Text

Final Rept Acute Toxicity of Betz Clam-Trol CT-1 in Menidia Menidia
	ML17223B306
Person / Time
Site:	Saint Lucie
Issue date:	06/24/1991
From:	; AQUA SURVEY, INC.
To:	;
Shared Package
ML17223B307	List: L-91-299, Forwards Copy of NPDES Permit Notification Request Sent to EPA on 911016,per Section 3.2.4 of Environ Protection Plan; ML17223B306; ML17223B308; ML17223B309; ML17223B310; ML17223B311;
References
	91-089E, 91-89E, BR91-1513E, NUDOCS 9111140222
	Download: ML17223B306 (37)
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ATTACHMENT2, RQ"R ~URVCV, INC.

iINAL REPORT TklE ACUTE TOXICITY UF BET~ CIAN TROLe CT 1

IN NENIDIQ gL'N~DTA JULY 24, 1991 BR&1-3 513E JOB

$91-089E 499 Point Breeze Road o Flemlngton, New Jersey 08822

~ Telephone (908) 788-8700 FAX (908) 788-9165

. 9iiii40222 9iii0i PDR ADOCK 05000335 P.

PDR

1 Z-

'1 1

RQUR SURVEY, INC.

Clam-Trol~ CT-1 Acute Bioassay with Menidia Menidia Data Re i e e t

~uter York Terrell Stud Com leted o

July 12, 1991 Performin Laborator Aqua Survey, Inc 499 Point Breeze Road Flemington, New Jersey 08822 Laborator Pro'ect I.D.

91-089E 1 of 12

RECUR SURVEY, INC.

STATEMENT OF NO CONFIDENTIALITY CLAIMS No claim of confidentiality is made for any information contained in this study on the basis of its falling within the scope of FIFRA Section 10 (D)

(1)

(A),

(B) or (C).

BETZ LABORATORIES, INC.

4636 Somerton Road

Trevose, PA 19047

r. Lar ons Company Agent A

atic Toxicolo ist Laborator Mana er Title Date Signature ASI Project Number:

91-089E 2 of 12

RECUR SURVEY, INC.

THE ACUTE TOXICITY BIOASSAY OF CLAM-TROL, CT-1 ON ~ENIDI MENIDIA This study does not meet the requirements for 40 CFR Part

160, Submitter:

Signature:

Betz laboratories, Inc.

4636 Somerton Road

Trevose, PA 19047 Date Sponsor:

Signature:

Betz Laboratories, Inc.

4636 Somerton Road

Trevose, PA 19047 Date Study Director:

ork Terrell Date 3 of 12

RECUR SURVEY, lgC.

QUALITY ASSURANCE UNIT INSPECTION STATEMENT FOR THE ACUTE TOXICITY OF CT-1 TO MENIDIA MENIDIA In accordance with the regulations set forth in Good Laboratory Practice for Nonclinical Laboratory Studies, 40 CFR 792, Federal

Register, vol. 48, November 29, 1983, part 4, The phase of study inspection, along with the dates(s) of inspection are shown below:

ase o

Stud Preparation and set-up Exposure period and daily observations Notebook entries Concentration validation Correlation of notebook entries to final report a

e s o

s ectio 7/8/91

'/10-11/91 7/11/91 7/8,9/91 7/23/91 Comments:

At the time of this inspection, all work had been or was being performed in a manner consistent with the Good Laboratory Practices.

rl Cer o

uality Assurance Officer Date 4 of 12 ar

~

v

~

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RECUR SURVCV, INC.

Summary A sample of Betz Clam-Trol, CT-1, received from Betz Laboratories, Inc., Somerton

Road, Trevose, PA 19047 on March 21,

1991, was tested for potential acute toxicity to the saltwater finfish ~enidia menidia.

The test was conducted under static conditions with daily renewal of the test solutions at nominal concentrations of 0.625, 1.25, 2.5, 5.0 and 10.0 ppm.

Concentration validation made before renewals at TO and T73 revealed a mean concentration of 0.563, 1.14, 2.46, 4.30 and 10.31 ppm while concentration validation made after renewals at T23 and T96 revealed a mean concentration of 0.39, 0.85, 1.97, 4.11 and 7.73 ppm.

After 96 hours0.00111 days 0.0267 hours 1.587302e-4 weeks 3.6528e-5 months mortality ranged from 25 percent at the 5.0 ppm concentration to 100 percent at the 10.0 ppm concentration.

The nominal" 96 hour0.00111 days 0.0267 hours 1.587302e-4 weeks 3.6528e-5 months LC50 was 6.02 ppm calculated by the Binomial method.

5 of 12

RECUR SURVEY, INC.

I,.

Ob) ective The objective of this study was to determine the acute toxic effects of Betz CT-1 in a marine/estuarine aquatic environment with regard to finfish.

The measure of potency is that concentration, in water, which produces a

significant toxic response in the exposed animals after 96 hours0.00111 days 0.0267 hours 1.587302e-4 weeks 3.6528e-5 months (4 days).

II.

Test material Source:

Betz Laboratories, Inc.

Somerton Road

Trevose, PA 19047 Name:

Density:

Clam-Trol~,

(CT-1) 4 Solubility in Water:

100 Date Received:

March 21, 1991 Amount Received:

1 pint III. Materials and Methods A.

Method The method employed was a modification of the method outlined in Methods for Measuring the Acute Toxicity of Effluents to Freshwater and Marine Organisms EPA/600/4-85/013 March 1985.

(See Appendix A for the Protocol).

B.

Test Organisms

~Secies The test species, representing a typical temperate saltwater finfish, is M~ie idia m~eidia.

6 of 12

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FIQUH SURVEY, INC.

Size e

P sica Co ditio Animals used for this test were )uvenile field collected ~enidia

~n~e

.dia

. Animals appeared to be healthy and in good physical condition.

Source cclimatio All animals utilized in this test were field collected from Sandy Hook, New Jersey on May 29, 1991.

The animals were acclimated to filtered (0.45 microns)

Manasquan Inlet Water (natural seawater) for 23.25 hours2.893519e-4 days 0.00694 hours 4.133598e-5 weeks 9.5125e-6 months at a moderate changeover rate.

C ~

Test System Source of D lutio ater Water utilized for this test was filtered (0.45 microns) natural seawater obtained from Manasquan River Inlet, Manasquan, New Jersey.

Tem erature The test temperature was 20 +/-

2 C

Test essels The test vessels were 20 liter, 20 x 25 x 40 cm tanks containing 6,000 ml of test solution at a depth of 9.0 cme Photo eriod A 14-hour light/10-hour dark photoperiod with a 30 minute transitional period was utilized.

~Lo cQgg Each test chamber contained ten organisms with an average weight of 0.171 gram each in 6,000 mls of test solution, resulting in a loading factor of 0.285 gram per liter.

7 of 12

RQUH SURVEY, INC.

D.

-Test Design A range finding test was conducted separately.

Three concentrations of the test material were evaluated using 5 organisms per treatment with no replication.

The definitive test was conducted using 10 organisms in each of 2 replicates at each of five treatment levels.

~Co trol A control treatment was run concurrently with the test substance treatments using the same dilution water and the same number of organisms as per the test concentrations.

es Testing was conducted under static conditions with daily renewal of the test solutions.

An initial test material stock solution of 1,000 ppm was prepared with distilled water.

Test solutions were prepared from the stock solution and then dispensed into the test chambers.

The test was initiated when, within 30 minutes of test solution preparation, the test organisms were transferred to the test chambers.

The range-finding test spanned 24 hours2.777778e-4 days 0.00667 hours 3.968254e-5 weeks 9.132e-6 months and was conducted using 10 organisms at each of three treatment levels: 0.1, 1.0 and 10 ppm.

Test results indicated a toxic response between 1 and 10.0 ppm.

Exposure at the lower concentration level resulted in no mortality after 24 hours2.777778e-4 days 0.00667 hours 3.968254e-5 weeks 9.132e-6 months , while exposure at the higher level resulted

-in 804 mortality after 24 hours2.777778e-4 days 0.00667 hours 3.968254e-5 weeks 9.132e-6 months .

The definitive test was of 96 hours0.00111 days 0.0267 hours 1.587302e-4 weeks 3.6528e-5 months (4 days) duration and was conducted using two (2) replicates of ten organisms each at each of five treatment levels, 0.625, 1.25, 2.5, 5.0 and 10.0 ppm.

Definitive test concentration levels were determined based upon 24-hour Rangefinding Test results.

Test vessels were examined at each 24 hour2.777778e-4 days 0.00667 hours 3.968254e-5 weeks 9.132e-6 months interval from test initiation through test termination.

Survival/mortality determinations were recorded for each chamber.

Dead animals were removed and discarded.

8 of 12

RECUR SURVEY, INC.

C emical nal ses Concentrations were validated at TO, T23, T73, and T96 using Clam-Trol

, CT-1 methyl orange method (supplied by Betz Lab) in the range of 0.2 3.0 mg/l.

A Bausch

& Lomb Spectronic 21 was used for the absorbance readings (see Appendix, page B-l).

Ph sical C emical Parameters The temperature, pH, dissolved oxygen (DO) concentration and salinity were measured and recorded for each treatment level at the beginning and end of each 24 hour2.777778e-4 days 0.00667 hours 3.968254e-5 weeks 9.132e-6 months test interval.

Meic~hi q At termination of the test, a random sample of test organisms was measured and weighed.

IV.

Results The definitive test resulted in mortality ranging from 25% at the 5.0 ppm concentration to 1004 mortality at the 10.0 ppm concentration (See Table I).

The test solution temperature was maintained between 18.0 21.5 C (See Table II).

Dissolved oxygen was maintained between 5.1 and 7.4 mg/l (See Table III).

The pH ranges during the test were between 7.8 and 8.1 (See Table IV).

The salinity ranges during the test were between 29.0 and 30.0 ppt (See Table V).

The mean concentration validation before each renewal period at TO and T73, and at the end of each renewal period at T23 and T96 can be seen in Table VI.

V.

Source of Documentation All original data documentation is being maintained at Aqua Survey, Inc.,

499 Point Breeze

Road, Flemington, NJ 08822, in Betz Laboratories Notebook 002, pages93-107.

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RECUR SURVEY, INC.

Table I:

ortalit Data Dead Exposure Time Control (hrs

)

A B

0 625 A

B 2

25 A

B 2.50 A

B

~0 A

B 10.0 A

B 0.0 24 0

0 0

0 100 100 48 72 96 0

0 0

10 100 100 0

0 0

0 100 100 0

0 0

0 20 0

100 100 Table II Te erature i De rees C

Exposure Time

~Co h~o 0 625 (hre.)

A B

~5.

A B

10.0 A

B 0.0 48 72 96 21.5 21.5 21.5 21.5 21 5 21.5 21 5 21 5 21.5 21.5 21.5 21.5 19.5 19.5 1

5 19.5 19 1

5 9

5 19 5

1 5 19 5

19.

1 5 19.5 19.5 19 0

1 5

19 5

5 19.0 19.0 19.5 19.5 19.5 19 5 19.5 19 5 19.5 19.5 18.0 18.0 18.0 18 0

18 0

8 0

18 0

1 0 18 5

Table III Disso d Ox e

Exposure Time

~otto (hrs.)

A B

~06 ~+

A B

~LB'i

~50 A

B A

B

~00 A

B 0.0 24 5.8 5.8 5.8 5

8 5.8 5.8 5

8 5.8 5.8 5.8 5.8 5.8 7.2 7.2 7.2 7

2 7.3 7.3 7.3 7

3 7.4 7.4 6

5 6.

6 6.

6 6

6 72 96 6.5 6

5 6

6 6

6.

6 6

6.6 6

6 6

6.6 5.4 5.2 5.2

.3 5.3 5.2 5.2 5.1 5.2 5.1 Table IV Exposure Time Control (hrs.)

A B

0. 625 A

B

~25

5. 0 A

B A

B 10.0 A

B 0.0 8 ~ 0 8 ~ 0 8.0 8.0 8

0 8.0 8.0 8

0 8.1 8.1 8 ~ 1 8.1 24 8.0 8.

.0 8

0 8.0 0

8 8

0 8.0 8

0 8

8 0

0 8

0 8.0 8.0 8

0 8.0 8.0 72 7.9 7.9 8.0 8.0 8.0 8.0 8

0 8.0 8.0 8.0 6

7 8

7 7

10 of 12 r

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RECUR SURVEY, IN(.

Table V

Sa i Exposure Time

~Co trol (hrs.)

A B

0.625 A

B

~1 A

B 0

A B

5.0 A

B 10.0 A

B 0

0 24 48 96 29.0 29.0 29.0 29.0 29.0 9.0 29 0

9 0 29.0 29.0 29.0 29.0 2

0 29.0 29.0 29.0 29.0 9

0 29 0 29.0 9

0 9.0 30 0 30.0 30.0 30.0"30.0 30.0 30 0 30 0 30.0 30.0 2

5 29.5 2.5 29 5 29.5 29.5 9

5 29 5

.5 29 5

2 5 29.5 29.5 29.5 29.5 9.5 29.5 29.5 29.5 29.5 Table VI o ce tratio Validatio Before Renewal Conc.

ppm

0. 625

1. 25 2.5 5.0 10.0 0.54 1.09 2'7 4.26 10.31 0.59 1.19 2.54 4.34 Mean 0.56 1.14 2.46 4.30 10.31 Co ce tratio Va idatio fter e

l Conc.

ppm 0.625 1.25 2.5 5.0 10.0 T23 0.34 0.71 1.92 3.88 7.73 T96 0.44 0.98 2.02 4.34 Mean mcCml 0.39 0.85 1 ~ 97 4.11 7.73 ll of 12 899 Po(r t dree:e.<oca

~ Flerirgron New.'cree. 08822

~ re.eor,""e F906) 738 "7CG AC RO~ 330~O

~ "-" On AOige '.Ouieiana 7068-'

le!e~'rare l300) '54. -'d-'

Il OTC16 JC1

>)

CONC.

NUMBER NUMBER PERCENT

~

EXPOSED DEAD DEAD 20 20 100 20 5

25 2.5 20 0

0

1. 25 20 0

0

.625 20 0

0 THE BINOMIALTEST SHOWS THAT 5 AND 10 CAN BE USED AS STATISCALLY SOUND CONSERVATIVE 95 PERCENT CONFIDENCE LIMITS SINCE THE ACTUAL CONFIDENCE LEVEL ASSOCIATED WITH THESE LZMXTS IS 97.93044 PERCENT.

AN APPROXIMATE LC50 FOR THIS SET OF DATA IS 6.02491 BXNOMIAL PROB- (4) 9.536743E-05 2.069473 9.536743E-05 9.536743E-05 9.536743E-05 WHEN THERE ARE LESS THAN TWO CONCENTRATIONS AT WHICH THE PERCENT DEAD ZS BETWEEN 0 AND 100, NEXTHER THE MOVING AVERAGE NOR THE PROBZT METHOD CAN GIVE ANY STATISTICALLY SOUND RESULTS.

12 of 12

A E

N D

I

PROTOCOL ACUTE TOXXCZTY BZOASSAY POR SZLVERSXDE ggg~( ggml~

ASX HO'100 '2 June 25, 1991 SPONSOR:

et o ato 'es c.

4 6

oe o

oa ev 1 047 STUDY NUMBER:

TESTING FACILITY:

Acpxa Survey, Inc.

(ASI) 499 Point Breeze Road Flemington, New Jersey 08822 United States of America PROPOSED START DATE:

u 8

99 PROPOSED COMPLETION DATE:

STUDY DIRECTOR QA OFFICER Signat xe Si at

/,

Date SPONSOR APPROVAL:

Signature Date 1 of 7

PURPOSE

'o determine the acute toxicity of the test material to the Silverside and to establish the median lethal dosage (LC50) of the test material under static renewal conditions for 96 hours0.00111 days 0.0267 hours 1.587302e-4 weeks 3.6528e-5 months .

TEST ARTICLE:

The test article is which was received from e

on

the test article is c

(description).

The sample is labeled with an ASZ number 9 -08 Any test article remaining after the test is completed will be disposed of according to instructions from the sponsor or returned to the sponsor.

TEST ARTICLE CHAEULCTERISATZON:

Data concerning stability, uniformity, composition and additional chemical/physical characteristics of the test article will be provided by the sponsor on the Test Substance Form (supplied by ASZ).

C".emical analyses will be the responsibility of the sponsor unless prior arrangements have been made for ASZ to assume that responsibility.

CONTROL ARTICLE None required.

TEST SYSTEM~

Testing is performed with the Silverside, g~n'd~ g~ejg~, representing an estuarine/marine finfish.

JUSTZPZCATION Silverside are considered the appropriate test system as they are a

characteristic system in which the response to toxicological agents can be evaluated.

DILUTION WMER Whenever possible, reconstituted sea water will be used.

Reconstituted water will be aged one or two weeks and intensely aerated prior to use.

Zf use of reconstituted water is not possible, an alternative dilut'on

water, uncontaminated and of constant quality, will be used.

2 of 7

SOLVENTS Whenever possible, the toxicant will be introduced into the test solution without the use of solvents other than water. If alternative solvents are necessary, they will be used sparingly, not to exceed 0.5 ml/1 in a solution.

TEST MATERIAL The technical grade, end-use product or both will be used in this study.

The brand name or chemical names and a lot number are used to define a

test material.

Mixtures are defined by ingredient and percent of each ingredient, where possible.

TEST ORGANISMS The Silverside, ~e~d'e~i~,

is the organism specified for this test.

Juveniles up to 90 days old, with all organisms within a +

3 day age class, will be used.

The standard length of the longest fish will be no more than twice that of the shortest.

The age of the fish will be ascertained from the supplier along with any disease treatment schedule.

EXPOSURE CHAMBER:

Nineteen (19) liter all glass aquarium or other appropriate size glass chambers will be used.

RANGE-PZNDINQ TEST Zf the toxicity of the test substance is not already

known, a range finding test will be performed to determine the range of concentrations to be used in the definitive test.

DEPZNZTIVE TEST:

The purpose of the definitive test is to determine the concentration-response curves and the 48 and 96 hour0.00111 days 0.0267 hours 1.587302e-4 weeks 3.6528e-5 months LC50 values.

A minimum of 20 fish per concentration will be exposed to five or more concentrations of the chemical.

Each designated treatment group will be exposed to a concentration of toxicant that is at least 504 of the next highest concentration.

Test organisms will be divided into two chambers per treatment group (10 fish each).

All organisms will be randomly assigned to test vessels.

3 of 7

TEST PROCEDURES Zn preparation for the test, the chambers are filled with appropriate volumes of dilution water.

The test substance is introduced into each

~

chamber.

The test is started by randomly introducing fish acclimated in accordance with the test design into the test chambers within 30 minutes after the addition of the test substance.

Fish in the test chambers are observed periodically during the test, the dead fish removed and the findings recorded.

Dissolved oxygen concentration, Ph, temperature, the concentration of test substance, and other water quality characteristics are measured at specified intervals in test chambers.

The test solution will be renewed daily.

ACCLZMATZON Organisms will be acclimated to the dilution water as long as possible.

The fish will receive standard commercial chow and newly hatched brine shrimp, ~e~m'

~sa '~, daily until two days prior to testing, at which time feeding will be discontinued.

Fish will not be fed during test.

Test organisms will be observed prior to testing for signs of disease,

stress, physical damage and mortality.

Znjured, dead and abnormal individuals will be discarded.

Zf organisms show any of these signs, remedial action will be taken during the acclimatization period and not during the test phase.

Organisms that have been treated for disease are acceptable for testing

~

provided they do not exhibit signs of disease during the 48 hours5.555556e-4 days 0.0133 hours 7.936508e-5 weeks 1.8264e-5 months of pretest.

Organisms will not be used if they appear to be diseased or stressed or if more than 34 die during the 48 hours5.555556e-4 days 0.0133 hours 7.936508e-5 weeks 1.8264e-5 months immediately pr'or to testing.

TEST PARAMETERS:

CONCENTRATZON MEASUREMENT Analytical measurements of the test substance will be made for each concentration at T, T>, T

, and T> of the test by a method validated before beginning tVe test. Qy appropriate laboratory practices.

TEMPERATURE

'ilversidewill be tested at 20 +/- 2'C.

Temperature will be measured continuously in at least one test vessel during the entire study.

4 of 7

pH The pH will be measured at the beginning of the test and daily thereafter at each toxicant concentration as long as animals are surviving at that level.

SALINITY

'he salinity will be measured at the beginning of the test and daily thereafter at each toxicant concentration as long as animals are surviving at that level.

DISSOLVED OXYGEN Dissolved oxygen (DO) will be measured at the beginning of the test and daily thereafter.

Measurements will be taken from each concentration as long as animals are surviving at that concentration.

The DO concentration during the first 48 hours5.555556e-4 days 0.0133 hours 7.936508e-5 weeks 1.8264e-5 months shall be between 60 and 100%

saturation and must be between 404 and 1004 saturation after 48 hours5.555556e-4 days 0.0133 hours 7.936508e-5 weeks 1.8264e-5 months .

PHOTOPERIOD A 14 hour1.62037e-4 days 0.00389 hours 2.314815e-5 weeks 5.327e-6 months light and 10 hour1.157407e-4 days 0.00278 hours 1.653439e-5 weeks 3.805e-6 months dark photoperiod with a 15 to 30 minute transition period will be employed.

LOADING The size of the test vessels will be such that the loading factor is no greater than 0.8 g/l.

OBSERVATIONS:

The fish will be observed at 24, 48, 72, and 96 hours0.00111 days 0.0267 hours 1.587302e-4 weeks 3.6528e-5 months with particular attention being given to general behavior, partial or total loss of equilibrium, fin erection and mortality.

A study is not acceptable if more than 104 of the control organisms die during a test.

5 of 7

%SIGHT AND LENGTH:

After all 96 hour0.00111 days 0.0267 hours 1.587302e-4 weeks 3.6528e-5 months evaluations have been performed, the test is terminated.

A random sample of 30 exposed surviving fish are sacrificed for weight and length determinations.

REPORT The following are included in the final report:

Test Material - Zf technical grade product is tested, its

source, batch and exact purity are reported.

When end-use product is tested, the exact percent of active ingredient and the type of formulation (i.e. granular, wettable powder) are reported.

Dilution Rater - Dilution water source, its chemical/physical characteristics, and pretreatment are reported.

3 ~

6 ~

7 ~

8 ~

Exposure Chambers - The volume, diluent depth, and container construction material are reported.

Test Organisms - Source, quarantine, holding and acclimatization, inclusive of feeding schedules and disease treatment procedures, are reported.

The age and scientific names are reported.

Range Finding Test Procedures and results are reported for the range finding study.

Included at a minimum are sample size, concentrations tested and mortality data.

Definitive Test - Procedures used to prepare toxicant stock solutions are described.

The method of dosing is reported.

The criteria for, determining effects are defined.

At 6, 24, and 48

hours, raw data or percentage of deaths/effects at each treatment level along with the number of organisms exposed at each level is reported.

Toxic symptoms, both physical and behavioral, observed during the test are reported.

Calculated LC50 Value LC50 values (24 and 48 hours5.555556e-4 days 0.0133 hours 7.936508e-5 weeks 1.8264e-5 months if possible) with the corresponding 954 conf'dence intervals and slopes of the concentration response lines and method of calculation will be reported.

Temperature/DO/pH/salinity - Temperature, dissolved

oxygen, pH and salinity measurements are reported along with the range and mean of temperature.

6 of 7

Chemical Analyses - When chemical analyses are made to validate toxicant concentrations, the analytical method is reported as well as the results.

Residue observed in exposure chambers is described in the report.

~

10.

Testing Protocols - This protocol is referenced in the report.

11.

Deviations - Deviations from protocol or standard operating procedures are reported.

12.

Certification The Study Director and the QA Manager certify the final report.

RECORDS All raw data, data manipulations, draft reports and final reports will be retained by Aqua Survey, Znc. for a period of five years from the date of completion of testing.

Records will be surrendered to the sponsor upon their written request.

QUALZTY ASSURANCE This study will be conducted in accordance with the EPA Good Laboratory Practice Regulations (Federal Register, Volume 48, November 29, 1983) and Methods for Measuring the Acute Toxicity of Effluents to Freshwater and Marine Organisms EPA/600/4-85/013 March 1985.

7 of 7

0

CLAM-TROL CT-1 METHYLORANGE METHOD APPARATUS REQUIRED Beaker, glass, 50 mL (2 requfred)

Code

~*

Cylinder, graduated, 25 mL 2622 Funnel Rack, separatory 936 Funnel, separatory, with a Teflon stopcock, 250 mL ~~

(2 required)

Glass Rod 114 Optical Cell, (2 requfred)

Spectrophotometer GENERAL APPARATUS e 121 917 CHEMICALS REQUIRED 1, 2 - Dlchloroethane (reagent) grade or equivalent)

Code 1666 Cylinder, graduated, 100 mL Cylinder, graduated, 250 mL Flask, volumetric, 1 L, glass (4 required) 935 Plpet, glass, graduated, 1 mL 140 Plpet, glass, volumetric, 1 mL 866 Plpet, glass, volumetric, 3 mL OO Pipet, glass, volumetric, 5 mL 124 Pipet, glass, volumetric, 10 mL 123 Plpet, glass, volumetric, 15 mL 861 Plpet, glass, volumetric, 20 mL 0*

Pipet, glass, volumetric, 25 ml 117 Plpet, glass, volumetric, 30 mL SO

The general apparatus required for the test ls deter-mined by the specific test procedure used.

~~ Apparatus not available through Betz Lab Supply should be obtained through a local supplier.

CT-1 Buffer Reagent Methanol (reagent grade or equivalent)

Drying Reagent, with a plastic dipper

SUMMARY

OF METHOD 1591 GENERAL PROCEDURE Use a well-ventilated or hooded area to run the test.

Always use a safety bulb when pipetting liquids.

1.2 - Dlchloroethane (also known as Ethylene Dichlo-ride) is a priority pollutant and a specifically-listed RCRA-regulatedmaterial subject to specific disposal re-strictions and/or prohibitions. For this reason, all used 1,2 - dichloroethane should be segregated from other waste streams. Dispose ofwaste 1,2-dichloroethane in an approved manner (e.g., labpacking or incineration).

in this procedure the dye in the CT-1 Buffer Reagent com-plexes with the active ingredients in Clam-Trof CT-t. This complex is extracted into 1, 2 - dlchloroethane.

The or-ganic layer containing the complex Is separated from the aqueous layer and dried withadryfng reagent containing anhydrous sodium sulfate. The color intensity of the 1, 2 dichloroethane layer is then measured in a spearopho-tometer at 415 nm.

This method must be customized to each specific aopfi-catlon. Varythe volumes of sample, CT-1 Buffer Reagent, and 1, 2 - dichloroethane according to the test range (see Table 1). Ifa higher absorbance is needed. increase the volume of sample or decrease the volume ot t. 2-dichloroethane. When increasing the sample voiume it may be necessary to increase the volume of CT-1 Buffer Reagent used. For samples <150 mLuse 10 mL of CT-1 Buffer Reagent; for samples between 150 and 300 mL use 15 mL of CT-1 Buffer Reagent.

Make sure that enough 1, 2 - dlchloroethane is used to leave a small plug of solvent in the separatory funnel when the oottom layer of solvent is removed and to fill the ootfcai cell properly.

AP 368 9003 1990 BETZ LABORATORIES. INC. ALLRiGHTS RESERVED.

B-1 Page 1

I@hie 1. Suggested Volumes for Various Ranges of CT-1.

0.2-3.0 1.0 - 25.0 0.2 - 1.0 10 15 Range Volume Volume CT-1 (mg/L)

CT-1 Buffer Dlchloroethane (mL)

(mL) 15 10 Volume Sample (mL)

Optical Cell Size 10cm<<

2.5 cm '<<

50cm <<<<*

<<Thel.Lcm cell (Code 1312) can be used with Hach spectrophotometers using a 1~ cell adapter (Code 2776C).

<<>> The 2.&cm cell is the standard Hach 1-in. cell (Betz Code 2601).

Five centimeter cells are not available for use with the Hach photometers. Many laboratory spectrophotometers require an adapter to accommodate &cm cells. Check with the Instrument manufacturer.

1.

Transfer an aliquot of the water sample to a separa-tory funnel (the sample). Transfer the same volume of distilled (or deionized) water to a second separa-tory funnel (the blank). Run the blank once for each set of samples tested (see Notes 1, 2, and 3).

2.

Add CT-1 Buffer Reagent to both the sample and the blank.

3.

Using a plpet, add 1, 2-dichloroethane to both se-paratory funnels.

4.

Insert the stoppers in each ofthe separatoryfunnels.

Invert and briefly open the stopcock to vent the fun-nels (see Notes 4 and 5). When venting the funnels, point the tip of the funnel away from yourself and others.

5.

Shake the funnels moderately for 30 sec, vent the funnels, then allow them to stand for 10 min (but no longer than 15 min).

6.

Collect the lower layer (1, 2 - dlchloroethane) from each funnel in 5&mLbeakers leaving about 1-2 mL in the funnel. This willprevent significant removal of water.

7.

Using the plastic dipper, add 2scoopsof Drying Re-agent to each beaker and stir with a glass rod for 15 sec (but no longer than 30 sec).

8.

Wait approximately 1 to 2 min (but not more than 5 min). Then carefully decant the extract offofthe dry-ing reagent into an optical cell.

9.

Set the spectrophotometer at 415 nm and zero with 1,2-dlchloroethane. Measure andrecord the absor-bance of the blank and the sample (see Note 6).

10, The sample absorbance minus the blank absor-bance is used to determine the concentration of CT-1 in the sample.

From a prepared calibration curve, determine the CT-1 concentration in the sam-ple (see Calibration Curve Preparation).

11. Clean the cells after each measurement (see Note 7).

CALIBRATIONCURVE PREPARATION 1.

Prepare a 1000 mg/L CT-1 stock solution by accul rately weighing 1.00 g of CT-1 into 1 Lof distilled (or deionized) water.

2.

Pipet designated volumes of the stock solution into 1-L volumetric flasks. These are the standard solu-tions used in preparing a calibration curve. Use Table 2 to make appropriate dilutions of the stock solution for each specific app! Ication.

3.

Followthe General Procedure using the specific so-lution volumes that have been determined for the application and prepare a calibration cu!ve. Deter-mine the absorbance of a blank solution using dis-tilled (or deionized) water. Th!s blank can be sub-tracted from the sample absorbance or used to zero the spectrophotometer so that the calibration curve goes through the origin. The calibration curve should be linear over the indicated ranges.

NOTES 1.

For maximum accuracy the calibration curve should be checked by every operator using this test and shouldbe verified a minimum oftwice per monthus-ing a freshly prepared CT-1 standard.

2.

Ablank measurement must be recordedfor each set of samples.

The blank reading may vary slightly; however, the absolute difference between the sam-ple and the blank remains relatively constant.

3.

Chlorine causes a negative inter'.erence in the test.

This can be eliminated by adding 0.1 N Sodium Thiosulfate (Code 235) to the water sample before running the test. The amount added be is based on the concentration of chlorine in the system.

For a 1tXhmLwater sample containing 0.3 mg/L chlorine, add10 drops of0.1 N Sodium Thiosulfate to remove the interference.

Page 2 B-2 AP 3S8 9N3

Concentration CT-1 Desired (mg/L)

CT-1 Stock Solu-tion Added to Make 1 L (mL) 0.2 0.4 0.6 0.8 1.0 5.0 10.0 0.2 0.4 0.6 0.8 1.0 5.0 10.0 Table 2.

DIIutlona for Calibration Curve Prepara-tion Based on a FInal Solution Volume of1L procedure. Shake the funnel for 30 sec, vent it, then allow It to stand for 5 min. Gently Invert the funnel once then allow the funnel to stand for 5 min.

5.

It Is important to vent the separatory funnel bothbe-fore and after shaking it. Othetwise, a pressure will build up in the funnel that can cause the stopper to be forced out of the top of the funnel.

6.

Use caution when inserting or removing the sample cell in the photometer. The 1, 2-dlchloroethane can damage the cell compartment.

7.

It is imperative that the sample cells are kept clean during the tunning ofthe test. Itis recommended that the cells are cleaned after each measurement using the following procedure:

a)

Rinse the cell three times with distilled (or deionized) water.'5.0 20.0 25.0 15.0 20.0 25.0 b)

Rinse the cell three times with methanol.

c)

Rinse the cell three times with 1, 2 - dichloro-ethane to remove methanol from the cell.

4.

Aslight emulsionmay form whenuslng natural water samples.

When this happens, vary step 5 of the 8.

This method is basedupon Wang, L.K.;Langiy, D.F.

Ind. Eng. Chem.,

Prod.

Res.

Dev., 1975, 14, 3, 210-212.

AP 36S 9003 41990 BETZ LABQRATOIIIEJINC.ALLRIGHTS RESERVED.

Page 3

Pro ject No.:

9117891 LoB in No. :

7861 P.O.

No.

t Pending Oate

April 30, 1991 ANALYTICALOATA REPORT PACXAGE FOR Aqua Survey tnc.

499 Point Breexe Rd.

fletttington, NY 08822 ATTN:

REF)

Jiitt Todd l.ab Mater SAHPLE IOENTIFICATION LABORATORY NUHBER SAHPLE HATRIX SEE NEXT PAGE ME CERTIFY THAT THIS REPORT IS A TRUE REPORT OF RESUI.TS OBTAINED FRON OUR TEST'S OF THIS HATERIAL.

RESPE LLY SUB)tIT EO, I

EHV OHHEHT L INC PARAG X, SHAH, Ph 0.

ORGANIC LAB, NANAGER OIXI HEELEY ORY OIRECT R

/

J art¹ 73469 by~~ tO ~~IS) R<<)<<t o" sarnptets) obtarhett by us aopties onty tp IOt sarnpteO.

Intorrnatrort h

~~tpbe~t<<n~~~~by~O ~~~S 0Nls)~be~I<<~~~~at oateot report uruess speoriicaay reouestett o hervvrse by orient. In the event mat mere are ponens or pans ol samotels) rernarnrh9 att<<Nytest haa cornotetert me reourreo tests. )eytest snarl have me opuoh ot recumrnt) suah sarnptets) to me arertt at me <<ti<<trs eapense.

box l5l8 a 60 seaview blvd., port washington, ny 1 1050 a {516) 625-5500 C-1

LABORATORY NUMBER SAMPLE ZDENTZFZCATZON TYPE OF SAMPLE 7861001 7861002 7861003 LG SALT LG FRESH LP FRESH Water Water Water C-2

nytest enviIonmenta DATA RZPORTZiVG QUALITYEZRS U

Indicates compound was analyzed for but not detected.

Re ort the minimum detection 1'm't for the sample with the U (e.g.

>0 U ) based on necessary concentration dilut'on act'ors.

(Th's is not necessar'ly the ins ~ent detect'on 1 mit.)

he footnote should read U-Compound was analyzed or but no-detec ed.

The number is the minimum attainable detec" d "..'"

for the sample.

indicates an est'mated value.

This flag 's used e't'..e=

.~hen estimating a concentrat'on or tentatively 'dentif'ed compounds whe e a 3.:1 response is assumed or wnen t"..e -...ass spectral data ind'cates the presence of a co-ound tha"

=,e -'s the 'dent'ication c 'ter a but the result 's less t.".a..

speci ied detec"'ion limit but greate than ze=o (e.g.:

limit of detection 's 10 ug/1 and a concentration of 3 uc/

's calculated, repor" as 3J. )

This flag is used when the analy e 's ourd. in the bla."'~

as wel's a sample.

" 'ndicaies possible/probable

'".-.'(

contamination and. warns

='.".e data use= to - ke appropr'c" ion.

above he me"hod detec" io.". 1'm'ts.

1 a4 NA Th's lag indicates that the compounds a

not appc A

Aldol condensation product.

Note:

Data on soil samples expressed on a d y we'ght '"as's.

All non-water samples are reported on soil forms. Th's inc'udes samples whose matrix is lis ed as m'sce'ne us.

The initial and continuing calibration dates and t'mes ="r "he volatile fraction are 1's"ed on the BFB summary forms.

The init'al and continuing calibration dates and t'mes for "'.".e semi-volatile fractions are listed on the OFTPP summary orms'-3 00003

nytest environmental Report of Tests Water Suitability Test We find as follows:

The sample was analyzed according to Standard Methods for Examination of Water and Wastewater, 14th Ed.,

page 888.

Sample ZD:

LP FRESH Growth Ratio F 08 Lab ZD No.:

7861003 Remar.cs o

The sample is of acceptable suitability for the use in bacteriological testing.

A ratio greater than 3.0 would indicate growth promoting substances present in the water.

A ratio less than 0.8 indicates the presence of growth inhibiting subs ances.

C-4 00004

nytest environrnenl.al REPORT OF ANALYSZS Log Zn No. s 7861 Me find as Collows:

Parameter(s)

Sample Zdenti ication LQ SALT LC FRESH LP FRESH Method (7861001)

(7861002)

(7861003)

Blank pHSalinity, ppt 7.66 29 '

NA Results in mg/1:

Ammonia Nit ogen Bromide Fluor'de Zod'ne Nitrate Phosphate Residual Chlorine Sul"'de Sulfate Total Cyanide Total Suspended Solids 0.'30 40.8 0.576

<<0.04

<<0 '4

<0,

<<0.'0

~ Q'0

<<0.01 3

0'2

<0 1

<0.1

<0.05

<'.0

<0.02

<1

<0.04

<0.1

<0-10

< 1

<0.01

<1 ppt

~ parts per thousand C-5 00005

nytesl environrnenlal, REPORT OF ANALYSZS Log Zn No.:7861 Ne find as follows:

Results in mg/1:

Parameter(s)

WWWWMWWWM Sample Zdentification LG SALT LG FRESH LP FRESH Method (7861001)

(7861002)

(7861003)

Blank Aluminum A=senic Beryll'm Boron Cadmium Calc'um Chrcmium Cobalt Copper Z on Lead Magnesium Manganese Mercury Molybenum Nickel Potassium Selenium Silver Zinc Total Organic Carbon

<0 '

<0.010

<0.005 3.3

<0.005 271

<0.010

<0.05

<0.025

<0.050

<0.050 932

<0.015

<0.0002

0. 16

<0.040 348

<0.010

<0.020 20 '

11'3

<0. 010

<0.005

<0.025

<0.050

<0.0002

<0.040

<0.020

<0.2

<0.010

<0.005

<0. 1

<Q.005

<1.0

<0.010

<Q.05

<0.025

<0.050

<1.0

<0.015

<0.0002

<0.010

<0.040

<'.0

<0.010

<0.020

<1. 0 C-6

1 0-T NYTEST ENVIRONMENTAL INC.

TCL PESTICIDE/PC8 ORGANICS ANALYSIS OATA SHEET SAMPLE MATRIXt MATER CONC. LEVEL: LOU EXTRACTION GATEt 4/9/91 ANALYSIS OATE: 4/18/91 SAMPLE IOt LAB SAMPLE IOt OIL fACTOR:

X MOISTUREI UG/L I.G SALT 7861001 1.00 NA CMPO 4 CAS Nunber PESTICIOE/PCB CCKPIXJlQ I 319-84.6 2

) 3'19-&5-7 3

I 319 86-8 4

I 58-89-9 5

) 76-44-8 6

I 309.00.2 7

I 1024.57 3 8

I 959.98.&

9 I 60 57 1

10

( 72-55-9 11 I 70-20.8 12 I 33213-65-9 13 I 72 SC 8 14

( 1031.07-8 15 I 50 29 3 16 I 53494 70 5

\\7

) 72-43-5 18 I 57 74.9 19

( 8001-35 Z

20

( 12674-11-2 21 I 11104.28.2 22

( 11141.16-5 23

( 53469.21-9 24

) IZ672-29.6 25

) 11097-69-1 26 I 11096-82 5

I

) Alpha-BHC

( Beta-BHC

( OeLta.BHC

( Gamna-BHCILIndane)

( Heptachlor

( Aldrln

( Heptachlor Epoxide

( EndosuLfan I

( Oleldrin 4,4'-OOE

( Endrin

( Encosulfan I I 4,4 000

) EndosuLfan SuLfate 4,4'-OOT

( Endrin Ketone

( Methoxychlor

( Chlordane

( Toxaohene

( Aroclor-1016

) Aroclor.1221

( Aroclor-1232

( Aroclor-124Z

( Aroclor-IZC8

( Aroclor-1254

) Aroclor-1260 0.050 U.

0.050 U.

0.100 U.

0.'IOO U.

0.100 U.

O. IOO U.

0.100 V.

0.100 U.

0.100 V.

0.500 U.

1.000 U.

0.500 U.

0.500 V.

0.500 U.

1.000 U.

C-7 noo07

ORGANOPHOSPHOROUS PESTZCXDES Log in No.:

7861 Sample ID No.:

LG SAL=

Lab ID No.:

7861001 Parameters (ug/1)

Detec ion Limit (ug/1)

Found Vapona (Dichlorvos)

Phorate Diazinon Naled (Dibron)

Dementon -

S Disulfoton Ronnel Chlorpyr'os (Dursban)

Bolstar (Sulprofos)

Stirophos Fensulf othion Azinphos methyl (Guthion)

Coumaphos Malathion Parathion 0 2 0.2 0.6 0.2 0

2 0.2 0.3 0.3 0 '

2.0 5.0 1.5 1.5 0.3 0.3 ND ND iVD ND ND ~ Not Detected C-8 oooos

1 0-T NYTEST ENVIRONMENTAL INC.

TCI. PESTlCLDE/PCB ORGANlCS AMAI.YSlS OATA SHEET SAMPLE MATRIX: MATER CONC LEVEL: LOM EXTRACTION OATE: 4/9/91 ANALYSIS OATE! 4/19/91 SAMPLE l0!

LAB SAMPLE la:

01L FACTOR:

X NOLSTUREI Ua/l.

PBLK1 A040005 1.00 MA CNPO ¹ CAS Ntnker PESTlCIOE/PCS CDIPOIMO 1

I 2

I 7

(

8 I

9

(

10

(

11 I

12

(

13 I

14 15 I

16 I

18 19 I

Za

(

21

(

22

(

23

(

24 I

25 26 I

I 319-84.6 319-85-7 319.86.8 58.89-9 76.44.8 309-00-2 1024.57.3 959 98 8 60 57-1 7Z-55-9

70. 20.8 33213-65-9 7Z.S4.8 1031.07.8 50-29-3 53494.70.5 72-43-5 57-74.9 8001 35-2 1Z674. 11.2 11104.28 2

11141-16-5 53469 21-9 12672-29 6 11097-69 1

11096 82 5

( Alpha-BHC Beta-BHC

( OeLta BHC

( Canea-BHCLLindane)

( HeptachLor

( Aldrin

( Heptachlor Epoxide

( EndosuLfan I

( OieLdrin 4,4'-OOE

( Endrin

( Endosulfan ll I 4)4 aoo

( Endosulfan Sulfate 4,4~

OOT

( Endrin Ketone

( Hethoxychlor

( Chloraane

( Toxaanene

( Aroclor-1016

( Aroclor-1221

( Aroclor-1232

( Aroclor-124Z

( Aroclor-1248

( Aroclor.1254

( Aroclor-1260 o.asa u.

0.050 u.

O.OSO u.

O.asa u.

(

0.050 u.

0.050 U.

O.asa u.

0.050 U.

I 0.100 U.

I 0.100 u.

0.100 U.

I 0.100 U.

I 0.100 u.

0.100 u.

0.100 U.

I O.sao u.

O.SOO u.

1.aaa u.

O.Sao u.

O.S00 u.

O.SOO u.

(

O.S00 u.

1.000 U.

I 1.000 u.

I C-9 OOOla

ML17223B306

Text

SUMMARY

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