p. 1 of 5

From: Putney, David
Sent: Monday, August 19, 2013 10:56 AM
To: 'Backfisch Don (NORALNM)' Subject: RE: Noranda

Don,

Thanks so much for this information. I’ll let you k now if I have any more (last, hopefully) questions on the report once I get a chance to discuss these respons es with our testing folks.

Thanks again,

David Putney, Environmental Engineer U.S. Environmental Protection Agency Office of Air Quality Planning and Standards Sector Policies and Programs Division 109 T.W. Alexander Drive, RTP, NC 27711 Mail Drop D243-02 Ph: (919) 541-2016 Fax: (919) 541-3207
Email: putney.david@epa.gov

From: Backfisch Don (NORALNM) [ mailto:Don.Backfisch@noralinc.com ]
Sent: Monday, August 19, 2013 8:49 AM
To: Putney, David Subject: FW: Noranda

Below is the explanation we got from the lab (in re d) concerning your questions. I apologize for not getting these to you sooner. Let me know if you ha ve other questions and I’ll try to get them answered as quickly as I can.

Don Backfisch

From: Scott Brown [ mailto:sbrown@cleanair.com ]
Sent: Tuesday, August 06, 2013 8:54 AM
To: Backfisch Don (NORALNM) Subject: FW: Noranda

Don, See the lab responses below.

Scott B.

From: Ron McLeod [mailto: Ron.McLeod@alsglobal.com ]
Sent: Tuesday, August 06, 2013 8:50 AM
To: Scott Brown Subject: RE: Noranda

Below in red type are my respective responses to th e Noranda enquiries below.

Regardsp. 2 of 5

Ron



### Ron McLeod Ph.D.

Director, Air Toxics and Special Chemistries, Easte rn Canada ALS Life Sciences Division | Environmental

5420 Mainway Drive #5 Burlington, ON Canada, L7L 6A4 T +1 905-331-3111 ext. 222 M +1 905-516-2687 F +1 905-331-4567

www.alsglobal.com

From: Scott Brown [ mailto:sbrown@cleanair.com ]
Sent: Wednesday, July 31, 2013 2:22 PM
To: Ron McLeod Subject: Noranda

Ron, This was sent to Don and Nancy at Noranda. Pl ease respond with whatever enlightenment you can.

Nancy,

I have done a quick review of the ICR data submitte d for the Noranda primary aluminum facility in New Madrid, MO, and have a few comments and questions f or you and the testing/lab contractors. Note that i n the discussions below, unless otherwise specified, plea se refer to page G-124 of the lab data (see page 62 6 of 748 in the pdf Final Report) when discussing dioxin/fur an (D/F) data and refer to page G-165 of the lab da ta (see page 667 of 748 in the pdf Final Report) when discu ssing polychlorinated biphenyl (PCB) data as “typic al” examples. These data are for run 1 on the paste pla nt.

• Some of the target analytes are flagged with an “R” which, according to the footnotes in the lab report, indicates that the ion abundance ratio for the compound in question did not meet the acceptance criterion. These flags occur in both the PCB and D/F analyses, but are more common in the D/F analyses. I need assistance in interpreting the concentration values associated with the analytes flagged with an R. How were data flagged with an R handled by the lab? How was the data used in interpreting the analyte concentrations? (i.e. Wha t value was used when calculating concentrations?)

One of the method requirements for positive peak id entification is that the observed ion abundance rat io of the two monitored chlorine isotope m/z responses ne eds to be within 15% of the theoretical ratio. I f a peak fails this criterion, then it cannot be identified as a real PCDD/F or PCB congener. However, the presence of a peak at the right retention time can mask the prese nce of a real peak. Therefore we quantify this v alue based upon the instrument response to the lower of the tw o monitored masses and report this value with a ‘<’ in front of the value to represent the maximum possibl e level. Then this <value is flagged with the ‘R’ flag. Note that by standard protocols we are to quantify down to 2.5:1 signal to noise. As you ca n imagine, as one approaches 2.5:1 signal to noise (presented as the EDL), that there is significant random noise contribution to each peak response. Therefore, a s one approaches the EDL, the frequency of ‘R’ flag ged data increases. These data points may represent real P CDD/F or PCB values, but have failed the tight +/-1 5% ion abundance ratio criterion. In our judgment and ac cording to the method, ‘R’ flagged data are not con firmedp. 3 of 5

peaks of PCDD/F or PCB. However, for the calculat ion of upper bound TEQs, we include the full maximu m possible concentration for that peak in the corresp onding calculations. For lower bound TEQ values, we take the ‘R’ flagged results as zero.

CARB 428 Section 6.7.4 (reproduced below for conven ience) requires calculating the EMPC when the quantitation ion is determined to be greater than t he EDL but the ion abundance ratio criteria is not met. It appears that the lab used the secondary ion to repo rt the results instead of the quantitation ion. Ho wever, there does appear to be some confusion on this poin t, as the lab states the value is based on the “low er of the two monitored masses” but that it represents the “m aximum possible level”. Please confirm or clarify our interpretation that your calculation procedure uses the standard calculation to quantitate target comp ounds for the “upper” bound TEQ and flags these data as E MPC if appropriate. Please also confirm or clarify our interpretation that your calculation procedure uses the smaller of the characteristic compound ions to quantitate target compounds for the “Lower” bound T EQ. The EMPC would be the maximum possible level, which is the value using the method required quanti tation ion, not the secondary ion. Please confirm which value reported with the less than sign is the EMPC.

Additionally, if the results provided are not the E MPC values, we would like these values to be provid ed, or if they are provided already, please identify your var iable name and where this value is found in your re port.

6.7.4 Estimated Maximum Possible Concentration If the response of the quantitation ions is determi ned to be greater than 2.5 times the background sig nal, but qualitative identification criteria are not met, an “estimated maximum possible concentration” must be calculated according to Equations 428-7 and 428-8.

• I need help interpreting the concentration values a ssociated with the analytes that are flagged with a “J” (which, according to the footnotes in th e lab report, indicates that the analyte was detect ed below the calibrated range) but which have listed c oncentrations well above the listed EDL. For example, for Total MonoCB – which is flagged with a J on page G-165 of the final report - the EDL is listed as 24 picograms (pg) whereas the listed conc entration is 2400 pg.

‘J’ flag generally refers to estimated value and be low the instrument calibration range. The flag an d basic interpretations are derived from the US EPA CLP ana lytical program. Below is the actual wording from the PCB CLP document CBC01.2, the CLP version of 1668A. Note that the CRQL is at the concentration equi valent
to the level in the low calibration standard.

“J - Indicates an estimated value. This flag is use d when the mass spectral data indicate the presence of an analyte m eeting all the identification criteria in Exhibit D, but the resul t is less than the Contract Required Quantitation Limit (CRQL), as listed in Exhibit C, but greater than the calculated Estimate d Detection Limit (EDL).”

Although not specifically defined in CBC01.2, by so me interpretations, any homologue group total value s are ‘J’ flagged. Perhaps this is due to the summation of peak responses in which some or many are below the level
of the low calibration standard.

• The concentration values associated with the analyt es that are flagged with both “J” and “R” are listed in the spreadsheets as below detection limit (BDL). See for example OCDD (flagged with J and Rp. 4 of 5

in the lab report and listed as BDL in the D/F port ion of the associated Excel spreadsheet PrAl_ICR_ PastePlant.xls). Why are these data marked as BDL w hen they were analyzed above the MDL? Data that is flagged with only a J is not marked as BDL. This is what we would expect; we would expect onl y U flagged data to be marked BDL.

BDL should be a flag on ‘R’ flagged data but not ‘J ’ flagged data. ‘J’ flagged data should be ADL. You are correct that U flagged data should be BDL.

Why are the R flagged data marked at BDL? Doing so assumes that any time the quality assurance indica tors of the method are not met that the compound is not detected, when there is no indication that this assumption is accurate. Many R flags occur with a J flag, indicating that R flagged data may very wel l have been detected. If data is both R and J flagged – h ow can data be both BDL and ADL?

• The material throughput rates listed in the Final R eport do not always agree with those listed in the summary spreadsheets. For example, Tables 2-13, 2-19, 2-23, and 2-28 list throughput rates of 10.33 tons per hour for potline 2, 6.30 tons per ho ur for potline 3 (listed as 161 duct), 7.79 tons p er hour for carbon bake, and 33.7 for paste plant, res pectively. However, the PCB summary spreadsheet for potline 3 (again, listed as 161 duct) lists a t hroughput of 7.79 tons per hour. Please confirm the material throughput rates for the tested potlines, the carbon bake furnace and the paste plant during the testing.

For Scott Brown:

• The carbon bake furnace and the paste plant summary spreadsheets indicate throughput materials of aluminum as opposed to the expected ma terial of green anode. Please confirm the throughput materials for the carbon bake furnace an d the paste plant and whether the pounds per ton emissions rates cited in these spreadsheets are in units of pounds of pollutant per ton of aluminum produced or pounds of pollutant per ton of green an ode processed.

For Scott Brown

• Specifically regarding the PCB analyses - I notice that although the lab reports cite values of PCB in units of pg, those values were listed in the ass ociated summary spreadsheets in units of nanograms (ng). That is, for example, the lab results indicat e 2,400 pg of total monochlorinated biphenyls whereas the PCB portion of the associate d spreadsheet (PrAl_ICR_PastePlant.xls) indicates 2,400 ng of total monochlorinated biphenyls. This w ould appear to have caused an overestimation of PCB emissions from your facility by a factor of 1,0 00. Please confirm or modify, as appropriate, the P CB emissions values cited in the summary spreadsheets.

For Scott Brown’s input. We reported in pg

.

• Specifically regarding the PCB analyses - I notice that for the homologue group totals the EDL is
sometimes lower than the cited concentration for th ose homologue groups flagged with a U. For example, for the Total OctaCB homologue group (whic h is flagged as U) the lab report cites a concentration of <23 pg (which would suggest a meth od detection limit of 23 pg) but an EDL of 9.1 pg. Please clarify how the EDL is less than the method detection limit for these groups.

The EDL value by each total homologue group total i s from a general signal:noise measurement for the e ach homologue group total region. However there are m any peaks for each homologue group totals. For example for octachlorobiphenyl, there are 12 congen ers (11 peaks, one co-elution). Each peak has it’ s own EDL determined. The <23 value is the highest EDL among the individual octa- peaks.p. 5 of 5



### Please provide the D/F and PCB MDLs per page 3 of A ttachment 1 of the ICR. (Note that the ICR specified that you must use the MDL determination p rocedure in EPA Method 301, Section 15 to develop the MDL and further specified that the MDL must be determined in the same matrix as the samples that will be analyzed.)

Please provide your definition of, and your current values for, Level of Detection (LODs) and Level of Quantitation LOQs for D/F and PCBs. Please clarify why you flag some data that is well above the EDL as “J” (For example (see page 610 of 748 in the pdf version of the report), OCDD is reported at more than 18 times EDL but is still J flagged.)

Additionally, in the lab report (for example, see p age 610 of 748 in the pdf version of the report) we need an explanation on why there are two runs on th e samples. Did these compounds fail to meet quality specifications in the first analysis, requi ring dilution or reprocessing archived samples to determine the concentration? Or does your procedur e perhaps use different GC columns to resolve particular congeners?

• Specifically regarding the D/F analyses - When the cited mass for a total homologue group is preceded by a “<” symbol does this indicate below d etection limits? I ask because the lab report does not provide a “U” flag for these homologue groups.

Yes it identifies the values as non-detected at the listed value.

Note that my contractor and I have not finished rev iewing the report yet, and we may have other questi ons in the future. We are trying to resolve questions as we find them instead of holding them until the end.

Thanks,

David Putney, Environmental Engineer U.S. Environmental Protection Agency Office of Air Quality Planning and Standards Sector Policies and Programs Division 109 T.W. Alexander Drive, RTP, NC 27711 Mail Drop D243-02 Ph: (919) 541-2016 Fax: (919) 541-3207
Email: putney.david@epa.gov

Regards,



### Scott Brown Senior Project Manager CleanAir 847-654-4544 (office) 847-612-0561 (cell)