|
bi ,i +W
<br />,I~i
<br />,` ~1 .D 4374
<br />of the
<br />order to
<br />bypassed
<br />~tauly to
<br />l is news
<br />rtuination
<br />'d for the
<br />;omplexes
<br />itioD. The
<br />Toying the
<br />min with
<br />JV quartz
<br />with 5 %
<br />td 10 min
<br />appears to
<br />eves.
<br />mtomated
<br />urer man-
<br />on, pump
<br />.,
<br />h concen-
<br />iination as
<br />to recorder
<br />efollowing
<br />be system:
<br />;id, 5 % by
<br />S Of gases
<br />t the flow
<br />iOIULOn Of
<br />carbonate,
<br />rample and
<br />is -, .
<br />filling, 'and
<br />ndrmal by
<br />dfected by
<br />P..
<br />,.~
<br />valuate the
<br />triable fcya-
<br />the 17dited
<br />1}1sts: Foul
<br />1G!i Z°t
<br />SF~irinli
<br />ttt~:ap•to6z.
<br />:F!+ ?se~
<br />~~aide levels:were•chostn.between;zero;and 200-µg(L..~ :•~. t•
<br />Qlper thane reagent ,distilled- water,•,1litferent :field: sample;.
<br />matrices were used, that i@;,oatura{lgrougd:fwellrveter, lake, to
<br />~"water, mw sewage, prechlorinated, and chlorinated treated
<br />~
<br />
<br />effluents. , ~ 1 ~ i ' p WTlllx 9T
<br />tx /
<br />%~ 15.1.1 Precision-The overall and single operator preci- ~ se
<br />lion, Sr and So of the acid dissociable cyanides and total ~ to sT
<br />cyanides show that the standard deviation increases .with ~.r .~~
<br />so
<br />cyanide concentration, and somewhat higher in field samples a
<br />than distilled water, as presented in Figs. 4 and 5,.; .;, rr ~' ~ , ; ..
<br />15.1.2 Bias-Recoveries ofknown amounts of dissociable ~ s
<br />cyanides and total cyanides from reagent water and selected ~;
<br />field water matrixes are presented in Tables 1 and 2.
<br />- 15.1.2.1 Cyanide recoveries from .reagent. watersamples -
<br />yielded good values, witliin3 %. Recoveries
<br />of.totaf cyanides,
<br />.. ~ :.
<br />E
<br />_
<br />, .,
<br />from field samples were within 5, %.,.Only„recoveries -of.; ,. ,
<br />dissociable cyanides from field samples showed losses up to -
<br />°o so too tso xoo zso
<br />8 %. Greater losses were observed in other studies and could - -
<br />be due t0 riratrixes containing COmplexing 3gent5 .makrng - - CY•NIDE CONCE NTe•TIOM, MRrI
<br />sometCyanides not avvlable for such ineasuremetit._ _ rAtae:
<br />a, ~ ,- 50, •g, Sr ~ overall standartl tlevmtion,
<br />16. Quality Assurance/Quality Control (QAJQC~ s, ~ single-operator standard deviation,
<br />16
<br />1 Before these test methods area had to the anal sis
<br />pp Y water =reagent distilled water, and
<br />tl fi
<br />r m
<br />ri
<br />l
<br />t
<br />ltl
<br />t
<br />ln
<br />M
<br />. wa
<br />xes.
<br />x = 5e
<br />eo
<br />a
<br />at
<br />e
<br />e
<br />e
<br />of samples of unknown cyanide and tlilocyanate concentra=
<br />
<br />lions, the analyst must establish quality control by the - F(G. 5 Precision .N Total Cyanides
<br />procedures given in I'raMici: D 4210 and Guide D 385ti.
<br />16.2 A duplicate sample and known standard must be
<br />.z
<br />TABLE 1 Recoveries of Acid Dissociable Cyanides
<br />analyzed each day
<br />that an analysis is _pedormed_ The
<br />_
<br />_
<br />duplicate and standard shall meet the limits as established by
<br />Amount Average Statistical Signifi-
<br />cence (95% Cory
<br />the COnlf01 chart before a determination is considered Adtletl, Fountl, Sias, %
<br />fitlence level)
<br />satisfactory, pgn p9/L
<br />t -rest
<br />16.3 A blank and a spiked.sample shall be analyzed each t.o 1.02 z.o No
<br />day that an analysis is performed. Spiking shall be in 30 30.3 1.0 No
<br />accordance with that outlined in 11.11 of Gttide D 3856. 41 az.3 3.1 vas
<br />1o3 los.a z.a res
<br />The blank shall be low enough that it will not unduly Selectetl Fiala water Matnxes
<br />influence the data.
<br /> l.o 0.6 -e.o No
<br /> 30 27.7 -7.7 Yes
<br />~ ,`.
<br />r ~
<br />~x i
<br />,. F
<br />r
<br />e
<br />e
<br />-- s
<br />,! o
<br />F
<br />..~ ~
<br />~n
<br />~'.
<br />~K
<br />aT
<br />90
<br />R ST
<br />E so
<br />41 39.1 -4.6 Yes
<br />' t03 101.7 -t,3 No
<br /> TABLE 2 Recoveries. of Total Cyanides
<br />Amount Average Staasucal Signi6-
<br />Atltletl, Found, Elias, % mince (95% Confi-
<br />49/L p9/L dente levee
<br /> t -Test
<br />21 21.5 2.5 Yes
<br />30 30.5 1.6 No
<br />81 81.5 0.6 No
<br />171 171.1 0.1 No
<br /> Seleotetl Field Writer Matnxes
<br />21 20.1 -4.1 Yes
<br />30 26.6 -4.2 Yes
<br />81 76.5 -5.4 Yes
<br />171 173.3 1.4 No
<br />.,,~~,
<br />cr•RtpE eoftcEara.rloa, wn 16.4 One sample must be analyzed in duplicate with each
<br />' group of ten or fewer samples. The results must meet the
<br />$r~orerau sttuWard aeviatian, ~ limiu established in Section IS of these test methods before
<br />~So ~ slrgb-operaWr staMard deviatbn,
<br />water = reegent d1s611etl wafer, end the data for that batch or set of ten samples are acceptable.
<br />.° selected rleld water mebixes. 16.5 Other QA/QC portions of these test methods have
<br />i_, .- FlG. 4 Preolslon of Dlssociabb ganmea - not been completely established at this time. Analysts
<br />
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