Document Dw890eBy2gL2amrn7MqXqgZB
g6HQ -0800.373
LG3INAL
[p1%6--037>3
PHYSICALICHEMICAL PROPERTIES a. s \NAL
5=8 on
TESi T SUBSTANCE > 3
Identity:[2r-e(fNe-rrEetdhytlopaesrfBl1u2o2r8o,ocDt-a1n,esuElIfFoOnSaEmiAd,o)oretFhXy-l1a3c.ry(l2a-tPer;ompaenyoiaclsaocibd&, 2- 4)
[ethyllheptadecafluorooctysulfonyljaminolethyl ester, CAS # 423-82-
5)
Remarks: Material is an amber solid.
0
Lo LR
Remarks: Report states that sample purity is 99% or more based on information supplied by Sponsor. The purity/identity of the test substance cannot be substantiated. As presented in the report, the structural formula indicates that "purity" cannot be assigned as "39% or more". The lot number was 101.
METHOD
_
WHaydtreorlSyosliusbialsitay:FunOctEiCoDn o1f05p,H:ShOaEkCe DFl1a1s1k Method &
DPiarstsiotciioantCiooenffCiocnisetnatn(t1s-oicntWaantoleirw:atOeEr)CbDy1H12P,LCSp:ecOtEroCpDho1t1o7metric Method 87
Vapor Pressure: OECD 104, Gas. Saturation Method
Nn
3
GLP (YIN): Yes
FG
Year completed: 1994
*
3
Remarks:
wy
Details from these studies can be found in one report entitled: "Determinationof
Physico-chemical Properties of Sample D-1".
RESULTS
RETINA Water Solubility: 0.89 mg/L at 25C
Hydrolysis as a Function of pH: At 25C the reaction rate constants of the test
substance at pH 4, 7, and 9 were 0.017, 0.020, and 0.046day" with half life
timesof 42, 35, and 15 days, respectively.
DsiusbssotcainacteiwonerCeondsettearnmtisneidn Wbaetcearu:seNothdeissspoeccitartaioonf ctohnestteasnttssuobfstthaencteesatt
different pH values did not significantly differ from one another.
Partition Coefficient: Ko, > 6
Vapor Pressure: 6.0 x 10 Pa at 25C
&epa-oTs
000432
0008118100
Remarks: The study results indicated that the test substance was composed of different components which, in some cases, yielded results different from each other.
Water solubility: It is suggested that the water solubility of each component of the test substance is different from the others. Hydrolysis as a function of pH: The chemical structure of the test substance suggests that the reaction rate of each component is similar to each other. Dissociation constants in water: The water solubilityof the test substance is too low to find ionized and unionized forms of the test substance. The laboratory did not investigate its constants further by either the titration method or the conductometric method in the OECD Guideline because both methods are considered not suitable for substances with such a low solubility. However, the chemical structure of the test substance suggests that its dissociation potential is very low. Parition coefficient: The test substance was detected as ten peaks or more by HPLC, Vapor Pressure: The chemical structureof the test substance suggests that the vapor pressure of each component is different from the others. DATA QUALITY Water Solubility Reliability: Kiimisch ranking 2. The report states a purity of the substance of "99% or more". Since the purity/identity of the test substance cannot be substantiated, the stated average solubility of the test substance is not defensible. As presented, the structural formula indicates that "purity" cannot be assigned as "99 % or more". Since the methodof detection is not compound specific, and was not validated, it cannot be determined if the peaks detected in the sample chromatograms do indeed arise from the test substance. Hydrolysis Reliability: Kiimisch ranking 2. Without the purity/identity information on the test substance and compound specific analytical techniques, the experimentally determined rate constant cannot be substantiated. Dissociation Constants in Water Reliability: Kiimisch ranking 1. Potential foar compound of the given structure to ionize at any pH is low. Octanol/Water Partition Coefficient
000433
Reliability: Kimisch ranking 3. Since the purity/identity of the test substance cannot be substantiated, the stated partition coefficient is not defensible. It was not established in this study what the retention time(s)ofthe test substance(s) is. The UV detector is not compound specific and it has not been definitively established that the >10 peaks assigned as belonging to the test compound are actually related to the test material. Furthermore, it has not been established that this method for determining the octanol/water partition coefficient applies to fluorochemical compounds similar in structure to the test material. Vapor Pressure Reliability: Klimisch ranking 3. The purity/identity of the test substance cannot be substantiated. The chromatogramofthe test substance has a distinctly different profile that that of the standard. It has not been established that under the conditions of the experiment the nitrogen passed over the substance has become saturated with gas phase test substance. The reference compound (benzoic acid) has a measured vapor pressure ~ 16 times that determined for the test substance. It would be appropriate to choose a reference compound with a vapor pressure closer to that determined for the test compound The lower molecular weight constituents will have a higher vapor pressure than the n=8 component. REFERENCES Study conducted at the request of Sumitomo 3M LTD by Mitsubishi Chemical Safety Institute Ld., Yokohama, Japan OTHER Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 Last changed: 5/22/00
000434
M.S.L. Report No. 4B223-4B227
Determination of Physico-chemical Properties of Sample D-1
Submitted to: SUMITOMO 3M LTD.
Prepared by:
Mitsubishi Chemical Safety Institute Ltd.
February 14, 1996 (The original report was submitted on August 8, 1994)
000435
PESEMEN
D -2ses \
Determination of Physico-chemical Properties of Sample D-1
-
(English version)
Study No.:
Study Title:
Sponsor:
4B223-4B227
Determination of Physico-chemical Properties of Sample D-1
SUMITOMO 3M LTD.
This test was conducted in Yokohama Laboratory of Mitsubishi Chemical Safety Institute Ltd., 1000 Kamoshida-cho, Aoba-ku, Yokohama 227, Japan.
This report is the English version of the original, which was written in Japanese. `The undersigned hereby declare that this version faithfully reflects the original report
to the best of our knowledge.
Translated by
Shiro IWAMI, M.Sc. Environmental Science Division of the Yokohama Laboratory
Approved by
Jufl TORIYA, B.Sc:
Head of the Yokohama Laboratory,
000436
Testing Facility
Study No.: ~~ 4B223-4B227 Study Title: Determination of Physico-chemical Properties of Sample D-1 Sponsor: SUMITOMO 3M LTD.
Testing Facility: Yokohama Laboratory, Mitsubishi Chemical Safety Institute Ld.t (M.S.L), 1000 Kamoshida-cho, Aoba-ku, Yokohama 227, Japan (telephone: 045-963-3541)
* The company's name was changed on October 1, 1994.
(Theformer name: Mitsubishi-kasei Institute ofToxicological and Environmental Sciences)
Facility Management:
Jun TORIYA, B.Sc. Head of the Yokohama Laboratory
Sealed date: August 8, 1994
Study Management:
`Tadayoshi SHIGEOKA, Ph.D.
Sealed date: August 8, 1994
Chief Research Scientist,
Environmental Science Division of the Yokohama Laboratory
Study Director:
`Takemi NAKANOME, B.Sc.
Sealed date: August 8, 1994 -.
Senior Research Scientist,
Environmental Science Division of the Yokohama Laboratory
Experimental Scientist:
Akiko TAKEDA, M.Sc.
Sealed date: August 8, 1994
Environmental Science Division of the Yokohama Laboratory
000437
Contents
BUSI corso ES 1
page soomsssssessommmoons)
1 TES SUBSIAICEw..vvvvvvvvssnssnnnssssssssssssssssssssssssssssssssssnssssnsss senses 11 TAENGFICRUON 1.vvvvvverrsssonsvsssssssssssssnnnnnsnnnssss sesso
2 Water Solubility [SNOt.4Bu223d] y w..ccvvvvvvvevennnnnnnnnnnnnnnnnnnnsneressssssssssss 2.1 MateanrdMiethaodsl...s....oocvvveeeresserssssssssssssssssssssnssssssnnnnnnnneens] 2.2 Results ad DISCUSSION. .vvvvvvvvrrsrrsssssssssssssssssssissssssnnnnnnnnnensd Tanbd FIlGUIEeS..vs vvvvssesssssvonnivnsnnsnsssnnsnnnnnnnenssssssssssssssonsnn2n1n
3 HydrasoaflunyctisonoifpsH [Study No. 4B224] .......covvvvverrernrrsssrsssssssss 10
21 Metal RIMESmmmscesecssensamssmsssssmmmmmmmmerssstseeeseerss
3.2 Resultsand DISCUSSION...vvvrrsveessssssssssssssonnnssssnsnnnnnnrnsssssssnss1s4s
Telit WL PU
onsscmmemsssssmomssismmomsssssssssssmrssssssooss3S
4 Dissociation Constants in Water [Study No. 4B225)..............oorrrrrrsrrrsssnsssss 16
4.1 Materials and Methods.
eta--------seetss16
4.2 ReasduDISCUlSSIOtN...s...o.vvcevesseressssrssssssssssssnnnnnssnnssnsnresssnensss 18
5 Partition Coefficient (1-octanol/water) by HPLC Method [Study No. 4B226]).....19 * 5.1 Materialsand Methods .......ovvvvvvenernnnensenrsssssssssssssnsnnsnisssnnsnnnns 19 5.2 RESUS 8 DISCUSSION. .....oovvvsssennssssssssssssssssssssserssssrssssssssssssssedl FEHR sessceeecemrmmimmmmmmmssissessassesacusmmnmimimmimissenisssassssssssSssU
6 Vaporpressure[Study No. 4B227].........ccurvummmmmmmmmmenrmnnnnnnnnenerssssssssssss2s2n 6.1 MateandrMEtihodaS...l..osooeceeessesssssssnssnennsssssnsnnnnsssssssssssssssss 22 6.2 REanS dDISU CUSSS ION...vv-..evrrsvvvvnnnnssssossns rns:26 THOSUU FHIorsscssmmserssmommssssssmsmmsssssmssseammssssmoossiol (59 pages in all)
000438
Abstract
Study No.:
Study Title: Sponsor:
48223-48227
Determination of Physico-chemical Properties of Sample D-1 SUMITOMO 3M LTD.
1 Test Substance
Name:
Sample D-1
Chemical name: 2-[N-ethyl-N-perfluoroalkyl (C=1-8) sulfonylamino]
ethyl acrylate
Structural formula: Cy1Fy8.+(1a=S8:0a;ppNro(x.C7o8H%s: )n=CH1.7,: CapHpr,o.0CCH21(==%C)0H,)
2 Water Solubility [Study No. 4223]
2.1 Methods: No.10ST "Water Solubility" (Flask Method)
22 Results: Water solubilityofthe test substance was 0.89 mg/L at 25C.
3 Hydrolysis as a function of pH [Study No. 4B224]
3.1 Methods: No.111" "Hydrolysis as a function of pH", (testing at pH 4, 7,
and 921 25C) 3.2 Results: At 25C reaction rate constants of the test substance at pH 4, 7,
and 9 were 0.017, 0.020, and 0.046 day! with half life time of 42, 35, and 15 days, respectively.
4 Dissociation Constants in Water [Study No. 4B225]
4.1 Methods: No.112 "Dissociation Constants in Water" (Spectrophotometric
Method) 3.2 Results: No dissociation constants of the test substance were determined
because the spectra of the test substance at different pH did not significantly differ from one another. (But the chemical structure of the test substance suggests that its dissociation potential is very
low.)
5 Partition Coefficient (1-octanol/water) by HPLC Method [Study No. 48226] 5.1 Methods: No.1l7' "Parition Coefficient _(n-octanol/water), High Performance Liquid Chromatography (HPLC) Method" 52 Results: The test substance was detected as ten peaks or more by HPLC. The log Pow value of the main component was more than 6.
6 Vapor Pressure [Study No. 4B227)
6.1 Methods: No.104" "Vapor Pressure Curve" (Gas Saturation Method)
6.2 Results: Vapor pressure of the test substance was 6.0 103 Pa at 25C.
Number in Organizationfor Economic Cooperation and Development (OECD) Guidelines Jor Testing of Chemicals
000439
1 Test Substance
1.1 Identification
1)Namet: Chemical namet:
Sample D-1 2-[N-ethyl-N-perfluoroalkyl(C=1-8) sulfonylamino] ethyl acrylate
2)Structural fortm:CuylFpa +.1S0,N(CoHs)CHoCH,0C(=0)CH=CH, n=1-8 (n=8: approx. 78 %; n=1-7: approx. 21 %)
3)Physico-chemical properties: Solubilityt: water: insoluble acetone: 50 % or more DMSO: insoluble Melting point: 27-42C Boiling point: approx. 150C (1 mm Hg)
+ provided by the sponsor
1.2 Source
DBatch#:
Lot No. 101
2)Supplier:
Misao SHIBA, SUMITOMO 3M LTD.
=
3)Supplied quantity: approx. 100 g
4)Puritys:
99 % or more
5)Appearance: amber like wax
+ provided by the sponsor
000440
2 Water Solubility [Study No. 4B223]
A solution is a homogeneous mixture of different substances in a solvent. The particle sizes of the dispersed substances are of the same magnitude as molecules and ions. Therefore, the smallest volumes which can be obtained from a solution are always of uniform composition.
Solubility in water is a significant parameter because the spatial and temporal movement (mobility) of a substance is largely
determined by its solubility in water; water soluble substances gain ready access to humans and other living
organisms; the knowledge of the solubility in water is a prerequisite for testing biological
degradation and bio-accumulation in water and for other tests.
2.1 Materials and Methods
This study was conducted in accordance with. the standard procedure "Water Solubility" (Flask Method) in the OECDt Guidelines for Testing of Chemicals No.105 (1981). This method is summarized as follows:
The test substance (Solids must be pulverized.) is dissolved in water at a temperature somewhat above the test temperature. When saturation is achieved the mixture is cooled and kept at the test temperature, stirring as long as necessary to teach equilibrium. Subsequently, mass concentration of the test substance in the aqueous solution, which must not contain any undissolved particles, is determined by a suitable analytical method.
+ Organizationfor Economic Cooperation and Development
2.1.1 Reagents
anc-ehteoxnaen:e:
WWaakkoo PPuurree CChheemmiiccaall IInndduussttrriieess,, LLttdd.,, gguuaarraanntteeeedd rreeaaggeenntt
2.1.2 Apparatus
icnecnutbraitfougra:l separator:
Taitec Corporation, Hitachi Lid.
model M-100 model SCT 15B
ingtaesgrcahtroormatograph(GC): SShhiimmaaddzzuu CCoorrppoorraattiioonn,, mmooddeell GCC--R134AA
000441
2.1.3 Test procedure Two hundred milligrams of the test substance was dissolved in 10 mL of acetone
in an Erlenmeyer glass flask. The solvent was evaporated with stirring to deposit a thin layer of the test substance onto inner surface of the flask. The residual solvent was thoroughly removed by stream of nitrogen gas . Four hundred milliliters of distilled water was added to the flask, which was then shaken at 400.2C over 2 3-day period. A 50-mL aliquot of the water phase was sampled after 1, 2, and 3 days. The aliquot was subsequently shaken at 25+0.2C for 1 day or more to reach equilibrium of dissolution of the test substance.
: `The operation by the above procedure was repeated once more.
2.1.4 Analytical methods The concentration of the test substance was measured by gas chromatography
(GO). Prior to GC analysis, each equilibrated aliquot was treated as follows:
The aliquot was centrifuged at 4000 rpm (3000 X g) at 25C. Sodium chloride, 1.2 g, was dissolved in the supernatant, to which 4 mL of n-hexane was then added. They were shaken for 1 minutes and then centrifuged at 4000 rpm (3000 X g) at 25C. The n-hexane phase (supernatant) was analyzed by GC under the following conditions:
GC conditions
column:
`Shimadzu Corporation, wide bore column CBP20-W25-100,
0.53 mm i.d.,25 min length
:
temperature: column: 120C; injector: 200C; detector: 240C
carrier:
nitrogen gas (flow rate: 20 mL/min)
detector:
electron capture detector (ECD)
injection volume: 3 iL
As informed by the sponsor, the components of the test substance differ in length of the perfluoroalkyl chain (see $1.1). In fact, the test substance was detected as four major peaks with retention time of 3.8, 4.5, 5.1, and 6.0 minutes by GC under the conditions described above. Therefore, the concentration of the fest substance was based on total area of the four peaks.
00044
:
2
2.1.5 Calibration curve
Standard solutions of the test substance were prepared to make concentrations of
0,02, 1.0, and 5.0 mg/L in n-hexane. These standard solutions were analyzed by GC under the conditions described in 52.1.4. The total peak area of the four peaks
was calculated and plotted against the concentration of the test substance. The calibration curve yielded a straight line passing through the origin and its correlation coefficient was calculated to be 0.999 by the least square method described in Japanese Industrial Standards (JIS) Z 9041-1968.
[Figure 2.1 and Figure 2.2) At measurement of the test substance concentration, the standard solution with 1.0 mg/L was analyzed. Concentration in each test sample was calculated from ratio of total peak area for the sample to that for the standard solution. 2.1.6 Recovery An acetone solution of the test substance was prepared to make a concentration of 483 mg/L. Two milliliters of the solution was dissolved in 1000 mL of distilled water (final concentration of the test substance: 0.97 mg/L). Sodium chloride, 1.2 g, was dissolved in 4 mL of the water solution, to which 4 mL of n-hexane was then added. They were shaken for 1 minutes and then centrifuged at 4000 rpm (3000X g) at 25C. The concentration of the test substance. in the n-hexane phase (supernatant) was measured by GC under the conditions described in 52.1.4 to evaluate recovery.
[Table 2.2 and Figure 2.3] The recovery of the test substance was 94 %. The concentrations of the test substance reported below were corrected by this factor.
2.2 Results and Discussion
Average water solubility of the test substance was 0.89 mg/L at 25 C. [Table 2.1 and Figure 2.4.1 to Figure 2.4.3]
`The component with GC retention time of 4.5 minutes was rather soluble in water compared with the others. Dissolution of this component at 40C reached equilibrium within 1 day.
Itis suggested that water solubility of each component of the test substance differs from one another.
000443
3 Hydrolysis as a Function of pH [Study No. 48224]
`The testing of substance for hydrolysis is relevant to their persistence. Hydrolysis is one of the most common reactions controlling abiotic degradation and is therefore one of the main degradation paths of substances in the environment.
A procedure to determine hydrolysis is important also in indicating whether other testing should be carried out on a parent compound or its hydrolysis product. It is the degradation products that are crucial.
Hydrolysis behavior needs to be examined at pH values normally found in the environment (pH 4-9) and under more acidic conditions (pH 1-2) for physiological purpose.
Surface-controlled reactions can sometimes predominate over bulk solution hydrolysis, especially in the soil environment. This may result in different degradation rates than would be predicted from this methods based upon rates in homogeneous solutions.
3.1 Materials and Methods
`This study was conducted in accordance with the standard procedure "Hydrolysis as a function of pH" in the OECD Guidelines for Testing of Chemicals No.111 (1981).
In the environment, chemicals usually occur in dilute solution, which means that water is present in large excess, and therefore, the kinetics of hydrolysis are generally pseudo-first order at fixed pH and temperature.
`The hydrolysis reaction may be influenced by acidic or basic species H3O* (H*) and OH, in which case itis referred to as specific acid or specific base catalysis.
The concentration of the test substance is determined as a function of time. The logarithms of the concentrations are plotted against time and the slope of the resulting straight line (assuming first-order or pseudo-first order behavior) gives the rate constant.
000414
3.1.1 Reagents and water
acetone:
`Wako Pure Chemical Industries, Ltd.,
n-hexane:
Kishida Chemical Co., Ld.
sodium chloride: Junsei Chemical Co., Ltd.
sodium hydroxide: ~~ Junsei Chemical Co., Lid.
`monopotassium phosphate:
`Wako Pure Chemical Industries, Lid.,
`monopotassium citrate: Nacalai Tesque Inc.,
boric acid:
Wako Pure Chemical Industries, Ltd.,
potassium chloride: Junsei Chemical Co., Ltd.
water:
deionized water purified by Milli-Q
guaranteed reagent guaranteed reagent guaranteed reagent guaranteed reagent guaranteed reagent extra pure reagent guaranteed reagent `guaranteed reagent
3.1.2 Apparatus incubator: PH meter: gas chromatograph(GC):
integrator:
Taitec Corporation,
model M-100
`Toa Electronics Lid.,
model HM-50S
Shimadzu Corporation, `model GC-14A
equipped with an electron capture detector (ECD)]
Shimadzu Corporation, model C-R3A
3.1.3 Test procedure 3.1.3.1 Preparationofbuffer solutions
Buffer solutions were prepared by the following two methods described in the annex of the Guideline No. 111
Buffer mixtures of Clark and Lubs Citrate buffer of Kolthoff and Vleeschouwer
Each buffer solution of pH values 4, 7, and 9 was prepared to be 1000 mL using the following reagents: 1) pH 4: 0.1 M monopotassium citrate and 0.1 N sodium hydroxide 2) pH 7: 0.1 M monopotassium phosphate and 0.1 sodium hydroxide 3)pH 9: 0.1 M potassium chloride, 0.1 M boric acid and 0.1 sodium hydroxide
`The buffer solutions obtained were passed through Millipore filter of pore size
0.25 um. The pH values of the filtrates were determined to be 4.05, 7.02, and 9.05 for nominal values of 4, 7, and 9, respectively.
3.1.3.2 Preparationofstock solutionof the test substance
The test substance, 80 mg, was dissolved and diluted with acetone to prepare a
stock solution with 40 mg/L.
000445
3.1.3.3 Preliminary test (at 50C)
Four milliliters of the stock solution (prepared in 3.1.3.2) was added to 400 mL
each of the three buffer solutions to prepare test solutions of pH values 4, 7, and 9. The solutions thus prepared were tested under the following conditions:
1) Conditions
pH:
tceomnpceenrtartautrieo:n: testing period: tteesstt vveoslsueml:e:
4,7,and 9
50.04.00:m0g./1LC 5 days with continuous shaking 4E0rl0emnmLey(ecrongtlaaisnsinfglas1 k% acetone)
II) Analytical methods
The concentration of the test substance was measured by GC. Prior to GC
analysis, the test solutions were treated by the following procedure:
Sodium chloride, 128 g, was dissolved in each of the three 400-mL solutions, from which the test substance was then extracted with 100 mL of n-hexane. The
extraction was repeated twice more. The three extracts were combined and
concentrated to 50 mL, which was then transferred into a 200-mL glass volumetric
flask and filled to 200 mL with n-hexane. The hexane solution was analyzed by GC
under the following conditions:
GC conditions
column:
Shimadzu Corporation, wide bore column CBP20-W25-100, *
0.53 mm i.d., 25m in length
temperature: column: 120C; injector: 200C; detector: 240C
carrier:
nitrogen gas (flow rate: 20 mL/min)
detector:
ECD
injection volume: 3 pL
As described in 2.1.4, the concentration of the test substance was based on total
area of the four peaks detected by GC (retention time: 3.6, 4.3, 4.9, and 5.8
minutes).
00044@
III) Recovery Four milliliters of the stock solution (prepared in 3.1.3.2) was added to 400 mL
of water in an Erlenmeyer glass flask (final concentration: 0.4 mg/L). Sodium
chloride, 128 g, was dissolved in this solution, from which the test substance was then extracted with 100 mL of n-hexane. The extraction was repeated twice more.
The three extracts were combined and concentrated to 50 mL, which was then
transferred into a 200-mL glass volumetric flask and filled to 200 mL with #-hexane.
The concentration of the test substance in the final solution was measured by GC under the conditions described in 3.1.3.3.I1.
Recovery was determined to be 101 %. The concentrations of the test substance
reported for this preliminary test were corrected by this factor. [Table 3.6 and Figure 3.1]
3.1.3.4 Further investigation (at 25C)
Four milliliters of the stock solution (prepared in 3.1.3.2) was added to 400 mL
each of the three buffer solutions to prepare test solutions of pH values 4, 7, and 9. Six S-mL aliquots from each of the test solutions were transferred into glass tubes. `These solutions were examined asa function of time under the following conditions:
1) Conditions
pH:
concentration:
temperature:
testing period:
test volume:
test vessel:
4,7,and 9
0.40 mg/L
25.00.2C
33 days with no shaking
5 mL (containing 1 % acetone)
glass tube
II) Analytical methods
The concentration of the test substance was measured by GC. Prior to GC
`analysis, the test solutions were treated by the following procedure:
;
Sodium chloride, 1.6 g, was dissolved in the S-mL aliquot treated in the tube.
Two milliliters of n-hexane was added to this solution. They were shaken for 1
`minutes and then centrifuged at 3000 rpm. The n-hexane phase (supernatant) was
analyzed by GC as described in 3.1.3.3.
As described in 2.1.4, the concentration of the test substance was based on total area of the four peaks detected by GC (retention time: 3.6, 4.3, 4.9, and 5.8 minutes).
I) Recovery
000447 Four milliliters of the stock solution (prepared in 3.1.3.2) was added to 400 mL
of water in an Erlenmeyer glass flask (the final concentration: 0.4 mg/L). Sodium
chloride, 1.6 g, was dissolved in a S-mL sample of this solution, to which two milliliters of n-hexane was then added. They were shaken for 1 minutes and then
centrifuged at 3000 rpm. The n-hexane phase (supernatant) was analyzed by GC
under the conditions described in 3.1.3.3.
Recovery was determined to be 95 %. The concentrations of the test substance
reported for this further investigation were corrected by this factor.
[Table 3.7 and Figure 3.3]
3.1.3.5 Calibration curve
The calibration curve prepared in 2.1.5 (Determination of Water Solubility) `was used.
[Figure 2.1 and Figure 2.2]
At measurement of the test substance concentration, the standard solution of the test substance with 1.0 mg/L was analyzed. Concentration in each test sample was calculated from ratio of total peak area for the sample to that for the standard solution.
3.1.3.6 Calculations
Residual percent of the test substance was calculated as follows:
re =100(Ct/ Crp)
`where
Io
residual percent of the test substance after "t" days
.
Cy:
concentration of the test substance after "t" days (mg/L)
Cty:
initial concentration of the test substance (0.4 mg/L)
Assuming that the logarithms of the residual concentrations are first order as a
function of time, their reaction rate constants were calculated as follows:
where k=t1 In(100/r)
k:
reaction rate constant of the test substance (day!)
Using the average of these rate constants, half life time of the test substance was
calculated as follows:
tip =klin2
where
000415
ty: half life time of the test substance(days)
3.2 Results and Discussion
1) Preliminary test After 5 days at 50C the residual percents of the test substance at pH 4, 7, and 9
were 76, 76, and 52, respectively. [Table 3.5 and Figure 3.2]
On the basis of the results, it is suggested that the test substance is transformed at
least by 24 %.
Relating to the preliminary test result, there is the following description in the
OECD Guideline:
If less than 10 per cent of the reaction is observed after 5 days (tz, > 1 year), the chemical is considered hydrolytically stable and no additional testing is required.
`Therefore, we decided to perform the further investigation described below.
2) Further investigation
At 25C the reaction rate constants of the test substance at pH 4, 7, and 9 were
0.017, 0.020, and 0.046 day! with half life time of 42, 35, and 15 days, respectively.
[Table 3.1 to Table 3.4 and Figure 3.4]
The chemical structure of the test substance (shown in 2.2) suggests that the
reaction rate of each component is similar to each other.
000449
4 Dissociation Constants in Water [Study No. 4B225]
The dissociation of a chemical in water is of importance in assessing its impact upon the environment. It governs the form of the substance which in turn determines its behavior and transport. It may affect the adsorption of the chemical on soils and sediments and adsorption into biological cells.
4.1 Materials and Methods
`This study was conducted in accordance with the standard procedure "Dissociation Constants in Water" (Spectrophotometric Method) in the OECD Guidelines for Testing of Chemicals No. 112 (1981). General summary of this method is as follows:
A wavelength is found where the ionized and unionized forms of the compound have appreciably different extinction coefficients. The UV-visible absorption spectrum is obtained from solutions of constant concentration under a pH condition where the substance is essentially unionized and fully ionized and at several intermediate pH's. This may be done, either by adding increments of concentrated acid (base) to a relatively large volume of a solution of the compound in a multicomponent buffer, initially at high (low) pH, or by adding equal volumes of a stock solution of the compound in e.g. water, methanol, to constant volumes of various buffer solutions covering the desired pH range. From the pH and absorbance values at the chosen wavelength, a sufficient number of values for the pKa is calculated using data from at least 5 pH's where the compound is at least 10 per cent and less than 90 per cent ionized
4.1.1 Reagents and water
methanol: 0.1 Nhydrochloric
acid:
~
Junsei Chemical Co., Lid., Kishida Chemical Co., Lid.,
guaranteed reagent reagent for titration
0N.sod1 ium hydroxide:
(diluted 10 0.01 Nwith water prior to use) Kishida Chemical Co., Ld., reagent for titration
water:
(diluted 10 0.01 Nwith water prior to use) Deionized water was distilled.
4.1.2 Apparatus UV-visible spectrophotometer: Shimadzu Corporation, Model UV-260
000450
4.1.3 Test procedure
4.1.3.1 Preparationofstock solutionofthe test substance A stock solution of the test substance with 80 mg/L in methanol was prepared
using 20.0 mg of the substance.
4.1.3.2 Preparation of test solutions For measurement of UV-visible spectra of the test substance, three solutions of
the test substance were prepared as follows:
1) Acid solution of the test substance `Two millilitersofthe stock solution (prepared in 4.1.3.1.) and 2.4 mL of 0.01 hydrochloric acid were transferred into a 200-mL glass volumetric flask, which
was then filled to 200 mL with water. (final concentration of the test substance: 0.8 mg/L)
2) Alkaline solution of the test substance Two milliliters of the stock solution and 2.4 mL of 0.01 N sodium hydroxide
were transferred into a 200-mL glass volumetric flask, which was then filled to 200 mL with water. (final concentration of the test substance: 0.8 mg/L)
3) Neutral solution of the test substance
Two milliliters of the stock solution was transferred into a 200-mL glass
volumetric flask, which was then filled to 200 mL with water. (final concentration
of the test substance: 0.8 mg/L)
:
4.1.3.3 Measurement of UV-visible spectrum `The UV-visible specira of the test substance in the solutions of three different pH
values were measured with the apparatus shown in 64.1.2.
000451
4.2 Results and Discussion
No dissociation constants of the test substance were determined because the spectra of the test substance at different pH did not significantly differ from one another.
[Figure 4.1]
The water solubility of the test substance is t00 low to find an ionized and unionized forms of the test substance. We did not investigate its constants further by either "Titration Method" or *Conductometric Method" in the OECD Guideline because the both methods are considered not suitable for the substance having such a low solubility (0.89 mg/L, reported in 52.2).
But the chemical structure of the test substance (shown in S1.1.2) suggests that its dissociation potential is very low.
000452
5 Partition Coefficient (1-octanol/water)
-
by HPLC Method [Study No. 48226]
The partition coefficient (P) is defined as the ratio of the equilibrium
concentrations of
largely immiscible
a dissolved
solvents. In
substance in a
case of -octarol
two-phase
and water,
system
consisting
of
two
Pow = Co/ Cw
where
Pow:
CCou::
1-octanol/water partition coefficient
c`coonnsceennttrraattiioonn iinn w1a-toectrapnohlaspehase
"The partition coefficient being the quotient of two concentrations is usually given
in the form of its logarithm to base ten (log Pow).
Pow is a key parameter in studies of the environmental fate of chemical substances. A highly-significant relationship between the Pow of substances and their bioaccumulation in fish has been shown. It has also been shown that Pow is a useful parameter in the prediction of adsorption on soil and sediments and for establishing
quantitative structure-activity relationships for a wide range of biological effects.
000.
453
5.1 Materials and Methods
`This study was conducted in accordance with the standard procedure "Partition = _
Coefficient
Method" in
(thne-oOctEanColD/wGautiedre),linHeisghforPTeersftoirnmgaonfceChLeimqiuciadlsCNhor.o1m1a7t(o1g9r8a9p)h.y
P(riHnPcLipCl)e
of this method is as follows:
HPLC is performed on analytical columns packed with a commercially available
solid phase containing long hydrocarbon chains (e.g. Cg, Cg) chemically bound onto
silica.
Chemicals injected onto such a column move along it by partitioning between the mobile solvent phase and the hydrocarbon stationary phase. The chemicals are retained in proportion to their hydrocarbon-water partition coefficient, with water
srocliuabiloenshcihpemicbaeltsweeenlutetdhe firrsteteanntdionoilt-siomleubleon cheamicraelvsersleas-tp.haTsehis coenlaubmlnes
the
and
the 1-octanol/water partition coefficient to be established.
5.1.1 Reference compounds As reference compounds whose Pow values are well known, we selected five
substances: methyl benzoate, bromobenzene, diphenyl, dibenzyl, and DDT. In addition, thiourea was used for determination of the dead time. A mixture of the six substances was prepared in acetonitrile.
5.1.2 Correlation between retention time and Pow
`The mixture of the reference compounds (shown in 5. 1.1) was analyzed by high performance liquid chromatography (HPLC) under the conditions described below:
HPLC conditions
column: mobile phase: flow rate: wavelength: temperature:
GL Sciences Inc., Inertsil ODS-2 4.6 mm i.d., 250 mm in length (Cy chemically bound onto silica)
acetonitrile/water = 75/25 (v/v) 1.0 mL/min. 210 nm 25 C
`The HPLC retention time of the reference compounds were corrected as follows:
Rt = Rt'- Rig
where Rt: corrected retention time of the compound (minutes) Rt': retention time of the compound (minutes) Rio: retention time of thiourea (minutes)
Correlation equation between the corrected retention time of the five compounds and their corresponding Pow was computed by the least square method, resulting in the following equation:
log Pow = 5.274 log Rt - 0.0219 (r = 0.973) [Figure 5.1 and Figure 5.2]
5.1.3 Retention time of the test substance A mixture of the test substance and thiourea was prepared in acetonitrile. The
mixture was analyzed by HPLC under the conditions described in 5.1.2. Based on the chromatogram, retention time (R', minutes) were determined for components of the test substance.
000454
5.2 Results and Discussion
The, test substance was detected as ten peaks or more by HPLC. The corrected retention time (Rt) of the main component was determined to be 29.245 minutes, while that of DDT (Log Pow is reported to be 6.20.) was 13.263 `minutes. Based on the correlation equation shown in 5.1.2, the log Pow value of the main component was more than 6.
[Figure 5.2]
000455
6 Vapor pressure [Study No. 48227]
The environmental
reasons:
relevance
of
vapor
pressure
is
accounted
for
by
thefollowing
The vapor pressure gives an indication of the probability of the phase
transitions, liquid/gas and solid/gas.
The vapor pressure, together with the solubility in water, is the major
auxiliary variable for calculating the volatilityof a substance from an aqueous solution.
Vapor pressure is thus a significant factor for predicting atmospheric
concentrations.
The vapor pressure of a substance can furthermore be useful as a basis for
deciding whether or not a photochemically induced degradation study (in the
homogeneous gas phase or in an absorbed phase) is necessary.
6.1 Materials and Methods
This study was conducted in accordance with the standard procedure "Vapor Pressure Curve" (Gas Saturation Method) in the OECD Guidelines for "Testing of Chemicals No.104 (1981). This method is summarized as follows:
A stream of inert carrier gas (nitrogen gas) is passed over the substance in sucha
way that it becomes saturated with vapor of the substance and the vapor is then
collected in a trap adsorbent. Measurement of the amount of material transported by a known amount of carrier gas is used to calculate the vapor pressure at a given
temperature.
6.1.1 Reagents
acetonitrile: Wako Pure Chemical Industries, Ltd., reagent for HPLC
adsorbent: GL Sciences Inc.,
Tenax GC, 60-80 mesh
.
000456
6.1.2 Apparatus saturator column: adsorbent column: glass bead: flow meter: gas chromatograph: data processor:
Sibata Scientific Technology Lid., 12 mm i.d., 150 mm in length
Sibata Scientific Technology Lid., 12 mm i.d., 150 mm in length
Iuchi Seieido Co., Lid., | mm in diameter Shinagawa Corporation, model NWK-IC Shimadzu Corporation, model GC-14A. Shimadzu Corporation, model C-R3A
6.1.3 Vapor pressure measuring apparatus For measurement of vapor pressure of the test substance, an apparatus shown in
Figure 6.5 was assembled and set in a room air-conditioned at 25+1C. [Figure 6.5]
The glass beads coated with the test substance were packed into the saturator column up to 7 cm in length. Nitrogen gas, kept at a constant flow rate by the pressure controller and the flow gauge, was introduced to this column.
`The nitrogen gas saturated with vapor of the test substance was delivered to the
Tenax GC-packed column to trap the test substance. Total amount of the nitrogen
gas which passed through this trap column was measured by the flow meter.
Preparation ofsaturator column
1) Ten milligrams of the test substance was dissolved in 10 mL of acetonitrile in
a 100-mL round bottom glass flask.
.
2) Eight milliliters of glass beads was added into the flask. The solvent was removed by rotary evaporation. The residual solvent was thoroughly eliminated with a vacuum pump at room temperature. (The test substance was thus coated onto the glass beads.)
3) The glass beads coated with the test substance was packed into the saturator column up to 7 cm in length. Both open sides of the column were held by quartz glass wool, which was then incorporated in the vapor pressure measuring apparatus.
000457
nitrogen gas 1) Nitrogen gas was delivered into the vapor pressure measuring apparatus for 70
hours. Total volume of the carrier gas was measured with the flow meter and
determined to be 1.017 m3. (average flow rate: 242 mL/min)
2) The total volume of the gas was corrected as follows: V = Vr[73/T)(76/706-0P])
where
V:
Vr:
T:
P:
total gas volume corrected (m3)
amount of the gas measured by
temperature of the nitrogen gas
the flow meter
(298 K)
(1.017
m3)
pressure difference between at the flow meter
and at the absorber-packed column (0.4 mm Hg)
The total volume of the carrier was thus corrected by factors of the temperature
and pressure difference, resulting in 0.973 m3.
Adsorbent column
1) Eight milliliters of the adsorbent (Tenax GC) was packed into the absorbent
column. Both open sides of the column were retained with quartz glass wool. `The column thus prepared was connected to the saturator column.
2) The test substance trapped by the Tenax GC was desorbed by the procedure
described in 6.1.4.
6.1.4 Analytical methods
`The test substance trapped by the adsorbent was desorbed as follows:
1) The adsorbent packed in the column was transferred into a glass filter. The = inside of the vacant column was rinsed with 20 mL of acetonitrile, which was
then transferred in the glass filter. The rinse of the Tenax GC was repeated
twice more with 20 mL and 10 mL each of acetonitrile.
2) The three filtrates were combined and transferred into a 50-mL volumetric glass flask, which was then filled to 50 mL with acetonitrile. An aliquot of the
solution was diluted 50 fold in volume.
3) The concentration of the test substance in the final solution was measured by GC under the following conditions:
000458
GC conditions
column:
Shimadzu Corporation, wide bore column CBP20-W25-100,
temperature:
0.53 mm i.d., 25 m in length column 120 C, injector 200 C, detector 240 C
carrier:
nitrogen gas (flow rate: 20 mL/min)
detector:
ECD
injection volume: 3 uL
Calibration curve Standard solutions of the test substance were prepared to make concentrations of
0, 0.25, 0.5, and 1.0 mg/L in acetonitrile. They were analyzed by GC under the above conditions.A calibration curve prepared by the method described in 52.1.5 generated a straight line which crosses the origin and its correlation coefficient was calculated to be 0.999.
[Figure 6.1 and Figure 6.2]
At measurement of the test substance concentration, the standard solution with 1.0 mg/L was analyzed. Concentration in each test sample was calculated from ratio of total peak area for the sample to that for the standard solution.
Desorption efficiency (Recovery)
Desorption efficiency of the test substance from Tenax GC was determined
according to the following procedure:
1) Twenty five mililiters of the solution of the test substance with 1 mg/L in acetonitrile (mass of the test substance: 25 yg) was added to 4 mL of the * adsorbent in a S0-mL round bottom glass flask. The solvent was removed by
rotary evaporation to adsorb the test substance onto the Tenax GCP,
2) The test substance adsorbed on the Tenax GC was recovered by the desorption
procedure described above (except that the substance was extracted with 10, 10, and 5 mL of acetonitrile and the filtrates were transferred into 25-mL volumetric glass flask, which was then filled to 25 mL). The concentration of the test substance in the final solution was measured by GC to evaluate desorption efficiency. `The desorption efficiency was determined to be 97 %. For measurement of vapor pressure, the concentration of the test substance was corrected by this factor.
[Table 6.3 and Figure 6.3]
000479
6.1.5 Calculation of vapor pressure
Vapor pressureofthe test substance was calculated as follows:
P = (W/M)RT/V)
where P: W:
M:
R: V:
T:
vapor pressure (Pa) amount of the test substance trapped (g)
molecular weight of the test substance (g mole-1)
gas constant (8.31 Pa m3 mole"! K-1) total volume of the carrier gas corrected (m3)
temperature (K)
6.2 Results and Discussion
Vapor pressure of the test substance was 6.0% 10-3 Pa.
[Table 6.1 to Table 6.2, and Figure 6.4]
But the chemical structure of the test substance (shown in 1.1.2) suggests that vapor pressure of each component is different from one another.
Vapor pressure of benzoic acid (a reference substance in the OECD Guideline) was 0.10 Pa (24 C) under the conditions employed in this study.
000450
Table 2.1 Calculation of concentration of the test substance
-
dissolved in water
Measurement No. 1
conc. inStd moll peak area, 4Vsec
sta. test solution
concentration factor
x
Lot
Lot
1.01
B | 2sesses [2miraas | 2msems
|asors8 | 24140m1 | 2230298
0
1
1
1
Calculation equation E =ACC/8)(1/0)(1/0.96)
Measurement No. 2
conc. inSta. moi
peak area, usec su test solution
concentration factor
2
Lot
1.01
Lor)
5 |2sesees | 2rinaes | 2nseens
|ansosr | 2310268 | 228854
o
1
1
1
El Calculation equation =ACC/B(1/0)(1/0.94) average water solubility:
_0.83as/1
000461
ES
"Table 2.2 Calculation of recovery
conc. of the substance added, mail cone. in Std, mL. peak area, usec
ste. test solution concentration factor
4
0.97
5
Lot
| 2128221
0| 24ses07
|
conc. of thesubstance recovered, moll
0.51
recovery
F
a
Calculation equation F8(0/0) (1/8) (100/4)
000462
Figure 2.1 Calibration curve of the test substance
Curve Fitting (Least Sauare Method]
Input
No 12 i3
Data ConcentXr(antg/i1o)n 0.20160 1.5.00048
YP(eUaVk-sAeree)a 550784o
132171598974382
= 5.0483X 104 + 2.5966% 108 X x!
r= 0.99995
X 1000000 15
Calibration Curve
14
13
12
1
30
>A] 2s
i
Zs
3s
4
3
2
1
o 0.00 1.00 2.00 3.00 4.000 Concentration (mg/l)
000463
%
5.00 6.00 x1
: 222H 1;
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Calculations of reaction rate of the test substance (Table
constant and half 3.1-Table 3.3)
life time
Table 3.1 (pH 4 at 25C)
mdaey,s || roefstihduealsupbesrtcaenncte_, rdaatye!constant, mak () w
8891..73
0o.l0o2i27
78'00
00..001147
6682.13
00..001145
haavlefraitgeetriomtee cCotns1t,a2n)t 420.a0v1s7day"!
calculation equatKi=on1s/tXIn 100/c tes /kXn 2
Table 3. (pH 9 at 25C)
iGmayes,|| Ww | 5z 125 1t5]
orefstihduealsupbesrtcaenncte, monic)
27.844 6957..01 5301.12
rdaatye'lconstant) w
00..004408 00..004487 00..005418
averagetraiteeconstant 105.d0a4v8sday"!
Table 3.2 (pH 7 at 25C)
mdaey,s|| roefstihdeusalubpsetrcaenncte, 0 | mon
55
8885..69
1155
7634.15
23
593.a9
average ratteoceonstant
rdaatye'!constant) o0l.0012s4 00..002103 00..002108 35_0.d0or2s0day!
"
000469
Table 3.4 fCoarlFcuulratthieornisnvoefstreisgiadtuiaoln c(oantc2e5n.tr0at0i.o2noCf)the test substance
- pewakoarenJUoStS ecosnoi.n ppeasirdcunet
Bo
0
2 5 oeeeiss zszures 0.11 sed
s o 7 iaasse siims mlzeaermeeiss 000..333108s18 8T898e.6d7
o1 szZmoeeomlnisaszs zziesassmizss 0D0..i33v50e1 68997.s30
12s esusszs Isesits 0.220 51.1
1s 1o agfaearrmilieesecesss zsiooisieseliss0 000...32008z08 77s14o.1z0 lo 1 Z2e77i0osms c1ossmee0cnols 00..237098 6769.38
a eis loz olsz 317 ws 7 Zmeerrmees zlotemrrs 0o.z54s1 6Se6i3s ss 7T Zzamoemeeriss misissovesss 00..2z5i0e 6820..18
cConcoontrnaticonoffaactthoenrstatndaardstaluotonn(A): 21.501 mall.
.
Toocvoavlarcyo(nac)antation of the test substancelF): 05.4%02 mall
calculation equation:
D=A(C/DI+E1+F1(100/G) +100
000470
Table 3.5 Calculations of residual concentration of the test substance "for Preliminary test (after 5 days at 50.00.1C)
initial concentration of the test substance, mall
after days conc. in:Std., mgt. peak area, 4V sec std test solution concentration factor onc. in the test solution
x
8
1.00
1.00
1.00
| 3022268
D | 1867539
E
2
0.308
3022269 1876183
2 0.307
3022289 1284465
2 0.207
calculation equation * F =B(0/C)(/E)/A(1/1.01)100
000471
.
Table
3."6foCralcPurlealtiimoinnaorfy
recovery test
Conc. o the test subs"tadndcse, mo conc. in Std, mail
peak area, uvsec Sua test solution
concentration factor
A
0.402
5
100
| | 2em220
0| 262022
2
conc. of the test sruebcsotvaenrceed, mail
0.408
recovery, %
F 101
CalculaFtio=nBe(qu0a/tiCon)(1/EX1/1A0)0
Table 3.7 fCoarlFcuulratthieornionfverseticgoavteiroyn ---
conc. of ithe test subsatadndceed man conc. inSta mall peak area, psec
ste.
_
test-solution
concentration factor
A
0.402
5
Lot
| zms2zn
o | 2639838
25
conc. of the test seucbosvtearnscde, mail
recovery, %
F
CalculaFtio=n Beq(ua0t/ioCn)1/EX1/1N0)0
000472
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Figure 4.1 UV spectrum of the test substance in acidic, neutral, and alkaline solutions concentation of the test substance 0. 8ag2/
acidic
neutral
aialine
|
000484
Figure 5.1 Correlation between HPLC retention time and Pow -.of the reference compounds:
Curve Fitting (Least Sauare Method Input Data
No
log Rt
log Pow
2|
00..365256
22.9192
3a
00.891831
338716
5
1123
8.20
yr== 0-.29.71285188% 1072 + 5.1282 X x}
x1 7.00 5.00 5.00 z 1.00
2
= 3.00
6
2.00
1.00
0.00 00 0.2 04 08 08 1.0 12
logRt
*1
000485
Figure 5.2 HoPfLtChechrrefoomraatnocgercaommspounds and the test substance
wweell
Loriod
BHEEE},
i3 i
reference compounds
w 1,
20e|dd de8 ne
reFH sR r- oeres
EE Teee S sR ion EEfeS es a weel ye
mE i
it i
oPPoosuemmmonon
uw ol
EE ERrdIemCbusEEISdRNSA ia
or
test substance
h-e
4
.
wo]
oo
10 O02R9?ES G o e NI\
000486
PetLPVto oRoeol sTmimne obwTroe Wtuuidmmnth 5o Loom o Haue nnw ouuSiaenc aDDSOooRERmmEENowOnEo oOWmus
ncEcS2na ae to'3w s ae 8
RaiRmu looagsEsU iE NE
l1iogPmnor IR
eRGees
8
EE om iE hw bm i
Wanene a
8 8
RHRaEmw IiImmRIoioEh EER IE 8
Table 6.1 Calculation of vapor pressure
tapped test substance (corrected mass),
molecular weight of the test substance gas constant, Pasmaemole+K:1 corrected total volume of the carer ans, m3 temperature, K
v La7x10? x es 8.31 V 0.973 To |e
Calculation equations. ve P= WR
Table 6.2 Calculation of mass of the trapped test substance
cone. iniStd. moll
peak area, uV+sec su test solution
con. in th test solution, mai. final volume, mi dition factor
A
1.008
5 | 2483087
| 1ai2087
0.571
50
E
1)
wrapped test subsat5amnecaesured mass, as corrected mass,
asx? vo | rarxioe
calculati=onAe(qCu/atBi)oEnCD/1000)(1/0.97) (1/1000)
000487
Table 6.3 Calculation of desorption efficiency
conc. of the test substaadndceed, mall conc. inStd, mall peak area, uV+sec
st. test solution
final volume, mL
A
0.02515
5
1.008
| 2451408 | 2872200
25
cone. of the test sruebcsotvaenrecde, man. desorption efficiency, %
Calculation equations E =8(0/C)(25/1000)
E
0.02434
F
97
F =(E/n100
000488
Figure 6.1 Calibration curve of the test substance
Curve Fitting (Least Square Hethod
tnput ata
vo ConcaniKreainison
:i
00.525s2:
i
[ie
VPerkAAres (650324713s05 pri
YTl= a-9a.s1e5s0r6X 103 + 2.4740X 106 X x!
x 1000000
Calibration Carve
2 2 22 20 Tis
S>3 i1a.6
:
<1.2 31.0
os "0.8
0
-
0
0.0 Co oT Coonwcentratoisontns/o1)s io x ie
000489
Figure 6.2 foGrCcacthbrraotmiaotnogcurravmes -o-f the test substance
Std. Omg/2
Std. 0.25m8/2
Std. 0.50mg2/
SZErD OoFv R330E%E4
std. 1.0 mg/2
000490 GemioF u3i0 OE
\ po :
Figure6.3 GC chromatograms of the test substance
-- for desorption efficiency
Std.(1.0mg/ 2)
test solution
dfs
OEIIIE 2
Fe Folin E
000491
Figure 6.4 GC chromatograms of the test substance
.--- for measurement of mass of the trapped test substance ---
Std. (1.0mg2)/
test solution
28el
|
} 2821)
T lEELaFaine
Fe r oGean E
GH ow dese ime E ghesd 2
AEST feeds BE
000497
ee
a
oe (OF
;
{Tenax GC?
2:
= flow meter
I=
i
1
H23IRSEHle
i] &
0004953
