NC0000175_Wasteload Allocation_19990326

NPDES DOCUHENT :;CANNING COVER SHEET
NPDES Permit:
NC0000175
Unimin Quartz Operation
Document Type:
Permit Issuance
(WaSte1Oad Allocatio -,.
Authorization to Construct (AtC)
Permit Modification
Complete File - Historical
Engineering Alternatives (EAA)
Correspondence
Owner Name Change
Instream Assessment (67b)
Speculative Limits
Environmental Assessment (EA)
Document Date:
March 26, 1999
'Miss dactirnertt is printed on reuse paper - ignore arty
content on the rezzerse wide

urnmin
Quartz Operation
P. O. Box 588
Bakersville Hwy.
Spruce Pine, NC 28777
[phone]
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 toxicity
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

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 results, 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.

Once again, we appreciate the time provided by departmental staff in listening to
our proposal. We anticipate receiving your letter confirming DENR's re -permitting
strategy to allow for an orderly renewal of each of our individual NPDES permits.
cc: Forest Westall
Regional Supervisor
Water Quality Section
Division of Water Quality
NC DENR
29 Woodfin Place
Asheville, NC 28801
Joe Turner
Plant Manager
The Feldspar Corporation
P. O. Box 99
Spruce Pine, NC 28777
Sincerely,
5. 9
Charles F. Stover
Regional General Manager
Unimin Corporation
Matt Matthews
Aquatic Toxicology Group Leader
Water Quality Section
ND DENR
4401 Reedy Creek Road
Raleigh, NC 27607
Dennis Buchanan
Plant Manager
K-T Feldspar
P. O. Box 309
Spruce Pine, NC 28777

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
Chronic Toxicity Test
Acute Toxicity Results
12-13
14-35
36 — 55

1)Df4 FD 12_._
CERiODAPITNIA DUBIA ACUTE AND CONIC TOXICITY TESTING
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 Ceriodaplm a prior to the testing outlined below, so that the
q
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) the
necessary to perform the conditioning above, as well as the water required for
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 successful 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 total) Chronic Toxicity Testing (9 totall
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 pprn F 3.0 ppm F
30.0 ppm F 4.0 ppm F
40.0 ppm F 8.0ppm F
16.0 ppm F
5. The successful bidder will provide full written document on form ATIor AT3,
(plus bench sheets,) as appropriate for each of the 17 tests outlined above. Those
forms should include residual chlorine, pH, 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
1

Chart 1 - Chronic Toxicity
Reproduction vs. Fluoride Concentration
ETT Laboratory
Average
Reproduction
Fluoride
Measured
PPM
Case
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
25
0 20
tri
2 15
a.
aw 10
a)
co
Q 5
0
Reproduction vs. Fluoride
Concentration
0
4 8
Fluoride PPM
-�- ETT
12
16
Page 2
2

Chart 2 -Chronic Toxicity
Reproduction vs. Fluoride Concentration
(2 Labs)
ETT Laboratory
Burlington
Average
Reproduction
Laboratory
Fluoride
Conc. PPM
Measured
Average
Reproduction
Fluoride
Measured
PPM
Case
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
30
c 25
0
z 20
0
d 15
d
13) 10
L.
a
5
0
Reproduction vs. Fluoride
Concentration
0
r
4 8
Fluoride PPM
-♦- Burlington -■- ETT
12
16
Page 3
3

Chart 3 - Chronic Toxicity
Average of Both Labs
ETT Burlington
Grand Averages
Fluoride
Design
PPM
Average
Reproduction
20.6
Average
Reproduction
19.2
Grand
Average
Reproduction
19.9
Grand
Avg. % of
Control Reproduction
100%
0
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%
Average Reproduction
25
20
15
10
5
0
Reproduction vs. Fluoride Concentration
0
4 8
Fluoride PPM
12
--� Grand Avg. Reproduction
16
Page 4

TABLE 1. SUMMARY OF TEST RESULTS
Zemex Corporation Fluoride Testing of Ceriodaphnia Dubia
by ETT Environmental Inc.
2/23 - 3/4/99
Chronic Bioassay Test Results
Test Level Test Results
Fluoride Concentration mQ/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 Bioassay Test Results
Test Level Test Results Fluoride Concentration mW/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

03/24/99 WED 10:45 FAX [phone] THE FELDSPAR CORP.
Mar-24-99 10:14A ETT Environmental, Inc. 844 877 893t5
Zoos
P 01 . '"_ TT f
r vironmentet, Inc.
[phone] • FAX [phone]
P.O. Box 16414, Greenville, SG 29606
Measured Fluoride Concentrations
Zemez - N. Toe River Water Spiked w/ Fluoride
February 1999
4 Craftsman Court, Greer, SC 29650
Acute Toxicit' Tests
Nominal Measured
Concentration Concentration
0,0 mg/L
5.0 mg/L
10.0 ma
15.0 mg%L
20.0 mg/L
30.0 mg/L
40.0 mg/L
L5 .
Chronic Tlcxicity Tgctc
<0.1 mg!L
4.5 mg/L
8.7 mg/L
13.0 mg/L
IS.0 mg/L
24.0 mg/L
33.0 mg/L
/IoI-v,,, .
Nominal Measured
Concentration Concentration
0.0 mg/L <0.10 mg/L
0.5 mg/L 0.59 mgfL
1.0 mg/L 0.98 mg/L
1.5 mg/L 1,4 mgfL
2.0 mg/L I.8 mg/L
3.0 mg/L 2.8 mg/L
4.0 mg/1.. 3.7 mg/L
8.0 mg/L 7.1 mg/L
16.0 mg/L 14.0 mg/L
CJ�S 3/zN 95
Fluorides were measured using Standard Methods 186 Edition SM 4500-F C.
NC Certification No. 4 02 .
Submitted By:
Robert W. Kelley, Ph.D.
Page 6

. nvr - - = v•+ . r ct r G r r v -t ru n, nC rl Ld I, 1PC . LSOw 23/ / L7y.323
P.04
Effluent Aquatic Toxicity Report FornUPhase It Chronic Ceriodaphnia
Facility: Zemex River Water Spiked wl Fluoride
Laboratory Performing Test: ETT Environmental Comments:
Pipe4
Courry: Mitchell
S9nature o/
$gnature d
Sample Information
Collection Start Date
Grab
Composite (Duration)
Hardness (mg/L)
Spec. Cold. (umhos.cm)
Chlorine (mg/L)
Sample temp. at Receipt
$ampta 1
2/23199
X
<0.05
0.6
Srnpk 2
Comm!
Control
Effluent %
'0.5 mg/L
Effluent
# Young
1
23
Test
Info
Trptttment
pH lnd.
pH 6inal
D,O.Ind
D.O. Final
Temp Ind
Trmp r✓+al
Star) Date
2/24/99
Time
1800
- End Date
03/04/99
Time
1800,
suet
ca12
Days
Stert
9a72
13¢75
16mgti
16
16
control
control
/
control
7,13
7 ZS
7.37
7.10
7.06
7.60
7.58
7.61
•
7,56
a 7.42
7.50
7.32
0.4
8.0
e.5
8.2
8.7
61
0,7
8.7
6.6
8.6
8.7
8.8
24.2
25.2
24.2
24.2
^
25.2
24.2
24.2
25.2
24.2
24.2
25.2
24.2
Organism #
2 3 4 5 6 7 8 9 10 11 12 ww,
23
20
18
9
19
19
23
L
21
lost
lost
20.6
Adult
L
L
# Young
1 2 3 4 5 6 7 8 9 10 11 12 Moan
19
19
22
20
21
20
8
19
9
20
lost
lost
Adult
,L
L
1 2 3 4 5 6 7 8
Young: 22
23
16
19
19
21
20
21
L
17
11.0 mg/L
Effluent %
Adult
L ,L
1 .2 3 4 5 6 7 8
L
L
L
17.7
1d%
Final Coot Mort. SG
% Corn 3rd Brood
Chronic Test Results
100%.
cmtloI Repro cv 10%
48 Hour Mortality
Carrot NYC
0of10
I0af10
Significant? No
Final Mortality Sign. 1
I of No. conc.
Reproduction Analyses r�:D 9 10 Mean Repro LOEC= EC-
.20 19.8 Method, Dunnetl's T Test
nea' Po Normal Dist? yes Method snap -mks
L 4%, Statistic Critical 0.930
Equal Val no Method eartserts
Statistic Critical 15.10
20 18,6 t-Test
i6 gede" Menet Donnee,Y
L 1 10% Effuent % t Critical
9 10 wean
# Young
18
17
19
16
20
19
19
19
19
1.4 mglL
Effluent °%
Adult
L
L
1 2 3 4 5 6 7 8 9 10 Veal.,
-*Young
Adult
Effluent %
1 2 3 4 5 6 7 8 9 10 scan
# Young
Adult {
'so wa
IIti�r�l'#tratyst :r' •
ResUl�" RiRS3/ Alti br
Chtoni6Va16e
NOEC=
•MAIL Environmental Sciences
TO: Div. of Environmental Management
N.C. Dept. otEHNR
4401 Reedy Creek Rd.
Raleigh. NC 27607
DEM Form AT-3 Rev, 11/95
inn r 1
Page 7
L i
'd2I0D 2IVdS11133 2111 COZO 29L 1701. ZVd Z ' : LO 3!1Z 66/9T/C0

03/16/99 TUE 11:49 FAX [phone] THE FELDSPAR CORP.
mar-i(-99 11:46A ETT Environmental, Inc. 864 877 6938
CZ 0 0 2
P-pl
Effluent Aquatic Toxicity Report Form/Phase 1I Chronic Ceriodaphnia
Facility.
Zemex River Water Spiked w/ Fluoride (Revised wl Measured Concs.)
County: Mitchell
Laborato Performing Test ETT Environmental Comments:
Signature of
Sample Information
Collection Start Dote
Grab
Composite (Duration)
Hardness (mg/L)
Spec. Cond, (urnhas.cm)
Chlorine (mg/L)
Sample temp, at Receipt
Sample 1
V23/99
<0.05
0.6
Stemple 2
Cmlml
Control
Test
Info
Treatment
PI Inn.
pH Feral
0,0. Ink
0,0. Find
Tamp Ink
-romp Final
Start Date
2/24/99
ISlart I1:
h12 1
14 rngR,
14
Time
1800
Day5
14
End Date
03/04/99
Start
t 4 rpl
Time
1800
Dart
control
De/5
c nlrol
7,13
7,25
7,37
7.10
7,36
7.60
7.55
7,61
7.Sc
7.42
7,5,0
7.32
6.9
9.0
8.5
5.2
B.7
6,6
6.7
8,7
8.8
8.8
8.7
8,8
2.4.2
25,2
24,2
24.2
25.2
24,2
24.2
25.2
24.2
24.2
25.2
24.2
Organism 0
1 2 3 4 5 6 7 8 9 10 11 12 Mean
# Young
23
23
20
18
19
19
19
23
L
21
-lost
Final Cora Mon. %
% Cool 3rt1 Entree
Contra; Revco CV
Chronic Test Results
100%
10%
lost
Adult
Effluent % #t Young
11.8 mg/L Adult
Effluent %
L
1 2 3 4 5 6 7
17
18
19
16
17
16
20
20.6
8 9 10 11 12 Moan
19
17
19
lost
lost
# Young_
1
19
2
L
_L
L
L
17,8
% Rea
13%
48 Hour Mortality
Conlroi
LID of 10
Significant?
Final Mortality Sign,
twc
0 of 10
No
or [No. conc7
Reproduction Analyses
es
2 3 4 5 6 7 8 9 10 Mn Repro LOEC= 7.1 mg/L NoEC-
v
1 17,9 Method: Ounnett's T Test
TRca Normal Dist? yes Method Snap. fzs
L 13% Statistic 0.961 Critical 0.930
Equal Var? no Method 84rrferts
16
21
20
19
17
2.8 mg/L
Adult
L
L
L
L
L
22
r
D
2
20
L
1 2 3 4 5 6 7 8 9 10 moan
Effluent % '# Young
16
8
21
10
16
15
23
21
17
18
3,7 mg/L
Adult
16,5
stag
20%
Effluent %
# Young
1 2 3 4 5 6 7 8 9 1 Q tan
9
13
8
14 17_
11 17
18 6 18 13.1
'St -ties 7.1
7.1 mi/L
Effluent
Adult
# Young
1 2 3 4 5 6 7
7
1
1
121 3
3 10
14 mg/L
Adult
L IL
MAIL Environmental Sciences
TO: Div. of Environmental Management
N,C, Dept, of EHNR
4401 Reedy Creek Rd,
Raleigh, NC 27807
_D L
L 36% 14
8 9 10Mmn
7 6 2 �l5.2
L L L 75%
3.7 mg/L
Statistic 19.20 Critical 15.10
t-Test
Method: Punnets
EtflAnt m4LE, t Critical
1.8 1,50 2.39
2.8 1.45 2.39
3.7 2.21 2.39
4,Db 2.31-
8.37 2.39
AnPlY4111
Result = PASS/FAIL or
Test LOEC: 7.1 mg/L NOEC= 3.7 mg/L
Chronic Value= 5.1 mg/L
DEM Form AT-3 Rev. 11/95
Page 8
IN
7-

03/-24/99 WED 10:44 FAX [phone] THE FELDSPAR CORP.
mar-24-99 10:13A ETT Environmental, Inc. 864 877 oWsts
�003
nvlrontnsntal, Inc.
P.O. Box 16414, Greenville. SC 29806
[Client: Feldspar J
n Date: 2 4i99 Time: 1800
e Date: 2/26/99 Time: 1800
TA
[phone] FAX [phone]
4 Craftsman Court, Greer, SC 28650
Sample 1D: Zemex Lab 1D# T11364
Set By: SC Test Species:
Ended By: RK ICerlodaphrila dubia
Dilution Water: MFISF
[Measures
-
Rep.
-- - - -Cumulative
orprLama
Morality
2der 411hr Mr 951.,
Mean 1
�+-
0%
.
A
3'
0
0
_
<4.t mg1L
8
5
0-0
tCw
5�
0�
0.
D
S
0
0
Al
4.5 mg/L
($,M,ft of ?.uy
A
5
0
1 0
0%
B
5
0
0'
C
5
' 0
0
8.7 mg/L
(eeam;nat ru N
0'%a
B
5
0`
04
,
C
5'
a
0
,
13 mg'L
(wawa Is.0)
0%
B
5
0'
0
C
0
0
0•
0
5
0
0
18 mg/L
(rmmival20.0)
A "-'
5'
0'
0'.
0%
: B+
5,'
0.
0
C
5
0
0
D
5
, 0
0
25 mg/Ls
(nominal)
A
S
0.-
0
0%
B
5
' 0-
0r
C
5
0
0
,
D
5
_ 0
0,
STATISTICAL ANALYSIS
48 Hour LCSO > 33 a sgiL effluent
95% Confidence Limits: Upper NA
Lower. NA
`Method: Spearman Karber
COMMENTS:
WATER QUALITY DATA
Measured Va1Ui
&xT eter
'1
units
Mu 2Ahr sir 72he e+akr
IMO
111111
Dissolved
Oayson
rttg/L
mom-
iva-ren1"1
8.6
pas,aasewal
9.5
PH
prrnn.,.d
7.86
poteteoesst
.
7.19
8.8
7.42
'Dissolved
Oxygen
mg/L
milt.
pr►rrue.af
teemswit
9.4
PH
prm weave
ttaat•tmcve
7.09
Dissolved
Oxygen
nigi1.
vrr.tssewat
puun ewe
8.8
92
pH
`ng/L
pretcns.at
..us•sf
7.26
11
7.14
Dissolved
Q en
mg4.
engll.
pripetvewif
patvrsund
8.7
7.27
8.7
7.64
-
9,0
PH
Rtgamind
pat•nsewd
7.17
Dissolved
Oxygen
mglt.
mgll.
peAssmil
por<.r+eaee.d
9.2
PH
v[Mirreeat
o° i-i w it
7.✓
Dissolved
01Y81m
` 8IL
ingfL
pr♦nrveewf
cst•to. al
8.6
8.8
pH
`
praa+w.t
_oovraeornl
7.93
, 7.31
•Nominal concentration.
All concentrations are expressed as measured concentrations
except the 25 mg/L concentration for which no measured
concentration was available.
Approved By: "
Date: 7
Page 9
9

03F•24/99 WED 10:45 FAX [phone] THE FELDSPAR CORP.
islar- 24 -99 1O : 13A ETT Environmental, Inc. 864 8i i OW4i,
Z 004
[phone] • FAX [phone]
P.O. Box 164i4, Greenville, SC 29606
Client: Feldspar — Set By: SC
Start Date: 2/24/99 Time: 1800
End Date: 2/26/99 Time: I1 S00 Ended B : RK
rbilutioniWat�e: Ma r
WATER QUALITY DATA
Measured Value
qet 2slt sfbr "Ms
8,8
4 Craftsman Court. Greer, SC 29650
MORTALITY DATA
Measures
Rop.
# [Cumulative Mortality Mean
2asr +5bI Ust 'fit %u
24 mg/L , B
(mx.0..t .o),C
r 0
S
4'76
o
1
A
33 mglL `' g�
tiud•ao)
5 0 0
5 0
D
0%
A
F3
D
A
8
A
.1111111
Sample ID: Zeroes
STATISTICAL ANALYSIS
Parameter
Dissolved
Oxygen
pH
Dissolved
Oxygen
pH
'Dissolved
Oxen
pH
Dissolved
Oxygen
PH
Disco{vc�i
Oxygen
PH
Dissolved
Oxyrn
pH
units
mg/L
Ingf 1.
freeemni
mg/L po*tvas.s1
mg/I.
mg/L.
mgiL
mg/L
progawall
t
miqcocwa
onk4easwai
peal
YAWL perrerewil
mg/L ^ !
mNt.
mgli.
peal
PuiPleatiVel
prelevrini
Icrammewil
'Nominal concentration.
48 Hour LC50 > 33 mlEJi. effluent All concentrations are expressed as measured concentrations
95% Confidence Limits: Upper: NA except the 25 mg/L concentration for which no measured
Lower: NA concentration was available.
8.7
1
724.
Lab ID# T11364
Test Species*.
Ce loss jIMla dubta �.
cur
7.52
8.8
8.6
7.31
7.s7
•
Method: Spearman Kerber
COMMENTS:
Approved By: Aa��!
Dare: 7 -2, 4 /
Page 10
10

MAR 04 '99 04:14PM BURLINGTON RESEARCH
P.2/2
BURLINGTON
RESEARCH,
11- g VE 2.. S V Mw+Pee-- Y C) F 9,1MU L-r
Aquatic Bioassay Testing • Aquatic) Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
1302 Belmont Street • Burlington, NC 27215-6935 • Phone [phone] • Fax [phone]
Unimin Corporation Fluoride -. Testing
2J24-3/3/99
CI__Egagj3ioassay Test Results
est Level
Test Result • Fluoride Concentration mglL_
0 Pass . 0.11
0.5 Pass 0.51
1 Pass 0.98
1.5 Pass 1.47
2 ' Pass 1.93
3 Pass 2.89
4 Pass 3.86
9 Pass 7.2
16 Pass 48 9 15 .9
CiE
r+tte Bioassay Test Results
Test Level Test Result Fluoride Concentration mglL
0 >100 °% LC50 * 0.11
5 >100°%LC50 6.24
10 >100 % LC50 10.4
15 >100%LC50 15.9
20 >100 % LC50 20.8
25 >100 % LC50 27
30 >100 °% LC50 30.5
40 >100 °% LC50 41.5
* > 100% indicates no toxicity Le no mortalities
were observed at any concentration of fluoride.
Page 11
Water Environmental Services - Eden
Dirtision of Buffington Research, Inc.
370 W. Meadow Road • Eden, NC 27288
Phone [phone] • Fax [phone]
s*cs v81
Page 1
Water Environmental Services -Kinston
Division of Burlington Research, Inc.
100 E Gordon Street • Kinston, N 28501�
Phone [phone] • Fax (252) 5 o-

MAR 04 '99 04:13PM BURLINGTON RESEARCH
4 TO LJHIMIN QUARTZ
P.1/2
Cam,
APPLNDI X 2_, — 1� Ut2C.ttJG,TQtJ R.sple.0144 Axis,
FAX Transmission Sheet
Burlington Research, Inc.
1302 Belmont Street
Burlington, NC 27215-6935
Phone: [phone]
FAX: [phone]
FAX ONLY ,_ X FAX & MAIL
DATE: March 4, 1999
TO: Roy Rittle
SU *th12(
COMPANY: onimin
FAX #: [phone] ALU T E
ToXkLkl'i
FROM: John Bauxnmer, BRI Biomonitoring lab Manager
SUBJECT: Completed reports
You should receive 2 pages including this cover sheet. 1f yore do not receive all pages, or
have a question regarding content please call me at 910/570-4661, F.xL 289.
COMMENTS:
Roy:
Completed table
Questions, please call
John
Page 12
)

MAR 04 '99 04:14PM BURLINGTON RESEARCH P.2/2
II 1
BURLINGTON
RESEARCH
Aquatic BIoassay Testing • Aquatio Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
1302 Belmont Street • Burlington. NC 27215-6935 • Phone [phone] • Fax [phone]
Unimin Corporation Fluoride - Testing
2/24-3/3/99
Chronic_Bioassay Test ResuttS
Test Level , Test Result • Fluoride Concentration mg/I,
0 Pass . 0.11
0.5 Pass 0.51
1 Pass 0.96
1.5 Pass 1.47
2 Pass 1.93
3 Pass 2.89
4 Pass 3.86
8 Pass 7.2
16 Pass =� IS .9
Acute Bioassay Test Results
CA
Test Level Test Result Fluoride Concentration mg/L
0 >100%LC50* 0.11
5 >100 °% LC50 6.24
10 >100 % LC50 10.4
15 >100%LC50 15.9
20 >100 % LC50 20.8
25 >100 % LC50 27
30 >100 % LC50 30.5
40 >100 °% LC50 41.5
* > 100% indicates no toxicity Le no mortalities
were observed at any concentration of fluoride.
Water Environmental Services - Eden
Dildsion of Burtington Research, Inc.
370 W. Meadow Road • Eden, NC 27288
Phone [phone] • Fax [phone]
Page 1
_
Page 13
Water Environmental Services -Kinston
Division of Burlington Research, Inc.
100 E. Gordon Street • Kinston, NC 28501
Phone [phone] • Fax [phone] ) z.

MAR 04 '99 02:46PM BURLINGTON RESEARCH
• TO UNIMIN QUARTZ
P.1/22
tab
FAX Transmission Sheet
Burlington Research, Inc.
1302 Belmont Street
Burlington, NC 27215-6935
Phone: [phone]
FAX: [phone]
FAX ONLY _X_,,,
DATE: March 4, 1999
TO: Roy Rattle
COMPANY: Unimin
FAX & MAIL
C,1-A 12_ oth
TOM C\TY
-r -__,,
FAX #: [phone]'(--
FROM: John Baummer, BR1 Biomonitoring Lab Manager
SUBJECT: Completed reports
You should receivpages Including this cover sheet. If you do not receive all pages, or
have a question regarding content, please call me at 910/57 4661, Ext. 289.9/
COMMENTS:
Roy:
Completed reports
Questions, please call
John
3/�
Page 14

MAR 04 '99 02:46PM BURLINGTON RESEARCH
P.2/22
BURLINGTON
RESEARCH
Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
1302 Belmont Street • Burlington, NC 27215-6935 • Phone [phone] • Fax [phone]
March 4,1999
Unimin 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 Workorder 9B607. Please call if you have any questions.
Thank you.
Sincerely,
BURLINGTON RESEARCH, INC.
ohn C. Baummert
Manager, Biomonitoring Dept.
[phone] Ext, 289
Page 15
214.21ho
Water Environmental Services - Eden
Division of Burlington Research, Inc.
370 W. Meadow Road • Eden, NO 27288
Phone [phone] • Pax [phone]
Water Environmental Services -Kinston
Division of Burlington Research, Inc.
100 E. Gordon Street • Kinston, NC 23E01
Phone [phone] • Fax (252) 62a-9922

MAR 04 '99 02:46PM BURLINGTON RESEARCH P.3/22
BURLINGTON
RESEARCH
Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Poporting & Data Handling Services
1302 Belmont Street • Burlington, NC 27215-6935 • Phone [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: Mr. Roy Rittle
SAMPLE DESC: FEB, MONITORING
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 02/24/99 11:30 SITE: 0 ppm
WORK ORDER #: 9B607.001
RECEIVED: 02/24/99
REPORTED: 03/04/99
PO NUMBER:
PARAMETER
DATE/TIME/ANALYST MQL
RESULT
Fluoride by IC Analysis
EPA 300.0
Started 03/02199 11:53 0.10
Analyzed 03/02/99 by TAR at BRI - Burlington
0.11 rng/L
Ceriodaphnia Pass/Fail Chronic
NCDEM 9/89
Started 02/24/99 14:00 NIA
Analyzed 03/04/99 by 7CB at BRI - Burlington
Pass Pass/Fall
MQL = Minimum Quantitation Limit
Page 16
Water Environmental Services - Eden
Division of Burlington Research, Inc.
370 W. Meadow Road • Eden, NC 27298
Phone [phone] • Fax [phone]
6fi4 IAD
Page 1
Water Environmental Services -Kinston
Division of Burlington Research, Inc.
100 E. Gordon Street • Kinston, NO 28501 ) S
Phone [phone] • Fax [phone]

. MAR 04 '99 02:47PM BURLINGTON RESEARCH
P.4/22
Effluent Toxicity Report Farm - Chronic Pass/Fail and Acute LC5O
Facility: FLUORIDE SAMPLES
Dote: 03/04/99
MPDESif: NC
Laboratory Performing Teats BURLINOTON RESEARCH. INC.
x
Sigture of Operator in Responsible Charge
snature of Laboratory Supervisor
Pipet: County: MITCHELL
Counts: 0 PPM: North Toe River
mmale
* PASSED: -8.68% Reduction
work Order: 98607-001
MAIL ORIGINAL TO:
North Caroline Ceriodaphnia
Chronic Pass/Fail Reproduction Toxicity Test
CONTROL ORGANISMS
Environmental Sciences Branch
Div. of Environmental Management
N.C. Dept. of EHNR
4401 Reedy Creek Road
Raleigh, North Carolina 27607-6445
1 2 3 4 5 6 7 8 9 10 11 12
Chronic Test Results
Calculated t s •0.757
Tabular t s 2.518
% Reduction = •8.68
d Young Produced
1211 24
20 79
21
28
19
N'15
12
13
Adult (L)Ive (D)ead
L
L L L
L IL
Effluent %: 100%
TREATMENT 2 ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12
4 Young Produced 21 15
21
24
17
21
18
23 22 21 9 18
Adutt (L)Ive Mead 1L
L L L
% Mortality
Avg.Reprod.
0.00
Control
17.64
Control
0.00
Treatment 2
19.17
Treatment 2
Control CV
31.291%
% control orgy
producing 3rd
brood
83%c
PASS FAIL
[:::
Check One
•
pH
control
Treatment 2
D.0.
Control
Treatment 2
1st sample
7.59
7.30
7.94
1st sample 2nd sample
7.46 7.16
L
7.60
7.21
s s
t e t e
a n 8 n
r d r d
t t
1st sample 1st sample
117
8 . 0
8.4
8.2
1817
8.8.3
7.43
7.31
6,86
7.41
t e
a n
r d
t
2nd stele
8.1
8.5
8.4
8.5
LC50/Acute Toxicity Test
Complete This For Either Test
Test start Oates 02/24/99
Collection (Start) Date
Sample 11 02/24/99 Sample 2:
Sample Type/Durotfon
arab
Carp.
Duration
hrs
Sample 1 X
Semple 2 hrs
Hardness(t/t)
spec. Cand.(Amhos)
Chlorine(mg/l)
Sample temp. at receipt(•C)
L
u
T
2nd
1st P/P
8
A
M
P
A
M
P
40
tag
85
40.5
KAU
n/a
3.2
(Mortality expressed as x, combining replicates)
x�,
Concentration
Mortality
start/end
LC50 tt ..__-
Method of Determination
95% Confidence Limits
Moving Average ,,,. Probst
Y -- _ ,,%
Spearman Karber _ Other •„_
__
pH
Organism Tested: Ceriodaphnfa dubia
buration(hrs):
Notes Please
Complete This
Section Also
Control
start/end
High
Conc.
C.O.
Page 17
Copied from OEM form AT-1 (3/87) rev. 11/95 (DUBIA ver. 4.32)
t6

MAR 04 '99 02:47PM BURLINGTON RESEARCH P.5/22
BURLINGTON
RESEARCH
Aquatic Bioassay Testing • Aquatic TbxicIty Reduction Evaluations
Chemical Product Environmental Assessments • NPDE3 Testing
Reporting 8 Data Handling Sorvicas
1302 Belmont Street • Burlington, NC 27215-6935 • Phone [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: Mr. Roy Rittle
SAMPLE DESC: FEB. MONITORING
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 02/24/99 11:35 SITE: 0.5 ppm
WORK ORDER #: 9B607-002
RECEIVED: 02/24/99
REPOH I bD: 03/04/99
PO NUMBER:
PARAMETER
DATE/TIME/ANALYST
MOL RESULT
Fluoride by IC Analysis
EPA 300.0
Started 03/02/99 11:53 0.10 0.51 mg/L
Analyzed 03/02/99 by TAR at BRI - Burlington
Ceriodaphnia Pass/Fail Chronic
NCDEM 9/89
Started 02/24/99 14:00 N/A Pass Pats/Fait
Analyzed 03/04/99 by JCB at BRI - Burlington
MQL = Minimum Quantitation Limit
Page 18
Water Environmental Services - Eden
Division of Burlington Research, Inc,
370 W. Meadow Road • Eden, NC 27288
Phone [phone] • Fax [phone]
Page 2
Water Environmental Services • Kinston
Division of Burlington Reward), Ino.
100 E. Gordon Street • Kinston, NC 23501
Phone [phone] • Fax [phone]
I7

. MAR 04 '99 02:47PM BURLINGTON RESEARCH
P.6/22
Effluent Toxicity Report Form - Chronic Pass/Fail and Acute LCSO Date: 03/04/99
Facility: FLUORIDE SAMPLES NPDES#: NC
Laboratory Performing Tests BURLINGTON RESEARCH, INC.
x
Signature of Operator in Responsible Charge
x
Si tore of Laboratory Supervisor
Piped: County: MMITCHELL
Comments: 0.5 PPM m a males
* PASSED: -5.91% Reduction *
Work Order: 98607-002
MAIL ORIGINAL TO:
North Carolina Ceriodaphnia
Chronic Pass/Fail Reproduction Toxicity Teat
CONTROL ORGANISMS
Environmental Sciences Branch
Div. of Environmental Management
N.C. Dept. of EHNR
4401 Reedy Creek Rood
Raleigh, North Carolina 27607-6445
1 2 3 4 5 6 7 8 9 10 11 12
Chronic Test Results
Calculated t = -0.700
Tabular t ti 2.528
% Reduction n -5.91
9 Young Produced
21
15
21
24
17
21
18
23
22
21
9
18
Adutt (L)iVe (D)ead
Effluent X: 100X
TREATMENT 2 ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12
* Young Produced
22
18
17
23
23
24
16
16
20
24
Adult (L)ive (D)ead
1.
% Mortality
Av9.Reprod.
0.00
control
19.17
Control
0.00
Treatment 2
20.30
Treatment 2
Control CV
21.550%
% control ergs
producing 3rd
brood
100%
PASS FAIL
Check One
1st sample
pH
Control
Treatment 2
7.30
7.22
7.94
7.48
s
t e
6 n
r d
t
1st sample
0.0.
Control 8.8 8.2
Treatment 2 8.8 8.2
•
1st sample 2nd sample
7.60 7.21
7.40 7.21
6.86
6.83
740 7.40
.
a s
t c t e
a n a n
r d r d
t t
lit sample 2nd sample
8.7
8.3
8.7
3. 8
8.4
8.4
8.7
Complete This For Either Test
Teat Start Date: 02/24/99
Collection (Start) Date
Sample 1: 02/24/99 Sample 2: / /
Semple Type/Duration
Sample 1
Sample 2
LCSO/Acute Toxicity Test
(Mortality expressed as %, combining replicates)
Grob
x
Duration
C D
L
u
Comp.
hrs
2nd
1st P/F
$ s
A A
M N
P P
Hardness(mg/t)
Spec. cond.(u t%os)
Chtorine(mg/l)
Sample temp. at receipt(•C)
40
Wit
�C�vv�ti
85
42.8
:fir...
n/a
%
%
%
%
%
x
x
x
%
%
%
%
%
x
%
%
%
%
X
%
Concentration
Mortality
start/end
3.2
I
Notes Please
Complete This
Section Also
start/end
LCSO a
Method of Determination
Moving Average _ Probit
Spearman Kerber Other
Control
95% Confidence Limits
.....- -- _
�--
high
Cone.
pH
rganism Tested: Ceriodaphnia dubia
Duratien(hrs):
Copied trap DEM form AT-1 (3/87) rev. 11/99 (DUBIA ver. 4.32)
D.O.
Page 19
1�

. MAR 04 '99 02:48PM BURLINGTON RESEARCH P.7/22
BURLINGTON
RESEARCH
Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling $ervicas
1302 Belmont Street • Burlington, NC 27215-6935 • Phone [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: Mr. Roy Rittle
SAMPLE DESC; FEB. MONITORING
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 02124/9911:40 SITE: 1 ppm
WORK ORDER #: 9B607-003
RECEIVED: 02/24/99
REPORTED: 03/04199
PO NUMBER:
PARAMETER
DATE/TiME/ANALYST MQL
RESULT
Fluoride byIC Analysis
EPA 300.0
Started 03/02/9911:53 0.10
Analyzed 03/02/99 by TAR at BRI - Burlington
0,96 mg/
Ceriodaphnia Pass/Fail Chronic
NCDEM 9/89
Started 02/24/99 14:00 N/A
Analyzed 03/04/99 by JCB at BRI - Burlington
Pass Pass/Fail
MQL = Minimum Quantitation T At it
Page 20
Water Environmental Services • Eden
Division of Burlington Research, Inc.
370 W. Meadow Road • Eden, NC 27288
Phone [phone] • Fax [phone]
9R•2 1/49
Page 3
Water Environmental Services • Kinston
Division of BurUnglan Research, Inc.
100 E. Gordon Street • Kinston, NC 28501
Phone [phone] • Fax [phone]

MAR 04 '99 02:48PM BURLINGTON RESEARCH
Effluent Toxicity Report Farm - Chronic Pass/Fail end Acute LC50
Date: 03/04/99
P. 8/22
Facility: FLUORIDE SAMPLES NPDES#: NC
Laboratory Performing Tests RURLINGTON RESEARCH, INC.
x
signature of Operator to Responsible Charge
X .f'w..
1gnature of Laboratory Supervisor
Piped: County: MITCHEL L,�
Camrents: 1.0 gm m = males
'- _PASSED: 19.42% Reduction *i
York Order: 92607-003
MAIL ORIGINAL TO:
North Carolina Ceriodaphnia
Chranle'Pass/Fail Reproduction Toxicity Test
CONTROL ORGANISMS
# Young Produced
Environmental Sciences Brach
Div. of Environmental Management
N.C. Dept. of EHNR
4401 Reedy Creek Road
Raleigh, North Carolina 27607-6445
1 2 3 4 5 6 7 8 9 10 11 12
21
15
21
24
17
21
18
23
22
21
9
Adult (L)ive (D)ead
L L
18
L L
Effluent %: 100%
TREATMENT 2 ORGANISMS 1 2 3 4 5 6 7 8 9
10 11 12
# Young Produced
18
14
18
11
ael 3
Adult (L)ive (D)eed
LLLL
PH
Control
Treatment 2
D.O.
Control
Treatment 2
1st ample 1st sample 2nd sample
mt
t
a
r
a
n
d
s
a
r
e
n
d
t t
lot sample 1st sample
8.8 8.2
8.8 8.2
8.7 8.3
8.6
8.3
s
t e
a n
r d
t
2nd sample
8.4 8.5
8.3 8.6.
8
Chronic Test Results
Calculated t = 2.337
Tabular t = 2.539
ii Reduction is 19.42
Mortality
Avg.peprod.
0.00
Control
19.17
Control
0.00
Treatment 2
Control CV
21.550%
15.44
Treatment 2
% control orgs
brood ing 3rd
100%
PASS FAIL.
x
Check One
LCSO/Acute Toxicity Test
Complete This For Either Test
Test Start Date: 02/24/99
Collection (Start) Date
Sample 1; (12/24/99 Sample 2: / /
Sample Type/Duration
Sample 1
Semple 2
Grab Carp. Duration
hrs
hrs
Hardnoss(mg/t)
Spec. Cord.(Wrhos)
Chlorine(mg/t)
Sample temp. at receipt('C)
D
I 8
L A
u M
T P
40 Ma
2nd
1st P/F
$
A
M
P
(Mortality expressed as %, combining replicates)
%
x
%
%
%
%
% %
%
%
%
%
%
%
%
%
% %
%
%
L95% Confidence limits
% -• x
45.9
3.
�''•
2
Notes Please
Concentration complete This
Section Also
Mortality
start/end start/end
Method of Determination Control
Moving Average _ Probit
spoormsn Karber Other ..r
PH
High
-- Conc.
D.O.
Organism Tested: Ceriodaphnia dubie Duration(hrs)$
Copied from DEM form AT-1 (3/87) rev. 11/95 (DUBiA ver. 4.32)
Page 21

• MAR 04 '99 02:48PM BURLINGTON RESEARCH
P.9/22
BURLINGTON
RESEARCH
Aquatic Bioassay Tasting • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments ' NPDE9 Tasting
Reporting a Data Handling Services
1302 Belmont Street • Burlington, NC 27215-6935 • Phone [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: Mr. Roy Rittle
SAMPLE DESC: FEB, MONITORING
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 02/24/99 11:45 SITE; 1.5 ppm
PO NUMBER:
ORDER #; 9B607.004
RECEIVED: 02/24/99
REPORTED: 03/04/99
LfARAMETER
Fluoride byIC Analysis
EPA 300.6
Ceriodaphnia 9Pass/Fail Chronic
NCDEM 9/89
DATE/TIME/ANALYST MOL.
Started 03/02i9911:53 0.10
Analyzed 03/02/99 by TAR at BRI - Burlington
Started 02124/9914:00 N/A
Analyzed 03/04/99 by JCB at BRI - Burlington
RESULT
1.47 mg/L
Pass Pass/Fail
MQL = Minimum Quantitation Limit
Water Environmental SoMcee • Eden
Division of Burlington Resew, Inc.
370 W. Meadow Road • Eden. NC 27288
Phone [phone] • Fax [phone]
Page 4
Page 22
Water Environmental San/ices -Kinston
Division of Burlington Research, Inc.
100 E. Gordon Street • Kinston, NO 28501
Phone [phone] • Fax [phone]
WS VW
21

• MAR 04 '99 02:49PM BURLINGTON RESEARCH
P.10/22
Effluent Toxicity Report Form - Chronic Pass/Fail and Acute LC50 Date: 03/04/99
Facility: FLUORIDE SAMPLES NPDES#: NC Pipe#: County: MITCHELL
Laboratory Performing Test: BURLINGTON RESEARCH, INC.
Signature of Operator in Responsible Charge
'mature of Laboratory Supervisor
Nark Order: 98607-004
Comments: 1.5 ppm; m p male
* PASSED: 19.13% Reduction *
MAIL ORIGINAL TO:
North Carolina Ceriodaphnia
Chronic Pass/Fail Reproduction Toxicity Test
Environmental SEiiiias Branch
Div. of Environmental Management
N.C. Dept. of EHNR
4401 Reedy Creek Road
Raleigh, North Carolina 27607-6445
CONTROL ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12
Chronic Test Results
Calculated t 2.569
Tabular t 2.528
% Reduction = 19.13
# Young Produced
21 15 21 24 17 21 18
23
22 21 9 18
Adult (L)ive (D)ead
Effluent %: 100%
TREATMENT 2 ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12
# Yong Produced
Adult (L)ive (D)ead
15
14
L L
1
4 tel
3
16 14 18
17
L
1€
15
X Mortality
Avg.Reprod.
0.00
Control
19.17
Control
0.00
Treatment 2
15.50
Treatment 2
Control CV
21.550X
% control orgs
producing 3rd
brood
loox
PASS FAIL
Check One
0.
1st sample
PH
Control 7.30 7.94 7.60 7.21
Treatment 2 7.13 7.22 7.19 7.02
1st sample 2nd sample
D.O.
Control
Treatment 2
6.86
6.76
7.41
7.28
s $ s
t e t e t e
a n a n a n
r d r d r d
t t t
lst sample 1st suiple 2nd sample
8.8
8.2
8.8
8.3
8.7 8.3
8.6 8.2
8.4 8
8.2 .fl
8.7
LC50/Acute Toxicity Test
Complete This For Either Test
Test Start Date: 02/24/99
Collection (Start) Date
Sample 1: 02/24/99 Sample 2: / /
Sample Type/Duration
Grab Comp.
Duration
Sample 1 X hrs
Sample 2 hrs
Herdness(m9/t)
spec. Cond.(umhos)
Chlorine(mg/t)
Sample temp. at receipt('C)
2nd
1st P/F
D
I S S
L A A
U M M
T P P
40
85
48.4
Na
3.2
(Mortality expressed as X, eoa+bining replicates)
X
X
X
%
%
%
%
X
X
X
%
%
X
X
X
%
X
%
%
%
Concentration
1
Mote: Please
Complete This
Section Also
Mortality
start/end start/end
LC50 x Method of DeterminationControt
95X Confidence Limits Moving Average Probit r---
X -- % Spearman Kerber Other amok a� Conc.
PH D.0•
Organism Tested: Ceriodaphnia dubia Deration(brs)$
Page 23
Copied from DEM for AT-1 (3/87) rev. 11/95 (DU91A ver. 4.32)
�jL

MAR 04 '99 02:49PM BURLINGTON RESEARCH
P.11/22
BURLINGTON
RESEARCH
Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Service
1302 Belmont Street • Burlington, NC 27215-6935 • Phone [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO; Mr. Roy Rittle
SAMPLE DESC: FEB. MONITORING
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 02/24/99 11:50 SITE:
2 ppm
WORK ORDER #: 9E607.005
RECEIVED: 02/14/99
REPOK I LD: 03/04/99
PO NUMBER:
PARAMETER
DATE/TIME/ANALYST MQL RESULT
Fluoride by IC Analysis
EPA 300.0
Started 03/02/991153 0.10
Analyzed 03/02/99 by TAR at BRI -Burlington
1.93 mg/L
Ceriodaphnia Pass/Fail Chronic
NCDEM 9/89
Started 02/24/9914:00 N/A
Analyzed 03/04/99 by J'CB at BRI - Burlington
Pass Pass/Fail
MQL = Minimum Quantitation Limit
Page 24
Water Environmental Services - Eden
Division of Burlington Research, Inc..
370 W. Meadow Road • Edon, NC 27288
Phone [phone] • Fax [phone]
Page 5
Water Environmental Services - Kinston
Division of Burlington Research, In0-
100 E. Gordon Street • Kinston, NC 2d501
Phony [phone] • Fax [phone]
Z'

MAR 04 '99 02:49PM BURLINGTON RESEARCH P.12/22
Effluent Toxicity Report Form - Chronic Pasa/Fail and Acute LC50 Date: 03/04/99
Facility: FLUORIDE SAMPLES NPDES#: NC
Laboratory Performing Test: BURLINGTCII RESEARCH, INC.
x
Signature of operator in Responsible Charge
wture of Laboratory Supervisor
Pipe#: county: NITCHELL
Comments: 2.0 ppm
PASSED: 4.35% Reduction
Work Order: 98607-005
MAIL ORIGINAL TO:
vorth Carolina Ceriodaphnia
Chronic Pass/Fail Reproduction Toxicity Test
Environmental Sciences Branch
Div. of Environmental Management
N.C. Dept. of EMIR
4401 Reedy Creek Road
Raleigh, North Carolina 27607-6445
C011TR0L ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12
Chronic Test Results
Calculated t = 0.568
Tabular t = 2.508
X Reduction m 4.35
1 Young Produced
Adult (L)ive (0)ead L L L L
21
15
24
17
21 18 23 22 21 9 18
Effluent %: 100% .
TREATMENT 2 ORGAN I SMS 1 2 3 4 5 6 7 8 9 10 11 12
# You Produced
Adult (L)ive (D)ead
20
24
18
15
21
20
15 19 15
16
L L
X Mortality
Av9.Reprod.
0.00
Control
19.17
Control
0.00
Treatment 2
18.33
Treatment 2
Control CV
21.550%
X control orgs
producing 3rd
broad
100%
PASS FAIL
x
Check One
pH
Control
Treatment 2
1st sample
D.O.
Control
Treatment 2
8.8
8.2
8.3
lot sample 1st sample 2nd sample
7.30
7.94
7.10
7.16
7.60 7.21
7.14 7.11
6.86
7.41
6.71
7.25
s s s
t e t e t e
a n a n a n
r d r d r d
t t t
1st sample 2nd sample
8.7
8.3
8.6
8.2
a.4
8.2
8.5
8.7
LC50/Acute Toxicity Test
Complete This For Either Test
Teat Start Date: 02/24/99
Collection (start) Date
Sample 1: 02/24/99 Sample 2: / /
sample Type/Duration
sample 1
Sample 2
Grab
Carp.
Duration
hrs
hrs
2nd
1st P/F
0
I S S
L A A
U M N
T P P
Hardness(ms/l)
Spec. Cond.(Wohos)
Chlorine(mg/L)
sample temp. at receipt(%)
40
85
51.3
n/a
3.2
(Mortality expressed as %, combining replicates)
x
x
X
X
%
%
%
%
%
%
X
X
X
X
%
%
X
%
X
X
Note: Please
Concentration Cosptete This
Section Also
Mortality
start/end
start/end
LC50 a %
Method of Determination
Moving Average Probit-
Spearman Kerber Other �.
Control
95% Confidence Limits
x •- %
--.-•
High
Conc.
�---
_
-
PH
organism Tested: Ceriodaphnia dubia Duration(hrs):,
D.O.
Page 25
21
Copied from DEM form AT-1 (3/87) rev. 11/95 (DUBIA ver. 4.32)

MAR 04 '99 02:49PM BURLINGTON RESEARCH
P. 13/22
BURLINGTON
RESEARCH
Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporting 8 Data Handling Services
1302 Belmont Street • Burlington, NC 27215-6935 • Phone [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: Mr. Roy Riffle
SAMPLE DESC: FEB. MONITORING
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 02 /9911:55 SITE: 3 ppm
WORK ORDER #: 913607-006
RECEIVED: 02/24/99
REPORTED: 03/04/99
PO NUMBER:
PARAMETER
DATE/TIME/ANALYST MQL RESULT
Fluoride by IC Analysis
EPA 300.0
Started 03/02/99 11:53 0.10
Analyzed 03/02/99 by TAR at BM - Burlington
2.89 mg/L
Ceriodaphnia Pass/Fail Chronic
NCDEM 9/89
Started 02/24/9913:45 N/A
Analyzed 03/04/99 by JCB at BRI - Burlington
Pass Pass/Fait
MQL = Minimum Quantitation Limit
Water Environmental Services - Eden
Division of Burlington Research,
370 W. Meadow Road • Eden,�9
Phone [phone] • Fax [phone]
Page 6
Page 26
Water Environmental Services -Kinston
Division of Burlington Research, Inc.
1E10 E. Gordon Street • Kinston, NC 29501
Phone [phone] • Fax [phone]
eR 2 u!•

MAR 04 '99 02:50PM BURLINGTON RESEARCH
Effluent Toxicity Report Form - Chronic Pass/Fail and Acute LC50 Dates 03/04/99
P.14/22
Facility: FLUORIDE SAMPLES NPDESB: NC
Laboratory Performing Test: BURLINGTON RESEARCH, INC.
K
Signs, re of Operator in Responsible Charge
ture of Laboratory Supervisor
Uork Orders 98607-006
MAIL ORIGINAL TO:
Worth Carolina Ceriodephnia
Chronic Pass/Fail Reproduction Toxicity Test
Pipe#: County: MITCHELL
Comments: 3 ppa
* PASSED: -31.30% Reduction *
Environmental Sciences Branch
Div. of Environmental Management
N.C. Dept. of EHNR
4401 Reedy Crest Road
Raleigh, North Carolina 27607.6445
CONTROL ORGANTSHs 1 2 3 4 5 6 7 8 9 10 11 12
Chronic Test Results
Calculated t g
Tabular t ■
X Reduction = -31.30
0 Young Produced
21
15 21 24
17
21
18
23
22
21
9
18
Adult (L)ive (D)ead
L L L
Effluent %: 100X
TREATMENT 2 ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12
8 Young Produced
27 16
31
26
7
26
Adult (L)ive (D)eed
29
L
33
32
23
26
26
X Mortality
Avg.Reprod.
0,00
Controt
19.17
Control
0.00
Treatment 2
25.17
Treatment 2
Control CV
21.550%
% controt ergs
producing 3rd
brood
100%
PASS FAIL
X
Check One
PH
Control
Treatment 2
D.O.
Control
Treatment 2
1st sample lst sample 2nd sample
7.59 7.32
7.60 7.31
7.40
6.78
6.91
7.43 7.11
6.73 7.16
s s s
t e t e t e
e n a n a n
✓ d r d r d
t t t
1st sample 1st stele 2nd sample
8.7
8.9
8.2
8.1
8.1
8.0
8.3
goomomismommloommillIMMaammomm
LC50/Acute Toxicity Test
(Mortality expressed as %, combining replicates)
Complete This For Either Test
Test Start Date: 02/24/99
Collection (Start) Date
Sample 1: 02/24/99 sample 2: / /
Sample Type/Duration
Sample 1
Sample 2
Grab
Coop.
Duration
2nd
1St P/F
D
1 s S
hrs 1. A A
U M H
hrs T P P
Hardness(ag/t) 40
Spec. Cond.(guhes) 85
Chlorine(ma/t) We
-
,..0.
54.7
Sample temp. at receipt(%) Ham 3.2
Note: Please
This
%
%
% % X
%
%
%
%
%
X
%
x % %
%
%
%
x
%
LC50 a
95% Confidence Limits
Concentration
Complete
Section
Also
so
Mortality
start/end start/end
Method of Determination
Moving Average _ Probit _
Spearman Kerber Other
•
Control
High
Cone.
pH D.O.
Organism Tested: Ceriodaphnia dubia Duretion(hrs): ..
Page 27
Copied from DEM form AT-1 (3/87) rev. 11/95 (DUBIA ver. 4.32)
ZG

MAR 04 '99 02:50PM BURLINGTON RESEARCH
P.15/22
BURLINGTON
RESEARCH
Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
1302 Belmont Street • Burlington, NC 27215-6935 • Phone [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: Mr. Roy Rittle
SAMPLE DESC: FEB. MONITORING
SAMPLE TYPE: WASTEWATER GRAB
COLLECTED: 02/24/99 11:55 S fTE: 4 ppm
WORK ORDER #: 9B607-007
RECEIVED: 02/24/99
REPOH i tD: 03/04/99
PO NUMBER:
PARAMETER
DATE/T1ME/ANALYST MQL RESULT
Fluoride by IC Analysis
EPA 300.0
Started 03/02/99 11:53 0.10
Analyzed 03/02/99 by TAR at BRI - Burlington
3.86mg/L.'
Ceriodaphnia Pass/Fail Chronic
NCDEM 9/89
Started 02/24/99 14:00 N/A
Analyzed 03/04/99 by JCB at BRI - Burlington
Pass Pass/Fail
MQL = Minimum Quantitation Limit
Page 28
BR-1 1na
Water Environmental Services • Eden
Division of Burlington Research, Inc.
370 W. Meadow Road • Eden, NC 27288
Rhone [phone] • Fax [phone]
Page 7
Water Environmental Services -Kinston
Division of Buriington Research, Inc_
100 E. Gordon Street • Kinston, NC 29501
Phone [phone] • Fax [phone]

MAR 04 '99 02:50PM BURLINGTON RESEARCH
Effluent Toxicity Report Fora - Chronic Pass/Fait and Acute LCSO Date: 03/04/99
P.16/22
Facility: FLUORIDE SAMPLES
NPDES#: NC
Laboratory Performing Test: BURLINGTON RESEARCH. INC.
t___-
signature of Operator in Responsible Charge
x
lure of Laboratory supervisor
work order: 98607-007
MAIL ORIGINAL TO:
North Carolina Ceriodaphnia
chronic Pass/Fail Reproduction Toxicity Test
Pipe#: County: MITCHELL
Comments: 4 ppn
* PASSED: -17.83% Reduction
Environmental Sciences Branch
Div. of Environmental Management
N.C. Dept. of EHNR
4401 Reedy Creak Road
Raleigh, North Carolina 27607-6445
CONTROL ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12
# Young Produced
21
15
21
24
17
21
18
23
22
21
9
18
Adult (L)ive (D)ead
Effluent %: 100%
TREATMENT 2 ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12
# Young Produced
21
32
25
5
21
22
16
22
31
18
31
27
Adult (L)ive (D)ead
L
L
L
L
L
L
L
L
L
L
L
L
PH
Control
Treatment 2
0.0.
Control
Treatment 2
1st sample
7.30
7.48
s
t
a n
r d
t
1st sample
8.8
8.8
. e2
let sample 2nd sample
7.60
7.26
7.21
6.85
6.86
6.65
7.41
7.221
s s
t e t e
a n a n
✓ d r d
t t
1st sample 2nd sample
8.7 8.3
8.5 8.4
8.3 8.6
Chronic Test Results
Calculated t - -1.369
Tabular t - 2.508
% Reduction = -17.83
% Mortality
Avg.Reprod.
0.00
Control
19.17
Control
0.00
Treatment 2
.111.111111.
22.58
Treatment 2
Control CV
21.550%
% control orgs
producing 3rd
brood
100%
PASS FAIL
Check One
Complete This For Either Test
Test Start Date: 02/24/99
collection (Start) Dote
sample 1: 02/24/99 sample 2:
Sample Type/Duration
Sample 1
Sample 2
LC50/Acute Toxicity Test
(Mortality expressed as %, combining replicates)
Grab
Coop.
X
/ /
2nd
1st P/F
Duration D
I S
hrs 1, A
U M
hrs T P
A
N
P
Hardness( /t)
Spec. Cond.(pmhos)
chlorine(mg/l)
ample temp. at receipt(•C)
40
85
58.1
n/a
3.2
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
LCSO X
95% Conf deuce Limits
%-- x
Concentration
Mortality
start/end
Method of Determination
Moving Average Probit
Spearman Kerber ._. other
L
v.
Note: Please
Complete This
section Also
start/end
Control
organism Tested: Ceriodaphnio dubia Duration(hrs): _
Copied from DEM form AT-1 (3/87) rev. 11/95 (DUBIA ver. 4.32)
High
Conc.
J
D.o.
Page 29

MAR 04 '99 02:51PM BURLINGTON RESEARCH
P.17/22
BURLINGTON
RESEARCH
Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDESTesting
Reporting & Data Handling Services
1302 Belmont Street • Burlington, NC 27215-6935 • Phone [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: Mr, Roy Kittle
SAMPLE DESC: FEB. MONITORING
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 02/24/9912:00 SITE: 8 ppm
WORK ORDER #: 9B607-008
RECEIVED: 02/24199
REPOH I HD: 03/04/99
PO NUMBER:
PARAMETER
DATE/TIME/ANALYST MOL
RESULT
Fluoride by IC Analysis
EPA 300.0
Started 03/02/9911:53 0.10
Analyzed 03/02/99 by TAR at BRI - Burlington
7.20 mg/L
Ceriodaphnia Pass/Fail Chronic
NCDEM 9/89
Started 02/24/9914:00 N/A
Analyzed 03/04/99 by JCB at BRI - Burlington
Pass Pass/Fail
MQL = Minimum Quantitation Limit
Page 30
Water Environmental Services • Eden
Division of Burlington Research, Inc.
370 W. Meadow Road • Eden, NC 27288
Phone [phone] • Fax [phone]
Page 8
Water Environmental Services-Kins1On
Division of Burlington Research, Inc.
100 E. Gordon Street • Kinston, NC 23501
Phone (252) 52P-9921 • Fax [phone]
L J

MAR 04 '99 02:51PM BURLINGTON RESEARCH
•
P.18/22
Effluent Toxicity Report Form - chronic Pass/Fail and Acute LC50 Date: 03/04/99
Facility: FLUAIDE SAMPLES IJPDES#: NC
Laboratory Performing Test: BURLINGTON RESEARCH, INC.
X
SignDture of Operator in Responsible Charse
gnature of Laboratory supervisor
piped: County: MITCHELL
Comments: 8 ppm
* PASSED: •28.26% Reduction gi
Work Order: 98607-008
MAIL ORIGINAL T0:
worth Carolina Ceriodaphnia
ChreniC Pass/Fait Reproduction Toxicity Test
Environmental Sciences Branch
Div. of Environmental Management
K.C. Dept. of EMNR
4401 Reedy Creek Road
Raleigh, North Carolina 27607-6445
CONTROL ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12
Chronic Test Results
Calculated t -2.932
Tabular t = 2.508
% Reduction = -28.26
Young Produced
21
15
21
24 17
21
Adult (L)ive (D)ead
L L L
18 23 22 21
L L L l
9
18
Effluent %: 100%
TREATMENT 2 ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12
# Young Produced
27
16
32
31
21
23
22 26 19 23
30 25
Adult (L)ive (D)ead L L
PH
Control
Treatment 2
D.O.
Control
Treatment 2
L L
% Mortality
Avg.Reprod.
0.00
Control
19.17
Control
0.00
Treatment 2
24.58
Treatment 2
control CV
21.550%
% control orgs
broducing 3rd
rood
100%
PASS FAIL
X
Check One
1st sample let sample 2nd sample
7.60 7.21
7.26 6.65
S S
t e t e
a n a n
✓ d r d
t t
1st sample 1st sample
118
8.8
8.2
8.2
8.7 8.3
8.5 8.4
6.86 7.41
6.65 7.22
t e
a n
✓ d
t
2rd sample
8.4
A.3
8.5
1
4 . a� 8.
Complete This For Either Test
Test Start Date: 02/24/99
Collection (Start) Date
sample 1: 02/24/99 Sample 2: / /
Sample Type/Duration
LC50/Acute Toxicity Test
Sample 1
Sample 2
Grab
X
Col*.
Duration
hrs
hrs
2nd
1st P/F
D
1 S S
L A A
u K M
T P P
Hardness(mg/l)
Spec. Cond.(phos)
Chtorine(mg/l)
Sample temp. at receipt('C)
85
72.8
n/a
EA?'
3.2
•
Mortality expressed as %, combining replicates)
X
X
x
x%%
x
XI
XI
X
%
%
%
%
x
x
% % %
Concentration
Note: Please
Complete This
Section Also
Mortality
start/end start/end
Control
Hid' Conc. Page 31
PH D.O.
mINNI
LC50 a % Method of Determination
95% Confidence Limits Moving Average _ Probit _
% .. % Spearman Kerber Other
Organism Tested: Ceriodaphnia dubia Duration(hrs):
Copied from DEM form AT-1 (3/87) rev. 11/95 (DUBIA ver. 4.32)
3
c

MAR 04 '99 02:51PM BURLINGTON RESEARCH
P.19/22
BURLINGTON
RESEARCH
Aquatic Bioassay Testing • Aquadc Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
1302 Belmont Street • Burlington, NC 27215-6935 • Phone [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: Unimin Corp,
REPORT TO: Mr. Roy Rittle
SAMPLE DESC: FEB. MONITORING
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 02/24/99 12:00 SITE: 16 ppm
WORK ORDER #: 9B607-009
RECEIVED; 02/24/99
RCPORTED: 03/04/99
PO NUMBER:
PARAM ETE R
DATE/TIME/ANALYST MQL RESULT
Fluoride by IC Analysis Started 03/02/991153 0.10
EPA 300.0 Analyzed 03/02/99 by TAR at BTU - Burlington
15,9 mg/L
NCDEMh g
Pass/Fail Chronic Analyzed 903/04/99 by JCB at BR1 Burlington
Pacq Pass/Fai1
MQL ^ Minimum Quantitation Limit
Certifications:
BRI - Burlington
NC Chemistry: #85, Biomonitoringg: #002, Drinking Water: #37743, Radiation License: #001-0904-0G
VA SWCB ID: #000061, Drinking Water: #00018
SC Laboratory ID' #99042
EPA Chemistry Lab JD: N000137, Bioassay Lab ID: NC2721500
Page 32
Water Environmental Services -Eden
Division of eurlingron Research, Inc.
370 W. Meadow Road • Eden. NC 27288
Phone [phone] • Fax [phone]
BR-2 1)4D
Page
9
Water Environmental Services -Kinston
Division of Burtington Research, Inc.
100 E. Gordon Street • Kinston, NC 28501
Phone [phone] • Fax [phone]
3l

MAR 04 '99 02:52PM BURLINGTON RESEARCH
P.20/22
Facility: FLUORIDE SAMPLES NPDES#: NC
Laboratory Performing Test: BURLINGTON RESEARCH, WC.
x
Signature of Operator in Responsible Charge
xgnature of Laboratory Supervisor
Effluent Toxicity Report Form - Chronic Pass/Fail and Acute LC50 Dates 03/04/99
Piped: County: MITCHELL
Comments: 16 ppm
* PASSED: •1.74% Reduction *
Work Order: 98607-88YO01
MAIL ORIGINAL TO:
North Carolina Ceriodaphnia
Chronic Pass/Fail Reproduction Toxicity Test
CONTROL ORGANISMS
Environmental Sciences Branch
Div. of Environmental Management
N.C. Dept. of EHNR
4401 Reedy Creek Road
Raleigh, North Carolina 27607-6445
1 2 3 4 5 6 7 8 9 10 11 12
Chronic Test Results
Calculated t = •0.114
Tabular t 2.508
% Reduction c -1.74
iiYoung Produced
21
15
21
24
17
21
18 23 22
21
9
18
Adult tL)ive (D)eed
LLLL
Effluent X: 100%
TREATMENT 2 ORGANISMS
1 2 3 4 5 6 7 8 9 10 11 12
# Young Produced
24
28
24 28 30
26126l6
15111
Adult (L)ive (Wad
pH
Control
Treatment 2
D.O.
Control
Treatment 2
l
.LILIL
1st sample 1st sample 2nd sample
7.30
7.94
7.45
7.21
s
t e
a n
✓ d
t
1st sample
8.8
8.8
8.2
8.1
7.60 7.21
7.22 6.84
6.65
7.41
7.25
s S
t e t e
n a n
✓ d r d
t t
1st sample 2nd sample
8.7 8.3
8.3 8.1
5 11
D
% Mortality
Avg.Reprod.
0.00
Control
19.17
Control
8.33
Treatment 2
19.50
Treatment 2
Control CV
21.550%
% control ores
pry ing 3rd
br100%
PASS FAIL
EcC
Check one
8.4 8.5
8.3
8.5
LC5O/Acute Toxicity Test
Complete This For Either Test
Test Start Date: 02/24/99
Collection (Start) Date
Sample 1: 02/24/99 Sample 2: / /
Sample Type/Duration
Grab Conp4Duration D
---- i
hra L
U
hre T
Sample 1 X
Sample 2
2nd
1st P/F
S S
A A
N M
P P
Hardnesstm9/l) 40 ;; i;::::
Spec. Cond.(grmhos) 85 116.8
Chtorino(ag/L) fmr• n/a
Sample temp. at receiptt'C) egg 3.2
(Mortality expressed as X, combining replicates)
x x x x x x x
x x x x x x x
Concentration
Mortality
start/end start/end
Control
1_
Note: Please
Conptete This
Section Mao
LC50 *
95% Confidence Limits
% -- x
Method of Determination
Moving Average Probst
Spearman Kerber .r Other
Nigh
con*.
PH o.o.
Organism Tested: Ceriodaphnia dubia
Duration(hrs):
Page 33
d 1
Copied from DEM foram AT-1 (3/87) rev. 11/95 (DUBIA ver. 4.32)
3

II BURLINGTON RESEARCH, INC.
1302 Belmont Street
Burlington. NC 27215-6935
Phone [phone]
Fax [phone]B
370 West Meadow Road
Eden, NC 27286
Phone [phone]
Fax [phone]
CHAIN OF CUSTODY RECORD
CLIENT: U(1,>s" (Or iP
Facility/Site: A 7 CQl Prs
i•A,
SEND REPORT TO:
Phone:
No
sC/A 3y 1 441-�-_
Li 100 tbnl .iorQon Sorel
Kinston, NC 28551
Phone [phone]
Fax [phone]
Fax:
Sampler: (Print) Ta, inn r (Srgnaiuru> f,,,A.-+y 1,,,,,,--.—...— . _. _..�
_
`_FORBRI
LAB.USE,ONLY.
• Preservation Codes_
A = Ice E= NaOH ,
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the
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ill the resu
FOR CLIENT USE ONLY
Data
Z1L4/91
pats:
goo
Time:
Time:
Received by. (Sig.)
Date:
Time.:
Iv/tattled of Shipment
d of Shipment.
"WO
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Un
02:52PM BURLINGTON RESEARCH
r
fV
UR-17 7?6
.. - .-.,-., r.n.. nl:nnf log Gi..•.l Annnri
r'arr:iru - 13RI - Lahnratnnr
Pink - BR! - Laboratory Goldenrod - Client - Copy

1302 BE:III[ont Street
Buihngton, NC 27215-6935
(3361
BURLINGTON RESEARCH, INC. Faxnc(336)5770-469B
CLIENT: /71/P7/7 ar,p& ij�/8l1
Facility/Site: ,71i121 /t/G 7ii'c r
370 West Meadow flood
Edon, NC 27288
Phone [phone]
Fax [phone]
CHAIN OF CUSTODY RECORD
Sampler: (Print)Se;" J/ 1501 (Signature
100 East Gordon Street
Kinston, NC 28501
Phone [phone]
Fax [phone]
y /
SEND REPORT TO-1�/ 19Arr/7' �r'1� - S e1 %/A-,
Phono: 07,70093 J'/, e Fax C�rrP1 So?-9-%/l
Purchase Order No.:
•
SAMPLE
IfJ
CHLORINATED I
SYSTEM
SAMPLE
COLLECTION
TEA
AT TTTIME OFME OF
COLLECTION
17 CI
SAMPLE TYPE
NUMBER OF
CONTAINERS
SENT
ANALYSES
REQUIRED
SAMPLE
INTEGAETY
;FOR
,
inip,A.=
{4 r.)
•
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-• Preserv?tloo Codes: .
ice .'• E= NaOH -
B =HNO3 F= None
DD= HCI .. ft= HEHO[C
COMPOSITE
CRAB
STARTED
ENDED
DATE
?/Id1E—
DATE
TIMEc-M
NAND
AUTn
X
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Yes
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Yes
No
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Yes
No
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Was the sample dechlor[nated et Time of oaf/et-lion? Yes ❑ No ❑ A./RD WM the results be used for regulatory monitoring purposes? Yes
FOR CLIENT USE ONLY
ifr... Ished by
�`Pi/ .,<<f
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9
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Method of Shifxrterri�� '
Method of Shipment - - ,
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0i►-tt7Oft

MAR 04 '99 03:12PM BURLINGTON RESEARCH P.1/20
= TO UNIMIN QUARTZ
FAX Transmission Sheet
Burlington Research, Inc.
1302 Belmont Street
Burlington, NC 27215-6935
Phone: [phone]
FAX: [phone]
FAX ONLY _X..._.
DATE: March 4, 1999
TO: Roy Rittle
COMPANY: Unimin
FAX #: [phone]
FAX &MAD.
11-LOTTD k CA TY
Q.0
FROM: John Baummer, BRI Biomonitoring Lab Manager
SUBJECT: Completed reports
You should receiv,,; - • : -s including this cover sheet. If you do not receive all pages, or
have a question r garding c tent, please call me at 910/570-4661, Ext. 289.
COMMENTS:
Roy:
Completed reports _ o
Questions, please call
John
Page 36

MAR 04 '99 03:12PM BURLINGTON RESEARCH
P.2,20
BUR RESEARCHINGTON
Aquatic Bioassay Testing • Aquatic lbxlclty Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
1302 Belmont Street • Burlington, NC 27215-8935 • Phone [phone] • Fax [phone]
March 4,1999
Unirnin Corp.
P.O.BOX 588
Spruce Pine, NC 28777
Attention: Mr. Roy Kittle
Enclosed please find the reports for your samples received 03/03/99, assigned
to BRY Workorder 9C104. -Please call if you have any questions.
Thank you.
Water Environmental Services - Eden
Division of Burlington Research, Inc.
370 W. Meadow Road • Eden. NC 27288
Phone [phone] • Fax [phone]
Sincerely,
BU,INGTON RESEARCH, INC.
hn C. Baurnmer
Manager, Biomonitoring Dept.
[phone] Ext. 289
Page 37
Water Earonmentai Services • Kinston
Division of Burlington Research Inc.
100 E. Gordon Street • Kinston. NC 28501
Phone [phone] • Fax [phone]
Bit! V$1
3-b

MAR 04 '99 03:13PM BURLINGTON RESEARCH
P.3/20
BURLINGTON
RESEARCH
Aquatic Bioassay Testing • Aquatic Toxici y Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
1302 Belmont Street • Burlington, NC 27215.6935 • Phone [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER, Unimin Corp.
REPORT TO: Mr. Roy Rittle
SAMPLE DESC: SPRUCE PINE
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 03/02/99 16:00 SITE: 0 PPM
WORK ORDER #: 9C104-001
RECEIVED: 03103/99
REPORTED: 03/04/99
PO NUMBER:
PARAMETER
Fluoride
EPA 340,2
DATE/TIME/ANALYST
MOL RESULT
Started 03/04/9910:00 0,10
Analyzed 0304/99 by JCB at BRI - Burlington
0.11 mg/L
Ceriodaphnia EPA600491027F our Acute Static Bioassay Analyzed 03/04/99 by JCB at MU Burlington
MQL = Minimum Quantitation Limit
> 100 LCSO fo
Page 38
Water Emironmental Services • Eden
Division o{ Burlington Research, Inc.
370 W. Meadow Road • Eden, NC 27288
Phone (336) 623•a921 • Fax [phone]B
BR-z 1,1.f
Page 1
Water Environmental Sery eo - Kinston
Division of Burlington Research, Inc.
100 E. Gordon Street • Kinston, NC 20501
Phone [phone] • Fax [phone]

MAR 04 '99 03:13PM BURLINGTON RESEARCH
P.4,20
BURLINGTON
RESEARCH
Effluent Toxicity Re ort Form - Acute LC50 Date: 3/4/99
Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Asseasments • NPDES Testing
Reporting & Data Handling services
1302 Belmont Street • Burlington, NO 27215-6935 • Phone [phone] • Fax [phone]
Facility UNIMIN NPDES* R&D Pipe* County
Laboratory PerfOrMing Test Burlington Research, Inc. - Cert. # 002
x
Signal e cif Operator In Responelble Charge
Organism Tested:
Ceriodaphnia dubla
'Acidified Nan DEng kern AT•1 (3W) rsv. B/08
Water Environmental Services - Eden
Division of Burlington Research, Inc.
370 W. Meadow Road • Eden, NC 27288
Phone [phone] • Fax [phone]
Environmenta sciences sranc
Div. of Water Quality
NC Dept. of ENR
4401 Ready Creek Road
Raleigh, NC 27607-8445
Herdneoe(mg/L)
Spec. Cond.(mlcromhoc)
Chlorine(mg/L)
Sample temp @ rocalpt
(dog. C)
BRI rev. IWOG
0:VOM1SVAnd farm
Page 3 9
Water Environmental Services -Kinaton
Division of Burlington Research, Inc.
100 E. Gordon Street • Kinston, NO 28601
Phone [phone] • Fax [phone]
3E
BA-2 1:1"

MAR 04 '99 03:14PM BURLINGTON RESEARCH
P.5/20
U RESEARCH
RE
Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
1302 Belmont Street • Burlington, NC 27215-6035 • Phone [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: Mr. Roy Rittle
SAMPLE DESC: SPRUCE PINE
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 03/02/99 16:05 SITE: 5 PPM
PARAMETER
WORK ORDER #: 9C104-002
RECEIVED: 03/03/99
REPORTED: 03/04/99
PO NUMBER:
DATE/TIME/ANALYST MCA.
RESULT
Fluoride
EPA 340.2
Started 03104/9910:00 0.10
Analyzed 03i04199 by JCB at Btu - Burlington
6.24 mgiL'
Ceriodapbnia 48-Hour Acute Static Bioassay Started 003102/99 16:55 NSt BRI -/A
BurlingEon
EPA600491027F Analyzed /0419 by JCB
MQL = Minimum Quantitation Limit
> 100 LC5096
DioeSecc.
v t ngtonResah, Inc.
370 W Meadow Road • Eden, NO 27289
Phone [phone] • Fax [phone]
Bfw? IM
Page 2
Page 40
Water Environmental 8eMcea-lKnston
Division of Burlington Research Inc.
100 E. Gordon Street • Kinston.
528501
0 ti9 22
Phone [phone] • Fax (252)
35

MAR 04 '99 03:15PM BURLINGTON RESEARCH
P.6/20
BURLINGTON
RESEARCH
Aquatic Bioassay Tesdng • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
1302 Belmont Street • Burlington, NO 27215-6935 • Phone [phone] '0 Fax [phone]
Effluent Toxicity Report Form - Acute LC50
NPDES# R&D Plpe#
Burlington Research, inc. • Cert. # 002
Signet of Operator in Responsible Charge
E • • -• °noes Branch
Div. of Water Quality
NC Dept. of ENR
4401 Reedy Creek Road
Raleigh. NC 27607-6445
LC50/Acute Toxicity Teat
(Mortality expressed as % combining replicates)
Date:
Hardne55(mg/1-)
spec. Cont(rnlcrontios)
Chlorine(mglL)
Sample temp @ receipt
(deg. C)
Method of Determination
Moving Average
Spearman Karber
Modified tram OEM farm AT-1 (3/87) teiV, 8/68
Water Environmental Services -Eden
Division of Burlington Research, lno.
370 W. Meadow Road • Eden, NC 27288
Phone [phone] • Fax [phone]
Dilution
314199
BRI rod. 12/35 aVamiAtMhmm
Page 4 1
Water Environmental Seivices • Kinston
Division of Burlington Research, inc.
100 E. Gordon Street • Kinston, NC 28501
Phone [phone] • Fax [phone].A
PIMA 11*4

MAR 04 '99 03:16PM BURLINGTON RESEARCH
P.7/2d
BURLINGTON
RESEARCH
Aquatic Bioassay Testing • Aquatic Toxicrty Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
1302 Belmont Street • Burlington, NC 27215-6935 • Phone [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: Mr. Roy Rittle
SAMPLE DESC: SPRUCE PINE
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 03/02/99 16:10 SITE: 10 PPM
PARAMETER
WORK ORDER #: 9C104.003
RECEIVED: 03/03/99
REPORTED, 03/04/99
PO NUMBER:
DATE/TIME/ANALYST MQL
RESULT
Fluoride
EPA. 340.2
Started 03/04/99 10:00 0.10
Analyzed 03/04/99 by JCB at BRI - Burlington
10.4 mg/I.
Ceriodaphnia 4-8-Hour Acute Static Bioassay SSted
Started
EPA600491027F 03/04/99 by KB at BRI -Burlington
MQL - Minimum Quantitation Limit
>100 LCSO%
Water Environmental Servlces - Eden
Division of Burlington Research, Ina
370 W. Meadow Road • Eden. NC 27288
Phone [phone] • Fax [phone]
Page
3
Page 42
Water Environmental Services - Kuntvn
Divis on of Burlington Rasaarch.Inc.
100 E. Gordon Street • Kinston, NO 28501
Phone [phone] • Fax [phone]

MAR 04 '99 03:16PM BURLINGTON RESEARCH
P.8,20
BURLINGTON
RESEARCH
Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product EmAronmentat Assessments • NPDES Testing
Reporting & Data Handling Services
1302 Belmont Street • Burlington, NC 27215-6935 • Phone [phone] • Fax [phone]
11111b.
Effluent Toxicity Re • ort Form - Acute LC50
NPDES# R&D P1po#
Burlington Research, inc. - Cert. # 002
Signet re of Operator In Responsible Charge
Environmental Sciences Bran
Div. of Water Quality
NC Dept. of ENR
4401 Reedy Creek Road
Raleigh, NC 278074445
LC50/Acute Toxicity Test,
(Mortality expressed as %, combining replicates)
modtRotf from DEM farm AT-1 (3)57) rev. 8/63
Water Environmental Services - Eden
Division of Burrulgton Research, Inc.
370 W. Meadow Road Eden, NC 27268
Phone [phone] • Fax [phone]
Date: 3/4/90
Spec. Cond.(mlcromhos)
Chlorine(mg/L)
Sample temp @ receipt
(deg. C)
BRI NV. 12)93 etfamaxutt form
Page 4 3
Water Environmental Services -Kinston
Division of Burlington Research, !M-
UM E. Gordon Street • Kinston, NO 28501
Phone [phone] • Fax [phone]
4 I
IIR-2 1110

MAR 04 '99 03:18PM BURLINGTON RESEARCH
P.9/20
BURLINGTON
RESEARCH
Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
1302 Belmont Street • Burlington, NG 27215-6935 • Phone [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: Unitnin Corp.
REPORT TO: Mr. Roy Rittle
SAMPLE DESC: SPRUCE PINE p0 NUMBER:
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 03/02/99 16:15 SITE: 15 PPM
DATE/TIME/ANALYST MOL RESULT
PARAMETER
OM •
WORK ORDER #: 9C104-004
RECEIVED: 03/03/99
REPORTED: 03/04/99
Fluoride
EPA 340.2
Started 03/04/9910:00 0.10
Analyzed 03/04/99 by JCB at BRI - Burlington
15.9 mg!L
Ceriodaohnia 48-Hour Acute Static Bioassay Started Analyzed 03/02/99 /9916:45 JCB at BRI N/A
- Burlington
EPA60C'491027F
>100 LC50%
MQL = Minimum Quantitation Limit
Water Environmental Services - Eden
Division of Burlington Research. Inc.
370 W. Meadow Road • Eden, NC 27288
Phone [phone] • Fax [phone]
Page 4
Page 44
Water Environmental Services - Kinston
Division of Burlington Research, Inc.
Phone [phone] • Fax [phone]
Bit-2 1AA

. MAR 04 '99 03:18PM BURLINGTON RESEARCH
P.i0/20
BURLINGTON
RESEARCH
Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
1302 Belmont Street • Burlington, NC 27215-6935 • Phone [phone] • Fax [phone]
Effluent Toxic' Report Form Acute LCSO
• modino Iran DEM form AT-1 (3/87) rev. 8198
Water Environmental Services -Eden
Division of Burlington Research, Inc.
370 W. Meadow Road • Eden; NC 27288
Phone [phone] • Fax [phone]
nvironmentel Soleness ranch
Div. of Water Quality
NC Dept of ENR
4401 Reedy Creek Road
Raleigh, NC 27607-6445
Date:
Hardnees(mg/1.)
Spec. Cond.(mIcrornhos)
Chlorine(mg/L)
sample temp @ receipt
(deg. C)
Wu rev. 12/03
3/4/99
Wormfttkatikmm
Page 4 5
Water Environmentai Services -Kinston
Division of Burlington Research, Inc.
100 E. Gordon Street • Kinston, NC 28501
Phone [phone] • Fax [phone]
AO., VS.

MAR 04 '99 03:19PM BURLINGTON RESEARCH
P.11/20
BURLINGTON
RESEARCH
Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporling & Data Handling SenAces
1302 Belmont Street • Burlington, NC 27215-6935 • Phone [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: Mr. Roy Rittle
SAMPLE DESC: SPRUCE PINE
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 03/02/99 16:20 SITE: 20 PPM
WORK ORDER #: 9C104-005
RECEIVED: 03/03/99
REPORTED: 03/04/99
PO NUMBER:
PARAMETER
Fluoride
EPA 340.2
DATElT1ME/ANALYST
MQL RESULT
Started 03/04/99 10:00 0.10
Analyzed 03/04/99 by JCB at BRI - Burlington
20.8 mg/I.:
Ceriod pphnia 48-Hour Acute Static Bioassay Started 03//04/9916: 5 at S� NBurlington
EPA600491027F Analyzed 03/04/99
by
MQL = Minimum Quantitation Limit
> 100 LC50%
Water Environmental Services -Eden
Division oI Burlington Research. Inc.
370 W. Meadow Road • Eden. NC 27288
Phone [phone] • Fax [phone]
Page 5
Page 46
Water Environmental SeMCes -Kinston
Division of Burlington Research. Inc. cF
100 E. Gordon Street • K lnston. NC 28501
Phone [phone] • Fax [phone]

MAR 04 '99 03:20PM BURLINGTON RESEARCH
P.12/eW
BURLINGTON
RESEARCH
Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
1302 Belmont Street • Burlington, NC 27215-6935 • Phone [phone] • Fax [phone]
•
Effluent Toxic' Report Form - Acute LC50
NPDES* R&D Pipet&
Burlington Research, Inc. - Cert. # 002
nvironmental times Branch
Div. of Water Quality
NC Dept of ENR
4401 Reedy Creek Road
Raleigh, NC 27607-6445
X. •
• 9r. 4!!Iit
LC50/Acuto Toxlclty Test
(Mortality expressed as combining replicates)
Modified from DEM term AT•1 (5/437) rev. 8/9/3
Water Environmental Services - Eden
Division of Burlington Research, Inc.
370 W. Meadow Road • Eden, NC 27288
Phone [phone] • Fax [phone]
Date:
Hardness (mg/L)
pec. Cond.(m1crornhos)
Chlorine(mg/L)
Sample temp ® receipt
(deg, C)
BRImtiNn
Dilution
314190
alformAst\oti ken
Page 4 7
Water Environmental Services -Kinston
Division al Burlington Roseate:Nine.
100 E. Gordon Street • IGnston, NC 28501
Phone [phone] • Fax. [phone]
Oft., via.%

MAR 04 '99 03:21PM BURLINGTON RESEARCH
P.13/20
BUR
RESEARCH
Aquatic Bioassay Tasting • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDESTesting
Reporting & Data Handling Services
1302 Belmont Street • Burlington. NC 27215-6935 • Phone [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER Unimin Corp.
REPORT TO: Mr. Roy Rittle
SAMPLE DESC: SPRUCE PINE SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 03/02/99 16:25 SITE: 25 PPM
WORK ORDER #: 9C104-006
RECEIVED: 03/03/99
REPORTED: 03/04/99
PO NUMBER;
PARAMETER
Fluoride
EPA 340.2
DATE/TIME/ANALYST
MQL RESULT
Started 03/04/9914/9
Analyzed by CB at BRI - Burlington
0.10
27.0 mg/L '
Ceriodaphnia 48-Hour Acute tatic Bioassay Started 03/02/99 16:45 N/A >100 LCSO%
EPA604491027F Analyzed 03/04/99 by JCB at BRI - Burlington
MQL = Minimum Quantitation Limit
Water Environmental RM oeas -E
• do
Division of BurlingtonNC 27288
c.
370 W. Meadow Road • Eden.
Phone [phone] • Fax [phone]
Page 6
Page 48
Water Environmental Services -Kinston
Division at Burlington Research. Inc.
100 E. Gordon Sveelt � Piton. ) 5 a9�2
Phone [phone] (

MAR 04 '99 03:21PM BURLINGTON RESEARCH
a
P.14/20
BURLINGTON
RESEARCH r--
Effluent Toxici Report Form - Acute LC50
Facility UNIM1N
Laboratory Performing Test
NPDE8* R&D Pipet
Burlington Research, inc. - Cort. # 002
&loafed horn DEM tarn AT-1 C3187) rev. Me
Water Environmental Services - Eden
Division of Burrmgton Research, Inc.
370 W. Meadow Road • Eden, NC 27288
Phone [phone] • Fax [phone]
Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Freponing & Data Handling Services
1302 Belmont Street • Burlington. NC 27215-6935 • Phone [phone] • Fax [phone]
,M1114
Date:
Dilution
H ardnos (mg/1.)
Spec. Cond.(micromhos)
Chlorino(mg/1.)
Sample tamp @ receipt
(dog. c)
314199
Wirev.12/93 calerrnsiAatitcrm
Page 4 9
Water Envtronmental Services -Kinston
Division of Burlington Resoarch, ino.
100 E Gordon Street • Kinston, NO 28501 •
Phone [phone] • Fax [phone].
PIRA 1,001

MAR 04 '99 03:23PM BURLINGTON RESEARCH
P.15/20
QURLIN
RESEARCH
Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NP )ES Testing
Reporting & Data Handling Services
1302 Belmont Street • Burlington. NC 27215-6935 • Phone [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: Mr. Roy Rittle
SAMPLE DESC: SPRUCE PINE SAMPLE TYPE:WASTEWATER,GRAB
03 2/99 16:30 SITE 30 PPM
COLLECTED: /0
WORK ORDER #: 9C104-007
RECEIVED: 03/03/99
REPORTED: 03/04/99
PO NUMBER:
LPAIR
Fluoride
EPA 340.2
Cerio60d�ap hnia 48- our Acute Static Bioassay Started 03/02/99 16:45 N/A > 100 LC50%
� - -
• Burlington
DATE/TIME/ANALYST MQL
RESULT I
Started 03/04/99 10:00 0.10
Analyzed 03104/99 by 3CB at BRI - Burlington
30.5 mks,
EPA 0491027E Analyzed 03/04/99 by 7Ca at BRI
MQL = Minimum Quantitation Limit
Water Environmental Services -Eden
Dlv)slon of Burlington Research. Inc.
370 W. Meadow RoPhone (336) 823.892 1 Eden,
(32a) 623-5878
Page 7
Page 50
Water Environmental Services -Kinston
Division of Bur)ington Research. 104-
10o E. Gordon Street • Kinston, NC 28501 45
Phone [phone] • Fax [phone]

• MAR 04 ' 99 03 : 23PM BURLINGTON RESEARCH
P.16/20
BURLINGTON
RESEARCH
Effluent Toxicity Report Form - Acute LC5O
Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
1302 Belmont Street • Burlington, NC 27215-6935 • Phone [phone] • Fax [phone]
Facility UNiMIN
Laboratory Performing Test
x
NPDES# R&D Pipe* County
Burlington Research. inc. - Cert. # 002
Comments:
Date:
3/4/99
Signs re of Operator In Responsible Charge
30 PPM
1 SI nature at Laboratory Supervisor
ERI# 90104-007
nvirorirtal Solar Ices Branch
Div. of Water Ouality
MAIL ORIGINAL TO: NO Dept. of ENR
4401 Reedy Creek Road
Raleigh. NC 27607-6445
Test
(Mortality expressed as , combining replicates)
LC60 = >ioo %
95% Confidence Limits (%) Moving Average
N/0 tO Spearman
Organism Tested:
Ceriodaphnia dubia
MoSiod Vern OEM tom AT-1 (3/87) OM
Water Environmental Services -Eden
Division of Burlington Reseatch, Inc.
370 W. Meadow Road • Eden. NC 27288
Phone [phone] • Fax [phone]
Tax
Sample
Hardnesa(M51/1..)
Spec. Cond.(mIcromhos)
Chlorine(mg/L)
sample temp ® receipt
(deg. C)
Problt
Kerber Other
Method of Determination
Mart Erbd
7.85
7105
Concentration (%)mortality (%)
Start End
7.31 Control 8.1 1 8.3
7.43 High 8.1 1 8.6
PH
13AI rev. tz/s3 otVormavogetfeem
Page 51
Water Environmental Services -Kinston
Division of Burlington Research, Inc.
100 E. Gordon Street • Kinston, NO 28501 9
Phone [phone] • Fax [phone]

MAR 04 '99 03:25PM BURLINGTON RESEARCH
P.17/20
BURLINGTON
RESEARCH
Aquatic bioassay Testing ► Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
1302 Belmont Street • Burlington, NC 27215-6935 • Phone [phone] • Fax [phone]
a.
ANALYTICAL REPORT
CUSTOMER: Unimin Corp.
REPORT TO: Mr. Roy Rittle
SAMPLE DESC: SPRUCE PINE
SAMPLE TYPE: WASTEWATER, GRAB
COLLECTED: 03/02/99 16:35 SITE: 40 PPM
WORK ORDER #: 9C104-048
RECEIVED: 03/03/99
REPORTED: 03/04/99
PO NUMBER:
PARAMETER DATET[ 1ME/ANALYST
Fluoride
EPA 340.2
MQL RESULT
Started 03/04/99 10:00 0.10
Analyzed 03/04/99 by JCB at BRI - Burlington
41.5
Ceriodaphnia 48-Hour Acute Static Bioassay StaAnalyzed 03/02/99 /99 16:45
y JCB at BRI N/A
Burlington
EPA600491027F
> 100 LC50 %
MQL = Minimum Quantitation Limit
Certifications:
$RI - Burlington
NC Chemistry: #85, Biomonitoring: #002, Drinking Water: #37743, Radiation License: #001-0904-0G
VA SWCB ID: #000061, Drinking Water. #00018
SC Laboratory YD: #99042
EPA Chemistry Lab ID: NC00137, Bioassay Lab ID: NC2721500
Water Environmental Services -Eden
Division of Burlington Research, inc.
370 W. Meadow Road , NC 27288
Phone [phone] • • Fax (n336) 623-5878
Page
8
Page 52
Water Environmental Services - Kristen
Division of Burlington Research, Inc.
100 E. Gordon Street • Kinston, NC 28501
Phona [phone] • Fax [phone]

, MAR 04 ' 99 03: 25PM BURLINGTON RESEARCH
P.18/20
BURLINGTON
RESEARCH
Aquaic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
1302 Belmont Street • Burlington, NC 27215-6935 • Phone [phone] • Fax [phone]
Effluent Toxicity Re ort Form - Acute LC50
Facility UNIM1N
Laboratory Performing Teat
x
NPDES# R&D PIpe#
Burlington Research, Inc. - Cett. # 002
Signature at Operator In Responsible Charge
Date:
nvironmantal Sciences ranc
Div. of Water Quality
NC Dept. of ENR
4401 Reedy Creek Road
Raleigh, NC 27607-8445
Spec. Cond.(mlcromhoa)
ChIorine(mg/L)
Sample temp @ receipt
(deg. C)
Method of Determination
Moving Average
Spearman Kerber
140018ed treat DEM tarn AT-1 (3/87) reV.0/90
Water Environmental Services Edon
Division of Burlington Research, Inc.
370 W. Meadow Road • Eden, NO 27288
Phone [phone] • Fax [phone]
SRI rem. 12103
3J4/99
catormaVAattiarrn
Page 5 3
Water Environmental Services -Kinston
Division of Burlington Research. Inc.
100 E. Gordon Street • Kinston. NC 28501
Phone [phone] • Fax [phone]
11114 1443

llI 8URL1t3GTdN RESEARCH, INC.
CHAIN OF CUSTODY; RECORD
u 3rOvqest
Edon, NC�27288
Phone (336)
Fax ((336) 623-B7B
623-8921
1302 BoNC
Burlington, Street27215.6935
no
570-4661
Fax [phone]
CLIENT: `)/1(M SEND REPORTTO:_ ✓ purchaso Ord©r No.:
Facility/Site: nature
Y l : �� ` (Sig
Sampler (Prrni) -- SAMPLE TYPE o cc`t" o rc z �y ANALYSIS
REQUIRED
COMPOSITEm3 W
GRAB =o 6i1Gt�`"t
-r HAND AUTO z ll
SAMPLE
ID
DATE_
TIME
DATE
TIME
SAMPLE
COLLECTION
STARTED
Yost No
Ye3i No
Yes; ND
to dechtorinated at time of collection? Yes Q No
Waathesamp FOR CLIENT USE ONLY
Dote-
3
D.te:
Ipp©d by: (Sig.
Received by: (Sig.)
Method of Shipment
Qhone [phone]
fax [phone]
Fax:
66f b0 anN
taiWVFORBRIILABiUSE`ONI Y:Fti► "';
preservation Codas:
iENIP. A ==1ce O3 F = E = NaOH
B HNNone
'4� C' C H2SO4 G = CUPRIC
- D = NCI H S HCHO
1111111111111
ur osos? Yes No❑
Will the results be used for regulatory monitoring p p
1`FOR i:AB USESPNLY.700,01 ..
plo Int
aty Comment
• ..1,nv-,lnro
Pink - BRI - Laboratory Goldenrod - C1lont - Copy
03:26PM BURLINGTON RESEARCH
r)

1II BURLINGTON RESEARCH, INC.
CHAIN OF CUSTODY RECORD
CLIENT:
Facillty/Site:
Sampler: (Print)
SAMPLE
ID
Yost No
(Signature
SAMPLE
COLLECTION
STARTED
DATE__
ENDED
DATE
TIME
1302 Belmont Street
Burlington, NC 27215.6935
Phone [phone]
Fax [phone]G96
COMPOSITE
Was the sample dechlor(nated at time
of collection? Y es
FOR USE ONLY ❑
De e:
if /bi
ate.
Received by: (Sig.
Y:4 f)
Edon, NC 27298
Phone [phone]
Fax [phone]
Phone [phone]
Fax [phone]
D
SEND REPORT TO: fie. ,T 1
Fax: r7✓ 2-1/) - 4 ///
Phone:,
Purchase Order No.:
ANALYSIS
REQUIRED
fir(///,,
%,�//7//
y _ ._F EIRf;LAB USE;ONLY:YW.
Preservation Codes:_
A-1ce. E=NaOK
B = HNO3 F =.None
C = H2SO4 G-= CUPRIC
D=HCI H=HCHO
TEMP.
(4° C)
No 0 MN Will the results be used for regulatory monitoring purposes? Yes ❑ No
• FOR LAECUSEtONLY`g."5,�' s����• `�:�.. s.
no�o• Time:
Method of Shipment
rani - 1 �hnr1tr rV
/03-D
Pink - BRI - Laboratory Goldenrod - Client - Copy
H0eid3S3d N010NI1df1 Wd 2 :E2
fV
m
ry
t)R•4T T-0a

Unimin/K-T Feldspar/Felspar Corporation Meeting
March 19,1999
Opening comments from Charlie Stover, Unimin- NPDES permit renewal in Dec. 2001.
Wanted to meet to get DWQ ideas on Dept.'s renewal. Fluoride limits allocated #'s
waited to approach and find out any changes in the permits.
He also talked about data submitted to DWQ. Did some toxicity testing, fluoride toxicity
testing is imprecise. Concerns: 1) knowledge of acute toxicity. Use studies on
ceriodaphnia. Did acute and chronic study in past two months and sent conclusions.
Existing standard is protective of the environment- overly so, standard could be
increased. Acute and chronic toxicity — duplicated by two separate labs, ETT and
Burlington. Chronic shows 8 — 16 ppm failure of fluoride toxicity.
Reports include lab sheets from labs, show acute and chronic toxicity info to address the
area of acute to chronic results.
Chronic to acute results 8ppm lowest failed in chronic, 40 ppm lowest failed in acute. 7
ppm is protected , 1.8 ppm standard for NC.
2) Are any changes in fluoride calculations to be made in the permit? Feel that 1.8
ppm for fluoride is too restrictive for North Toe River. Want to know if fluoride
would be ratcheted down Are we looking at the fluoride standard being reduced?
What are DWQ intentions with the limits? Higher correction or lower correction?
Unimin, Feldspar, and KT Feldspar can live with what they have right now. Not looking
for higher poundage, don't want any reduction in existing poundage.
Unimin have developed two new plants in the last couple of years, Asian market took
some business. Any reduction, were there any discrepancies in calculations?
DWQ will give written response to the companies and a copy of the Alcoa report by
the end of April.
Companies will correct typos and submit updated report to DWQ.
March 29, 1999 — Rec'd letter from Unimin requesting clarification of permit renewals
and recommending that 7 parts per million of fluoride would be protective of aquatic life
in the North Toe River. Indicated that Unimin, K-T Feldspar, and Feldspar were
requesting no change in the Fl poundage limits.
April 20,1999 — Rec'd copy of letter to Rep. Gregg Thompson from Charles Case,
Unimin's attorney, supporting House Bill 928 which allows for additional study on the
fluoride issue.

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Unimin Corp. K-T Feldspar
Date Ups FI Dwn FI Ups FI Dwn FI
Feb-99 1.03 0.93
Jan-99 1.13 1.05
Dec-98 1.99 1.74 * 1.67 2.17 *
Nov-98 2.25 1.89 * 1.96 2.45 *
Oct-98 1.77 1.7 * 1.93 2.1 *
Sep-98 1.92 1.7 * 1.97 2.14 *
Aug-98 1.4 1.53 * 1.21 1.42 *
Jul-98 1.34 1.24 * 1.42 1.57 *
Jun-98 0.8 0.77 1.1 1.17 *
May-98 0.54 0.51 0.95 0.78
Apr-98 0.67 0.55 0.95 0.92
Mar-98 0.68 0.63 *U 0.629 0.95
Feb-98 0.54 0.5 0.519 0.633
Jan-98 0.57 0.54 0.13 0.806 *
Dec-97 1.34 1.38 * 1.18 1.31 *
Nov-97 1.37 1.38 * 1.27 1.64 *3.5u,2.9d
Oct-97 1.86 1.85 * 1.76 2.06 *3.9d
Sep-97 1.6 1.72 2u,2.9d 1.7 1.79 *
Aug-97 1.38 1.42 * 1.18 1.53 *
JuI-97 0.73 0.7 0.62 0.975
Jun-97 0.73 0.71 0.65 1.02
May-97 0.69 0.65 0.66 0.81
Apr-97 0.55 0.5 -
Mar-97 0.42 0.38 0.36 0.7
Feb-97 0.65 0.58 0.6 0.96
Jan-97 0.72 0.77 0.71 0.75
* - indicates a reported sample value > the FI standard of 1.8 mg/I
Values in bold indicate a monthly average > the FI standard of 1.8 mg/I.