Fluid Loss Control Pills

5.1. HEC Pills

Objective

The objective of the test is to verify HEC polymer stability in a 1.19 s.g. sodium chloride (NaCl) and sodium
bromide (NaBr) brines as HEC is documented (SPE 38155 and 58728) to precipitate out of solution in near
saturated NaCl brines at high temperatures. Test with NaBr is done to offer an alternative pill formulation
at the required density.

Executive Summary

•As expected, HEC polymer precipitated out of the 1.19 s.g. NaCl-based pill after static aging for 16 hours
at 220 ⁰F. Precipitated polymer was observed as a semi-solid polymer layer on top of the fluid (see Figure
1).

•HEC pill formulated in 1.19 s.g. NaBr brine was stable after static aging for 16 hours at 220 ⁰F. No sign of
polymer precipitation was observed.

•At BHT temperatures of 220 ⁰F and above, it is recommended to use NaBr as base brine for HEC pills with
densities above 1.10 s.g. or near NaCl saturation point (1.20 s.g.) to prevent polymer precipitation down
hole and potential formation damage.

Discussion

Two pills were formulated using 1.19 s.g. NaCl brine and 1.19 s.g. NaBr brine as base fluids and 6 ppb
SAFE-VIS E liquid HEC (2.5 ppb active HEC concentration). Formulations are shown in Table 1. The pills
were mixed until polymers were fully yielded and put to static age at 220 ⁰F for 16 hours. Observations
were made before and after static aging the fluids and photographs were taken.

Table 1—NaCl- and NaBr-based high viscosity pill formulations with HEC (SAFE-VIS E)

NaCl-based Pill NaBr-based Pill

Product Concentration Concentration
Water 0.897 bbl/bbl 0.637 bbl/bbl
NaCl salt 102.7 lb/bbl -
12.5 ppg NaBr brine - 0.368 bbl/bbl
SAFE-VIS E 6 ppb (2.5 ppb active HEC) 6 ppb (2.5 ppb active HEC)

Figure 1 and 2 show photographs of the pills, NaCl-based and NaBr-based, respectively, before and after
static aging at 220 ⁰F for 16 hours.

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 Figure 2—Digital images of 1.19 s.g. NaBr-
Figure 1—Digital images of 1.19 s.g. NaCl-
based HEC pill: a) base brine; b) HEC pill before
based HEC pill: a) base brine; b) HEC pill before
aging; and c) HEC pill after static aging at 220
aging; and c) HEC pill after static aging at 220
⁰F. Note pill was stable after static aging. No
⁰F. Note polymer precipitated on top of the
sign of polymer precipitation was observed.
fluid after aging.

Appendix

References

Hodge, R.M.1998. HEC Precipitation at Elevated Temperature: An Unexpected Source of Formation

Damage. SPE 38155.SPE Drilling and Completion.
MARCOS, Anez. HEC High-Viscosity Pill in Sodium Chloride and Sodium Bromide Brines.

5.1.1. HEC Compatibility with Brines at Bottom-Hole Conditions

The purpose of this laboratory test was to check the compatibility of Safe-Vis E in NaCl/NaBr brine. Table
1 shows the formulation used for the test. Formulation 1 was prepared without Safe-Vis E, and in

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formulations 2, 3, 4 & 5 Safe-Vis E was used with the same concentration, but different pH. The pH was
measured after 1:1 dilution with water. Maximum viscosity will be achieved at a pH in the range of 7 to 9.
Table 1 – Formulations
Formulation # 1 2 3 (pH= 7) 4 (pH= 8) 5 (pH= 9)

Products ppg Mix Order Time (min) ppg Mix Order Time (min) ppg Mix Order Time (min) ppg Mix Order Time (min) ppg Mix Order Time (min)
Water 248.22 1 248.22 1 248.22 1 248.22 1 248.22 1
NaCl 39.88 2 5 39.88 2 5 39.88 2 5 39.88 2 5 39.88 2 5
NaBr (12.5 ppg) 132.25 3 5 132.25 3 5 132.25 3 5 132.25 3 5 132.25 3 5
Safe Vis-E 6 4 15 6 4 15 6 4 15 6 4 15

Samples 1 & 2 were blended and dynamically aged for 16 hours at 220 ⁰F.
Formulation # 1 2 3 (pH= 7) 4 (pH= 8) 5 (pH= 9)
Date of Test: 16-17 Nov 2015 16-17 Nov 2015 24-Nov-15 24-Nov-15 24-Nov-15
PERIOD AGED Hours 16 16
TEMPERATURE ºF 220 220
DYNAMIC/STATIC D/S Initial S Initial S Initial Initial Initial
Mud Weight ppg 10
RHEOLOGY: T (ºF) 120 120 120 120 120 120 120 120 120 120
600 RPM 135 114 126 180 134
300 RPM 102 85 98 142 104
200 RPM 90 71 84 125 89
100 RPM 67 49 64 97 66
6 RPM 15 7 14 25 13
3 RPM 10 4 9 16 7
GELS 10" lb/100ft2 10 5 9 16 7
GELS 10' lb/100ft2 10 5 10 16 7
APPARENT VISC. cP 0 0 67.5 57 63 0 90 0 67 0
PLASTIC VISC. cP 0 0 33 29 28 0 38 0 30 0
YIELD POINT lbs/100ft2 0 0 69 56 70 0 104 0 74 0

Figure 1 and 2 show formulation 1, NaCl/NaBr brine without SAFE-VIS E, before and after static aging at
220 ⁰F for 16 hours.

Figure 1 - Before Aging Figure 2 - After Aging

Figure 3 and 4 show formulation 2, NaCl/NaBr brine with Safe-Vis E, before and after static aging at 220
⁰F for 16 hours.

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 Figure 3 - Before Aging Figure 4 - After Aging

Conclusion

No precipitation was observed in formulation 2 after static aging.

References
RASHEED, Ami. Project Number: LJ-151117-M-302 – ADMA HEC compatibility test and pH effect. 29 April
2014.

5.1.2. HEC temperature Stability

The objective of the test is to verify HEC polymer stability after heat aging at 220 ⁰F and 250 ⁰F with
different exposure times. The first test shows the rheology stability after 96 hours heat aging at 220 ⁰F.

According to the table below, there is a little decrease in rheology when heat aging for 96 hours,
comparing to 24 hours aging, but no significant change over that.

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 PRODUCT 24 h 96 h 168 h
SAMPLE Mix Time Mix Time Mix Time
COMPOSITION ppb Order (min) ppb Order (min) ppb Order (min)
WATER 109.66 1 109.66 1 109.66 1
11.6 PPG CaCl2 Brine 324.20 2 3 324.20 2 3 324.20 2 3
SAFE-VIS E 7.15 3 7.15 3 7.15 3
Defoam X 0.10 4 30 0.10 4 30 0.10 4 30
Properties
Tested By: Naseer Naseer Naseer

Date of Test: 21-22 Oct 2015 21-25 Oct 2015 28-Oct-15

PERIOD AGED Hours 24 96 168
TEMPERATURE ºF 220 220 220
DYNAMIC/STATIC D/S S S S
Mud Weight ppg 10.5 10.5 10.5
RHEOLOGY: T (ºF) 122 122 122 122 122 122
600 RPM 244 91 244 68 244 63
300 RPM 192 52 192 38 192 34
200 RPM 166 37 166 25 166 23
100 RPM 128 20 128 13 128 12
6 RPM 30 1 30 1 30 1
3 RPM 20 1 20 1 20 1
GELS 10" lb/100ft2 20 1 20 1 20 1
GELS 10' lb/100ft2 21 1 21 1 21 1
APPARENT VISC. cP 122 45.5 122 34 122 31.5
PLASTIC VISC. cP 52 39 52 30 52 29
YIELD POINT lb/100ft2 140 13 140 8 140 5
pH-Direct 9.56 9.38 9.56 7.8 9.56 7.8

Comparison of rheology after heat aging for 24, 96 and 168 hours at 220 ⁰F

The table below shows the rheology of the samples heat-aged at 220 ⁰F and at 250 ⁰F, for 24, 144 and
170 hours. The rheology dropped dramatically after heat aging for 144 hours at 250 ⁰F.

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 PRODUCT ID No. #1 (24 h) #2 (144 h) #3 (170 h)
Mix Time Mix Time Mix Time
SAMPLE COMPOSITION ppb Order (min) ppb Order (min) ppb Order (min)
WATER (Fresh Tap water) 109.66 1 109.66 1 109.66 1
11.6 PPG CaCl2 Brine IP.10.05.15-011 324.20 2 3 324.20 2 3 324.20 2 3
SAFE-VIS E IP.02.09.12-002 6.00 3 6.00 3 6.00 3
Defoam X IP.07.10.15-001 0.10 4 30 0.10 4 30 0.10 4 30
Properties
Tested By: Naseer Dennis Dennis

Date of Test: 9-10 Nov 2015 9-15 Nov 2015 9-Nov-15

PERIOD AGED Hours 24 24 144 144 170 170
TEMPERATURE ºF 220 250 220 250 220 250
DYNAMIC/STATIC D/S S S S S S S
Mud Weight ppg 10.4 10.4 10.4
RHEOLOGY: TEMP. ºF 120 120 120 120 120 120 120 120 120
600 RPM 190 101 75 190 83 7 190 82 4
300 RPM 146 59 44 146 49 4 146 48 3
200 RPM 123 39 31 123 35 2 123 34 2
100 RPM 92 23 16 92 20 1 92 19 1
6 RPM 18 2 1 18 2 0 18 2 0
3 RPM 10 1 1 10 1 0 10 1 0
GELS 10" lb/100ft2 9 1 1 9 2 0 9 1 0
GELS 10' lb/100ft2 10 1 1 10 3 0 10 2 0
APPARENT VISC. cP 95 50.5 37.5 95 41.5 3.5 95 41 2
PLASTIC VISC. cP 44 42 31 44 34 3 44 34 1
YIELD POINT lb/100ft2 102 17 13 102 15 1 102 14 2

pH-Direct 9.5 9 8.95 9.5 8.51 6.01 9.5 8.01 3.95

Comparison of rheology after heat aging for 24, 144 Comparison of rheology after heat aging for 24, 144
and 170 hours at 250 ⁰F and 170 hours at 220 ⁰F

Reference

NASEER. Project Number: LJ-151021-M-274 – HEC TEMPERATURE STABILITY TEST. 3 November 2011.
2014.

NASEER/DENNIS. Project Number: LJ-151109-M-291 - HEC TEMPERATURE STABILITY TEST. 3 November

2011.

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 5.2. Cross-linked HEC Pills
The objective of the test is to evaluate SAFE-LINK performance at 220 ⁰F. The tables below show the
formulation of the sample and the rheology at 220 ⁰F.
PRODUCT ALOXITE DISC PART ALOXITE DISC PART
SAMPLE Mix Time Mix Time
COMPOSITION ppg Order (min) ppg Order (min)
Water 205.88 1 - 205.88 1 -
SAFE-LINK 110 176.00 3 5 176.00 3 5
SAFE-VIS E 8.34 2 15 8.34 2 15
SAFE-LINK formulation
Properties
Tested By: Dennis Teodoro Dennis Teodoro
Date of Test: 1-2 Mar 2015 3-4 Mar 2015
PERIOD AGED Hours - -
TEMPERATURE ºF - 220
DYNAMIC/STATIC D/S D Initial D
Mud Weight ppg 9.36 9.36 9.36 9.36
RHEOLOGY: TEMP. ºF 122 122 122 122
600 RPM >300
300 RPM >300
200 RPM 277
100 RPM 228
6 RPM 91
3 RPM 68
GELS 10" lbs/100ft2
GELS 10' lbs/100ft2
SAFE-LINK rheology at 220 ⁰F

HTHP test was done in order to evaluate fluid loss and pill stability over time. According to the fluid loss
test, SAFE-LINK maintains stable during the first 4 days.

Reference
TEODORO, Dennis. Project Number: LJ-150301-M-075 – ADMA OPCO SAFELINK Evaluation. 3 November
2011. 2014.
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