# SCOTT

- MARRIN, INC.

6531 BOX SPRINGS BLVD. • RIVERSIDE, CA 92507

- 0725 PHONE (951)653

- 6780 • FAX (951)653

- 2430 • jack@scottmarrin.com
January 30 , 2005

Robert W right, Air Pollution Prevention and Con trol Division US Environmental Protection Agenc y Research Triangle Park, NC 27711 wright.bob@epa.gov

References: 1) “Request for Suggestions for Revisions to EPA Traceability Protocol for Gaseous Calibration Standards”, Robert S. W right, em ail dated Dec em ber 23, 2004. 2) “EPA Traceability Protocol for Assay and Certification of Gaseous Calibration Standards”, Report Number EPA

- 600/R

- 97/121 dated September 1997 3) http://www.epa.gov/airmarkets/monitoring/calgasauditfailurerateby referencestandard.xls

Dear Bob, Thank you for the opportunity to respond to your Request for Suggestions for Revisions to the EPA Traceability Protocol (Ref 1) . Our company, Scott

- Marrin, Inc. has been producing gas mixtures since 1974. Our mixtures have been audited by EPA beginning in the late 1970s and we have been producing EPA Protocol mixtures since the middle 1980s when the first EPA protocol documents were published. Weare a small company competing against very large companies and the majority of our business is producing EPA protocol mixtures. My first comment addresses your proposal to revive the audit program by contracting with NIST to perform the audits with t he costs of this audit program being borne by the EPA Protocol Gas producers themselves. This is a departure from all previous audits where the audits were performed by third party contractors presumably selected on a competitive bid basis and the costs were provided through the budget of the USEPA. I have two problems with your proposed approach. First, although NIST is qualified to provide accurate analyses of gas mixtures, their prices to provide analytical services and program management are sure to be much higher than qualified private sector com panies presumably contracted on a competitive bid basis. Although I have no first hand knowledge of what EPA was paying for the previous EPA Protocol G as audits, I am very familiar with the prices of NIST SR Ms and the price to have NIST periodically recertify these SRMs when they expire. W e consider NIST pricing to be very expensive, but necessary to achieve accurate SRM gas standards traceable to NIST. I believe that it would be much more suitable for NIST to be the auditor of a competitively selected private sector Protocol Gas auditor. In any case, a reliable, independent audit of the work of any EPA Protocol Gas auditor, including NIST, should be a requirement. Second, s ince our company is a producer o f EPA Protocol G as mixtures, it is proposed that we directly pay for the audit services. I am concerned about the equity and affordability of this new approach. This is especially true since our company is one of the smallest companies currently manufact uring and sellingour own EPA P rotocol G as mixtures. Our manufacturing competitors have an annual gross income which

is 20 to 1000 times our annual gross income

. I am very concerned about a small company such as ours being required to pay a currently unk nown large am ount of money relative to our net income to participate in the audit program compared to the small am ount relative to the net income of the large specialty gas com panies. The relative sizes of our competitors would unfairly penalize small com panies such as ours if this audit proposal is adopted. Since Congress has presumably seen fit to inadequately fund EPA for this activity, I am suggesting that alternate funding sources, such as the much larger user community who are currently regulated by EPA and who benefit from using EPA Protocol Gases, be sought to pay for the audit function. The audit program costs spread over a much larger population will not burden any small group.

In general, I consider the EPA Protocol

- 97 document (Ref 2) to be an excellent guide to producing quality gas mixtures which doesn’t need a lot of modifications. I also believe that the use of performance specifications in the present EPA Protocol document is the best approach, while leaving the exact details of how to specifically meet the performance specifications up to the individual gas manufacturers. Regarding the list of informal suggestions which you have supplied, I have the following comments:

- include a procedure specifically for the use of Fourier Transfor m Infrared Spectroscopy; Comment: Does this suggestion imply that EPA is going to include a recommended list of analyzers or methods to be used to analyze EPA Protocol Gases? Or i s this instrument being singled out for inclusion in the Protocol document because of its inherent operational complexity? If this is the case, then standardized operating procedures should be included in the Protocol document.

- improve statistical procedures for uncertainty calculations and revise the Excel spreadsheet; Co mment: The EPA Protocol

- 97 statistical procedures for uncertainty calculations are very sophisticated and although I am not a statistician nor do I have a statistician on my staff, the calculations have always appeared to be inappropriate when considering the very limited number data points, namely 3, which they are being applied to. In their defense, the EPA Protocol

- 97 calculations give a desirable result and they are useful in finding problems, however, whether they truly represent the accuracy of the analyses is questionable. Perhaps this is why you are considering a change in the calculations?

- include mercury calibration standards in the protocol; Comment: Wedon’t have any experience with these standards; however, if there is a need, they mi gh t as well be included.

- eliminate (or retain) gas manufacturers intermediate standards (GMISs); Comment: The elimination of the use of the GMIS is the MOST TROUBLING SUGGESTION on yo ur list. As shown on your summary spreadsheet of the most recent EPA Protocol Gas audit (Ref 3.), the use of a GMIS does not result in failures of mixtures to meet the EPA accuracy specifications. In fact, one might conclude from your spreadsheet that the use of SRMs and NTRMs leads to higher failure rates. I’m not sugges ting this is an accurate interpretation; however, it certainly is an accurate interpretation that the GMIS is NOT an impediment to achieving accurate analys e s. In addition, m y review of past EPA gas audits dating back to the early 1980s shows that our com pany , Scott

- Marrin, Inc. is one of the only if not the only manufacturer that has provided gases which have all had an accuracy of better than the EPA 2% specification. Since we have always used the GMIS or its predecessors as intercomparison standards wh en performing our EPA Protocol analyses, our accuracy achievement is due to our focus on using accurately analyzed GMIS reference standards and carefully following the published EPA procedures. In addition, eliminating the use of the GMIS would require th e use of either an SRM or an NTRM. Since the SRMs contain too small a volume of gas to use as daily intercomparison standards, the NTRMs will be the sole reference standards to use for EPA Protocol Gas production. Our company is too small to produce NTRM s; therefore, we would be forced to purchase very expensive NTRMs from ourcom petitors. This assumes, of course, that ALL NTRMs are available for purchase any time they are

required. This availability is nowhere near guaranteed and based on past experien ce is probably not going to happen. A review of the internet sites and catalogs of all known producers of NTRMs shows no listing of available NTRM products, let alone prices for these products. A recent telephone conversation with a large producer of NTR Ms confirmed the lack of a guaranteed availability for commercial customers of these products. In addition, the availability of every NTRM as a companion to an existing SRM is also not assured. Since the use of the GMIS does not pose a technical problem as evidenced by your recent audit data, I am very suspicious that the elimination of the GMIS is a suggestion by one or more of the NTRM producers to achieve a competitive advantage over other manufacturers. One final point; even though NTRMs are declared to be equivalent to SRMs, they are to m y k nowledge, secondary to SRMs. The GMIS, if it is compared directly to an SRM, is also secondary to an SRM. As a point of information, our company perform s additional work on the GMISs which we produce. For examp le, we initially analyze each GMIS 4 or more times over a 3 month period and we analyze each GMIS every year rather the required 2 years. Wefeel these additional analyses increase the accuracy and reliability of the GMIS and, by the way, the annual analyses exceed the analysis requirements of NTRMs. Please do not elim inate the GMIS.

- lengthen the certification periods for EPA Protocol Gases; Comment: These comments are the result of our experience performing EPA Protocol Gas recertifications over ma ny years. They also err on the conservative side. I apologize for not having supporting documentation to submit. a) The recertification interval for CH4, O2, CO2, and C3H8 can certainly be greater than 3 years. Although these gas mixtures are usually us ed up in 3 years, these mixtures will certainly be stable for 4 to 6 years and probably much longer. b) A 36 month interval for CO from 8 to 50 ppm seems to be a prudent. W e have never seen CO change at higher concentrations in aluminum cy linders, so 4

- 6 ye ars is acceptable above some threshold around 20 to 50 ppm. c) The  4 ppm Nitric Oxide concentration range for 24 months specified in the EPA Protocol

- 97 document is too low a threshold. The lower threshold for Nitric Oxide mixtures should be more like 20 ppm to warrant a 24 month recertification interval. For concentrations in the range of 4 to 20 ppm, a range of 12 mo nths would be more appropriate. For less than 4 ppm Nitric Oxide, a 6 month initial interval followed by a 12 month interval if successfully demonstrating concentration stability seems appropriate. d) The current intervals of 40 to 499 ppm SO2@ 24 months and  500 ppm SO2 @ 36 months should remain unchanged. e) The current interval of 4+ ppm H2S@ 12 months should remain unchanged. If higher concentration H2S SRMs are made available then a 24 month interval should be considered for concentrations exceeding 50 to 100 ppm.

- change the cylinder pressure limitations for EPA Protocol Gases; Comment: The current recertification pressure limit of 500 psig is about right. Below this concentration, the recertification is not cost effective any way . The minimum use pressure limit of 150 psig could be lowered to 100 psig without problem. Most gas mixtures in aluminum cy linders are going to be stable to less than 25 psig, however, some ‘reactive’ gas mixtures may not be.

- include a procedure for analyzing and certi fying zero gases; Comment: This would be very desirable. Several different standardized grades should be specified to include the range of EPA Protocol Gas applications

.

- include gas dilution systems in the protocol; Comment: This too would be very desirable. Performance specifications and calibration standards and methods are required.

- tighten documentation requirements;Comment: I have no idea what this is referring to. The documentation requirements s pecified in

the EPA Protocol

- 97 Gas do cument seem appropriate and complete.

- develop audit participant identification number for regulatory data reporting purposes; Comment: OK, if this really has a useful purpose.

- require ISO 17025 accreditation for producers of environmental calibra tion gases; Comment: Weare not currently ISO certified nor do we have any expertise with ISO certification. However, in looking into the ISO 17025 accreditation standard, it would seem to duplicate some of the existing EPA Protocol

- 97 Gas document requ irements. I believe the EPA Protocol Gas document is a sufficient controlling standard that can be used to achieve the goal of producing accurate EPA Protocol Gas standards. Therefore, I don’t think it is necessary or desirable to be ISO 17025 accredited to achieve the EPA Protocol Gas program goals. I also don’t think it should be required, since it would be costly and favor large companies.

- include provision for preparation and analysis of batches of EPA Protocol Gases; Comment: To my

knowledge there is no provision against preparing EPA Protocol Gases in batches. Therefore, i n the absence of specifics, this suggestion im plies that a procedure for the batch analysis of EPA Protocol Gases be considered. This would seem to defeat the main tenet o f EPA Protocol Gases, namely that of maintaining quality by individually certifying each and every mixture to elim inate errors.

- require on -site visits of specialty gas producers by EPA representatives; Comment: OK. My only objection would be the cos t to perform this level of audit. Perhaps this should be considered for those specialty gas producers who fail an audit.

- provide for technical assistance/outreach to specialty gas producers by NIST representatives; Comment: Isn’t his already availab le?
I only have one additional recommendation. NIST should be encouraged to produce the following additional SRMs to support the EPA Protocol Gas program. 50 and 100 ppm Hydrogen Sulfide in Nitrogen, 250 ppm Sulfur Dioxide in Nitrogen, 5 ppm Carbon Mon oxide in Air, and 50, 100 and 1000 ppm Methane in Air or Nitrogen are not currently available and their availability would improve the EPA Protocol Gas program. The fact that I am not submitting many additional suggestions is only an indication that I thi nk the EPA Protocol

- 97 Gas document in its presen t form is very good and could only be a little better with some additions and a little tweaking. In summary, the unspecified costs of your audit proposals and the elim ination of the GMIS are very bad ideas which I feel would seriously impact our ability t o produce EPA Protocol Gases and thereby threaten the existence of our company. Please feel free to discuss any of the above comments with me. I can be contacted by phone at 951

- 653

- 6780 or by email at jack@ scottmarrin.com. Best regards,

Jack Marrin President