Method 4500

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By Authority Of

THE UNITED STATES OF AMERICA

Legally Binding Dou!ent

By the Authority "e#ted By $art % of the United State# Code & %%'(a) and

$art * of the Code of Regulation# & %* the attahed dou!ent ha# +een duly

INCOR$ORATED B, REFERENCE and #hall +e on#idered legally

+inding u-on all iti.en# and re#ident# of the United State# of A!eria/

HEED THIS NOTICE 0 Cri!inal -enaltie# !ay a--ly for nono!-liane/

Dou!ent Na!e0 A$HA Method 1%223NO'0 Standard Method# for the

E4a!ination of 5ater and 5a#te6ater

CFR Setion(#)0 12 CFR *78/7(a)

Standard# Body0 A!erian $u+li Health A##oiation

Standard

For the

E4a!ination of

5ater and

5a#te6ater

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0 !!

I!!9!!!!9!!!9

$re-ared and -u+li#hed :ointly +y0

A!erian $u+li Health A##oiation

A!erian 5ater 5or;# A##oiation

5ater En A$HA> Chair!an

Lenore S/ ?e#eri> 5EF

Andre6 D/ Eaton> A55A

Managing Editor

Mary Ann H/ Fran#on

$u+liation O@e


*2*% Fifteenth Street> N5

5a#hington> DC '222%

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Co-yright **> *'2> *'7> and *'% +y


Co-yright *77> *78> and *18 +y



Co-yright *%%> *82> and *8% +y



5ater $ollution Control Federation

Co-yright ** +y




Co-yright *8 +y




Co-yright * G* +y




Co-yright *G% +y




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Co-yright *G +y




Co-yright *' +y

A ! erian $u+ lie Health A##oiation


5ater En In/> Hano Maryland

Set in0 Ti!e# Ro!an

$rinting0 "itor =ra-hi#> In/> Balti!ore> Maryland

Binding0 A!erian Trade Bindery> Balti!ore> Maryland

Co In/> Arlington> "irginia

NITRO=EN (NITRITE) (1%223NO ' )Colori!eth Method

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13G%

1%223NC" NITRO=EN (NITRITE)J

1%223NOo A/ Introdution

*/ Ourrene and SigniKane

For a di#u##ion of the he!ial harateri#ti#> #oure#>

eet# of nitrite nitrogen> #ee Setion 1%223N/

A--ro

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1%223NOo B/ Colori!etri Method

*/ =eneral Di#u##ion

a/ $rini-le0 Nitrite (NO>) i# deter!ined through for!ation

of a reddi#h -ur-le a.o dye -rodued at -H '/2 to '/% +y ou-ling

dia.oti.ed #ulfanila!ide 6ith "3(l3na-hthyl)3ethyIenedia!ine

dihydrohloride (NED dihydrohloride)/ The a--lia+le range

of the !ethod for #-etro-hoto!etri !ea#ure!ent# i# P to *222

f4g N2 ' 3NL/ $hoto!etri !ea#ure!ent# an +e !ade in the

range % to %2 4g NL if a % 3! light -ath and a green olor Klter

are u#ed/ The olor #y#te! o+ey# Beer# la6 u- to *G2 4g N L

6ith a *3! light -ath at %17 n!/ Higher N2 7 onentration#

an +e deter!ined +y diluting a #a!-le/

+/ Interferene#0 Che!ial ino!-ati+ility !a;e# it unli;ely

that N2 ' > tree hlorine> and nitrogen trihloride (NCU) 6ill

oe4i#t/ NC* 7 i!-art# a fal#e red olor 6hen olor reagent i#

added/ The follo6ing ion# interfere +eau#e of -rei-itation under

te#t ondition# and #hould +e a+#ent0 S+3 "l > Au 7 > Bi *i > Fe 7t >

$+ 7 Q > Hg ' Ag > hloro-latinate ($tCl 8 ' )> and !eta

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'/ A--aratu#

Colori!etri eui-!ent0 One of the follo6ing i# reuired0

a/ S-etro-hoto!eter> for u#e at %17 n!> -ro -ro

and either Ba(OH) ' or Ca(OM) ' / Redi#till in an all3+oro#iliate3

13G8

INOR=ANIC NONMETALS (1222)

gla## a--aratu# and di#ard the initial %2 !L of di#tillate/ Collet

the di#tillate fration that i# free of -er!anganate a red olor

6ith D$D reagent (Setion 1%223CI/F/'8) indiate# the -re#ene

of -er!anganate/

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') Add * !L one H ' S= 1 and 2/' !L MnS2 1 #olution (78/1

g MnS2 1 H ' 2l 22 !L di#tilled 6ater) to eah * L di#tilled 6ater>

and !a;e -in; 6ith * to 7 !L Mn21 #olution (122 !g Mn2 1

L di#tilled 6ater)/ Redi#till a# de#ri+ed in the -reeding -ara3

gra-h/

U#e nitrite3free 6ater in !a;ing all reagent# and dilution#/

+/ Color reagent0 To G22 !L 6ater add *22 !L G%V -ho#3

-hori aid and *2 g #ulfanila!ide/ After di##ol add * g A 3(l3na-hthyl)3ethylenedia!ine dihydro3

hloride/ Mi4 to di##ol then dilute to * L 6ith 6ater/ Solution

i# #ta+le for a+out a !onth 6hen #tored in a dar; +ottle in

refrigerator/

/ Sodiu! o4alate> 2/2'%M (2/2%N)0 Di##ol u#e a fre#h +ottle of reagent for -re-aring

the #to; #olution and ;ee- +ottle# tightly #to--ered again#t the

free ae## of air 6hen not in u#e/ To deter!ine NaN2 ' ontent>

add a ;no6n e4e## of #tandard 2/2%M (2/2%") P"lnO/> #olution

(#ee ** h +elo6)> di#harge -er!anganate olor 6ith a ;no6n

uantity of #tandard redutant #uh a# 2/2'%M Na ' C ' 1 or 2/2%M

Fe(NM 1 ) ' (S2 1 ) ' > and +a;3titrate 6ith #tandard -er!anganate

#olution/

*) $re-aration of #to; #olutionW Di##ol

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') Standardi.ation of #to; nitrite #olution W $i-et> in order>

%2/22 !L #tandard 2/2%M Mn2 1 > % !L one H ' S2 1 > and %2/22

!L #to; N2 ' #olution into a gla##3#to--ered Ya#; or +ottle/

Su+!erge -i-et ti- 6ell +elo6 #urfae of -er!anganate3aid

#olution 6hile adding #to; N2 ' #olution/ Sha;e gently and

6ar! to 2 to G2C on a hot -late/ Di#harge -er!anganate

olor +y adding #u@ient *23!L -ortion# of #tandard 2/2'%M

Na ' C ' 1 / Titrate e4e## Na ' C ' 1 6ith 2/2% Af MnO> to the faint

-in; end -oint/ Carry a 6ater +lan; through the entire -roedure

and !a;e the nee##ary orretion# in the Knal alulation a#

#ho6n in the euation +elo6/

If #tandard ()/Z)%M ferrou# a!!oniu! #ulfate #olution i# #u+3

#tituted for Na 7 C ' 2/:> o!it heating and e4tend reation -eriod

+et6een Mn2 1 and Fe [ 3 Q to % !in +efore !a;ing Knal Mn2 1

titration/

Calulate N2 ' 3N ontent of #to; #olution +y the follo6ing

euation0

(B 4 ? 3 (\] 4 \)^ 4

Eah * /22 !L 2/?%M Mn2 1 on#u!ed +y the NaNO> #olution

orre#-ond# to *%2 (4g NO> 3N/

/ Inter!ediate nitrite #olution0 Calulate the => of

#to; N2 ' #olution reuired for the inter!ediate N2 ' #olution

fro! = 3 *'/%L Dilute the

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h/ Standard -ota##iu! -er!anganate titrant> 2/2%M Di##ol X 3 c g) ? 9 9

6here0

A 3 !L titrant tor #a!-le and

B X !L titrant for +lan;/

A

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#olid#> Klter through a 2/1%3:UL!3-ore3dia! !e!+rane Klter/

+/ Color de

ad:u#t to that range 6ith IN HC* or NH 1 OH a# reuired/ To

%2/2 !L #a!-le> or to a -ortion diluted to %2/2 !L> add ' !L

olor reagent and !i4/

/ $hoto!etri !ea#ure!ent0 Bet6een *2 !in and ' h after

adding olor reagent to #a!-le# and #tandard#> !ea#ure a+#or+3

ane at %17 n!/ A# a guide u#e the follo6ing light -ath# for the

indiated N(b 3 3N onentration#0

Light $ath Length

!

NO 0 3N

4gL

*

%

/*2

'3'%

'38

'

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6here

A

B

nig N2 ' 3N!L in #to; NaN2 ' #olution>

total !L #tandard Mn2 1 u#ed>

C 3 nor!ality of #tandard Mn2 1 >

D 3 total !L #tandard redutant added>

E X nor!ality of #tandard redutant> and

F X !L #to; NaNO> #olution ta;en for titration/

%/ Calulation

$re-are a #tandard ur 2/%%> and */21 !g NO_ > N2 ' 3NL> the

#tandard de 2/221> 2/22%> and

2/2*> re#-eti the reo *2'V> and *22V> re#-eti

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13G

/ Referene

*/ U/S/ En D/C/

G/ Bi+liogra-hy

n3

Bolt.> D/F/> ed/ *%G/ Colori!etri Deter!ination of Non!etal#/

ter#iene $u+li#her#> Ne6 ,or;> N/,/

Nydahl> F/ *8/ On the o-ti!u! ondition# for the redution of nitrate

+y ad!iu!/ Talanta '7071/

1%223NO ' _ C/ Ion Chro!atogra-hi Method

See Setion 1**2/

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Method 4500