adsorption studies of some pesticides on fly ash
TRANSCRIPT
ADSORPTION STUDIES OF SOME PESTICIDES ON FLY ASH
DISSERTATION SUBMITTED IN PARTIAL FULFILMENT OF THE REQUIREMENTS
FOR THE AWARD OF THE DEGREE OF
MASTER OF PHILOSOPHY IN
CHEMISTRY
BY
TAHIRA BEGUM
DEPARTMENT OF CHEMISTRY ALIGARH MUSLIM UNIVERSITY
ALIGARH (INDIA) 1988
29 m' \n%
mm DS1275
2)r . at. O . (Ralherm
OBABBB
Chemistry Section, Zakir Husain College of
Engg. & Technology, Aligarh Muslim University ALIGARH-202001 INDIA
Dated .?«>yBMOBR...^l988
DBCLABATIOM
I cer t i fy tbat the i«ork presented la t h i s dlBsertatloii
has been carried out by Miss Tahira Begum and that i t i s
suitable for submission towards partial fulfilment of the
requirements for the award of the degree of Master of
Philosophy in Chemistry of the Aligarh Muslim University,
Aligarh,
/ H.S.Rathore /
ACKWOHLBPGEMBNT
I • x p r e s a my d«ep ind«bt«dii«»« t o Or. i i«S.Ratl ior«,
S««der, 0«i»«rt««nt of Appllod Clioalttry, Z.R. Collego of
BnglnoArinc and Toehaology, Alifarii Maoll« UolTorsity, Aligarli
for b i s «M« gttldaaee throughout the prograaa of th is work
and for oontlnued intaraat during the proparation of th i t
•anttforif»t.
My slttoi>r« thanka ara dua to Prof. K.T.Naooon,
Chalman and Prof. A.U.Mat Ik, fonaur Chaiman, Da|>art«AQt of
Apfil&ad Choaiatry for providing aaeaaaary raaaaroh f a o l l l t l e a
during thl« Inveatlgatlon.
My profound thanka ara du« to Dr. Iahtla4| A l l , Header
Tkepartamnt of Applied Chenlatry, S.H.College of Snglneerlng
and Teehnology, Allgaili lhaellai Unlyaralty, Allgarh for hie
dedleated 9ar« and eonoem of my ifork.
I Miet be thankful to ay oolleaguea* Dr. S.B.Sharaui,
Or. S. Gupta, Mr. R.A.Khan, Mr. S.K.Saxena and Mr. Anoop Itoaar
for the ir Yaluable help and ao-operatloa froa t l ae to t l a e .
Speolal BentIon Huat be aade of ay reapeeted parents
for providing mm oonstant enoourageaient and aoral support at
every stage of my work.
/ TABIRA BBGUM /
C O N T E N T S
PAGE
LIST UF ABBREVIATIONS ( l )
LIST OF TABLS5 ( i i )
LIST OF PUBLICATIONS ( i l l )
ABSTRACT ( I T )
CHAPTBR - I
INTRODUCTION 1
REFERENCES k
CHAPTER . I I
CHROMATOGRAPHIC BEHAVIOUR OF 30I« AGRO CONPOUNRS
ON LRAClffiD n.Y ASH
INTROnUCTION 8
EXPERIMENTAL 9
RESULTS 13
DISCUSSION 29
RSrSRENCXS 27
LIST or ABBHBYIATIOKS
CPX A-Chlorophenoxyaoetlo aoid
2,4-T> 2,4«1)iohloropbeiiox/ao0tlc acW
QA Gallio acid
lAA Iiidole-3*ati«ti<3 aold
XFA lndole>3-*lpropionic acid
MPA ^ -Naphthaleneaoetic aoid
MPX jB-NapbihO3tyaO0ti4S a o i d
OA Oxalic acid
VEX Phanoxyaoatie aoid
TCA Trlohlonciacatie aoid
2,*,5-T 2,<i,5-^ricliilarophaaoxyao«tlo acid
Fl Ply ath laached with aoatio aoid
f2 Fly ash laaohad with l^anzeue
F5 f ly a«ii l«»«obed with d i t t i l l e d watar
F4 f ly a ah laaohad with ethanol
F5 Fly aah l«acli«!l with sulphario acid/ hydrochloric acid
F6 Fly aah lynched with aodliin carbonate/ aodlttoi hydrozida
T>w Diat l l led water
( i )
hist OF TABLES
PAOE
TABL8 I
TABLC I I
TA&B I I I
TAO^g lY
TABLB Y
TABLB YI
TABLE YII
TAHiB YIII
TABLB IX
B^ YALinSS OP SOME HBBBICIDBS ON fLY ASH
LBAC»iBD VITH ACSTIC ACID IN DIPPBRBNT
SOLYENTS. 1%
B YALUBS OP mm HSBBICIDBS ON PLY ASM
LBACRBD WITH BBNZENB IN DIPPB86NT
SOLVENTS, 15
B^ YALtms OP SONS RBBBICIDBS ON VLT ASH
LBAGRB1) VITH DISTILLED VATBB IN DIFPRRRNT
SOLYBNTS. 16
K YALUBS OP 90m HBBBICIDBS ON PLY ASH
LBACHED WITH BTHANOL IN DIPFBBENT
SOLVENTS. 17
Bf VALUBS OF SOW BBBBICIIKS ON PLT ASH
LBAOHBB WITH SULPHURIC ACIO/BTDBOCHLORIC
ACID IN DIPFSBBNT SOLVENTS. IS
B VALUES OP SOME mEBBlClOBS ON FLY ASH
LBAOIED WITH SODIUM CABBONATB/SODIUM
HTDBOXIDB. I9
SEPARATIONS ACHIEVED ON LEACHED PLY ASH. 20
BINARY QUANTITATIVE SEPARATIONS OP lAA
P«OM 6A ON PLY ASH LBACRBD VITH SULP»JRIC
ACIT> IN CBLOBOPORM. 22
BINARY QUANTITATIVE SEPARATIONS OP lAA
PROM OA ON FLY ASH LEAGUED VITH SULPHURIC
ACID IN CRLOROPORN. 2^
( It )
LIST or Final*ICATI0W8
1. "ChroMitofrafhio Baharionr of Soa« Afro Coapottads on
liMobed Fly Ash*, R,3.Batbor«, I«All and T.B«gu»,
Pre««at«d at National Syapoalna on Analytioal Applleationa
la Karth sel«>ne«a hold fron 15*^7 Nov, 1988 at North-
Eaatem Hill Oalvoralty, Sbllloag.
( 111 )
ABSTBACT
Thin-layer ehroaa tog rafale bahaviour of ao««
oailioxyllc herliioldca tuob B» 4««hloroi»heiioxyaeetio aeld,
2»4Hliolilorofib««oxyao«tio aold, trloliloreaeetio aold,
2,4,5*trioh1orofiheiioxfae#tio aold and filant grovth refulatora
naaaly ga l l l o aold, lndole-5-aeetlo aold, lndol«-3-proi»loiilo
aold, ^ Hiai^tlialttii«acetle aold, ^ naaphthoxyaoetlo acid and
I»haao3tyac^tlo a d d haa b^en attidlad on laaobod f ly aah. Th«
f ly aah waa leachad vltb baaxane, d i s t i l l ad watar, atbanol,
afliuaotta aolutloaa of aoatlo aold (O.lN), hydroohlorlo aold
(O.lN), aalphurlo aold (O.IH), aodlna earbonat« (O.lN) and
aodla* hydroxide (O.lN). Banzane, oarbon tatraohlorida,
ohlorofom, d lat l l lad watar, athyt aoatata and aqaoona aolntloa
of aodlnw ohlorlda (i%) vara uaad aa davalopera. Many
aapenitlona Inoludlng Indola-'3*M«tle MSld (Tjug) froa gal l lo
(340-680 fig) and ozallo (252*90% jog) soldo on f ly aah laaohad
with aulphnrlo aold (O.lN) were aohloYod In ohlorofom.
( iv )
inmommion
IlffBOIHICTlON
Fly ash i s oae of th« solid indttstrial wast« iprodueed
in hufe quantity at th«rwil fK>w«r s tat ions . It i s a ooa|il«x
•ixtura of various so l ids , saai-sol ids and gaseous phases of
hundreds of inorfanies and ovianios. The presence of aore
than thirty eleaents was detected in f ly ash vith the help of
theraial and eiptherauil neutroa-aotiTation analysis (1 and 2) .
Many inorganics such as quarts, aluvina, s i l i c a , coes i te and
unbumt carbon, sereral autagenio nitro-organic ooapounds (3) ,
polyeyct ie aroMitio hydrocartions (4,5)t ond dibeasofuran and
dibenso-p-dioxin Mixtures (6) were also detected in fly ash.
Therefore f ly ash i s a source Material of winy substances as
well as i t i s a source of environaental pollution (7) .
Rfforta haTe been Made to use f ly ash for the
preparation of eenent (8) , oeraaic t i l e s (9) , concrete (10),
fabric f i l t e r s ( H ) , f e r t i l i z e r s (12) and therwil insulating
Materials (I3) . Possible uses of f ly ash for flue gas
treatvent (14), l ining of acid so i l s (15)» the strengthening
of s o i l s (16), the reaoval of a ir f e l t (17), ifaate water
treatMent (18), land f i l l (I9) , the recovery of vanadiuM (20),
slag sludge hardening (2i ) and for the Manufacture of
ferroTanadinn al loys (22) have been suggested.
The f ly ash obtained froH theraal power station
Katlapur, I n d i a , ooosi t ta iiradoainantly of <|oartK with
atuaina, a i l i o a , ooaalte and nnbumt oarbon (23) along with
•ar loua inorfaniea and organlea tMntlonad alioTe. I t can b(>
naad fo r th<i oo«|>l«t« raawvat of toxio mat at tono aveh as
A « ( m ) ( 2 * , 2 5 , 7 ) , H t ( I l ) ( 2 6 ) . JSn(Il) (27) and C r ( I l ) (28,29)
and organloa auoh aa v l e t o r l a bln« ( 3 0 ) , earboxylie aoids (3^) ,
phanol and oraaol and t h a i r aixtttraa (32) and e o l i f o m baoteria
f ro« aquaoua aolnt lona, Ad«iztttraa of f l y aah and ohlna olay
(FC) can b« uaad for tha raamval of C n ( I l ) froM aqnaoua
aoltttlona ( 3 3 ) . F ly aab lapratnatod wi th bydroxidaa of A t ,
Cd, Cu, F« and Nl ean ba naad for tba raaoral o f e innaalo,
lndo la -3 -ao«t lo , /B HBiapbtbalanaaeatie, ^-nanhtboxyaoatle,
oxal io and t r ieb loroaoat le aeida f ro« a^naona oolntiona (23 ) .
Tba adaorotlon on f l y aah waa found to ba dapandant of t i a a
of oontaot. I n i t i a l aa l t eoneantmtlon and fB o f tha aolnt ion
( 2 4 , 3 2 , 3 ^ ) . Adaorntlon on f l y aah l a a ehoaiaoration doninatinc
aiaohaniaai ( 2 3 ) .
Leaching of f l y aah (35) with varioua raaganta by
diffar<>nt prooaduraa waa parforaad for atudying i t a a t a b i l i t y ,
ehaaioal ooaipoaition, and adaorptioB-daaorption eharae ta r ia t iea .
Fbr axa«pla, raleaaa of Aa (and aavaral othar alananta) f rov
f l y aah into watar l a r g a l y dapanda on tha i iaantity and oontaot
pariod of tha aolrent uaad, pB, tha ohaaieal fora of tha
• lavant and tha phyaiooohaaiieal proport iaa of tha watar (24 ,25 ) .
S«v<»rat trp«* o ' n.y ash ir«r« l«Ach«d vith talphurlo aoid and
th« so lo l i l l l ty behaTlour of wijor ash oo«poa«iita was axaaiiiiad
(36).
LlakowltK «t a l . (37) reported that leaotaiiiK of f ly
ash with water gawe a soxt»eBt with oa^aclty to absorb irarious
«l««#nts in aaounts in aveeas of that or ig inal ly laaohad.
llttss «t a l . (38) reported that the aiitieons solubillzed
f ly ash leaohate obtained by treating f ly ash with aqueous
base, washing with water and then treating with hydroohlorlo
acid was useful as a ooagulant/floeoalent for the treatnent
of water or waste water and for the oondltioaing of sludge to
reduce i t s resletaaoe to dewatering leaohates generated froa
selected fly ash were evaluated in of^er to provide the data
base needed to develop an envlroaaentally safe disposal
•anageaent strategy (39).
In view of the above poiata i t was decided to study
the ohroaatographie behaviour of f ly ash leached with
different reagents, fhe results obtained are presented in
th i s dissertat ion.
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C H A P T K R « I I
CHROMATOCBAPHIC BBHATIOUR OF 80MB
AGSO OONPOtmns ON LEACSBD FtY ASH
iifraoppcTioy
In oontlauatloB to oar pr«¥lou« work now ohromto-
trairtiie %«h«Tiottr of Itaehod f l y aoh for CI*X, 2,4-11, GA, IAA*
IFA, NPA, IfPX, OA, mx, T<U and 2,4,9-T has 1>«ott oxaaiaad
itt boBBoiit, earbon tatraolilorido, oMorofom, WK, othyl
aeatata and aodiuB ehlorido. Ply aata loaohad v l tb aoatio
aeld, lioasana, d la t l l lod iiator, othanol, attl^nrlo aeld,
liydroolilorlo aold, sodlua eai^onata and aodlna hydrozida
vaa naad aa a eoating aatarial on glaaa plataa for
okromi tog raphy •
The raaalta oUtainad ar« dlaeasaod in thia ohapter.
.1
A Stahl amiarattts with a aniTersal appl ioator
(adjuatatole thieimaas of tha apii l iad l ayer from (0 ,25-2 .00 H I ) ,
hot a i r c l eo t r i c d r i e r , glasa plataa (20 % h om), f l a a a Jara
(25x5 OB}f taaperature eontro l lad e laot r io oven, e leot r io
oentrifttge wiohine, aa inet ie a t i r r e r , Bauaoh and Loab
S9eotroiiie-20 aod ASTN ataadard t e a t aievea ware uaad.
Ghewioal a
AO(>tone ( n ) B , I n d i a ) , %enseae (3 .N .0he« io» la , Ind ia } ,
oaloiua attlphate prec ip i ta ted powder, oailion te t raoh lor ide ,
ohlorofora, e tbyl aoetate, propanol (B .Nerok, Ind ia ) , liroao-
phenol b lue , %-ohlorophenoxyaoetio ae id , 2,4-dicbloroptoenoxr>
aoetio ae id , g a l l i c ac id , indole-7Hicet ic ac id , indole -3*
propionic a c i d , A -oapbtbaleneaoetie ac id , JB-napbthoxjracetic
a c i d , pbenoxraoetic ac id , t r ieb loroacet io ac id , 2 ,4 i ,5* tr iehlero-
phenoxracetie aeid (9igm,1ISA), oxal ic acid (B•Merck,India)
and f l y aab (100-200 Meah) from Ittaaian Plant of TberMl Power
S ta t ion , Kaaiapur, Ind ia , U«P, were need. A l l other reagenta
need were o f ana ly t ica l grade.
Preparation of Solntioaa
Solutiona (2^) of 4-ehloroi^eaoxyaoetic, 2 ,4«diehloro-
<)
f»h«noxyaeetle, g a l l i e , inilot«-3-«o«tie, ittdol»-3*'pro|»ioiii«,
^ «iiafihthal4»neae«ile, p-nai^tboxyacatie, pbanoxyaeatle aod
2,4,5-trl«bloroiili«iioxya««tl« aelds and 0.1^ l>roa»fAanot blue
ware prepared in atbanol. Solutions of oxatlo aeid (2^) and
triobloroaoctio aeid (5^) were prepared in d i s t i l l e d water.
For speotropbotovetrie deteraination of indole~3*-aoetic aeid,
freshly prepared reagent obtained by aixing 1 lil 0.5M ferrlo
ohloride in 50 al of 39^ ( • / • } pereblorio aeid was used.
Leaohing of Fly Ash
A portion of f ly ash (40 g) and 100 ml of a leaohing
reagent were tAk«n in a breaker of 250 ail eapaeity and the
systew was kept with oeoasional shaking at rooM teaperature
(30 C) for 2k hr. The leaohing reagent was reaowed by
deoantation, the f ly ash so obtained was washed seyeral t iaes
with fW in order to reaove trsoes of the reagent, dried at
rooa teap<»rnture and then the f ly aah was ready for ohronato-
graphio studies . The f ly ash saaples were leached with acetic
acid (O.lN), benseene, DV, ethanol, hydrooUlorio «oid (O.lN) or
sulpburic aeid (O.iH) anrl tsodium oarbonate (O.lN) or aodlua
hydroxide (O.IH).
Preparation of Plates
A slurry obtained by aixing f ly ash (40 g ) , ealoiua
li
sulphate (13.33 c ) with Hv (80 a l ) was ajpplied on the glass
platas with ths help of an applicator so that the thiokoess
of the ooatlnc was 0.3 mm. The plates were f i r s t allowed to
dry at room temperature and then in a teatperatvre oontrolled
eleetrio orpn at 110 C for 1 hr before use.
TIeteotion of Aelds
the aoids under study were looated on the plates by
0,i% ethanolle allcaline bromphenol blue solution.
Spotting of Teat Solutions
Test solutions were spotted on the plates with the
help of a fine capil lary and the solvent was renowed by hot
a ir drier. The plates vera developed in a solvent, dried and
then aoids were looated by spraylns broBM>phenol blue. The
distanoe ascended by the developer was lO oa. For t a l l i n c ,
the front l i « i t (KI) and the rear H a l t (RT) were seasured
while for other aoids R. values were taken as usual
S m distance travelled hy solute (o«) ' nistanee travelled by solvent front (on)
Qualitative Separations
To achieve qualitative separations of acids, one of
th(» acids wnn spotted and the solvent was renoved, then second
•ol(f was apett«d anA th« solv<"nt vaa roaovad afain. The
plates ^*frm then dereloiied, dried and aeids were located
aa abowe.
Quantitative Separatjona
A known voluae of standard aeld was spotted on the
plate with the help of a gradnated sloroplpette with iraettupet
controlt the solvent was remoTed, plates were developed and
the 8P0t» were looated as above. The denareated area of the
ooatinK was soratohad out, the aeld was e«traoted with ethanol
(5 Ml ) and the solid was reMOved by oentrlfucatlon. The
acid In thf* oentrlfugate was deteralned speotrophotonetrloally
by the following procedure.
In the extract (1 wl) contalninf; lAA, 2 wl of freshly
prepared reagent were rapidly added dropwlse with continuous
agitat ion. The sanple wns Incubated In dark for 1 br for
colonr development. Finally the absoiHanee was neasured at
510 nn agiainst a blank containing ethanol (1 fA ) and reagent
(2 Hi ) .
i •»
wsmuTs
1 . iralttes of oaTlK»xyllo li«i%leld«« and rcl«t«d
eoajjioniidfl on l««<sh«d f ly ••*> AV-e giirtn In Tallies I-YI and
Fls* 1. Soaa laportant aaparatlona ar« raeorded in Tablt* VII.
Th« raaults of iinantitatlva toparationa ara givan In Tables
VIII and IK, Tha analytioal paraamtars vara ealealatad by
the folloving axprasalons
N-1 . . . (1)
C.V. <^^x 100
( 2 )
«)iere
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N
a-C.V.
•aaanrad valttaa
aTaraga valaa
nnmbar of sets
standard davlatioa
re lat ive atandard deviation or
the eoeff ic ient of Tariatloa.
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Fl h f3 ^4 h h LEACHED FLY ASH
Fig. 1-Plots Of R vs leached fly ash in different solvents I Benzene 2 Carbon tetrachloride 3 Chloroform 4 Distilled water and 5 Sodium chloride ( aq ) ^ 1 Tailing I- A-I — - - o •
y a-
H 2 . 4 - D H TCA ^ 2 . 4 , S - ^
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6
_EACHED FLY ASH
mscussiow
Fig. 1 rii»ws that It Yiiluet of 2,4*4>, 2,%,5«>T and TCA
artt at Boat th« aaaa on dlffarant aaaplaa of leaohed f ly aiUi
In the aama aolvant. For «3taflipl« R. •alaaa of 2,4>^ la i.O
on leaehaa f ly aah aawfilea Fl, F2, F3t f^t ^5 ond F6 in
hansana. Sl«l tar ia tha hahaviour of othar harliieldaa and
ralatad eoapouBda on a l l tha aiz aaao^** of laaohad f ly aah
In tha aa«e aolTant (hanKanf" or oar%on tatraohlorld# or
ohlorofona or d ia t i l lad vatar or athyl aeatata or aquaoua
aodluH ohlorida). Hanoa It aaaaa that tha fkortlon of dlffarant
adaoiHanta mieh aa qaartx, aluwlna, a i l loa and ooaaita In tha
f ly aah laaohad with dlffarant raaganta i s naarly tha aaaa.
It ia alao olaar frov Fig. 1 aa trail aa Table I , that H. ralua
of a particular hartiieida on laaohad f ly aah la tha fnnotlon
of aolTant nsad aa a daralopar. For axavplay R valuaa of
2,*-T> are 1.0, 1,0, 1,0, 0,0, 1,0 and 0,0 on Fl in henxana,
enilion tetrsohlorlda, chlorofom, d i s t i l l e d water, ethyl
acetate and aqnaons sof llum chlorida raapeotively. The aa«a
la the trend of R values of 2,^,5-T on Fl In tha above
aolventa. Similar behaviour of the other hertiicidei and
ralatad oonpotinds vith minor devlationa has been obaarvad on
different aanplaa of laaohad f ly aah (Tables I-TI), Aa 2,%->Ti,
2,4,9-T, c m , MPA, NPX, lAA, IFA hava aaro R valuaa on al l
tha aai^»laa of laaohad f ly aah In d ia t i l lad vatar, f ly aah ean
Zii
%• tt»«d for the ir r««oiral froa wetcir. The reteation of tli«
alHiTe aentloQodi ti«r1ilolde8 ana related ooMfiOttiidt (R^ value O.O)
on f l y anh la veter saggests that the t o l l s amended vith
f ly ash ( l ln ln f } (1) will not allow their translooatloa.
Therefore, i t oan eheek the pollntlon dne to peatloidea plant
pToteetlon.
The datit recorded la Tattles I-VI show that aaajp
separations of the ooaponads aader stndy are possible oa
leached f ly ash. The separations vhleh have beea aohlered
are recorded In Table VII. A long l i s t of binary separatleas
(Table YII) shows the laportaaee of leaehed f l y ash as a
ohroaatographle smterial. Tables VIII and IX show that
f ly aah oan be need for the quantitative separation of plant
growth regulator, lAA (2) fro« another plant growth regulator,
OA and related eoaqioands OA,
At theraal power station Kaslapur (India) the fly ash
Is avallnble froa Gerawin, Japaaese and Rasslan plants . The
appearance, fineness and the ooaposltlon of the f ly ash
oolleeted froa the above three plants are different . The f ly
ash eollacted froa Susslan plant Is powdered aad contains a
very snail percentage of uaburat oavboa. Therefore i t was
selected for the above studies .
d>
•EFEitENCgS
1. To(!yaRlt«tcii ,r.N., Khla.Sel *sk, iOiox., 8, 33-36 (1983).
2 , Mahad«von,A, nnrl Slr«!har,R., M«tho<)s In phys lo lof ioa l
plant pathology, ifSivaicami pab l loa t lons , 3rfl Kd, 270
(1986) .