NC0000175_Testing Results_19990326

URIMIR
Quartz Operation
P. O. Box 588
Bakersville Hwy.
Spruce Pine, NC 28777
(828) 765 -4283
Fax: [phone]
March 26, 1999
Mr. David Goodrich
Chief, NPDES Unit
Division of Water Quality
NC DENR
512 North Salisbury Street
Raleigh, NC 27604 -1148
Dear Mr. Goodrich:
Thank you for the time which you spent meeting with us on Friday March 19th in
your office concerning our fluoride- bearing effluent, being discharged into the North Toe
River, Mitchell County. I am attaching to this letter the promised revised final version of
the Ceriodaphnia Dubia testing information which we reviewed in that meeting.
The three companies: K T Feldspar Corporation, The Feldspar Corporation, and
Unimin Corporation performed the Ceriodaphnia Dubia Acute and Chronic tonicity
testing to support their position that there should be no reduction in the total fluoride
poundage per day discharged by the three companies. The present limitation of 574
pounds per day of contained fluoride should be maintained without change.
We believe the above toxicity testing demonstrates that an in- stream waste
concentration limit of some seven parts per million fluoride would be protective of the
indigenous species in the North Toe River. That conclusion is based upon a chronic to
acute ratio of .20 (8 ppm chronic failure versus 40 ppm NOEC acute for Ceriodaphnia
Dubia) calculated from this testing. Applying that .2 factor to the 36.1 ppm F acute
toxicity rainbow trout limit provides an allowable waste concentration of 7.2 ppm
fluoride. That value is some 400% of the present North Carolina standard of 1.8 ppm F
and is about 175% of the 4 ppm fluoride limit allowed under the Federal EPA Drinking
Water Standard.
The above testing involved the water flea Ceriodaphnia Dubia, which is the
organism used for quarterly toxicity testing required for each company under its NPDES
permit. This testing included both chronic and acute toxicity determinations using state -
certified independent laboratories which routinely perform such testing. The tests were
performed using North Toe River water (the receiving stream), to remove effects which

a
might be due to the laboratory synthetic water called for in the quarterly test. The
protocol used for the test, including the designed fluoride doping levels, is attached.
The results allow calculation of a chronic to acute ratio based upon measured
response of the organism for which toxicity must be measured under the existing NPDES
permits. It allows replacement of an assumed chronic to acute ratio quoted in the June
1986 NC DENR report "North Carolina Water Quality Standards Documentation:
Toxicity of Fluoride to Fresh Water Biota ", which assumption was deemed to be
conservative even at that time. The new data clearly supports the companies' position
that the present standard is set artificially low at a level not substantiated by scientific
observation.
The new chronic to acute ratio described above utilized the most adverse data set
obtained from duplicate testing at the two entirely separate laboratories. Table 1 and
Chart 1 summarize these test reaft and Appendix 1 provides the detailed laboratory
results. In summary, the acute toxicity tests showed zero mortality at all fluoride
concentrations from 0.1 ppm up to and including 33 ppm F. In the chronic toxicity
testing, failures were observed at the 7.0 ppm and 14 ppm F levels.
The second lab's data are shown in attachments Table 2, Chart 2 and Appendix 2.
The acute toxicity data from the second laboratory confirmed zero mortality at all
fluoride concentrations, from 0.1 to 41.5 ppm F. On the chronic toxicity test, the second
laboratory shows a "Pass" at all levels, from 0.1 ppm through 15.9 ppm F. These results
would give a chronic to acute ratio of about .40. Application of this factor (.40 chronic :
acute ratio times 36.1 ppm acute trout level) yields an allowable fluoride in- stream waste
concentration of 14.3 ppm
To incorporate results from both of these data sets, the Average Reproduction for
Ceriodaphnia Dubia was itself averaged for each pair of observations at a given fluoride
concentration, and then compared to the averaged control reproduction. By this means,
the data shown in Chart 3 was obtained. In that case, a nominal 16 ppm fluoride chronic
toxicity level is obtained, as that is the only concentration at which an averaged "Fail"
result occurs. The resulting chronic to acute ratio would be about .4 (16 ppm/40 ppm),
and gives an allowable in- stream waste concentration of about 14 ppm F when applied to
the rainbow trout acute toxicity data previously referenced.
At this time, we are requesting that the NPDES permit fluoride poundage per day
be left unchanged. We believe the data clearly shows the status quo is fully protective of
the environment.
We will consider the potential for Site Specific Water Quality Standards, and look
forward to reviewing the draft document you mentioned. We may wish to explore that
approach, as well as rule making procedures, for the 2006 — 2010 permitting cycle which
will arrive sooner than any of us care to admit.

f
I
� s
I
• I
Once again, we appreciate the time provided by departmental staff in listening to
our proposal. We anticipate receiving your letter confirming DENR's g
strategy to allow for an order renewal of each of our individual NPDES permits.
Sincerely,
f
. I
Charles F. Stover
Regional General Manager
Unimin Corporation
I
i
cc: Forest Westall
Matt Matthews
Regional Supervisor
Aquatic Toxicology Group Leader
Water Quality Section)
Water Quality Section
Division of Water Quality
ND DENR
NC DENR
4401 Reedy Creek Road
29 Woodfin Place
}
Raleigh, NC 27607
Asheville, NC 28801
i
Joe Turner
Dennis Buchanan
Plant Manager
Plant Manager
The Feldspar Corporation
K T Feldspar
P. O. Box 99 I
P. O. Box 309
Spruce Pine, NC 28777'
. i
I
• i
Spruce Pine, NC 28777
r
i
I
I
I
• j
11
I
I
-

TABLE OF CONTENTS
Fluoride Toxicity Testing
Spruce Pine, North Carolina
February 23 — March 4, 1999
Description Page
Basis for Toxicity Testing 1
Chart 1— Chronic Toxicity (ETT Environmental) 2
Chart 2 — Chronic Toxicity (ETT and Burlington Labs) 3
Chart 3 — Chronic Toxicity (Average both Labs) 4
Table 1— Summary of Test Results (ETT Environmental) 5
Appendix 1— ETT Environmental data 6-10
(Chronic and Acute Toxicity data)
Table 2 — Summary of Test Results (Burlington Research) 11
Appendix 2 — Burlington Research data
Summary data 12-13
Chronic Toxicity Test 14-35
Acute Toxicity Results 36-55

1�AC'-.�-ts F-'-o 2..
CERIODAP11MA DUBIA AC11'R AND CRONIC TOXICITY TASTING
"NYL 1,51210
1. The successful bidder will collect North Toe River water from the river at Bent
Road, Avery County (immediately above the Spruce Pine Water intake at North
Carolina 19E bridge in Avery County). The water collected will be used to
adequately condition Ceriodaplinia prior to the testing outlined below, so that the
organisms are used to this water versus the synthetic water normally used for
North Carolina DENR chronic toxicity testing.
2. The successful bidder will collect the necessary North Toe River water(s)
necessary to perform the conditioning above, as well as the water required for the
acute and chronic tests specified below. The bidder should indicate whether one
single large sample of water to be split into aliquots as necessary to perform those
tests, or whether separate water samples are required in order to have sufficiently
fresh water for the entire testing protocol.
3. The successfid bidder will make up the various fluoride (F) concentrations
required for each of the 17 individual tests, and will also analyze and report the
fluoride concentration actually measured during each of those tests.
4. The 17 individual tests are set out below. The 0.1 ppm fluoride test is intended to
represent the background fluoride level within the river, and could be considered
to be a control on the experiment. The intent is that no fluoride be added to this
water, but that the actual fluoride concentration be measured and reported upon
by the successful bidder.
Acute Toxicity Testing 8 to Chronic Toxicity Testing (9 total)
0.1 ppm F (no fluoride added) 0.1 ppm F (no fluoride added)
5.0 ppm F 0.5 ppm F
10.0 ppm F 1.0 ppm F
15.0 ppm F 1.5 ppm F
20.0 ppm F 2.0 ppm F
25.0 ppm F 3.0 ppm F
30.0 ppm F 4.0ppmF
40.0 ppm F 8.0 ppm F
16.0 ppm F
5. The successful bidder will provide full written document on form AT1 or A13,
(plus bench sheets,} as appropriate for each of the 17 tests outlined above. Those
foams should include residual chlorine, pIT, dissolved oxygen, conductivity, F,
and any other parameters normally required under the North Carolina DENR
protocol.
6. The bidder is to provide all sample containers, coolers, chain of custody forms,
etc.
7. The successful bidder will provide all written results within 10 days after
commencement of testing of the Ceriodaphnia. (No later than 20 days following
issuance of purchase order).
8. All laboratory results are to be kept confidential and shared only with the client.
Page 1

Chart 1 - Chronic Toxicity
Reproduction vs. Fluoride Concentration
Reproduction vs. Fluoride
Concentration
25 M1. A
0 20
0 15
L
a
a�
--
a� 10
rn
�a
> 5
Q
0 4 8 12 16
Fluoride PPM
-*-- ETT
Page 2
7
ETT Laboratory
Fluoride
Average
Measured
Case
Reproduction
PPM
1
20.6
0.1
2
17.7
0.5
3
19.8
1
4
18.6
1.4
5
17.8
1.8
6
17.9
2.8
7
16.5
3.7
8
13.1
7.1
9
5.2
14
Reproduction vs. Fluoride
Concentration
25 M1. A
0 20
0 15
L
a
a�
--
a� 10
rn
�a
> 5
Q
0 4 8 12 16
Fluoride PPM
-*-- ETT
Page 2
7

Chart 2 - Chronic Toxicity
Reproduction vs. Fluoride Concentration
(2 Labs)
Reproduction vs. Fluoride
Concentration
Fluoride PPM
—a Burlington ---ETT I
12
16
Page 3
ETT Laboratory
Burlington Laboratory
Fluoride
Fluoride
Average
Measured
Average
Conc. PPM
Case
Reproduction
PPM
Reproduction
Measured
1
20.6
0.1
19.2
0.11
2
17.7
0.5
20.3
0.51.
3
19.8
1
15.4,
0.96
4
18.6
1.4
15.5
1.47
5
17.8
1.8
18.3
1.93
6
17.9
2.8
25.2
2.85-
7
16.5
3.7
22.6
3.86:
8
13.1
7.1
24.6
7.2
9
5.2
14
19.5
15.9
Reproduction vs. Fluoride
Concentration
Fluoride PPM
—a Burlington ---ETT I
12
16
Page 3

� r �
Chart 3 - Chronic Toxicity
Average of Both Labs
25
Reproduction vs. Fluoride Concentration
c
ETT
Burlington
Grand Averages
Fluoride
15
a
Grand
Grand
Design
Average
Average
Average
Avg. % of
PPM
Reproduction Reproduction
Reproduction
Control Reproduction
0
20.6
19.2
19.9
100%
0.5
17.7
20.3
19
95%
1
19.8
15.4
17.6
88%
1.5
18.6
15.5
17.1
86%
2
17.8
18.3
18.1
91%
3
17.9
25.2
21.6
108%
4
16.5
22.6
19.6
98%
8
13.1
24.6
18.8
94%
16
5.2
19.5
12.4
62%
25
Reproduction vs. Fluoride Concentration
c
20
0
15
a
10
m
L
a
5
0 1 1
0 4 8
Fluoride PPM
r
12 16
A Grand Avg. Reproduction
Page 4
■

r
TABLE 1. SUMMARY OF TEST RESULTS
Zemex Corporation Fluoride Testing of Ceriodaphnia Dubia
by ETT Environmental Inc.
2/23 - 3/4/99
Chronic Bioassav Test Results
Test Level Test Results Fluoride Concentration ma/L
0
Pass
<0.1
0.5
Pass
0.6
1
Pass
1.0
1.5
Pass
1.4
2
Pass
1.8
3
Pass
2.8
4
Pass
3.7
8
Fail
7.1
16
Fail
14.0
Acute Bioassav Test Results
Test Level Test Results Fluoride Concentration ma/L
0
>100 % LC50 *
<0.1
5
>100 % LC50
4.5
10
>100 % LC50
8.7
15
>100 % LC50
13.0
20
>100 % LC50
18.0
25
>100 % LC50
Not measured
30
>100 % LC50
24.0
40
>100 % LC50
33.0
* > 100% indicates no toxicity I.e. no mortalities
were observed at any concentration of fluoride.
Page 5

03/14/99 WED 10:45 FAX [phone] THE FELDSPAR CORP. QD005
Mir'- 2y4 -99 10:14A ETT Environmonta 1 . Inc. 664 077 0930 r.ara
'FTT Wc- I)ArT,4
M►irotrrrAw, hu. (864) 677.69612 • FAX [phone]
P.O. "1 16414, Gread ve. SC 299 4 Craftsman Court, Omer, SC 29650
Measured Fluoride Conuutratious
Zen= - N. Toe River Water Spiked w/ Fluoride
February 1999
Nomiml
Meaxyrad
Concenr►arfon
C OMvMtratfon
0.0
mg/L
<0.1
mglL
3.0
mg/L
4.5
nV/L
10.0
mg/L
8.7
mall,
15.0
mS/L
13.0
mg/L
20.0
nWL
11.0
mg/L
30.0
mg/L
24.0
mgt
40.0
mg/L
33.0
m&IL
2'•K) V-5/L gof v a0.s".*A . US r nic MaidrX Tem 7 �$I99
Nominal
Measurer!
Concentration
Cancentradon
0.0
mg/%
<0.10
mg/L
O•S
MIA
0.59
mg/L
1.0
tng/L
0.91
mg/L
1.5
mg/L
1.4
mg/L
2.0
mg/L
1.1
mg/L
3.4
mg/L
2.1
Ms/L
4.0
mg/L
3.7
mg/L
8.0
mg/L
7.1
mg/L
16.0
mg /L
14.0
mg/!.
Fluorides vmm measurM using Standard Methods 111i Edition SM 45MF C.
NC Certification No. 402.
Suhnitted By.
�1
Robeat W. Kelley, Ph.D.
Page 6
CO

•1q! -iJ -79 Vim. -7.?r
L! ! cllvIrunF119wrILS 1, InC. &304 Off
OVSU P.04
I
Effluent Aquatic Tonicity Report FomVPhase II Chronic
Ceriodaphnia
Facility: Zemex River Water
Spiked w/ Fluoride Pipes
County: Mitchell
Laboratory Performing Test
ETT Environmental
j
Comments:
sis� of
rerl UM of
II
Test Start pate Time
End Date Time
Info 2124!99 1900
03/04199 taw
Sample Information
s"pu 1
sample! cer"
son Days -DAYS
sue Dart oer6
Collection Start Date
212396
TreM�era1 16 mg& 16 16
camel scrAfel eo"
Grab
X
ON Uwl. 7.13 7.7s 7.37
7.14 7.38 7.60
Composite (Duration)
PH Pipe 7.66 7.91 7s1
7.42 7.50 7.32
Hardness (mg&)
0.0• n6 6.9 !.0 0.5
0.2 9.7 6.6
Spec Cond. (umhos.cm)
D.O.FNN 6.7 6.7 6.6
$A V 1A
Chlorine (mg&)
<0.05
Tamp Mai 262 75.2 24.2
241.2 25.2 2e.2
Sample temp. at Reeelpt
0.6
Tenor fine! 24.2 2S.2 24.2
24.2 25.2 24s
Chronic 'I set Results
FnM caw Me& %
0%
Organism 0
.x CON 3rd Mad
100%
1
.
1
2 3
4_ 5 6 7
8 9 10 11 12 wean
eo*a It"re ev
10%
Control S Young
23
23
20
ZS
19
19
19
23
21
lost
20.8
48 Hour Mortality
Adult 1L
iL
IL 1L
�L
�L �L
�L 1-1.
L
�L
Ilost
L
IL
canes rwre
100110 1 10 of 10
1
2 3
4 5 6 7
8 9 10 11 12 Meee
Significant? No
Emuent %
# Young
19
19
22
20 21
20
19
9
20
lost lost
17.7
Final Mortality Sign. Q
IL
IL
IL
IL #L
IL
ID81
IL
IL
�L IL
�
0.5mg/L
Adult
L
1 x
% e. No.canc. I I 1
Reoroductian Analyses
1
2 3
4 5 6 7
8 9 10 preen Repro LOEC=
Noe-c-
Frlhmt %
a Young
22
23 16
19
19
21
.20
21
17
.20 19.8 mefte
Ounnerf's T rest
IL
rkee Normal Dist?
yes Method saWmks
1.0 MOIL
Adult
L L
L
L
L
L
L
.
LL
4% statistic
Critical 0.930
Equal Varl
no Method maerm
1
.2 3
4 5 6 7
8 .9 10 mw - Statistic
Critical 15.10
Effluent 'x
#Young
18
17 19
16 20
19
19
19
19
20
'`8.6 t -Test
I
IL
I I
I
WrAd.
1
�t
1.4 MWL
Adult
L L
L L
L
L
L
L
L
10% Etfuent %
_ Critical
1 2 3 4 5 6 7 8 9 10 mow
.01(tent .% j# YoU"Q
I 1 Adult 1 I I I I MY
011eaatt:Argt+istr+�; ••
1 2 3 4 5 6 7 8 9 10 Wean Retlillf t PAS9ii1L br
Effluent % Young
17'ast LDE6: '`:'
i
Adult� I , , I.Cliconialralrie -..
-MAIL Environmental Sciences
TO: Div. of Environmental Management
N.C. Dept of EHNR
4401 Reedy Creek Rd.
Raleigh. NC 27607
DEM Form AT -3 Rev, 1ims
NOEL= ,.
Page 7 6 7
ennR 'd)T00 )TFdsQ-T33 HU COZO 99L tOL JY3 ZS:LO 3172 66/9T/CO

03/16/99 TUE 11:49 FC.T 704 765 0203 THE FELDSPAR CORP. 16002
M8r- Aft -99 11:46A ETT Environmental, Inc. 864 877 6938 P_01
Effluent Aquatic Toxicity Report Form /Phase II Chronic Ceriodaphnia.
Facftr- Zemex River
wader Spited vd Fluoride (Revised w/ Measured Concs.)
County: Mitchell
laeorato Test
ETT Environmental
Comments:
uns of
spnaurs IN
Test Start Date Tma
End Date Time
Info 2124/99
1800
03104/99 1800
Sample Information
swow 1
sw vw 2
L mm
SM
0.,2 oars
sun D.r2 Ono
Collection Start Date
W23M
Tro n ant 14 ffWL
14 14
r"*w w"Im cmdm
Grin
X
P" Ink. 7.13
7.23 7.37
7.10 7.36 7.00
Composite (Duration)
PH Fmt 7.56
7.61 7.66
7.42 7.60 7.32
Hardness (mg/L)
D.O. ink e.3
9.0 8.5
9,2 e.7 9.6
Spec. Cond. (umhos.cm)
O.C. Flnel 5.7
e,7 s.s
6.5 a.7 s,a
Chlorine (mg/L)
00.05
Temp Ink 242
2S2 24.2
24.2 25.2 2412
Sample temp. at Receipt
0.5
Tamp Final 24.2
2S.2 24.2
24.2 25-2 24,2
Chronic Test Results
fhnah cea MGM. %
0%
Organism a
% CaN 3M e1001
100°/Q
1
2 3 _
4
5
fi _ 7 _
8
_ 9. 10 11
12 mom
C&wW RWO CV
10%6
Control
# Young
231
231
20
18
19
19
19
23
L
21
lost
IL
lost
20.6
48 Hour Mortality
Adult I
L
L
LILILILILILIL�LIL
I-
ce,ww nwc
of 10 10 Of 10 1
1
2 3
4
5
6 7
8
9 10 11
12 _Mean
Significant? No
Ef kmrt %
# Young
17
111
19
1$
17
16
20
19
17
19
IOst
Final Mortality Sign,
IL
1103ti17.81
X Rao
M 1.8 mgll
Adult
L
L
L
L
L
L
L
L
L
L
L
13%
or I No. conc, I
ReDroduction
AnaNses
1
2 3
4
5
6 _ 7 _
8-
9-10-m=m
Repro LOEC= 7.1 mg/L wocc■ 3.7 mg/L
Effluent %6 # Young
1191211111121120119117122
21201-17.9
Method:
Ounnett s T Test
I
I
#A Roo
Normal Dist?
yes Method snwmu
12.8 mpn.. Adult
L
L
L
L
L
L
L
L
D
L
13%
Statistic
0.961 Critical 0.930
Equal van
no Method motto&
1
2 3
4
5
6_ 7
8
9 10 mew
Statistic
19.20 Critical 16.10
Effluent 96
16
8
2111011111151
23
21
17
18
16.5
t -Test
10Younpj
x Red—
Maned:
DLrrAMS
3.7 m
Adult
L
L
L
L
L
L
L
L
L
L
N%
Effuent In
t Crnk�1
1.8
1.50 2.39
1
2 3
4
5
6 7
8
9 10 Moan
2.8
1AS 2.39
Effluent %
# Younq
11113
B
14
17
11
17
18
6
18
13.1
3.7
2.21' 2.39
1
w nw
1.1
a,ua 11 AV
17.1 mg/L
Adult
L
L
L
L
L
L
L
L
L
L
36%
14
8.37 2.39 ,
gywralll Artatrals
1
2 3
4
5
6 7
8_
9 10 Mean
Result = PASSfFAIL or
Effluent %
# Young
7
1
1
12
3
3
10
7
ILBIL
2
_ 5.2
Test LoEC:
7.1 rnWL NCEC= 3.7 mg/L
14 m9/L
I Adult
I L
I L
I L
I L
IL
I D
I L
I L
75%6
Chronic values 5.1 m /LL
MAIL En*orinental Sciences
TO: Div. of Environmental Management
N.C. Dept. of EHNR
4401 Reedy Creek Rd.
Raleigh. NC 27807 OEM Form AT-3 Rev. 11/95
Page 8
611

03/$4/99 WED 10:44 FAX [phone] THE FELDSPAR CORP.
Mav- -a4 -99 10;13A E'rT Environrnantal, Inc- 864 suer oysss .-_..� f�003
lrontetetthl. Ina.
P.O. Box 161141 Or"11 -008. SC 29606
[phone] - FAX (884) ST74938
4 Craftsman Court, Greer, SC 29650
Client:
Feldspar
5
0
Simple ID:
Zemax
Lab IDt T11364
Stare Darr:
2/24/99
Time:
1800
Set By:
Sc
Test Species.
�CeNodapkais
End Date:
0
2126199
Time:
1880
Ended By:
RK
labia
cw�1W �.of
C
5
0
0
uitution water: MH$F
PH
ra w
MORTALITY DATA
7.42
WATER QUALITY DATA
Measures
0
4
Cumulative Mortality
Mean
,.r
Mnsurod Value
Re0•
'Vwi w
34hr Oft 7W ear
RN
Paamctcr
units
on 7+M aW Tau why
mall.
A
3
0 0
8.7 mg/L
Mewed
mg/L r`mew
8.6'
<0. t mWL
9
5
0 0
00/1,
thypa
MVL P— „..1
9.5
C
C
5
0 0
PH
r.,....a
7,16
D
S
0 0
5
0
0
7.19
STATISTICAL ANALYSIS
"Nominal concentration,
48 Hour LC50 > 33 moll. effluent All concentrations are expressed as measured concentrations
95% Confidence Limits: Upper. NA except the 25 mg& concentration for which no measured
Lower. NA concentration was available.
Method: Spearman Kerber
COMMENT& Approved By:
Date: 9 *Jq� 7
Page 9
A
5
0
0
Diuulvcd
MX&
P--
8.8
4.5 tng/L
S
5
0
0
06/6
Oxygm
mWL
„a,.w.”
9.4
cw�1W �.of
C
5
0
0
PH
ra w
7.42
D
5
0
0
,.r
7.09
A
5
0
0
'
Dissolved
mall.
rr. ne.wf
9.9
8.7 mg/L
B
5
0
0
00%
Oxygen
mt/L
2
("M; l ,a o)
C
5
0
0
PH
ere+ar.d
7.26
D
5
0
0
,.„..,
7.14
A
5
of
0
Msoived
mtlL
6,7
13 mg/L
51
01
0
0%
0xyso
9,0
IharlW ls.o�
0
Oj
0
PH-
p,.,a,,.r
727
D
5
0
0
,,.,,..
7.17
A
5
0
0
l7is50lved
MWL
M. +.rw
8,7
18 mg/L
B
5
0
0
06A
Oxygen
m
,..e.o
9.2
(Dow" ».o)
L
5)
0
0
PH
r
7.64
D
5
0
0
�.,,...n
7,09
A
S
0
Dissolved
M6l1.
VL
a,4
25 mg/L•
B
5
0
0
0%
C*rr n
,n VL
(nominal)
C
$
0
0
PH
r.,....t
7.91
D
5
0
0
�.
o.,,,am. w
7.311
1
STATISTICAL ANALYSIS
"Nominal concentration,
48 Hour LC50 > 33 moll. effluent All concentrations are expressed as measured concentrations
95% Confidence Limits: Upper. NA except the 25 mg& concentration for which no measured
Lower. NA concentration was available.
Method: Spearman Kerber
COMMENT& Approved By:
Date: 9 *Jq� 7
Page 9

03624/99 SPED 10:45 F.Al 704 785 0203 THE FELDSP -4A CORP.
"Av-- Z4 —99 10:13A ETT Environmental , Inc. cod* Or i oyssa �I 004
ETAMMINIMM
-— t
nwrafmafttal, lee. (864) M-6942 • FAX (864) 877 -SON
P.O. Om 16414, OtwrMIG, SC 2SGOG 4 Craftsman Court, Gnu, SC 2MO
Clieat: Feldspar
Start Date: 2114/99
Ind Date: 2126199
Siunpic 1D., Zemoz Lab 113# T11364
Time: lx00 Set By: SC Test Specim.
Time: 1400 Frded 8 : RK �C- r/odAPhNla dvM
iili11%=LaM-. KIISF
MORTALITY DATA
Msaseres # Cunwlstivc Morwiry Merl
ROIL --rd 1, 7ar +w 7M %k Pik 'par�mtler
S 0" 0 Dissolved
24 mg/L 8 5 0 0 0% Oxygen
r.,,,;,w.00► C 5 0 0 PH
D 5 0
0
A S 0
0
33 mg/L B 5 0
0
C 5 0
0
p 5 0
0
B
C
m=/l-
D
1.7
A
a
C
PM K.,.a
7.52
8
min,
C
11
Mg&
B
2.6
C
D
STATISTICAL ANALYSIS
49 Hour LC50 > 33 MVL
effluent
95°X. Confidence Limits:
Upper. NA
ms/t.
Lower. NA
Method- Spearman Karber
COMMEnrra:
am
Diswlved
0% Oxygen
PH
Dissohee
Omen
PH
Dimivcd
Oxytcn
PH
Dissolved
Oxygen
PH
t?issolved
Oxyygr
P11
WATER QUALITY DATA
Messurcd Value
Writs
Ok 34k
.Wr 7M Pik
me/L
m=/l-
pwa emwa
1.7
�..�
724
PM K.,.a
7.52
min,
1
11
Mg&
PMMVM -W
2.6
p�rww.a
7.31
po-nnevM
7.57
ms/t.
mg/i.
am
pie
MI/L
PM-M—w
MSIL
pw..rr�.al
ms/t.
soe.1016
mp/L
Pon.rawnr
pc�ew.tl
pow -tared
0151Ly
mWL
rM.-M -r
Per
'Nominal concentration.
All concentrations are expmsssed as measured concentrations
except the 25 mg/L concentration for which no measured
concentration was avaitabk.
Approved By: 12 QG�/
Due: 7-24-17
Page 10
ID

MAR 04 199 04 :14PM BURLINGTON RESEARCH P.2/2
Aquadc Bioassay Tesdng • Aqualo ToxWV Reduction Evaluations
Chemical Produd En*onmer%W Assesstnonts • NPDES Teaft
Roporang A Data Handling Sarvkas
BURLINGTON 1302 Belmont Street * Burlington, NC 27215 -6935 • Phone [phone] • Fax [phone]
RESEARCH - —
Ls Z S V m mp v `( g2j P-- -' AMT �muvrl
Unimin Corporation Fluoride - Testing
2/24 -=199
Qhronla Bioassav Test Results
Test Level
0
0.5
1
1.5
2
3
4
a
16
Acute Bloassai
Test Level
0
5
10
15
20
25
30
40
Test Result
Pass.
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
r Teat Res=
Test Result
>100 °% LC50 }
>100 % LC50
>100 % LC50
>100 % L050
>100 % LC50
}100 % LC50
>100 % LC50
>100 % LC50
Fluoride Concentration mo/4
0.11
0.51
0.98
1.47
1.93
2.89
3.86
7.2
Fluoride Concentration ma/L
0.11
6.24
10.4
15.9
20.8
27
30.5
41.5
* > 100% indicates no toxicity i.e no mortalities
were observed at any concentration of fluoride.
Page 11
Wafer ErwlronrnonW Services - Eden water Em*onene W Sembas - Kinston it
Dkislon of W ftton Research, In*. Page 1 Otvision of Buft om Research, me
370 W. Meadow Road • Eden, NO 272M 100 E Gordon StreO • Kinston, NO 28501
Phone [phone] • Fax [phone] Phone [phone] • Fax [phone]
rR W"

i
MAR 04 199 04 :13PM BUZL_INGTON RESEARCH P. 1/2
.., TO I NIMIN QUARTZ
ct
1'pga x 2, RaL7friw,4 WrA
FAX Transmission. Sheet
Burlington Research, Inc.
1302 Belmont Street
Burlington, NC 27215 -6935
Phone: [phone]
FAX: [phone]
FAX ONLY
DATE: March 4, 1999
TO: Roy Rittle
COMPANY: Unimin
FAX #: [phone]
FAX & MAII,
<5() MM'P1'2-Y
ROPM7
GkA-V-ICWC
ALVT E
-Toxic Y
FROM: John Bau comer, BRl Biomonitoring Lab Manager
SUWECT: Completed reports
You should receive 2 pages cludi this cover sheet V you do not receive all page; or
have a question regarding content please call me at 9101570 -4661, Fat: 289
COMMNTS:
Roy:
Completed table
Questions, Please call
ELM
Page 12

MAR 04 199 04s14PM BLRL.INGTON RESEARCH
I R
mi
BURLINGTON
RESEARCH
aka w
Aquatic Bioassay Testing • Aquatic Toxicity Roduction Evaluations
Chemicei Product Environmental Assessments • NPDES Testing
Reporting A Data Hmm" Sarvlcas
P.2 /2
1302 Belmont Street • Burlington. NC 27215 -6935 • Phone [phone] • Fax [phone]
Unimin Corporation Fluoride - Testing
=4 -33/99
ChmnlcBloassav Test Result1
Test Level
0
0.5
1
1.5
2
3
4
8
1a
TIM, Result
Pass.
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Acute Bioassav Test Resuft
Test Level
0
5
10
15
20
25
30
40
Test Result
>100 % LC50
1100 % LC50
>100 % LCSO
>100 % LC50
>100 % LC50
>100 % LC50
>100 % LC50
>100 % LC50
Fluoride Concentration mold
0.11
0.51
0.98
1.47
1.93
2.89
3.86
7.2
Fluoride Concentration mg1L
0.11
6.24
10.4
15.9
20.8
27
30.5
41.5
* > 100% indicates no to)dclty 1.e no mortalities
were observed at any concentration of fluoride.
Water Environtnen al Servi a -Eden
Division of Burtinplon Research, Inc„
370 W. Meadow Rood • Eden, NO 27286
Phone [phone] • Fax [phone]
Page 13
Water Envirorrner►td SwAces -Kfmm
Page 1 Wagon of Burlinam Reeearch, Inc.
100 E Gordon Street • Kinston, NO 29501
Phone [phone] • Fax [phone] ) Z

. w MAR 64 177 02:46PM BLIRLINGTON RESEARCH
TO UNIMIN QUARTZ
&I
FAX Transmission Sheet
Burlington Research, Inc.
1302 Belmont Street
Burlington, NC 27215 -6935
Phone:VM70 -4661
PAX: 9101584 -5305
FAX ONLY _X�
DATE: March 4, 1999
TO: Roy Rittle
COMPANY: Unimin
FAX #:
FROM:
828-765-0912
33
o
FAX & MAIL
Cl�2eN�C_
-MM(IkT I
John Baununer, BRI Biomonitoring Lab Manager
P. 122
SUBJECT: Completed reports
You should receiva pages wig this cover sheet jyyou do not recelve all pages, or
have a question regarding content, please call me at 91 4661, Fa. 289.
coMNIEnrrs: �y
Completed reports
Questions, please call
John
W
f
i
t"e;
rhAA69,
Page 14
1 i

MAR 04 '99 02 :46PM BURLINGTON RESEARCH
BURLINGTON
RESEARCH
■■A 1AY
Aquatic Bioassay Testing lb Aquatic Toideity Reduction Evelusilom
Chwnical Product Environmental Assessmanb • NPDES TsOny
Reporting A Data Handling Services
P.2/22
1302 Belmont Street a Burlington, NO 27215-6933 • Phone [phone] a Fax [phone]
March 4,1999
Uni nin Corp
P.O. BOX 588
Spruce Pine, NC 28777
Attention: Mr. Roy Rittle
Enclosed please find the reports for your samples received 02/24/99, assigned
to BRI Workordcr 9B607. Please call if you have any questions.
Thank you.
Water EnM wew to Services • Eden
Division d Burlington Reaaarch, Inc.
870 W. Meadow Road • Eden, NO 27288
Phone [phone] • Fax [phone]
Sincerely,
BURLINGTON RESEARCH, INC,
ohn C. Baummer,
Manager, Biomomtoring Dept.
[phone] EzL 289
Page 15
Water Errviroruma W services • Kinston
Division d 9u ftion Research, Inc.
100 E. 0ordon street • Kinston, NC 28601 lg,
Phona [phone] • Fax [phone]

MAR 04 '99 02 :46PM BURLINGTON RESEARCH P.3i22
Aquatic Bioassay Tasting • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments a NPDES Testing
Reporting & Data Handling Services
BURLINGTON 1302 Belmont Street • Burlington, NO 27216.6935 • Phone [phone] • Fax [phone]
RESEARCH
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: Mr. Roy Rittle
SAMPLE DESC: FEB. MONITORING
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 02/24/9911:30 SITE: 0 ppm
I PARAMETER
Fluoride YC Analysis
EPA 300.
Ceriodaphnia Pass/Fail Chronic
NMEM 9/89
WORK ORDER #s
9B607.001
RECEIVED:
02124/99
REPORTED:
03104/99
PO NUMBER:
DATEMME/ANALYST MOL
Started 03/02/9911 :53 0.10
Analyzed 03/02/99 by TAR at BRI - Burlington
Started 02/24/9914 :00 N/A
Analyzed 03/04/99 by 1C.'B at BRI - Burlington
MQL = Minimum Quantitation Limit
RESULT
0.11 mg/L
Pass Pass/Fall
Page 16
Water Envirormantal Servlcee -Eden Page i Water Enrironmantal Ser*u - Kinston
Division d Burlington Research, Ina Division of Bwlington Research, Inc.
370 W. Meadow Road • Eden, NO 27288 100 E. Gordon Street • Knston, NO 28501
Phone [phone] • fax [phone] Phone [phone] a Fax (252) 62o -9922 1 S
tk! 1Ap

MAR 04 '99 02 :47PM BURLINGTON RESEARCH P.4/22
Effluent Toxicity Report Form - Chronic Pass /Fail and Acute LC50 Dates 03 /04/99
Facilitys FLUORIDE SAMPLES NPOEWS NC Pipedts Countys MITCHELL
Laboratory performing Tests BURLINGTON RESEARCH. INC.
Comments: 0 PPMs North Toe River
V
fi ture of Operator in Responsible Charge m = mole
S na ere of La story fupervisor * PASSCOS -8.682 Reduction
work Orders 98607 -001 Environmental sciences Branch
MAIL ORIGINAL Tot Div. of Environmental Management
N.C. Dept. of EHNR
4401 Reedy Croak Road
Raleigh, North Carolina 27607 -6445
North Caroltns Ceriodaphnia
Chronic Pass /Fail Reproduction Toxicity Test Chronic Test Results
Calculated t a •0.757
Tabular t ■ 2.518
CONTROL ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12 X Reduction u •8.68
8 Young Produced 12 11 24 20 19 21 28 19 M 15 12 13 % Mortality Avp.Reprod.
0.00 17.64
Adult (L)tve Mead L L L L L L L L L L L L Control Control
0.00 19.17
Treatment 2 Treatment 2
Effluent Xt 1002
TREATMENT 2 OROAMISMS 1 2 3 4 5 6 7 8 9 10 11 12 Control CV
31.29iX PASS FAIL
A Young Produced 21 15 21 24 17 21 18 23 22 21 9 18 % control orpe
producing 3rd il
b
Adult (L)ive (D)ead L L L L L L L L L' L L L road 83X ; Check q0m
1st somplo
PH Control 7.59 7.921
Treatment 2 7.30 7.941
s
t a
s n
r d
t
1st sample
1st sample
7.46 7.16
7.60 7.21
s
t e
a n
r d
t
1st sample
2nd sample Complete This For Either Yost
Test start Dates 02/24/99
7.4317.311 Collection (start) Date
Sample 11 02/24/99 Sample 21
6.86 7.41 Sample Type/Duration 2nd
1st P/F
a Grob Comp. Duration D
t e t a B
a n Sanple 1 X hrs L A A
r d U M M
t sample 2 hrs T P P
2nd ample
D.O. - - Nardness(mp/l) 40 ', {;r,�#'• is < #j- -
Control 8.7 9.4 8.7 18.4 116.1 8.5
Spec. Cond.(pmhos) 85 40.5
Treatment 2 a.0 18.2 8.7 8.3 8.4 8.5
LC50 /Acute Toxicity Test Sample temp. at reeeipt('C) "`:`.fib 3.2
(Mortality expressed as X, combining replicates)
Notes Please
X 11 X % % % II 11 X % Concentration Canptat* This
% % % % % X % % % % Mortality section Also
start /and start /end
LC50 % Method of Determination Control
95X Confidence Limits Moving Average Probit _
x --
___.X spearmon Kerber :: Other High
eons.
PH D.O.
MOrganise Tasteds Ceriodaphnis dubia Duration(hra)S Page 17
Copied from DER form AT -1 (3/87) rev. 11/95 (DUBIA ver. 4.32)
16

MAR 04 '99
BURLINGTON
RESEARCH
02 :47PM BURLINGTON RESEARCH P.5/22
Aquatic Bloomy Testing • Aquaft Twl 1y Reduction EvalUatione
Chaff" Product Environmental Assessments • NPDES 7604
Reporting A Data Handling Services
1302 Belmont Street • Burlington, NC 27215 -8935 Phone [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: Un3min Corp.
REPORT TO: fAr. Roy Rittle
SAMPLE DESC: FEB. MONITORING
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 02%24/9911:35 SITE: 0.5 ppm
PARAMETER
Fluoride VIC Analysis
EPA 300
Ceriodaphnia PawTail Chronic
NCDEM 9/89
DATE/TIME/ANALYST
WORK ORDER #: 9B607402
RECEIVED: 02/24/99
REPORTED: 03)04199
PO NUMBER:
MQL RESULT
Started 03102/9911:53 0.10
Analyzed 03/02/99 by TAR at BRI - Burlington
Started 02/24/9914:00 N/A
Analyzed 03/04/99 by 7CB at BRI - Burlington
MQL - Min1muin lQuandtation Limit
0.51 VIA
Pass PauMail
Page 18
Waver En*wmsnW SeMae - Eden Page 2 Water Erwironmen%l S#Mcee - Kinston
Olvision of Burlington Research, Inc. Division or &A"ton Research, hr.
970 W. Meadow Road • Eden, NO 27288 100 E Gordon Street • Kinston, NO 28601
Phone [phone] • Fax [phone] Photo [phone] • Fax [phone]
ssr
to" 17

MAR 04 '99 02 :47PM BURLINGTON RESEARCH
Effluent Toxicity Report Form - Chronic Pass /Fail and Acute LC50
Facility: FLUORIDE SAMPLES NPOESS: NC Pipmih
Laboratory Performing Test: BURLINGTON RESEARCH, INC.
Comments: 0.5 PPM e ■ aisles
Date: 03/04/94
County] MITCHELL
X
signature of Operator in Responsible Charge
X
s, tore of Laboratory supervisor * PASSED: -5.91% Reduction
Vark orders 98607.002 Environmental Sciences Branch
MAIL ORIGINAL TO: Div. of Environmental Management
N.C. Dept. of ENMR
4401 Reedy Creek Reed
Raleigh, North Carolina 27607.6445
North Carolina Ceriodaphnia
Chronic Pass /Fail Reproduction Toxicity Test Chronic Test Results
Calculated t * -0.700
Tabular t ■ 2.528
CONTROL ORGANISM$ 1 2 3 4 5 6 7 8 9 10 11 12 X Reduction ■ -5.91
% Mortality Avg.Reprod.
M Yaung Produced 21 15 21 24 17 21 18 23 22 21 9 18
0.00 19.17
Control Control
Adult (L)Ive (Wood L L L L L L L L L L L L
0.00 20.30
Treatment 2 Treatment 2
Effluent X1 100X
TREATMENT 2 ORGANISM$ 1 2 3 4 5 6 7& 9 10 11 12 Control CV _
21.550% PASS FAIL
9 Young Produced 22 18 17 23 23 24 16 16 M N 20 24 X control arcs pCheck producing 3rd
brood gone
Adult (L)ive (D)ead L L L L L L L L L L L L 100%
1st sample let aaepls 2nd sample Complete This For Either Teat
PH Test start Date: 02/26/94
Control 7.30 7.94 7.60 7.21 6.86 7.41 Collection (start) Data
Sample 1: 02/24/99 sample 2:
Treatment 2 7.22 7.48 7.40 7.21 6.83 7.40 Sampla Type/Durstton bid
tat P/F
s s a Grab Comp. Duration D
t e t e t e I S s
a n a n a n sample 1 X bra L A A
r d r d r d U N N
t t t sample 2 bra T P P
tat apple let ample Znd sample
0.04 Nardness(mg /l) 40
Control 8.8 18.2 8.7 18.3 8.4 18.3
$Pee. Cond.Whos) 85 42.8
Treatment Z 8.8 8.2 8.7 8.3 8.4 8.7
Chlorine(mg /l) :fit ?:; n/a
LC50 /Acute Toxicity Teat Sanple temp. at recelpt(•C) OtV "V 3.2
(Mortality expressed as X, combining replicates) ,
Note: Please
X X X X X X X X X X Concentration Complete This
X X % % % X X % % X Mortality section Also
start /end start /end
LCSO % Method of Determination Control
95X Confidence Limits Moving Average Probft
-�. _x -• _ +X Spearman Kerber Other _ high
Cone.
PH D.O.
Organises Tested: Cerlodsphnia dubia Ourstiah(hra)s N
Copied from OEM form AT -1 (3/87) raw. 11/93 (DUBIA ver. 4.32)
P. 6/22
Page 19
1�

MAR 04 '99 02r4EF'M BURLINGTON RESEARCH P. 7/22
Aqustb Bbassay Tasting • Aquado Taxleity Raduodon Evalua!lona
MR I Chemical Product EnYronmental Assessmanls • NPDES ThUng
FiepoNng A Data Handling 8mvicas
BURLINGTON 1302 Belmont Street • Burlington, NC 27215 -6935 9 Phone [phone] • Fax [phone]
RESEARCH
ANALYTICAL REPORT
CUSTOMER: Unim3n Corp.
REPORT TO: Mr. Roy Rittle
SAMPLE DESC: FEB. MONITORING
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 02,r2419911:40 SITE: 1 ppm
IPARAMETER
DATEITIMEIANALYST
WORK ORDER #: 9B607 -003
RECEIVED: 02/24/99
REPORTED: 03/04/99
PO NUMBER:
MOL RESULT
Fluoride by YC Analysis Started 0310219911;$3 0.10
EPA 300.6 Analyzed 03/02/99 by TAR at BRI - Bullngton
Ceriodaphnia PasOail Chronic Started 02/24/99 14:00 NIA
NMEM 9189 Analyzed 03/04/99 by JCB at BRI - Burlington
MQL = Minimum Quantitation Limit
0.96 mg/L
Pass Pasoall
Page 20
Water ErwiravatW SeMw - Eden Pap 3 Water EnvfronmanW Services - Kkulon
Division of Burlington Research, Inc. Division of SurOnglon Research, Inc.
310 W. Meadow Road • Eden, NO 27288 100 E. Gordon Street • I(inaton, NO 2001
Phone [phone] • Fax (338) &23.5878 Phone (252) 52HO21 • Fax (252) 52MG22
eras uM
I°

MAR 04 '99 02 :48PM BURLINGTON RESEARCH
Effluent Toxicity Report Fora - Chronic Pass /Fail and Acute LC50 Patti 03 /04/99
Faoilitys FLUORIDE SAXPL911 NPOESEI NC Piperla Countya 14i7CRELL
Laboratory Performing Tests BURLINGTON RESEARCH, INC.
Cemnenta: 1.0 ppm sa ■ asilss
X
Signsture of Operator In Responsible Charge
Ignature of La ratory Supervisor --*._PASSEDs 19.42% Reduction
York Orders 95607.003 Envlrow*ntal Sciences Branch
MAIL ORIGINAL TOi Div. of Ernrironmental Management
N.C. Dept. of ENNR
4401 Reedy Creek Road
Rateiph, North Carolina 27607.6445
North Carolina CeriodophnI4
Chronie,Pass /Fail Reproduction Toxicity Teat Chronic Test Results
Cslculeted t s 2.337
Tabular t ■ 2.539
CONTROL ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12 % Reduction ■ 19.42
I
0 Young Produced 21 15 21 24 17 21 18 23 22 21 9 18 X Mortality Avg.Reprod.
0.00 19.17
control Control
Adult (L)iva (0)ead L L L L L L L L L L L L
0.00 15.44
treatment 2 Treatment 2
Effluent XI 100%
TREATMENT 2 ORGANISMS 1 2 3 4 5 6 7 3 9 10 11 12 Control CV
21.3502 PASS FAIL
9 Young Produced ti 14 18 110'16 13 18 A 3 -l8 X control orgs
v br
producing 3rd
ood
Adult Wive Mood L L L L L L L L L L L L 100% Check One
let sample 1st swiple 2nd sample Complete This For Either Test
pN Test start Dates 02/24/99
Control 7.3017.94117.6017021116. Collection (start) Date
Bample 1s 02/24/99 Sample 2s / /
Treatment 2 7.16 7.33 7.28 T.11 6.78 7.33 Sanpte Type/Duration 2nd
1st P/F
1 18 s Grab Carp. Duration D
t e t e t e I 8 S
a n a n a n Sample 1 X hrs L A A
r d r d r d U M N
t t t Seapto 2 hrs T P P
lot sample let sample 2nd sample
D 0 Nardnosa(ag/l) 40
Control 6.8 8.2 8.7 18.3 18.4 18.5.1 Spec. Cord.lpraf+os) 85 45.9
Treatment 2 8.8 8.2 8.6 8.3 8.3 8.6
Chlorineimg/t) �i:i� Na
LC50 /Acute Toxicity Test Sample tap. at receipt(•CI:. 3.2
(Mortality expressed as %, ocabining replicates) i
Notes Please
X % 7l % X X Y x X X Concentration Complete This
Section ALSO
start /end start /end
LC50 a % Method of Determination Control
95% Confidence Limits Moving Average Probit _
`% •• __x %mirson karber _ _ other _ Nigh
Cos1C.
pN D.O.
Organism Testedt Cariodaphnis dubie Durstion(hrs)t I
Copied from DEM form AM (3/87) rev. 11/95 (DUBIA ver. 4.32)
P. 8/22
Page 21
2

• MAR 04 '99 82 :48PM B(RLINGTON RESEARCH P.9/22
Aquatic Bioassay ThatInq a Aquatic Tax'icity Redudlon Evaluallom
Chemical Product Envirronmantel Assessments a NPDti9 Tasting
FleporM9 a Data Handling Sendces
BURLINGTON 1302 Belmont Street - Burlington, NO 27215 -6935 • Phone [phone] - Fax [phone]
RESEARCH,
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: Mr. Roy Ritdt
SAMPLE DESC: FEB. MONITORING
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 02124/9911:45 SITE: 1.5 ppm
PARAMETER
DATE/TIME/ANALYST
WORK ORDER #: 9B607.004
RECEIVED: 02,124199
REPORTED: 03/04/99
PO NUMBER:
MOL RESULT
Fluoride by IC Analysis Started 031021991133 0.10
EPA 300.0 Analyzed 03/02/99 by TAR at BRI - Burlington
Ceriodaphnia Pass/Fail Chronic Started 0212419914 :00 NIA
NC:DEM 9189 Analyzed 03104/99 by JCB at BM - Burl(ngton
MQL - Minimum Quantitation Limit
Water Emr mmerital Sar*u - Eden
Wsion of BtxlingW Raseard% Inc.
910 W. Meadow Road - Eden, NO 272M
Phone (336) 02&Ml a Fax [phone]
IN tee
1.47 mglL
Pass Pass1781
Page 22
Pap 4 Water EmrirurmntWSeNIM- Kftton
DM&Ion of 8udhghon Researdi. Ino.
100 E. Cordon Street • Kinalm, NO 28501
Phone [phone] a Fax [phone]
V

MAR 04 '99 02 :49PM BURLINGTON RESEARCH P.10i22
• Effluent Toxicity Report Fora - Chronic Pan/Fail and Acute LC50 Date: 03 /04/99
facility: FLUORIDE SAMPLES NPOES#s NC Pipe#: 0untys MITCHELL
Laboratory Performing Test: BURLINGTON RESEARCH, INC.
Comments: 1.5 ppm; a ante
X
Signature of Operator In Responsible Charge
4n,otur/4�1aboratory Supervisor * PASSED: 19.13% Reduction
York orders 98607 -004 Envirormentat`scienceg Branch
MAIL ORIGINAL TO: Div. of Environmental Management
N.C. Dept. of ENNR
4401 Ready Creek Road
Raleigh, North Carolina 27607.6445
North Carolina Ceriodaphnia
Chronic Pass /Fail Reproduction Toxicity Test Chronic Test Results
Calculated t a 2.569
Tabular t = 2.528
CONTROL ORGANISMS 1 2 3 4 5 6 7 6 9 10 1? 12 X Reduction ■ 19.13
X Mortality Avg.Reprod.
# Young Produced 21 15 21 24 17 21 18 23 22 21 9 18
0.00 19.17
Control Control
Adult (L)ive Mead L L L L L L L L L L L L
0.00 15.50
Treatment 2 Treatment 2
Effluent It 100%
TREATMENT 2 ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12 Control CY
I 21.550% PASS FAIL
d Young Produced 15 14 141 "3 16 14 18 17 11 M,, 15 X control ores X I
producing 3rd -�
brood
Adult (L)ive Mead L L L L L L L L L L L L 1001 Check One
lot sample 1st sample 2nd sample Complete This For Either Test
pM Test Start Was 02/24/99
Control 7.30 7.94 7.60 7.21 6.86 7.41 Collection (Start) Date
sample 1: 02/24/99 Sample 2s
Treatment 2 7.13 7.22 7.19 7.02 6.76 7.26 Sampla Type/Duration 2nd
lot P/P
s s s Grab Comp. Duration D
t e t a t a I s s
a n a n a n Sample I X hra L A A
r d r d r d U IS M
t t t Sample 2 hra T P P
tat sample lot asepla 2nd sample
D.O. Hardness(mg/L) 40
Control 8.e 18.2 8.7 15.3 118.4 18.5
Spec. Cond.(amhos) 85 48.4
Treatment 2 8.8 8.3 8.6 8.2 8.2 8.7
Chlorint(mp /!f :;: >:,'•;� Na
LCSO /Acute Toxicity Test Sample temp. at raeoiptV C) :trti v 3.2
(Mortality expressed as X, combining repticetea) i
Pl
Note: easa
II X X X II II II X X X Concentration Complete This
Section Also
1t X % % X X % % X % Mortality
start /and start /end
1050 • X Method of Determination Control
95% Confidence limits Moving Average Probit _
-- ,_,x Spearman Kerber = Other _, Nigh
Corte. pH 0.0, Page 23
Organtsa Tested: Ceriodophnis dubia Duration(hrs)s
Copied from DFA form AT -1 (3/87) rev. 11/95 (DUBIA ver. 4.32)
?i�L

MAR 04 '99 02 :49PM BURLINGTON RESEARCH P.11i22
• • A
MR I Aquatic Bioassay Testing - Aquatic Toxkity Reduction Evatuatl6m
Chemical Product Environmental Asseasmenls - NPDES Tasting
Reporting 6 Data HarKoft Setvloe*
BURLINGTON 1302 Belmont Street • Burlington, NC 27215-6935 - Phone [phone] - Fax [phone]
RESEARCH
ANALYTICAL REPORT
CUSTOMER. Unimin Corp.
REPORT TO: Mr. Roy Ritdc
SAMPLE DESC: FEB. MONITORING
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 02424/99 11:50 SITE: 2 ppm
WORK ORDER 41%
98607 -005
RECEIVED:
02/24/99
REPORTED:
03/04/99
PO NUMBER:
PARAMETER DATEMME/ANALYST MOL RESULT
Fluoride by IC Analysis Started 03/02/9911:53 0.10 1.93 mgd
EPA 300.0 Analyzed 03/02/99 by TAR at BRI - Bu rlinrton
Ceriodaphnia pass/Fail C hmnle Started 02/24/9914 :00 N/A Pass Pass/Fall
NCDEM 9/89 Analyzed 03/04/99 by J'CH at BM - Buruaaton
MQL = Minimum Qmititation Limit
I VaW Env MMw M Services - Ed*n
Division of auMvIon R*s*arch, Inc.
370 W. Meadow Road - Eden, NC 27298
Phone [phone] • Fax [phone]
V4 vu
Page 24
Page S water Em&on mend sarA= - Kinston
100 L Gorrddo�n SV 10v % NNC 22M
Phone [phone] - FAX [phone]
Z7

MAR 04 '99 02 :49PM BURLINGTON RESEARCH
Effluent Toxicity Report Fora - Chronic Pass /Fafl and Acute LC50 Date: 03/04/99
Facility: FLUORIDE SAMPLES NPDES4: NC Pipe#: County: MITCHELL
Laboratory Performing Test: BURLINGTON RESEARCH, INC.
Comments: 2,0 ppn
V
Signature of Operator in Responsible Charge
X4� I--- a PASSED: 4.35X Reduction
Si ature of Laboratory Supervisor
York Order: 98607-005 Envirorv*ntal Sciences Branch
MAIL ORIGINAL TO: Div. of Envirormental Management
W.C. Dept. of ERWR
4401 Reedy Creek Road
Raleigh, North Carolina 27607 -6445
worth Carolina Ceriodaphnia
Chronic Pass /Fail Reproduction Toxicity Test Chronic Test Results
Calculated t = 0.568
Tabular t r 2.508
CONTROL ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12 X Reduction r 4.35
X Mortality Avg.Reprod.
8 Young Produced 21 15 21 24 17121 18 23 22 21 9 18
0.00 19.17
Control Control
Adult (L)ive (D)ead L L L L L L L L L L L L 0.00 18.33
Treatment 2 Treatment 2
Effluent %: 100%
TREATMENT 2 ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12 control cV PASS FAIL
I Young Produced 20 24 18 15 21 20 15 19 15 16 16 21 % control orgs pCh.k producing 3rd
brood One
Adult (L)ive (D)ead L L L L L L L L L L L L 100%
1st sample 1st sample 2nd sample Complete This For Either Test
PH Test Start Date: 02/24/99
Control 17.3017.94 7.60 7.21 16.86 7.41 Collection (start) Date
Sample 1: 02/24/99 Sample 2: / /
Treatment 2 7.10 7.16 7.14 7.11 6.71 7.25 Sample Type/Duration 2nd
1St P/F
s s S
t e t e t e
3 n a n a n
r d r d r d
t t t
1st sample 13t sample 2nd sample
D.O.
Control 8.11 18.2 1 8.7 18.3 1 8.4 18.5
Grab Comp. Duration D
I S S
sample 1 X hrs L A A
U M M
Sample 2 hrs T P P
Hardness(mg /L) 40:;r; ::;.;:••:
Spec. Cord.(AMOG) 85 51.3
Treatment 2 8.8 8.3 8.6 8.2 8.2 8.7
Chlorine(mg /L) 1*.;:;:: n/a
LC50 /Acute Toxicity Test Sample temp. at receipt(•C) ;.:;;;:;;: 3.2
(Mortality expressed as X, combining replicates) Note: I Please
X X X % X X X % % X Concentration SeoctioneA hi
X X X % X X X X X X X MortalitYstart /end start /end
LC50 % Method of Determination Control
95% Confidence Limits Moving Average ^ Probit _
X -- % Spearman Karber _ Other High
Cone.
PH D.O.
I organism Tested: Ceriodaphnia dubia Ouration(hrs): _
IIIICopied from DEM form AT -1 (3/87) rev. 11/95 (DUBIA ver. 4.32)
P.12/22
Page 25
U

MAR 04 '99
El
BURLINGTON
RESEARCH
02:49PM BURLINGTON RESEARCH P.13i22
Aquatic Bioassay ToWng • Aquatic Toxicity Reduction Evaluations
ChemIeal Product EnAronmental Assessments • NPOES Testing
Reporting A Data Handling Sorvk s
1302 Belmont Street • Burlington, NC 27215 -6935 a Phone [phone] • Fox (336) 570 -4698
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: Mr. Roy Riffle
SAMPLE DESC: FEB. MONITORING
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 02t24/99 11:55 SPTE: 3 ppm
IPARAMETER
Fluoride ICAnalysis
EPA 300.0
Ceziodap'hnia Pass/Fail Chronic
NCDEM 9/89
WORK ORDER A
98607 -006
RECEIVED:
02124/99
REPORTED:
03/04/99
PO NUMBER:
DATEMME /ANALYST MQL
Started 03/02/9911:53 0.10
Analyzed 03/02/99 by TAR at BRI - Burlington
Started 02/2419913 :45 N/A
Analyzed 03104199 by JCB at BRI - Burlington
MQL = Minimum Ouantitation Limit
Water Enviraxwer W Somkos - Eden
Division of BurUn m Research, Inc.
374 W. Meadow Road • Eden, NO 2M8
Phone [phone] - Fax [phone]
Eris v»
RESULT
189 m&IL
Pass Pan/Fail
Page 26
Page 6 Water EnvtrorsrwntW Savicea - Xk3ton
Division of Burlington A""rch, Inc.
100 E. Gordon Street • Kinston, NO 20501
Phone (252) 520,-9921 Fax [phone]
Z.`

MAR 04 '99 02:50PM BLRL.INGTON RESEARCH
P.14/22
effluent Toxicity Report form - Chronic Pass /Fail and Acute LC50 Dates 03 104199
Facility: FLUORIDE SAMPLES NPOES /: NC PipeNI County: MITCHELL
Laboratory Performing Tests BURLINGTON RESEARCH, INC.
Comments e 3 ppim
x
Sienr of Operator in Responsible Charge
x
;en
sf ttN�e o Laboratory supervisor
' PASSED: - 31.30% Reduction
work orders 96607 -006
Envirornontal Sciences Branch
MAIL ORIGINAL
TO: Div. of Envirarmental Management
N.C. Dept, of ENNR
4401 Ready Creek Road
Raleigh, North Carolina 27607.6445
North Carolina Ceriodophnis
Chronia Pass /Fail Reproduction Toxicity Test Chronic Test Results
Calculated t •
Tabular t ■
CONTROL ORGANISMS 1 2 3 4 5 6 7 8
9 10 11 12 x Reduction w -31.30
X Mortality Avg.Reprod.
9 Young Produced 21 15 21 24 17 21 18 23
22 21 9 18
0,00 19.17
Control Control
Adult (L)ive (0)ead L L L L L L L L
L L L L
0.00 25.17
Treatment 2 Treatment 2
Effluent Is 100%
TREATMENT 2 ORGANISMS 1 2 3 46 5 6 7 8
9 10 11 12 Control CV
21.550% PASS FAIL
N Young Produced 27 16 31 26 7 26 29 33
32 23 26 26 X control orgs X
producing 3rd _..J
gom
brood Cheek
Adult (Dive Mead L L L L L L L L
L L L L 100%
lot sample 1st sample 2nd sample
Complete This For Either Test
PH
Test Start Date: 02/24/99
Control
7.59
7.32
7.46
6.78
Collection (Start) Date
17.431?.Ill
Sample It 02/246/99 Sample 2: / /
Treatment 2
7.60
7.31
7.40
6.91
6.73
7.16
Sample Type/Duration 2nd
lot P/F
s a s
Grab Comp. Duration 0
t e t e t e
I S S
a n a n a n
Sample 1 X hrs L A A
r d r d r d
U N M
t t t
Sample 2 hra T P P
lot sample 1st sample 2nd sample
D.O.
Control
8.7
8.s
8.1 8.!
18-1
1_18.7
epee. Cond.(wohos) i5 54.7
Tratmot 2
8.9
8.2
8.3
8.3
8.0 8.3
LC50 /Awte Toxicity Test
Saapte temp. at receipt(•C) ::r:; 3.2
(Mortality expressed as x, combining replicates)
Note: Please
x
%
%
%
x
x
x
x
x
x
Concentration
Complete This
I
Section Also
x
x
x
X
x
X
x
x
X
X
Mortality
start /end start /and
LC50 ■ % Method of Determination Control
95% Confidence Limits Moving Average
Probit
_
X -- Spearman Karber
other _ Nigh
PH D.O.
Organism Tested: Coriodaphnia debts Duration(hrs): I
Copied from PER form AM (3/67) rev. 11/95 (DURIA var. 4.32)
Page 27
716

MAR 04 '99 02 :SWM BLRLINGTON RESEARCH P. 15/22
Aquaec ekm ay T"gn9 - Aquatic Toxicity Reduction Evaluations
rmpli Chen*4 Product EnArorunenW Assessments - NPDES Tostin9
Ropor*V 6 Data Handling Services
BURLINGTON 1302 Belmont Street - Burlington, NC 27215.6935 - Phone (336) 5MA661 - Fax [phone]
RESEARCH
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: Mr. Roy Rittle
SAMPLE DESC: FEB. MONITORING
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 02/24/9911:55 SITE: 4 ppm
IPARAMETER
DATE/TIME/ANALYST
WORK ORDER #: 9B607 -007
RECEIVED: 02/24/99
REPORTED: 03/04/99
PO NUMBER:
MOL RESULT
Fluoride IC Analysis Started 0310219911x3 0.10
EPA 300. Analyzed 03102/99 by TAR at BRI - Burlington
Ceriodaphnia Pass /Fail Chronic Started 02/24/9914 :00 N/A
NMEM 9/89 Analyzed 03/04/99 by JCB at BRI - Burlington
MQL = Minimum Quantitation Limit
Water ErwkorrnenW Sorviom - Eden
Division of Bw&vjton Research, Inc.
970 W. Meadow Road - Eden. NO 77288
Photo [phone] ■ Fax [phone]
3.86 mg/I.
Pass Pass/Fail
Page 28
Pap 7 Water Erwkorxnoruar 8eMoes - Kkrstun
Division d Budkgton Reseadh Inc.
100 E. Gordon Street - Kinston. NC 28501
R me [phone] - Fax [phone]
Z7

MAR 04 '99 02 :SOPM BLIRLINGTOIV RESEARCH
Effluent Toxicity Report Form - Chronic Pass /Fail and Acute LCSO Date: 03 /04/99
Faciiity: FLUORIDE SAMPLES NPDESS: NC Pipes: County: MITCHELL
Laboratory Performing Tests BURLINGTON RESEARCH, INC.
Comments: 4 ppm
X
Signature of Operator in Responsible Charge
it
symature of Laboratory supervisor
York Order: 9B607-007
MAIL ORIGINAL TO:
North Carolina Ceriodaphnia
Chronic Pass /fail Reproduction Toxicity Test
PASSED: - 17.832 Reduction
Environmental Sciences Branch
Div. of Environmental Management
W.C. Dept. of EHNR
4401 Reedy Creak Road
Raleigh, Worth Carolina 27607.6445
Chronic Test Result&
Calculated t * -1.369
Tabular t = 2.508
CONTROL ORGANISMS
1 2 3 4 5 6 7 8
9 10 11 12 2 Reduction ■ -17.83
f%
Mortality Avg.Reprod.
Young Produced
21 15 21 24 17 21 16 23
22 21 9 18
1
0.00 19.17
Control Control
Adult (WV& (0)ead
L L L L L L L L
L L L L
0.00 22.58
Treatment 2 Treatment 2
Effluent Xs 100%
TREATMENT 2 ORGANISMS
1 2 3 4 5 6 7 8
9 10 11 12 Control CV
21.550% PASS FAIL
s Young Produced
21 32 25 5 21 22 16 22
31 18 31 27 X control s
1
E
3rd -
broad Check One
Adult (L)ive (D)ead
L L L L L L L L
L L L L 100%
let saWte
1st sample 2nd sample
Complete This For Either Test
PH
Test Start Date: 02/24/99
Control
7.30
7.94
7.6017.21116.8617
4 4i
Collection (Start) Date
Sample 1: 02/24/99 Sample 21 / /
Treatment 2
-1.4817.211
7.26
6.85
6.65
7.22
Sample Type/Duration 2nd
laic P/F
s
s a
Grab Comp. Duration D
t a
t e t a
I S S
a n
a n a n
Sample 1 X bra L A A
r d
r d r d
U M M
t
t It
Sample 2 bra T P P
1st seeple
let saaQle 2nd sample
D.O.
Nardness(mg /l) 40 c;ri • "` i'k
Control
8.8
8.7
a.3
8.4
18.9
18.2
18.5
sPee. eond.(pnhos) 85 58.1
Treatment 2
8.2
8.5 18.1.
8.3
8.4
chtorine(me/U ..., js n/a
LC50 /Acute Toxicity Test
Sample temp. at receipt(- C)c <:;: 3.2
(Mortality expressed as %, combining replicates)
Note: Please
X
><
%
X
%
X
%
X
X
%
Concentration
Complete Tbis
Section Also
X
%
%
%
%
X
X
X
X
%
Mortality
start /end start /end
LC50 %
Method of Determination
Control
952 Confidence Limits
Moving Average
Probit
Spearman Kerber
_
Other _
Nigh
Como.
PH D.O.
Organism Tested: Ceriodaphnia dubis Duration(hrs): 1
Copied from OEM form AT -1 (3/87) rev. 11/98 CDl1BIA ver. 4.32) 1111
P. 16/22
Page 29
7.�

MAR 04 '99 02 :SIP11 BURLINGTON mu-p- i-H P. 17/22
Aquatic Bioassay Tasting • Aqualio Toxloily Radunion Evaluations
rRI I - Cherntoal Product EnvironmentalASSessments • NPDES Testing
Reporting & Data Handling Services
BURLINGTON 1902 Belmont Street • Burlin0ton. NO 27215 -6935 • Phone [phone] a Fax [phone]
RESEARCH
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: Mr. Roy Rittic
SAMPLE DESC: FEB. MONITORING
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 02/24/'9912:00 SITE: 8 ppm
IPARAMETER
WORK ORDER #:
9R607 -008
RECEIVED:
02124)99
REPORTED:
03/04/99
PO NUMBER:
DATE/TIME/ANALYST MQL
Fluoride by IC Analysis Started 03102/'9911:53 0.10
EPA 300.0 Analyzed 03/02/99 by TAR at BRI - Burlington
Ceriodaphnia Pass/Fail Chronic Started 0284/9914:00 N/A
NCDEM 9/89 Analyzed 03/04/99 by" at BRI - Burlington
MQL = Minimum Quantitation Limit
RESULT
7.20 mg/L,
Pass Pass/Fall
Page 30
Water ErnAronnenW Services -Eden Pago g Water Environmental Servloes - KMston
Division of Burlingim Research, Inc. Division of 8urtirrg1n Research, Inc.
370 W. Ma2dow Road o Eden. NO 27288 100 E Gordon Street • Kinston, NC 28501
Phone CMM 623.8021 • Fax [phone] Phone [phone] • Fax [phone] Z9

MAR 04 '99 02 :51PM BURLINGTON RESEARCH
Effluent Toxicity Report Forts - Chronic Pass /fell and AMU LC50 Date: 03/04199
Facility: FLUORIDE SAMPLES NPDESS: NC Pipelts Countys 141TCHELL
Laboratory Performing Teat: BURLINGTON RESEARCH, INC.
COMF*ntS: 8 PPP
x
7 Si lure of Operator in Responsible Charge
x .�., 4'
gnatura of Laboratory Supervisor • PASSED: - 28.262 Reduction '
York Order: 98607 -008 Environmental Sciences Stanch
NAIL ORIGINAL 70s Div. of Environmental Managemont
N.C. Dept. of EHNR
4401 Ready Creak Road
Raleigh, North Carolina 27607.6445
Borth Carolina Ceriodophnis
Chronic Pass /Fail Reproduction Toxicity Test Chronic Test Results
Calculated t = -2.932
Tabular t ■ 2.508
CONTROL ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12 X Reduction o -28.26
1st sample 1st sample 2nd sample Complete This for Either Test
PH Test Start Dates 02/24/99
Control 7.30 7.94 7.60 7.21 6.86 7.41 Collection (Start) Date
Sample It 02/24/99 Sample 2:
Treatment 2 7.48 7.21 7.26 6.65 6.65 7.22 Sample Type/Duration 2nd
1st P/F
a a s Grab Camp. Duration 0
t e t c t e I S S
a n a n a n Sample I X bra L A A
r d r d r d U M N
t t t Sample 2 bra T P P
tat sample tat sample 2nd sample
D.O. Hardness(ma/l) 40:iit ; { >i:: ,:ff:
Control 18.6 18.2 118.7 18.3 15.4 8.5 1 1
Spec, Cond.(pmhoa) 85 72.8
Treatment 2 8.8 8.2 8.5 8.4 8.3 8.4
ChlorineCroJU •:•K-.* n/a
LC50 /Acute Toxicity Test Sample teV. at reeeipWQ - ;:,'.:' ^. 3.2
(Mortality expressed as %, combining replicates)
Note: Pleast
% X X X % X % % % % Concentration Complete This
Section Also
X X X Ti % X X % X % Mortality
start /end start /and
LCSO ■ % Method of Determination Control
95% Confidence Limits Having Average Probit _
Spearman !Garber ` other
Cone.
PH D.O.
Organism Tested: Ceriodaphnia dubia Duration(hrs):
Copied from DEN form AT -1 (3/87) rev. 11/95 (DUSIA ver. 4.32)
P. 18/22
Page 31
7 C
% Mortality
Avg.Reprod.
8 Young Prod ad
21 15 21 24 17 21 18 23 22 21 9 18
0.00
19.17
Control
Control
Adult (L)ive (D)ead
L L L L L L L L L L L L
0.00
24.58
Treatment 2
Treatment 2
Effluent X: 100%
7REATMENT 2 ORGANISMS
1 2 3 4 5 6 7 8 9 10 11 12
Control CV
21.550%
PASS FAIL
N young Produced
27 16 32 31 21 23 22 26 19 23 30 25
%roduciol
3rd
brood
Check One
Adult (L)Iva CD)ead
L L L L L L L L L L L L
100%
1st sample 1st sample 2nd sample Complete This for Either Test
PH Test Start Dates 02/24/99
Control 7.30 7.94 7.60 7.21 6.86 7.41 Collection (Start) Date
Sample It 02/24/99 Sample 2:
Treatment 2 7.48 7.21 7.26 6.65 6.65 7.22 Sample Type/Duration 2nd
1st P/F
a a s Grab Camp. Duration 0
t e t c t e I S S
a n a n a n Sample I X bra L A A
r d r d r d U M N
t t t Sample 2 bra T P P
tat sample tat sample 2nd sample
D.O. Hardness(ma/l) 40:iit ; { >i:: ,:ff:
Control 18.6 18.2 118.7 18.3 15.4 8.5 1 1
Spec, Cond.(pmhoa) 85 72.8
Treatment 2 8.8 8.2 8.5 8.4 8.3 8.4
ChlorineCroJU •:•K-.* n/a
LC50 /Acute Toxicity Test Sample teV. at reeeipWQ - ;:,'.:' ^. 3.2
(Mortality expressed as %, combining replicates)
Note: Pleast
% X X X % X % % % % Concentration Complete This
Section Also
X X X Ti % X X % X % Mortality
start /end start /and
LCSO ■ % Method of Determination Control
95% Confidence Limits Having Average Probit _
Spearman !Garber ` other
Cone.
PH D.O.
Organism Tested: Ceriodaphnia dubia Duration(hrs):
Copied from DEN form AT -1 (3/87) rev. 11/95 (DUSIA ver. 4.32)
P. 18/22
Page 31
7 C

MAR 04 '99 02 :51PM BLRLINGTON RESEARCH P.19i22
• Agoads Bioassay Testing - Aquads ToxWq Reduction Evaluedons
Chemical Product Environmental Assonmsnts - NPDES Testing
Reportirg 6 Date Handling Services
BURLINGTON 1302 Belmont street • Burlington, NC 27215 -6935 • phone [phone] • Fax [phone]
RESEARCH ,
ANALYTICAL REPORT
CUSTOMER: Unimin Corp,
REPORT TO; Nc. Roy ltittle
SAMPLE DESC: FEB. MONITORING
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 02/24/9912;00 SITE: 16 ppm
PARAMETER
Fluoride 0 IC Analysis
EPA 300.
Ceriodapbnia P&%Tall Chmnic
NCDF.M 9/89
DATMIVE/ANALYST
WORK ORDER #: 9B607.009
RECEIVED; 02/24/'99
REPORTED: 03104/99
PO NUMBER:
MQL RESULT
Started 03/02/991133 0.10
Analyzed 03/02/99 by TAR at BRI - Burttngton
Started 02/,4/9914:00 NIA
Analyzed 03/04/99 by 7CB at BRI - Bu rlingtou
MQL = Minimum Quantitat ion Limit
15,9 mg/L .
Pass PauXan
Cer ificationx
BRI - Burlin ton
NC Semishhyy.� #85, Biomonitorin : #002, Drinking Water. #37143, Radiation License: #0014904 -0Gr
VA SWC;B ID: #000061, Drinking Water. #00018
SC Laboratory M! #99042
EPA Chemistry Lab TA: N000137, Bioassay Lab M: NC 2721S00
Water l:n*pnrnental Servtcss -Eden
DiA&Ion of Surlir g m Research. Inc.
970 W. Meadow Road • Eden. NO 27M
Phone [phone] - Fax [phone]
Page 32
Page 9 Division d Bl�rtAro � p""r^ him
100 K:. Gordon Street • Kinston, NC 28501
Phone =) 520.8821 - Fax [phone]
e� ury
31

MAR 04 '99 02:52PM BLR- INGTON RESEARCH
Effluent Toxicity Report Fong - Chronic Pass/Fail mid Acute LC50 Dates 03 /04/99
Facilitys FLUORIDE OWLES NPDESI: NC Pipe+h County: MITCHELL
Laboratory Parforntng Test: BURLINGTON RESEARCH, INC.
tom entas 16 ppm
X
Signature of Operator in Responsible Charge
4�t tory Supervisor
York Order: 9WANW001
NAIL ORIGINAL T0:
North Carolina Cariodaphnis
Chronic Pass /Fait Reproduction Toxicity Test
* PASSED: -1,74% Raduction •
Environssental Sciences Branch
Div. of Enviror ental Management
N.C. Dept. of EHNR
4401 Reedy Crock Road
Raleigh, North Carotins 27607 -6445
Chronic Test Results
Calculated t - -0.114
Tabular t - 2.508
CONTROL ORGANINd 1 2 3 4 5 6 7 8 9 10 11 12 X Reduction + -1.74
% Mortality Avg.Reprod.
0 Young Produced 21 15 21 24 17 21 18 23 22 21 9 18
0.00 19.17
Control Control
Adult (01ve (D)*md L L L L L L L L L L L L
8.33 19.50
Trs.toent 2 Treatment 2
Effluent X: 100%
TREATMENT 2 0RGANISM8 1 2 3 4 5 6 7 8 9 10 11 12 Control CV
21.5501 PASS FAIL
0 Young Produced 24 28 24 28 30 26 26 6 15 11 5 11 % control orgs X I
producing 3rd —J
brood Cheek 9M*
Adult (L)ive (D)ead L L L L L L L L L L D L 100%
1st ample 131 sample 2nd ample Complete This For Either Test
PH Test Start Date: 02/24/99
Control 7.30 7.94 7.60 7.21 16.6617,411 Collection (Start) Date
Smmple 1: 02/24/99 Sample 2:
Treatment 2 7.45 7.21 7.22 6.84 6.65 7.25 Sample Type/Duration 2nd
1st PIP
s s s Grab Comp. Duration D
t a t o It 0 1 S S
a n a n a n Sampte 1 X hrs L A A
r d r d r d U N N
t t t Semple 2 hrs T P P
lot wept. tat *mote 2nd sample
D.O. Hardness ( t /l) 40 ;x? ; :i :.itFy
Control. 8.1 a.2 a.7 18.3 118.4 15.5
Spec. Cord.(�smhos) 85 116.8
Treatment 2 8.6 8.1 - 8.3 8.1 8.3 8.5
Chtortne(mg /l) : ;` fix; We
LC50 /Awte Toxicity Test Sample temp. at receiptVC) 3.2
(Mortality expressed as X, combining replicates)
Note: Please
% % % X X X X % % % Concentration Complete This
Section Also
% X % % X X % % % X Mortality
start /end start /end
LC50 * % Method of Determination Control
95% Confidence Limits Moving Average Probit _
"nun Karber _ � Other _ Nigh
Cono
PH D.O.
Organism Tested: Ceriodephnis dubin Durattan(hra): _-^
Copied from OEM fans AT -1 (3/87) rev. 11/95 (DUgiA ver. 4.32)
Page 33
3Z

1302 Belmont Street 370 West kk%dDw Road V 100 £act Gorcbm slooet
Burlington, NC 27215.69M Eden. NC 272BS Kitson. NC 2850'r
[Ell BURLINGTON RESEARCH, INC. Fax (�i 5770.4699 Phone tom) 623-W21 Phone (252) 520
i
CLIENTT:-L'w'�- for . SEND REPORT TO: heo" f"441 -P.,
Fadfly/5ite: �' 's - - .-.� -� rte, Acs 1-y. t-- Phony, Fax:
Sampler. Pvnr) r),6 t& t*w-- - (Signarrire) Purchase Order No.: �$
c SAMPLE �� SAMPLETYPE emu' l:i:l:llR�1:1II-- 1443pIE'� (n
SAM ME W COLLECTION �w u Z- L; ANALYSIS , .. Preservation Cottex 3b
¢ H STARTED ENDED ag 4 �„ COIdPOSTTE m Q w a -¢ TEMP.. A =1ce �= NaOH
o>- A�� GRAB ~a' REQUIRED j4° B =HNO3 -- F.= Norte
DATE DATE � e-o � z /1,/)�j _ /'{"� C = H2SO4- --G .CUPRIC
TIME TIME "�° HAND AUTO z� 'i1�JiQ(J 1 -D=HCI- H=HCHD
Yes; na 2 —(R
j 1J��L��r ' it Q n�►: it1L' 0
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Y"I No
Yes1 No
—M Yial No
eft/
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Yes 1 o f Y L W•.
Yes =11s llrsiV' � 2 �� ll m .. .. ✓.:`' . '
Yeti No
Yes: ND kt
NO
Was No sample dechlorinaled at time of collection? Yes
FOR CLIENT USE ONLY
� Rest i�hee bir (S '
ro ed Sig,) Dais.
w
� Received by: (M) Date:
No Wk Will the results be used for regulatory monkoring purposes? Yes ❑ N01*
&00
TV=
Timm
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-.- •_ - . • • - •••-.� nr+� .,,m ,a...... �.. nirnM Mnih Finol r7nnnA
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plaints omrnerrt - - rr)
r`aranv - SRI - LahnrnMnr Pink - SRI - Laboratory Goldenrod - Grid - Copy

1.102 Belmont Street 370 West Meadow Reed
E111Stshnglon. NC x,215.6W6 Ede (n33, 33NC 27288 BURLINGTON RESEARCH, INC. Fax nc13366�5'70.4698 Phone x (336)623.58781
Q 100 East Gordan Street
lonston. NC 28501
Phom Fax ((M) 52D-Nn
CHAIN OF •DRECORDS
CUENT:_i 7 /0l1 SEND REPORT TO: /�Sf JY!/7'CQ' �i'1G ` Ade- YA114,
FaciR Y/SH e:.A / -/V TG �ll�i�►� Phon Fa
e_ t'��� ',��%S //.9 r.
Sampler (P" �!' / M S (Sx,�rxtiuna Purchase Older Nt' • N
SAMPLE z MPLETYPE �-e1
COLLECTION o 0 ° 04- u w PresinMflon Codex 3
SAMPLE 10 o STARTED EPII)ED �M j OOMPOSITE >;RAB Mz W IiEQ RED le cccc TEMP. 9 = FINOO F =None
7WE TIME � � HAND AUTO 2: � � { CI D =lW . � C
ZYes+ m n - • ,
of A616 Txic{v
Yes No '
�� Fly.• .. -.:. = . ..
Yee Ito .
Veal No
Ypi ke ,
Yea�No " •••- -,
YON ft
Yes! Nb _
Yes; No
Was the sample dbchWrtnsbed at time of collection? Yes Q No ❑ A(Ill WHI no results be used for regulatory monitoring purposes? Yes ❑ No
,. FOR CLIENT USE ONRLY p O' FOR LAB +
bed 1 / Ti[t�: 3 Received in lib Fii011t (SW
j Deaec T'UW
rCLJ �
Method or Sh�eat
Fleaelved trp: Tlme: :311311" ' �Dt:SCT ) Dater g�j I `� . z— , IOettmd o(Sl�pmeru y rtteld - •• _ . • ` .
a etEn�.e

MAR 04 '99 03: 12PM TB�IIMINQUARTZ �
•
FAX Transmissions Sheet
Burlington Research, Inc.
1302 Belmont Street
Burlington, NC 27215 -6935
Phony 910/5704661
FAX: [phone]
FAX ONLY , X�
DATE: March 4, 1999
TO: Roy Rittle
COMPANY: Unimin
FAX #: [phone]
FAX & MAIL
L V T�
`ioxIcr
FROA John Bawmmer,-BRI Biomoanitoring Lab Mana$er��
SUBJECT: Completed reports
You should receiv 2gardino 7nti his cover sheet V you do not receive all page& or
have a question r ase call me at 9101570 -4661, Fxt 289.
COMNMNTS;
Completed reportg
Questim�s, p lease
John
P. 120
Page 36

MAR 04 '99 03:12PM WRLINGTON RESEARCH
-311
BURLINGTON
RESEARCH,
R" va
Aquado Bioassay Tea$ng • Aquatic Toxicity Reduction Evaluations
chemical Product EnAmninmW Assessments • NPDES Testing
Reporting & Data Handling Services
P.2/20
1302 Belmont Street • Burlington, NO 27215 -8935 • Phone [phone] • Fax [phone]
March 4,1999
Unimin Co
P.O. BOX 586
Spruce Pine, NC 28777
Attention: Mr. Roy Rittle
Enclose�d� please find the reports for your samples received 03/03/99, assigned
to BRI Workorder 9C104. Please call if you have any questions.
Thank you.
Water Erwtrorxnerttal 6eMoee • Eden
Dlviaion of Burlington Rsawwoh. WA
370 W. Meadow Road • Eden. NO 27288
Phone [phone] - Fax [phone]
Sincerely,
TBhnQZ)aummer GTON RESEARCH, INC.
410--1
Manager, Biomo2toring Dept.
(336)570 -4661 E4 289
Page 37
Water Ewmnmenw Sor&aa • Kinston
DiAslon of Burlington Fteasarch Inc.
100 E. Gordon Street • Kinston, Rd 28501
Phone [phone] • Fax [phone]

MAR 04 '99 03 :13PM BURLINGTON RESEARCH
Aquedo B'roassay Tesdnq a Aquatic 7o3ddW Reduction Evalusdahs
Chemical Product EnvhorwnenW Assessments - NPDES Testing
Repordrng ✓1 Data Handling Senrlaras
w
BURLINGTON 1302 Belmont Street - Burlington, NC 27216.6935 - Phone [phone] - Fax [phone]
RESEARCH ' --"
ANALYTICAL REPORT
CUSTOMER:
Unimin Corp.
REPORT TO:
Mr. Roy Rittle
SAMPLE DESC; SPRUCE PINE
SAMPLE TYPE:
WASTEWATER, GRAB
COLLECTED:
03102/9916 :00 SITE: 0 PPM
WORK ORDER 0
9C104 -001
RECEIVED:
03103/'99
REPORTED:
03/04/99
PO NUMBER:
PARAMETER DATE/TIME/ANALYST MOIL RESULT
Fluoride Started 0310419910:00 0.10 0.11 ttng/L
EPA 3402 Analyzed 03104/99 by 7CB at BRi - Burungton
Ceriodapphnia 48 -Hour Acute Static Bioassay Started 03/02/991635 N/A > 100 LC50%
EPA600491027F Analyzed 03/04/99 by JCS at BPj - Burlington
MOL = Minimum Quantitation Limit
Page 38
WaterErrAronmentelServices -Eden page i WaterEnvlrorwnMUrServtca- Kinston
Divulan of su&vton RM ", Ino. Division of Burlington Research, ho.
Ptr�on� ON Meadow 6 t 921 a Fait [phone] Phone Gordon
520.992 t • Fax [phone]

MT 04 '99 03:13PM BURLINGTON RESEARCH P.4i20
Aquatic 8ioessay Testing • Aquatic Toxicity Reduction Evaluatlons
Chemical Product EmIronmentalAssessments • NPDES Testing
Reporting S Data Handling services
BURLINGTON 1302 Belmont Street + Burlington, NO 27215 -6935 • Phone [phone] a Fax [phone]
RESEARCH
Effluent Toxicity Report Form - Acute LC50 Date: 3/4/09
Facility UNIMIN , NPDES* R&D Pipes �i County
Laboratory Performing Toot Burlington Research, Inc. - Cart. * 002
x Comments:
Signatilre of operator In Responsible Charge 0 PPM
X
SI ature of Laboratory Supervisor SRI# 90104-001
Environmental Sciences 6rancn
Div. of water Ouarity
MAIL ORIGINAL TO: NO Dept. of ENR
4401 Ready Crook Road
Raleigh, NO 27607 -6445
LC50 /Acute Toxiclty Test
(Mortality expressed as %, combining replicates)
Test Start Date: 1312/99 312/99
Collection Start Date:
Ssmple Type/Du_rstlon
urea
vamp,
yurarinn
rime
X
I
I
I
� Tox
Dilution eampte
Hardness(mg/L)
4r.240.5
Spec Cortd.(mlcromhoa)
'N
Chlorins(mg/L)
sample temp ® reoalpt
(dog. C)
0 12.5 25 50 1 75 100 Concentration (%)
0 0 0 0 0 o 1 1 1 Mortality ( %)
LC50 >1oo % Method of Determination
05% Confidence Limits (%) Movina Average Problt
N/C to Spearman Kerber Other
Organism Tested:
Ceriodaphnla dubla
1lodriod from OEM fan AT-1 (07) qv. AM
Water Environmental services - Eden
Division of Burlington Research. Inc.
370 W. Meadow Bond • Eden, NC 27286
Phone (338) 823 -ap21 • Fax [phone]
am-: fns
Stan End Stun End
7.85 1 8,34 Control 8.1 8.5
7,2 7.85 High 8.1 I 815
PH Cons D.O.
BN reM. tithe s..VarnsuAlinfonn
Page 39
Water Environrrtenial Bervices - Kinston
Division of Burlington Research, Inc.
100 E. Gordon Street * Kinston, NO 28501
Phone [phone] • Fax [phone]
3f

MAR 04 '99
BURLINGTON
RESEARCH r
03 :14PM BLRLINGTON RESEARCH P.5/20
Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product EnvironmentalAssessment& • NPDES Testing
Reponing A Data Handling Services
1302 Belmont Street • Burlington, NC 27215 -8935 Phone [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT T0: Mr. Roy Rittla
SAMPLE DESC: SPRUCE PINE
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 0310219916:05 SITE: 5 PPM
IPARAMETER
Fluoride
EPA 340.2
DATE/TIME/ANALYST
WORK ORDER #: 9C104.002
RECEIVED: 03103/99
REPORTED: 03104199
PO NUMBER:
MOL RESULT
Started 0310419910:00 0.10
Analyzed 03104/99 by JCB at BRI - Burlington
Ceriodaphnia 48 -Hour Acute Static BioassayStarted 03102/9916:55 N/A
EPA600491027F Analyzed 03/04/99 by JCB at BRI - Burlington
MQL = Minimum Qnantitation Limit
war ErWnmwM 3arvleee • Eden
Division of Budington Research, Inc.
$70 W. Meadow Road • Eden, NO 97288
Phone [phone] • Fax (338) x-5878
am ,n.
6.24 mgM '
> 100 LC5096
Page 40
Pap 2 WatarEnvironmenWSwvicos- tCutston
Division of Burlington Research. Ina
100 E. Gordon Street • Kinston. NO 28501
Phone [phone] - Fox [phone]
39

MAR 04 '99 03 :16PM BRRLINGTON RESEARCH
Aquatic Bioassay Tesdnp • Aquatic Tmd ft Reduction Evaluations
Chemical Product Envborrnemtal Assossmerds - NPDES Testing
- MR I Ropor ft d Data Handit Seroiccee
BURLINGTON 1302 Belmont Street - Burlington, NC 2721"935 e Phone [phone] - Fax [phone]
RESEARCH
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: Mr. Roy Rittle
SAMPLE DESC: SPRUCE PINE
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 03/02/9915:10 SITE: 10 PPM
IPARAMETER
DATE/TIME/ANALYST
WORK ORDER #: 9C104 -003
RECEM: 03/03/99
REPORTED: 03104/99
PO NUMBER:
MQL RESULT
Fluoride Started 0310419910:00 0.10 10.4 mg/L
EPA 340.2 Analyzed 03104/99 by 7CB at BRI - Burlington
Ceriodaphnia 48 -Hour Acute Static Bioassay Started 03/0219916:4S N/A > 100 LC50%
EPA600491027F Analyzed 03/04199 by JCB at BRI - Burlington
MQL = Minimum Quantitation Limit
Page 42
waterErMimomnor>btServices -Edon Page 3 VAWewtronv+neroolsw*."- Kinston
370 W M Meadow Road Eden NCt22MIk 100 EE Gordon sv6M * *I town No 9M
Phone [phone] - Fox (336) MS878 Phone [phone] • Fax [phone]

MAR 04 '99
BURLINGTON
RESEARCH.
03:18PM BURLINGTON RESEARCH P.9i20
Aquaac aloassay Testing - Aquatio Toxicity Reduction Evaluatioru
Chemical Product Environmental Assessn+onts - NPDES Tasting
Reporting & Data Hwang 8wAm
1302 Belmont Street - Burlington. NC 27215 -6935 a Phone [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: B& Roy Rittic
SAMPLE DESC: SPRUCE PINE
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 03/02/'9916:15 SITE: 15 PPM
IPARAMETER
Fluoride
EPA 340.2
DATEITIME /ANALYST
WORK ORDER#: 90104-004
RECEIVED: 03103/99
REPORTED: 03/04/99
PO NUMBER:
MOL RESULT
Started 0310419910:00 0.10 15.9 mgIL .'
Analyzed 03/04/'99 by JCB at BRI - Burlington
Ceri�60od��apphnia 48 -Hour Acute Static Bioassay Started 03102/9916:45 N/A > 100 LC50%
£P,A0491027F Analyzed 03/04/99 by JCB at BRI - Burlington
MQL = Minimum Quantitation Limit
Page 44
VWtorEmkonment lgw*as -Eden Page 4 %WEn%&orrnarW$aMoaa- Kinston
Division of Butington Research. Inc. ONWon of BudftWn Reseerctt, Inc.
3770 W. Meadow Road • Eden, NC 27288 too E. Gordon Sted - Kinston, NO 26501
Phone (336) 823.x921 - Fax (336) UH975 Phone [phone] - Pax [phone] 43
ow:,"

MAR 04 '99 03 :19PM BURLINGTON RESEARCH P.1120
• • Aquatle bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product ErrAroNnental Assessments • NPDES Testing
Reporting S Data Handling Sef&"
BURLINGTON 132 Belmont Street • Burpngton, NC 27215 -6935 • Phone [phone] • Fax [phone]
RESEARCH
ANALYTICAL REPORT
CUSTOMER: 13niink Corp.
REPORT TO: W. Itoy Rittle
SAMPLE DESC: SPRUCE PINE
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 03/02/9916:20 SITE: 20 PPM
IPARAMETER
DATEf l'1ME/ANALYST
WORK ORDER #: 9C104.005
RECEIVED: 03/031'99
REPORTED: 03/04/'99
PO NUMBER:
MOIL RESULT
Fluoride Started 0310419910:00 0.10
EPA 3402 Analyzed 03/04/99 by JCB at BRI - Burlingtom
Ceriodapphnia 48 -Hour Acute Static Bioassay Started 03/02/9916:45 N/A
EPA,600491027F Analyzed 03/04/99 by 7CB at BRI - Burlington
MQL = Minimum Quantitation Limit
20.8 mgt. A
> 100 L.C50%
Page 46
%terF.nvkornenW SenAces -Eden Water Ertvlronmanfaf SOMCOQ- iatsion
DIYWon of f3cxWon Research, Ina pSgC S Division of Su Rion Rosaarch, Inc. Q
370 W. Meadow Road • Eden. NO 212 100 E Gordon Street • KhMon. NO 28501
Phone (sas) 6S "MI - Fax (338) 62MO78 PhMe [phone] • Fax [phone]
N •.Y

M.21.

MAR 04 '99 03:21PM BURLINGTON RESEARCH
• P. 13/20
Aquatio Bioassay Tasting - Aquatic Tesicity Reduction Evaluations
Chemical Produd Envirw"ntsl Asswsmenfs - NPOES Testing
Reporting & Data Handling Servic"
BURLINGTON 1302 Belmont Street - Sudington, NC 27216.6935 - Phone [phone] a Fax [phone]
RESEARCH - -
ANALYTICAL REPORT
CUSTOMER: 13nintin Corp.
REPORT TO: Mr. Roy Rittle
SAMPLE DESC: SPRUCE PINE
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 03/02/9916:25 SITE: 25 PPM
WORK ORDER #:
9CI04 -006
RECEIVED:
03/03/99
REPORTED:
03/04/99
PO NUMBER:
PARAMETER DATERIME/ANALYST MOL RESULT
Fluoride Started 03/04/9910:00 0.10 27.0 mg/L
EPA 3402 Analyzed 03/04199 by JCB at BRI - Burlington
Ceriodapphnia 48 -Hour Acute Static Bioassay Started 03/02J9916:45 N/A > 100 LC50%
EPA600491027F Analyzed 03/04/99 by JCB at BRi - Burlington
MQL, = Nnimum Quantitation Limit
Page 48
W&WEnWrorxnenWSanAm -Eden
page 6 Vft1*( vonw1wS ws- non Dvsion d 8urVon Reearch, Ina
Divtslon d burrmmggtan Ra:aarch, kro.
978 W. Meadow Road • Eden, NG 27288 100 E. Gordon Sveet • Kinston, NC 28501
Phone [phone] - Fax (336) 623,5878 Phone [phone] a Fax [phone]
ees v�

MAR 04 199 03:23PM RRLINGTON RESEARCH P.is/20
FR"11 Aquatic Bioea %sdnq • Aquatic Toxicity Redwson &Wuatiom
Chemical Prodsict ErMrorunenW Assesamonts • NPDES Tasting
Rspordng A Date HeW&V Services
BURLINGTON 1302 Belmont Street • Burlington. NC 27215 -6935 • Phone [phone] • FOY [phone]
RESEARCH,
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: Mr. Roy R.ittle
SAMPLE DESC: SPRUCE PINE
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 03/02/9916 :30 SITE; 90 PPM
WORK ORDER #:
9CI04007
RECEIVED:
03)03/99
REPORTED:
03/D4)99
PO NUMBER:
PARAMETER DATEMMEIANALYST MOL RESULT
Fluoride Started 0310419910:00 0.10 30.5 mg(L `
EPA 340.2 Analyzed 03/04/99 by ]CB at BRi - Burlington
Ceriodaphnia 48-Hour Acute Static Bioassay Started 03M916:45 NIA > 100 LCs0%
EPA600491027F An0lyrzed 03/04/99 by 7CB at BRI - Burlington
MQL = Minimum Quantitation Limit
Page 50
WaterEnvmnnvntalSerAM -Edon Pap 7 lfihro 9Mforrrre W Services- Kinston
t9vk1on of Bur koon Resoarch. Inc, oivieton of B ton Research, u,o
370 W. Meadow Road • Eden. NO 27288 '100 E. Gordon" • Kinston. NC 28501
Phone (M) 62.021 • Fax [phone] Phone [phone] • Fax [phone]
am ua

. MAR 04 '99 03 :25PM RJRLINGTON RESEARCH P.17/ew
Aquatic Bioassay TGating - Aquatic TWelty Reduction Evaluations
Chemfcal Product Environmental Assessments - NPDES Testina
Reporting 3 Data Handling SOMC08
BURLINGTON 1302 Belmont Street s Burlington, NC 2721548935 • Phone [phone] • Fax [phone]
RESEARCH
ANALYTICAL REPORT
CUSTOMER: 'Unimin Corp.
REPORT TO: W. Roy Rittic
SAMPLE DESC: SPRUCE PINE
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 03/02/9916:35 SITE: 40 PPM
PARAMETER
Fluoride
EPA 340.2
DATEinME/ANALYST
WORK ORDER P. 9C104.009
RECEIVED: 03/03/99
REPORTED: 03104/99
PO NUMBER:
MQL RESULT
Started 03/04/9910:00 0.10 41.5 mVL
Analyzed 03//04/99 by ICE at Btu - Burlington
Cerlodaphnia 48 -Hour Acute Stadc Bioassay Started 03MN916:45 N/A
IEPA600491027F Analyzed 03/04199 by JCB at URI - Burlington
MQL = Minunum Quantitation Limit
> 100 LC50%
Certifications:
SRI - Burlington
NC Chemistry: #85, Biomonitoring: #002, Drinking Water: #37743, Radiation License: #001 -0904 -00
VA SWCB ID: #000061, Drinking Water. #00018
SC Laboratory m: #99042
EPA Chemistry Lab ID: N000137, Bioassay Lab ID: NC2721500
Page 52
Water Envftrlmontal Ssr*as - Eden Water En*onrnenml s 86rv1* - l&won
D' olon of Bufington Research, Inc. Page 8 Division of Burlington Asscuch, Inc. I--/
370 W. Moadaw Roed s Eden, NC 27288 100 E Gofdon Street - )Grww, NC 28501
Phone [phone] - Fax [phone] Phone (252) WA -9821 - Fax [phone]
NM VN

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BURLINGTON RESEARCH, INC.
[Ell%
f
1302 Belmont Stteat
8udinglon. NC 27215.6935
��° "e�33ti ;570.4698
l..l +� •• ��• •• -••-
Edon, NC 27288
Fax �(33G�Gg?�3.58T�
- fWIDIWy,wwd.. �-
Phone [phone]'
Fax 252;0.9520 -9922
CLtENT:_.L17 /i/i SEND REPORT 'iO: �r' !. f'•`-�'
Facpliy/Sfte• .��D /1y� �i ��Gr,'�' ♦ Phone:,✓'i%.i�1 Fax:
Sampler: fpnw)�� IA -,154M �Signafumt n Purchase Order No.: - - - -
O LE - zMPLETYPE
U �
Preerneon Codes: C
COLLECTION
SAMPLE FARTED ENDED Uj a COMPOSITE m a ANALYSIS TEMP. A - Ice' . E = NtiOH
ID o GRAB �" REQUIRED C . B = HNO3 ' F - None
§!!;8 HAND AUTO z ° " �� C = MO4 G•= CUPR�
TIME TIME q k' _ - 0 = HCI H = HCHO
Yesj No _f.11v1
: f 1 5' : I r! l ��i Ir�l,�•�r; /v
IX 7,-;iyw
�
Yes to ff
Yss1 No .
I i No
Yes; No
Yes No -
• Yes Ab
Yast No
yagi NO
1- was the sample dechlorinated at time of collection? Yes ❑ No 01 /;r Will the results be used for regulatory monitoring purposes? Yes 0
FOR CLIENIT USE OJ4LY FOR ONLY
N hed Received In Lab FROM Sig.) Date:
u' � ig..y / 8• Time:
br; DOW Tiima
VT Method of Shoment ;/
-14 1 �G
M4T ?4!
x
Method of ShOnod
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