Document oDa3VY9nn9VmVMk7eqzbpNGyX
ARi%-o%7
WATER SOLUBILITY TEST SUBSTANCE
f n /* " L&Mw
Identity: N-methylperfluorooctane sulfonamidoethanol; may also be referred to as N-MeFOSE Alcohol, FC-790, or FM-3925. (1Octanesulfonamide, N-methyl-1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8heptadecafluoro-N-(2-hydroxyethyl)-, CAS # 24448-09-7)
Remarks: Material is an off-white, waxy solid. Sample was taken from 3M lot number 505. Purity information was not recorded.
METHOD:
Method followed: The Veith-Comstock technique, G. D. Veith and V. M. Comstock, J. Fish Res. Board Can., 32, 1849 (1975)
GLP: No Year study was performed: 1979
RESULTS:
Value (mg/L) at 18 + 1C: 0.82
Remarks: Initial values for saturated solutions resulting from circulating the system for 24 hours indicated a solubility of approximately 2.3 mg/L. It was suspected that this number was inaccurate as it was considerably higher than the solubility of the closely related material, N-EtFOSE alcohol. Since it's known that water-soluble impurities and some homologues are preferentially solubilized by this technique, the saturated water was replaced with fresh water and was allowed to recirculate for 5 hours. Replicate solubility values of the recirculated solution then indicated a solubility of 0.82 ppm.
CONCLUSIONS:
The test substance is relatively insoluble in water.
DATA QUALITY:
_______________
Reliability: Klimisch ranking = 3. This study does not meet criteria for quality testing. This study lacks sufficient characterization of the test substance purity. The properties of the test water were not noted. Additionally, the second circulation of fresh water for only 5 hours without any sampling during that time period or for extended times is inadequate to definitively conclude that the solubility is 0.82 ppm. Although solubility
006509
apparently plateaued between 4 and 6 hours initially in the first 24 hour cycle, it doesn't follow that the same effect will occur in the absence of impurities or homologues. Additionally, there was no identification of the homologues or impurities in the sample. Their presence is assumed, thus they are only possibly interfering with the solubilization of N-methyl FOSE alcohol. The extraction efficiency with ethyl acetate was not characterized. The analytical method was not validated. Electron capture detector is not analyte specific to the target analyte (FM-3925), therefore peak used for quantitation may not be target analyte. REFERENCES: This study was conducted by the 3M Company, Environmental Laboratory, 1979. OTHER Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 Last changed: 5/17/00
006510
3EX3
Firm6747 11-A
TECHNICAL REPORT SUMMARY
Oat* 1 /8 /7 9
TO: TECHNICAL COMMUNICATIONS CENTER - 201-2CN
(Im p o rta n t -- I f rep o rt s p rin ted on both sides o f paper, send tw o copies to TCC .)
Division E n v iro n m e n ta l L a b o ra to ry (EE & PC)
Proiact Raport TitlaP r e m a n u f a c t u r i n g N o t i c e FC -790
Dapt. Numbar 0535
Proiact Numbar 9970012600 Raport Numbar
S o l u b i l i t y o f FM 3925 To
V. P o th a p r a g a d a
Author(t)
^
A. N. W elter/RBiiA'iiiiReinerX,:,
Not,book Rafaranc. NB 4 6 2 6 0 -5 3 ; W
,4 4 ; NB 4 2 6 6 9 -4 1 ;
NB 4 8 2 7 7 -8 ; S e e E n v ir o n m e n ta l Lab R e q u e s t 4 1 9 7
014
Employ* Numbr(i) 09362/47816
No. of PagasIncludingCoversheat
SECURITY ^
L < Opan (Company Confidential)
Closed (Special Authorization)
3M CH EM ICAL w REGISTRY "
New Chemicals Reported
Yes
Q No
KEYWORDS: (Select terms from 3M Thesaurus. Suggest other applicable terms.)
CURRENT OBJECTIVE:
To d e te r m i n e t h e w a t e r s o l u b i l i t y o f FM 3925 ( L o t 5 0 5 ) .
EE & PC D iv . (E nvironm ental
Lab)
F luorochem ical
R E P O R T A B S T R A C T : (200-250 words) This abstract information is distributed by the Technical Communications Center to
alert 3M'ers to Company R&D. It is Company confidential material.
S o l u b i l i t y S t u d i les
( V e i t h T e c h n iq u e ) T he s o l u b i l i t y o f FM 3925 w as d e te r m in e d b y a m eth o d
in w hich w a te r was r e c ir c u la te d from a r e s e r v o ir through v
a colum n c o n ta in in g g la s s b ead s c o a te d w ith FM^3925.
A n a l y s i s o f w a t e r s a m p le s show ed t h a t t h e FM 3925
c o n c e n tr a tio n re a c h e d a p la te a u o f ^ 2 .3 mg/1 a t 4 to
6 h o u r s . S in c e w a te r s o lu b le im p u r itie s and more
s o lu b le ch em ical hom ologs a re p r e f e r e n t i a l l y s o lu b iliz e d
by t h is te c h n iq u e , th e s a tu ra te d w a ter was re p la c e d w ith
fre s h w a te r. The second s e q u e n tia l c ir c u la tio n o f w a te r
g a v e an FM 3925 s o l u b i l i t y o f 0 .8 2 m g /1 . T h is s o l u b i l i t y
v a lu e i s c o n s id e re d more r e a l i s t i c .
Information Liaison . Initials:
006511
-2-
In tro d u ctio n
FM 3 9 2 5 , b a s e d on i t s s t r u c t u r a l s i m i l a r i t y t o FM 3 4 2 2 , may reasonably be expected to p o ssess s im ila r physicochem ical c h a r a c t e r i s t i c s . The l a t t e r compound i s m in im ally w a te r s o lu b le (0 .0 5 ppm) and l i p o p h i l i c .
T echniques have been developed fo r d e te rm in in g th e s o l u b i li t ie s o f s o - c a lle d h y d ro p h o b ic m a te r ia ls w h ile a t th e same tim e p ro v id in g s a tu ra te d so lu tio n s fo r exposure to a q u a tic organism s.
The d a ta in t h i s r e p o r t r e f l e c t s th e r e s u l t s o f s tu d ie s ; w h e re in , a m o d ific a tio n o f th e V eith-C om stock te c h n iq u e has been used in d e t e r m i n i n g t h e w a t e r s o l u b i l i t y o f FM 3925 ( 1 ) .
M ethods
The m ethod and a p p a ra tu s u sed in d e te rm in in g w a te r s o l u b i l i t y was m odeled a f t e r t h a t o f V e ith and Com stock ( 1 ) . In b r i e f , w a te r in a re s e rv o ir is co n tin u o u sly s a tu ra te d w ith th e chem ical by c i r c u la tin g th e w ater through a bed o f an in e r t s u b s tra te im pregnated w ith th e chem ical under in v e s tig a tio n .
W ater s o lu b ility s tu d ie s w ere c a r r ie d o u t a t 18+ 1C. in a dark t e m p e r a t u r e - c o n t r o l l e d c h a m b e r. 2 0 0 mg FM 3925 w as d i s s o l v e d in r e a g e n t - g r a d e a c e t o n e . T h is s o l u t i o n w as t h e n a d d e d t o 2 mm s o l i d g la s s b ead s and a llo w e d to e v a p o ra te o f f in room a i r . The c o a te d g la s s b ead s w ere th e n p ack ed in to a g la s s column f i t t e d on each end w ith rubber sto p p e rs co n ta in in g s u ita b le g la s s -to -tu b in g co n n ecto rs (2 ). (A ttachm ent 1, E nvironm ental L aboratory P ro to c o l.)
One h u n d re d (1 0 0 ) ml w a te r s a m p le s w e re w ith d ra w n a t 1 , 2,- 4 , 6 , 8, and 24 hours a f t e r b e g in n in g th e e x p erim en t. At 24 hours fre s h w ater was added to th e system and fo llo w in g 5 h o u rs r e c i r c u la tio n , r e p lic a te sam ples w ere w ithdraw n fo r a n a ly s is . A ll w a te r flow ed w ere re tro g ra d e : from b o tto m to top o f colum n.
Sam ples w ere a n aly ze d u sin g th e fo llo w in g m ethodology: H e w le ttP ackard Model 5713 gas chrom atograph w ith e le c tr o n c a p tu re u sin g
N i a s t h e s o u r c e . C olum ns 6 ' x 1 / 8 " O .D . SS, p a c k e d w i t h 10% C arbow ax 20M on C hro m o so rb W-AW 6 0 / 8 0 m e sh . T e m p e r a tu r e s D e te c to r 300 C . , I n j e c t i o n te m p e r a tu re 2 0 0 C ., Oven - 180 C. I s o t h e r m a l ; flo w : 40 c c / m i n . 95% A rgon/5% M e th a n e . A b s o lu te low er d e te c tio n lim it - 0 .5 nanogram s.
R esu lts and D iscussion
W a te r s o l u b i l i t i e s o f FM 3925 a s a f u n c t i o n o f e x p o s u r e tim e com p r i s e TABLE 1 . C h r o m a to g r a p h ic t r a c e s , 10 ppm s t d . , 6 , 8 , a n d 24 h o u rs, o f th e s e r e s u l t s a re appended as A ttachm ent 2 . The re p lic a te d v alues are in good agreem ent,
006512
-3-
TABLE 1 WATER SOLUBILITY OF FM 3925 - VEITH TECHNIQUE
Sam ple Tim e, H rs .
1 2 4 6 8 24
ppm FM 3925
1 .7 2 , 1 .9 0 ,
2 .1 0 , 2 .3 3 , 2 .3 4 , 2 .1 7 ,
1 .8 2 1 .8 7
2 .1 7 2 .3 0 2 .3 5 2 .1 4
When f r e s h w a t e r w as a d d e d t o t h e s y s te m a n d a llo w e d t o re c irc u la te fo r fiv e hours, re p lic a te s o lu b ility values o f 0 .8 2 , 0 .8 2 ppm w ere o b t a i n e d (A tta c h m e n t 3 ) .
The v a r ia b ility in s o l u b i l i t i e s o b ta in e d d u rin g th e 2 4 -h o u r
run v ersu s th a t o b ta in e d a f te r th e a d d itio n of fre sh w ater
may b e e x p l a i n e d by t h e p r e s e n c e o f t r a c e i m p u r i t i e s i n t h e
2 4 -h o u r run sa m p le s. I t i s known t h a t when t e s t i n g m a te r ia ls
o f in h e r e n tly low s o l u b i l i t i e s , i t i s p o s s ib le t h a t th e t r a c e
i m p u r i t i e s may b e m ore s o l u b l e th a n t h e m a t e r i a l u n d e r s t u d y .
The r e c ir c u la te d w a te r w i l l th en te n d to s o lu b iliz e th e
i m p u r i t ie s , h en ce h ig h e r a n a l y t i c a l v a lu e s . Upon th e a d d itio n
of fre sh w ater to th e system and in th e p ro b ab le absence o f
tr a c e im p u r itie s , a more r e a l i s t i c w a te r s o l u b i l i t y v a lu e o f
0 .8 2 ppm FM 3925 w as r e c o r d e d .
.%
R eferences:
( 1 ) V e i t h , G. D. a n d V. M. C o m sto ck . A p p a r a tu s f o r C o n t in u o u s l y S a tu ra tin g W ater w ith H ydrophobic O rganic C hem icals. J . F ish R es. B oard Can. 32:1849-1851, 1975.
(2 ) E nvironm ental "Laboratory W ater S o lu b ility P ro to c o l.
ANW/EAR/cen A ttachm ents: 1, 2, 3
006513
Attachment 1
AM 1/8/79
3M ENVIRONMENTAL LABORATORY PROTOCOL FOR THE DETERMINATION OF WATER SOLUBILITY
D iscussion:
A t r u e s o l u t i o n may b e d e f i n e d a s a " p h y s i c a l l y hom ogeneous m ix tu re o f two o r more s u b s ta n c e s " ( 1 ) . In a tr u e s o lu tio n ( p a r tic le d iam eter o f le s s th an 1 n), no h e te ro g e n e ity can be d e te c te d and s o lu te s cannot be s e p a ra te d from each o th e r by m echanical means. In g e n e ra l, most o rg a n ic compounds a re n o t s o lu b le in w a te r and many te n d to form c o l l o i d s . In c o l l o i d a l d i s p e r s i o n s ( p a r t i c l e d i a m e t e r s b e tw e e n 1 nm a n d ly m ), t h e p a r t i c l e s may n o t b e r e a d i l y d i s c e r n i b l e , b u t t h e y w ill s c a tte r lig h t (T yndall e ff e c t) and can be se p a ra te d by p h y sic a l means.
A s a tu r a te d s o lu tio n in w a te r i s d e fin e d as one in w hich no more s o lu te w ill d is s o lv e a t a g iv en te m p e ra tu re , o r th e chem ical p o te n tia l o f th e u n d isso lv e d s o lu te e q u als th e chem ical p o te n tia l o f th e d isso lv e d s o lu te .
The p r in c ip a l m ethod fo r d e te rm in in g th e s o l u b i l i t y o f a c h e m ic a l a t s a t u r a t i o n i s to a n a ly z e th e s o l u t io n by some s u i t a b l e p h y s i c a l o r c h e m ic a l m e th o d . No s i n g l e m eth o d i s a v a ila b le to cover the e n tire range o f s o lu b ilitie s in w ater from r e la tiv e ly so lu b le o rg a n ic ch em icals to very in s o lu b le c h em ic als. T h e re fo re , s e v e ra l m ethods can be used to co v er th e range o f s o l u b i l i t i e s . The m ethod and a p p a ra tu s chosen was m odeled a f t e r th a t o f V e ith and Comstock ( 2 ) . B r ie f ly , w ater in a re s e rv o ir is continuously sa tu ra te d w ith the chem ical by c ir c u la tin g th e w a ter th ro u g h a bed o f an in e r t s u b s tra te im pregnated w ith th e chem ical under in v e s tig a tio n . E xperim ents are c a rrie d out in d u p lic a te .
For very hydrophobic chem icals w hich form c o llo id s , c o n c e n tra tio n tim e s tu d ie s are conducted to en su re th a t tru e s a tu ra te d e q u ilib riu m s o lu b ility has been reached as evidenced by a p la te a u in such s tu d ie s .
The ap p aratu s fo r th ese s o lu b ility d ete rm in a tio n s is housed in a te m p e r a tu re - c o n tr o lle d w a lk -in e n v iro n m e n ta l room whose c o n s ta n t te m p e r a tu re ( u s u a l ly 18C) i s k e p t below t h a t o f room tem p era tu re to p rev e n t hydrophobic compounds from p r e c ip ita tin g , c o n g e a lin g , o r o th e rw ise coming o u t o f s o lu tio n once i t i s t r a n s f e r r e d from t h i s e n v iro n m e n ta l room to th e la b o r a to r y f o r f u r th e r a n a ly se s. The p o s s ib ility o f such an ev en t happening w ould be more l i k e l y i f th e room te m p e ra tu re i s below t h a t o f th e environm ental cham ber.
006514
Attachment 2
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006bX V
H E TECHNICAL REPORT SUMMARY
Ont
1/17/79
j *' TECHNICAL COMMUNICATIONS CENTER - 201-2CN
(Im p o rta n t - I f re p o rt s p rin te d on both sides o f paper, send two copies to TCCJ
Oiviiion E n v iro n m e n ta l L a b o ra to ry (F,E & PC)
Project Fate o f Fluorochem icals
Report l <tla
A n a ly tic a l M ethodolosy and Support To
D. L . Bacon AmUiOrU)
A rth u r Mendel Nottboofc Htlaranc
41947, 44191, 462C9, 47703, 48277, 49400
s e c u r it y >
O Open (Company Confidential)
I . Closed (Spacial Authorization)
3M CH EM ICAL REGISTRY w
KEYWORDS: (Salact terms from 3M
Thesaurus. Suggest other .i|*ihcu|jiu tin ms.)
CURRENT OBJECTIVE: P r o p e r e : ;.s l i t ' p o r t .
EE & PC -D iv. FIuorochem icals
Oept. Number 0535
Project Number 9970612643 Heport dumber
008
Employee NumberUI 043939
22
New Cham oils Rapar led
Ye*
H No
R EP O R T A B S T R A C T : (200-250 wordsl This abstract information is distributed by the Technical Communications Canter to alert 3M'*rs to Company R AD . It is Company confidantial material.
Information Liaison Imtiqls: . ' ) / \ ^ J
006518
- 2 0 - BEST COPY AVAILABLE
TLC OF B i o d e g r a d a t i o n S t u d i e s on R a d i o a c t i v e F C - 9 5 . FC -1 43, and FM 3 4 2 2 ( 4 7 7 0 3 ; 6 - 1 4 , 2 1 , 2 5 - 2 7 , - 3 5 ; 3 9 - 4 3 , 4 6 )
D e t a i l s o f the b io d eg ra d a tio n s t u d ie s on la b e le d FC-95, FC-143, FM 3 4 2 2 , and c o n t r o l s a r e d e s c r i b e d i n E. A. R e i n e r ' s r e p o r t ( 1 4 ) . In the present work, the n in eteen samples each from slu d g e , w ater, and e t h y l a c e t a t e e x t r a c t s generated from b io d eg r a d a tio n s t u d i e s w e r e a p p l i e d d i r e c t l y t o p l a t e s ( 2 0 x 2 0 cm, E. Merck GF 2 5 4 s i l i c a g e l ) . The p l a t e s were d e v e lo p e d in e t h y l a c e t a t e th en exam ined f i r s t by u l t r a v i o l e t l i g h t (lo n g and s h o r t w avelen gth ) and then by a u t o r a d io g r a p h y . The p l a t e s were exp o sed t o Kodak x -r a y f i l m f o r one week, and th e film was then developed and examined. Comparison w ith control samples ind icated no s ig n if ic a n t d if fe r e n c e s .
In a s e c o n d p a r t oT t h i s e x p e r i m e n t , a p o r t i o n o f th e e t h y l a c e t a t e e x t r a c t from the various samples was m eth ylated w ith diazomethane t o c o n v e r t any n o n v o l a t i l e c o m p o n e n ts t o GC v o l a t i l e s p e c i e s . Both
th e unmethylated and m ethylated samples were then analyzed by gas c h r o m a t o g r a p h y . No d i f f e r e n c e s w e r e n o t e d b e t w e e n t h e s e and c o n t r o l
s a m p l e s . GC c o n d i t i o n s a r e d e t a i l e d i n N o t e b o o k 4 7 7 0 3 - 4 3 .
D e t e r m i n a t i o n o f t h e S o l u b i l i t y o f N -M et h yl FOSE A l c o h o l FM 3 9 2 5
( 4 8 2 T 7 - 8 ; 4 6 2 6 9 - 5 ! ;';" 42'665'-4`) "*
'
Abo ut 20 g o f FM 3 9 2 5 Lot 505 was m e l t e d ( s t e a m b a t h ) t o o b t a i n a ho m o g en eo u s s a m p l e . The c o o l e d , s o l i d m a t e r i a l , 20 0 mg, was d i s s o l v e d in a b o u t 2 0 0 ml o f r e a g e n t g r a d e a c e t o n e , and t h i s s o l u t i o n was added t o prec*. l o a n e d 2 mm d i a m e t e r s o l i d g l a s s h e a d s c o n t a i n e d in a beaker. Heads were pree.leancd .successively with heptane,
ch lo ro fo rm , a c e t o n e , w ater, methanol, and then a i r d r ie d . The
FM 3 9 2 5 c o a t e d g l a s s b e a d s w ere p l a c e d i n a g l a s s column ( 3 5 0 x 1 8 mm) and s u p p o r t e d by .lass wo ol ( p r e t r o a t e d w i t h G l a s t r e a t R) . The e n d r u b b e r s t o p p e r s w e r e c o n n e c t e d t o U e v - L i n o Vu t u b i n g and a p e r i s t a l t i c pump was u s e d t o c i r c u l a t e d e i o n i z e d w a t e r t h r o u g h t h e c o l u m n . The e n t i r e setup was conducted in th^ dark in a te m p e r a tu r e -c o n tr o lle d w a l k - i n e n v i r o n m e n t a l room ( 18+11 ) . P r i o r t o the* s t a r t o f t h i s e x p e r i m e n t , w a t e r was pumped f o r 5 h o u r s t h r o u g h Lhe s e t u p , and t h i s w ater was d is c a r d e d . The purpose o f t h i s was t o remove any im p u r it ie s t h a t would be as s o l u b l e a s , or more s o l u b l e than,
FM 3 9 2 5 . F r e s h w n t e r was ther. p l a c e d i n t o t h e s y s t e m and a t i n t e r v a l s ( s e e T a b l e 3 ) , 100 ml ( v o l u m e t r i c p i p e t ) o f w a t e r was w i t h d r a w n from t h e main 2 - l i t e r s t o r a g e chamber. Each o f t h e .100 ml s a m p l e s was q u a n t i t a t i v e l y t r a n s f e r r e d t o x s e p a r a t o r y f u n n e l , and 10 ml o f s a t u r a t e d a q u e o u s sodiu m c h l o r i d e was added f o l l o w e d by 15 ml o f e t h y l a c e t a t e . The m ixture was e x t r a c t e d and th e s e p a r a t e d o r g a n ic phase was q u a n t i t a t i v e l y tr a n s f e r r e d to a 10-ml v o lu m e tr ic f l a s k . The a q u e o u s p h a s e was r e e x t r a c t e d w i t h 4 ml o f e t h y l a c e t a t e , and th e o r g a n ic phase was added to the 10-ml v o lu m e tr ic f la s k whose v o lu m e was f i n a l l y b r o u g h t t o t h e mark w i t h e t h y l a c e t a t e . An a l i q u o t was u s e d l o r gas chromatography u s i n g an e l e c t r o n c a p t u r e
d e t e c t o r and a s i x - f o o t ( 1 . 8 m e t e r s ) column o f Carbowux CW20M run a t 180. The r e s u l t s are rep o rted in Table 3.
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Table 3
BEST COPY AVAILABLE
S o l u b i l i t y o f FM 3925 i n Water
Tim o f Water C i r c u l a t i o n ( h r s . )
1
2 4 6
8
24
FM 3925 (ppm)
1.72; 1.90; 2.10;
2.33; 2.34; 2.17;
1.82 1.87 2.17
2.30 2.35 2.14
Avg. ( H r s . 4 - 2 4 ) = 2 . 3 ppm
The s o l u b i l i t y o f FM 3 9 2 5 i s f o r t y - s i x t i m e s t h a t o f FM 3 4 2 2 . The r e t e n t i o n time o f FM 3925 i s c l o s e to Hint o f FM 3 4 2 2 , and the gas chromatographic p a ttern s (s e e Figure 2 in r e fe r e n c e 1) a r e e s s e n t i a l l y the same.
REFERENCES
( 1 ) " A n a l y t i c a l M e t h o d o l o g y on FM 3 4 2 2 , " A. M e n d e l ' s p r o g r e s s r e p o r t t o D. I,. B a c o n , d a t e d 1 1 / 1 5 / 7 7 , p . 8 .
( 2 ) D. B. E a s t y and 11. A. Wabers, A n a l y t i c a l L e t t e r s . 1 0 , 857 (1977).
( 3 ) I n t e r o f f i c e c o r r e s p o n d e n c e o f 0 . A. V r a s p i r t o D. L. Ba con , March 2 6 , 197(5, e n t i t l e d "Gas C h r o m a to g r a p h ic A n a l y s e s o f FM 3 4 2 2 . " The d i s t r i b u t i o n c o e f f i c i e n t i s d e f i n e d a s t h e r a t i o o f th e r>incentration o f compound s o l u b l e in n - o c t a n o l phase to the concentration o f a l l sp e c ie s in the aqueous p h a s e a t a g i v e n pH ( u s u a l l y 7 ) .
( 4 ) A. O t s u k i and K. Fuwa, T a l a n t a , 2 4 . 584 ( 1 9 7 7 ) .
( 5 ) G. T. W a l l a c e , J r . , I . S. F l e t c h e r , and R. A. D u c e , J . E n v i r o n , S c i . H e a l t h , A12 4 9 3 ( 1 9 7 7 ) .
( 6 ) G. D. V e i t h and V. M. Comstock, J_;_ F i s h . R e s , B oa rd C a n . . 32, 1849 (1975).
( 7 ) U. F. H e in e and R. R. Bur f o r d , C. G. K l a u s , J . D. L a Z e r t e , J . W. S a r g e n t . (Unpublished)
( 8 ) A. Mendel r e p o r t on F a t e o f F I u o r o o h e m i c a l s t o D. L. B ac on , Nov. 15, 1977.
( 9 ) C. T. C h io u , V. 11. F r e e d , D. W. Sc hm eddin g and R. L. Ko hn er t En v i r o n m o n ta l S c i e n c e and T e c h n o l o g y , ljL, 47 5 ( 19 77 ) .
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