that represents half the applicable standard.
    10.7 HPLC Calibrations. See Section 11.1.

11.0 Analytical Procedure

    11.1 Analytical Calibration. Perform a multipoint calibration of
the instrument at six or more upscale points over the desired
quantitative range (multiple calibration ranges shall be calibrated,
if necessary). The field samples analyzed must fall within at least
one of the calibrated quantitative ranges and meet the performance
criteria specified below. The lowest point in your calibration curve
must be at least 5, and preferably 10, times the MDL. For each
calibration curve, the value of the square of the linear correlation
coefficient, i.e., r\2\, must be >=0.995, and the analyzer response
must be within 10 percent of the reference value at each
upscale calibration point. Calibrations must be performed on each
day of the analysis, before analyzing any of the samples. Following
calibration, a secondary standard shall be analyzed. A continual
calibration verification (CCV) must also be performed prior to any
sample and after every ten samples. The measured value of this
independently prepared standard must be within 10
percent of the expected value. Report the results for each
calibration standard secondary standard, and CCV as well as the
conditions of the HPLC. The reports should include at least the peak
area, height, and retention time for each isocyanate compound
measured as well as a chromatogram for each standard.
    11.2 Concentration of Samples. Transfer each sample to a 1,000-
ml round bottom flask. Attach the flask to a rotary evaporator and
gently evaporate to dryness under vacuum in a 65 [deg]C water bath.
Rinse the round bottom flask three times each with 2 ml of
acetonitrile and transfer the rinse to a 10-ml volumetric flask.
Dilute the sample to volume with acetonitrile and transfer to a 15-
ml vial and seal with a PTFE lined lid. Store the vial <=4 [deg]C
until analysis.
    11.3 Analysis. Analyze replicative samples by HPLC, using the
appropriate conditions established in section 10.2. The width of the
retention time window used to make identifications should be based
upon measurements of actual retention time variations of standards
over the course of a day. Three times the standard deviation of a
retention time for a compound can be used to calculate a suggested
window size; however, the experience of the analyst should weigh
heavily in the interpretation of the chromatograms. If the peak area
exceeds the linear range of the calibration curve, the sample must
be diluted with acetonitrile and reanalyzed. Average the replicate
results for each run. For each sample you must report the same
information required for analytical calibrations (Section 11.1). For
non-detect or values below the detection limit of the method, you
shall report the value as ``<'' numerical detection limit.

12.0 Data Analysis and Calculations

    Nomenclature and calculations, same as in Method 5, section 6,
with the following additions below.
    12.1 Nomenclature.

AS = Response of the sample, area counts.
b = Y-intercept of the linear regression line, area counts.
BR = Percent Breakthrough
CA = Concentration of a specific isocyanate compound in
the initial sample, [micro]g/ml.
CB = Concentration of a specific isocyanate compound in
the replicate sample, [micro]g/ml.
CI = Concentration of a specific isocyanate compound in
the sample, [micro]g/ml.
Crec = Concentration recovered from spike train,
[micro]g/ml.
CS = Concentration of isocyanate compound in the stack
gas, [micro]g/dscm
CT = Concentration of a specific isocyanate compound
(Impingers 1-4), [micro]g/dscm
Cspike = Concentration spiked, [micro]g/ml.
C4 = Concentration of a specific isocyanate compound
(Impingers 14), [micro]g/dscm
FIm = Mass of Free Isocyanate
FTSrec = Field Train Spike Recovery
Im = Mass of the Isocyanate
Imw = MW of the Isocyanate
IUm = Mass of Isocyanate-urea derivative
IUmw = MW of the isocyanate-urea
M = Slope of the linear regression line, area counts-ml/[micro]g.
mI = Mass of isocyanate in the total sample
MW = Molecular weight
RPD = Relative Percent Difference
VF = Final volume of concentrated sample, typically 10 ml.
Vmstd = Volume of gas sample measured by the dry-gas
meter, corrected to standard conditions, dscm (dscf).

12.2 Conversion from Isocyanate to the Isocyanate-urea derivative.
The equation for converting the amount of free isocyanate to the

    corresponding amount of isocyanate-urea derivative is as follows:
12.2 Conversion from Isocyanate to the Isocyanate-urea derivative.
The equation for converting the amount of free isocyante to the
corresponding amount of isocyante-urea derivative is as follows:
[GRAPHIC] [TIFF OMITTED] TR04MR19.001

The equation for converting the amount of IU derivative to the
corresponding amount of FLm is as follows:
[GRAPHIC] [TIFF OMITTED] TR04MR19.002

    12.3 Calculate the correlation coefficient, slope, and
intercepts for the calibration data

using the least squares method for linear regression. Concentrations
are expressed as the x-variable and response is expressed as the y-
variable.
    12.4 Calculate the concentration of isocyanate in the sample:
    [GRAPHIC] [TIFF OMITTED] TR04MR19.003

    12.5 Calculate the total amount collected in the sample by
multiplying the concentration ([mu]g/ml) times the final volume of
acetonitrile (10 ml).
[GRAPHIC] [TIFF OMITTED] TR04MR19.004

    12.6 Calculate the concentration of isocyanate ([mu]g/dscm) in
the stack gas.
[GRAPHIC] [TIFF OMITTED] TR04MR19.005

    12.7 Calculate Relative Percent Difference (RPD) for each
replicative sample
[GRAPHIC] [TIFF OMITTED] TR04MR19.006

    12.8 Calculate Field Train Spike Recovery
    [GRAPHIC] [TIFF OMITTED] TR04MR19.007

    12.9 Calculate Percent Breakthrough
    [GRAPHIC] [TIFF OMITTED] TR04MR19.008

Where:

K = 35.314 ft\3\/m\3\ if Vm(std) is expressed in English units. =
1.00 m\3\/m\3\ if Vm(std) is expressed in metric units.

13.0 Method Performance

    Evaluation of sampling and analytical procedures for a selected
series of compounds must meet the quality control criteria (See
Section 9) for each associated analytical determination. The
sampling and analytical procedures must be challenged by the test
compounds spiked at appropriate levels and carried through the
procedures.

14.0 Pollution Prevention [Reserved]

15.0 Waste Management [Reserved]

16.0 Alternative Procedures [Reserved]

17.0 References

1. Martin, R.M., Construction Details of Isokinetic Source-Sampling
Equipment, Research Triangle Park, NC, U.S. Environmental Protection
Agency, April 1971, PB-203 060/BE, APTD-0581, 35 pp.
2. Rom, J.J., Maintenance, Calibration, and Operation of Isokinetic
Source Sampling Equipment, Research Triangle Park, NC, U.S.
Environmental Protection Agency, March 1972, PB-209 022/BE, APTD-
0576, 39 pp.
3. Schlickenrieder, L.M., Adams, J.W., and Thrun, K.E., Modified
Method 5 Train and Source Assessment Sampling System: Operator's
Manual, U.S. Environmental Protection Agency, EPA/600/8-85/003/
1985).
4. Shigehara, R.T., Adjustments in the EPA Nomograph for Different
Pitot Tube Coefficients and Dry Molecular Weights, Stack Sampling
News, 2:4-11 (October 1974).
5. U.S. Environmental Protection Agency, 40 CFR part 60, Appendices
A-1, A-2, and A-3, Methods 1-5.
6. Vollaro, R.F., A Survey of Commercially Available Instrumentation
for the Measurement of Low-Range Gas Velocities, Research Triangle
Park, NC, U.S. Environmental Protection Agency, Emissions
Measurement Branch, November 1976 (unpublished paper).

18.0 Diagrams
[GRAPHIC] [TIFF OMITTED] TR04MR19.009

[FR Doc. 2019-01902 Filed 3-1-19; 8:45 am]
BILLING CODE 6560-50-P