### Example Proposed MDL Calculations using 2009 Post-FACDQ Pilot Study Data

Data generated during EPA’s 2009 post-FACDQ Pilot Study (EPA 821 -R-11-005) were usedto provide an example of how the proposed procedure would be used to calculate MDLs based on blank results and

on spiked sample results . The 2009 study included an assessment of various detection limit (DL) procedures using blank and/or spiked sample data generated with EPA Methods 200.7 and 625 . Because one of those DL procedures utilized the same calculation formula that is used in the proposed MDL, the 2009 study contains data from which the proposed MDL procedure could be applied.

The 2009 study included the evaluation of more than one limit: single

-laboratory MDLs calculated using

a t

-statistic (DLT

### ) and a tolerance limit k (DLK

### ), single-lab LCMRLs, and an MRL determined using the individual laboratories’ LCMRLs . The multi

-phase study included calculation of initial start-up limits

, verification/adjustment of the initial limits using additional data, and use of a third set of blank and spiked sample data to independently evaluate the calculated limits based on pre-determined detection and quantitation MQOs . Due to the large number of analytes to be assessed using the two methods, the laboratories often analyzed extra spiked samples at some concentrations and analyzedadditional concentrations that weren’t required for that analyte. As a result, the number of available results for which the proposed MDL procedure could be applied varied across laboratories and analytes.

Details regarding the specific set of 2009 Pilot Study data used in the calculation of the MDL based on blanks (MDLb

### ) and spiked samples (MDLs

### ) for each method and laboratory are as follows

.

•

•

• MDLb 

### (both methods): All pre

-existing blank sample data submitted by the labs at the start of the 2009 study, including those used in the calculation, lab evaluation, and independent statistical evaluation of the 2009 limits, were used in this calculation, with the exception of any results that were flagged as invalid by the laboratory or data reviewers. This yielded78-131 available blank results for each lab/analyte for Method 200.7, and 30-32 blank results for each lab/analyte for Method 625.

MDLs 

### (Method 200.7): All spiked sample data at the spike level chosen as appropriate for a Quantitation Limit (QL) based on the laboratories’ DLT

### calculated during the 2009 study were used. These spiked samples included the initial evaluation of MQOs at that spike level,the ongoing evaluation of MQOs at that spike level, and any additional results from samples spiked at the same concentration that were not required but were reported. Any results that were flagged as invalid by the lab or data reviewers were excluded. This yielded between 14 and 28 available spiked sample results for most labs/analytes (Laboratory 3 used slightly different spike levels during the QL verification analyses that did not exactly match the determined QLs for some analytes, so only seven spiked samples were available for some analytes).

MDLs 

### (Method 625): All spiked sample data at the spike level chosen as appropriate for a QL based on downspiking evaluations performed by the laboratories’ during Task 2 of the 2009 study were used. These spiked samples included the initial evaluation of MQOs at that spike level, the ongoing evaluation of MQOs at that spike level, and any additional results from samples spiked at the same concentration that were not required but were reported. Any results that were flagged as invalid by the laboratory or data reviewers were excluded. As a result, at least 7, and as many as 16, spiked samples were available for the calculation for most labs/analytes (in some cases a laboratory used slightly different spike levels during the QL verification analyses that did not exactly match the determined QLs for some analytes, so only seven spiked samples were available for those analytes).Page 1 of 24 NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Copper All results in ug/L

MDL Summary

Lab 1

Blanks Spikes No. of results 78 15 Spike Conc. NA 4 Mean -0.005525609 NA Std. Dev. 0.651297421 1.429282 t-statistic 2.375756994 2.624494

MDLb 1.541798795 MDLs 3.751142658 Spike/MDLs 1.066341743 OK Max. MDL 3.751142658 Data source for Max MDL spikes Lab 2 Blanks Spikes No. of results 131 14 Spike Conc. NA 6 Mean 0.080381679 NA Std. Dev. 1.559765961 0.745143 t-statistic 2.355374585 2.650309

MDLb 3.754214782 MDLs 1.974858542 Spike/MDLs 3.038192292 OK Max. MDL 3.754214782 Data source for Max MDL blanks Lab 3 Blanks Spikes No. of results 93 14 Spike Conc. NA 20 Mean -0.0221251 NA Std. Dev. 2.66471693 2.685339 t-statistic 2.36756577 2.650309

MDLb 6.286767494 MDLs 7.1169769 Spike/MDLs 2.810181947 OK Max. MDL 7.1169769 Data source for Max MDL spikes

NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Copper All results in ug/L

MDL Data

Lab 1 MB Lab 1 Spike

Result Result 0.110192198 3.904315291 -1.172794574 3.473491248 -0.410128994 3.833579032 0.184235903 4.037972079 0.135578175 4.109013187

0.22177357 3.069275774 0.60628568 4.507359741 -0.168719745 3.665449667 1.434762742 9.188680853 -0.329757351 4.698745904 0.546078285 4.760787246 -0.425599897 4.671931822 0.626738615 4.68827267 -0.390079261 4.74388168 0.139936755 5.763216588 0.016945955 0.046957889 -0.646932899 -0.343701375 Lab 2 MB Lab 2 Spike Result Result -1 5.53 0.98 6.16 1.33 6.5941 0.94 5.48 1.31 6.25 0.14 5.3466 2.49 5.1603 -0.76 5.5009 -0.33 4.3021 -0.61 6.8877 -0.75 6.508 -1.96 5.8244 -2.56 6.766 -1.68 6.6588 -0.33 -1.21 -0.85 -1.84 -0.47 Lab 3 MB Lab 3 Spike Result Result -4.591831376 20.2 -3.879824183 19.4 -0.872600748 23.2 -0.667889009 23.8 0.986243953 16.2 3.211006913 17.6 3.318523541 18.9 -3.596476278 23.4 -4.919131008 23.8 -5.836270553 22.6 -0.947259598 19.6 5.588759485 20.2 6.379432274 18.7 7.549726956 16.3 6.881223767 2.081867584 -1.233152897 2.253657908 -0.64847756Page 2 of 24 NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Copper All results in ug/L

MDL Data

Lab 1 MB Lab 1 Spike

Result Result -0.3588574 -0.102554651 -0.828046993 0.433466795 0.064076761

0.39685425 0.375563998 -0.059071791 0.311081507 -0.828321407 0.392678633 0.097757272 -0.161907832 0.187397003 -0.507532146 -1.295727469 0.328143311 0.171099157 0.534106735 0.036357735 0.416425235 0.952534423 1.155377186 0.523802194 -0.354632341 -0.013640397 0.350564903 -0.143705215 1.1479094 0.246609916 0.212729772 -0.368725013 -1.157498786 -0.553013253 -0.880721356 -1.121877272 -0.459824289 0.187241916 0.150739308 -0.131231976 Lab 2 MB Lab 2 Spike Result Result -0.66 -0.39 -1.94 0.05 -0.29 -1.54 -0.62 -0.98 1.08 0.72 1.52 2.43 3.48 0.05 0.77 -2.36 0.58 -0.89 -1.93 -0.19 0.88 -1.37 3 -1.65 1.07 -0.14 0.59 1.27 0.29 -0.58 1.11 1.84 1.02 0.44 2.37 0.65 3.49 0.85 0.43 -0.47 Lab 3 MB Lab 3 Spike Result Result -6.123918829 2.327201914 0.429690413 0.379531136 -1.666120762 -0.335349391 -3.309510774 3.644419725 1.037008668 3.685436725 3.551120536 -1.905364228 0.390009411 0.668776259 0.007814075 -0.891098859 0.503700004 -1.337329948 -0.337700116

3.41617634 -0.060301119 1.145106548 0.127701491 3.183536644

3.10385928 0.823500842 0.378234309 -0.997287001 -1.494213866 -0.262263845 -0.679475493

-0.35853038 0.503621875 -0.620339762 0.852734187 1.389700349 -0.315385951 -2.251664879 -2.054771117 -2.431827731Page 3 of 24 NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Copper All results in ug/L

MDL Data

Lab 1 MB Lab 1 Spike

Result Result 0.760452094 0.408115203 0.021368439 -0.341096861 -0.720774585 -0.335755679 -1.289879145 0.767373303 -0.391282385 -0.752602741 -1.143802567 -0.650297186 -0.406086623 0.401588143 1.742103952 1.787142836 0.668550909 -0.673370395 0.189856294 Lab 2 MB Lab 2 Spike Result Result -2.2 -1.76

-2.3 -2.45 -1.91 -2.49 -0.38 -0.23 1.21 2.57 2.15 -0.72 -2.98 -1.93

-1.4 0.14 -1.78 1.65 0.98 0 -0.33 0.24 0.71 2.59 1.21 2.73 2.53 2.35 -1.75 0.05 -0.14

0.7 -0.88

-1.3 -1.54 0.96 0.05 0.96 0.05 1.63 Lab 3 MB Lab 3 Spike Result Result -2.456182528 -4.632705316 3.024572093 0.385143052 2.096686253 3.515015516 1.589134146 2.144785609 -1.970505942 -0.705776349 -0.863588199 -0.666133421 1.532329711

0.2856228 2.116116657 0.054010691 0.237685197 -3.746769119 0.148143566 -1.798935847

-3.00034412 -6.147546282 -1.200529664

-1.09135812 -1.588174933 -3.359588071 -2.961591992

0.27692216 -1.030095785

-0.16914572 1.594202589 -0.86589601 2.431306668 -0.408399091Page 4 of 24 Lab 1 MB

Result Lab 1 Spike Result Lab 3 MB Result Lab 3 Spike Result NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Copper All results in ug/L

MDL Data

Lab 2 MB Lab 2 Spike

Result Result 2.48 1.54 2.11 2.67 -0.68 -0.24 0.54 -0.68 -0.24 0.54 0.13 0.13 -0.22 0 3.76 -0.11 0.18

0.8 0.67 -1.26 -1.22

-2.6 -1.34 -3.67

-3.8 0.98 -0.65 -0.72 1.53 2.92 1.69 1.48Page 5 of 24 NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Silver All results in ug/L

MDL Summary

Lab 1

Blanks Spikes No. of results 78 15 Spike Conc. NA 4 Mean 0.07703704 NA Std. Dev. 0.250260716 0.769163 t-statistic 2.375756994 2.624494

MDLb 0.671595688 MDLs 2.018664855 Spike/MDLs 1.981507722 OK Max. MDL 2.018664855 Data source for Max MDL spikes Lab 2 Blanks Spikes No. of results 131 14 Spike Conc. NA 15 Mean -0.49374046 NA Std. Dev. 2.338797303 1.61556 t-statistic 2.355374585 2.650309

MDLb 5.015003269 MDLs 4.281733304 Spike/MDLs 3.503254158 OK Max. MDL 5.015003269 Data source for Max MDL blanks Lab 3 Blanks Spikes No. of results 100 14 Spike Conc. NA 6 Mean 0.025338134 NA Std. Dev. 0.70945164 0.458584 t-statistic 2.364605862 2.650309

MDLb 1.702911641 MDLs 1.215389706 Spike/MDLs 4.936688182 OK Max. MDL 1.702911641 Data source for Max MDL blanks

NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Silver All results in ug/L

MDL Data

Lab 1 MB Lab 1 Spike

Result Result 0.009797505 3.702886257 1.044387899 3.363311619 0.078363692 3.400041844 0.326414874 3.322684964 -0.138432618 3.374602593 -0.132879628 3.403947192 0.035874404 3.028962158 0.009409216 3.419865493 0.136225658 6.364382097 0.042956834 3.939958896 0.206638231 3.685154805 0.091295681 3.988008742 0.352511018 3.759445222 -0.059856745 3.728240463 -0.046618457 3.685483405 -0.242465187 0.019637518 -0.32641973 -0.217056903 Lab 2 MB Lab 2 Spike Result Result 2.89 11.16 3.16 14.08 2.92 14.4946 2.49 13.86 1.43 13.86 -0.38 12.0578 1.74 13.5971 -1.81 15.4911 -0.98 13.4923 0.53 16.5105 -3.06 16.0789 -1.94 16.2632 -2.92 13.7577 -1.34 16.2615 -1.34 -2.77 -0.92 -1.54 0.39 Lab 3 MB Lab 3 Spike Result Result 0.370310279 6.83 0.003748583 6.42 2.142445021 5.36 -0.155697473 5.78 0.059735263 6.85 0.050421867 6.76 -0.477142907 6.49 -2.137285509 6.4 -1.435526378 7.12 -1.567383004 6.56 -1.158318585 6.58 0.020029751 6.8 0.671563372 6.28 -0.036067628 6.76 -0.024960758 0.044847021 -0.289745193 0.343485421 0.229751575Page 6 of 24 Lab 1 MB Lab 1 Spike

Result Result -0.054387721 0.172753877 -0.063035217 0.031704528 0.469200175 0.310700459 0.213488197 0.101577445

0.08865954 -0.27513639 -0.205149301 -0.421075724 0.302345334 -0.037481913 0.028310651 -0.243765409

0.16704158 0.19516165 -0.274230827 0.267822014 -0.314993321 -0.394076364 0.312740889 -0.030790471 0.012583753 0.254795797 0.016413244

0.34159559 0.228616754

0.57980794 -0.13896459 -0.111172988 0.110551477 0.101702178 0.374889831 -0.047342733 0.160526657 0.114460323 -0.06542586 -0.117710454 Lab 2 MB Lab 2 Spike Result Result 1.62 -1.04 -0.65 0.07 -0.4 -0.09 -2.34 -2.85 2.08 0.43 3.24 3.82 6.56 -1.63 -1.55 -3.27 -1.09 -2.69 -3.34 -2.25

-0.4 -3.78 -2.49 -3.42 -0.16 -2.07 -2.04 -0.17 -0.33 -3.39 -1.61 0.97 -0.56 -0.65 1.41 2.19 3.14 -1.77

1.1 1.19 Lab 3 MB Lab 3 Spike Result Result -0.202983787 0.405372471 0.196055758 -0.143462681 0.559464344 -0.133825535 -0.287863647 -0.702189306 -0.200629867 0.010732786 0.022558387 0.028061631 0.087223783 -0.505353109 0.357322988 -0.702167451 -0.272161172 -0.726957461 0.015662706 0.391527909 -0.43127135 0.191945511 -0.077860364 -0.698838576 0.052248205 0.814793787 0.158620062 -0.324208227 0.544542538 -0.271840976 -0.330026719 -0.4541795 -0.354093858 -0.500156688 -0.424019242 -0.438924252 -0.039927028 0.079008976 -0.348089451 -0.091171165 NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Silver All results in ug/L

MDL DataPage 7 of 24 Lab 1 MB Lab 1 Spike

Result Result 0.109410402 -0.087319938 0.307342944 -0.133214481 0.129406555 0.182589501 0.277991919 0.5704949 0.031544285 -0.010716933 0.042909546 -0.307620728 -0.132356153 0.202781638 0.165695684 0.034744986 0.267729916 0.616930193 0.388051057 Lab 2 MB Lab 2 Spike Result Result -6 -5.74 -4.56 -4.73 -3.21 -6.17 -1.38 -0.08 2.21 4.74 1.74 2.43 -1.09 -1.01 1.34

4.1 1.76 -1.02 2.29 0 -0.99 -1.99 1.16 1.73 1.47 3.54 2.68 0.43 -3.17 -2.13 -2.48 0.43 -2.82 -2.56 -2.31 0.34 0.35 0.34 0.35 1.75 Lab 3 MB Lab 3 Spike Result Result -0.037220206 -0.042882522 0.110044999 0.215118562 0.257063251 0.003569978 0.207336273 0.305278244 0.439466786 -0.657680402 0.405884935 0.392036424 0.149543779 0.812413497 0.630166587 -0.027663274 -0.655725259 -0.650703187 -0.343881669 0.355994103 0.052477333 -0.589910821 2.387938611 -1.876231688 0.651168524 1.376003189 1.782828969 0.972235129 0.765953592 0.004253357 1.267816407 0.217527647

-0.2441594 0.014174874 -0.046912526 -0.511572061 -0.860185941

0.52025353 -0.067076142 0.959059331 NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Silver All results in ug/L

MDL DataPage 8 of 24 Lab 1 MB

Result Lab 1 Spike Result Lab 3 MB Result Lab 3 Spike Result 1.982859409 NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Silver All results in ug/L

MDL Data

Lab 2 MB Lab 2 Spike

Result Result 3.25

1.5 1.67 0.71 -2.83 -2.51 -0.24 -2.83 -2.51 -0.24 0.14 -0.36 0.72 -0.64 3.38 -2.16 -1.25 -1.62 0.51 -1.11 -3.03 -3.16 -1.89 -1.89 -4.75 2.26 -2.63 -4.12 -0.72 1.81 -0.07 -0.15Page 9 of 24 NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Potassium

All results in ug/L

MDL Summary

Lab 1

Blanks Spikes No. of results 78 14 Spike Conc. NA 2000 Mean 198.7266104 NA Std. Dev. 528.5911551 127.1687 t-statistic 2.375756994 2.650309

MDLb 1454.530744 MDLs 337.0362707 Spike/MDLs 5.934079427 OK Max. MDL 1454.530744 Data source for Max MDL blanks Lab 2 Blanks Spikes No. of results 131 28 Spike Conc. NA 300 Mean -0.20717557 NA Std. Dev. 52.00354179 16.12467 t-statistic 2.355374585 2.47266

MDLb 122.2806451 MDLs 39.87081607 Spike/MDLs 7.524300468 OK Max. MDL 122.2806451 Data source for Max MDL blanks Lab 3 Blanks Spikes No. of results 95 21 Spike Conc. NA 1800 Mean 73.51775379 NA Std. Dev. 290.5936506 283.8647 t-statistic 2.366674361 2.527977

MDLb 761.2582962 MDLs 717.603534 Spike/MDLs 2.508348851 OK Max. MDL 761.2582962 Data source for Max MDL blanks

NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Potassium

All results in ug/L

MDL Data

Lab 1 MB Lab 1 Spike

Result Result 153.5441665 1969.219406 361.5118446 1990.862782 38.76742755 1798.061089 48.07283271 1972.452254 106.7234948 2055.727622 19.81261286 1912.960465 0.909211466 1912.289557

61.0455934 1958.383366 62.48872311 1910.276379 58.13170403 1897.510389 142.4393888 1861.136013

86.2978145 1851.173622 251.9017681 1679.223782 289.0659868 1575.220055 572.4680848 82.16176787 171.0982955 218.9532263 166.8923286 Lab 2 MB Lab 2 Spike Result Result 0 276.347 -33.14 292.902 -19.22 287.144

-0.64 292.901 -8.27 290.741 2.54 265.554 -2.55 266.994 1.28 287.088 4.49 273.977 32.69 296.06

3.81 269.835 12.06 256.722 10.15 291.228 33.63 308.483 21.57 295.42 -10.15 290.438 23.37 251.996

7.58 251.995 0.63 275.488 Lab 3 MB Lab 3 Spike Result Result 126.3033319 1420 -26.78716695 1360 -211.6862651 1330 -128.9135447 1330 -19.52748924 1330 -81.05942982 1130 171.6546612 1290

338.263206 1630 531.599417 1320 155.962646 1720 911.1728204 1860 -100.5229058 1460 187.0836177 1700 210.0579937 1620 -291.3230065 1130 -157.9649219 941 -234.1425776 1060 -93.65549832 1980 84.09563527 1760Page 10 of 24 NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Potassium

All results in ug/L

MDL Data

Lab 1 MB Lab 1 Spike

Result Result 72.93611538 28.36882459 112.0623529 134.5576667 -48.23320623 155.8903944 -108.933274 252.5675393 1.214680164 213.4874181 -158.002266 -181.9862722 93.28303269 -246.1674985 -84.31565478 84.90830281 19.01310612 -145.0030105 -248.2746899 -102.2709378 -173.9781196 -146.7327156

-174.758202 -124.9487393 33.25802864 129.9873229 130.4768636 175.1769682 4479.513501 479.4832186 72.69011653 63.53852414 295.6684696 212.9293114 318.0144852 321.5147792 245.0584679 224.8612263 249.6272341 317.2926056 Lab 2 MB Lab 2 Spike Result Result 51.78 265.526 -85.47 277.627 -134.85 281.418

-66.48 296.816 -44.32 251.313 -55.17 280.009 -54.45 254.113 -28.66 279.312 14.33 258.31 -11.47 -6.3 0 5.04 17.6 31.2 12.32 51.52 28.82 -9.63 -45.91

-38.8 -59.49 13.42 -9.14 15.78 -27.41 -78.84 -65.88 -62.85 -18.57 -24.33 -31.38 -23.06 -20.49

-5.52 25.17 -18.21 -13.96 -14.16

8.01 Lab 3 MB Lab 3 Spike Result Result -264.5595625 1500 222.1398379 1850 81.33553815 408.4785567 -5.841011147 -166.3709312

115.446366 351.1169385

239.096944 -87.04116169 -504.8530763 444.0816064 307.4220166 347.5674832 220.4657369 -480.2216703 807.2152463 773.3170995 -109.672253 -75.47753188 -207.9060183 -54.88481857 -196.9939038 136.9111424 260.5558568

51.6151023 60.74552727 104.3139823 181.4399576 221.1779418 96.68036868 44.50546335 162.4306251 128.0224961 -77.40426397 42.15066833 42.61556196 -128.9252091 91.29660848 -47.9637055Page 11 of 24 NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Potassium

All results in ug/L

MDL Data

Lab 1 MB Lab 1 Spike

Result Result 503.141199 572.342068 118.2082291 50.43457085 225.8285203

295.402048 186.8943287 261.2031968 718.6896406

211.239011 237.577879 86.78275129 269.4539994 329.2981428

649.808391 322.5924649 167.4277477 146.4096638 281.8795196 Lab 2 MB Lab 2 Spike Result Result 1.2 -7.78 12.56

5.38 4.78 -5.39 -15.86 -17.69 -17.38 -11.17 -11.17 15.71 -25.13 -47.12 -10.05

-1.26 -25.13 -10.79 -3 -20.99 -12.91 -22.76 -41.82 -37.67 -11.02 -34.43 -55.24 -35.73 -16.26 10.04 -1.89 9.41 -31.38

-3.77 -13.18 26.64 53.27 26.64 53.27

29.4 Lab 3 MB Lab 3 Spike Result Result -24.653982 47.64982897 -47.2494881 97.22695285 -29.96755426 -55.26157139 202.6678408 141.9904871 -47.99762911 624.3390425

465.785158 -9.291738868 -385.5434929 142.0124277 655.3401427 373.3956547 1366.572985 26.31389793 -137.2029207 14.76850179 75.02435449 1.311240121 45.70967162 -22.88442993

-159.857568 29.00855051 -44.19259202 -43.87674144 45.68359401 -169.8328224 -95.69571903 -146.82273 -26.21455002 -229.3366186 -111.2840695 -488.0875804Page 12 of 24 Lab 1 MB

Result Lab 1 Spike Result Lab 3 MB Result Lab 3 Spike Result NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Potassium

All results in ug/L

MDL Data

Lab 2 MB Lab 2 Spike

Result Result 37.98

7.97 22.05

8.58 16.48 21.53 29.78 16.48 21.53 29.78 326.44 302.06

69.24 120.68

50.77

10.9 17.8 52.14 1.9 -15.26 -13.99 -26.68 -39.05 -27.99 -86.57 -37.89 -31.67 -19.27 34.17 47.84 41.57 -16.79Page 13 of 24 NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Calcium All results in ug/L

MDL Summary

Lab 1

Blanks Spikes No. of results 78 14 Spike Conc. NA 250 Mean 27.49377235 NA Std. Dev. 34.82303817 45.19941 t-statistic 2.375756994 2.650309

MDLb 110.2248488 MDLs 119.7924039 Spike/MDLs 2.086943678 OK Max. MDL 119.7924039 Data source for Max MDL spikes Lab 2 Blanks Spikes No. of results 131 28 Spike Conc. NA 300 Mean 31.9110687 NA Std. Dev. 105.7077811 14.98377 t-statistic 2.355374585 2.47266

MDLb 280.8924898 MDLs 37.04977941 Spike/MDLs 8.097214202 OK Max. MDL 280.8924898 Data source for Max MDL blanks Lab 3 Blanks Spikes No. of results 99 14 Spike Conc. NA 150 Mean 7.41557008 NA Std. Dev. 22.50332782 10.81437 t-statistic 2.36500241 2.650309

MDLb 60.63599463 MDLs 28.66141438 Spike/MDLs 5.233517021 OK Max. MDL 60.63599463 Data source for Max MDL blanks

NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Calcium All results in ug/L

MDL Data

Lab 1 MB Lab 1 Spike

Result Result 8.913142194 267.8350768 41.80811894 268.9355953 29.40816248 263.7230263 10.27613846 290.8747667

29.6154687 266.6347153 8.306378544 255.6012775 11.63235774 415.3567715 75.91422161 243.955909 7.621454791 239.3540887 18.19284447 247.9937423 289.4407611 239.1199719 39.53694632 244.4710158 54.26445595 249.5400299 37.39104407 242.7548859 28.42708863 20.62375633 12.36559774

64.9723499 23.91174729 Lab 2 MB Lab 2 Spike Result Result 22.07 313.16 16.08 310.379

0.2 335.71 18.16 321.256

-3.9 337.675 4.39 319.594 -1.49 333.278 34.29 341.154

37.1 317.843 14.8 314.813 2.82 313.164 6.59 318.147 -3.6 334.949 16.79 327.453 17.66 316.685 25.43 334.543 42.14 308.041 16.03 308.449

5.44 348.367 Lab 3 MB Lab 3 Spike Result Result 20.5338322 161 8.218626397 161

-14.319041 162 -48.44428121 156 6.671077364 157 11.32476353 147 14.75476233 157 5.063183633 161

6.67419835 152 9.005259978 153 6.486946168 167 6.333796544 170 9.711455931 181 8.426476602 186 8.838786697 12.13515428 33.44102443 13.09764017 34.75989421Page 14 of 24 NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Calcium All results in ug/L

MDL Data

Lab 1 MB Lab 1 Spike

Result Result 24.48508725 25.19133925 11.08306372 28.99811075 21.90470669

19.7446982 26.55246466 17.72517506 27.89258055 16.39258824 15.04434212 51.05002125 15.21591395 20.02405267

23.8692069 53.57314802 45.57639819 14.98814351 18.58349649 41.27535995 28.69730425 18.13008953 61.93229633 34.43297974 17.11431166 15.37759284

81.1820023 10.21123331 17.05850903 33.39540955 34.47712061 19.29418565 14.36840874 12.14495135 -10.5168588 -14.16260231

-16.1774911 27.45565075 23.85681897 35.29783554 Lab 2 MB Lab 2 Spike Result Result 9.92 368.856 33.66 326.972 13.88 318.305

-3.7 323.132 -2.34 314.316 10.28 318.957 16.14 322.925

3.23 324.414

5.5 360.396 2.38 15.89

4.68 5.24 11.26 20.81 136.81 166.17 127.91

-0.13 -3.61 11.79 -2.19 364.02 7.87 121.83

-6.71 -6.87 20.44

1.44 7.68 7.86 15.76

8.54 0.95 14.7 13.89 13.68 14.25 -6.93 1.34 Lab 3 MB Lab 3 Spike Result Result 15.77100097 13.59143752 39.73524978 23.61807531 -1.67363297 14.9442262 -2.068797368 -0.664686617 29.01147732 -13.94078994 -30.01336099 32.16409025 19.20749472 -71.30266166 19.85615409 17.15794487 25.77726059 4.205912261

12.0480773 12.14073181

9.58671388 12.27271679 7.175008875 10.24436224 18.33283828 27.26688639 18.51051388 16.56076594 -0.523139105 8.572334376 12.82961547 18.84218348 8.684011672 10.18217272 2.462600559 6.442615425 7.173828945 6.674856611 10.84960634

8.32790055Page 15 of 24 NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Calcium All results in ug/L

MDL Data

Lab 1 MB Lab 1 Spike

Result Result 13.81335341 12.03330775 22.89086559 19.46839316 29.91832208 15.44028746 12.00521671 14.66326967 13.03371031 43.95358652

13.9338787 6.147445834 4.050128647 10.16934582 50.73693579 29.01294052 6.750605507 14.64279939 36.48816957 Lab 2 MB Lab 2 Spike Result Result 18.92 23.93

9.21 11.39

7.01 8.15 13.62

0.03 17.49

4.33 5.99

6.3 -2.5 1.41 29.08

2.63 -10.14

7.04 39.28 -4.75 10.51

-1.7 -3.42 23.88 68.41 -4.61 73.79

5.97 -4.36 4.87 3.58 0.94 -9.71 1.68 -7.73 12.17

9.39 12.17

9.39 28.47 Lab 3 MB Lab 3 Spike Result Result 11.14364811 34.69268841 20.62108321 4.181814697 11.70315135 13.05949312 7.702409302 9.027679095

27.5405228 -93.54798682 -75.62916982 -76.52538025 5.349697248 9.993973563 7.290918245 9.623527556 7.257183426 36.76606233 21.82859029 -0.163404341 2.140220528 23.23631054 1.233069858 -1.863066383 -2.843308588 7.033667634 -4.222525496 5.949150223 17.61840384 3.310065839 1.858570627 4.500041364 41.13049693 24.72913088 3.951067967

4.70263025 9.146684111 59.18512295 4.367238812 4.314811207Page 16 of 24 Lab 1 MB

Result Lab 1 Spike Result Lab 3 MB Result Lab 3 Spike Result NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Calcium All results in ug/L

MDL Data

Lab 2 MB Lab 2 Spike

Result Result 7.85 11.21

5.21 25.77 10.66 85.28

15.5 10.66 85.28

15.5 28.88 -0.51 9.39 8.36 788.61 138.05

11.53 101.66 806.56 1.4 -3.7 -1.47 -0.47

-8.6 -27.2 -8.61 7 2.22 8.96 10.54 164.19

0.21

### Page 17 of 24 NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Pyrene All results in ug/L

MDL Summary

Lab 4 Blanks Spikes No. of results 30 14 No. of numeric results 16 14 Spike Conc. NA 0.5 Mean 0.019159977 NA Std. Dev. 0.042880952 0.044464 Maximum 0.22893 0.42 99th percentile NA NA t-statistic 2.46202136 2.650309

MDLb 

### 0.22893 MDLs 

### 0.117842905 Spike/MDLs 

### 4.24293681 OK Max. MDL 0.22893 Data source for Max MDL blanks Lab 5 Blanks Spikes No. of results 30 16 No. of numeric results 0 16 Spike Conc. NA 3 Mean 0 NA Std. Dev. 0 0.25691 Maximum 0 3.1627 99th percentile NA NA t-statistic 2.46202136 2.60248

MDLb 

### NA MDLs 

### 0.668604509 Spike/MDLs 

### 4.486957478 OK Max. MDL 0.668604509 Data source for Max MDL spikes Lab 6 Blanks Spikes No. of results 32 14 No. of numeric results 13 14 Spike Conc. NA 5 Mean 0.04625 NA Std. Dev. 0.128734536 0.933141 Maximum 0.7 6.148 99th percentile NA NA t-statistic 2.452824193 2.650309

MDL b 

### 0.7 MDLs 

### 2.473111317 Spike/MDLs 

### 2.021744822 OK Max. MDL 2.473111317 Data source for Max MDL spikes

NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Pyrene All results in ug/L

MDL Data

Lab 4 MB Lab 4 Spike

Result Result 0 0.331 0.012821 0.317 0.0094173 0.322 0 0.328 0 0.325 0 0.309 0 0.261 0.017668 0.324 0 0.323 0 0.342 0 0.42 Lab 5 MB Lab 5 Spike Result Result 0 2.64 0 2.5341 0 2.5245 0 2.318 0 2.2889 0 2.8363 0 2.7627 0 2.5053 0 2.4808 0 2.2325 0 2.6486 Lab 6 MB Lab 6 Spike Result Result 0 4.132 0 3.931 0 4.252 0 5.222 0 5.585 0 5.546 0 6.148 0 2.967 0.01 3.205 0.01 3.985 0 4.787

### Page 18 of 24 NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Pyrene All results in ug/L

MDL Data

Lab 4 MB Lab 4 Spike

Result Result 0.014878 0.388 0 0.415 0 0.389 0.010825 0.015674 0.073021 0.044789 0.0338 0 0.22893 0.014736 0 0.015995 0.014865 0.028986 0.015488 0 0 0.022906 Lab 5 MB Lab 5 Spike Result Result 0 2.6518 0 2.9103 0 2.8412 0 3.1627 0 2.9375 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Lab 6 MB Lab 6 Spike Result Result 0.01 4.906 0 5.107 0 5.337 0.03 0 0.19

0.7

0 0 0 0.02 0.15 0.02 0 0.04 0 0.1 0.1 0.1

0 0

### Page 19 of 24 N ELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Diethyl Phthalate All results in ug/L

MDL Summary

Lab 4 Blanks Spikes No. of results 30 14 No. of numeric results 26 14 Spike Conc. NA 5 Mean 0.0369351 NA Std. Dev. 0.0214302 0.561984 Maximum 0.086134 3.71 99th percentile NA NA t-statistic 2.46202136 2.650309

MDLb 

### 0.086134 MDLs 

### 1.489432005 Spike/MDLs 

### 3.356984397 OK Max. MDL 1.489432005 Data source for Max MDL spikes Lab 5 Blanks Spikes No. of results 30 16 No. of numeric results 30 16 Spike Conc. NA 3 Mean 0.161691583 NA Std. Dev. 0.139731288 0.748013 Maximum 0.553688 5.2446 99th percentile NA NA t-statistic 2.46202136 2.60248

MDLb 

### 0.505712998 MDLs 

### 1.946688909 Spike/MDLs 

### 1.541078282 OK Max. MDL 1.946688909 Data source for Max MDL spikes Lab 6 Blanks Spikes No. of results 32 14 No. of numeric results 24 14 Spike Conc. NA 5 Mean 0.068125 NA Std. Dev. 0.06502791 0.723742 Maximum 0.2 5.198 99th percentile NA NA t-statistic 2.452824193 2.650309

MDLb 

### 0.2 MDLs 

### 1.918138986 Spike/MDLs 

### 2.606693278 OK Max. MDL 1.918138986 Data source for Max MDL spikes

NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Diethyl Phthalate All results in ug/L

MDL Data

Lab 4 MB Lab 4 Spike

Result Result 0.025296 2.28 0.030486 2.42 0.018012 2.63 0 2.11 0.074166 3.33 0 3.71 0.027538 3.5 0.025252 2.08 0.032436 1.87 0.029906 2.49 0.031746 2.57 Lab 5 MB Lab 5 Spike Result Result 0.160398 5.2446 0.122293 3.4178 0.198404 2.4641 0.208915 2.325 0.301039 2.2989 0.098144 3.2585 0.471467 3.2292 0.127886 2.5672 0.0970539 2.5383 0.0712565 2.1807 0.0931468 2.4748 Lab 6 MB Lab 6 Spike Result Result 0 4.2 0.07 4.676 0.03 3.409 0 4.421 0 4.952 0 5.198 0.09 5.169 0.07 3.191 0.04 3.066 0.02 4.717 0.05 4.319

### Page 20 of 24 NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Diethyl Phthalate All results in ug/L

MDL Data

Lab 4 MB Lab 4 Spike

Result Result 0.058708 2.3 0 2.09 0 2.52 0.047148 0.030289 0.034525 0.070956 0.048454

0.03305 0.05196 0.043045 0.035834 0.032243 0.041832 0.062209 0.046217 0.038617 0.086134 0.051994 Lab 5 MB Lab 5 Spike Result Result 0.171461 2.526

0.33681 2.725 0.101924 2.8085 0.489194 3.3927 0.0481936 3.2934 0.0659635 0.03912 0.0436056 0.0343616 0.0590028

0.241974 0.0656188

0.070244 0.087202 0.110891 0.098961 0.0590694

0.553688

0.22346 Lab 6 MB Lab 6 Spike Result Result 0.07 4.142 0.09 4.9 0.05 5.117 0.12 0.05 0 0 0.2 0.03 0.06 0.04 0.15 0.03 0.12

0.1 0.1 0.2

0 0.2

0 0.2

### Page 21 of 24 NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Isophorone

All results in ug/L

MDL Summary

Lab 4 Blanks Spikes No. of results 30 14 No. of numeric results 0 14 Spike Conc. NA 5 Mean 0 NA Std. Dev. 0 0.306488 Maximum 0 4.71 99th percentile NA NA t-statistic 2.46202136 2.650309

MDLb 

### NA MDLs 

### 0.81228665 Spike/MDLs 

### 6.155462485 OK Max. MDL 0.81228665 Data source for Max MDL spikes Lab 5 Blanks Spikes No. of results 30 16 No. of numeric results 0 16 Spike Conc. NA 3 Mean 0 NA Std. Dev. 0 0.23941 Maximum 0 2.9075 99th percentile NA NA t-statistic 2.46202136 2.60248

MDL b 

### NA MDLs 

### 0.623060596 Spike/MDLs 

### 4.814940986 OK Max. MDL 0.623060596 Data source for Max MDL spikes Lab 6 Blanks Spikes No. of results 32 14 No. of numeric results 1 14 Spike Conc. NA 5 Mean 0.003125 NA Std. Dev. 0.01767767 0.631533 Maximum 0.1 5.013 99th percentile NA NA t-statistic 2.452824193 2.650309

MDL b 

### 0.1 MDLs 

### 1.673756255 Spike/MDLs 

### 2.987292795 OK Max. MDL 1.673756255 Data source for Max MDL spikes

NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Isophorone

All results in ug/L

MDL Data

Lab 4 MB Lab 4 Spike

Result Result 0 3.5 0 3.57 0 3.73 0 3.67 0 4.71 0 3.95 0 4.15 0 4.03 0 4.13 0 4.03 0 4.05 Lab 5 MB Lab 5 Spike Result Result 0 2.4807 0 2.4643 0 2.6111 0 2.3982 0 2.3692 0 2.7877 0 2.6608 0 2.3932 0 2.3027 0 1.9861 0 2.183 Lab 6 MB Result Lab 6 Spike Result 0 3.706 0 3.809 0 3.725 0 4.481 0 4.989 0 5.013 0 4.98 0 3.1 0 3.393 0 3.892 0 4.295

### Page 22 of 24 NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = Isophorone

All results in ug/L

MDL Data

Lab 4 MB Lab 4 Spike

Result Result 0 4.04 0 3.79 0 4.16 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Lab 5 MB Lab 5 Spike Result Result 0 2.3252 0 2.5669 0 2.5902 0 2.9075 0 2.7958 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Lab 6 MB Lab 6 Spike Result Result 0 4.739 0 4.645 0 4.601 0 0 0 0 0 0 0 0 0 1 0 0 0 0 0 0 0 0 0.

### Page 23 of 24 N ELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = 2-Nitrophenol All results in ug/L

MDL Summary

Lab 4 Blanks Spikes No. of results 30 14 No. of numeric results 0 14 Spike Conc. NA 5 Mean 0 NA Std. Dev. 0 0.398486 Maximum 0 4.16 99th percentile NA NA t-statistic 2.46202136 2.650309

MDLb 

### NA MDLs 

### 1.056111355 Spike/MDLs 

### 4.734349247 OK Max. MDL 1.056111355 Data source for Max MDL spikes Lab 5 Blanks Spikes No. of results 30 16 No. of numeric results 0 16 Spike Conc. NA 3 Mean 0 NA Std. Dev. 0 0.237567 Maximum 0 2.9452 99th percentile NA NA t-statistic 2.46202136 2.60248

MDL b 

### NA MDLs 

### 0.61826255 Spike/MDLs 

### 4.852307489 OK Max. MDL 0.61826255 Data source for Max MDL spikes Lab 6 Blanks Spikes No. of results 32 14 No. of numeric results 0 14 Spike Conc. NA 5 Mean 0 NA Std. Dev. 0 0.688035 Maximum 0 5.003 99th percentile NA NA t-statistic 2.452824193 2.650309

MDL b 

### NA MDLs 

### 1.823506539 Spike/MDLs 

### 2.741969876 OK Max. MDL 1.823506539 Data source for Max MDL spikes

NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = 2-Nitrophenol All results in ug/L

MDL Data

Lab 4 MB Lab 4 Spike

Result Result 0 3.01 0 3.07 0 3.02 0 3.04 0 4.16 0 3.54 0 3.67 0 2.8 0 3.26 0 3.45 0 3.23 Lab 5 MB Lab 5 Spike Result Result 0 2.1296 0 2.1702 0 2.2667 0 2.0943 0 2.0304 0 2.3275 0 2.3552 0 2.1765 0 2.2279 0 2.0016 0 2.1995 Lab 6 MB Result Lab 6 Spike Result 0 3.059 0 3.881 0 3.529 0 4.495 0 4.578 0 4.163 0 4.786 0 3.121 0 2.97 0 4.077 0 4.946

### Page 24 of 24 NELAC MDL Calculations from Post-FACDQ Pilot Study Dataset Analyte = 2-Nitrophenol All results in ug/L

MDL Data

Lab 4 MB Lab 4 Spike

Result Result 0 3.31 0 3.75 0 3.97 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Lab 5 MB Lab 5 Spike Result Result 0 2.262 0 2.4377 0 2.5325 0 2.9452 0 2.5661 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Lab 6 MB Lab 6 Spike Result Result 0 4.355 0 3.951 0 5.003 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0