Drilling fluids containing an alkali metal formate

BACKGROUND OF THE INVENTION

[0002] The present invention relates to the drilling industry and more particularly relates to drilling fluids used in drilling, such as the drilling of a well for the recovery of hydrocarbons or other materials.

[0003] In drilling operations, such as the drilling that occurs in oil field operations, drilling fluids are designed/formulated to serve several functions. These functions include acting as a lubricant to the drill bit to reduce wear and friction during drilling and also to seal the formation surface by forming a filter cake. Currently, in the industry, both oil-based muds (OBMs) and water based muds (WBMs) are typically used. More commonly, synthetic based muds (SBMs) are also used in drilling operations. In the drilling fluid, agents for lubrication are present as well as weighting materials in order to achieve a density that typically produces a pressure greater than the surrounding pressure in the well bore. Furthermore, the drilling fluid will also contain a sealing or fluid loss agent, such as calcium carbonate for pore bridging especially polysaccharides and other polymers, in order to form the filter cake on the formation surface of the well bore. In addition, when the drilling fluids are used during drilling, the drilling fluid will also contain drilling fines, such as shale and sandstone fines. During the drilling operations and afterwards, the filter cake seals the formation surface of the well bore so that the well bore can be completely formed without any leakage from the formation surface into the well bore and/or without any leakage of the drilling fluids into the formation surface. While the filter cake is beneficial for these reasons, once the drilling is completed, and the recovery of hydrocarbons is the next step, the filter cake can act as a severe impediment to the recovery of hydrocarbons. For instance, the filter cake can prevent the recovery of hydrocarbons from the formation surfaces which have been blocked or sealed by the filter cake. Furthermore, when injectors are used to retain reservoir pressures, the injection of sea water, for instance, can be significantly reduced due to the filter cake preventing the sea water from entering the formation and hence restricting the flow of water into the reservoir. Accordingly, the industry prefers to remove the filter cake from the well bore in order to optimize productivity. If the filter cake is not removed, the filter cake can block the pores that are part of the formation surface of the well bore which will interfere with the recovery of hydrocarbons. In many drilling operations, the drilling fluid can contain up to 5% by weight of a pore bridging material such as calcium carbonate. Calcium carbonate (CaCO3) is typically a blend of particle sizes with a particle size distribution designed to optimize the bridging of the pores found in the formation. The pore size distribution of the formation is determined from its permeability, preferably by direct porosity and permeability measurements of core plugs extracted from the reservoir.

[0004] Once drilling operations have been completed, the well is prepared for the completion operations whereby the mud used for drilling is often displaced by a completion fluid. Completion fluids are typically water based clear fluids and are formulated to the same density as the mud used to drill the well in order to retain the hydraulic pressure on the well bore. There are numerous methods of completing a well, amongst which are open hole completions and gravel packed screened systems. The clear fluids are typically halide based brines such as calcium bromide, calcium chloride, and zinc bromide; or organic based brines such as the formate based fluids.

[0005] In drilling an oil or gas well, the use of hydrocarbon-based drilling fluids are greatly preferred because of the inherent advantages of having an external phase fluid in contact with the formation. However, one severe disadvantage to a hydrocarbon-based drilling fluid is that weighting materials, such as barite, calcium carbonate, or hematite must be added to increase the density of the fluid. These weighting-material solids are capable of inducing formation damage to producing formations.

[0006] Thus, there is a need to provide hydrocarbon-based drilling fluids that are preferably solids free or have low solids in the contents in the drilling fluid in order to avoid the above-mentioned disadvantages.

SUMMARY OF THE PRESENT INVENTION

[0007] A feature of the present invention is to provide drilling fluids which are solids free or contain low amounts of solids in the drilling fluids.

[0008] Another feature of the present invention is to provide drilling fluids which are a hydrocarbon-water emulsion which are suitable for use as drilling fluids.

[0009] A further feature of the present invention is to provide drilling fluids which can have a variety of different densities in order to be useful in a variety of drilling situations depending on drilling depth and/or other variables.

[0010] Another feature of the present invention is to provide a more environmentally friendly drilling fluid that can be primarily aqueous based.

[0011] Additional features and advantages of the present invention will be set forth in part in the description that follows, and in part will be apparent from the description, or may be learned by practice of the present invention. The objectives and other advantages of the present invention will be realized and attained by means of the elements and combinations particularly pointed out in the description and appended claims.

[0012] To achieve these and other advantages, and in accordance with the purposes of the present invention, as embodied and broadly described herein, the present invention relates to a drilling fluid which contains at least one alkali metal formate and preferably at least one surfactant. Additional alkali metal formates, wetting agents, hydrocarbons, solid weighting materials, sealing or fluid loss agents, filtration control agents, and/or polymers to further control viscosity and/or other conventional additives such as organoclays and the like can also be optionally present for purposes of the present invention.

[0013] The present invention further relates to a method to drill a well comprising drilling of a well in the presence of the above-mentioned drilling fluid of the present invention.

[0014] The present invention further relates to a method to minimize or eliminate solids in a drilling fluid by substituting at least a portion of the solids weighting material with at least one alkali metal formate and preferably at least one surfactant.

[0015] It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are intended to provide a further explanation of the present invention, as claimed.

DETAILED DESCRIPTION OF THE PRESENT INVENTION

[0016] The present invention relates to drilling fluids for use in drilling operations. For instance, the drilling fluid can be used in the drilling of a well for hydrocarbon recovery such as oil and/or gas. The drilling fluids of the present invention can also be used in other drilling operations where drilling fluids are used.

[0017] The drilling fluid of the present invention contains at least one alkali metal formate or monovalent carboxylic acid salt and preferably at least one surfactant or emulsifier. The drilling fluid of the present invention can contain an emulsion of an aqueous-based solution with a hydrocarbon-based fluid for purposes of forming the drilling fluid wherein the drilling fluid contains at least one alkali metal formate and preferably at least one surfactant along with at least one hydrocarbon-based fluid.

[0018] Preferably, the drilling fluid contains cesium formate as the alkali metal formate. More preferably, the drilling fluid contains two or more alkali metal formates, wherein preferably one of the alkali metal formates is cesium formate. A preferred combination of formates includes, but is not limited to, cesium formate with potassium formate. Other combinations of alkali metal formates can be used, such as sodium formate and potassium formate or sodium formate and cesium formate. Essentially, any combination of one or more monovalent carboxylic salts can be used for purposes of the drilling fluids of the present invention.

[0019] The alkali metal formates are commercially available. For instance, the cesium formate can be obtained from Cabot Corporation. The cesium formate can be made, for instance, by following the description as set forth in International Published Patent Application No. WO 96/31435, incorporated in its entirety by reference herein. The cesium formate that is present in the drilling fluid, preferably as a soluble salt, as stated above, can be present in any concentration and the cesium formate solution is a liquid at room temperature. Therefore, the concentration of the cesium formate in the drilling fluid can be from about 1% to about 100% by weight, and more preferably is present in an amount of from about 40% to about 95% by weight, and even more preferably is present in the drilling fluid at a range of from about 55% to about 85% by weight or is present in the drilling fluid at a range of from about 70% to about 85% by weight based on the weight of the drilling fluid. Besides the optional ingredients and preferably the surfactant and/or hydrocarbon fluid, the remainder of the drilling fluid can be water or other aqueous solutions. Conventional ingredients used in drilling fluids can also be used with the drilling fluid of the present invention.

[0020] Other alkali metal formates that can be used in the present invention are potassium formate and sodium formate which are commercially available. These alkali metal formates can also be prepared in a similar fashion as the cesium formate solution described above, and are also frequently obtained as by-products from ester hydrolysis.

[0021] Preferably, with respect to the drilling fluid of the present invention, at least 35% by volume of the fluid in the drilling fluid is an aqueous-based solution containing at least one alkali metal formate. More preferably, at least 50% by volume of the fluids present in the drilling fluid is an aqueous-based solution containing at least one alkali metal formate and even more preferably at least 75% by volume of the fluids present in the drilling fluid of the present invention is an aqueous-based solution containing at least one alkali metal formate. Most preferably, at least 90% by volume of the fluids present in the drilling fluid of the present invention is an aqueous-based solution containing at least one alkali metal formate. In another embodiment, at least 95% or more by volume of the fluids of the present invention contain an aqueous-based solution containing at least one alkali metal formate. In one embodiment, all of the fluids present are an aqueous-based solution containing at least one alkali metal formate wherein essentially no hydrocarbon, or oil is present in the drilling fluid. Since the alkali formate is preferably dissolved in the aqueous solution, the drilling fluid can be solids free since the alkali formate preferably acts as a lubricant and a weighting material.

[0022] When a hydrocarbon fluid or synthetic mud fluid is present in the drilling fluids of the present invention, conventional hydrocarbon fluids or synthetic mud fluids can be used in the drilling fluids of the present invention. Examples include, but are not limited to, diesel oil such as diesel oil number 2, crude oil, synthetic oils (such as paraffin oils, olefin oils, vegetable oils, and the like), as well as other conventional hydrocarbon fluids. Combinations of various hydrocarbon fluids or synthetic mud fluids can be used for purposes of the present invention. If a hydrocarbon or synthetic mud fluid is present in the drilling fluid of the present invention, various ratios of the hydrocarbon fluid to the aqueous-based solution described above can be used, such as ratios of 65% by volume hydrocarbon fluid: 35% aqueous based solution to 1% by volume hydrocarbon fluid: 99% by volume aqueous based solution.

[0023] When a hydrocarbon fluid is present with the aqueous-based solution containing at least one alkali metal formate, at least one emulsifier or surfactant is preferably present in order to produce an emulsion of the ingredients. Essentially any emulsifier(s) or surfactant(s) capable of forming an emulsion between the hydrocarbon fluid and the aqueous based solution can be used for purposes of the present invention. Examples include, but are not limited to, a dimer trimer acid such as Witco DTA 350, imidazoline, tall oil (stearic acid), Integrity Synvert IV, Integrity Synvert TWA, and the like. Any amount of surfactant or emulsifier can be used to form the emulsion such as from about 1 to about 30 pounds per barrel, wherein a barrel is about 42 gallons.

[0024] Other optional ingredients that can be present in the drilling fluids of the present invention include a filtration control agent or pore bridging materials such as Gilsonite and the like. These filtration control agents can be used in conventional amounts.

[0025] Other ingredients that can be present in the drilling fluids of the present invention include solid weighting materials such as barite, hematite, and/or calcium carbonate. These solid weighting materials can be used if desired. The amount of solid weighting material, which is optional, can be from about 0.5 pound per barrel to about 500 pounds per barrel.

[0026] Another optional ingredient in the drilling fluids of the present invention is a wetting agent which can be helpful in emulsifying the alkali metal formate fluids with the hydrocarbon-based external fluids. An example of a suitable wetting agent is Integrity Synvert TWA. Conventional amounts can be used in combination with the emulsifiers described above in order to achieve desired emulsions of the formate fluids with the hydrocarbon-base external fluids.

[0027] Other ingredients that can optionally be present include, but are not limited to, other drilling fluid products such as polymer(s) to add to viscosity, hydrophilic clays, organophilic clays, fluid loss control additives, amine-treated clays, clays treated such that they provide viscosity in non-aqueous fluids, and the like. These other optional ingredients can be used in conventional amounts known to those skilled in the art.

[0028] The alkali metal formate that is present as part of the aqueous-based solution can be not fully saturated in the aqueous-based solution so as to permit any remaining water-soluble components to preferably solubilize in the solution along with the alkali metal formate. Thus, the alkali metal formate that is present in the aqueous-based solution can be present in an amount of less than 80% by weight, based on the aqueous-based solution basis, and more preferably is from about 60% to about 80% by weight.

[0029] The important advantage of the present invention is the ability for the density of the drilling fluid to be adjusted to any desired density. This can especially be done with the introduction of a combination of alkali metal formates, such as potassium formate with cesium formate. As an example, an aqueous-based portion of the drilling fluid can contain cesium formate which can range from about 1.8 to about 2.4 s.g. This density range can be adjusted with the introduction of potassium formate. For instance, when 0 to 100% by weight of potassium formate is included in the aqueous-based portion of the drilling fluid, the density of the overall aqueous-based portion of the drilling fluid can range from about 1.2 to about 2.4. Thus, the density of the drilling fluid can essentially be “dialed-in” to meet the density needed for the drilling fluid to be used in the drilling of the well bore at the appropriate depths. For lower density ranges, sodium formate can be added to the potassium formate, hence, “dialing-in” lower density drilling fluids.

[0030] Thus, the drilling fluids of the present invention make it possible to achieve a variety of different densities and to minimize or completely eliminate the solid weighting material that is present in conventional drilling fluids.

[0031] The drilling fluids of the present invention can be introduced into the well bore by any conventional technique such as, but not limited to, being pumped into the drill pipe. Further, the drilling fluids can be recovered using conventional techniques.

[0032] The drilling fluids of the present invention can be prepared by mixing all of the components together. When an emulsion is prepared, typically, the components will be mixed together such as by shearing in order to ensure a dispersion that is preferably uniform with respect to the components.

[0033] For example, a typical paraffinic hydrocarbon oil such as ESCAID 110, having a density of 0.803 s.g. (6.7 ppg) and a cesium formate solution having a density of 2.2 s.g. (18.36 ppg) when combined in a ratio of 1:1 and by addition of an emulsifier or a series of emulsifiers admixed by shearing, the fluids together can produce an emulsion or microemulsion that has a cesium formate invert phase or (internal phase) and an oil external phase. The density of the combined mixture of this example is 1.51 s.g. (12.6 ppg).

[0034] For purposes of the present invention, when a hydrocarbon-based external fluid is used with at least one formate fluid as described above, the formate fluids can be partially or totally emulsified into the hydrocarbon-based fluid. Or, in the alternative, when a majority of the drilling fluid is a formate fluid, the hydrocarbon-based fluid, if present, can be partially or totally emulsified into the formate fluid.

[0035] Optionally, the drilling fluids of the present invention can also contain at least one acid. Preferably, the acid is an acid containing at least one carboxylic group and more preferably is formic acid or an acid derivative thereof. Other examples of acids that can be used include, but are not limited to, acetic acid, ascorbic acid, citric acid, tartaric acid, phthalic acid, glycolic acid, and combinations thereof. The acid can be present in various amounts such as from about 1% or less to 25 weight % or more based on the weight of the drilling fluid. The presence of the acid has the capability of adjusting the pH of the drilling fluid as well as providing other benefits to the drilling fluid. When an acid is present, for instance, the alkali metal formate fluid, such as cesium formate, can be present in any molar amount, but is preferably present in an amount of about 3 M. Similarly, the acid, when present, can be present in any molar amount, and is preferably present in an amount of from about 2.2 M to about 15 M. The pH of the drilling fluid can be any pH.

[0036] The present invention will be further clarified by the following examples, which are intended to be purely exemplary of the present invention.

EXAMPLES

[0037] Various drilling fluid formulations were prepared and tested to determine the ability of the drilling fluids to serve as suitable fluids for drilling.

[0038] In the Examples, cesium formate was used and as can be seen in the results summarized in the various tables, a drilling fluid was made that had low or zero solids content and had the capability to “dial-in” various densities using a combination of components described herein.

[0039] In the examples, a barrel is generally 42 gallons of liquid. IA-35 is a synthetic oil from Integrity Industries. Integrity Synvis is a viscosifier. Witco DTA 350 is a wetting agent. Baroid Baracarb 50 is calcium carbonate. Initial ES (volts) is electrical stability at the temperature shown below the values. Initial properties refers to apparent viscosity using a Fann 35 viscometer. SA refers to static-aged ES testing and 250 refers to testing at 250° F. for 16 hours. “Silv” refers to a Silverson mixer.

[0040] The tests in the Tables were conducted in accordance with Recommended Practice Standard Procedure for Field Testing oil-based drilling fluids, API, 13B-2 (2nd Ed., Dec. 1, 1991), and Recommended Practice Standard Procedure API Recommended Procedure 13-I (5th Ed., Jun. 1, 1995), incorporated in their entirety by reference herein.

1Cesium formate, IA - 35 (50/50 mixture, 2.3 s.g. CsF) 2.3 sg csfMixing Procedure:1.Measure out IA - 351A.Add Synvis, mix 5 minutes2.Add CsF, mix 10 min.3.Add Emulsifier Synvert, mix 10 minutes3A.Add calcium carbonate, mix 10 minutes4.Run initial ES, viscosities at 120° F.5.Put 10 ml sample in a vial, SA for 24 hrs at 75° F.,measure volumes6.Hot-roll for 16 hours at 150° F.7.Remix, run rheology, ES, API, HTHP at 150° F.8.Put vials in oven and static-age at 150° F. for 24 hrs,measure volumes9.If 150° F. HTHP is good, run at 250° F.41.6/58.4 oil/csf ratioSample #337338339IA - 35,98.2698.2693.26gramsCesium445 (2.366)445 (2.366)445 (2.366)Formate,gramsIntegrity252520Emulsifier,lb/bblIntegrity0.510.5Synvis,lb/bblWitco———DTA 350,lb/bblBaroid505050Baracarb50, lb/bblInitial ES,103129167166114151voltsHot-rolled11410214814013913816 hrs, ESInitial Properties120° F.150° F.120° F.150° F.120° F.150° F.600 rpm162116186118164115300 rpm9365114679666200 rpm674783497048100 rpm402749294128 6 rpm879676 3 rpm657555Plastic695172516849Viscosity, cPYield Pt, lb/241442162817100 ft{circumflex over ( )}2Gels, 10 sec/6/76/66/75/65/65/510 min.Settling innonononononothermocupHR 16 hrsat 150° F.600 rpm161113187123162114300 rpm9364116709766200 rpm684686527248100 rpm3927523047328 6 rpm8610676 3 rpm658554Plastic684971536548Viscosity, cPYield Pt,251545173218lb/100 ft{circumflex over ( )}2Gels, 106/65/67/95/66/65/5sec/10 min.API filt,1.00.20.4ml totalAPI filt,———ml oilAPI filt,1.00.20.4ml emulsionAPI filt,———ml brineHTHP at0.2150° F., mlHTHP at11.4250° F., ml250° F. oil0.0250° F.6.8emulsion250° F. brine4.6CommentsNOTE:1. Sample 337 and 338 looked grainy with 15 lb/bbl Synvert V.Concentration was increased to 25 lb/bbl.After hot-rolling at 150° F., #337and #338 still appear grainy.2. Mud weight of 339 is 14.7 lb/gal (CsF in337-339 is 2.366 s.g)41.6/58.4 oil/csf ratioSample #340347348IA - 35, grams93.2688.2688.26Cesium455 (2.366)445 (2.3)445 (2.3)Formate,gramsIntegrity202525Emulsifier,lb/bblIntegrity1——Synvis,lb/bblWitco—0.51DTA 350,lb/bblBaroid505050Baracarb 50,lb/bblInitial ES,117128212192205243voltsHot-rolled12211814814525224716 hrs, ESInitial Properties120° F.150° F.120° F.150° F.120° F.150° F.600 rpm183126177132182132300 rpm109731067811180200 rpm805377578361100 rpm4731463475238 6 rpm8687108 3 rpm656576Plastic745371547152Viscosity, cPYield Pt, lb/352035244028100 ft{circumflex over ( )}2Gels, 10 sec/6/75/56/66/68/86/710 min.Settling innonononononothermocupHR 16 hrs at150° F.600 rpm184129179140184144300 rpm111751098411388200 rpm825580628566100 rpm493248375241 6 rpm8687109 3 rpm656587Plastic735670567156Viscosity, cPYield Pt,382839324232lb/100 ft{circumflex over ( )}2Gels, 106/75/66/65/58/87/9sec/10 min.API filt,0.33.56.2ml totalAPI filt,———ml oilAPI filt,0.33.56.2ml emulsionAPI filt,———ml brineHTHP at0.219.4(0.8 brine)150° F., mlHTHP at4.4250° F. ml250° F. oil0.0250° F.3.2emulsion250° F.1.2brineCommentsNOTE1. Mud weight of 339 is 14.7 lb/gal (CsF in 340 is2.366 s.g)2. Mud weight of 347 is 14.6 lb/gal (CsF in 347-348is 2.30 s.g)41.6/58.4 oil/csf ratioSample #341342343344345346IA - 35,88.2688.2698.2698.2693.2693.26gramsCesium445445445445445445Formate,gramsIntegrity252515152020Emulsifier,lb/bblIntegrity0.51————Synvis,lb/bblWitco——0.510.51DTA 350,lb/bblBaroid505050505050Baracarb 50,lb/bbl

[0041]

2

Cesium Formate, Escaid 110 (50/50 mixture)

Mixing Procedure:

1. Measure out Escaid 110, add Organoclay, mix 10 minutes

2. Add emulsifier(s), mix 5 minutes, add Gilsonite, mix 10 minutes

3. Add CsF, mix 10 min on HB, add CaCO3, mix 10 min on HB

4. Run initial ES, viscosities at 120 F.

5. Put 10 ml sample in vial, SA for 24 hrs at 75 F., measure volume

6. Hot Roll for 16 hrs. at 150 F.

7. Remix, run rheology es, HPHT @ 250 F.

8. Put vial in oven SA 24 hrs @ 150 F.

Sample #
E-1
E-2
E-3
E-4

Integrity Synvert IV, lb/bbl
10
15
10
10

Dimer-Trimer acid, lb/bbl
0
0
0
1

Integrity Synvert TWA, lb/bbl
0
0
0
6

Organoclay, lb/bbl
0
0
4
4

Gilsonite, lb/bbl
0
0
5
5

CaCo3, lb/bbl
0
0
50
50

ES @ 120 F.
225
289
170
175

Hot-rolled 16 hrs, ES @ 120 F.
395
440
365
350

Initial Properties

600 rpm @ 120 F.
28
30
85
92

300 rpm @ 120 F.
15
16
40
50

200 rpm @ 120 F.
10
11
31
41

100 rpm @ 120 F.
5
6
15
25

6 rpm @ 120 F.
0
1
3
6

3 rpm @ 120 F.
0
0
1
5

Plastic Viscosity, cP
13
14
45
42

Yield Point, lb/100 ftsq
2
2
5
8

Gels, 10 sec/10 min
0/0
0/1
1/4
5/8

HR 16 hrs @ 150 F.

600 rpm @ 120 F.
31
33
96
110

300 rpm @ 120 F.
16
18
49
62

200 rpm @ 120 F.
10
12
35
53

100 rpm @ 120 F.
5
6
20
40

6 rpm @ 120 F.
0
2
4
10

3 rpm @ 120 F.
0
1
2
6

Plastic Viscosity, cP
15
15
47
48

Yield Point, lb/100 ftsq
1
3
4
14

Gels, 10 sec/10 min.
0/0
1/1
3/4
7/9

HPHT @ 250 F., ml
30
26
8
6

Water in filtrate, ml
4
3
0
0

24 hrs @ 75 F.

Free Oil %
10
8
5
3

Emulsion %
90
92
95
97

Free Brine %
0
0
0
0

[0042]

3

Cesium Formate, IA-35 (75/25 mixture)

Mixing Procedure:

1. Measure out IA-35, add Organoclay, mix 10 minutes

2. Add emulsifier(s), mix 5 minutes, add Gilsonite, mix 10 minutes

3. Add CsF, mix 10 min on HB, add CaCO3, mix 10 min on HB

4. Run initial ES, viscosities at 120 F.

5. Put 10 ml sample in vial, SA for 24 hrs at 75 F. measure volume

6. Hot Roll for 16 hrs. at 250 F.

7. Remix, run rheology es, HPHT @ 150 F.

8. Put vials in oven SA 24 hrs @ 150 F.

Sample #

1
2
3
4
5

Integrity Synvert IV, lb/bbl
10
15
10
10
15

Dimer-Trimer acid, lb/bbl
0
0
0
1
1

Integrity Synvert TWA, lb/bbl
0
0
0
6
6

Organoclay, lb/bbl
0
0
4
4
4

Gilsonite, lb/bbl
0
0
5
5
5

CaCo3, lb/bbl
0
0
50
50
50

ES @ 120 F.
226
250
270
175
225

Hot-rolled 16 hrs, ES @ 120 F.
185
200

Initial Properties

600 rpm @ 120 F.
251
265
t
t
t

300 rpm @ 120 F.
169
172
o
o
o

200 rpm @ 120 F.
135
133
o
o
o

100 rpm @ 120 F.
92
184

6 rpm @ 120 F.
26
13
t
t
t

3 rpm @ 120 F.
20
8
h
h
h

i
i
i

Plastic Viscosity, cP
82
93
c
c
c

Yield Point, lb/100 ftsq
87
79
k
k
k

Gels, 10 sec/10 min
24/28
8/12

HR 16 hrs @ 150 F.

600 rpm @ 120 F.
276
259

300 rpm @ 120 F.
175
166

200 rpm @ 120 F.
140
101

100 rpm @ 120 F.
99
22

6 rpm @ 120 F.
29
14

3 rpm @ 120 F.
22
8

Plastic Viscosity, cP
101
93

Yield Point, lb/100 ftsq
74
73

Gels, 10 sec/10 min.
22/23
8/12

HPHT @ 250 F., ml
23
16

Water in filtrate, ml
8
4

24 hrs @ 75 F.

Free Oil %
1
0
0

Emulsion %
99
100
100

Free Brine %
0
0
0

24 hrs @ 150 F.

Free oil %
2
2
0

Emulsion %
98
98
100

Free Brine %
0
0
0

Observational Notes:

Emulsion is clear at temperatures above 130 F.

Amount of shear imparted to system is directly related to emulsion stability

Heating the emulsion to 150 F. acts to stabilize emulsion (similar to shearing)

Oil/Water ratios as low as 25/75 are achievable with this system

[0043]

4

Cesium Formate, IA-35 (50/50 mixture)

Mixing Procedure:

1. Measure out IA-35, add Organoclay, mix 10 minutes

2. Add emulsifier(s), mix 5 minutes, add Gilsonite, mix 10 minutes

3. Add CsF, mix 10 min on HB, add CaCO3, mix 10 min on HB

4. Run initial ES, viscosities at 120 F.

5. Put 10 ml sample in vial, SA for 24 hrs at 75 F., measure volume

6. Hot Roll for 16 hrs. at 150 F.

7. Remix, run rheology es, HPHT @ 250 F.

8. Put vials in oven SA 24 hrs @ 150 F.

Sample #

1
2
3
4
5

Integrity Synvert IV, lb/bbl
10
15
10
10
15

Dimer-Trimer acid, lb/bbl
0
0
0
1
1

Integrity Synvert TWA, lb/bbl
0
0
0
6
6

Organoclay, lb/bbl
0
0
4
4
4

Gilsonite, lb/bbl
0
0
5
5
5

CaCo3, lb/bbl
0
0
50
50
50

ES @ 120 F.
226
255
241
150
231

Hot-rolled 16 hrs, ES @ 120 F.
425
475
427
320
444

Initial Properties

600 rpm @ 120 F.
39
42
162
181
155

300 rpm @ 120 F.
20
22
93
131
92

200 rpm @ 120 F.
14
15
66
110
67

100 rpm @ 120 F.
7
8
36
81
39

6 rpm @ 120 F.
0
1
3
33
6

3 rpm @ 120 F.
0
0
2
28
4

Plastic Viscosity, cP
19
20
69
50
63

Yield Point, lb/100 ftsq
1
2
24
81
29

Gels, 10 sec/10 min
0/0
0/2
3/7
29/32
7/7

HR 16 hrs @ 150 F.

600 rpm @ 120 F.
51
55
169
195
188

300 rpm @ 120 F.
27
29
101
145
114

200 rpm @ 120 F.
14
14
75
113
86

100 rpm @ 120 F.
9
10
43
87
51

6 rpm @ 120 F.
1
1
4
37
8

3 rpm @ 120 F.
0
1
2
30
5

Plastic Viscosity, cP
24
26
68
50
74

Yield Point, lb/100 ftsq
3
3
33
95
40

Gels, 10 sec/10 min.
0/0
0/1
3/3
33/35
5/6

HPHT @ 250 F., ml
28
22
15
14
6

Water in filtrate, ml
4
3
2
2
0

24 hrs @ 75 F.

Free Oil %
5
10
4
3
2

Emulsion %
95
90
96
97
98

Free Brine %
0
0
0
0
0

24 hrs @ 150 F.

Free oil %
18
15
10
0

Emulsion %
92
85
90
94

Free Brine %
0
0
0
0

[0044]

5

Cesium formate, Escaid 110 (50/50 mixture)

175 ml Escaid 110 (0.803 sg) - (140.5 grams)

175 ml Cesium Formate (2.2 sg) - (385 grams)

Mixing Procedure:

1.
Measure out Escaid 110, add Geltone II, mix 10 minutes

2.
Add emulsifiers (Below in bold), mix 5 minutes, add Barablock, mix 10 minutes

3.
Add CsF, mix 10 min. on HB, add Lo-Wate, mix 10 min. on HB

4.
Run initial ES, viscosities at 120° F.

5.
Put 10 ml sample in a vial, SA for 24 hrs at 75° F., measure volumes

6.
Hot-roll for 16 hours at 150° F.

7.
Remix, run rheology, ES, API, HTHP at 150° F.

8.
Put vials in oven and static-age at 150° F. for 24 hrs, measure volumes

9.
If 150° F. HTHP is good, run at 250° F.

Sample #

225
226
227
228
229
230

Integrity
7
7
7
7
7
7

Synvert II

(Lot# 991512),

lb/bbl

Witco DTA 350
1
1
1
1
1
1

(dimer-trimer),

lb/bbl

Integrity
2
4
6
2
4
6

Synvert TWA

(Jan. 24, 2000,

D116), lb/bbl

Baroid Geltone
—
—
—
4
4
4

II, lb/bbl

Baroid
—
—
—
—
—
—

Barablock 400,

lb/bbl

M-I Lo-Wate,
50
50
50
50
50
50

lb/bbl

Initial ES,
107
194
247
127
123
128

volts

Hot-rolled 16
426
450
290
150
185
170

hrs, ES

Initial Properties

600 rpm at
80
67
80
99
74
87

75° F.

300 rpm
58
48
60
75
52
60

200 rpm
49
40
51
64
43
48

100 rpm
37
31
39
49
31
35

6 rpm
13
10
13
18
12
13

3 rpm
10
5
4
15
10
11

Plastic
22
19
20
24
22
27

Viscosity, cP

Yield Pt,
36
29
40
51
30
33

lb/100 ft{circumflex over ( )}2

Gels, 10 sec/10 min.
11/7
5/7
7/3
15/15
10/10
10/11

HR 16 hrs at 150° F.

600 rpm at
71
89
95
94
75
70

120° F.

300 rpm
53
69
74
68
52
48

200 rpm
44
59
63
56
43
39

100 rpm
34
45
49
42
31
28

6 rpm
10
12
12
17
12
10

3 rpm
4
5
4
13
10
8

Plastic
18
20
21
26
23
22

Viscosity, cP

Yield Pt,
35
49
53
42
29
26

lb/100 ft{circumflex over ( )}2

Gels,
7/4
9/4
10/4
12/13
10/11
9/9

10 sec/10 min.

API filtrate,
0.8
1.1
1.1
1.6
0.9
0.6

ml

API Filtrate,
0
0
0
0
0
0

oil

API Filtrate,
0
0
0
0
0
0

brine

HTHP at
8.8
3.0
5.0
3.5
1.6
0.8

150° F., ml

Water in
6.0
2.5
2.5
1.5
0.4
0.0

filtrate?

HTHP at
24.0
18.0
12.0
8.2
4.2
2.5

250° F., ml

Water in
12.0
9.0
3.1
2.6
1.7
0.6

filtrate?

24 hrs at 75° F.

Total fluid
34
35
34
35
36
33

heighth

free oil
6
3
2
1
1
2

heighth

emusion
28
32
32
34
35
31

heighth

free brine
0
0
0
0
0
0

heighth

free oil, %
18%
9%
6%
3%
3%
6%

emusion, %
82%
91%
94%
97%
97%
94%

free brine, %
0%
0%
0%
0%
0%
0%

24 hrs at 150° F.

Total fluid
34
36
35
35
37
32

heighth

free oil
8
8
6
3
3
4

heighth

emusion
26
28
29
32
34
28

heighth

free brine
0
0
0
0
0
0

heighth

free oil, %
24%
22%
17%
9%
8%
13%

emusion, %
76%
78%
83%
91%
92%
88%

free brine, %
0%
0%
0%
0%
0%
0%

Difference (72 hrs/24 hrs at 150° F.)

free oil, %
6%
14%
11%
6%
5%
6%

emusion, %
−6%
−14%
−11%
−6%
−5%
−6%

free brine, %
0%
0%
0%
0%
0%
0%

Sample #

231
232
233
234
235
236

Integrity
7
7
7
7
7
7

Synvert II

(Lot# 991512),

lb/bbl

Witco DTA 350
1
1
1
1
1
1

(dimer-trimer),

lb/bbl

Integrity
2
4
6
2
4
6

Synvert TWA

(Jan. 24, 2000,

D116), lb/bbl

Baroid Geltone
—
—
—
4
4
4

II, lb/bbl

Baroid
5
5
5
5
5
5

Barablock

400, lb/bbl

M-I Lo-Wate,
50
50
50
50
50
50

lb/bbl

Initial ES,
139
263
249
105
133
161

volts

Hot-rolled
402
314
307
144
196
245

16 hrs, ES

Initial Properties

600 rpm at
81
90
85
86
81
84

75° F.

300 rpm
63
69
65
62
57
60

200 rpm
52
59
55
50
47
49

100 rpm
40
46
43
37
34
37

6 rpm
17
14
14
12
14
14

3 rpm
12
5
5
10
12
12

Plastic
18
21
20
24
24
24

Viscosity, cP

Yield Pt,
45
48
45
38
33
36

lb/100 ft{circumflex over ( )}2

Gels, 10
17/15
10/5
11/6
10/11
12/13
12/12

sec/10 min.

HR 16 hrs at 150° F.

600 rpm at
111
118
122
63
90
110

120° F.

300 rpm
84
92
96
43
62
76

200 rpm
71
78
83
35
50
62

100 rpm
53
61
65
25
37
45

6 rpm
17
18
21
9
13
16

3 rpm
7
7
7
7
11
14

Plastic
27
26
26
20
28
34

Viscosity, cP

Yield Pt,
57
66
70
23
34
42

lb/100 ft{circumflex over ( )}2

Gels, 10
13/5
12/6
13/5
7/8
10/11
13/14

sec/10 min.

API filtrate,
1.2
1.2
0.3
0.2
0.2
0.0

ml

API Filtrate,
0
0
0
0
0
0

oil

API Filtrate,
0
0
0
0
0
0

brine

HTHP at
2.6
2.0
1.4
2.0
trace
trace

150° F., ml

Water in
0.0
0.0
0.0
0.0
0.0
0.0

filtrate?

HTHP at
9.0
8.0
6.0
7.0
5.0
4.0

250° F., ml

Water in
0.0
0.0
0.0
0.0
0.0
0.0

filtrate?

24 hrs at 75° F.

Total fluid
35
35
35
34
34
34

heighth

free oil
3
2
3
2
1
1

heighth

emusion
32
33
32
32
33
33

heighth

free brine
0
0
0
0
0
0

heighth

free oil, %
9%
6%
9%
6%
3%
3%

emusion, %
91%
94%
91%
94%
97%
97%

free brine, %
0%
0%
0%
0%
0%
0%

24 hrs at 150° F.

Total fluid
35
36
35
34
35
35

heighth

free oil
7
6
6
6
4
3

heighth

emusion
28
30
29
28
31
32

heighth

free brine
0
0
0
0
0
0

heighth

free oil, %
20%
17%
17%
18%
11%
9%

emusion, %
80%
83%
83%
82%
89%
91%

free brine, %
0%
0%
0%
0%
0%
0%

Difference (72 hrs/24 hrs at 150° F.)

free oil, %
11%
11%
9%
12%
8%
6%

emusion, %
−11%
−11%
−9%
−12%
−8%
−6%

free brine, %
6%
0%
0%
0%
0%
0%

[0045]

6

Mixing Order:

1. Measure out IA 35 base oil

2. Add Synvert IV

3. Add cesium formate

4. Mix on HB, Silverson to 135° F.

Sample #

1
2
3
4
5

IA-35, %
90
75
50
25
10

Synvert IV,
20
20
20
20
20

lb/bbl

2.2 s.g. Cs
10
25
50
75
90

Formate, %

Initial Rheologies

Mud weight,
7.81
9.4
11.94
14.47
17.18

lb/gal

600 rpm at
7
13
42
>300
too

120° F.

300 rpm
4
7
21
274
thick

200 rpm
3
5
14
218
to

100 rpm
2
3
7
149
measure

6 rpm
0.2
0.5
1
38

3 rpm
0.2
0.5
0.5
28

PV
3
6
21
—
—

YP
1
1
0
—
—

Gels
.5/.5
1/1
1/1
28/32
—

ES
373
310
362
328
133

Vials 16 hrs at 75° F.

Total Heighth
32
32
32
31

Oil
18
1
0
0

Emulsion
14
31
32
31

Formate

Samples H.R. for 16 hours at 150° F.

600 rpm at
6
13
45
>300
too

120° F.

300 rpm
3
7
23
273
thick

200 rpm
2
4
16
222
to

100 rpm
1
2
8
158
measure

6 rpm
0
0
2
49

3 rpm
0
0
2
40

PV
3
6
22
—
—

YP
0
1
1
—
—

Gels
1/1
0/0
2/2
38/42
—

ES
1069
211
232
271
115

Vials 7 hrs at 150° F.

Total Heighth
32
32
32
32

Oil
22
3
1
0

Emulsion
10
29
31
32

Formate

Vials 64 hrs at 200° F.

Total Heighth
105
103
100
100
105

Oil
89
66
40
0
0

Emulsion
8
12
60
100
105

Formate
8
25
0
0
0

Vials 64 hrs at 250° F.

Total Heighth
103
100
100
100
110

Oil
95
70
30
32
0

Emulsion
8
7
65
60
110

Formate
0
23
5
8
0

Vials 64 hrs at 300° F.

Total Heighth
102
105
102
102
104

Oil
92
70
42
32*
19*

Emulsion
10
10
10

Formate
0
25
50
70
85

*combination oil and emulsion

[0046]

7

Integrity Synvert IV Sample 1 gallon can

Test Procedure

1.
Mix sample

2.
Place aliquots of sample in large test tubes

3.
Static-age samples for 24 hours at 200, 250, and 300 F.,

300 psi N2

4.
Static-age samples for 72 hours at 200, 250, and 300 F.,

300 psi N2

5.
Measure total heighth, oil, emulsion, and brine

200° F.
250° F.
300° F.

24 hour tests

Total heighth, mm
100
99
99

Free Oil, mm
9
16
30

Emulsion, mm
84
73
46

Free Brine, mm
7
10
23

% Oil
9.0%
16.2%
30.3%

% Emulsion
84.0%
73.7%
46.5%

% Brine
7.0%
10.1%
23.2%

72 hour tests

Total heighth, mm
96
101
97

Free Oil, mm
5
10
30

Emulsion, mm
81
71
22

Free Brine, mm
10
20
45

% Oil
5.2%
9.9%
30.9%

% Emulsion
84.4%
70.3%
22.7%

% Brine
10.4%
19.8%
46.4%

Note:

the 24 hr 300° F., and the 72 hour 200 and 250° F. fluids appeared

to have two phases in the emulsion portion. One phase is more

distinctly oil and the second phase is more distinctly emulsion.

Sample of 50/50 mix from Integrity (one gallon can)

600 rpm at 75° F.
90

300 rpm
49

200 rpm
34

100 rpm
18

6 rpm
2

3 rpm
1

PV
41

YP
8

Gels
2/2

ES
457

Integrity Turpene-Formate Sample

3 days
7 days

Vials 3 and 7 days at 200° F.

Total Heighth
50
52

Oil
20
15

Emulsion
0
0

Formate
30
37

Vials 3 and 7 days at 250° F.

Total Heighth
54
51

Oil
17
15

Emulsion
0
0

Formate
37
36

Vials 3 and 7 days at 300° F.

Total Heighth
51
50

Oil
15
15

Emulsion
0
0

Formate
36
35

Sample #

SA 250
SA 250

SA 250
SA 250

Initial
Silv.

Initial
Silv.

349
349.5
349.75
350
350.5
350.75
353

IA - 35, grams
94.26
94.26
94.26
94.26
94.26
94.26
89.26

Cesium Formate,
445
445
445
445
445
445
445

grams

Integrity
20
20
20
20
20
20
25

Emulsifier,

lb/bbl

Integrity
0.5
0.5
0.5
0.5
0.5
0.5
0.5

Synvis,

lb/bbl

Witco DTA
—
—
—
0.5
0.5
0.5
—

350, lb/bbl

Baroid
—
—
—
—
—
—
—

Barablock,

lb/bbl

M-I Lo Wate,
50
50
50
50
50
50
50

lb/bbl

Initial
227

256

301

ES, volts

Hot-rolled
109

209

339

16 hrs, ES

Static-aged

113

154

ES, volts

Initial Properties
120° F.
120° F.
120° F.
120° F.
120° F.
120° F.
120° F.

600 rpm
188
147
—
179
148
—
203

300 rpm
113
90
—
108
88
—
122

200 rpm
83
68
—
80
65
—
90

100 rpm
49
41
—
48
39
—
53

6 rpm
8
6
—
6
6
—
7

3 rpm
5
4
—
4
4
—
5

Plastic
75
57
—
71
60
—
81

Viscosity, cP

Yield Pt,
38
33
—
37
28
—
41

lb/100 ft{circumflex over ( )}2

Gels, 10
5/6
5/6
—
4/5
4/6
—
6/6

sec/10 min.

Settling in
no
no
—
no
no
—
no

thermocup

Initial
253

266

295

ES, volts

Hot-rolled
205
145
331
222
175
330
242

16 hrs, ES

HR 16 hrs at 150° F.
150° F.
150° F.
150° F.
150° F.
150° F.
150° F.
150° F.

600 rpm
137
98
121
137
104
121
158

300 rpm
81
58
70
82
60
70
95

200 rpm
60
42
51
61
44
51
70

100 rpm
36
25
30
37
26
30
42

6 rpm
7
4
5
7
5
5
8

3 rpm
5
3
3
5
3
3
6

Plastic
56
40
51
55
44
51
63

Viscosity, cP

Yield Pt,
25
18
19
27
16
19
32

lb/100 ft{circumflex over ( )}2

Gels, 10
6/6
3/3
3/4
5/5
3/4
3/4
6/6

sec/10 min.

API filt,
0.7
—
—
0.4
—
—
0.3

ml total

API filt,
0
—
—
0
—
—
0

ml oil

API filt,
0.7
—
—
0.4
—
—
0.3

ml emulsion

API filt,
0.0
—
—
0.0
—
—
0.0

ml brine

HTHP at
3.2
—
1.6
8.8
—
2.0
4.8

250° F., ml

250° F.
2.4
—
—
6
—
—
3.6

oil

250° F.
0.8
—
1.6
2.8
—
2.0
1.2

emulsion

250° F.
—
—
—
—
—
—
—

brine

Free Oil, %

22%

25%

Sample #

SA 250
SA 250

SA 250
SA 250

Initial
Silv.

Initial
Silv.

353.5
353.75
354
354.5
354.75

IA - 35, grams
89.26
89.26
89.26
89.26
89.26

Cesium Formate,
445
445
445
445
445

grams

Integrity
25
25
25
25
25

Emulsifier,

lb/bbl

Integrity
0.5
0.5
0.5
0.5
0.5

Synvis,

lb/bbl

Witco DTA 350,
—
—
0.5
0.5
0.5

lb/bbl

Baroid
—
—
—
—
—

Barablock,

lb/bbl

M-I Lo Wate,
50
50
50
50
50

lb/bbl

Initial ES,

384

volts

Hot-rolled 16

306

hrs, ES

Static-aged
150

240

ES, volts

Initial Properties
120° F.
120° F.
120° F.
120° F.
120° F.

600 rpm
159
—
224
205
—

300 rpm
97
—
138
125
—

200 rpm
73
—
103
93
—

100 rpm
44
—
65
56
—

6 rpm
7
—
10
9
—

3 rpm
5
—
7
7
—

Plastic
62
—
86
80
—

Viscosity, cP

Yield Pt,
35
—
52
45
—

lb/100 ft{circumflex over ( )}2

Gels, 10
6/7
—
7/8

—

sec/10 min.

Settling in
no
—
no
no
—

thermocup

Initial

387

ES, volts

Hot-rolled
161
369
314
218
336

16 hrs, ES

HR 16 hrs at 150° F.
150° F.
150° F.
150° F.
150° F.
150° F.

600 rpm
114
136
167
133
157

300 rpm
68
80
102
78
94

200 rpm
50
59
76
57
69

100 rpm
30
35
47
34
41

6 rpm
5
7
10
6
6

3 rpm
4
5
8
4
4

Plastic
46
56
65
55
63

Viscosity, cP

Yield Pt,
22
24
37
23
31

lb/100 ft{circumflex over ( )}2

Gels, 10
4/5
5/6
8/8
5/5
5/5

sec/10 min.

API filt,
—
—
1.8
—
—

ml total

API filt,
—
—
0.1
—
—

ml oil

API filt,
—
—
1.7
—
—

ml emulsion

API filt,
—
—
0.0
—
—

ml brine

HTHP at
—
2.4
3.6
—
4.8

250° F., ml

250° F. oil
—
—
0.4
—
0.3

250° F.
—
1.0
3.2
—
2.5

emulsion

250° F.
—
1.4
—
—
2.0

brine

Free Oil, %

25%

25%

Sample #

351
355
359

IA - 35,
94.26
89.26
84.26

grams

Cesium
445 (2.3)
445 (2.3)
445 (2.3)

Formate,

grams

Integrity
20
25
30

Emulsifier,

lb/bbl

Integrity
0.5
0.5
0.5

Synvis,

lb/bbl

Witco
0.5
0.5
0.5

DTA 350,

lb/bbl

Baroid
10
10
10

Barablock,

lb/bbl

M-I Lo Wate,
50
50
50

lb/bbl

Initial ES,
301
300
357
365
440
492

volts

Hot-rolled
308
348
328
325
368
389

16 hrs, ES

Initial Properties
120° F.
150° F.
120° F.
150° F.
120° F.
150° F.

600 rpm
195
193
241
227
300+
300+

300 rpm
117
120
147
143
253
233

200 rpm
87
91
111
110
196
182

100 rpm
53
56
70
70
127
119

6 rpm
7
10
12
15
28
29

3 rpm
5
7
8
11
20
22

Plastic
78
73
94
84
—
—

Viscosity, cP

Yield Pt,
39
47
53
59
—
—

lb/100 ft{circumflex over ( )}2

Gels, 10
5/6
8/9
8/10
11/14
19/22
22/26

sec/10 min.

Settling in
no
no
1
2
9
10

thermocup

HR 16 hrs at

150° F.

600 rpm
300+
226
300+
274
300+
300+

300 rpm
201
140
246
171
300+
242

200 rpm
154
106
188
129
282
186

100 rpm
98
67
119
81
181
121

6 rpm
20
15
25
19
42
32

3 rpm
15
11
19
15
32
26

Plastic
—
86
—
103
—
—

Viscosity,

cP

Yield Pt,
—
54
—
68
—
—

lb/

100 ft{circumflex over ( )}2

Gels, 10
14/19
11/12
18/22
14/15
32/33
25/27

sec/10

min.

API filt,
0
0.0
0.0

ml total

API filt,
—
0.0
0.0

ml oil

API filt,
0
0.0
0.0

ml emulsion

API filt,
—
0.0
0.0

ml brine

HTHP at

150° F., ml

HTHP at
trace
1.2
trace

250° F., ml

250° F.

0.0
0.0

oil

250° F.

1.2
trace

emulsion

250° F.

0.0
0.0

brine

[0047]

8

Cesium formate, IA - 35 (42/58 mixture, 2.3 s.g. CsF) 2.3 sg csf

Mixing Procedure:

1.
Measure out IA - 35

2.
Add Synvis, mix 5 minutes

3.
Add CsF, mix 10 min.

4.
Add Synvert 5, mix 10 minutes

5.
Add DTA 350, mix on Silverson to 120° F.

6.
Add calcium carbonate, mix 10 minutes on HB

7.
Run initial ES, viscosities at 120° F.

8.
Put 10 ml sample in a vial, SA for 24 hrs at 75° F., measure

9.
Hot-roll for 16 hours at 150° F.

10.
Remix, run rheology, ES, API, HTHP at 150° F.

11.
Put vials in oven and static-age at 150° F. for 24 hrs, measure

12.
If 150° F. HTHP is good, run at 250° F.

Sample #

349
350
351
352

IA - 35,
94.26
94.26
94.26
94.26

grams

Cesium
445 (2.3)
445 (2.3)
445 (2.3)
445 (2.3)

Formate,

grams

Integrity
20
20
20
20

Emulsifier,

lb/bbl

Integrity
0.5
0.5
0.5
0.5

Synvis,

lb/bbl

Witco DTA
—
0.5
0.5
1.0

350, lb/bbl

Baroid
—
—
10
—

Barablock,

lb/bbl

M-I Lo Wate,
50
50
50
50

lb/bbl

Initial
227
253
256
266
301
300
283
365

ES, volts

Hot-rolled
109
205
209
222
308
348
262
276

16 hrs, ES

Initial Properties
120° F.
150° F.
120° F.
150° F.
120° F.
150° F.
120° F.
150° F.

600 rpm
188
138
179
134
195
193
179
146

300 rpm
113
81
108
80
117
120
112
92

200 rpm
83
59
80
59
87
91
84
70

100 rpm
49
35
48
35
53
56
53
43

6 rpm
8
6
6
5
7
10
7
6

3 rpm
5
5
4
4
5
7
4
4

Plastic
75
57
71
54
78
73
67
54

Viscosity, cP

Yield Pt,
38
24
37
26
39
47
45
38

lb/100 ft{circumflex over ( )}2

Gels, 10
5/6
5/5
4/5
4/5
5/6
8/9
4/5
5/5

sec/10 min.

Settling in
no
no
no
no
no
no
no
no

thermocup

HR 16 hrs

at 150° F.

600 rpm
187
137
196
137
300+
226
189
143

300 rpm
114
81
120
82
201
140
119
90

200 rpm
85
60
90
61
154
106
91
69

100 rpm
52
36
56
37
98
67
60
44

6 rpm
9
7
9
7
20
15
12
9

3 rpm
7
5
7
5
15
11
8
6

Plastic
73
56
76
55
—
86
70
53

Viscosity, cP

Yield Pt,
41
25
44
27
—
54
49
37

lb/100 ft{circumflex over ( )}2

Gels, 10
7/7
6/6
6/8
5/5
14/19
11/12
8/10
6/7

sec/10 min.

API filt,
0.7
0.4
0
1.2

ml total

API filt,
—
—
—
0.1

ml oil

API filt,
0.7
0.4
0
1.1

ml emulsion

API filt,
—
—
—
—

ml brine

HTHP at
—
—

150° F., ml

HTHP at
3.2
8.8
trace
3.6

250° F., ml

250° F. oil
2.4
6.0

2.8

250° F.
0.8
2.8

0.8

emulsion

250° F.
0.0
0.0

0.0

brine

Comments

24 hrs at

75° F.

Total fluid
38
38
38
38

heighth

free oil
0
0
0
0

heighth

emusion
38
38
38
38

heighth

free brine
0
0
0
0

heighth

free oil, %
0
0
0
0

emusion, %
100%
100%
100%
100%

free brine, %
0
0
0
0

24 hrs at

150° F.

Total fluid
38
38
38
38

heighth

free oil
0
0
0
0

heighth

emusion
38
38
38
38

heighth

free brine
0
0
0
0

heighth

free oil, %
0
0
0
0

emusion, %
100%
100%
100%
100%

free brine, %
0
0
0
0

Sample #

355
356
357
358

IA - 35, grams
89.26
89.26
84.26
84.26

Cesium Formate,
445 (2.3)
445 (2.3)
445 (2.3)
445 (2.3)

grams

Integrity
25
25
30
30

Emulsifier,

lb/bbl

Integrity
0.5
0.5
0.5
0.5

Synvis,

lb/bbl

Witco DTA
0.5
1.0
—
0.5

350, lb/bbl

Baroid
10
—
—
—

Barablock,

lb/bbl

M-I Lo Wate,
50
50
50
50

lb/bbl

Initial
357
365
329
311
335
316
344
321

ES, volts

Hot-rolled
328
325
307
307
298
301
301
272

16 hrs, ES

Initial Properties
120° F.
150° F.
120° F.
150° F.
120° F.
150° F.
120° F.
150° F.

600 rpm
241
227
196
154
235
182
245
190

300 rpm
147
143
121
95
147
110
150
116

200 rpm
111
110
92
72
108
82
113
86

100 rpm
70
70
59
46
67
51
70
53

6 rpm
12
15
11
10
13
11
13
11

3 rpm
8
11
8
7
10
8
9
8

Plastic
94
84
75
59
88
72
95
74

Viscosity, cP

Yield Ft,
53
59
46
36
59
38
55
42

lb/100 ft{circumflex over ( )}2

Gels, 10
8/10
11/14
8/9
7/8
9/10
9/9
9/10
8/9

sec/10 min.

Settling in
1
2
3
4
5
6
7
8

thermocup

HR 16 hrs

at 150° F.

600 rpm
300+
274
201
153
229
174
245
185

300 rpm
246
171
124
94
140
106
151
112

200 rpm
188
129
95
71
105
79
114
84

100 rpm
119
81
60
49
65
49
70
52

6 rpm
25
19
12
10
13
12
14
11

3 rpm
19
15
9
8
10
9
10
8

Plastic
—
103
77
59
89
68
94
73

Viscosity, cP

Yield Pt,
—
68
47
35
51
38
57
39

lb/100 ft{circumflex over ( )}2

Gels, 10
18/22
14/15
9/10
8/8
10/10
9/10
10/11
8/9

sec/10 min.

API filt,
0.0
1.8
0.0
1.0

ml total

API filt,
0.0
0.1
0.0
trace

ml oil

API filt,
0.0
1.7
0.0
1.0

ml emulsion

API filt,
0.0
0.0
0.0
0.0

ml brine

HTHP at

150° F., ml

HTHP at
1.2
7.4
4.8
4.4

250° F., ml

250° F. oil
0.0
0.0
0.0
0.0

250° F.
1.2
7.4
4.8
4.4

emulsion

250° F.
0.0
0.0
0.0
0.0

brine

Comments

24 hrs at

75° F.

Total fluid
38
38
38
38

heighth

free oil heighth
0
0
0
0

emusion heighth
38
38
38
38

free brine
0
0
0
0

heighth

free oil, %
0
0
0
0

emusion, %
100%
100%
100%
100%

free brine, %
0
0
0
0

24 hrs at

150° F.

Total fluid
38
38
38
38

heighth

free oil
trace of oil
trace of oil
trace of oil
trace of oil

heighth

emusion
38
38
38
38

heighth

free brine
0
0
0
0

heighth

free oil, %
trace
trace
trace
trace

emusion, %
100%
100%
100%
100%

free brine, %
0
0
0
0

Sample #

353
354
359
360

IA - 35, grams
89.26
89.26
84.26
84.26

Cesium Formate,
445 (2.3)
445 (2.3)
445 (2.3)
445 (2.3)

grams

Integrity
25
25
30
30

Emulsifier,

lb/bbl

Integrity
0.5
0.5
0.5
0.5

Synvis,

lb/bbl

Witco DTA
—
0.5
0.5
1.0

350, lb/bbl

Baroid
—
—
10
—

Barablock,

lb/bbl

M-I Lo Wate,
50
50
50
50

lb/bbl

Initial
301
295
384
387
440
492
457
481

ES, volts

Hot-rolled
339
242
306
314
368
389
377
366

16 hrs, ES

Initial Properties
120° F.
150° F.
120° F.
150° F.
120° F.
150° F.
120° F.
150° F.

600 rpm
203
155
224
171
300+
300+
261
219

300 rpm
122
92
138
104
253
233
167
142

200 rpm
90
68
103
77
196
182
129
109

100 rpm
53
41
65
47
127
119
84
70

6 rpm
7
7
10
8
28
29
14
12

3 rpm
5
5
7
7
20
22
9
8

Plastic
81
63
86
67
—
—
94
77

Viscosity, cP

Yield Pt,
41
29
52
37
—
—
73
65

lb/100 ft{circumflex over ( )}2

Gels, 10
6/6
5/6
7/8
7/7
19/22
22/26
9/11
8/10

sec/10 min.

Settling in
no
no
no
no
9
10
11
12

thermocup

HR 16 hrs

at 150° F.

600 rpm
212
158
225
167
300+
300+
262
192

300 rpm
131
95
140
102
300+
242
168
123

200 rpm
97
70
105
76
282
186
131
95

100 rpm
60
42
66
47
181
121
86
64

6 rpm
11
8
13
10
42
32
20
14

3 rpm
8
6
10
8
32
26
15
11

Plastic
81
63
85
65
—
—
94
69

Viscosity, cP

Yield Pt,
50
32
55
37
—
—
74
54

lb/100 ft{circumflex over ( )}2

Gels, 10
8/9
6/6
10/10
8/8
32/33
25/27
14/15
10/12

sec/10 min.

API filt,
0.3
1.8
0.0
0.3

ml total

API filt,
—
0.1
0.0
trace

ml oil

API filt,
0.3
1.7
0.0
0.3

ml emulsion

API filt,
—
—
0.0
0.0

ml brine

HTHP at

150° F., ml

HTHP at
4.8
3.6
trace
3.6

250° F., ml

250° F. oil
3.6
0.4
0.0
0.0

250° F.
1.2
3.2
trace
1.6

emulsion

250° F.
0.0
0.0
0.0
2.0

brine

Comments

24 hrs at

75° F.

Total fluid
38
38
38
38

heighth

free oil
0
0
0
0

heighth

emusion
38
38
38
38

heighth

free brine
0
0
0
0

heighth

free oil, %
0
0
0
0

emusion, %
100%
100%
100%
100%

free brine, %
0
0
0
0

24 hrs at

150° F.

Total fluid
38
38
38
38

heighth

free oil
0
0
0
0

heighth

emusion
38
38
38
38

heighth

free brine
0
0
0
0

heighth

free oil, %
0
0
0
0

emusion, %
100%
100%
100%
100%

free brine, %
0
0
0
0

Sample #

SA 250
SA 250

SA 250
SA 250

Initial
Silv.

Initial
Silv.

349
349.5
349.75
350
350.5
350.75
351
352

IA - 35, grams
94.26
94.26
94.26
94.26
94.26
94.26
94.26
94.26

Cesium Formate,
445
445
445
445
445
445
445
445

grams

Integrity
20
20
20
20
20
20
20
20

Emulsifier,

lb/bbl

Integrity
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5

Synvis,

lb/bbl

Witco DTA
—
—
—
0.5
0.5
0.5
0.5
1.0

350, lb/bbl

Baroid
—
—
—
—
—
—
10
—

Barablock,

lb/bbl

M-I Lo Wate,
50
50
50
50
50
50
50
50

lb/bbl

Initial
227

256

301
283

ES, volts

Hot-rolled
109

209

308
262

16 hrs, ES

Static-aged

113

154

ES, volts

Initial Properties
120° F.
120° F.
120° F.
120° F.
120° F.
120° F.
120° F.
120° F.

600 rpm
188
147
—
179
148
—
195
179

300 rpm
113
90
—
108
88
—
117
112

200 rpm
83
68
—
80
65
—
87
84

100 rpm
49
41
—
48
39
—
53
53

6 rpm
8
6
—
6
6
—
7
7

3 rpm
5
4
—
4
4
—
5
4

Plastic
75
57
—
71
60
—
78
67

Viscosity, cP

Yield Pt,
38
33
—
37
28
—
39
45

lb/100 ft{circumflex over ( )}2

Gels, 10
5/6
5/6
—
4/5
4/6
—
5/6
4/5

sec/10 min.

Settling in
no
no
—
no
no
—
no
no

thermocup

HR 16 hrs

at 150° F.

600 rpm
187

196

300+
189

300 rpm
114

120

201
119

200 rpm
85

90

154
91

100 rpm
52

56

98
60

6 rpm
9

9

20
12

3 rpm
7

7

15
8

Plastic
73

76

—
70

Viscosity, cP

Yield Pt,
41

44

—
49

lb/100 ft{circumflex over ( )}2

Gels, 10
7/7

6/8

14/19
8/10

sec/10 min.

Comments

Initial
253

266

300
365

ES, volts

Hot-rolled
205
145
331
222
175
330
348
276

16 hrs, ES

Initial Properties
150° F.

150° F.

150° F.
150° F.

600 rpm
138

134

193
146

300 rpm
81

80

120
92

200 rpm
59

59

91
70

100 rpm
35

35

56
43

6 rpm
6

5

10
6

3 rpm
5

4

7
4

Plastic
57

54

73
54

Viscosity, cP

Yield Pt,
24

26

47
38

lb/100 ft{circumflex over ( )}2

Gels, 10
5/5

4/5

8/9
5/5

sec/10 min.

Settling in
no

no

no
no

thermocup

SA 250
SA 250

SA 250
SA 250

Initial
Silv.

Initial
Silv.

HR 16 hrs at 150° F.
150° F.
150° F.
150° F.
150° F.
150° F.
150° F.
150° F.
150° F.

600 rpm
137
98
121
137
104
121
226
143

300 rpm
81
58
70
82
60
70
140
90

200 rpm
60
42
51
61
44
51
106
69

100 rpm
36
25
30
37
26
30
67
44

6 rpm
7
4
5
7
5
5
15
9

3 rpm
5
3
3
5
3
3
11
6

Free Oil, %

22%

25%

Sample #

SA 250
SA 250

SA 250
SA 250

Initial
Silv.

Initial
Silv.

353
353.5
353.75
354
354.5
354.75
355

IA - 35,
89.26
89.26
89.26
89.26
89.26
89.26
89.26

grams

Cesium
445
445
445
445
445
445
445

Formate,

grams

Integrity
25
25
25
25
25
25
25

Emulsifier,

lb/bbl

Integrity
0.5
0.5
0.5
0.5
0.5
0.5
0.5

Synvis,

lb/bbl

Witco DTA
—
—
—
0.5
0.5
0.5
0.5

350, lb/bbl

Baroid
—
—
—
—
—
—
10

Barablock,

lb/bbl

M-I Lo Wate,
50
50
50
50
50
50
50

lb/bbl

Initial
301

384

357

ES, volts

Hot-rolled
339

306

328

16 hrs, ES

Static-aged

150

240

ES, volts

Initial Properties
120° F.
120° F.
120° F.
120° F.
120° F.
120° F.
120° F.

600 rpm
203
159
—
224
205
—
241

300 rpm
122
97
—
138
125
—
147

200 rpm
90
73
—
103
93
—
111

100 rpm
53
44
—
65
56
—
70

6 rpm
7
7
—
10
9
—
12

3 rpm
5
5
—
7
7
—
8

Plastic
81
62
—
86
80
—
94

Viscosity, cP

Yield Pt,
41
35
—
52
45
—
53

lb/100 ft{circumflex over ( )}2

Gels, 10
6/6
6/7
—
7/8

—
8/10

sec/10 min.

Settling in
no
no
—
no
no
—
1

thermocup

HR 16 hrs

at 150° F.

600 rpm
212

225

300+

300 rpm
131

140

246

200 rpm
97

105

188

100 rpm
60

66

119

6 rpm
11

13

25

3 rpm
8

10

19

Plastic
81

85

—

Viscosity, cP

Yield Pt,
50

55

—

lb/100 ft{circumflex over ( )}2

Gels, 10
8/9

10/10

18/22

sec/10 min.

Comments

Initial
295

387

365

ES, volts

Hot-rolled
242
161
369
314
218
336
325

16 hrs, ES

Initial Properties
150° F.

150° F.

150° F.

600 rpm
155

171

227

300 rpm
92

104

143

200 rpm
68

77

110

100 rpm
41

47

70

6 rpm
7

8

15

3 rpm
5

7

11

Plastic
63

67

84

Viscosity, cP

Yield Pt,
29

37

59

lb/100 ft{circumflex over ( )}2

Gels, 10
5/6

7/7

11/14

sec/10 min.

Settling in
no

no

no

thermocup

SA 250
SA 250

SA 250
SA 250

Initial
Silv.

Initial
Silv.

HR 16 hrs at 150° F.
150° F.
150° F.
150° F.
150° F.
150° F.
150° F.
150° F.

600 rpm
158
114
136
167
133
157
274

300 rpm
95
68
80
102
78
94
171

200 rpm
70
50
59
76
57
69
129

100 rpm
42
30
35
47
34
41
81

6 rpm
8
5
7
10
6
6
19

3 rpm
6
4
5
8
4
4
15

Free Oil, %

25%

25%

Sample #

356
357
358
359
360

IA - 35, grams
89.26
84.26
84.26
84.26
84.26

Cesium Formate,
445
445
445
445
445

grams

Integrity
25
30
30
30
30

Emulsifier,

lb/bbl

Integrity
0.5
0.5
0.5
0.5
0.5

Synvis, lb/bbl

Witco DTA
1.0
—
0.5
0.5
1.0

350, lb/bbl

Baroid
—
—
—
10
—

Barablock,

lb/bbl

M-I Lo Wate,
50
50
50
50
50

lb/bbl

Initial
329
335
344
440
457

ES, volts

Hot-rolled
307
298
301
368
377

16 hrs, ES

Static-aged

ES, volts

Initial Properties
120° F.
120° F.
120° F.
120° F.
120° F.

600 rpm
196
235
245
300+
261

300 rpm
121
147
150
253
167

200 rpm
92
108
113
196
129

100 rpm
59
67
70
127
84

6 rpm
11
13
13
28
14

3 rpm
8
10
9
20
9

Plastic
75
88
95
—
94

Viscosity, cP

Yield Pt,
46
59
55
—
73

lb/100 ft{circumflex over ( )}2

Gels, 10
8/9
9/10
9/10
19/22
9/11

sec/10 min.

Settling in
3
5
7
9
11

thermocup

HR 16 hrs at

150° F.

600 rpm
201
229
245
300+
262

300 rpm
124
140
151
300+
168

200 rpm
95
105
114
282
131

100 rpm
60
65
70
181
86

6 rpm
12
13
14
42
20

3 rpm
9
10
10
32
15

Plastic
77
89
94
—
94

Viscosity, cP

Yield Pt,
47
51
57
—
74

lb/100 ft{circumflex over ( )}2

Gels, 10
9/10
10/10
10/11
32/33
14/15

sec/10 min.

Comments

Initial
311
316
321
492
481

ES, volts

Hot-rolled
307
301
272
389
366

16 hrs, ES

Initial Properties
150° F.
150° F.
150° F.
150° F.
150° F.

600 rpm
154
182
190
300+
219

300 rpm
95
110
116
233
142

200 rpm
72
82
86
182
109

100 rpm
46
51
53
119
70

6 rpm
10
11
11
29
12

3 rpm
7
8
8
22
8

Plastic
59
72
74
—
77

Viscosity, cP

Yield Pt,
36
38
42
—
65

lb/100 ft{circumflex over ( )}2

Gels, 10
7/8
9/9
8/9
22/26
8/10

sec/10 min.

Settling in
no
no
no
no
no

thermocup

HR 16 hrs

at 150° F.

600 rpm
153
174
185
300+
192

300 rpm
94
106
112
242
123

200 rpm
71
79
84
186
95

100 rpm
49
49
52
121
64

6 rpm
10
12
11
32
14

3 rpm
8
9
8
26
11

Free Oil, %

[0048]

9

Cesium formate, IA - 35 (50/50 mixture, 2.3 s.g. CsF)

Mixing Procedure: 2.3 sg csf

1.
Measure out IA - 35

1A.
Add Synvis, mix 5 minutes

2.
Add CsF, mix 10 min.

3.
Add Synvert 5, mix 10 minutes

3A.
Add calcium carbonate, mix 10 minutes

4.
Run initial ES, viscosities at 120° F.

5.
Put 10 ml sample in a vial, SA for

24 hrs at 75° F., measure volumes

6.
Hot-roll for 16 hours at 150° F.

7.
Remix, run rheology, ES, API, HTHP at 150° F.

8.
Put vials in oven and static-age at 150° F.

for 24 hrs, measure volumes

9.
If 150° F. HTHP is good, run at 250° F.

41.6/58.4 oil/csf ratio

Sample #

337
338
339
340

IA - 35, grams
98.26
98.26
93.26
93.26

Cesium
445
445
445
445

Formate,
(2.366)
(2.366)
(2.366)
(2.366)

grams

Integrity
25
25
20
20

Emulsifier,

lb/bbl

Integrity
0.5
1
0.5
1

Synvis,

lb/bbl

Witco DTA
—
—
—
—

350, lb/bbl

Baroid
50
50
50
50

Baracarb 50,

lb/bbl

Initial
103
129
167
166
114
151
117
128

ES, volts

Hot-rolled
114
102
148
140
139
138
122
118

16 hrs, ES

Initial Properties
120° F.
150° F.
120° F.
150° F.
120° F.
150° F.
120° F.
150° F.

600 rpm
162
116
186
118
164
115
183
126

300 rpm
93
65
114
67
96
66
109
73

200 rpm
67
47
83
49
70
48
80
53

100 rpm
40
27
49
29
41
28
47
31

6 rpm
8
7
9
6
7
6
8
6

3 rpm
6
5
7
5
5
5
6
5

Plastic
69
51
72
51
68
49
74
53

Viscosity, cP

Yield Pt,
24
14
42
16
28
17
35
20

lb/100 ft{circumflex over ( )}2

Gels, 10
6/7
6/6
6/7
5/6
5/6
5/5
6/7
5/5

sec/10 min.

Settling in
no
no
no
no
no
no
no
no

thermocup

HR 16 hrs at

150° F.

600 rpm
161
113
187
123
162
114
184
129

300 rpm
93
64
116
70
97
66
111
75

200 rpm
68
46
86
52
72
48
82
55

100 rpm
39
27
52
30
473
28
49
32

6 rpm
8
6
10
6
7
6
8
6

3 rpm
6
5
8
5
5
4
6
5

Plastic
68
49
71
53
65
48
73
56

Viscosity, cP

Yield Pt,
25
15
45
17
32
18
38
28

lb/100 ft{circumflex over ( )}2

Gels, 10
6/6
5/6
7/9
5/6
6/6
5/5
6/7
5/6

sec/10 min.

API filt,
1.0
0.2
0.4
0.3

ml total

API filt,
—
—
—
—

ml oil

API filt,
1.0
0.2
0.4
0.3

ml emulsion

API filt,
—
—
—
—

ml brine

HTHP at

0.2
0.2

150° F., ml

HTHP at

11.4
4.4

250° F., ml

250° F. oil

0.0
0.0

250° F.

6.8
3.2

emulsion

250° F.

4.6
1.2

brine

Comments

41.6/58.4 oil/csf ratio

Sample #

347
348
341
342
343
344
345
346

IA - 35,
88.26
88.26
88.26
88.26
98.26
98.26
93.26
93.26

grams

Cesium
445
445
445
445
445
445
445
445

Formate, grams
(2.3)
(2.3)

Integrity
25
25
25
25
15
15
20
20

Emulsifier,

lb/bbl

Integrity
—
—
0.5
1
—
—
—
—

Synvis,

lb/bbl

Witco DTA
0.5
1
—
—
0.5
1
0.5
1

350, lb/bbl

Baroid
50
50
50
50
50
50
50
50

Baracarb 50,

lb/bbl

Initial
212
192
205
243

ES, volts

Hot-rolled
148
145
252
247

16 hrs, ES

Initial Properties
120° F.
150° F.
120° F.
150° F.

600 rpm
177
132
182
132

300 rpm
106
78
111
80

200 rpm
77
57
83
61

100 rpm
46
347
52
38

6 rpm
8
7
10
8

3 rpm
6
5
7
6

Plastic
71
54
71
52

Viscosity, cP

Yield Pt,
35
24
40
28

lb/100 ft{circumflex over ( )}2

Gels, 10
6/6
6/6
8/8
6/7

sec/10 min.

Settling in
no
no
no
no

thermocup

HR 16 hrs at

150° F.

600 rpm
179
140
184
144

300 rpm
109
84
113
88

200 rpm
80
62
85
66

100 rpm
48
37
52
41

6 rpm
8
7
10
9

3 rpm
6
5
8
7

Plastic
70
56
71
56

Viscosity, cP

Yield Pt,
39
32
42
32

lb/100 ft{circumflex over ( )}2

Gels, 10
6/6
5/5
8/8
7/9

sec/10 min.

API filt,
3.5
6.2

ml total

API filt,
—
—

ml oil

API filt,
3.5
6.2

ml emulsion

API filt,
—
—

ml brine

HTHP at
19.4
(0.8

150° F., ml

brine)

HTHP at

250° F., ml

250° F. oil

250° F.

emulsion

250° F.

brine

Comments

NOTE:

1. Sample 337 and 338 looked grainy with 15 lb/bbl Synvert V. Concentration was increased to 25 lb/bbl. After hot-rolling at 150° F., #337 and #338 still appear grainy.

2. Mud weight of 339 is 14.7 lb/gal (CsF in 337-340 is 2.366 s.g)

3. Mud weight of 347 is 14.6 lb/gal (CsF in 347-348 is 2.30 s.g)

[0049]

10

Cesium formate, IA - 35 (50/50 mixture)

175 ml IA - 35 (0.828 sg) - (144.9 grams)

175 ml Cesium Formate (2.2 sg) - (385 grams)

Mixing Procedure:

1.
Measure out IA - 35

1A.
Add Synvis, mix 5 minutes

2.
Add CsF, mix 10 min.

3.
Add Synvert 5, mix 10 minutes

3A.
Add calcium carbonate, mix 10 minutes

4.
Run initial ES, viscosities at 120° F.

5.
Put 10 ml sample in a vial, SA for

24 hrs at 75° F., measure volumes

6.
Hot-roll for 16 hours at 150° F.

7.
Remix, run rheology, ES, API, HTHP at 150° F.

8.
Put vials in oven and static-age at 150° F.

for 24 hrs, measure volumes

9.
If 150° F. HTHP is good, run at 250° F.

50/50 ratio

Mud weight, 13.1 Lb/gal

Sample #

313
314
314A
314B
315
316
317
318

IA - 35, grams
134.9
134.9
134.9
134.9
134.9
134.9
134.9
134.9

Cesium
385
385
385
385
385
385
385
385

Formate,

grams

Integrity
10
10
15
20
10
10
10
10

Emulsifier,

lb/bbl

Integrity
0.5
0.5
0.5
0.5
0.5
0.5
1
1

Synvis,

lb/bbl

Witco DTA
1
1.25
1.125
1.125
1.5
1.75
1
1.25

350, lb/bbl

Baroid
50
50
50
50
50
50
50
50

Baracarb 50,

lb/bbl

Initial
330
332
353
355
437
402
298
330

ES, volts

Hot-rolled
416
343
284
290
396
427
344
396

16 hrs, ES

Initial

Properties

600 rpm at
89
102
70
72
108
120
91
104

120° F.

300 rpm
58
66
40
39
78
83
59
70

200 rpm
47
53
30
28
66
70
48
57

100 rpm
35
42
19
16
53
56
36
44

6 rpm
20
26
4
2
32
31
20
25

3 rpm
17
21
3
1
26
19
18
22

Plastic
31
36
30
33
30
37
32
34

Viscosity, cP

Yield Pt,
27
30
10
6
48
46
27
36

lb/100 ft{circumflex over ( )}2

Gels, 10
23/19
25/25
4/9
2/3
19/25
19/19
17/23
23/27

sec/10 min.

Settling in
No
No
No
No
No
No
No
No

thermocup

HR 16 hrs at

150° F.

600 rpm at
93
93
82
73
93
95
113
124

120° F.

300 rpm
67
67
54
40
67
69
81
93

200 rpm
57
57
44
29
58
60
69
81

100 rpm
46
47
34
17
48
49
55
67

6 rpm
23
25
14
3
28
27
22
32

3 rpm
17
19
10
2
20
19
18
24

Plastic
26
26
28
33
26
26
32
31

Viscosity, cP

Yield Pt,
41
41
26
7
41
43
49
62

lb/100 ft{circumflex over ( )}2

Gels, 10
19/23
21/21
12/15
3/4
23/23
21/19
21/26
26/21

sec/10 min.

API filt,
1.2
1.8
5.8
2.6
2.2
1.2
0.2
3

ml total

API filt,
0.8
1
0.7
0.6
1
0.2
0.1
0.9

ml oil

API filt,
0.4
0.8
5.1
2.0
1.2
1
0.1
2.1

ml emulsion

API filt,
0
0
0
0
0
0
0
0

ml brine

HTHP at

150° F., ml

HTHP at

250° F., ml

Comments

oil on

oil on
oil on

top

top
top

of jar

of jar
of jar

24 hrs at

75° F.

Total fluid
38
38

38
38
38
38

heighth

free oil
0.1
1.0

0.1
0.1
0.1
0.1

heighth

emusion
38
37

38
38
38
38

heighth

free brine
0
0

0
0
0
0

heighth

free oil, %
0.3%
2.6%

0.3%
0.3%
0.3%
0.3%

emusion, %
100.0%
97.4%

100.0%
100.0%
100.0%
100.0%

free brine, %
0.0%
0.0%

0.0%
0.0%
0.0%
0.0%

24 hrs at

150° F.

Total fluid
38
38

38
38
38
38

heighth

free oil
4
4

3
3
2
2

heighth

emusion
34
34

35
35
36
36

heighth

free brine
0
0

0
0
0
0

heighth

free oil, %
10.5%
10.5%

7.9%
7.9%
5.3%
5.3%

emusion, %
89.5%
89.5%

92.1%
92.1%
94.7%
94.7%

free brine, %
0.0%
0.0%

0.0%
0.0%
0.0%
0.0%

72 hrs at

150° F.

Total fluid

heighth

free oil

heighth

emusion

heighth

free brine

heighth

free oil, %

emusion, %

free brine, %

50/50 ratio

Mud weight, 13.1 Lb/gal

Sample #

319
320
321
322
323
324

IA - 35, grams
134.9
134.9
134.9
134.9
134.9
134.9

Cesium
385
385
385
385
385
385

Formate,

grams

Integrity
10
10
10
10
10
10

Emulsifier,

lb/bbl

Integrity
1
1
1.5
1.5
1.5
1.5

Synvis,

lb/bbl

Witco DTA
1.5
1.75
1
1.25
1.5
1.75

350, lb/bbl

Baroid
50
50
50
50
50
50

Baracarb 50,

lb/bbl

Initial
309
377
245
282
263
358

ES, volts

Hot-rolled
346
355
324
268
380
382

16 hrs, ES

Initial

Properties

600 rpm
115
111
91
117
127
136

at 120° F.

300 rpm
77
78
52
74
85
97

200 rpm
64
64
38
59
70
82

100 rpm
49
49
23
43
54
66

6 rpm
27
27
7
23
30
36

3 rpm
22
22
6
19
24
28

Plastic
38
33
39
43
42
39

Viscosity, cP

Yield Pt,
39
45
13
31
43
58

lb/100 ft{circumflex over ( )}2

Gels, 10
24/24
23/26
7/12
21/26
26/29
29/29

sec/10 min.

Settling
No
No
No
No
No
No

in thermocup

HR 16 hrs at

150° F.

600 rpm
122
118
133
140
147
148

at 120° F.

300 rpm
90
90
98
101
111
111

200 rpm
78
79
83
86
96
97

100 rpm
64
65
68
69
78
78

6 rpm
32
32
28
31
34
34

3 rpm
23
23
22
23
25
25

Plastic
32
28
35
39
36
37

Viscosity, cP

Yield Pt,
58
62
63
62
75
74

lb/100 ft{circumflex over ( )}2

Gels, 10
24/19
21/18
25/31
27/258
26/26
28/26

sec/10 min.

API filt,
2
1.5
2.3
2.4
1.0
0.8

ml total

API filt,
1
1
0.5
0.8
0.3
0.6

ml oil

API filt,
1
0.5
1.8
1.6
0.7
0.2

ml emulsion

API filt,
0
0
0
0
0
0

ml brine

HTHP at

150° F., ml

HTHP at

250° F., ml

Comments
oil on
oil on

top
top

of jar
of jar

24 hrs at

75° F.

Total fluid
38
38
38
38
38
38

heighth

free oil
0.1
0.1
1.0
0.1
0.1
0.1

heighth

emusion
38
38
37
38
38
38

heighth

free brine
0
0
0
0
0
0

heighth

free oil, %
0.3%
0.3%
2.6%
0.3%
0.3%
0.3%

emusion, %
100.0%
100.0%
97.4%
100.0%
100.0%
100.0%

free brine, %
0.0%
0.0%
0.0%
0.0%
0.0%
0.0%

24 hrs at

150° F.

Total fluid
38
38
38
38
38
38

heighth

free oil
3
2
4
3
2
2

heighth

emusion
35
36
34
35
36
36

heighth

free brine
0
0
0
0
0
0

heighth

free oil, %
7.9%
5.3%
10.5%
7.9%
5.3%
5.3%

emusion, %
92.1%
94.7%
89.5%
92.1%
94.7%
94.7%

free brine, %
0.0%
0.0%
0.0%
0.0%
0.0%
0.0%

[0050]

11

Cesium formate, IA - 35 (50/50 mixture)

175 ml IA - 35 (0.828 sg) - (144.9 grams)

175 ml Cesium Formate (2.2 sg) - (385 grams)

Mixing Procedure:

529.9
350

2.2 sg

331.4

csf

1.
Measure out IA - 35

559.24
8

50
18.52

13.1080

1A.
Add Synvis, mix 5 minutes

50
18.52

2

2.
Add CsF, mix 10 min.

609.24
350
1.740686

22.5

3.
Add Synvert 5, mix 10 minutes

1.6871

2.70108

0.373

3A.
Add calcium carbonate, mix 10 minutes

0.828
5
0.309258

0.626

4.
Run initial ES, viscosities at 120° F.

2.2
5
1.3783

5.
Put 10 ml sample in a vial, SA

1.687558

for 24 hrs at 75° F., measure volumes

559.2

6.
Hot-roll for 16 hours at 150° F.

2.3 sg
4
331.48

csf

7.
Remix, run rheology, ES, API, HTHP at 150° F.

50
18.52

609.2

14.4999

8.
Put vials in oven and static-age at 150° F.

4
350
1.740686
1

for 24 hrs, measure volumes

1.687

1

9.
If 150° F. HTHP is good, run at 250° F.

0.828
0.4163
0.344696

2.3
0.5837
1.34251

1.687206

Additional 0.5 lb/bbl

137.995

1
114.26

193.484
445.015

9
2

37/63 Oil/Formate ratio 14.4 lb/gal

Sample #

H.R. 16 hrs

at 250° F.

325
326
327
328
329
329
329
330

IA - 35, grams
87.5
87.5
87.5
87.5
87.5
87.5
87.5
87.5

Cesium
456.9
456.9
456.9
456.9
456.9
456.9
456.9
456.9

Formate,

grams

Integrity
15
15
15
15
15
15
15
15

Emulsifier,

lb/bbl

Integrity
—
1
2
2
1
1
1
—

Synvis,

lb/bbl

Witco DTA
—
1
1
2
—
—
—
1

350, lb/bbl

Baroid
50
50
50
50
50
50
50
50

Baracarb 50,

lb/bbl

Initial
167
395
413
443
303
303

378

ES, volts

Hot-rolled
221
372
377
488
284
284
259
324

16 hrs, ES

Initial Properties

120° F.

600 rpm
163
233
300+
300+
251

247
177

at 120° F.

300 rpm
97
142
210
300+
154

156
106

200 rpm
71
107
162
253
116

121
78

100 rpm
42
64
104
185
71

71
46

6 rpm
6
9
22
66
11

13
5

3 rpm
4
6
16
53
8

10
3

Plastic
66
91
—
—
97

91
71

Viscosity, cP

Yield Pt,
31
51
—
—
57

65
35

lb/100 ft{circumflex over ( )}2

Gels, 10
4/5
6/7
15/18
53/81
7/9

10/18
3/4

sec/10 min.

Settling in

slight

thermocup

sag

HR 16 hrs at 150° F.

150° F.
150° F.

600 rpm
177
267
300+
300+
273
179
165
200

at 120° F.

300 rpm
108
177
260
300+
180
114
101
128

200 rpm
80
137
208
300+
140
87
76
99

100 rpm
48
92
140
252
91
54
46
65

6 rpm
8
21
40
98
20
10
8
15

3 rpm
5
16
32
80
15
7
6
11

Plastic
69
90
—
—
93
65
64
72

Viscosity, cP

Yield Pt,
39
87
—
—
87
49
37
56

lb/100 ft{circumflex over ( )}2

Gels, 10
5/6
15/33
30/57
80/114
14/17
7/8
6/6
10/11

sec/10 min.

API filt,
0.7
0.8
0
0
0

9

ml total

API filt,
0
0
0
0
0

0

ml oil

API filt,
0.7
0.8
0
0
0

9

ml emulsion

API filt,

ml brine

HTHP at

150° F., ml

HTHP at

12.6
7.2

250° F., ml

250° F. oil

0
0

250° F.

11.8
6.4

emulsion

250° F.

0.8
0.8

brine

Comments

24 hrs at

75° F.

Total fluid
39
38
38
38
38

38

heighth

free oil
1.0
0.0
0.0
0.0
0.0

0.0

heighth

emusion
38
38
38
38
38

38

heighth

free brine
0
0
0
0
0

0

heighth

free oil, %

emusion, %

free brine, %

24 hrs at

150° F.

Total fluid

heighth

free oil

heighth

emusion

heighth

free brine

heighth

free oil, %

emusion, %

free brine, %

72 hrs at

150° F.

Total fluid

heighth

free oil

heighth

emusion

heighth

free brine

heighth

free oil, %

emusion, %

free brine, %

37/63 Oil/Formate ratio 14.4 lb/gal

Sample #

Hot roll

16 hrs

at 250° F.

331
332
332
332
333
334

IA - 35, grams
82.5
82.5
82.5
82.5
82.5
82.5

Cesium
456.9
456.9
456.9
456.9
456.9
456.9

Formate,

grams

Integrity
20
20
20
20
20
20

Emulsifier,

lb/bbl

Integrity
—
1
1
1
—
0.5

Synvis,

lb/bbl

Witco DTA
1
—
—
—
—
—

350, lb/bbl

Baroid
50
50
50
50
50
50

Baracarb 50,

lb/bbl

Initial
427
285
285

351
337
310
277

ES, volts

Hot-rolled
391
363
363
293

16 hrs, ES

Initial Properties

120° F.
120° F.
150° F.
120° F.
150° F.

600 rpm
223
247

273
218
170
230
170

at 120° F.

300 rpm
137
152

172
132
103
139
103

200 rpm
104
14

131
98
76
104
76

100 rpm
63
69

83
59
46
62
46

6 rpm
9
12

15
8
8
9
8

3 rpm
5
8

11
6
5
6
5

Plastic
86
95

101
86
67
91
67

Viscosity, cP

Yield Pt,
51
57

71
46
36
48
36

lb/100 ft{circumflex over ( )}2

Gels, 10
5/6
8/9

12/15
6/7
6/6
6/7
6/6

sec/10 min.

Settling

in thermocup

HR 16 hrs at 150° F.

150° F.
120° F.
120° F.
150° F.
120° F.
150° F.

600 rpm
223
280
186
174
222
179
245
176

at 120° F.

300 rpm
140
179
117
103
139
112
155
111

200 rpm
106
138
89
76
106
86
119
83

100 rpm
66
89
55
45
67
54
76
52

6 rpm
11
19
11
8
13
11
15
10

3 rpm
7
14
8
6
9
8
10
7

Plastic
83
101
69
71
83
67
90
65

Viscosity, cP

Yield Pt,
57
78
48
32
56
45
65
46

lb/100 ft{circumflex over ( )}2

Gels, 10
7/8
14/18
8/9
6/7
9/10
8/9
10/15
7/8

sec/10 min.

API filt,
3.5
0

1.1
0.3

ml total

API filt,
0
0

0.0
0.0

ml oil

API filt,
3.5
0

1.1
0.3

ml emulsion

API filt,

ml brine

HTHP at

150° F., ml

HTHP at

11.4
9.6
40.0
23.2

250° F., ml

250° F. oil

0
0
0.0
0.0

250° F.

11.4
8.6
36.0
21.2

emulsion

250° F.

0.6
1.0
4.0
2.0

brine

Comments

24 hrs at

75° F.

Total fluid
38
38

heighth

free oil
0.0
0.0

heighth

emusion
38
38

heighth

free brine
0
0

heighth

37/63 Oil/Formate ratio 14.4 lb/gal

Sample #

Synvis added after h.r.

335
336
334A
336A

IA - 35, grams
82.5
82.5
82.5
82.5

Cesium
456.9
456.9
456.9
456.9

Formate,

grams

Integrity
25
25
20
25

Emulsifier,

lb/bbl

Integrity
—
0.5
1.0
1.0

Synvis,

lb/bbl

Witco DTA
—
—
—
—

350, lb/bbl

Baroid
50
50
50
50

Baracarb 50,

lb/bbl

Initial
400
278
337
344
405
297
381
312

ES, volts

Hot-rolled

297
313
312
353

16 hrs, ES

Initial Properties
120° F.
150° F.
120° F.
150° F.
120° F.
150° F.
120° F.
150° F.

600 rpm at 120° F.
245
192
264
206
300+
219
300+
227

300 rpm
151
119
162
127
194
135
197
141

200 rpm
114
90
122
96
151
102
150
108

100 rpm
70
56
75
59
96
63
94
68

6 rpm
12
10
14
12
18
12
18
14

3 rpm
8
7
10
9
13
8
13
11

Plastic
94
73
102
79
—
84
—
86

Viscosity, cP

Yield Pt,
57
46
60
48
—
51
—
55

lb/100 ft{circumflex over ( )}2

Gels, 10
8/9
8/9
10/11
9/10
12/16
8/9
13/17
11/11

sec/10 min.

Settling

in thermocup

HR 16 hrs at

150° F.

600 rpm
241
192
264
210
300+
200
297
220

at 120° F.

300 rpm
152
123
169
133
200
127
191
141

200 rpm
116
94
129
103
157
97
148
109

100 rpm
73
60
83
66
104
62
97
70

6 rpm
15
14
18
15
25
13
22
16

3 rpm
11
10
13
11
20
10
17
12

Plastic
89
69
95
77
—
73
106
79

Viscosity, cP

Yield Pt,
63
54
74
56
—
54
85
62

lb/100 ft{circumflex over ( )}2

Gels, 10
11/12
10/11
13/20
11/12
18/24
10/11
16/22
12/13

sec/10 min.

API filt,
1.4
0.2
—
0.2

ml total

API filt,
0.0
0.0
—
0.0

ml oil

API filt,
1.4
0.2
—
0.2

ml emulsion

API filt,

ml brine

HTHP at

150° F., ml

HTHP at
45.6
27.6
12.0
12.0

250° F., ml

250° F. oil
0.0
0.0
0.0
0.0

250° F.
35.6
27.0
10.0
11.0

emulsion

250° F.
10.0
0.6
2.0
1.0

brine

Comments

37/63 Oil/Formate ratio 14.4 lb/gal

Sample #

0.5 lb/bbl Synvis

added after h.r.

333
334
334A
335

IA - 35, grams
82.5
82.5
82.5
82.5

Cesium
456.9
456.9
456.9
456.9

Formate,

grams

Integrity
20
20
20
25

Emulsifier,

lb/bbl

Integrity
—
0.5
1.0
—

Synvis,

lb/bbl

Witco DTA
—
—
—
—

350, lb/bbl

Baroid
50
50
50
50

Baracarb 50,

lb/bbl

Initial
351
337
310
277
405
297
400
278

ES, volts

Hot-rolled

297
313

16 hrs, ES

Initial Properties
120° F.
150° F.
120° F.
150° F.
120° F.
150° F.
120° F.
150° F.

600 rpm at 120° F.
218
170
230
170
300+
219
245
192

300 rpm
132
103
139
103
194
135
151
119

200 rpm
98
76
104
76
151
102
114
90

100 rpm
59
46
62
46
96
63
70
56

6 rpm
8
8
9
8
18
12
12
10

3 rpm
6
5
6
5
13
8
8
7

Plastic
86
67
91
67
—
84
94
73

Viscosity, cP

Yield Pt,
46
36
48
36
—
51
57
46

lb/100 ft{circumflex over ( )}2

Gels, 10
6/7
6/6
6/7
6/6
12/16
8/9
8/9
8/9

sec/10 min.

Settling

in thermocup

HR 16 hrs at

150° F.

600 rpm
222
179
245
176
300+
200
241
192

at 120° F.

300 rpm
139
112
155
111
200
127
152
123

200 rpm
106
86
119
83
157
97
116
94

100 rpm
67
54
76
52
104
62
73
60

6 rpm
13
11
15
10
25
13
15
14

3 rpm
9
8
10
7
20
10
11
10

Plastic
83
67
90
65
—
73
89
69

Viscosity, cP

Yield Pt,
56
45
65
46
—
54
63
54

lb/100 ft{circumflex over ( )}2

Gels, 10
9/10
8/9
10/15
7/8
18/24
10/11
11/12
10/11

sec/10 min.

API filt,
1.1
0.3
—
1.4

ml total

API filt,
0.0
0.0
—
0.0

ml oil

API filt,
1.1
0.3
—
1.4

ml emulsion

API filt,

ml brine

HTHP at

150° F., ml

HTHP at
40.0
23.2
12.0
45.6

250° F., ml

250° F. oil
0.0
0.0
0.0
0.0

250° F.
36.0
21.2
10.0
35.6

emulsion

250° F.
4.0
2.0
2.0
10.0

brine

37/63 Oil/Formate ratio 14.4 lb/gal

Sample #

0.5 lb/bbl Synvis

added after h.r.

336

336A

IA - 35, grams
82.5
82.5

Cesium
456.9
456.9

Formate,

grams

Integrity
25
25

Emulsifier,

lb/bbl

Integrity
0.5
1.0

Synvis,

lb/bbl

Witco DTA
—
—

350, lb/bbl

Baroid
50
50

Baracarb 50,

lb/bbl

Initial
337
344
381
312

ES, volts

Hot-rolled

312
353

16 hrs, ES

Initial Properties
120° F.
150° F.
120° F.
150° F.

600 rpm at 120° F.
264
206
300+
227

300 rpm
162
127
197
141

200 rpm
122
96
150
108

100 rpm
75
59
94
68

6 rpm
14
12
18
14

3 rpm
10
9
13
11

Plastic
102
79
—
86

Viscosity, cP

Yield Pt,
60
48
—
55

lb/100 ft{circumflex over ( )}2

Gels, 10
10/11
9/10
13/17
11/11

sec/10 min.

Settling in

thermocup

HR 16 hrs

at 150° F.

600 rpm
264
210
297
220

at 120° F.

300 rpm
169
133
191
141

200 rpm
129
103
148
109

100 rpm
83
66
97
70

6 rpm
18
15
22
16

3 rpm
13
11
17
12

Plastic
95
77
106
79

Viscosity, cP

Yield Pt,
74
56
85
62

lb/100 ft{circumflex over ( )}2

Gels, 10
13/20
11/12
16/22
12/13

sec/10 min.

API filt,
0.2
0.2

ml total

API filt,
0.0
0.0

ml oil

API filt,
0.2
0.2

ml emulsion

API filt,

ml brine

HTHP at

150° F., ml

HTHP at
27.6
12.0

250° F., ml

250° F. oil
0.0
0.0

250° F.
27.0
11.0

emulsion

250° F.
0.6
1.0

brine

Comments

[0051]

12

Cesium formate, Escaid 110 (50/50 mixture)

175 ml Escaid 110 (0.803 sg) - (140.5 grams)

175 ml Cesium Formate (2.2 sg) - (385 grams)

Mixing Procedure:

1.
Measure out Escaid 110

2.
Add emulsifiers, mix 5 minutes

3.
Add CsF, mix 10 min. on HB, mix on Silverson to 135° F.

3A.
Add Lo-Wate, mix 10 min. on HB

4.
Run initial ES, viscosities at 120° F.

5.
Put 10 ml sample in a vial, SA for 24 hrs at

75° F., measure volumes

6.
Hot-roll for 16 hours at 150° F.

7.
Remix, run rheology, ES, API, HTHP at 150° F.

8.
Put vials in oven and static-age at 150° F.

for 24 hrs, measure volumes

9.
If 150° F. HTHP is good, run at 250° F.

Sample #

273
274
275
276
277
278

Integrity Synvert
5
10
10
10
15
15

IV (Lot# 000329),

lb/bbl

Witco AX-180-2,
5
5
5
5
5
5

lb/bbl

Witco DTA

2
3

2

350, lb/bbl

dimer trimer

Baroid
50
50
50
50
50
50

Baracarb 50,

lb/bbl

Initial
363
360
425
572
454
417

ES, volts @ 120° F.

Hot-rolled 16 hrs. ES
399
410
378
489
403
329

Jar − S = Settling,
S 3
S 3
S
S 3
S
S

3 = 3 Phases, N = No

Initial

Properties

600 rpm at 120° F.
24
25
29
42
27
29

300 rpm
13
14
17
30
15
15

200 rpm
9
9
12
25
10
11

100 rpm
5
5
8
19
6
6

6 rpm
1
1
2
10
2
1

3 rpm
1
1
1
7
1
1

Plastic
11
11
12
12
12
14

Viscosity, cP

Yield Pt,lb/100 ft{circumflex over ( )}2
2
3
5
18
3
1

Gels, 10
1/1
1/1
2/2
7/8
1/2
1/1

sec/10 min.

Settling in
Y
Y
Y
N
Y
Y

thermocup

HR 64 hrs at

150° F.

600 rpm at 120° F.
24
26
31
54
28
28

300 rpm
12
13
18
40
15
15

200 rpm
8
9
14
34
11
11

100 rpm
5
5
9
28
7
6

6 rpm
1
1
3
19
2
1

3 rpm
1
1
2
11
2
1

Plastic
12
13
13
14
13
13

Viscosity, cP

Yield Pt,
0
0
5
26
2
2

lb/100 ft{circumflex over ( )}2

Gels, 10
1/1
1/1
2/2
14/8
2/2
1/1

sec/10 min.

Settling in
Y
Y
N
N
Y
Y

Thermocup

Settling in Jar
¼″
⅛″
{fraction (1/16)}″
—
{fraction (1/16)}″
⅛″

API filt,
3.2
1.8
2.0
2.0
1.4
2.6

ml total

API filt,
1.6
1.6
2.0
2.0
0.4
2.6

ml oil

API filt,
1.6
0.2
0.0
0.0
1.0
0.0

ml brine

HTHP at 150° F., ml
8.6
6.6
8.6
8.0
9.8
13.4

HTHP at 250° F., ml

17.2

29.0

Static Age - 64 hrs

at 75° F.

Total fluid height
32
32
32
32
32
32

free oil height
4
3
7
7
2
3

emusion height
28
29
25
25
30
29

free brine height
0
0
0
0
0
0

free oil, %
13%

9%
22%
22%

6%

9%

emusion, %
87.5%
90.6%
78.1%
78.1%
93.8%
90.6%

free brine, %
0.0%
0.0%
0.0%
0.0%
0.0%
0.0%

Total
100%
100%
100%
100%
100%
100%

MP = Multiple
MP
MP
MP
MP
MP
MP

Phase Emulsion

Static Age - 24

hrs at 150° F.

Total fluid height
32
32
32
32
32
32

free oil height
7
7
10
8
10
9

emusion height
25
25
22
24
22
23

free brine height
0
0
0
0
0
0

free oil, %
22%
22%
31%
25%
31%
28%

emusion, %
78.1%
78.1%
68.8%
75.0%
68.8%
71.9%

free brine, %
0.0%
0.0%
0.0%
0.0%
0.0%
0.0%

Total
100%
100%
100%
100%
100%
100%

MP = Multiple
MP
MP
MP
MP
MP
MP

Phase Emulsion

Difference (64 hrs/24

hrs at 150° F.)

free oil, %

emusion, %

free brine, %

Sample #

279
280
281
282
283
284

Integrity Synvert IV
5
5
5
5
2.5
2.5

(Lot# 000329), lb/bbl

Witco AX-180-2, lb/bbl
7.5
10
10
10
10
10

Witco DTA

2
3

2

350, lb/bbl

dimer trimer

Baroid
50
50
50
50
50
50

Baracarb 50,

lb/bbl

Initial
448
390
445
552
360
458

ES, volts @ 120° F.

Hot-rolled
398
431
345
288
359
229

16 hrs, ES

Jar − S = Settling,
S
S
N
N
S
S

3 = 3 Phases, N = No

Initial

Properties

600 rpm at 120° F.
26
24
30
47
24
32

300 rpm
14
13
18
33
13
19

200 rpm
9
9
13
28
9
15

100 rpm
5
5
9
21
5
10

6 rpm
1
1
3
9
2
3

3 rpm
1
1
3
6
1
2

Plastic
12
11
12
14
11
13

Viscosity, cP

Yield Pt,
2
2
6
19
2
6

lb/100 ft{circumflex over ( )}2

Gels, 10
1/2
1/2
3/4
6/6
1/2
3/3

sec/10 min.

Settling in
Y
Y
Y
N
Y
N

thermocup

HR 64 hrs

at 150° F.

600 rpm at 120° F.
25
25
32
56
25
35

300 rpm
13
13
20
42
13
22

200 rpm
9
9
16
36
9
13

100 rpm
5
5
11
28
5
12

6 rpm
1
1
4
15
1
4

3 rpm
1
1
3
8
1
4

Plastic
12
12
12
14
12
13

Viscosity, cP

Yield Pt,
1
1
8
28
1
9

lb/100 ft{circumflex over ( )}2

Gels, 10
1/1
1/1
4/5
7/5
2/2
5/3

sec/10 min.

Settling in
Y
Y
Y
N
Y
N

Thermocup

Settling in Jar
¼″
¼″
—
¼″
{fraction (5/16)}″
—

API filt,
3.0
3.2
2.0
2.1
2.1
2.2

ml total

API filt,
0.8
1.2
1.8
1.8
1.4
1.9

ml oil

API filt,
2.2
2.0
0.2
0.2
0.7
0.3

ml brine

HTHP at 150° F., ml
11.6
14.6
7.0
4.4
12.0
5.6

HTHP at 250° F., ml

15.0
12.4
20.8
14.8

Static Age - 64 hrs

at 75° F.

Total fluid height
32
32
32
32
32
32

free oil height
3
8
9
10
9
9

emusion height
29
24
23
22
23
23

free brine height
0
0
0
0
0
0

free oil, %
9%
25%
28%
31%
28%
28%

emusion, %
90.6%
75.0%
71.9%
68.8%
71.9%
71.9%

free brine, %
0.0%
0.0%
0.0%
0.0%
0.0%
0.0%

Total
100%
100%
100%
100%
100%
100%

MP = Multiple
MP
—
—
—
—
—

Phase Emulsion

Static Age - 24 hrs

at 150° F.

Total fluid height
32
32
32
32
32
32

free oil height
4
10
10
10
10
10

emusion height
28
22
22
22
22
22

free brine height
0
0
0
0
0
0

free oil, %
13%
31%
31%
31%
31%
31%

emusion, %
87.5%
68.8%
68.8%
68.8%
68.8%
68.8%

free brine, %
0.0%
0.0%
0.0%
0.0%
0.0%
0.0%

Total
100%
100%
100%
100%
100%
100%

MP = Multiple
MP
—
—
—
—
—

Phase Emulsion

Difference (64 hrs/24

hrs at 150° F.)

free oil, %

emusion, %

free brine, %

[0052]

13

Cesium formate, IA - 35 (50/50 mixture)

175 ml IA - 35 (0.828 sg) - (144.9 grams)
NOTE: Make up ½ bbl

175 ml Cesium Formate (2.2 sg) - (385 grams)
Equivalents

Mixing Procedure:

1.
Measure out IA - 35

1A.
Add Synvis, mix 5 minutes

2.
Add CsF, mix 10 min.

3.
Add Synvert 5, mix 10 minutes

3A.
Add calcium carbonate, mix 10 minutes

4.
Run initial ES, viscosities at 120° F.

5.
Put 10 ml sample in a vial, SA for

24 hrs at 75° F., measure volumes

6.
Hot-roll for 16 hours at 150° F.
NOTE: Make up ½ bbl

Equivalents

7.
Remix, run rheology, ES, API, HTHP at 150° F.

8.
Put vials in oven and static-age at 150° F.

for 24 hrs, measure volumes

9.
If 150° F. HTHP is good, run at 250° F.
NOTE: Make up ½ bbl

Equivalents

oil/cs ratio

50/50

50/50
50/50

50/50
53/47

Sample #

285
285
286
287
287
288
289

IA - 35, grams
119.9
119.9
119.9
119.9
119.9
119.9
144.9

Cesium
385
385
385
385
385
385
385

Formate,

grams

Integrity Synvert
25
25
25
25
25
25
25

5, lb/bbl

Integrity
5
5
5
10
10
10
5

Synvis,

lb/bbl

Baroid
—
—
50
—
—
50
—

Baracarb 50,

lb/bbl

Initial
823

680
646

595
641

ES, volts

Hot-rolled
494

619
551

528
509

16 hrs, ES

Initial

Properties

600 rpm at
273
164
300+
300+
300+
300+
142

120° F.

300 rpm
184
94
230
300+
290
300+
85

200 rpm
144
67
182
300+
230
300+
64

100 rpm
102
39
130
229
157
300+
40

6 rpm
39
7
41
81
45
119
10

3 rpm
26
5
37
72
38
105
8

Plastic
89
70
—
—

—
57

Viscosity, cP

Yield Pt,
95
24
—
—

—
28

lb/100 ft{circumflex over ( )}2

Gels, 10
23/27
5/7
33/37
65/72
35/42
87/96
7/9

sec/10 min.

Settling in
N

N
N

N
N

thermocup

API filt,
10 (8 min)

0
1.5

0
10 (2 min)

ml total

API filt,
0

0
0

0
0

ml oil

API filt,
0

0
0

0
0

ml brine

HTHP at 150° F., ml

HTHP at 250° F., ml

HR 16 hrs at

150° F.

600 rpm at 120° F.
270

294
300+

300+
197

300 rpm
171

184
300+

300+
120

200 rpm
132

148
300+

300+
90

100 rpm
89

100
300+

284
60

6 rpm
24

28
102

95
16

3 rpm
19

23
87

83
13

Plastic
99

110
—

—
77

Viscosity, cP

Yield Pt,
72

74
—

—
43

lb/100 ft{circumflex over ( )}2

Gels, 10
16/21

21/25
81/86

74/84
11/16

sec/10 min.

Comments

24 hrs at

75° F.

Total fluid
33

34
34

33
34

heighth

free oil
0

0
0

0
0

heighth

emusion
33

34
34

33
34

heighth

free brine
0

0
0

0
0

heighth

free oil, %
0%

0%
0%

0%
0%

emusion, %
100.0%

100.0%
100.0%

100.0%
100.0%

free brine, %
0.0%

0.0%
0.0%

0.0%
0.0%

24 hrs at

150° F.

Total fluid
33

34
34

33
34

heighth

free oil
0

0
0

0
0

heighth

emusion
33

34
34

33
34

heighth

free brine
0

0
0

0
0

heighth

free oil, %
0%

0%
0%

0%
0%

emusion, %
100.0%

100.0%
100.0%

100.0%
100.0%

free brine, %
0.0%

0.0%
0.0%

0.0%
0.0%

72 hrs at

150° F.

Total fluid
33

34
34

33
34

heighth

free oil
1

2
0

0
2

heighth

emusion
32

32
34

33
32

heighth

free brine
0

0
0

0
0

heighth

free oil, %
3%

6%
0%

0%
6%

emusion, %
97.0%

94.1%
100.0%

100.0%
94.1%

free brine, %
0.0%

0.0%
0.0%

0.0%
0.0%

API filt,

ml total

API filt,

ml oil

API filt,

ml brine

HTHP at 150° F., ml

HTHP at 250° F., ml

HR 16 hrs at

150° F.

600 rpm at 120° F.
292

200

300 rpm
192

124

200 rpm
151

94

100 rpm
102

59

6 rpm
31

14

3 rpm
25

11

Plastic
100

76

Viscosity, cP

Yield Pt,
92

48

lb/100 ft{circumflex over ( )}2

Gels, 10
23/26

10/12

sec/10 min.

Comments

oil/cs ratio

53/47
48.5/51.5
48.5/51.5
48.5/51.5
48.5/51.5
56/44
56/44

Sample #

290
291
292
293
294
295
296

IA - 35, grams
144.9
94.9
94.9
94.9
94.9
144.9
144.9

Cesium
385
385
385
385
385
385
385

Formate,

grams

Integrity Synvert
25
50
50
50
50
50
50

5, lb/bbl

Integrity
10
5
5
10
10
5
10

Synvis,

lb/bbl

Baroid
—
—
50
—
50
—
—

Baracarb 50,

lb/bbl

Initial
1032
452
392
409
337
651
698

ES, volts

Hot-rolled
660
469
442
373
341
490
645

16 hrs, ES

Initial

Properties

600 rpm at 120° F.
300+
262
300+
300+
300+
114
300+

300 rpm
300+
164
193
300+
300+
68
230

200 rpm
287
129
149
300+
300+
50
184

100 rpm
243
86
100
300+
221
33
126

6 rpm
83
24
28
115
73
11
38

3 rpm
73
19
22
98
61
9
31

Plastic
—
98
—
—
—
46
—

Viscosity, cP

Yield Pt,
—
66
—
—
—
22
—

lb/100 ft{circumflex over ( )}2

Gels, 10
64/69
19/25
21/28
89/103
57/76
4/4
29/36

sec/10 min.

Settling in
N
N
N
N
N
N
N

thermocup

API filt,
1.5
10 (2
0.0
7.0
0.0
6.9
10 (2

ml total

min)

min)

API filt,
0
0
0
0
0
0
0

ml oil

API filt,
0
0
0
0
0
0
0

ml brine

HTHP at 150° F., ml

HTHP at 250° F., ml

HR 16 hrs at

150° F.

600 rpm at 120° F.
300+
300+
300+
300+
300+
152
300+

300 rpm
300+
206
257
300+
300+
89
203

200 rpm
243
160
202
300+
300+
65
155

100 rpm
177
109
140
263
298
41
106

6 rpm
69
33
43
89
100
11
32

3 rpm
59
29
36
78
88
9
27

Plastic
—
—
—
—
—
63
—

Viscosity, cP

Yield Pt,
—
—
—
—
—
26
—

lb/100 ft{circumflex over ( )}2

Gels, 10
46/53
24/33
33/42
70/80
78/88
3/4
25/32

sec/10 min.

Comments

24 hrs at

75° F.

Total fluid
34
35
34
33
33
34
34

heighth

free oil
0
0
0
0
0
0
0

heighth

emusion
34
35
34
33
33
34
34

heighth

free brine
0
0
0
0
0
0
0

heighth

free oil, %
0%
0%
0%
0%
0%
0%
0%

emusion, %
100.0%
100.0%
100.0%
100.0%
100.0%
100.0%
100.0%

free brine, %
0.0%
0.0%
0.0%
0.0%
0.0%
0.0%
0.0%

24 hrs at

150° F.

Total fluid
34
35
34
33
33
34
34

heighth

free oil
0
0
1
0
0
1
0

heighth

emusion
34
35
33
33
33
33
34

heighth

free brine
0
0
0
0
0
0
0

heighth

free oil, %
0%
0%
3%
0%
0%
3%
0%

emusion, %
100.0%
100.0%
97.1%
100.0%
100.0%
97.1%
100.0%

free brine, %
0.0%
0.0%
0.0%
0.0%
0.0%
0.0%
0.0%

72 hrs at

150° F.

Total fluid
34
35
34
33
33
34
34

heighth

free oil
0
2
2
0
0
5
0

heighth

emusion
34
33
32
33
33
29
34

heighth

free brine
0
0
0
0
0
0
0

heighth

free oil, %
0%
6%
6%
0%
0%
15%
0%

emusion, %
100.0%
94.3%
94.1%
100.0%
100.0%
85.3%
100.0%

free brine, %
0.0%
0.0%
0.0%
0.0%
0.0%
0.0%
0.0%

HR 16 hrs at

150° F.

600 rpm at

300+

144

120° F.

300 rpm

240

83

200 rpm

189

61

100 rpm

129

38

6 rpm

41

9

3 rpm

34

7

Plastic

61

Viscosity, cP

Yield Pt,

—

22

lb/100 ft{circumflex over ( )}2

Gels, 10

32/38

7/9

sec/10 min.

Comments

[0053]

14

Cesium formate, Escaid 110 (50/50 mixture)

175 ml Escaid 110 (0.803 sg) - (140.5 grams)

175 ml Cesium Formate (2.2 sg) - (385 grams)

Mixing Procedure:

1.
Measure out Escaid 110

2.
Add emulsifiers, mix 5 minutes, add Barablock,

mix 10 minutes

3.
Add CsF, mix 10 min. on HB, mix on Silverson

to 135° F.

3A.
Add Lo-Wate, mix 10 min. on HB

4.
Run initial ES, viscosities at 120° F.

5.
Put 10 ml sample in a vial, SA for 24 hrs at

75° F., measure volumes

6.
Hot-roll for 16 hours all 50° F.

7.
Remix, run rheology, ES, API, HTHP at 150° F.

8.
Put vials in oven and static-age at 150° F.

for 24 hrs, measure volumes

9.
If 150° F. HTHP is good, run at 250° F.

Sample #

261
262
262
264
265
266

Integrity
10
15
20
15

Synvert IV (Lot #

000329), lb/bbl

Rhodia Miranol

7
10.5

CS, lb/bbl

Witco AX-180-2,

lb/bbl

Witco DTA

3

350, lb/bbl

dimer trimer

Baroid
50
50
50
50
50
50

Baracarb 50,

lb/bbl

Initial
285
306
355
327
8
1

ES, volts

Hot-rolled
320
350
314
376
2
1

16 hrs, ES

Initial

Properties

600 rpm at 120° F.
26
25
25
27
64
66

300 rpm
13
12
13
13
40
41

200 rpm
9
8
9
8
32
32

100 rpm
5
4
4
4
22
23

6 rpm
1
1
1
0
7
8

3 rpm
1
1
1
0
4
5

Plastic
13
13
12
14
24
25

Viscosity, cP

Yield Pt,lb/100 ft{circumflex over ( )}2
0
−1
1
−1
16
16

Gels, 10
0/1
0/1
1/1
1/1
6/4
6/5

sec/10 min.

Settling in
yes
yes
yes
yes
no
no

thermocup

API filt,
4.8
4.1
2.7
2.7
11 (1 min)
10 (1 min)

ml total

API filt,
—
—
—
—
—
—

ml oil

API filt,
—
—
—
—
4.2
7.0

ml brine

HR 16 hrs at

150° F.

600 rpm at 120° F.
26
26
27
42
63
54

300 rpm
14
13
14
25
40
34

200 rpm
9
8
9
20
31
28

100 rpm
5
5
5
14
19
20

6 rpm
1
1
1
3
6
6

3 rpm
1
1
1
3
4
3

Plastic
12
13
13
17
23
20

Viscosity, cP

Yield Pt,
2
0
1
8
17
14

lb/100 ft{circumflex over ( )}2

Gels, 10
1/1
1/1
1/1
1/1
4/5
5/4

sec/10 min.

Comments
settling
settling
settling
¼
3
3

inch oil
phases
phases

24 hrs at

75° F.

Total fluid
32
33
33
32
32
32

heighth

free oil
2
2
2
2
0
0

heighth

emusion
28
29
29
30
21
21

heighth

free brine
0
0
0
0
11
11

heighth

free oil, %
6%
6%
6%
6%
0%
0%

emusion, %
87.5%
87.9%
87.9%
93.8%
65.6%
65.6%

free brine, %
0.0%
0.0%
0.0%
0.0%
34.4%
34.4%

24 hrs at

150° F.

Total fluid
32
33
33
32
32
32

heighth

free oil
2
4
3
5
0
0

heighth

emusion
30
29
30
27
21
20

heighth

free brine
0
0
0
0
11
12

heighth

free oil, %
6%
12%
9%
16%
0%
0%

emusion, %
93.8%
87.9%
90.9%
84.4%
65.6%
62.5%

free brine, %
0.0%
0.0%
0.0%
0.0%
34.4%
37.5%

Difference (72 hrs/24

hrs at 150° F.)

free oil, %
0%
6%
3%
9%
0%
0%

emusion, %
6%
0%
3%
−9%
0%
−3%

free brine, %
0%
0%
0%
0%
0%
3%

Sample #

267
268
269
270
271
272

Integrity

Synvert IV (Lot#

000329), lb/bbl

Rhodia Miranol
14
10.5

CS, lb/bbl

Witco AX-180-2,

7
10.5
14
10.5

lb/bbl

Witco DTA

3

3

350, lb/bbl

dimer trimer

Baroid
50
50
50
50
50
50

Baracarb 50,

lb/bbl

Initial
1
37
151
318
349
345

ES, volts

Hot-rolled
0
18
175
351
419
321

16 hrs, ES

Initial

Properties

600 rpm at 120° F.
66
67
30
24
25
94

300 rpm
42
47
17
13
13
70

200 rpm
34
50
13
9
9
59

100 rpm
24
31
8
6
6
46

6 rpm
8
2
2
1
1
15

3 rpm
4
2
2
1
1
6

Plastic
24
20
13
11
12
24

Viscosity, cP

Yield Pt,
18
27
4
2
1
46

lb/100 ft{circumflex over ( )}2

Gels, 10
6/4
5/12
2/3
1/1
1/1
9/7

sec/10 min.

Settling in
no
no
no
yes
yes
no

thermocup

API filt,
10 (1 min)
1.9
2.6
1/1
0.9
0.4

ml total

API filt,
—
0.6
—
—
—
—

ml oil

API filt,
2.5
0.3
—
—
—
—

ml brine

HR 16 hrs at

150° F.

600 rpm at
62
67
33
28
28
79

120° F.

300 rpm
39
42
19
16
16
61

200 rpm
32
37
15
12
11
53

100 rpm
22
26
10
8
7
42

6 rpm
7
2
3
2
2
16

3 rpm
4
2
2
2
2
7

Plastic
23
25
14
12
12
18

Viscosity, cP

Yield Pt,
16
17
5
4
4
43

lb/100 ft{circumflex over ( )}2

Gels, 10
6/5
2/9
3/4
3/3
2/2
9/6

sec/10 min.

Comments
3 phases
2 phases
sagging
sagging
sagging
⅜ inch oil

24 hrs at

75° F.

Total fluid
32
32
32
32
32
32

heighth

free oil
0
12
4
4
4
5

heighth

emusion
23
20
28
28
28
27

heighth

free brine
9
0
0
0
0
0

heighth

free oil, %
0%
38%
13%
13%
13%
16%

emusion, %
71.9%
62.5%
87.5%
87.5%
87.5%
84.4%

free brine, %
28.1%
0.0%
0.0%
0.0%
0.0%
0.0%

24 hrs at 150° F.

Total fluid
32
32
32
32
32
32

heighth

free oil
0
12
7
5
5
12

heighth

emusion
22
20
25
27
27
20

heighth

free brine
10
0
0
0
0
0

heighth

free oil, %
0%
38%
22%
16%
16%
38%

emusion, %
68.8%
62.5%
78.1%
84.4%
84.4%
62.5%

free brine, %
31.3%
0.0%
0.0%
0.0%
0.0%
0.0%

Difference (72 hrs/24

hrs at 150° F.)

free oil, %
0%
0%
9%
3%
3%
22%

emusion, %
−3%
0%
−9%
−3%
−3%
−22%

free brine, %
3%
0%
0%
0%
0%
0%

[0054] Other embodiments of the present invention will be apparent to those skilled in the art from consideration of the present specification and practice of the present invention disclosed herein. It is intended that the present specification and examples be considered as exemplary only with a true scope and spirit of the invention being indicated by the following claims and equivalents thereof.

Drilling fluids containing an alkali metal formate

Information

Publication Number

Date Filed

Date Published

Inventors

CPC

US Classifications

International Classifications

Abstract

Description

Claims

Parent Case Info

Provisional Applications (1)