Conductivity and Permeability of the Submitted Samples
Of 30/50, 40/70, and 100 Mesh Frac Sands at
2 lb/ft2 and at 2,000 - 8,000 psi Closure Stresses at
150°F for 50 Hours between Ohio Sandstone
(Duplicate Testing)
Prepared For:
Mr. Rob Meyer
Mississippi Sand, LLC
12200 Big Bend Rd.
St. Louis, MO 63122
(314) 678-7844 Phone
(314) 378-6459 Mobile
[email protected]
Prepared By:
Stim-Lab, Inc.
P.O. Box 1644
7406 North Hwy 81
Duncan, OK 73534-1644
___________________________________________
Kathy Abney, Conductivity Supervisor
___________________________________________
Daniel Eddings, Research & Development Manager
P.O. Number: Per R. Meyer
File Number: SL 10618
April 2013
LL INTERPRETATIONS ARE OPINIONS BASED ON INFERENCES FROM SAMPLES AND LOGS, WHICH WERE SUPPLIED. WE CANNOT, AND DO NOT, GUARANTEE THE ACCURACY OR
CORRECTNESS OF ANY INTERPRETATIONS, AND WE SHALL NOT, EXCEPT IN THE CASE OF GROSS OR WILLFUL NEGLIGENCE ON OUR PART, BE LIABLE OR RESPONSIBLE FOR ANY LOSS,
COSTS, DAMAGES OR EXPENSES INCURRED OR SUSTAINED BY ANYONE RESULTING FROM ANY INTERPRETATION MADE BY ANY OF OUR OFFICERS, AGENTS OR EMPLOYEES. THESE
INTERPRETATIONS ARE ALSO SUBJECT TO OUR GENERAL TERMS AND CONDITIONS AS SET OUT IN OUR CURRENT PRICE SCHEDULE. NOTICE: SAMPLES SUBMITTED TO STIM-LAB, INC. FOR
USE IN TESTING SERVICES ARE SUBJECT TO DISPOSAL OR STORAGE FEES FOLLOWING THE COMPLETION OF THE TESTING SERVICES. DIRECTIVE AS TO THE DISPOSITION OF SAMPLES
MUST BE SUBMITTED IN WRITING WITH THE SAMPLES OR OTHERWISE PROVIDED DURING THE COURSE OF THE PROJECT. STIM-LAB, INC. RESERVES THE RIGHT TO REQUEST THAT YOU
PICKUP SAMPLES, WHETHER FORMATION MATERIAL, CHEMICALS SUPPLIED, FIXTURES OR OTHER MATERIALS RELATING TO A PROJECT. YOU MAY BE CHARGED A REASONABLE SHIPPING
AND PACKAGING FEE FOR RETURN OF SAMPLES FOR WHICH PICK UP ARRANGEMENTS HAVE NOT BEEN MADE. STIM-LAB, INC. EXPRESSLY DISCLAIMS LIABILITY FOR
INTENTIONAL DISPOSAL OR UNINTENTIONAL LOSS OF SUBMITTED SAMPLES FOR WHICH NO WRITTEN DIRECTIVE HAS BEEN PROVIDED.
STIM-LAB, Inc.
7406 North HWY 81
Duncan, Oklahoma 73533
Phone: 580-252-4309
Fax: 580-252-6979
[email protected]
[email protected]
April 17, 2013
Mr. Rob Meyer
Mississippi Sand, LLC
12200 Big Bend Rd.
St. Louis, MO 63122
(314) 678-7844 Phone
(314) 378-6459 Mobile
[email protected]
Dear Mr. Meyer:
STIM-LAB, Inc. has completed the conductivity evaluations of the samples submitted by
your firm marked 30/50, 40/70, and 100 Mesh frac sands. The samples arrived at StimLab on March 26, 2013. The samples were evaluated in duplicate at 2 lb/ft2 at 150 °F
and long-term for 50 hours at 2000, 4000, 6000, and 8000 psi closure stress between
Ohio Sandstone.
A summary of conductivity and permeability vs. stress is contained in Figures 1 and 2.
The conductivity data is presented in Tables 1 - 6. The sieve analyses of the samples
are provided in Table 7. The procedures utilized are outlined in the following section of
this report.
Thank you and Mississippi Sand, LLC for allowing STIM-LAB to perform this test series.
If you have any questions regarding the testing or results, please do not hesitate to
contact us.
Sincerely,
Daniel Eddings
Research & Development Manager
Kathy Abney
Conductivity Supervisor
PROCEDURE FOR CONDUCTIVITY AND
LIQUID PERMEABILITY MEASUREMENTS
MODIFIED PER CUSTOMER REQUEST FROM
(ISO 13503-5 / APIRP-19D)
1) The equipment used for the measurement of conductivity and liquid permeability
included:
(a) 75 ton Dake Press with air oil intensifier. API SS316 flow cells with 10
sq in. flow paths.
(b) Rosemont (smart family) 40:1 pressure transducers for measuring
pressure drop and rate plumbed with ¼ in. lines and calibrated with
the smart system computer and set at the 0-5 inch of water span
range.
(c) Two gallon nitrogen driven fluid reservoirs filled with 2% KCl and
deoxygenated with nitrogen.
(d) Internal gauges and calipers for measuring widths.
(e) PC to process data and calculate conductivity and permeability.
(f) Two - 10 sq in. Ohio Sandstone.
2.
An API cell was loaded with proppant sample to be tested. The proppant was
leveled with a blade device.
3.
The proppant sample was placed between the core slabs and was made a part
of a 2 separate 3-cell stacks.
4.
The cell were stacked to within 0.002 in. from top to bottom and positioned
between the platens of the Dake Press. Pressure was increased to 500 psi and
the system was evacuated and saturated with water at 70-75 °F.
5.
Once saturated, the closure pressure was increased to 1,000 psi, at a rate of 100
psi/min. The proppant was allowed to equilibrate as outlined in the data tables.
6.
The flow rate, pressure differential, and average width were measured at each
pressure in order to calculate conductivity and permeability. Measurements were
taken and averaged to arrive at each conductivity value. Flow rate was
measured with a LiquiFlow meter, which was calibrated with a balance to 0.01
ml/min. Darcy's Law was used for the calculations to determine the conductivity
and permeability.
7.
The test temperature was increased to 150 °F and allowed to equilibrate. The
temperature was left at 150 °F for 12 hours prior to increasing the closure.
8.
The conductivity and permeability of the proppant were collected at 1,000, 2,000,
4,000, 6,000, and 8,000 psi at 150 °F as stated in the data tables.
9.
The pressure was increased at 100 psi per minute at 1,000 or 2,000 psi
increments to 8,000 psi closure stress for the requested long-term conductivity
evaluation for 50 hours as outlined below.
10.
The conductivity and permeability of the proppant were continuously monitored at
2,000 psi and 150 °F for 50 hours.
11.
The conductivity and permeability of the proppant were continuously monitored at
4,000 psi and 150 °F for 50 hours.
12.
The conductivity and permeability of the proppant were continuously monitored at
6,000 psi and 150 °F for 50 hours.
13.
The conductivity and permeability of the proppant were continuously monitored at
8,000 psi and 150 °F for 50 hours.
All ISO13503-2:2006 / API RP-19C evaluations followed the procedures as outlined in
that document. These are the new procedures created from the old API RP 56, 58 and
60 procedures.
Figure 1
Long-Term Conductivity and Permeability
10000
1000
1000
100
100
10
30/50 Mississippi Sand - T1
40/70 Mississippi Sand - T1
100 mesh Mississippi Sand - T1
10
0
2000
4000
6000
8000
0
2000
4000
6000
1
8000
Closure Stress (psi)
SL 10618
April 3 - 12, 2013
Permeability (Darcy)
Conductivity (md-ft)
2 lb/ft² 30/50 - T1, 40/70 - T1 and 100 Mesh - T1 Mississippi Sand
Submitted by Mississippi Sand LLC at Stim-Lab on March 26, 2013
in 2% KCl between Ohio Sandstone at 150 °F
Figure 2
Long-Term Conductivity and Permeability
10000
1000
1000
100
100
10
30/50 Mississippi Sand - T2
40/70 Mississippi Sand - T2
100 Mesh Mississippi Sand - T2
10
0
2000
4000
6000
8000
0
2000
4000
6000
1
8000
Closure Stress (psi)
SL 10618
April 5 - 14, 2013
Permeability (Darcy)
Conductivity (md-ft)
2 lb/ft² 30/50 - T2, 40/70 - T2 and 100 Mesh - T2 Mississippi Sand
Submitted by Mississippi Sand LLC at Stim-Lab on March 26, 2013
in 2% KCl between Ohio Sandstone at 150 °F
SL 10618
Table 1
Conductivity and Permeability of
2 lb/ft² 30/50 Mississippi Sand - T1
Submitted by Mississippi Sand LLC at Stim-Lab on March 26, 2013
Between Ohio Sandstone core
Hrs at Closure
& Temperature
Closure
(psi)
Temp
(° F)
Conductivity
(md-ft)
Width
(in)
Permeability
(Darcy)
-14
-2
1000
1000
75
150
2792
2520
0.221
0.220
152
138
0
10
20
30
40
50
2000
2000
2000
2000
2000
2000
150
150
150
150
150
150
2249
2146
2123
2109
2099
2091
0.218
0.217
0.216
0.216
0.216
0.216
124
119
118
117
117
116
0
10
20
30
40
50
4000
4000
4000
4000
4000
4000
150
150
150
150
150
150
1648
1599
1587
1581
1576
1572
0.212
0.210
0.209
0.209
0.209
0.209
93
91
91
91
91
90
0
10
20
30
40
50
6000
6000
6000
6000
6000
6000
150
150
150
150
150
150
1164
965
919
892
873
858
0.206
0.204
0.203
0.203
0.202
0.202
68
57
54
53
52
51
0
10
20
30
40
50
8000
8000
8000
8000
8000
8000
150
150
150
150
150
150
748
565
523
498
480
466
0.199
0.197
0.196
0.195
0.195
0.195
45
34
32
31
30
29
April 3 - 12, 2013
Median Dia .= 0.471 mm
0.0185 inch
Sieve
20
25
30
35
40
45
50
60
70
80
100
pan
Total
% In Size as -30+50
% Retained
0.0
0.5
4.7
26.4
47.9
18.0
1.6
0.4
0.2
0.1
0.1
0.1
100.0
93.9
SL 10618
Table 2
Conductivity and Permeability of
2 lb/ft² 40/70 Mississippi Sand - T1
Submitted by Mississippi Sand LLC at Stim-Lab on March 26, 2013
Between Ohio Sandstone core
Hrs at Closure
& Temperature
Closure
(psi)
Temp
(° F)
Conductivity
(md-ft)
Width
(in)
Permeability
(Darcy)
-14
-2
1000
1000
75
150
920
890
0.218
0.217
51
49
0
10
20
30
40
50
2000
2000
2000
2000
2000
2000
150
150
150
150
150
150
820
786
778
773
770
768
0.214
0.213
0.213
0.213
0.213
0.213
46
44
44
44
43
43
0
10
20
30
40
50
4000
4000
4000
4000
4000
4000
150
150
150
150
150
150
633
626
624
623
623
622
0.210
0.209
0.208
0.208
0.208
0.208
36
36
36
36
36
36
0
10
20
30
40
50
6000
6000
6000
6000
6000
6000
150
150
150
150
150
150
549
499
487
480
475
471
0.204
0.202
0.202
0.202
0.202
0.202
32
30
29
29
28
28
0
10
20
30
40
50
8000
8000
8000
8000
8000
8000
150
150
150
150
150
150
416
366
354
348
343
339
0.200
0.199
0.199
0.198
0.198
0.198
25
22
21
21
21
21
April 3 - 12, 2013
Median Dia. = 0.290 mm
0.0114 inch
Sieve
30
35
40
45
50
60
70
80
100
120
pan
Total
% In Size as -40+70
% Retained
0.0
0.0
2.0
14.5
28.5
31.5
16.6
5.4
1.2
0.1
0.0
99.9
91.1
SL 10618
Table 3
Conductivity and Permeability of
2 lb/ft² 100 Mesh Mississippi Sand - T1
Submitted by Mississippi Sand LLC at Stim-Lab on March 26, 2013
Between Ohio Sandstone core
Hrs at Closure
& Temperature
Closure
(psi)
Temp
(° F)
Conductivity
(md-ft)
Width
(in)
Permeability
(Darcy)
-14
-2
1000
1000
75
150
729
588
0.226
0.225
39
31
0
10
20
30
40
50
2000
2000
2000
2000
2000
2000
150
150
150
150
150
150
536
531
530
530
529
529
0.224
0.223
0.223
0.223
0.223
0.223
29
29
29
29
28
29
0
10
20
30
40
50
4000
4000
4000
4000
4000
4000
150
150
150
150
150
150
392
360
352
348
345
342
0.219
0.217
0.217
0.217
0.217
0.217
22
20
19
19
19
19
0
10
20
30
40
50
6000
6000
6000
6000
6000
6000
150
150
150
150
150
150
279
245
237
233
229
227
0.215
0.211
0.211
0.211
0.211
0.211
16
14
14
13
13
13
0
10
20
30
40
50
8000
8000
8000
8000
8000
8000
150
150
150
150
150
150
204
171
163
158
155
153
0.208
0.206
0.205
0.204
0.204
0.204
12
10
10
9.3
9.1
9.0
April 3 - 12, 2013
Median Dia .= 0.186 mm
0.0073 inch
Sieve
40
45
50
60
70
80
100
120
140
170
200
pan
Total
% In Size as -50+140
% Retained
0.0
0.1
2.1
12.4
18.5
24.5
21.9
11.5
5.2
2.6
0.9
0.3
100.0
94.0
SL 10618
Table 4
Conductivity and Permeability of
2 lb/ft² 30/50 Mississippi Sand - T2
Submitted by Mississippi Sand LLC at Stim-Lab on March 26, 2013
Between Ohio Sandstone core
Hrs at Closure
& Temperature
Closure
(psi)
Temp
(° F)
Conductivity
(md-ft)
Width
(in)
Permeability
(Darcy)
-14
-2
1000
1000
75
150
2519
2461
0.221
0.220
137
135
0
10
20
30
40
50
2000
2000
2000
2000
2000
2000
150
150
150
150
150
150
2173
2148
2143
2139
2137
2135
0.218
0.217
0.217
0.217
0.217
0.217
120
119
119
118
118
118
0
10
20
30
40
50
4000
4000
4000
4000
4000
4000
150
150
150
150
150
150
1695
1667
1660
1657
1654
1652
0.213
0.211
0.211
0.211
0.211
0.211
96
95
95
94
94
94
0
10
20
30
40
50
6000
6000
6000
6000
6000
6000
150
150
150
150
150
150
1185
1025
989
967
952
940
0.209
0.207
0.207
0.206
0.206
0.206
68
60
57
56
56
55
0
10
20
30
40
50
8000
8000
8000
8000
8000
8000
150
150
150
150
150
150
856
623
569
537
515
497
0.202
0.200
0.199
0.198
0.197
0.197
51
38
34
33
31
30
April 5 - 14, 2013
Median Dia. = 0.471 mm
0.0185 inch
Sieve
20
25
30
35
40
45
50
60
70
80
100
pan
Total
% In Size as -30+50
% Retained
0.0
0.5
4.7
26.4
47.9
18.0
1.6
0.4
0.2
0.1
0.1
0.1
100.0
93.9
SL 10618
Table 5
Conductivity and Permeability of
2 lb/ft² 40/70 Mississippi Sand - T2
Submitted by Mississippi Sand LLC at Stim-Lab on March 26, 2013
Between Ohio Sandstone core
Hrs at Closure
& Temperature
Closure
(psi)
Temp
(° F)
Conductivity
(md-ft)
Width
(in)
Permeability
(Darcy)
-14
-2
1000
1000
75
150
829
823
0.217
0.217
46
46
0
10
20
30
40
50
2000
2000
2000
2000
2000
2000
150
150
150
150
150
150
771
754
750
747
746
745
0.215
0.214
0.213
0.213
0.213
0.213
43
42
42
42
42
42
0
10
20
30
40
50
4000
4000
4000
4000
4000
4000
150
150
150
150
150
150
666
636
629
625
622
620
0.210
0.209
0.208
0.208
0.208
0.208
38
37
36
36
36
36
0
10
20
30
40
50
6000
6000
6000
6000
6000
6000
150
150
150
150
150
150
549
509
499
494
490
487
0.206
0.204
0.204
0.203
0.203
0.203
32
30
29
29
29
29
0
10
20
30
40
50
8000
8000
8000
8000
8000
8000
150
150
150
150
150
150
429
370
356
348
342
338
0.200
0.199
0.198
0.198
0.197
0.197
26
22
22
21
21
21
April 5 - 14, 2013
Median Dia .= 0.290 mm
0.0114 inch
Sieve
30
35
40
45
50
60
70
80
100
120
pan
Total
% In Size as -40+70
% Retained
0.0
0.0
2.0
14.5
28.5
31.5
16.6
5.4
1.2
0.1
0.0
100.0
91.1
SL 10618
Table 6
Conductivity and Permeability of
2 lb/ft² 100 Mesh Mississippi Sand - T2
Submitted by Mississippi Sand LLC at Stim-Lab on March 26, 2013
Between Ohio Sandstone core
Hrs at Closure
& Temperature
Closure
(psi)
Temp
(° F)
Conductivity
(md-ft)
Width
(in)
Permeability
(Darcy)
-14
-2
1000
1000
75
150
633
598
0.225
0.224
34
32
0
10
20
30
40
50
2000
2000
2000
2000
2000
2000
150
150
150
150
150
150
544
526
522
519
518
516
0.223
0.222
0.221
0.221
0.221
0.221
29
28
28
28
28
28
0
10
20
30
40
50
4000
4000
4000
4000
4000
4000
150
150
150
150
150
150
405
354
343
336
331
327
0.218
0.217
0.216
0.216
0.216
0.216
22
20
19
19
18
18
0
10
20
30
40
50
6000
6000
6000
6000
6000
6000
150
150
150
150
150
150
271
212
198
190
185
180
0.214
0.212
0.211
0.210
0.210
0.210
15
12
11
11
11
10
0
10
20
30
40
50
8000
8000
8000
8000
8000
8000
150
150
150
150
150
150
162
117
107
101
97
93
0.207
0.204
0.203
0.202
0.201
0.201
9.4
6.9
6.3
6.0
5.8
5.6
April 5 - 14, 2013
Median Dia .= 0.186 mm
0.0073 inch
Sieve
40
45
50
60
70
80
100
120
140
170
200
pan
Total
% In Size as -50+140
% Retained
0.0
0.1
2.1
12.4
18.5
24.5
21.9
11.5
5.2
2.6
0.9
0.3
100.0
94.0
SL 10618
Table 7
Pre-Test Sieve Analysis of Submitted Samples
Submitted by Mississippi Sand LLC at Stim-Lab on March 26, 2013
ISO 13503-2, Section 6, "Sieve Analysis"
Sample I.D.
Mississippi Sand LLC
Frac Sand
30/50
US Standard
Weight %
Mississippi Sand LLC
Frac Sand
100 Mesh
Weight %
Mississippi Sand LLC
Frac Sand
40/70
Weight %
Sieve No.
Retained
Cumulative
Retained
Cumulative
Retained
Cumulative
8
10
12
14
16
18
20
25
30
35
40
45
50
60
70
80
100
120
140
170
200
pan
total
in-size
ISO Median Diameter
(mm) or d50, 6.5.3
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.5
4.7
26.4
47.9
18.0
1.6
0.4
0.2
0.1
0.1
0.0
0.0
0.0
0.0
0.1
100.0
93.9
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.5
5.2
31.6
79.5
97.5
99.1
99.5
99.7
99.8
99.9
99.9
99.9
99.9
99.9
100.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.1
2.1
12.4
18.5
24.5
21.9
11.5
5.2
2.6
0.9
0.3
100.0
94.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.1
2.2
14.6
33.1
57.6
79.5
91.0
96.2
98.8
99.7
100.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
2.0
14.5
28.5
31.5
16.6
5.4
1.2
0.1
0.0
0.0
0.0
0.0
100.0
91.1
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
2.1
16.6
45.1
76.6
93.2
98.6
99.8
99.9
100.0
100.0
100.0
100.0
ISO Mean Diameter
(mm) 6.5.2
April, 2013
= as -30+50
= as -50+140
0.471
0.186
0.290
0.479
0.194
0.297
= as -40+70