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ns Rev. 0 (3.9.15) Reporting water MDL is allowable) Preparatory Method Analysis Method The MDL programs and by covered The LOD reporting?

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Annually  M w  P  A  A MDL stud each qua determin NR 149.4 determin has revie continue this time determin The MDL o o If both M lab feels determin Many pa reported The LOD project p in order t Why doe programs determin monitorin an MDL stu Matrix (if the water MDL is Preparatory M Analysis Meth Analyte (whe Matri dies can be arter. Annua ation. 48 (2) (d) inc ned limit of d ewed a numb to explore d the logical c ation. L study pass LOD < sp LOD is no DL studies w the passing ative LOD (M rameters us to the LOD. D and LOQ s lans, where to meet thes es WI requir s. The cove ation of whe ng is require udy must be solid and aq s allowable) Method hod re an MDL s ix – Prep Me completed b ally, these qu cludes a pro etection by a ber of protoc different prot conclusion is ses if both th pike concent ot less than were conduc MDL is not MDL). sed in covere When repo should be be it is achieva se limits. re LOD/LOQ ered program ether or not a d is based o

Requir

performed f queous matr study is appr ethod – Ana by preparing uarterly repl vision for ve an establish cols and non tocols for ve s that the on he low and h ration, and 10% of spike cted properly realistic – p

R

ed programs rting results elow the regu able. In som Q reporting? ms use data an action lev on the samp

red freque

for each com rix methods a ropriate) alysis Meth g and analyz icate results erifying “the c ed and defe ne of them h rifying that a ly defensible

igh spike cri e concentrat y and the res protocol is pr

eporting

s under NR 1 to the LOD, ulatory limits me cases a m ? This requ to make env vel has been le results rel

ency

mbination of are identical hod – Analyt zing at least t s could then continued ap ensible proto has been dee

an establishe e approach

iteria are sat tion sultant MDL rovided on h 149 require t , the LOQ m s established more sensitiv uirement com vironmental n exceeded lative to the the following l, extrapolati te (or group two MDL stu be used for pplicability o ocol”. Howev emed to be “ ed LOD rem is to simply tisfied: L still does no ow to estab that sample must also be d by covered ve method m

mes from the impact asse or whether a LOD and LO

g:

ion from the

p)

udy replicate the LOD

of a previous ver, the prog “defensible” mains valid, b repeat the ot pass or th lish a realist results be reported. d programs a may be requi e covered essments. T additional OQ. es sly gram . We but at he tic, and ired The

(2)

o Begin o Befor CFR o Most analy o The b pass o The M be clo exam o If the appro o o o Perfo B. o o As pr o o n with establ re you attem Appendix B MDL study yzing the rep better you do the MDL stu MDL proced ose to the es mple, using 2 re is not a c oaches you 40 CFR A Use your sources, s orm the minim

Replicates time). This Running a determinat samples, n reviously dis LOD < sp LOD is no

M

lishing a val mpt the MDL MDL proce failures can plicates back o estimating udy the first ure requires stimated MD 2 - 3 times yo urrent MDL, can use to d Appendix B M knowledge such as the mum 7 (but s should be a s is critical to ll replicates tion. It advis not directly a scussed, the pike concent ot less than

MDL (LOD

id calibration study it is in dures for ho be attribute k to back in a the spike co time. s that a spike DL (the proce our current M or you susp determine a MDL proced on instrume instrument v we encoura analyzed ove o incorporate simultaneou able to anal after a blank MDL study ration, and 10% of spike

D) determ

n. n your best in ow to determ ed to spiking a single ana oncentration e concentrat edure refers MDL concen pect your MD good estima ures provide nt limitations vendor or an ge 8) replica er multiple d e day-to-day usly will freq

yze the repl . passes if it m e concentrat

mination

nterest to ta mine a good e at the wron alytical run. n the better y tion be used s to 1x – 5x y ntration woul DL is no long ated LOD: e instruction s, or the kno n authoritativ ate MDL stu days (run ~2 y variability i uently result icates distrib meets both tion ke the time t estimated LO g concentra your chance d in the MDL your current ld be a good ger valid, the on how to e owledge prov

ve reference dy in 40 CF 2 MDL spike

into the dete t in a failed M buted among of the follow to review the OD. tion and es are that yo L study that w LOD). For d idea.

ere are two estimate a M vided by oth e method. R Part, Appe samples ea ermination. MDL g routine wing criteria: e 40 ou will MDL. her endix ach

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Exam

PLE 1: A va ple 1, a valid e, this would

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If the initia the study Before yo the time t It is a very can be dis This is do Once you the signal an estima Then take the LOD,

mple 1: M

lid MDL det d LOD is obt d become yo

What do i d

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MDL (LOD)

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(4)

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(5)

An

If the lab o o o …then it This is us there are analysis. Step 1: D The first your dete One way nominal the nomi Another greater (t Step 2: R Answer t o H o A o H co Step 3: A Once cer one can concentr based on from blan Rememb LOQ. Yo signal tha Make su concentr Be sure t not lower Step 4: E The LOQ

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rmining a

st MDL study e of the LOD es to accoun a or results in h to establis sion instrume h as for ion c D is unreali t obtained u hat the nom d LCS prepa ere is no sig at the nomin onse found poor low en ve low level els and algo

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sely affected creasing con e instrumen that the resu ve).

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proved EPA etermined is ncentration e uantitative r ponse is not ethod blank rization of t ion? ot contributin e nominal L ination or ca , starting at t detect it at i onse can be between the h you can re ven better. igher than th at the determ

ative

LOD

ty and LOD d LOD. hose in which ow injection protocol, as not realistic equal to the result is belo significantly ks. the calibrat ng to blank LOD alibration iss the LOD its concentra e distinguish LOD and th eliably detec he nominal L minative LOD h s . ow y ion sues, ation hed e ct a LOD. D is

(6)

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(10)

Method condition LOD (Lim measure departme determin quantitat LOD is u to the pro Nom derive eithe accep Dete LOD an ap Meth meas zero water 136, LOQ (Lim quantitat requires statistics Lowest c standard LOQ for LOQ bein times the the low e N ca ca p R d blank = rea ns as the ass mit of detecti d, and repor ent purposes ed accordin ive recovery sed to set th ograms usin inal LOD = ed). It rema r a vetted 2n ptable to the rminative L obtained fro pproved alte hod Detectio sured and re as determin r. The metho Appendix B mit of quantit ive results c that there be define the L concentrati in the initial multi-analyte ng 10/3 of th e LOD. This end of the ca NOTE: Calib alibration mu alibration, w redominanc Reminder: determinatio gent water t sociated sam

ion) = the low rted with con s, the LOD a g to the prot y is not expe he LOQ and g that data. the LOD cal ains the Nom nd determinat e Departmen LOD = the ad om the initial rnate protoc on Limit (MD eported with ed from ana od detection . It is listed tation) = the can be obtain e a mathema LOQ as 10/3 on standar l calibration e methods. he LOD mea s situation sh alibration cur bration is arg ust be prope while also pro ce of “negativ the calibrat on MUST be

De

hat is proces mples – inclu west concen nfidence tha approximate tocol establis ected at the L for some pa lculated follo minal LOD un tion, or one nt. dopted LOD MDL study, col. DL) = the mi 99% confide alyses of a se limit is gene here becaus e lowest conc ned. A quan atical relatio 3 the LOD. d in the cal be near the Note howev ans that the l hould be avo rve (see Exa guably the m erly establish operly chara ve” blanks is tion levels a e the same a

efinitions

ssed simulta uding all pre ntration or am at the concen s the EPA’s shed in 40 C LOD. The s arameters de owing the ac ntil it has bee

determined

used for rep , the 2nd dete

inimum conc ence that the et of sample erated accor se most EPA centration or titative recov onship betwe ibration cur LOQ. “Nea ver that the c

low calibratio oided as muc ample 4). most critical p hed without o cterizing the s a primary in and calibrat as that used aneously wit paratory, cle mount of an ntration is no s MDL (meth CFR Part 13 study must b etermining a ccepted EPA en properly through som porting. The ermination, o centration of e stated con es containing rding to the A methods re r amount of very is expe een the LOD

rve = NR 14 ar” could be d combination on standard ch as possib part of determ over-extend e low end of ndicator of a tion algorith d for analys th and under eanup, and a alyte that ca ot a false po hod detection 6, Appendix e well done a true LOD is A protocol (s vetted or rep me alternativ adopted LO or the one d f an analyte ncentration is g the analyte protocol spe efer to the M an analyte f ected at the L D and the LO 49 requires t defined as 2 n of 5 times t could be as ble as it coul rmining an LO ding the uppe

the calibrati a poor calibr hm selected sis of samp r the same analysis step an be identifi sitive value. n limit) and i x B. A because the s very impor tatistically placed with ve protocol, OD may be th determined fr that can be s greater tha e in reagent ecified in 40 MDL. for which LOQ. NR 14 OQ. Traditio

that the lowe 2-5 times the the LOQ and s much as 17 ld lead to bia OD. The er limit of the ion. The ration. d for the LO ples and QC ps. ied, For s e rtant he rom an CFR 49 nal est e d the 7 as at e OD C.

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