|
rB nC4[aaM.umxx maM]I 16l4Mal YMIyr S03 www.[«/omab9/epaR^IInPbm xxw.rMOmab9/WaNImM.rom Wrlaar ID131(4[MgM 1Y1PoU MW[]I MINnPl a9
<br /> Results and Dlssusedon
<br /> Laboratory N:Table IV sunnmariaes the
<br /> instrument calibration and method pc,- alle,ll.,X Laboratory Y Lub.'aw,z
<br /> furnerval dam for laboratory X This lab- WWx Matrix Spike Relatbe Matrix Matrix Spike Relative Matrix Matrix Spike Relative
<br /> oratory's method and instrumentation Spike Nobe Sebe Dupliov Penal Spike Native Spike Duplicate Percent Spike Native Spike Optical Percent
<br /> achieved a man relative rerponse fetor of Target Anipe Concentration CommnVon Reavery pe) Recovery l%) Difference ps) Concentration Concentration Recovery l%) Recovery,l%I Difference(%1 Concentration Concentration Recovery(N) Recovery(%1 Diiferen[el%)
<br /> approximatdy 0.8 for MTBE, and the Sample 014
<br /> man relative rnpone factors for the ether MTBE 20 IA 93 0 0 25 0.91 102 los 3.0 10 1.0 be SEA 8.3
<br /> oxygenated target anilyea ranged from tart-Butyl alahol 150 NO 129 125 3 125 ND 104 100 0 W NO 83.2 114 309
<br /> 0.021 ro 0.038. These values Compare 2-Propanol 100 ND 101 93 8 250 ND 117 132 12 0 NO 110 113 27
<br /> P Anepia I% ND .77 72 0 25 ND 564 5" 2.8 0 NO 1% '16 29
<br /> fvombly, with the minimum relative j
<br /> tesponrc factor requirement of 0.01 speci- 919 53
<br /> fied for many,oxygenated compounds in the G 103 12.5
<br /> EPA Conrmtt fakesper ryPlogmm Statement 159 1.3
<br /> ar'WoeF for purge-and-tarp GC-MS s raly- 0' 118 >
<br /> sis(no minimum relative response foo: Simple 6Wy
<br /> requirements are established by EPA MTBE 12M 3010 69 0 11 20.000 2500 101 117 13.2 19,000 2200 74.1 74.3 02
<br /> Method 826118)(1.7).The rdauvermndard teTButyl akohd 3000 NO 112 113 1 25,000 ND 98.1 106 7.1 5$000 70 66.6 23.8
<br /> deviations(RSD,) for the mean relative DProparol 2000 NO 85 Be 1 50.000 NO "A 118 16.8 6000 ND 75 ,93• 21
<br /> response furors were well within he °IeM 3000 1D 77 n 7 SOW ND 48 54A 125 8000 p, ND 145 ''.24 15.6
<br /> Method 82608 limit of 15%for linar
<br /> responu(Table M,end the percent differ- 5 0 106 114 5 8
<br /> 0 01 61
<br /> anon vilua For daily calibration relative NO
<br /> ,;;,)W 116, .. 11:
<br /> response factors relative m the initial conn .. NO „ y
<br /> refuse response factors were 25%.11-
<br /> The
<br /> r lett I et8.3
<br /> The method performance atteined by 'RalI15 NNde real pm9ram income,aro Weaken oiMP(75-125%rKOKly ern 25%Ill
<br /> laboratory X in the demooxtrationsiteram- raratiseperant dieeeWel are is odd.
<br /> pies generally met program goals for ser i-
<br /> tiviry,accuracy,and precision.Laboratory
<br /> practical quaneiation limits and a8bration Table IT:Low spike recovery results
<br /> curvy extended below the program-
<br /> required thrahalds(ret Table M.As ma-
<br /> suredbyRSDsRedrelativeper¢ntdiffa- 11.. Spike Native Low Spikel tow Spikel Low Splke3 Spike Native Low Spikes Lpw Sp0e2 Low Splke3 Spun, Native Law Spikel Lov5pae2 Low Splke3
<br /> encu, the rripiiate analyse and matrix Sample 401-1 Concennabour Concentration Recovery l%) Recovery(%) Gerrit,(%) Cementm0on Concentrators Recovery l%) Recovny(%) RB[paeay(%) C.....runs. (a[edLouisa Rewvelyi�o) Recovery(%) Reraveryl%)
<br /> rpik<maerix spike duplicates were well MTBE 1 1.4 90 100 100 2 1 83.5 95 100 1 1.1 130 90 140
<br /> within the program precision limit of25%. ten Buiyl alcohol 10 ND 110 112 111 8 ND 59.5 637 65.2 5 NO 100 100 100
<br /> Although some matrix spikemavix spike 2 Propenoi 5 ND 110 136 130 80 NO 77.5 89.1 94.4 8 NO 625 112.5 75.0
<br /> du lint[sett l.pike recovaiu were out- '.Acetone 7.5 ND 93 04 100 8 NO 48.6 61.5 5L5 8 NO 125 ND 100
<br /> P P •!MTBE-1, 109 111 109 106 934 118
<br /> side the project accuracy goals of75-125%. •,!.cwt Butyl alcohol dlo 114 116 114
<br /> 92.5 BC 07
<br /> theseexreeirnceswereinvarisiWalighr.the ,. , q .
<br /> lowar reported recovery was 62%(MTBE) Gorki
<br /> Resws shat , _. 1 .:" '. '" '.•• ,°°tar ,,.,, a,::: ry ..
<br /> - I ... ,.,,: ......
<br /> and the highest mcovery esu 136% (2- 'r°M0`" Ali
<br /> propanol). Furthermore, recoveries of
<br /> MTBE-d3 and eewburyl alcohol-dlo•spiked
<br /> as oxygenated surrogates item the prop. Icy,which resulted in genre,precision and for this compound under nentrd pH condi- higher alum for accurate and MTBE.RSD and low spikes,ranging from 45 to 61% format¢criteria were not emecdedi
<br /> coney samples and msvix spikes,all were lower opportunity for analyte loss. bone and a half-life of G hat pH 2(8), values for the man relative response fecaors (sen Tabic 11).We also observed slightly,low mess spectral confirmation of target analyte
<br /> within the program accuracy criteria(sec Although not required to do so by the Because of the short apparent half-life of were less than the Method 82608 criterion recover9a for cart-butyl alcohol in the low derectiom again was comidercd acceptable
<br /> Tables I end 111).The[urger snslyte dirl scope of the method proficiency study,Lab tart-butyl formate and uncertainties in of 15%,with the perception of exempt.for spikes performed on sample 4014.ranging relative to the guiddinea in Method 82608.
<br /> fiction also was acceptable for the reported oratory X provided method performance proper prelervuion technique and holding which the laboratory reported an RSD of from 60 to 65%(see Table 111).We found As war observed for laboratory X,the mien.
<br /> dermumM,u well az the low-concenuation dam for sertburyl formates another deg«- dma fee this compound,we,had excluded 21%.A ample daily calibration provided no basis for the low raoveries of ecttane tion times of 2-propanol and aawrse were
<br /> spikes at the target practical quantitation dnion product of MTBE.Low recoveries of rare-butyl formate as a target arulyte for the by the laboratory reported percent differ- and umburyl alcohol during the raw data approximaely 0.1 min apart,and a Form-
<br /> limits,because it was consistent with the rers-buryl formas(9-30%)observed for tratmrnt technology demorutntions. cote wluer ofless than 15%farall four tar- reviews,which also noted consistently low tial forimerferencewas noredbecween these
<br /> rtvM spectral confirmation criteria outlined some matrix spiko-mavix spike dupficater Laboratory Y Table IV summaries the get arulyres. recoveries for aeeeane in the laboratory con. two compounds.
<br /> in Method 82608. and low,spikes could be searched to acid instrument calibration and method Geller. The method performance atminrd by trot sample(45-504b). Laboratory Z Table IV summuiaa the
<br /> In addition,we noted that the Varian hydrolysis of ova-buryl formate in the profi- mance dam for Iabotuory Y.The laboratory laboratory Y in the demonstration site sum- Although Laboratory Y'x method did not instrument calibration and method perf xr-
<br /> Archon-EST surompropler provided a dear dcncy Study samples,which were prererved attained mon relative response rectors of pin generally met progrun goals for MTBE include the use of oxygenated surrogates, mance dam for labamtory,Z.Low relative
<br /> .damage in the handling and subsequent with hydrochloric add.The laboratory also 0.023 end 0.013 for tert-buryl alcohol and and cert-butyl alcohol;however,quantim- the laboratory used tert-butyl alcohoi-d9 ar, man mi Live response factors of O.ODS and
<br /> purging of samples.The primary diBvenu suspected degradation of temburyl formate 2-propanol,respectively,which were grater elan limits and low-spike levels for 2- an internal standard.Reviews of raw dam 0.006 were reported for cart-bury)alcohol
<br /> esu the ability of this ....sampler to in some calibration standards and spiking than the EPA Canal Laboratory Program propanol wen,above the program goals,rand enabled .,her method quality control and 2-propanol,respectively.The daily ali-
<br /> process the ample with minimal sample solutions.A Study of the hydrolysis of tart- minimum aloe of 0.01 for awl-butyl all acetone meaveries were consistently,low in checks-instrument tuning and method bmtion check performance was monitored
<br /> handling and a high degree of rcpmducibil- butyl Forman reports half-life of five days hall and 2-propanol.laboratory Y obtained the matrix spike n atria spike duplicates blanks-which indicated that method per- in Grant of percent recovery rather than per-
<br />
|