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To access EPRI's "Lessons
Learned" Website, click on the EPRI logo below to login.
Once you
have logged in, select the "EPRI Collaboration" tab at the top right of
the
screen. Then select "Continuous Mercury Monitoring
Forum" in the Community Projects box on the left hand side of the
screen. This site is available
for EPRI members only.
Last Updated on 10/19/07 – See Below 10/19/07 Update
on Hg Elemental Calibrator
NIST Certification Our
last update on the status of
NIST Traceability of elemental Hg calibrators and EPA Traceability
Protocols
was on 8/21/07 or approximately two months ago. Input was
requested from
the involved parties was requested several days ago and is quoted
below.
In the cases where no response was received, that has been indicated
and I have
substituted the best information I have based on other sources. EPA "EPA
intends to temporarily
waive the NIST-traceability requirement for elemental and oxidized Hg
calibration gas standards until January 1, 2010. The
planned waiver
will only apply to the NIST-traceability requirement for the Hg
calibration gas
standards. It does not defer the CAMR requirement for Hg
monitoring
systems to be installed and certified by January 1, 2009. Please
note
that this planned waiver is subject to change and will not become
official until
our proposed Part 75 rule modification package is final. We
expect the
rule package will be signed and published within the next few months. EPA
plans to phase in the NIST
traceability requirement for Hg calibration gas standards during the
waiver
period. In the first phase (2008), EPA will invite stakeholders,
including, among others, Hg monitoring equipment vendors, cylinder gas
suppliers, key NIST personnel, and representatives from industry to
participate
in a demonstration program, the purpose of which will be to collect the
data
that EPA needs to finalize the NIST traceability protocols. Two
key
elements of the demonstration program will be: (1) assessment of the
field
performance of elemental and oxidized Hg generators; and (2) evaluation
of the
long-term stability of elemental Hg compressed gas cylinders.
Based on
the results of the demonstration program, EPA intends to finalize the
elemental
and oxidized Hg traceability protocols and issue them by December 31,
2008. During
the second phase (2009),
the affected sources will be required to implement the final protocols,
to
ensure that their generators and cylinders are certified as
NIST-traceable
before the waiver period expires. Beginning on January 1, 2010,
full NIST
traceability is required for all Hg calibration gas standards used in
the CAMR
program. Only those Hg gas generators and cylinders that meet the
requirements of the final traceability protocols will be considered
NIST-traceable. EPA is
currently revising the August
interim traceability protocol for elemental mercury gas generators,
taking into
account comments received from industry. We plan to incorporate major
components of the revised interim protocol into a draft work plan for
implementing the field demonstration program. EPA then plans to
hold a
meeting/conference call with key stakeholders in November to review the
draft
work plan and begin developing the field demonstration program." NIST No written
update was received
from NIST. I understand that two bottled gas vendors have
sent
cylinders
to NIST for evaluation (see below updates). NIST is presently
working
with those bottles and initially observed concentration drift during
gas
extraction. One bottle was rolled to thoroughly mix it and the
drift problem
disappeared. Tests have not been done on the remaining
bottles. Thermo “Thermo
has received two
certified vendor prime calibrators from NIST. These vendor primes
cannot
be used because no certification reports have been received from
NIST.
Thermo received and responded to an inquiry Email from EPA regarding
calibrator
test procedures. Thermo suggested a relaxed transfer protocol as
an
interim procedure so that user calibrators were related to the vendor
primes.” Tekran “Tekran
has received two certified
vendor prime calibrators from NIST. These vendor primes cannot be
used
because no certification reports have been received from NIST.
Tekran met
with NIST and EPA. Tekran also supports a relaxed transfer
protocol as an
interim procedure.” Hovacal “The
HovaCAL is now available in
a fully automated version. The HovaCAL Quick AC can be integrated
into an
Hg CEMS for daily, weekly or monthly calibration.” Spectra
Gases “The
Spectra Hg NTRM prime
cylinders are at NIST and we are waiting for their results.” Air
Gas “Airgas
has six elemental mercury
cylinders at NIST in a wide range of concentrations. They have
been
analyzed for two months now and we have been advised by NIST that they
are very
stable.” RMB As
noted in the last update (see
below), EPA transmitted draft elemental Hg calibrator Traceability
Protocols to
“selected” individuals on 08/14/07. RMB prepared comments on the
Protocols and sent them to EPA. Basically, the Protocols could
not be
implemented in a practical manner. Therefore, as noted in EPA’s
update
above, the requirement for NIST-traceability has been postponed until
January
1, 2010 and the Protocols will be revised to reflect field performance
of the
calibrators during calendar year 2008. RMB is presently working
on a draft
test plan outline for the field demonstration program discussed in
EPA’s
comments above. The outline will include tasks, responsible
parties,
deliverables and schedule for each task. In order to accomplish
the
objectives of the demonstration program, I need a number of utility
companies
to participate in the data gathering portion of the project. We
need a
cross section of both Thermo and Tekran users. If you are
interested,
please give me a call (919-510-0483) and we can discuss the
details.
There will be some manpower commitment necessary but it will serve as
excellent
training. 08/21/07 Update on Hg Elemental Calibrator NIST Certification It has been three weeks since our last update on the status of NIST Traceability of elemental Hg calibrators and EPA Traceability Protocols. I apologize for the long delay between updates but other project activity and considerable travel has interfered. I have also received a complaint from one of the interested parties concerning the posting of opinion in our last update. If you are not interested in my opinion, you are welcome to stop reading now. Input received from various interested parties for this update is quoted below. EPA “On August 14, EPA completed an
Interim Traceability Protocol
for Elemental Mercury Gas Generators and submitted it to generator
manufacturers and protocol collaborators for feedback prior to its full
implementation. The purpose of this interim traceability protocol is to
provide procedures for manufacturers or their designees (a) to qualify
representative samples of elemental mercury gas generators, (b) to
certify individual elemental mercury gas generators, and (c) to conduct
quality control checks in the field. The interim protocol incorporates
comments received on the previous May “working draft” traceability
protocol. At a later date, user-friendly uncertainty calculation The interim protocol uses qualification and certification tests to establish traceability of field generators (user-primes) to NIST-certified generators (vendor-primes). The qualification tests have been designed to examine representative sample generators for potentially significant operating variables (e.g., back pressure, temperature and flow control, operating environment temperature and voltage, drift, etc) and their effect on candidate generator output performance. In turn, certification tests have been designed to establish a quantitative relationship between each candidate user-prime generator and the reference vendor-prime generator. The interim traceability protocol also requires that field quality control (QC) checks be performed by the user or its designee on each certified elemental mercury (Hg) generator (i.e., user-prime) to insure that the traceability obtained during certification testing is maintained (i.e., to insure that the generator's output remains stable). The objective of the field QC checks is to show, to the greatest extent possible, that the user-prime did not change significantly between certification and use. The initially certified user-prime generators must be recertified on an annual basis or if they fail to attain the acceptance criterion for the field QC check. The recertification may be performed at the facility of the manufacturer that previously certified the user-prime or in the field by the manufacturer or another service provider using a vendor-prime (of the same model as the user-prime) and the same certification procedure. A memorandum accompanies the interim traceability protocol which summarizes the important points in the protocol and also includes a waiver or deferral period until January 1, 2009 in which certain procedures and acceptance criteria specified in the protocol will be relaxed. This waiver or deferral period allows sufficient time for generator performance data to be collected and analyzed to verify that the acceptance criteria outlined in the protocol are achievable and/or for manufacturers to modify the generators to attain the criteria. EPA plans to review these data as they become available during Calendar Year 2008 and make necessary adjustments/modifications as necessary to this interim traceability protocol prior to January 1, 2009. We believe this waiver or deferral period is reasonable because mercury monitoring data reported to EPA in 2009 will not be used in the trading of allowances, as allowance accounting under the Clean Air Mercury Rule (CAMR) does not begin until 2010. The acceptance criteria provided in the interim traceability protocol and accompanying memorandum do not take into account that fact that humidification of the Hg generation stream may be required in many applications in order for Hg CEMS to pass required daily calibration and weekly system integrity tests. Humidification will alter the certified concentration output of the user prime generator as well as increase its overall combined uncertainty. We will evaluate the effect of humidification during the waiver period (until January 1, 2009), and if appropriate, may add uncertainty acceptance criteria for generator gas stream humidification to the traceability protocol.” NIST “The elemental mercury work at NIST is continuing. The work on four elemental mercury generators, two for each of two manufacturers, has been completed. Specific set points on these generators have been certified. Reports are in process and the generators are being shipped to the manufacturers as Vendor Primes. We are starting work on three mercury mixtures in compressed gas cylinders. We continue to work with Western Research Institute to better understand the performance of the generators.” Thermo “Thermo is awaiting return of the certified vendor prime calibrators and certification reports from NIST.” Tekran “Tekran is awaiting return of the certified vendor prime calibrators and certification reports from NIST.” Hovacal “The HovaCAL digital MF (same as HovaCAL Quick with internal flow metering) was certified by TUV Rheinland, Germany for the components Mercury Chloride, Elemental Mercury, Water, Hydrogen Chloride, Hydrogen Fluoride and Ammonia. The requirements are derived from the European Guideline DIN EN 14 181. The TUV report is available in German or English language at info@hovacal.de” Spectra Gases “Spectra will be shipping Hg NTRM Prime cylinders to NIST by the end of the month.” RMB As you may recall from our last update (see below), NIST was having precision and accuracy problems with the first series of calibrator comparison tests. One of the Hg CEMS vendors dispatched an engineer to NIST to evaluate the situation. It was discovered that NIST had not plumbed the calibrators properly and had created a back pressure situation that was influencing the results. Obviously, the traceability tests had to be redone. As noted in the EPA update above, EPA transmitted draft Traceability Protocols to “selected” individuals on 08/14/07. However, EPA requested that the Protocols not be circulated. I have asked EPA to release those Protocols for broad distribution within the utility and stack testing industry so that the protocol requirements can be used for planning purposes. We will put the protocols on this web site if and when EPA releases them. 08/01/07 Update on Hg Elemental Calibrator NIST Certification I would like to update you on the latest news on the elemental Hg Vendor Prime calibrator certifications at NIST. This update is based on information received from NIST, EPA and the calibrator vendors over the past week. There has been some difficulty at NIST performing the Vendor Prime certifications. According to NIST the vendor calibrators have exhibited poor accuracy and precision. As of last Thursday, NIST had looked at four calibrators and the reproducibility (precision) ranged from 0.3 to 3%. The accuracy was not very good and the slopes of the calibration curves varied. In our opinion, reproducibility as high as 3% is virtually impossible considering the repeatability of the mass flow meters in the calibrators is 0.015%. In addition, some of the discussion concerning reproducibility and accuracy does not match our field experience at all. We have found the calibrators to be very reproducible and several different vendor’s calibrators have been cross compared with very good results. So the bottom line is we believe that something is wrong with the experimental setup and/or operation of the calibrators. To top it off, it turns out that EPA had given NIST a 1% acceptance criteria for reproducibility. While this specification may be desirable in a perfect world, it is “over the top” relative to our ability to make Hg measurements in power plant stacks. Therefore, NIST indicated that they could only certify one of the four calibrators. However, considering all the difficulty and variable data were not comfortable with that certification. We certainly agree that the problem has to be solved before “certified” calibrators are sent out the door. The bottom line is that no calibrators will be sent back to the vendors until NIST has the opportunity to discuss the situation with the vendors and discuss options with EPA. EPA is still working on traceability protocols and claims that they will have “working protocols” done by the first week in August. We will see if that really happens because that is over a month later than originally promised and I would not be surprised to see further slippage. 07/11/07 RMB - In response to a progress update request from RMB to Hg calibrator vendors, EPA, NIST and WRI, the below information was received. I only expected an update from EPA, NIST and WRI since “the ball has been in their court” for the past month. WRI did not provide an update. Thermo and Airgas did provided updates so they are also included. I am trying hard to be polite so I will only say that I am extremely disappointed in the glacial rate of progress on this project. Just to remind everyone, today is the two month anniversary of our departure from Phoenix and as of today there are no vendor prime generators and there are no protocols. And every week that passes puts another 20 calibrators in the field. This game gets uglier with every flip of the calendar. EPA - Here is our update on generator certification procedures / traceability protocols for July 10:
NIST - The NIST Prime Generator is certified and will be used to begin the certification process on two Vendor Primes on Monday July 16, 2007. Airgas - NIST now has a set of Airgas mercury calibration gases for verification. Thermo - Thermo is waiting for an update from NIST on the 4 elemental calibrators in NIST possession. NIST has indicated that the calibrators would be certified in July. Thermo had delivered a PO for NIST certification of the above units on 6/18/07. After Thermo receives the 3 Vendor Prime units, additional units will be shipped to NIST. Thermo believes that up to 5 additional Vendor Prime units may be required depending upon how field certification is ultimately defined by the EPA. Thermo has provided NIST with multiple (6-8) Hg concentration points that are required to have units certified on ranges from 10 to 40 microgram/m3. Thermo has shipped +30 HgCl2 generators, primarily as part of an upgrade program currently in place. The generator shipments will accelerate as we move forward into the 2nd half of 2007, and as first field testing is completed. 06/18/07 In response to a progress update request from RMB to Hg calibrator vendors, EPA, NIST and WRI, the following information was received. EPA – The following information was received from EPA for this update.
NIST – In response to my suggestion that consultants, integrators and testing companies may desire to obtain Vendor Prime calibrators, I received the following communication from NIST. “Anyone wishing to have an
elemental mercury generator
certified at NIST as a Vendor Prime must contact NIST in advance to
negotiate terms and timing. Timing is important since NIST wants
to minimize turn around time and a backlog of generators at our
facility will increase this time. Currently the cost of
certification is $10,000 per one unit or $15,000 per two
units. RMB – RMB transmitted a draft Field Calibrator Validation Protocol and Periodic QA/QC Protocol to EPA on 6/04/07. On 06/06/07 RMB received a call from EPA explaining that a different (more complicated) approach was needed to satisfy the “expanded uncertainty” mathematics. RMB anticipates no further activity until EPA has some words on paper to review. Western Research Institute – No additional information was received from Western Research for this update. Airgas – Airgas is submitting to NIST 6 mercury calibration gas standards within the month. Airgas is being very optimistic to believe that we will get results back sometime this fall according to NIST. Ducon – As previously reported, Ducon has sent two elemental calibrators to NIST for certification as Vendor Primes. Ducon is developing an automated calibration system with an oxidized mercury calibrator using the Hovaquick. Hovacal – Hovacal sent a note stating that they had no new information for this update. It should be noted that the Hovaquick is the oxidized Hg calibrator being used by EPA and RMB in the Hg CEMS development studies. Opsis – No response was received or expected since Opsis does not supply head space calibrators. PSA - PSA is still concerned about the technical correctness of the ICMPS approach used by NIST and potential conflicts with other International Standards. PSA referenced me to an ASTM method (D6350) for measuring Hg in natural gas as an example of a potential conflict. I have not had the opportunity to review this ASTM Method. PSA is working on an oxidized Hg calibrator. Spectra – Spectra is in the process of producing the NTRM prime cylinders for shipment to NIST. NTRMs spend a relatively long time "in house" before they are shipped to NIST for their analyses and naming. Tekran – Tekran prepared three reference calibrators and shipped two of them to NIST for certification as Vendor Prime calibrators. The third calibrator will be retained by Tekran to evaluate the returned calibrators for shipping damage. The calibrators were shipped to NIST on 6/13/07. Included in the shipment was a very nice spreadsheet on the calibration points and a computer programmed to automate the process. Tekran has an oxidized Hg calibrator in production. No results have been publicly reported. Thermo – Below is a slightly edited version of the response received from Thermo. Thermo has provided 4 calibrators to NIST, the first was to be the NIST Prime, the 3 that arrived end of May were designated as Vendor Primes. NIST has acknowledged receipt of these units, but has only done a visual inspection to date. They indicated receipt in good condition with no sign of damage. NIST indicated that they would go through "acceptance" tests this week (whatever that means), but they will not be certified until July. NIST also has asked for the following which Thermo is in the midst of completing:
Item 3 requires discussion with EPA and we have a phone conference this afternoon to finalize. NIST is also asking $15K per two units for their services which appears very high. Nevertheless, Thermo has given them a PO # to proceed. As far as the oxidizer is concerned, multiple units are in customer hands. All that are installed and operating are achieving between 70% - 90% oxidation, with recovery efficiencies ranging from 80's to 98%+. We are finding that (1) each site has its own issues/difficulties and (2) some adjustment of flows, as well as 24 - 48 hours of conditioning, improves performance. Thermo has also been modifying software to allow easier automation of the oxidizer module. We are making significant progress as more units are out there, but until all operate as required by regulation, we still have work to do. Sick – No response was received or expected since Sick does not supply head space calibrators. As an observation, I will note that we have been involved in a number of conversations recently concerning Hg CEMS certifications and testing schedules. Unfortunately, the way the rule is presently constructed, no Hg CEMS can be certified until it is equipped with a NIST traceable elemental and oxidized calibrator. Perhaps EPA plans to fix the rule in the upcoming rulemaking. I certainly hope so. 05/31/07 In response to a progress update request from RMB to Hg calibrator vendors, EPA, NIST and WRI, the following information was received. EPA – "The Agency very much welcomes RMB's initiative to track progress on this issue since it may provide for a means to effectively expedite the development of procedures to certify vendor prime and user prime (candidate field) generators and in completing the necessary mercury traceability protocol documents. We agree that this issue needs to be managed with a sense of urgency and as such we welcome the opportunity to communicate with the wider monitoring community, including EPRI, utilities, vendors, CEMS users and others, our progress updates on these traceability issues." "The following is our progress update on generator certification procedures / traceability protocols subsequent to the May CEMS User's Group conference:
Again thank you for your efforts to expedite this important effort." NIST – "Mercury work at NIST, in support of
implementing CAMR, is continuing along two lines, elemental and
oxidized mercury." RMB – RMB has provided comments to EPA and NIST on the Draft Traceability Protocol for Qualification and Certification of Elemental Mercury Gas Generators. A draft Field Calibrator Validation Protocol and Periodic QA/QC Protocol are in preparation and will be transmitted in the next few days. Yes – I am behind schedule on that transmittal. Western Research Institute - WRI has sent an elemental Hg calibrator to NIST for certification as a vendor prime. WRI is also setting up to conduct pressure and temperature stability tests. Receipt of an environmental chamber needed for these experiments is scheduled for the week of 06/04/07. Ducon – Two calibrators have been sent to Western Research. Comments on the draft Traceability Protocol are in preparation. Hovacal – An oxidized mercury calibrator (HovaCAL Digital 111-MF) was shipped to NIST on 03/06/06. Start up and training was conducted on 03/15/06. Hovacal has received no feedback on the status of the NIST evaluation. Opsis – No response was received or expected since Opsis does not supply head space calibrators. PSA - PSA is still negotiating terms with NIST, discussing how many calibrators would need to be certified and what costs are involved. Pending resolution, PSA has not yet sent an elemental Hg generator to NIST for the purpose of obtaining a certified Vendor Prime calibrator. PSA is still reviewing the EPA/NIST Draft Traceability Protocol for Qualification and Certification of Elemental Mercury Gas Generators. Comments should be finalized by 06/04/07. PSA uses an in house certification procedure which utilizes NIST certified components. PSA will continue to use this approach until it is satisfied with the technicalities of the EPA Traceability Protocol and NIST certification procedure. Tekran – Tekran has sent EPA and NIST comments on the draft Traceability Protocol. Tekran is preparing three reference calibrators and will ship two of them to NIST for certification as Vendor Prime calibrators. The third calibrator will be retained by Tekran to evaluate the returned calibrators for shipping damage. The scheduled shipping date is the first week of June. Thermo – Thermo has sent EPA and NIST comments on the draft Traceability Protocol. Thermo had previously sent a calibrator to be certified as a NIST Prime. This calibrator was received by NIST on 05/01/07. Three more calibrators were sent to NIST on 05/29/07 to be certified as Vendor Prime calibrators. Sick – No response was received or expected since Sick does not supply head space calibrators. As an observation, I will call your attention to the one month slippage (to July 1) in the NIST schedule to prepare the NIST Prime calibrators. As a practical matter, and in the absence of further delay, this means that Vendor Prime calibrators will not likely be in the hands of the vendors before August 1. My closing comment is that general weekly updates will likely be overkill (and a hell of a lot of work for everyone) so expect future updates about every two weeks. In the event that specific important activities occur, they will be posted as needed between updates. 05-14-07 This web page has been developed as a follow up to Richard McRanie’s presentation on May 10, 2007 at the EPRI CEM Users Group meeting. It is for the purpose of tracking EPA and NIST progress on delivering Vendor Prime elemental Hg calibrators and appropriate protocols. We will also track Hg monitor vendor progress in shipping calibrators to NIST and implementing the NIST protocols into the manufacturing process. It is RMB’s plan to update this web page on a periodic basis. Trimble County project supporters will receive a direct update by E-mail several days prior to the web page update As a reminder, NIST has committed to a 30-day turnaround of Vendor Prime calibrators from the date a calibrator is received from the vendor. EPA has also committed to a protocol development schedule that will not delay Vendor Prime transfer to User Prime implementation. The following schedule is suggested as an accountability marker:
The action items above are critical path. There are additional items that need to be accomplished with respect to Hg calibrator traceability. Below is a complete list for elemental calibrators and you will note that the first three items are scheduled above while the last three items have not been scheduled. It is our plan to add the last three to the schedule list after further discussions with EPA and NIST. We should also note that no action items have been scheduled for the oxidized Hg calibrators. Action items for elemental Hg calibrators:
05/31/07 In response to a progress update request from RMB to Hg calibrator vendors, EPA, NIST and WRI, the following information was received. EPA – "The Agency very much welcomes RMB's initiative to track progress on this issue since it may provide for a means to effectively expedite the development of procedures to certify vendor prime and user prime (candidate field) generators and in completing the necessary mercury traceability protocol documents. We agree that this issue needs to be managed with a sense of urgency and as such we welcome the opportunity to communicate with the wider monitoring community, including EPRI, utilities, vendors, CEMS users and others, our progress updates on these traceability issues." "The following is our progress update on generator certification procedures / traceability protocols subsequent to the May CEMS User's Group conference:
Again thank you for your efforts to expedite this important effort." NIST – "Mercury work at NIST, in support of
implementing CAMR, is continuing along two lines, elemental and
oxidized mercury." RMB – RMB has provided comments to EPA and NIST on the Draft Traceability Protocol for Qualification and Certification of Elemental Mercury Gas Generators. A draft Field Calibrator Validation Protocol and Periodic QA/QC Protocol are in preparation and will be transmitted in the next few days. Yes – I am behind schedule on that transmittal. Western Research Institute - WRI has sent an elemental Hg calibrator to NIST for certification as a vendor prime. WRI is also setting up to conduct pressure and temperature stability tests. Receipt of an environmental chamber needed for these experiments is scheduled for the week of 06/04/07. Ducon – Two calibrators have been sent to Western Research. Comments on the draft Traceability Protocol are in preparation. Hovacal – An oxidized mercury calibrator (HovaCAL Digital 111-MF) was shipped to NIST on 03/06/06. Start up and training was conducted on 03/15/06. Hovacal has received no feedback on the status of the NIST evaluation. Opsis – No response was received or expected since Opsis does not supply head space calibrators. PSA - PSA is still negotiating terms with NIST, discussing how many calibrators would need to be certified and what costs are involved. Pending resolution, PSA has not yet sent an elemental Hg generator to NIST for the purpose of obtaining a certified Vendor Prime calibrator. PSA is still reviewing the EPA/NIST Draft Traceability Protocol for Qualification and Certification of Elemental Mercury Gas Generators. Comments should be finalized by 06/04/07. PSA uses an in house certification procedure which utilizes NIST certified components. PSA will continue to use this approach until it is satisfied with the technicalities of the EPA Traceability Protocol and NIST certification procedure. Tekran – Tekran has sent EPA and NIST comments on the draft Traceability Protocol. Tekran is preparing three reference calibrators and will ship two of them to NIST for certification as Vendor Prime calibrators. The third calibrator will be retained by Tekran to evaluate the returned calibrators for shipping damage. The scheduled shipping date is the first week of June. Thermo – Thermo has sent EPA and NIST comments on the draft Traceability Protocol. Thermo had previously sent a calibrator to be certified as a NIST Prime. This calibrator was received by NIST on 05/01/07. Three more calibrators were sent to NIST on 05/29/07 to be certified as Vendor Prime calibrators. Sick – No response was received or expected since Sick does not supply head space calibrators. As an observation, I will call your attention to the one month slippage (to July 1) in the NIST schedule to prepare the NIST Prime calibrators. As a practical matter, and in the absence of further delay, this means that Vendor Prime calibrators will not likely be in the hands of the vendors before August 1. My closing comment is that general weekly updates will likely be overkill (and a hell of a lot of work for everyone) so expect future updates about every two weeks. In the event that specific important activities occur, they will be posted as needed between updates. 06/18/07 In response to a progress update request from RMB to Hg calibrator vendors, EPA, NIST and WRI, the following information was received. EPA – The following information was received from EPA for this update.
NIST – In response to my suggestion that consultants, integrators and testing companies may desire to obtain Vendor Prime calibrators, I received the following communication from NIST. “Anyone wishing to have an
elemental mercury generator
certified at NIST as a Vendor Prime must contact NIST in advance to
negotiate terms and timing. Timing is important since NIST wants
to minimize turn around time and a backlog of generators at our
facility will increase this time. Currently the cost of
certification is $10,000 per one unit or $15,000 per two
units. RMB – RMB transmitted a draft Field Calibrator Validation Protocol and Periodic QA/QC Protocol to EPA on 6/04/07. On 06/06/07 RMB received a call from EPA explaining that a different (more complicated) approach was needed to satisfy the “expanded uncertainty” mathematics. RMB anticipates no further activity until EPA has some words on paper to review. Western Research Institute – No additional information was received from Western Research for this update. Airgas – Airgas is submitting to NIST 6 mercury calibration gas standards within the month. Airgas is being very optimistic to believe that we will get results back sometime this fall according to NIST. Ducon – As previously reported, Ducon has sent two elemental calibrators to NIST for certification as Vendor Primes. Ducon is developing an automated calibration system with an oxidized mercury calibrator using the Hovaquick. Hovacal – Hovacal sent a note stating that they had no new information for this update. It should be noted that the Hovaquick is the oxidized Hg calibrator being used by EPA and RMB in the Hg CEMS development studies. Opsis – No response was received or expected since Opsis does not supply head space calibrators. PSA - PSA is still concerned about the technical correctness of the ICMPS approach used by NIST and potential conflicts with other International Standards. PSA referenced me to an ASTM method (D6350) for measuring Hg in natural gas as an example of a potential conflict. I have not had the opportunity to review this ASTM Method. PSA is working on an oxidized Hg calibrator. Spectra – Spectra is in the process of producing the NTRM prime cylinders for shipment to NIST. NTRMs spend a relatively long time "in house" before they are shipped to NIST for their analyses and naming. Tekran – Tekran prepared three reference calibrators and shipped two of them to NIST for certification as Vendor Prime calibrators. The third calibrator will be retained by Tekran to evaluate the returned calibrators for shipping damage. The calibrators were shipped to NIST on 6/13/07. Included in the shipment was a very nice spreadsheet on the calibration points and a computer programmed to automate the process. Tekran has an oxidized Hg calibrator in production. No results have been publicly reported. Thermo – Below is a slightly edited version of the response received from Thermo. Thermo has provided 4 calibrators to NIST, the first was to be the NIST Prime, the 3 that arrived end of May were designated as Vendor Primes. NIST has acknowledged receipt of these units, but has only done a visual inspection to date. They indicated receipt in good condition with no sign of damage. NIST indicated that they would go through "acceptance" tests this week (whatever that means), but they will not be certified until July. NIST also has asked for the following which Thermo is in the midst of completing:
Item 3 requires discussion with EPA and we have a phone conference this afternoon to finalize. NIST is also asking $15K per two units for their services which appears very high. Nevertheless, Thermo has given them a PO # to proceed. As far as the oxidizer is concerned, multiple units are in customer hands. All that are installed and operating are achieving between 70% - 90% oxidation, with recovery efficiencies ranging from 80's to 98%+. We are finding that (1) each site has its own issues/difficulties and (2) some adjustment of flows, as well as 24 - 48 hours of conditioning, improves performance. Thermo has also been modifying software to allow easier automation of the oxidizer module. We are making significant progress as more units are out there, but until all operate as required by regulation, we still have work to do. Sick – No response was received or expected since Sick does not supply head space calibrators. As an observation, I will note that we have been involved in a number of conversations recently concerning Hg CEMS certifications and testing schedules. Unfortunately, the way the rule is presently constructed, no Hg CEMS can be certified until it is equipped with a NIST traceable elemental and oxidized calibrator. Perhaps EPA plans to fix the rule in the upcoming rulemaking. I certainly hope so. 07/11/07 RMB - In response to a progress update request from RMB to Hg calibrator vendors, EPA, NIST and WRI, the below information was received. I only expected an update from EPA, NIST and WRI since “the ball has been in their court” for the past month. WRI did not provide an update. Thermo and Airgas did provided updates so they are also included. I am trying hard to be polite so I will only say that I am extremely disappointed in the glacial rate of progress on this project. Just to remind everyone, today is the two month anniversary of our departure from Phoenix and as of today there are no vendor prime generators and there are no protocols. And every week that passes puts another 20 calibrators in the field. This game gets uglier with every flip of the calendar. EPA - Here is our update on generator certification procedures / traceability protocols for July 10:
NIST - The NIST Prime Generator is certified and will be used to begin the certification process on two Vendor Primes on Monday July 16, 2007. Airgas - NIST now has a set of Airgas mercury calibration gases for verification. Thermo - Thermo is waiting for an update from NIST on the 4 elemental calibrators in NIST possession. NIST has indicated that the calibrators would be certified in July. Thermo had delivered a PO for NIST certification of the above units on 6/18/07. After Thermo receives the 3 Vendor Prime units, additional units will be shipped to NIST. Thermo believes that up to 5 additional Vendor Prime units may be required depending upon how field certification is ultimately defined by the EPA. Thermo has provided NIST with multiple (6-8) Hg concentration points that are required to have units certified on ranges from 10 to 40 microgram/m3. Thermo has shipped +30 HgCl2 generators, primarily as part of an upgrade program currently in place. The generator shipments will accelerate as we move forward into the 2nd half of 2007, and as first field testing is completed. Please contact Richard McRanie at mcranie@rmb-consulting.com if there are questions, comments or suggestions. | News | CAM | Training | FTP Library | Projects | Links | Services | Contact | Feedback | RMB Consulting &
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