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A n a l y t i c a l Chemis Cry Method No, 71-17 Job No. 1348006
DETERMINATION OF AROCLORS AND RELATED PRODUCTS IN MIXED LIQUOR SAMPLES FROM SEMI-CONTINUOUS
ACTIVATED SLUDGE UNITS BY ULTRAVIOLET ABSORPTION
SCOPE This procedure Is Intended fo r the e x tr a c tio n and measurement of A ro c lo r 1242, A ro c lo r 1142 re sid u e , Arobromchlor 1232, MCS 1016, MCS 1043 A ro c lo r 1221, 2 ,2 ' -d ic h lo ro d ip h e n y le th e r and t r ic h lo r o d ip h en y leth er from a c tiv a te d sludge mixed liq u o r sam ples. The data are used to determine the rate o f biod egradation o f the above components in sem i-continuous a c tiv a te d sludge (SCAS) u n it s . PRINCIPLE The compound o f In t e r e s t i s e x tra c te d in to sp ectrograd e hexane and the le v e l p resen t measured by u lt r a v i o l e t a b s o rp tio n . The w avelength(s) o f the ab so rp tio n maxima and a b B o r p t lv ltie s in l i t e r s / g . cm. are as fo llo w s :
A roo lor 1242 A ro c lo r 1142 Residue Arobromchlor 1232 MCS-IOI6 MCS-1043 A ro c lo r 1221 2 ,2 *-Dichlorodiphenyle ther Trichlorodiphenylether
245 nm. 248 248
245-5 244 245 273.5 280 & 227.5
3 7 .0 + 0.7 1/g cm 40.2 0.6 59.8 + 0.7 36.1 + 0.3 48.9 + 0.5 66.4 + 1.1
8 . 5O + 0.09
7.47 + O.07 & 63. I + 0.6
REAQENTS AND APPARATUS
1 . Spectrograde hexane - F is h e r C a t . No. H-334 or M a llin ck ro d t C a t. No. 5188.
2. Standard te s t m aterials -
A ro o lo r 1242
- Lot AK-255
A ro o lo r 1142 Residue
- OR-I59809
Arobromchlor 1232
- OR-16882
MCS-1016 MCS-1043
- OR-I5859I - OR-I5859I
A ro c lo r 1221
- Lot AK-2
2 ,2 * -D ich lo ro d ip h e n y le th e r - OR-I5066I
Trichlorodiphenylether
- 0R-174019
3* Undenatured a b so lu te e th y l a lc o h o l.
4 . Cary Model 14 Recording Spectrophotom eter w ith matched se ts o f 1 . 0, 2.0 and 5*0 cm. quartz c e l l s , or e q u iv a le n t.
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Method No. 71-17 Page 2_________________
PROCEDURE
1 . E x tr a c t the sample and a blank accord in g to A n a ly t ic a l Chemistry Method No. 71-1 u sin g sp ectrograd e hexane c o n c e n tra tin g the e x tr a c ts to a f i n a l volume o f 10 m l. as d e s c rib e d .
2 . Measure the ab so rp tio n from MOO to 210 nm. o f the concen tr a te d b lan k and sample e x tr a c ts from step 1 In s u it a b le path len gth c e lls using Bpectrograde hexane as a re fe re n ce .
3 . Record the absorbance o f the sample and blank a t the maximum wavelength fo r the component o f In te r e s t ( lis t e d In P rin c ip le s e c tio n )
CALCULATIONS
M illigram s o f Component m In SCAS u n it
(Sample absorbance-blank absorbance) (0.01)(10*)(1500)
[a b s o r p tiv ity )(c e ll patn, in cm .; (Sample volume, In m l.)
where a b s o r p t iv it y
__________ absorbance (cone, in g / l) ( c e ll p ath , in cm.)
A b s o r p tiv ltle s fo r s p e c ific components are lis t e d In P r in c ip le se c tio n .
RECOVERY DATA
Samples o f a c tiv a te d sludge were spiked in d u p lic a te a t two le v e ls w ith each component In undenatured a b so lu te a lo o h o l s o lu tio n and analyzed by the above procedure.
A ro o lo r 1242
- 83.8 + 1,356 recovered
A ro o lo r 1142 Residue
- 7 5 ,5 + 2.456 recovered
A robroaohlor 1232
- 92.4 + I .756 recovered
MCS-lOlfi*
- 9 1.6 + I .256 recovered
M0S-1045 .( '
" 94 7 + 1 . 0j6 recovered
Aroolor 1221
- 95.0 + I .456 recovered
2 ,2 ' -D io h lo ro d ip h e n y le th e r - 87-3 + 4.256 recovered
T r lo h lo ro d lp h e n y le th e r
- 95*1 6.356 recovered
The le v e ls s e le c te d were on e it h e r Bide o f the le v e l found in the SCAS units.
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Monsanto Company Organlo Chem icals D iv isio n Applied Sciences Section S t Louis, M issouri
6/71 - 0 . K ic k s , V . Saeger, E . S . Tucker
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