NH4 Determintation Method

8/17/2019 NH4 Determintation Method

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II. AUTOMATIC ANALYTICAL METHODS FOR ENVIRONMENTAL MONITORING AND CONTROLLaboratory exercises

I. ANALYTICAL TECHNIQUES FORENVIRONMENTAL MONITORING AND

CONTROL

Laboratory Exercises

1


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I.1. SPECTROPHOTOMETRIC DETERMINATION OF

AMMONIUM BY THE INDOPHENOL BLUE METHOD

This method is appi!a"e to the dete#mi$atio$ o% the ammo$i&m !o$te$t i$'ate#s (e.). p#e!ipitatio$* 'ithi$ the #a$)e +.+, to -.+ m) NH,L.

Principle

I$ a$ a/ai$e so&tio$ (pH 1+.,011.* ammo$i&m io$s #ea!t 'ith h2po!ho#iteto %o#m mo$o!ho#ami$e. I$ the p#ese$!e o% phe$o a$d a$ e3!ess o% h2po!ho#ite4 themo$o!ho#ami$e 'i %o#m a "&e !ooed !ompo&$d4 i$dophe$o4 'he$

$it#op#&sside is &sed as !ata2st. The !o$!e$t#atio$ o% ammo$i&m is dete#mi$edspe!t#ophotomet#i!a2 at 56+ m$.

Reagent an! Intr"#entati$n

A the !hemi!as m&st "e o% #e!o)$i7ed a$a2ti!a )#ade . The 'ate# &sed %o# di&tio$ a$d #i$si$) sho&d "e do&"e0distied o# de0io$i7ed a$d distied.• 8he$o (C5HOH*• Sodi&m $it#op#&sside (Na-Fe(NO* (CN* 9 -H-O*• Sodi&m h2d#o3ide (NaOH*

• Sodi&m h2po!ho#ite so&tio$ (NaOC* 1M: ma/e a so&tio$ !o$tai$i$) app#o3.6.; a!ti


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'ith 'ate# to the ma#/. This sta$da#d ammo$i&m so&tio$4 a$d the ammo$i&mso&tio$s made %o# p#epa#i$) the !ai"#atio$ !


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I% the sampe is t"id4 "oth the sampe a$d the "a$/ sho&d "e %ite#ed th#o&)h a'hite "a$d %ite#.

,


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I.(. DETERMINATION OF CHLORIDE IN )ATERS

The method !a$ "e &sed %o# di#e!t dete#mi$atio$ o% the !ho#ide io$ !o$te$t i$'ate# sampes 'ithi$ the #a$)e +.+ to m)L.

Principle

Cho#ide io$s 'i s&"stit&te the thio!2a$ate io$s i$ &$disso!iated me#!thio!2a$ate. The #eeased thio!2a$ate io$s #ea!t 'ith %e##i! io$s %o#mi$) a da#/ #edi#o$0thio!2a$ate !ompe3.

The a"so#"a$!e is meased at ,5+ $m.

- C0 ? H)(SCN*- H)C- ? -SCN0SCN0 ? Fe6? Fe(SCN*-?


Di$) the a$a2sis4 &se o$2 !hemi!as o% #e!o)$i7ed a$a2ti!a )#ade a$do$2 do&"e0distied o# deio$i7ed a$d distied 'ate#.• 8e#!ho#i! a!id (HCO,* -; • Me#! (II* thio!2a$ate (H)(SCN*-*• I#o$ (III* $it#ate $o$ah2d#ate (Fe(NO6*6 9 H-O*

• Sodi&m !ho#ide (NaC*• Etha$o (C-HOH*• 8e#!ho#i! a!id4 1:1. Mi3 1


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-. T#a$s%e# - mL o% the !ai"#atio$ so&tio$s to 1++ mL E#e$me2e# %as/s. To ea!h%as/ add 'ith pipettes mL me#! (II* thio!2a$ate so&tio$ a$d - mL i#o$ (III*$it#ate so&tio$. Mi3 'e "et'ee$ a$d a%te# the additio$s. A%te# -+ mi$&tes4mease the a"so#"a$!e i$ + mm !es at ,5+ $m. As #e%e#e$!e4 &se - mL 'ate# mi3ed 'e 'ith mL o% #ea)e$t (-* a$d - mL o% #ea)e$t (6*.8ot the #eadi$)s a)ai$st the !o$!e$t#atio$s a$d d#a' the !ai"#atio$ !


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I.,. DETERMINATION OF THE SO( CONCENTRATION IN AIR

Intr$!"cti$n

A se#io&s e!oo)i!a p#o"em is the atmosphe#i! po&tio$ "2 s&ph dio3ide'hi!h o#i)i$s a#e d&e to the !om"&stio$ o% s&ph !ompo&$d !om"&stio$ i$ e$)i$eso# "oie#s. The so' %i)ht a)ai$st this po&tio$ sta#ted #e!e$t2 i$ %a!t e)a #&es a#e


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Glassware Reagents

Sampi$) set(ma$&a !o$t#o statio$*Spe!t#ophotomete# Gass !e4 1+ mm i)ht path

Bate# &ait2 Mii0KH-O- HCO, -;H-SO, >;=a(CO,*- a$h2d#e1 mi!#opipet4 -+ µL

1+


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5* So&tio$ o% =a(CO,*- dio3a$e. Di&ted 1 mL o% the so&tio$ (=a(CO ,*-* 'ith,+ mL o% 'ate# mii0K a$d t#a$s%e# i$to a


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,* De


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I.. DETERMINATION OF SULPHATE IN )ATERS

This method is appi!a"e to the dete#mi$atio$ o% s&phate i$ 'ate#s 'ithi$ the#a$)e +.+ m) SL to , m) SL. Sampes !o$tai$i$) hi)he# !o$!e$t#atio$s m&st "edi&ted p#io# to the a$a2sis.

Principle

=a(CO,*- is added i$ e3!ess to p#e!ipitate the s&phate as "a#i&m s&phate i$a$ o#)a$i! so


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• Opti!a )ass spe!t#ophotomete# !es -+ mm• Mi!#o pipette: -+ L• =&" pipettes: 14 -4 64 ,4 4 54 4 >4 a$d 1+ mL•

=ette: + mL• Io$ e3!ha$)e !o&m$s: 1 !m e$)th4 1 !m diamete#• Test t&"es: 6+ mL• Vo&met#i! %as/s: +4 1++ a$d 1+++ mL

A )ass'a#e sho&d "e o% "o#osii!ate a$d sho&d "e tho#o&)h2 #i$sed i$distied 'ate# "e%o#e &se.

Cali%rati$n C"r+e

8#epa#e a se#ies o% sta$da#d so&tio$s !o$tai$i$) +4 +.4 1.+4 1. ..... , m) SL "2 di&ti$) +4 14 -4 64 ..... > mL o% the s&phate sta$da#d so&tio$ to 1++ mL 'ith 'ate#

i$


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1. 8e#sso$4 G.A. (155* A&tomati! !oo#imet#i! dete#mi$atio$ o% o' !o$!e$t#atio$so% s&phate %o# measi$) s&ph dio3ide i$ am"ie$t ai#. Air Water Pollut., 10, >,0>-.

16


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I./. DETERMINATION OF ATMOSPHERIC LEAD 0II

Intr$!"cti$n

The ead is a #ee


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A) Reagents

The )ass'a#e sho&d "e p#e metai! s&ppo#ts> metai! !i#!es>4 -+ mL )ass %&$$es1 pipettes mL-4 mL pipettesFite# pape#> !o$i!a %as/s

test t&"es (>*> t&"es 'ith !o#/ o% spi#a o% 1+ mLSpe!t#ophotomete# (VISI=LE*

B) Solutions to be prepared

1* m) L01 8"(II* so&tio$. The sta$da#d so&tio$ is p#epa#ed "2 addi$) -. mL %#omthe sto!/ so&tio$ !o$tai$i$) 1+++ m) L 01 a$d e


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i$to a po2eth2e$e "otte p#e


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As #epo#ted %o# the sampe so&tio$s4 the mi3te is sha/e$


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I.2. SEPARATION BY E3TRACTION AND

SPECTROPHOTOMETRIC DETERMINATION OF MERCURYFROM )ASTE )ATERS

Principle

The method p#oposed %o# the sepa#atio$ a$d dete#mi$atio$ o% me#! is "ased o$ the see!ti


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0 Sta$da#d so&tio$ o% me#! !ho#ide 'ith the !o$!e$t#atio$ o% + µ) H)(II*mLi$ distied 'ate#

0 So&tio$ o% Cadio$ A (,0$it#ophe$2 dia7oami$oa7o"e$7e$e* +.+1 ; i$ metha$o0 So&tio$ o% sodi&m a!etate +.- M0 So&tio$ o% sodi&m a$d potassi&m ta#t#ate -+ ; i$ distied 'ate#0 C2i$de#s o# test t&"es 'ith the


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p#e!ipitate %#om the #ea!tio$ media. S&"se&e$t2 the 'o#/i$) p#o!ede %o# the!ai"#atio$ !


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I.5. DETERMINATION OF LEAD BY ATOMIC ABSORPTION

SPECTROMETRY )ITH ELECTROTHERMALATOMI6ATION 0ET7AAS

Maria 7 Critina BRATU

Intr$!"cti$n

The metai! ead a$d its !ompo&$ds a#e to3i! the2 !a$ e$te# the o#)a$ism "2i$)estio$4 i$hai$)4 o# a"so#ptio$ th#o&)h the s/i$ (the a!&te ead poiso$i$) is #a#e d&eto the poo# a"so#ptio$*. The !o$ti$&o&s assimiatio$ o% sma &a$tities o% ead is "2%a# the most da$)e#o&s. I$itia24 the ead is 'ea/2 "o$ded to the e#2th#o!2tes a$do$2 a sma pa#t is eimi$ated th#o&)h the i$e4 most o% it "ei$) a!!&m&ated i$ the

"o$es.F#om a the o#)a$i! !ompo&$ds o% ead4 the t#ia/2 !ompo&$ds ha


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I$ this 'o#/ is p#ese$ted a p#o!ede %o# the dete#mi$atio$ o% ead %#om the ai# o% a 'o#/pa!e e3posed to this !hemi!a po&ta$t4 "2 the method o% atomi! a"so#ptio$spe!t#omet#2 'ith ee!t#othe#ma atomi7atio$.

Reagent an! Apparat"

0 Nit#i! a!id 5 ; S&p#ap ( Al!rich"4 ammo$i&m dih2d#o)e$ phosphate( #erc$ *4 distied 'ate# (!o$d&!ti


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The )#aphite t&"e is mai$tai$ed i$ positio$ i$ the %$a!e "2 t'o )#aphite!o$ta!ts that e$se the ee!t#i!a !o$ta!t %o# the heati$) o% the t&"e. The )#aphite t&"eis ma$&%a!ted %#om p2#o2ti! )#aphite a$d p#ese$ts a$ i$te)#ated pat%o#m L> positio$s4 i$ 'hi!h a#e pa!ed

the po2p#op2e$e


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T*e Te#perat"re Pr$gra# $' t*e 9rap*ite F"rnace- L o% "a$/sta$da#dsampe a#e i$t#od&!ed i$ the atomi7atio$ &$it a$d the

tempe#ate is i$!#eased )#ad&a2 to #emo


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disso!iatio$ o% the 5 o% the a&tosampe#* as a mat#i3 modi%ie#.

Fo# the )e$e#ati$) o% the !ai"#atio$ !


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"&""e Gii"#ato# -4 %o# ea!h sampe #e!o#di$) the e3a!t


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I.>. DETERMINATION OF MERCURY BY COLD ?APOUR

ATOMIC ABSORPTION SPECTROMETRY

Maria 7 Critina BRATU

Intr$!"cti$n

The to3i! metas a#e $ot "iode)#ada"e4 ha


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0 S$C- ; i$ HC 1+ ; .0 8otassi&m pe#ma$)a$ate so&tio$ 5;.0 H2d#o32ami$e h2d#o!ho#ide so&tio$ -+ ;.0 Sta$da#d so&tio$ o% me#! o% !o$!e$t#atio$ 1+++ m)L ( Al!rich*.0 Sta$da#d so&tio$ o% me#! o% !o$!e$t#atio$ 1+ m)L 0 p#epa#ed "2 di&tio$ o%

++ L o% sta$da#d so&tio$ o% me#! o% !o$!e$t#atio$ 1+++ m)L 'ith + mL o% a"so#"e$t so&tio$ %o# me#!


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The me#! sta$da#ds o% !o$!e$t#atio$s -4 4 1+ )L a#e p#epa#ed #i)ht "e%o#e the measeme$ts4 "2 i$t#od&!i$) i$ the #ea!tio$


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the %o' o% - mLmi$* a$d the i$e ("* to'a#ds the imme#sio$ t&"e. The )as %#om theimme#sio$ t&"e a$d the !o$i!a shape o% the #ea!tio$


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1+++XX

X*( ..6

t 2

c. mm( c sol a's 1( = (6*

'he#e D %o' #ate (Lmi$* t time (mi$*Th&s4 to dete#mi$e the !o$!e$t#atio$ o% me#! %#om the !oe!ted ai#

sampes is ta/e$ i$to !o$side#atio$ the !o$!e$t#atio$ o% me#! o"tai$ed %#om the!ai"#atio$ !


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sta"ii7atio$ o% the me#!*. The me#! sta$da#d 'ith the !o$!e$t#atio$ o% 1++)L is o"tai$ed "2 i$t#od&!i$) i$ a$ E#e$me2e# %as/ 'ith p&)4 o% ++ L me#!sta$da#d 'ith the !o$!e$t#atio$ o% 1+ m)L a$d mL !o$!e$t#ated H -SO,4 %oo'i$)the same mi$e#ai7atio$ p#o!ede as %o# the %ish sampes. Bith a the #ea)e$ts addedi$ the mi$e#ai7atio$ p#o!ess4 the ++ L o% me#! sta$da#d 'ith the !o$!e$t#atio$o% 1+ m)L 'i "e di&ted 'ith + mL o% #ea)e$t mi3te4 o"tai$i$) the me#!sta$da#d 'ith the !o$!e$t#atio$ o% 1++ )L.

Fo# )e$e#ati$) the !ai"#atio$ !


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!


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I.. DETERMINATION OF pH IN PRECIPITATION.

POTENTIOMETRIC METHOD

Principle

The method is "ased o$ the dete#mi$atio$ o% the pote$tia di%%e#e$!e "et'ee$a$ ee!t#ode pai# !o$sisti$) o% a )ass ee!t#ode se$siti


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Ho'e


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Anal&tical Pr$ce!"re

Mease the pH0


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I.1@. DETECTION OF PESTICIDE USIN9 PRUSSIAN BLUE7

SCREEN PRINTED BIOSENSORS

Intr$!"cti$n

This a"o#ato#2 e3e#!ise p#ese$ts a $e' method "ased o$ Pr"ian Bl"e#$!i'ie! creen7printe! electr$!e %o# s!#ee$i$) o% o#)a$ophospho#o&s a$d!a#"amate pesti!ides i$ 'ate#.

8esti!ides a#e amo$) the most impo#ta$t e$


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o3idase (ChO* the h2d#o27ed !hoi$e is o3idi7ed "2 ChO a$d the ee!t#oa!ti


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4lectro!es preparation S!#ee$0p#i$ted ee!t#odes &sed i$ this e3pe#ime$ta 'o#/ a#e home0made 'ith

a -, DE (Be2mo&th4 E$)a$d* s!#ee$0p#i$ti$) ma!hi$e. G#aphite0"ased i$/ (Ee!t#oda) ,-1* %o#m A!heso$ Itaia$a (Mia$4 Ita2* 'as &sed to p#i$t the 'o#/i$)ee!t#ode. The s&"st#ate is a %e3i"e po2este# %im (A&tostat HT* o"tai$ed %#omA&tot2pe Itaia (Mia$4 Ita2*. The ee!t#odes a#e p#od&!ed i$ %ois o% -+. The diamete# o% the 'o#/i$) ee!t#ode is +.6 !m #es&ti$) i$ a$ appa#e$t )eomet#i! a#ea o% +.+!m-4 the !o&$te# i$ )#aphite0"ased i$/ a$d the #e%e#e$!e i$ si


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,* A%te# that4 the "iose$so# is 'ashed 'ith "&%%e#4 a$d the -$d step is #epeateda$d the #esid&a e$72mati! a!ti


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Re'erence

1. FAO4 A)#i!&te to'a#ds -+1+4 i$: C 6, Do!&me$t o% - th Sessio$ o% the FAOCo$%e#e$!e4 Rome4 16.

-. Stan!ar! metho!s &or eamination o& 6ater an! 6aste6ater -+th ed. Ame#i!a$

8&"i! Heath Asso!iatio$ Bashi$)to$41> pp 5>05+.6. Lis/a I. So"od$i/ . J.Cromato(r.A 124 3774 -60->.,. 8#ei$i$)e# C. Bo%"eis O.S. Biosens. Bioelectron. 124 114 >10+.. =a)i#o.1-. Ema$4 G.L. Cot$e2 .D. A$d#es V Feathe#sto$e R.M. =io!hem. 8ha#ma!o.

1214 3 4 >>0.16. Ri!!i4 F. A#d&i$i4 F. Ami$e4 A. Mos!o$e4 D. 8aes!hi4 G. J. 4lectroanal. Chem.

(@@4 564 --0-6.1,. Ri!!i4 F. Ami$e4 A. T&ta C. Ci&!& A.4 L&!a#ei F. 8aes!hi. Anal. Chim. Acta

(@@,4 9854 11101-+.

,1


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I.11. DETERMINATION OF STRON9 AND )EA ACIDS IN

PRECIPITATION. COULOMETRIC TITRATION METHOD

Intr$!"cti$n

This method is appi!a"e to dete#mi$atio$ o% st#o$) a!ids i$ p#e!ipitatio$sampes 'ithi$ the !o$!e$t#atio$ #a$)e 1+0 to 1+06 M. The o'e# !o$!e$t#atio$ imitis !ose to the !o$!e$t#atio$s at "a!/)#o&$d sites 'itho&t a/ai$e mi$e#a d&st.

Principle

I$ the !o&omet#i! tit#atio$ method (Li"e#ti et a.4 1-*4 the a!id is tit#ated at

!o$sta$t !#e$t 'ith h2d#o32 io$s i"e#ated at a pati$&m ee!t#ode4 a si


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0 A ,. V d#2 "atte#2 'ith a$ ad&sta"e se#ies #esista$!e a$d a mA mete# iss&%%i!ie$t %o# measeme$ts4 "&t !o&omete#s a#e a


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G#a$s %&$!tio$

E#? & E#? & E#? & E#? &

1 1.+, ,1 ,.6 >1 -6., 1-1 111

- 1.+> ,- .16 >- -,., 1-- 11

6 1.1, ,6 .66 >6 -.6 1-6 1-+

, 1.1 ,, . >, -5.6 1-, 1-

1.-- , . > -., 1- 16+

5 1.-5 ,5 .> >5 ->., 1-5 16

1.61 , 5.-- > -.5 1- 1,+

> 1.65 ,> 5., >> 6+. 1-> 1,5

1.,- , 5. > 6-.+ 1- 1-

1+ 1.,> + .++ + 66.6 16+ 1>

11 1., 1 .-> 1 6,.5 161 15,

1- 1.5+ - . - 65.+ 16- 11

16 1.55 6 .> 6 6., 166 1

1, 1.6 , >.1 , 6>.> 16, 1>

1 1.>+ >.1 ,+., 16 1-

15 1.+ 5 >.> 5 ,-.+ 165 1

1 1., .-+ ,6.5 16 -+

1> -.+- > . > ,.6 16> -15

1 -.1+ ., ,.- 16 --,-+ -.1> 5+ 1+.6 1++ ,.1 1,+ -66

-1 -.-5 51 1+. 1+1 1.+ 1,1 -,-

-- -.65 5- 11.1 1+- 6.1 1,- --

-6 -., 56 11.5 1+6 .- 1,6 -5-

-, -., 5, 1-.1 1+, ., 1,, --

- -.5 5 1-. 1+ . 1, ->6

,,


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E#? & E#? & E#? & E#? &

-5 -. 55 16.+ 1+5 51. 1,5 -,

- -.>5 5 16. 1+ 5,., 1, 6+5-> -. 5> 1,.1 1+> 5.+ 1,> 61>

- 6.+ 5 1,.5 1+ 5. 1, 661

6+ 6.-1 + 1.- 11+ -., 1+ 6,,

61 6.6, 1 1.> 111 .6 11 61

6- 6.,> - 15. 11- >.6 1- 61

6, 6.51 , 1.1 116 >1. 16 6>5

6, 6. , 1.> 11, >,. 1, ,+-

6 6.+ 1>. 11 >>.1 1 ,1>

65 ,.+5 5 1.6 115 1.5 15 ,6,

6 ,.-6 -+.+ 11 .1 1 ,-

6> ,.6 > -+.> 11> >. 1> ,+

6 ,.5 -1. 11 1+6 1 ,>

,+ ,., >+ --. 1-+ 1+5 15+ +

E4prei$n $' Re"lt

The !o$!e$t#atio$ o% st#o$) a!id i$ the sampe is !a!&ated %#om the %o#m&a:

o#

'he#ei ee!t#o2sis !#e$t i$ ampe#este ee!t#o2sis time at e&i


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F Fa#ada2s !o$sta$t (!o&om"smo*Vo i$itia sampe


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,


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I.1(. DETERMINATION OF BEN6ENE TOLUENE AND 3ILENE IN

AIR BY 9ASS CHROMATO9RAFY

Intr$!"cti$n

The a#omati! h2d#o!a#"o$s ha


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Reagent an! Apparat"

Glassware and apparatus Reagents

Sampi$) set 8e$ta$eAdso#"e$t !a#t#id)es Sta$da#ds %o# GC:Gas !h#omato)#aph =e$7e$e (sta$da#d*Capia#2 !o&m$ $o$ poa# To&e$e (sta$da#d*Dete!to# FID _2e$e (sta$da#d*So%t'a#e %o# data p#o!essA$a2ti!a "aa$!e1 mL t&"es p#o


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Co&m$: H8 t2pe phe$2meth2sii!o$e (6+m 3 +.6- mm 3 +.- m*Gas !a##ie# : Hei&m4 %o'0#ate 1. mL mi$01

I$e!to# tempe#ate -6+ WCDete!to# tempe#ate -+ WC8#o)#ammed Co&m$ tempe#ate: Isothe#m at 6 @C di$) mi$.F#om 6 @C to 1,+ @C at 1 @C mi$01

Isothe#m at 1,+ @C - mi$Fi$a tempe#ate: 6 @C

.1.* Ide$ti%i!atio$ o% "e$7e$e4 to&e$e a$d 32e$e. A s&ita"e so&tio$ o% "e$7e$e a$d the$ o% to&e$e a#e i$e!ted to assi)$ the #ete$tio$ times'hi!h ao' ide$ti%2 s&!h !ompo&$ds eithe# i$ the !ai"#atio$ )#aph a$dsampes..-.* Sta$da#d i$e!tio$s. The di%%e#e$t sta$da#d so&tio$s o% "e$7e$e4

to&e$e a$d 32e$e a#e i$e!ted i$ the same !o$ditio$s o"tai$i$) the!o##espo$di$) !h#omato)#ams a$d !o##e!t i$te)#atio$ o% the a#eas o% the pea/s %#om these !ompo&$ds..6.* Sampe I$e!tio$. 1 L o% the e3t#a!t is aso i$e!ted i$ the same!o$ditio$s o"tai$i$) the !o##espo$di$) !h#omato)#am a$d the i$te)#atio$a#eas o% the "e$7e$e4 to&e$e a$d 32e$e pea/s 'hi!h 'i "e ide$ti%ied "2its #ete$tio$ time.

Re"lt

1* Ide$ti%2 the #ete$tio$ times (tR * %o# the th#ee !ompo&$ds.-* Ca!&ate the !o$!e$t#atio$ i$ ) L01 o% "e$7e$e4 to&e$e a$d 32e$e&si$) a dots i$ the !ai"#atio$ )#aph.

A 0t$c8 $l"ti$n )rite

Vo&me o% "e$7e$e (L* ++m) o% 'ei)hed "e$7e$e) L 01 o% "e$7e$eVo&me o% to&e$e ++m) o% 'ei)hed to&e$e

) L01 de to&e$eVo&me$ de 32e$e ++m) o% 32e$e (e3a!t 'ei)ht*) L01 o% 32e$e

Stan!ar! n 1 ( , /

Vo&me o% = so&tio$ (i$ mL*) L 01 o% "e$7e$e) L 01 o% to&e$e

+


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) L01 o% 32e$e

Write in the ta'les the area o& the pea$s in the cali'ration (raph

=e$7e$e µ)L`#ea

To&e$e µ)L`#ea

_2e$e µ)L`#ea

6* D#a' the !ai"#atio$ i$es. Rep#ese$t the a#eas o"tai$ed i$ the!h#omato)#ams vs. the !o$!e$t#atio$


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-


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I. 1,. DETERMINATION OF THE ?OLATILE OR9ANIC

COMPOUNDS FROM THE ATMOSPHERE USIN9 APORTABLE 9AS CHROMATO9RAPH

Maria7Critina BRATU

Intr$!"cti$n

The mo$ito#i$) o% the L a$d

6++ psi (=TE_ Gas Mi3*4 !o$sisti$) o% si3 a$a2tes 'ith the !o$!e$t#atio$ i$$it#o)e$ o% 1+ ppm ea!h4 as %oo's: "e$7e$e4 eth2 "e$7e$e4 to&e$e4 m032e$e4o032e$e4 p032e$e.

The dete#mi$atio$s o%


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i$te#$a !2i$de# o% the !h#omato)#aph e$ses its a&to$om2 %o# hos4 di$) thistime o$ site )as !h#omato)#aphi! measeme$ts !a$ "e do$e.

A%te# the !ha#)i$) 'ith !a##ie# )as4 the !h#omato)#aph is sta#ted "2 p&shi$)the O$O%% "&tto$4 "ei$) #e&i#ed a$ i$te#


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The &aitati


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o# the dea!ti


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I.1. SEPARATION AND DETERMINATION OF

TRIHALOMETHANES FROM )ATERS BY9ASCHROMATO9RAPHY

Intr$!"cti$n

The t#ihaometha$es (CHC64 CHC-=#4 CHC=# -4 CH=# 6* a#e %o#med i$ 'ate# di$) the !ho#i$atio$ p#o!ess. Se


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Fo# the p#epa#atio$ o% 1+ ) o% %ii$) the %oo'i$) p#o!ede is empo2ed:0 1 ) s&aa$ is disso


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Met*$! '$r t*e Preparing $' t*e Sa#ple an! Stan!ar!

a* The method %o# the p#epa#i$) o% the sta$da#ds is:0 I$ a


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The pea/s a#eas a#e app#e!iated %#om the !h#omato)#am o% the #e%e#e$!esampe. The %oo'i$)


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I.1/. DETERMINATION OF THE PHENOLIC COMPOUNDS IN

)ATER BY HI9H PERFORMANCE LI-UIDCHROMATO9RAPHY

Maria7Critina BRATU

Intr$!"cti$n

The phe$o a$d s&"stit&ted phe$os #ep#ese$t !ommo$ "20p#od&!ts i$ ma$2i$d&st#ia p#o!esses. At !o$!e$t#atio$s o% the o#de# o% pp"4 i$ e$+015+ m the po#ediamete#s a#e: 11+01 *.

0 Sta$da#d o% phe$os: E8A 5+,0M 8he$os Mi3 %Supelco" %o#med %#om a mi3te p#epa#ed i$ metha$o o% 11 a$a2tes4 at di%%e#e$t !o$!e$t#atio$s: phe$o (++)mL* ,0$it#ophe$o (-++ )mL* -4,0di$it#ophe$o (1++ )mL* -0!ho#ophe$o (++ )mL* -0$it#ophe$o (++ )mL* -4,0dimeth2phe$o (++)mL* ,450di$it#o0o0!#eso (-++ )mL* -4,0di!ho#ophe$o (++ )mL* ,0!ho#o0m0!#eso (-++ )mL* -4,450t#i!ho#ophe$o (1++ )mL*

pe$ta!ho#ophe$o (-++ )mL*.0 Sta$da#d o% phe$os: E8A 5+,0S 8he$os Mi3 %Supelco" %o#med %#om 11

i$di


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metha$o4 'ith the 6 mm a$d thediamete# ,.5 mm.

56


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A$ e&tio$ 'ith i$ea# )#adie$t o% the mo"ie phase 'i "e &sed: %#om 6 ;a!eto$it#ie'ate# (pH-.-* &p to 1++ ; a!eto$it#ie4 o


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/a$ing the calibration curve

The !ai"#atio$ !


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Ta%le B. Amo&$ts o% phe$os e3p#essed i$ ) %#om sta$da#d so&tio$s p#epa#ed %o# the!ai"#atio$ )#aph (i$e!ted


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metha$oa!eti! a!id 1;4 most phe$oi! !ompo&$ds !a$ "e easi2 dete#mi$ed at!o$!e$t#atio$s "eo' the


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1+ L o% a sampe o# sta$da#d so&tio$ is sepa#ated "2 &si$) a &ate#$a#2mi3te o% metha$o'ate#a!eto$it#ietet#ah2d#o%a$. The %oo'i$) ta"e sho's the)#adie$t p#o%ie 'hi!h is &sed.

K&ate#$a#2 )#adie$t 'hi!h sepa#ates the !a#"o$2h2d#a7o$es o% i$te#est (EME8* at a%o' #ate o% +.> mLmi$.

Ti#e G Tetra*&!r$'"ran G Acet$nitrile G )ater G Met*an$l

+.+ 1>.+ --.+ 5+.+ +.+

+. 1>.+ --.+ 5+.+ +.+

-+.+ >., 6., ,.- +.+

-,.+ +.+ +.+ 6,.+ 55.+

,+.+ +.+ +.+ 1.+ >.+

,1.+ +.+ +.+ 1.+ >.+

,.+ +.+ 1++.+ +.+ +.+

,>.+ 1>.+ --.+ 5+.+ +.+

The dete!tio$ a$d &a$ti%i!atio$ is !a##ied o&t at 65 $m ("a$d 'idth -- $m*&si$) ,, $m ("a$d 'idth + $m* as the #e%e#e$!e 'a


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-. A


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6. D2e4 C. a$d Oehme4 M. (1-*. Comme$ts !o$!e#$i$) the H8LC sepa#atio$ o% a!#oei$ %#om othe# C6 !a#"o$2 !ompo&$ds as -4,0di$it#ophe$2h2d#a7o$es:a p#oposa %o# imp#o.

+


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the sampe !o$tai$e# 'ith 'ate# %#om a #ep#ese$tati


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Optimisatio$ o% the a$ti"od2 !o$!e$t#atio$.

,. The #esid&a so&tio$ is #emo


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The t#a!e# is added to the optimised !o$!e$t#atio$ so that the %i$a

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NH4 Determintation Method

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