FORM ATE TE CH N I CA L M A N UA L C A B O T CHEMICAL AND PHYSICAL PROPERTIES SECTION A6 PH AND BUFFERING A6.1 pH of formate brines ....................................................................................................................2 A6.1.1 Controlling pH in formate brines .................................................................................3 A6.1.2 Measuring pH in formate brines .................................................................................3 A6.2 pH buffering of formate brines with carbonate / bicarbonate buffer ........................ 5 A6.2.1 How the carbonate / bicarbonate buffer works ...................................................5 A6.2.2 Buffer protection against CO2 influx ..........................................................................5 A6.2.3 Buffer protection against H2S influx .........................................................................6 A6.3 Buffer addition and maintainance ..........................................................................................7 A6.3.1 Buffer capacity .................................................................................................................7 A6.3.2 Total buffer concentration ............................................................................................8 A6.3.3 Determining buffer concentration and capacity .........................................................8 A6.3.4 Buffer requirement for field use .................................................................................9 A6.3.5 Maintaining buffer concentration and capacity ..........................................................11 References ...................................................................................................................................................11 The Formate Technical Manual is continually updated. To check if a newer version of this section exists please visit formatebrines.com/manual NOTICE AND DISCLAIMER. The data and conclusions contained herein are based on work believed to be reliable; however, CABOT cannot and does not guarantee that similar results and/or conclusions will be obtained by others. This information is provided as a convenience and for informational purposes only. No guarantee or warranty as to this information, or any product to which it relates, is given or implied. CABOT DISCLAIMS ALL WARRANTIES EXPRESS OR IMPLIED, INCLUDING MERCHANTABILITY OR FITNESS FOR A PARTICULAR PURPOSE AS TO (i) SUCH INFORMATION, (ii) ANY PRODUCT OR (iii) INTELLECTUAL PROPERTY INFRINGEMENT. In no event is CABOT responsible for, and CABOT does not accept and hereby disclaims liability for, any damages whatsoever in connection with the use of or reliance on this information or any product to which it relates. © 2013 Cabot Corporation, MA, USA. All rights reserved. CABOT is a registered trademark of Cabot Corporation. VERSION 4 – 09/13 FORMATE TECHNICAL MANUAL C AB O T A6.1 pH of formate brines pH is a measure of the acidity or alkalinity of a solution, numerically equal to 7 for neutral solutions, increasing with increasing alkalinity and decreasing with increasing acidity. For dilute solutions, pH can be defined as the negative logarithm base 10 of the hydrogen concentration in the solution [H +]: The pH of formate brine can be decreased to 3.75 by adding a strong acid, but the brine will resist further pH change until all the formate ions have been converted to formic acid ions. At a pH of 3.75, the formic acid and formate anions will exist in a 1:1 molar ratio. When the pH of a formate brine is raised or lowered one unit from this value the ratio of formate to formic acid will change by a factor of pH = − log [H +] (1) 1 approximately ten, as shown in Table 1. This means that 2 aH + the behavior of the ions pHmore = − log (aH + ) In concentrated solutions, in concentrated cesium formate brine with a formate in the −solution+ depends not on their concentrations, but concentration of around 10 mol/L and a pH of around Ka pKa 3 HCOO + H 3 O+Thus, ←in →reality, HCOOHa +more H2 O precise definition on is: 10 – 10.5, the concentration of formic acid is less than pH activities. = − log [H ] 1 0.000001 mol/L. Figure 1 shows how pH of unbuffered log [H +] 2 aH + 2 − formate brine pH 2=− − log+ (aHpK − − (2) + )a CO3 pKa HCO 3 changes with addition of a strong acid. CO3 + H ←→ HCO 3 4 a where H + is the activity. log (aH + ) Ka + pK pKa 3 − HCOO− − + H ← a → HCOOH + H2 O + 3O formate / formic acid molar ratio pKa HCO3 Table 1H‘Theoretical’ 5 2 CO 3 K a HCO3 + H ←→ H2 CO3 + pK + H 3 O ←→ Commonly HCOOH + H2used O high-density oilfield brines (CaCl2, as a function of pH. a CaBr pK ) have a− naturally acidic pH. Attempts 2− − 2 − , and ZnBr CO3 pKa HCO CO3 2+ H +←a 2→ HCO 3 4 pH 3 Approx. formate / formic acid molar ratio 6 CO−2raise (g )← → CO2to(aq ) to the pH alkaline levels in these2 −halide-based − + pKa CO3 pKa HCO 3 H ←→ HCO 3 − pK 10.75 10,000,000 − a + brines result of insoluble calcium →inHprecipitation pKa or HCO3 HCO3 +can H ← 5 H2 CO 3 2 CO3 pK 9.75 1,000,000 − zinc salts, e.g. Ca(OH)2, Zn(OH) . pKa 2 + H + ←a → H2 CO3 HCO3 H2 CO 3 2 2 1 1 2 2 2 2 1 1 1 8.75 100,000 Formate saltsCO dissolved in water exhibit a naturally alkaline 6 CO ( g ) ← → ( aq ) 7.75 10,000 2 2 CO2 (aq ) + H2O ← → H2CO3 (aq) 7 ← → CO2 (aq ) pH (8 – 10). The pH of the formate brines can be adjusted 6.75 1 000 to almost any level with common acids and bases without 5.75 100 Ka1 − of insoluble causing The pH of fluids H2 CO3 (aqthe ) ←precipitation → HCO3 (aq ) + H +(aqsalts. ) 8 4.75 10 based on formate brines can therefore be safely adjusted to 3.75 1 − ) ++H2O K − 3 (aq ) CO2 (2aq ← H2CO 79 a→ 2 the delivers the CO3level + Hthat ← → HCO 3 optimal performance. 2.75 0.1 ) + H2O ← → H2CO3 (aq) pH = − log [H +] 1 1.75 0.01 Kion − The in itself, and formate brines + a 1 is a buffer H2 COformate − (aq ) ← 8 − → HCO23− (aq ) + H (aq ) 3 0.75 0.001 HCO + natural OH+ ← → CO + H2O at pH = 3.75: K10 have − a2 1 aH + =3)−a+log aH +)) buffer3 capacity aq ) ← → HCO3pH (aq H ((aq Ka2 2− − + The pKa value in formate brines has been shown to 9 CO3 + H ← → HCO3 Ka + − K a3 − increase with temperature [1]. In very concentrated + 2 pK (3) + H O ←→ HCOOH −+ H2 O 2− a H ← 11→ HCO3HCOO CO 3 + CO 2 3+ H 2O → 2HCO3 brines, pH (and thereby pKa) are poorly defined. pKa = 3.75 − 2− 10 HCO23− + OH − ← → 2 + CO 3 + H2O pKa2( aq ) CO ( aq ) + Ca → 12 2− − − ↓ CaCO3 (s) − 32 − + H +← CO3 pKa2 HCO 3 → HCO 3 4 CO 32CO + OH − ← → +3H2O 2− [ ] (mol/L) CO 3 − K + = A −x exp( B × pH )brines pK← 13 CO 2 (−g − ) + +H 2O a→ HCO3 + H− (aq) pH behavior of unbuffered formate pK3−a]1 (mol/L) [ HCO HCO H 2← H2 CO HCO3 H2 CO 3 CO 32 3++CO + H 2O1→ → 2HCO 115 3 3 − CO 2 + H 2O → 2HCO3 +14 − 2− ] ) CO3 [(Haq])×+[HCO Ca 23+( aq → ↓ CaCO3 (s) 12 14 K = 12 26 + CO ( g ) ← → CO ( aq ) PCO32 (s)2 aq ) + Ca ( aq ) → 2 ↓ CaCO [CO32 −] (mol/L) − K =− A x exp(2B− × pH ) − 13 CO2 ( g ) + H2O ←→ HCO[3[ + 2H−]+ (mol/L) (aq − ) 2− − [CO 3 ] [HCO3 ] [OH − ] [CO OH [ HCO H2 SO4 pH =− − log HCO 15 K CO33− ] (mol/L) HCO 3 10 K − log PCO2 + logCO 3 ] 3 = A x exp( B × pH ) ) + H2O ←→ HCO3 + H + (aq) No formic acid [ HCO 3− ] (mol/L) [H +]8× [HCO 3 − ] Traces of 14− K = + 0. 02pH ×P ] × [HCO16 ] CO2 (aq ) +f6HP2COO2 ← → H2formic CO3 (aqacid ) 73 pK a = 3.75 2− − − PCO 2 15 [formate [OH − ] [CO ] OH − CO32 − HCO 3−50% 2 −3 ] H SO CO pH = 2 −− log K− − log PCO + log [HCO 3 ] [CO ] ( mg /[HCO 17 [CO3 ]+ [OH− ] = 0. 02 ×2Pf− ( mol / L2) − L )− =3 1200 × P2 f 4 3 2− − 50% formic − [CO 3 ] [HCO3 ] [OH ] [CO OH − CO3 H2 SO4 acid log K − log PCO2 + log[HCO 43 ] K HCO 3 a1 H2 CO3−(aq ) ← → HCO3 (aq ) + H +(aq) 8 2− [ ] [ ] CO ( kg / m3) = 1. 2 × Pf HCO = 0 18 3 16 0. 02 ×3 Pf2 K2 2− − 9 CO3 + H + ← a→ HCO3 Pf 2− 2− ] ( mg / L ) = 1200 × Pf 17 [CO3− ]+ [0OH −] = 0. 02 × Pf ( mol / L ) CO23−] (ppb [[CO [CO32−] )= 0. 42× Pf [ ] OH = 0 19 3 2 − − Addition of strong acid [ ] + [OH ] = 0. 02 × Pf ( mol −/−L ) − CO3 ( mg / L ) = 1200 × Pf 2 − 2− [CO3 ] ( kg / m3) = 1. 2 × Pf 10 HCO → CO 3 + H2O [HCO33-+]] =OH 0 ← 18 2[HCO = [CO ]/R (mol/L) 20 3 3 2− 3 Figure 1 Graph shows how the pH of unbuffered with the addition of a strong acid. [CO3 ] ( formate ]= 0 kg / m ) =brine 1. 2 × changes Pf 1 0 11 19 21 2− − CO [OH3 −]+=− CO 3 [HCO3P]0A=G02 E+ H2 2O →S2HCO ECTION 2− A6 2- 2 + CO + Ca ) → ↓ CaCO3 (s) [HCO ] =)[CO ]/R( aq (mol/L) 12 20 3 − 3( aq 3 22 [ OH ] = 0 2= [CO3 ]/R (mol/L) − K 13 CO2 (2g− ) + H2O ←→ HCO + H + (aq) [CO3 ]− = 0. 02 × Pf ( mol / L 3) 23 [CO32−] (ppb )= 0. 42× Pf [CO ] (ppb )= 0. 42× Pf [CO32−] pf = Vol (mL) /5 2− 3 [CO32 −] (mol/L) = A x exp( B × pH ) [ HCO − ] (mol/L) [CO32−] VER S IO N 4 – 09 / 13 SECTION A: CHEMICAL AND PHYSICAL PROPERTIES A6.1.1 Controlling pH in formate brines There are two means of controlling pH in formate brines: • Addition of hydroxide, in the form of NaOH or KOH. This method can be used to increase pH in unbuffered brines or increase buffer capacity in buffered brines. However, the OH– ion is not a buffer and in unbuffered formate brines, pH will drop immediately when the brine is contacted by acid gases. Relying on OH– addition to maintain pH of a formate fluid is therefore not advised in applications where the formate will be exposed to influxes of acid gases from the reservoir. • Buffering the formate brine with carbonate / bicarbonate. Unlike the heavy bromide brines based on the divalent calcium and zinc ions, formate brines are fully compatible with carbonate / bicarbonate buffer. Buffers are designed to resist changes in fluid pH and can cope with large influxes of acid gas. A6.1.2 Measuring pH in formate brines pH is a measure of the hydrogen ion (H+) activity of a solution. Hydrogen ion activity coefficients cannot be measured experimentally. In diluted solutions, the H+ activity is not very different from the actual H+ concentration and pH can therefore be measured quite accurately. In more concentrated solutions, however, where the H+ activity deviates significantly from the H+ concentration, the true pH cannot be determined. High-density formate brines are some of the most concentrated aqueous solutions that exist (see Section A3, Water Activity and Colligative Properties), and the H+ activity varies significantly from H+ concentration in these brines. Any attempt to measure pH in these brines will therefore result in a misleading value. Although pH cannot be measured accurately in highdensity oilfield brines, it is still important for users to know something about the acidity of these fluids. For halide brines it has been found that measuring pH directly on the neat brine, and only using the results in a relative sense, is the best method [2], [3]. The main use of pH readings in formate brines is to gain knowledge about the state of the buffer. For buffered formate brines, Cabot recommends diluting the fluid with about nine parts (vol/vol) deionized water in order to obtain the most meaningful pH measurement for determining buffer condition. A buffered formate brine or fluid should be diluted with about nine parts (vol/vol)deionized water before measuring pH. V ERSION 4 – 0 9/ 13 C A B O T The reasons for this recommendation are listed below and are illustrated in Figure 2 and Figure 3, which show examples of pH measurements made with glass electrode and pH papers (BDF pH indicator sticks) in buffered and unbuffered formate brines as a function of dilution [4]. The benefits of measuring the pH of formate brines after dilution are: 1.Consistency – The measured pH of a solution should be independent of the measuring method. Figures 2 and 3 show that for two different methods of measuring pH, i.e. glass electrode and pH paper, both give similar results in dilute buffered formate brines, although they differ by up to 3 pH units in concentrated buffered formate brines. This means at least one of these methods gives erroneous pH readings in buffered concentrated formate brines. In unbuffered concentrated formate brines, the difference between the two methods is not so significant. 2.Robustness – When measuring pH directly on the neat brine, the formate concentration in the brine has a large effect on the apparent pH (Figure 2 and Figure 3). Therefore, when such a method is used in the field, one would not have any feel for what this pH value means without knowing the concentration of the brine. When the dilution method is used, this variable is removed, and the measured pH value becomes a direct indicator of the buffer’s condition. 3. Accuracy of buffer component analysis – Traditional methods for measuring carbonate and bicarbonate concentrations in formate brines are complicated or require special equipment. Cabot has developed a new analytical method that only requires users to make two simple measurements: pH and phenolphthalein endpoint determination (see Section A6.3.3). This method, however, only works if the dilution method is used. 4. Meaningful and useful pH values – When pH is measured after dilution, realistic pH values for buffers and pH indicators can be measured. For example, in a diluted formate brine, carbonate / bicarbonate buffer buffers at pH = pKa 10.2. pH indicators also change color at correct pH value. In undiluted brines, buffer and indicator pH levels are too high and inconsistent. It is important to still keep in mind that diluting brine with nine parts of water does NOT provide a true pH measurement because it still does not give a true measure of the hydrogen ion activity in the original brine. However, it provides a consistent measure that is SECTION A6 PAGE 3 FORMATE TECHNICAL MANUAL C AB O T pH measurements in buffered and unbuffered potassium formate brine 15.0 KFo 1.56 g/cm3 buffered (glass electrode) KFo 1.56 g/cm3 unbuffered (pH paper) KFo 1.56 g/cm3 buffered (glass electrode) KFo 1.56 g/cm3 buffered (pH paper) 14.0 13.0 12.0 11 .0 pH 10.0 9.0 8.0 7.0 6.0 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 Dilution factor Figure 2 Effect of dilution when measuring pH in buffered and unbuffered 1.56 g/cm3 / 13.0 lb/gal potassium formate brines. pH measurement in buffered CsFo and CsKFo brines 15.0 KFo 2.2 g/cm3 buffered (glass electrode) KFo 2.2 g/cm3 unbuffered (pH paper) KFo 2.2 g/cm3 buffered (glass electrode) KFo 2.2 g/cm3 buffered (pH paper) 14.0 13.0 pH 12.0 11 .0 10.0 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 Dilution factor Figure 3 Effect of dilution when measuring pH in buffered 2.0 g/cm3 / 16.7 lb/gal CsKFo brine and buffered 2.2 g/cm3 / 18.3 lb/gal CsFo brine. PAGE 4 SECTION A6 VER S IO N 4 – 09 / 13 SECTION A: CHEMICAL AND PHYSICAL PROPERTIES C A B O T A6.2.1 How the carbonate / bicarbonate buffer works A buffered solution is defined as a solution that resists a change in its pH when hydrogen ions (H+) or hydroxide ions (OH–) are added. The ability to resist changes in pH comes about by the buffer’s ability to consume hydrogen ions (H+) and / or hydroxide ions (OH–). pH = − log [H +] independent of the measuring method, tells something about the buffer composition in the fluid, is independent of the formate brine type and concentration, and is robust enough for fluid engineers to use in the field. When the dilution method is used, pH measurements 1 can be made in formate brines both by pH electrode (potentiometric measurements) and by use of pH The carbonate / bicarbonate buffer system provides + 2 aH + pH = − log (aH + ) ] = − log [Hmethod paper, although1 the pHpH electrode is more strong buffering at two different pH levels: Ka + − accurate. Due to the significant difference between pH pKa 3 HCOO + H O ← → HCOOH + H + 2 3 2O aH + −pH log=(−aHlog + ) [H ] 1 pH =brines measured in neat formate and in diluted formate • Upper buffering level at pH = 10.2 Ka brines, it is important always record whether the + pKa 3 [H +]2to HCOO −pH + H=3−Olog ←( H2[HO+a] + aH1 +→ ) HCOOH pK 2− pH = −+log − 2− pH = − log 1measurement was made in diluted or neat brine. (4) CO3 pKa HC CO3 + H +←a → HCO 3 4H K apH = − log (a + ) + − 2 a + pK 3 pK +aaHH +3 O ← → HCOOHH + H2 O H 2 +a a − pH = − log (aH + ) 2 − HCOO pK − ]10.2 pH =3−−+log H= 15 →COH22−CO3 HCO − pKa HCO H + [← HCO3 H If pH is measured one would clearly where pK CO3brine, + H +← → HCO 4 in neat 3 3 3 a Ka + − pK 3 HCOO + H O ← → HCOOH + H O a K 3 2 + − also to report of measurement pKa2 3 have HCOO + H 3 Othe ←method a→ HCOOH Oa pK+ H2pK pHpH = −=log (a + ) ) the−buffered 2− a + − − 2+[−H +] a+ =3−− +CO log 15 electrode) →brine pK HCO H3and ← H2 → CO H2HCO (pH paper vs. glass the← type At 10.2 solution + H HCO 3 4pH 3 CO3 a (H pKa HCO 3 3HCO 3 contains 6 CO ( g ) ← → CO ( aq ) pK 2− − 2− a + 2 2 and concentration, otherwise the measured pH the same amount (CO3 ) andHCO 3− pKa K aof carbonate CO3 + H ←→ HCO 4 + − 3 pKa 3 HCOO − − + H2 O + +pKa 2 + pK 2 − + H 3 O ← −→ HCOOH − (a 2− a apH = −pH log ) + +H [ ] → pK = − log H HCO + ← H CO HCO 5 H2−CO 3 1 H H value isCO meaningless. bicarbonate ( HCO CO3 4 3 a 3 ). 2 − 3 + pK pKaa 3 + H ←→ HCO 3 3 + → pK HCO + H ← H CO HCO 5 H CO 6 CO2 ( g ) ← → 1CO2 (aq )pH = − log 3 a 3 [H ] 2 3 2 3 K + − − 3 + pK pK− + =H 3−Olog ←(aa+→ HCOOH + H2 OpK 2 aHCOO a pK ) 2− − 2− a + + a → HpH HCO3 + H ← CO HCO 5 H CO H •CO Lower level at pH = 6.35 H 3 buffering 2 3 2 3 CO3 pKa H 4a + 3 + H ←→ HCO 3 A6.2 pH1 buffering brines with +− → ) log 2← pH =6−of logformate a pH =CO ( a + + ) CO (aq ) 2 ([aq ] = −6CO log H 1[HCO]2 ( g−)pH ( g ) ← → H H 7 2 CO2 (aq ) + H2O ← → H2CO3 (aq) K + a 2 carbonate /3bicarbonate buffer pKpK HCOO +H O ←− → HCOOH + H2 O − − a a 2− + pKa 3 →COH22−CO3 HCO − (5) pKa H + ← HCO3 5 K a HCO3 +pK H ← → HCO 4 pH = CO +← 3 3 )+ 3 a −+ + H O + 3 aH O log (aH pK 3 HCOO → HCOOH + 6 +) CO22( g ) ← → CO2−(aq 2 [ ] aH + 1 = − logpH pH (a=H H+−) log a 3H 2 H applications Formate brines7used inCO oilfield should be ( aq ) + H O ← → H CO ( aq ) 2 2 pK 2 3 Ka − − pKHa COcarbonate H2 CO3 (aq →HCO HCO3− (aq2)−+HH +CO (aq) − − 8 +asodium Kor buffered by where = 6.35 −potassium →HCOOH pK)a← + H2++−← 5 HCOO − 2→ HCO 3++H 3OK a pK 2 3HCO 3 + Ha2→ ← 4ofHCO pK 3 addition + 3H3CO a pK 3 CO3 a pH = − log ( a ) a HCOO + H O ← → HCOOH + H O 3 O3 ← 2 + + 6 CO ( g ) ← → 3 −CO2 (aq 2aq ) + H O ← → H CO ) H CO2 (aqa) H pK 7 2− − − 2 a 2 2 3 + 2 and potassium or sodium bicarbonate. main CO2 (aqK)4+ H2OThe ← → H CO ( aq ) K 7 CO3 pK 2 − − HCO 3 CO + H ← → HCO + a 2 3 3 + a + pKa −3 9 CO + H ← → HCO − − a 3 3 K H CO ( aq ) ← → HCO ( aq ) + H ( aq ) 8 + − purpose of this buffer an alkaline and pH = 6.35 solution contains the same → HCO3 + H H2 CO HCOpK 5 is2 to 3provide H2 CO 3 pH 3 3 3← HCOO + 3H O ←a→AtHCOOH + H(2pK O a2 )− the buffered a− pK 2 −CO (+g ) ← a CO 2(−aq−) + pK − a + 3pKaK−a − − → + 2 − carbonic − (H CO ). 2a consequence to from of amount of bicarbonate ( ) and acid CO pK HCO +fluctuating H2 2H−← →Kas H CO ( aq ) ← → HCO ( aq ) + H ( aq ) 8HHCO → pK + H ← H CO HCO 5 CO24(the aq )pH +6HCO → )HCO 7 prevent 3 CO pK 2 3 3 3 3 a HCO + ← → HCO 4 3 a 3 2 3 2 3 2O 3← 2CO+3 (aqCO 3 3 3 + 3 a Ka − − 9 CO3the +HHbrine. ← a→ HCO 8into 3 HCO3 (aq ) + H (aq ) − 2− acid or base influxes − 2 CO3 (aq ) ←→ K 2 − − + a 10 HCO−3 + OH ← →− CO 3 + H2O pKa − pK pK 9 (+aq2CO +H ← 2− − a → HCO3 pK − CO − CO )← → )− +3a → HCO63 + H + 5← HCO 5 H CO 3HCO The exact and vary 2 ( g→ CO3somewhat H +← 4H 3of H pK a ) + H levels HCO +3H2 CO ← H2 CO 2 CO H2 CO 3 HCO 3 3 a will CO32 (aq → 3 a 3 (2aq )pK − 7 3→ HCO + +3 K a K9 2O ← 2CO − 2− a CO(aq+) +6 H H←in HCO CO (g )← → CO2 (aq ) with temperature and pressure. H2 COan ) ←→ ( aq )→ 8 3brines Maintaining alkaline pHHCO environment formate 3 (aq − 3 3 2 −2 10 − HCO3 + OH − ← → CO 3 + H−2O − + −pKa 2− 2− − → CO HCO + H+ OH ← HCO HCO3 5 H2 CO 3 10 HCO +H with carbonate is important 3for 23 CO 3 2OCO + H O → 2HCO3pKa 11←→ K a CO2 (aq )buffer 2− −+ H O ← 3 + 2 2 H2CO3 (aq )3 the 7/+bicarbonate 2 (aq→ K − 6 CO ( g ) ← → CO ) 9 + CO + H ← → HCO a 6 2 2 CO ( g ) ← → CO ( aq ) 3 3 H CO ( aq ) ← → HCO ( aq ) + H ( aq ) following reasons: Figure 8 2 22 − 2 3 4 demonstrates 3 how a pure carbonate buffer 10 2 − HCO3 −+ OH − ← → CO 3 −+ H2O 2− + − )water 2− CO ( aq + Ca 2when ( aq ) → ↓ CaCO 12 works in a strong acid3 (iss)added. The 3 CO + CO + H O → 2HCO 11 CO + CO + H O → 2HCO 11 → H2CO Ka − 3 3 3 (aq 2) 2 7 3 CO2 (2aq )K+a26H2O ← CO )← → CO (aq ) CO32 − +3H + ← − 2 (g + 9 → HCO 2 3 − − 2 • Alkaline pH helps control corrosion (see Section carbonate reacts with added acid until all carbonate H2 CO → HCO ) +B6) H (aq→ ) H CO 8 −← [CO32 −] (mol/L) 3 (aq 3 ((aq CO 10 − HCO3 + OH → CO +2)H← O 7 2+ K + 2+ 2 aq )2+− H2O ← 2 3 (aq ) 2− 3 13 −2 − CO ( g ) + H O ← → HCO + H ( aq ) CO ( aq ) + Ca ( aq ) → ↓ CaCO ( s ) 12 3 3 2 2 3 • Presence of12 carbonate special is consumed. As long as there is still carbonate[ HCO left − ] (mol/L) = A x exp( B × ( aq (+provides aqH) O → ↓ CaCO CO+)3++Ca → 2HCO33(s) 11 CO3/2 bicarbonate KCO − 3 a 2 K a2 − − 2 − + ] (mol/L) 9 CO 8 ←( HCO 2 − pH remains[ CO protection COCOcorrosion (see Section B6) solution, around= the ‘higher 3 3 + 3 )HCO −[− K HHCO )2(← → (aq (aq aq ) in + ] −(mol/L) 2 −high → H→ CO aq 7 against A x exp( B × pHbuffer ) 3 aq 3( g 13 2 (aq2) + H7 2O2 ← 3)(+ CO aq H O → ( ) CO ) +H)HK2+CO OH← → HCO +CO H+OH 3 (aq)← − O −← K 10 + 2 2 3 HCO + → CO + H 2 2 3 2 − 2 + − = A − 3 [x 2] (mol/L) − → HCO + H (aqa) 2 − 13 exp( Bcarbonate × pH ) HCO ( gCO ) +2HCO H Odecomposition 3 ) + Ca H2(CO aq33)(aq → ↓ CaCO ) 3[[)HCO lower formate rates level’ (10.2±1). is consumed, H 122OCO 2→ 3 ]soon as the ) ← → HCO + ]H×−+[](HCO aq)As 83← CO 3pH+ helps CO 2 + H 11• Alkaline 3 2( aq 3 (s 3K (aq (mol/L) Ka 14 2− − = + 3 − 2 9 CO + H ← → HCO + − (see Section A13) pH drops rather quickly down to the ‘lower buffer level’ 3 − 3 )[+ P H O ← → H CO ( aq ) [ ] (mol/L) − − 2 (aq 2CO 7 ] [ ] CO × H HCO CO 3 2 2 3 2 3 K a ( g← K+ 2 −K − 2 − 10 + − K a −+ +CO → CO + K++2aHCO 14 =O = A x−exp( B × pH )is available +OH 132HCO +CaCO H− 32]−O ← + H (aq (aq − )it remains (aq HH (→ aq )3 9 ← HCO − as long as bicarbonate CO38 of ( aqcarbonate ) +HCa → ↓)HHCO (CO s3→ ) +← 12 • Presence /3)[bicarbonate helps limit ] ×2 [→ H HCO ))+3where H +(3=2aq 2 CO3 (aq 8← H HCO PCO [CO 32 −] CO +− CO → 2HCO3 3 − ] ] (mol/L) 113→ 2 3CO 3 (3aq 3 OH − CO32 −to HCO 3− pH log2[K+HCO −Hlog 15 2O 3 PCO + log [HCO 14 K = − 2 2 − − − 2 − − − amount of formate2 decomposition A13) with3 the [COKK3− log ] (mol/L) [COto ]carbonic [OH − ] [C [HCO3 ] OH acid [HCO ]+ added H2 SO4 pH PCO react + log 15 Section CO3for conversion HCO 3 K aP−−CO+2 OH+(see − K + 3 K3a2=− +− log − 2=− A x exp( 2− −−← −a +− CO 10 HCO → H) ← O B 9 CO + H ← → HCO + 8 (aq 2× +pH ) 13 CO ( g ) + H O ← → HCO + H ) 3 2 H CO ( aq → HCO ( aq ) + H ( aq ) 9 3 3 − CO + H ← → HCO − − 2 2 2 3 [ ] [ ] 2 − − • Alkaline pH helps stabilize polymers and other acid. drop below this second buffer [OH − ] [CO ×3 HCO 2 −3 H−Hlog 3 (In aqorder )2+− Cafor (pH aq−)to → CaCO ] (mol/L) [ − ]12 −3− 2CO 3 (s) ] 2HCO 11 [CO↓ ] [HCO [HCO H2 SO4 pH3= +−KCO log P→ +3 log 15 CO HCO 3 COOH +3H O 2O 3 −3 HCO 14 CO =2 K+10 CO HCO 3 3 3 → 3 + OH ← 3 level,2 an 3acid needs 2− additives (see Section B5) to be added that is stronger than the 16 0 . 02 × P PCO16 f K [CO ] (mol/L) 2 − − + a 2 3 0. 02 × P← − K + 9 + − 2− CO + H → HCO f 2 + = A x exp( B × 3 3 13 CO ( g ) + H O ← → HCO + H ( aq ) [ ] [ ] − − 2 2 − − − 2 − − − • Presence of lowers risk H S gas carbonic acid, which is formed. As any CO gas influx × HCO H12carbonate − − of 2aq − into 3CO −aq ) + the ( Ca ( ) → ↓ CaCO ( s ) 2 2 3 − − 2 2 2 − [ ] [OH − ] 2 −[CO 3 3 2HCO 11153 + OH10CO [HCO (mol/L) [HCO H32]SO CO 3 pH log P→ + log HCO 3 HCO ← → CO2 3+K −H++2log HO2O 2OH − 14 = K 10 − CO3 3 =+−CO 3 +3H ]O 4 CO 3 ] [ HCO HCO OH ← → 2− 2 − CO 317 [CO3 ] ( m − 3 2 [ ] [ ] CO + OH = 0 . 02 × P ( mol / L ) − − 2 − 2 release (see16Section solution fdissolves and converts [CO3 ] ( mgto 3buffered 17 CO [+COCO [OH .→ 02 × Pthe ( mol / L ) ] (mol/L) / Lcarbonic ) = 1200 × Pf PCO 2 0A6.2.3 . 02 × Pfon next f 2HCO 3 ]++ [CO H 2]O= 0 11 Kpage) 3 − 33 +2 2H− O ← + − = A x exp( B × pH ) 2 + 2 − − 13 − 2 − − − CO ( g ) + → HCO + H ( aq ) − • Presence carbonate improves well by aH CO− 2][HCO influx therefore not capable − −↓ CaCO (sacid, aq10 ) +3Ca ( aq3)OH )2 − +3[H[HCO − ][× ] 3 ]is[HCO − [ 2 −of ]pulling [) = the ]control pH = of − log K −12log P2CO +COlog 15 HCO 3 [(2HCO 3CO (mol/L) HCO +→ OH ← → 3 3 ] 2 − H2 SO4 [CO OH 3 ] ( kg [CO32 −] ( kg / m3CO 1. 2 × Pf HCO 0CO [K3HCO 18 14 = 3 2]O= 30CO 18 3 2 − [CO 2 −]+ [OH −] = 0.202 2−−[3 2+ [CO ] (buffer ×A6.2.2 Pf ( mol / L)3)+] =Ca − 2HCO −pH much mg / L ) = 1200 × P sequestering of CO (see Section on below level. − ) this second 2s 0 . 02 × P 3 2 2+ CO 16 H O → 3 f 11 17 influx CO ( aq ( aq ) → ↓ CaCO ( 12 P f 3 + CO 2 3 CO + CO + H O → 2HCO [ ] (mol/L) 11 3 CO32 3 CO 3 2 3 − K2 + + ( g ) + H− O ← = A x2 −exp( 13 this page) 2− − B × pH ) 2− − − − [H−CO ]2× [HCO 3 2] → HCO3 + H15 (aq) pH = − log[ KHCO − ] (mol/L) ] (mol/L) [HCO ]] 3) = 1.22−OH − log PCO +[CO log[2CO CO3 HCO 3 [ 2−[]CO 3 ] 2 − 2 − − 3( kg32/ −m 2 + − − ] K 14 = K +− 3protection [ ] ×x=Pexp( HCO = 0 −P2 +](=mol 2[×OH 18 2 −19 [ A6.2.2 Buffer against CO [CO=2/3 Linflux ]A)(ppb 17 B.42 [ ] [ ] f )= 0 3 CO + OH = 0 . 02 / L ) 3 CO ( mg 1200 ×× PpH ×f Pf) 0 CO3 2− CO ( aq ) + Ca ( aq ) → ↓ CaCO ( s ) 13 12 (3g+) f+CO H22O+) ← → HCO ( aq ) 16 0. 02 × Pf − +(H H O → 2HCO − 3 11 3 ( aqCO )CO +2 Ca (3aq → ↓ CaCO s ) 3 12 P3CO CO 3 [ ] 2 3 CO3 (pp [OH ]3= 0 19 [ HCO 3 ] (mol/L) 2 2− − fluids is the The main reason for loss of pH control in× [oilfield of conventional 2− 2− − − 2 −cause [of− acidification − major [The ] (mol/L) − [KHK−−+]log ] 2[HCO CO 2HCO 2 −[ 3+ 3 ] (mol/L) 3 CO [ ] − log+ [ ] [ ] = [CO ]/R (mol/L) 2 − 20 2 − 15 ] OH [ ] H SO OH CO CO HCO pH = − log P HCO CO HCO − 14 − 3 2 + [ ] − 3 3 K × pH ) P3= A(xkgexp( + 4Pf 12. 2)× dioxide 3 3 CO 3/ mB) ×=pH =)S.0HCO 3 =←→ 133 gases [= ]2-(=mg g. 02 )as +×13 H H3O[ (← 17influx of [acid ]+ [OHCO ] =18 CO PK2[fOHCO (and mol L12 /3is Lexp( )influx = B1200 3 /] +aq (aq + Ca → ↓ CaCO (sA) x(mol/L) such CO HCO These completion carbon gCO)3++CO Hare → HCO + H)[[HCO (. aq 2 (0 2− or×diffusion 3 brines ] ×))[HCO 163 − ]3( aq 0 023−3)×]-](mol/L) PCO 20 2( 2 Hboth 2 P HCO f [CO3 3 ]/R[ HCO [3−CO ] (ppbf )= 0. 42of [CO32−] ] (mol/L) × Pf [OH −] = 02 19 CO 2 3 14 = K − 2 weak acids with a pKa higher than the pKa of formic acid.P gas (CO−2) into the from the rock ] (mol/L) 2 − surrounding − − 2 − wellbore − [ CO − 2 − − 3 − [ + CO K − CO ] [HCO ] 2[−CO OH P [(HCO + log [HCO3 ] = 0 15 [ +] [-pH = −− ]log ) = 13. 2 ×/ LP3[)fCO 20O ← = A3x]exp( H B 2×SO pH4 ) [OH − ] ()kg 18 3 ] 3 / mHCO 13 K −21log ]H H[OH =[HCO 3(aq −2− 3 + COCO [CO332 −]++CO 22 g )−3+ 2 17 → HCO formations: 2− [CO3 ] ( m H. 02××HCO −3 2 − − − ] = 0. 02 × Pf− ( mol [ ] [ ] 2 − − ] [ (mol/L) 16 0 P × H HCO [HCO ] = [CO ]/R (mol/L) HCO 20 3 [ [ ] f ] =15 CO ) = 0 . 42 × P [ OH 0 CO 3 ] (ppb [ ] 3 3 14 K =19 − [ ] OH [ ] H2 SO4 CO HCO pH = − log K − log P + log HCO CO HCO 3 f 3 14 K = 3 3 3 pf = Vol (3mL) /5 21 CO [HCO3 ] = 03 PCO 22 PCO 2[OH −] = 0 − 2 − 2− 2 + − [CO32 −] ( kg ] = 02− − 18 3 − ]− [HCO 2−− [/H − L )] × [HCO [2CO ] ([mg− /−L] )[= 1200 22−− × P [OH +.−02 .+02log ×2-P]/R − − ](mL )[/5 − =fCO0[CO f ( mol 3 ]K = Vol 20 [CO ]×3 PHCO ×3-]]P=pH ] (ppb ]] 4 [pfHCO OH[HCO CO− 3−]2 3−[CO3HCO [HCO ] H SO CO HCO = [−CO log log 15−] = 17 ) = 0 . 42 [OH 0 pH16 CO 19 [ [OH − ] f [OH 14 =−[CO K K(mol/L) 2 ] OH H SO 3log 2− P 3 3 CO 3 = 23 −3 log + log 15−0[HCO CO f 3 2 4 CO 22 3 ]= 0 3 3 3 3 [OH 21 [HCO3− ] = 0 16 3 ] =P0. 02 × Pf ( mol / L ) 0 . 02 × P CO 2 PAGE 5 f V E R S I O N 4 18– 0 9 /[HCO 1 3 ] = 02 − I( kg O N2/−A 63) = 1. 2 × P [SCOE C2 −T]CO − − 2−m f 3 [CO ]+ [OH ] = 0. 02 × P ( mol / L ) ] ( mg / L−) = 1200 [HCO3-] = [CO3172-]/R (mol/L) 20 [CO 32×−]Pf [HCO3−] [COH22−SO 3 3 ==0Vol OH/ −L )3 [CO ]× P) /5 (mL pH = −f log K −23 log PCO +[CO log−2]p−[=fHCO 15 HCO ] (pp 4 3 OH − 3 3 19 ] 0 . 02 ( mol − [ CO ] 2− 3 f − 22 [ OH ] = 0 − 3 21 [ ] HCO = 0 [CO32 −] ( mg / L ) = 1200 × P3f 16 0. 02 × Pf 16 ] = 0. 02 × Pf ( mol + [OH / L/)L ) 3 17 ( mol 24Pf[CO3 []HCO 3 ]= 2− − 0. 02 × 3 . . A exp (B pH ) [CO3 ] ( kg / m ) = 1. 2 × Pf [HCO3 ] = 0 18 2− 2− −2 − pf =3[2-CO [HCO3-] = [CO ]/R ((mol/L) 20-10 Vol −/5 ] (ppb )= 0. 42 ] 2[ −CO × P[fCO 2 −] ( kg[CO ] =]−[=0]OH OH 00−.]02 ××PPf 2((−25 mol // LL−))A−]==3.894 23 ]mL2[)CO 3 10 [ ] = 0 3OH 17 3−]19 [ ] [ / m3 3)×=P1. 2 × Pf HCO 0 + = . 02 mol CO ( mg / L ) = 1200 18 − 21 [HCO = 0[CO22 3 [CO 2×−]P(fmg 17 0. 02 3/ L ) = 1200 [16 ]3=×0P. 02 × P ( mol / L ) 3 CO f ]+ [OH 3 2 2 1 2 1 2 1 2 1 2 2 2 1 2 1 21 1 1 2 1 2 1 2 1 2 1 1 2 1 2 2 2 1 2 1 1 2 1 2 2 1 2 1 2 1 2 1 2 1 1 2 1 1 2 1 1 2 1 2 1 2 1 1 2 1 2 1 2 2 2 2 1 2 2 2 2 2 2 2 2 2 2 2 2− • 2 2− 2 FORMATE TECHNICAL MANUAL C AB O T pH behavior of carbonate / bicarbonate buffer when adding strong acid 12 11 pK a2 10 9 8 pH 1 1 2 2 1 3 3 2 4 43 5 5 4 6 65 O aq) O3 (s) q) 6 7 7 8 7 8 9 9 8 10 109 11 10 11 12 12 11 13 13 12 14 13 14 15 15 14 16 15 16 17 17 16 18 18 17 19 18 19 20 − OH 20 19 21 20 21 22 22 21 23 7 pK a1 pH = −6log [H +] pH = − log [H +] 5 aH + pH = − log (aH + ) 4 log (a ) aH + pH = − + H [H +]+ K a pH = −3− log pKa HCOO + H O ← → HCOOH + H O 0.6 3 K 0 0.2 0.4 2 1 1.2 1.4 1.6 1.8 2 pK0.8 HCOO − + H 3 O +←a→ HCOOH + H2 O a Fraction of buffer consumed aH + pH = − log (aH + ) pKa2 2− − − 2− CO32 − pKa2 HCO 3− CO32 − +− H +← →KHCO 3− a pK+← of strong acid a2 +H O pKAddition HCOO + → HCOOH + H O a CO pK HCO CO + H ← → HCO 3 2 3 3 3 3 a2 pKa1 − − + → pK HCO H +The ← H CO HCO H CO Figure pH in water buffered with carbonate as a function of added acid 3 a 3 − +4 2 3 2 3 (H ). The x-axis shows the fraction of pK 1 − a1 → pK HCO2 3− + H++ ← H CO HCO H CO 3 a 2 3 2 3 pK 2− − − 1 the that by the added acid. As be seen, CO3 carbonate pKcan HCO 3buffers twice, first at pH = pKa2 = 10.2 (upper CO3 buffer +H ← ais2→consumed HCO 3 a2 buffer level) and then at pH = pKa1 = 6.35 (lower buffer level). If the added acid is carbonic acid (from CO2 influx), the pH CO2 ( g−) ← → COa2 1(aq ) − + pK can drop lower than pKa1 = 6.35. → pKa1 HCO(3gnever H ← HCO3 H2 CO 3 3 CO )+← → CO much (aq H ) 2 CO 2 2 carbonic acid being present in the brine. With a large influx of CO2, the pH drops down to the lower buffering pKa level (pH = 6.35) where it stabilizes. Measurements of CO2 (aq ) + H2O ← → H2CO3 (aq) (7) pH in formate brines exposed to various amounts of CO2 (aq ) + H2O ← → H2CO3 (aq) 2− CO2 have confirmed that pH never drops below 6 – 6.5. − COK3a pKa HCO 3 − + H2 CO3 (aq ) ← → HCO ( aq ) + H ( aq ) (8) This pH is still close to neutral, meaning that this brine 3 − (aq ) a→ H CO COCO (aq ) + H2OK ← 2 (3aq H ) + H +(aq) −→ HCO 2 2 3 (aq ) ← 3 system cannot be ‘acidified’ to any great extent by = 6.35 pK HCO H CO K a3 −2 a2 − 3 CO32 −+ H + ← exposure to CO2. However, carbonic acid and a small K a→ HCO3 − + CO3 + H ← → HCO3 − athe original pH of +the receiving brine Depending onK amount of formic acid are also present. H2 CO3 (aq ) ← → HCO3 (aq ) + H (aq) system, dissolved CO22 −remains in the brine as either • Unbuffered formate brines: The pH of these brine − − HCO23−−+ OH+ ← CO 32 −− + H2O K→ a(H CO − carbonic ) 3in+equilibrium with dissolved CO2 systems responds in a similar fashion to halide brines CO3 ++ HOHacid ← →2 HCO 3 HCO ← → CO H O 3 3 2 gas or bicarbonate (HCO3–), according to reaction 8. This when exposed to CO2 gas. However, they do have a − more CO gas enters into 2− is demonstrated in→ Figure 5. As higher initial pH, and the pH drop will be limited as the CO + CO + H O 2HCO 2 2− 32 −− 2 − HCO OH2carbonic ← → CO +concentration H2O3 − 3++CO 3 2HCO the acid builds up and pH formate brine is a buffer in itself (pKa = 3.75). At such CO → 3 brine, 2 + H 2O 3 2− 2+ drops and allows unbuffered brines to acidify. low significant = − log [H +] amount of corrosive formic acid 1 pH apH CO ( aq ) → ↓ CaCO 32 −( aq ) + Ca 3 (s) CO32 −( aq ) + Ca 2 +( aq ) → ↓ CaCO ( s ) − 2 is present in the fluid. If there is any chance of an acid 3 − [CO3 ] (mol/L) CO + CO 2 + H 2OK → 2HCO − 2 B × pH aH + =) − log (aH + ) 2− = A xgas exp( pH the CO g ) + Hdifferent →brine HCO3systems + H3 + (aq)in Figure 5 react The23 (three influx, use of unbuffered formate brines is [ (mol/L) −]in CO 2O ← 3 − K ] [ (mol/L) + HCO = A x exp( B × pH ) 3 CO22(following g ) + H 2O ← →toHCO (aq) − Ka + − 3 +H − the ways a CO influx: highly discouraged. 2+ ] [ (mol/L) pKa 3 HCOO + H O ← → HCOOH + H O HCO 2 3 2 CO3 ( aq ) + Ca ( aq ) → ↓ CaCO3 (s) 3 [H +] × [HCO 3 − ] 2− [CO ] (mol/L) = [H +] × [HCO 3 −divalent K• Conventional − against H2S influx K] brines can not be3 − pK = A xA6.2.3 exp( B ×Buffer pH2 −) protection − HCO2O2 ←→ HCO3halide + H + (aq ) KCO=2 ( g ) + P pKa CO3 + H +←a → HCO 3 4 [ HCO 3 ] (mol/L) buffered with because the Influx into− a wellbore is often P carbonate / bicarbonate − − accompanied by 2 [CO 32 −of ] CO [ ] [ [ ] OH − CO32 − HCO 3− H SO OH CO HCO pH = − log KCO−2 log PCO + log[HCO 3 − ] pK 2 4 3 − a −+ (H − − → HH22SCO corresponding metal , ZnCO ) 2 − HCO − hydrogen sulfide S). is3 a[OH weak 5 2 −] HCO + − P + carbonate [CO ] acid [COwith a pKa of 3 + H ]← [HCO ] pH = [−Hlog − log log[HCO 3 (CaCO 3 OH 3 CO3 2 H2 SO ] × [KHCO 4 3 3 3 3 ] CO = K precipitates out of solution resulting in formation of around 7. This means that at a pH of 7, equal amounts PCO solids fluid. These of6hydrogen sulfide (H2S)) and hydrogen bisulfide 0 . 02 × Pinf the2 clear packer / completion − CO2 ( g ) ← − → CO2 (aq 2− − [CO–3)2 will ] be [OHAt− ]higher [COpH, more [HCO OH–−6), and [HCO 3 −low ] pH (2 H2the SO4 brine. = ×−Plog K − log PCO +alog CO3 HCO 3 (HS 3 ] 0pH . 02 divalent naturally present in f brines have 2− 2− − [CO ] ( mg [CO3influx ]+ [OHof ] =CO0.202 × Pf ( mol / L )on the partial pressure of the , dependent HS32– −will be/ Lpresent ) = 1200and × Pf at lower pH more H2S will exist. 2− − [ ] ( mg /unless [CO ]+ [OH ]lowers CO3, further = 0. 02 ×the Pf ( mol / L ) CO L ) = 1200 × carbonate Pf 3 pH. The CO2 partly converts to Therefore, the buffer in the formate 2− 2 − 2− 3 . 02 ×]P=f 0 [CO[03HCO ] (mol/L) [ ] CO ( kg / m ) = 1 . 2 × P f 3 3 carbonic acid 7),)which is very corrosive. brine by large influxes of CO2, the = A(Equation x exp( B × pH 2 − is overwhelmed − CO ( aq ) + H O ← → H CO ( aq ) 3 7 − 2 [CO3 ] ( kg / m [HCO ) = 1.22 × Pf 2 3 ] (mol/L) [ HCO 3 ]= 0 3 2− carbonate buffer traps and retains this toxic gas in its [CO ] [CO32 −]+ [OH −] = 0. 02 × Pf ( mol / L ) ( mg / L ) = 1200 × P 3 f • Buffered formate brines are capable of buffering less harmful form, Knamely bisulfide, HS–. − a [CO328−2]−(ppbH)2=CO03 .(42 [CO)3+2−H] +(aq) aq )×←P → HCO [OH −] =− 0 3 (aq f 2 − 2 − − [ ] large of CO2. Unless the influx is unusually ]0= 0 CO3 ] (ppb ( kg /)=m0). 42 = 1×. 2P× Pf HCO] =3amounts [CO [CO3 ] [[OH 3 Kf a 2− − + large, The fact that any H S is converted to HS– in buffered 9 CO + H ← → HCO - the brine 2- maintains a pH around the upper buffer 3 3 2 2− − [HCO 2 − ] = [CO− ]/R (mol/L) − 3 HCO 3 [CO 3 ] [HCO3 ] [ ] [ H SO OH CO CO 22 4 3 3 level3(pH = 10.2), formate brines does not mean that the gas is [HCO ] = [CO ]/Rwhich (mol/L)is high enough to prevent 3 [CO32−] (ppb )= 0− . 42×− Pf [CO32−] [OH −] = 0 2− CO2 ( g ) ← → CO2 (aq ) 2 1 1 2 (6) 1 2 1 2 2 CO3 1 HCO3 1 2 2 1 2 [HCO3P-−] A= G0E 62[HCO SECTION A6 [HCO33 ]] == 0[CO3 ]/R (mol/L) − [OH ] = 0 [CO32 −] ( mg / L ) = 1200 × Pf [OH −] =− 0 2− ]= 0 HCO 3 2− /L) [[CO 3 2 −] = 0. 02 × [P f ( mol ] ( kg / m3) = 1. 2 × P CO − 10 HCO3 + OH ← → CO 3 + H2O 11 CO 3 + CO 2 + H 2O → 2HCO3 12 CO3 ( aq ) + Ca 2 +( aq ) → ↓ CaCO3 (s) VER S IO N pf = Vol (mL) /5 pf = Vol (mL) /5 2− 4 – 09 / 13 − 2− 2− 2− 2 2 − − HCO 3 H2 CO 3 SECTION A: CHEMICAL AND PHYSICAL PROPERTIES C A B O T pH in various brine systems as a function of CO2 influx volume 12 11 Buffered formate brine 10 pH>6.35: CO2 mainly converted to bicarbonate (HCO3-), which does not promote corrosion 9 pH 8 Unbuffered formate brine 7 6 pH<6.35: CO2 mainly converted to carbonic acid (H2CO3), which promotes corrosion 5 4 Calcium bromide brine 0 50 100 150 200 250 300 350 BBL gas influx / BBL buffered formate brine ] / 70°F, 1 atm) pH = −(2% logCO[2H +21°C 400 450 500 1 Increasing 2 time of pHCO=2−influx log (aH + ) aH + Figure 5 pH as a function of CO2 influx in a typical halide brine, an unbuffered formate K brine, and a buffered formate brine. pKa 3 HCOO − + H 3 O +←a→ HCOOH + H2 O pK − 2− CO3 + H +←a2→ HCO 3 4 pK − be+ seen As can afrom → H2the pKa HCO CO3graph in Figure 5, the decrease 3 +H ← in pH of one unit is not really a good measure of how much carbonate buffer is present in the brine, CO2 (therefore g )← → COthe ) capacity of this buffer. Cabot and true 2 (aq therefore uses the actual carbonate concentration as a measure of the capacity of the buffer rather than the scientifically defined ‘buffer capacity’. scavenged and made permanently safe. If the buffer 5 was to be overwhelmed by an excessive influx of CO2 / H2S, then H2S gas would come back out of solution when pH dropped to below around 7.0. CO2 gas would 6 first be present in equilibrium with the bicarbonate in the brine at a lower pH (6.35). It is therefore important to remove any HS– contamination from used field + = − log 1 neverpH muds, and lower the[HpH] or let the buffer deplete 7 in a formate mud or brine that has been exposed to H2S 2 aH + – pH = − log (aH + ) without first checking if it is contaminated with HS . If K + − there is any corrosion H2S 8 3 concern HCOOabout + H 3HO2S-related ←a→ HCOOH + Hthen 2O scavenger should be added (see Section B6, Compatibility with Metals and Section B5, Compatibility with Additives). 9 pK − 2− CO3 + H +←a → HCO 3 4 + 1 1 1 2− CO3 − HCO3 H H CO2 (aq ) + H2O ← → H2CO3 (aq) In alkaline brines that are buffered with carbonate / bicarbonate buffer, the following equilibrium exists Ka − bicarbonate: + and H CO3 (aq )carbonate ← → HCO pKbetween 3 (aq ) + H (aq ) a 2 K 2− − CO3 + H + ← a→ HCO3 (9) 2− − pKa = 10.2 CO3 HCO 3 1 2 2 2 pH = − log [H ] pK − A6.3 Buffer addition and 10 amaintainance → H2 CO3 2 HCO3 + H + ← 5 pH = − log (a pKa2 − 2− − CO HCO + OH HCO ← → H2O pKthe 3 H In is2+CO typically lost by exposure 3 a 3 field, 3 aH + carbonate H Whenever formate brine is used in the field, it is important to influx of acid gas. As acid gas initially enters the K − 3 acidHCOO + H 3 O +←a→ HCOOH + H2 O to maintain the ability of the buffer to resist influxes. brine, (CO32–pK ) ais gradually converted to − 2 − carbonate CO + CO 2 + H 2O → 2HCO3 11 6 CO ( g ) ← → CO ( aq ) – + 3 2 2 In order to do this, both buffer capacity and total1 buffer (HCO3 ), whilst pH remains at around the ] pH = − log [Hbicarbonate pK 2− − −2 − 2− 2+ concentration need to be monitored and 4maintained. upper buffer (pH = pKa↓ =CaCO 10.2). all CO(3sWhen HCOcarbonate CO3 + H +← a → HCO 3 CO3 ( aq ) + Calevel ) → ) 3 2 a(H aq pH12= − log (aH + )3 + is converted, the buffer loses its ability to maintain pH. pKa − − [CO32 −] (mol/L) → H2 CO pK HCO3 + H + ← HCO3 5 H2 CO − a + K 3 Ka 3 A6.3.1 Buffer capacity = A x exp( B × carbonate component the buffer system is −now 13 − + H3The CO g )→+ HCOOH H2O ←→ H pK (aq 3 HCOO O +← + H2 O HCO3 +of a ) 2 ( [ HCO 3 ] (mol/L) In buffered brine, the referred to as ‘overwhelmed’ or ‘swamped’ and has no CO2 (aq ) + Hit2Ois← →carbonate H2CO3 (aq)component 7 formate 6 alkaline CO2 ( g ) ← →2 −CO2 (aq + − buffer pH at the upper buffering of the buffer that provides buffering at the level. pK capacity 2− − + )more ] ×3[−HCO 3to ] CO3 pK HCO CO3 + H ←a →[HHCO 4 14 = K pH of 10.2. Bicarbonate is mainly added in order to Any further influx of acid gas can anow easily lower pH3 PCO 2 Ka − + pK − − H2 CO (aqcarbonate ) ← → HCO (aqis ) +aHfunction (aq balance 8alkalinity of 3the as3 pH down the by3 a → to H2 CO HCOprovided 5 ) HCO3 + H + ← H2 2−CO 3 lower buffer level ( −pKa = 6.35) − −3 [CO 32 −] OH [ ] pH = − log K − log P + log HCO 15 CO3 HCO 3 CO 3 of the carbonate-to-bicarbonate ratio. The carbonate the bicarbonate. (See Figure 5.) K 2− − + 9 CO3 +isHtherefore ← a→ HCO CO2 (aq H2O ← → H2CO3 (aq) concentration alone the 3true7measure of)+CO 6 → CO2 (aq ) 2 (g )← the brine’s buffer capacity. It0.is to notice that whilst pH of a buffered 16 02important × Pf Ka − + formate brine is a function of the ratio of − 2− − H CO ( aq ) ← → HCO ( aq ) + H ( aq ) 8 2 3 3 10 HCO3 + OH ← → CO 3 + H2O 2− − The scientifically correct definition of buffer capacity concentrations of carbonate [CO32 −] ( m 17 [ ] [ ] CO + OH = 0 . 02 × Pf ( mol / L )and bicarbonate, the K 2− − 9 CO3 + H + ← a→ HCO3 3 is: “The number of moles of acid or base necessary toCO2 (aq )+ H2Ocapacity the buffer to maintain pH around 10 – 10.5 ← → H2COof 7 3 (aq ) − 2− [CO32 −] ( kg [HCO3−] = 0upon the actual carbonate concentration. change11the pH of liter of solution unit”. 18 depends COone →with 2HCOone 3 + CO 2 + H 2O 3 1 + ) − 1 2 2 1 1 2 2 1 1 1 2 2 1 2 10 12 V ERSION 13 4 2− 3 − 2− HCO3 + OH − ← → CO 3K a + H2O − 1 H2 CO3 (aq ) ← → HCO3 (aq ) + H +(aq) 8 CO ( aq ) + Ca ( aq ) → ↓ CaCO3 (s) – 2+ 0 9/ 13 11− K2 −a2 −] = 0− − [ OH 2− + 9 2 −+ COCO19 HCO ]→(mol/L) CO 3 + H [← CO → 3 2HCO3 3 3 2 + H 2O SECTION A6 K CO2 ( g ) + H2O ←→ HCO3 + H + (aq) 12 [H +] × [HCO 3 − ] = A x exp( B × pH ) − 2] (mol/L) [ HCO [HCO ] = [CO ]/R (mol/L) 3 20 2+ 3 CO ( aq ) + Ca− ( aq−) →3 ↓ CaCO 3 (s) 2− 10 2− 3 HCO3 + OH ← → CO 3 + H2O K − + [CO32 −] (mol/L) PAGE 7 [CO32−] (pp C AB O T 13 12 11 10 9 8 pH 7 6 5 4 3 2 4 pK − 2− CO3 + H +←a2→ HCO 3 5 pK − HCO3 + H + ←a1→ H2 CO3 2− 7 7 8 8 −+ + a1 − K a−1 a 1K H82 3CO ← → aq )H++(H3aq aq H)2K CO )HCO ← → ((aq H2 CO (aq )← → HCO ) +HCO ) ))+ H (aq) 3 (aq 3 ( 3 (aq 3 (aq 6 CO2 ( g ) ← → CO2 (aq ) 7 10 10 CO2 (aq ) + H2O ← → H2CO3 (aq) MANUAL K a−2 2 2K − a2 + − 2 − 2 − + + Ka Titration 9 + HCO ← +→ H HCO ←3 − 9 9curves COCO → HCO 3 → HCO3 3 3 3+ H ← − Phenolphthalein endpoint 2− − 2− −2 − − − − 10 HCO + OH ← CO +endpoint HCO O + H2O HCO + OH ← → Methyl HCO → COorange 3→ 3 +3OH ← 3 3+ H2O 2 3 Water + standard buffer KFo + standard buffer 2− − 2 − 2− CO + CO CO+ H+ OCO + 2HCO H 22HCO O → 2HCO3 CO11 → 11 11 3 CO 2→ 3 + 2 +2H32O 2 3 3 Ka1 − + H2 CO3 (aq ) ←→ HCO3 (aq ) + H (aq) 22−+ 2 + 2+ 2−2− CO ( aqCO ) + Ca ) → ↓) CaCO (↓s)CaCO3 (s) ( aq()aq + → Ca (↓aq → CaCO 12 12 CO12 3 (3aq ) + Ca3 ( aq ) 3 (s3) Ka2 2− − + CO3 + H ← → HCO3 2− 2− ] (mol/L) [CO32 −] (mol/L) [CO[3CO ]3(mol/L) − + − K− + + K K x exp( A×xpH = A= xAexp( B=×BpH )e CO ( g ) + H O ← → HCO + H ( aq ) CO ( g ) + H O ← → HCO + H ( aq ) 13 13 CO13 ( g ) + H O ← → HCO + H ( aq ) − − 2 3 2 2 2 22 3 3 ] (mol/L) [ HCO [ HCO 3− ] (mol/L) ] (mol/L) [ HCO 3 3 8 9 − -0.2 11 CO + CO 2 + H 2O → 2HCO315 15 + − − 2− HCO3 + OH − ← → CO 3 + H2O -0.1 0.0 0.1 14 14 10 -0.3 − CO3 pKa2 HCO 3 ( aq ) + H O ← → H CO ( aq ) CO ( aq ) + H O ← → H CO (aq) CO2CO (7aq ) + H O ← → H CO ( aq ) 2 2 22 F O 2R2 M2 3A T3 E− T 2E C 3H N I C A L pKa1 HCO3 H2 CO 3 [−H]3+−] ]× [HCO 3 − ] × [HCO [H +[]H×+[]HCO K= = 0.2K = 3 0.3 K 14 PCO 2 PCO P CO 2 2 0.4 0.5 1 pH = − log [H ] 2 aH + 2 − pH = − log (aH + ) CO3 ( aq ) + Ca 2 +( aq ) → ↓ CaCO3 (s) 12 Figure− 6 Titration curves for buffered water and buffered potassium formate. Both fluids 2− × Ka 0. 02 16 0. 02 Pf contain the same amount + 16 16 0. 02 × P×f P[fCO ] (mol/L) pK HCOO + Hcarbonate HCOOH + H2 Obuffer (17.8 kg/m 3 3 / 3.75 − K a 3 / 6.25 + 3 O ←→ = Albs/bbl x exp( BKHCO × pH )3). The of added /­bicarbonate 13 CO2 ( g ) + H2O ←→ HCO3 + Hlbs/bbl (aq) K2CO3 and 10.7 kg/m − ] [ (mol/L) HCO 2 − 2 − − 2− 2− − 3 2 − 13B-1 −alkalinity phenolphthalein and methyl orange endpoints from the standard API RP titrations are shown. [CO/ 17 17 [ ] [ ] [ ] [ ] CO + OH = 0 . 02 × P ( mol / L ) CO + OH = 0 . 02 × P ( mol / L ) No methyl [CO[CO ] ] ( mg 17 [CO3 ]3+ [OH ] = 30. 02 × Pf ( mol /L) f f 3 3( mg / L ) 2 −due to the formate orange endpoint the buffered formate brine / formic acid equilibrium starting to − 2− + − + pKa 2 can be− detected in [H ] × [HCO 3 ] pKa CO3 HCO CO3 + H ←→ HCO 3 − 2− 2− − 3− 2 [CO 14 K = [HCO /3 HCO3 ] = 0 [CO[CO ] ] ( kg 18 [HCO establish at a higher pH. 18 18 3 ]0=[0 3 3( kg / m 3 ]= P CO pK 2 − − pK HCO3 + H + ←a1→ H2 CO3 HCO− H2 CO 2− − − 3 [CO 32 −] [HCO3−] [OH − ] [CO OH H2 SO4 pH = − log K − log PCO2 +a1log[HCO 3 3] 15 CO3 HCO 3 A6.3.2 Total buffer concentration − 2− 2− − − total [CO)3= [CO[CO ] ] (ppb [OH = 0 [OH ]of = 0carbonate / bicarbonate buffer 19 ] = ]0amount 19 19 The[OH 3 3(ppb )= 0 The total buffer concentration in a brine that is available decreases by the amount of carbonate that CO2 ( g ) ← → CO2 (aq ) 2- -] =[HCO 2- 2--]]/R 16 / bicarbonate 0. 02 × Pf is defined as [HCO (mol/L) = [CO ]/R (mol/L) buffered with carbonate 20 [HCO ] = [CO[CO ]/R (mol/L) 2020 is precipitated. 3 3 3 3 33 2– the combined concentration of carbonate (CO3 ), pH = − log [H +] [CO32 −] ( mg 17 [CO32 −(H ]+ [CO OH −]),=and 0. 02any × Pf ( mol / L ) / L ) = 1200 × Pf bicarbonate (HCO3–), carbonic acid 3. Formate− decomposition increases buffer 2 3 − − 21 [ ] 21 [ ] HCO = 0 HCO = 0 21 [ ] HCO = 0 3 3 carbon dioxide in concentration 3 − the brine. If the a pH = − log (aH + ) (CO2) gas dissolved [CO32 −] ( kg / m3) = 1. 2 × Pf 18 H + [HCO3 ] = 0 total buffer Small amounts of− soluble carbonate and bicarbonate = Vol =) Vol CO2 (aq ) + H2Oconcentration ← → H2CO3 (aqhas ) been removed from p)f/5 /5 (mL) /5 pf =pfVol (mL(mL − − K + − 22 [OH = 0 [OH ] = 0 2222 can[OH ] = 0]as pKneed HCOOfluid + Hin ←a→ HCOOH + new H2 O buffer will a the reactions, to be form a result of formate decomposition if 3 Oother 2− − exposed 2− added to theKfluid. 19 the brine temperature 2 − 2is ] (ppb [CO32−] 0.an 42×extended Pf [+OH −] = 0 [CO ] = [0CO − . 02 ×] =Pfto0( mol )( mol .high 02 / L ) )=for a1 3 / L×/) PL[f CO 2323 [CO23 3 ]3= 0. 02 ×3 Pf ( mol H2 CO pK 2− − −3 (aq ) + H (aq) 2 − 3 (aq a → HCO + )← period of time (See Section A13, Thermal Stability). The CO3 pKa HCO CO3 + H ←→ HCO 3 3 2There ways in the buffer dominant decarboxylation reaction is reversible, and ] = [COconcentration ]/R (mol/L) 20 K 2 − are − which[HCO + three a 3 3 2 ] [CO3 2 − ] pK [CO[CO − + H+ ← − a CO → HCO 2 − ]3 2 − 3 − − ment3−of → Hcan pKuse: HCO + H ← HCO3 2424Hthe in a33formate brine establish­ equilibrium well a 2 CO3 be altered during field 2 CO [HCO ( mol / Lclosed ) ( mol / HPHT L) 24 [3HCO / .L )in 3 ] =[HCO 3 ] = . . ( mol 3 ]= . . . ( A exp ApH pH ) (B BpH )exp) (B decomposition A exp systems usually limits formate to a few -10 -10 • [HCO3−buffer ]= 0 •A = − − ) increases 2 21 A 3.894 =in3.894 103.894 10brine 1. Influx of−acid gas typical formate formulations. A =25 10•-10 2525 percent 2 H2O HCO OH ← → CO(CO CO ← → CO 3 )+ 3 + 2 (g 2 (aq ) concentration: pf = Vol (mL) /5 − B 2.193 =Determining 2.193 B = 2.193 22 B =26 [OH ] = 0 2626 A6.3.3 buffer concentration and capacity − 2− − − −] [ [ ] (10) For standard CO 3 + CO 2 + H 2O → 2HCO3 OH = 0 water-based mud filtrates, API RP 13B-1 [5] [CO32 −] = 0. 02 × Pf ( mol / L ) 27 27 [OH27] = 0 OH = 0 23 recommends that2 −carbonate and bicarbonate content 2− 2− CO2 (2aq → [CO − ) + H2O ← 2 + H2CO3 (aq ) ] ] = [0CO3 ] = 0 2828 [CO28 3 3= 0 CO + Caconverts ( aq ) → ↓ CaCOfrom Influx of )CO carbonate are measured by pH titrations. Alkalinity in the form 3 ( aq 3 (s) the buffer to 2 [CO3 2 − ] 2 − 2− − − − −2− 2− − − − pK a is OH OH CO CO bicarbonate. TheK carbonate concentration (buffer of content, content, and HCO [ ] (mol/L) pK apK OH CO CO HCO 3HCO 3 a content [ ] mol L ( / ) HCO = 24 3 3 3 3 3 − + 3 K − = A x exp( B × pH ) + . . a CO ( g ) + H O ← → HCO + H ( aq ) ( − ) exp A B pH H CO ( aq ) ← → HCO ( aq ) + H ( aq ) 2 2 3 capacity) therefore3 drops whilst the total buffer determined by the combination 2 3 2− of − [ HCO 3 ] (mol/L) − −a phenolphthalein − −] []HCO ] H SO [OH ]2−] 2−] [CO [CO[−CO [HCO ] ] [HCO [OH[OH ] P P 3 f H SO H2 SO4 3 3 3 3 -10 2 2orange 4 f4 concentration titration to an endpoint of pH3 = 8.2, and Paf methyl A = 3.894 •+10carbonic K a (carbonate 2− − 25 + bicarbonate + CO3 + H+ ← → HCO − 3 [ ] [ ] × H HCO 3 acid + dissolved CO2) increases by the amount of CO2 titration to an endpoint of pH = 3.1. K = B = 2.193 entering the PCO 2 brine. 26 − 2− − 2− − − − HCO + log H2O[HCO [OH formate ] = 0 OH − CO32 − HCO 3− In[CO 3 + ] [brines, [OH − ] of the [CO methyl 27 HCO3 ] theHdetermination pH =3 +−OH log K←→ − logCO PCO 2 SO4 3 ] 3 2 2. Influx of multivalent cations decreases buffer orange titration endpoint is complicated by the formate / 2− [CO3 ] = 0 28 concentration: formic acid equilibrium that is present at pH = 3.75 − 2− CO 3 + CO 2 + H 2O → 2HCO3 2− − 0. 02 × Pf ( pK a formic acid). This is illustrated in Figure 6. As can OH − CO3 HCO3 2− CO3 ( aq ) + Ca 2 +( aq ) → ↓ CaCO3 (s) − (11) be seen, the formate / formic acid equilibrium starts to 2 − − [CO ] [HCO3 ] [CO 2 P−] ( mgH/ LSO [CO32 −]+ [OH −] = 0. 02 × Pf ( mol / L ) [OH ] 1200 × Pf 2− 3 2 ) 3 f establish at a4=pH significantly higher than the methyl [ ] (mol/L) CO 3 − K + = A x exp( B × pH ) CO ( g ) + H2O ←→ HCO + H (aq) − 2 3 An influx of multivalent cations consumes the buffer orange endpoint. The fact that only one of the two ] (mol/L) [ HCO 2− − 3 3 [CO3 ] ( kg / m ) = 1. 2 × Pf [HCO3 ] = 0 by precipitating out insoluble calcium carbonate. standard titration endpoints can be determined in a + − 3 4 5 6 1 2 7 3 8 4 95 106 11 7 12 138 9 14 10 15 11 16 12 17 13 18 14 19 15 20 2− − 3 Added OH- [mol/L] −− − 2 − −2 − − − 2 − 2 −− −2 −− [CO [C [PHCO OH HCO ] COCO [CO ] ] [HC pH PCOKlog log =− −log −+ log log HCO 15 CO HCO [HCO pH = −=log KpH −Klog Plog 3 ][HCOOH CO 23+ ] 3 OH CO 2 + 3 33 3 3 33 3 2 Added H−+log [mol/L] 2 2 1 1 1 2 K = [H ] × [HCO 3 ] PAP GE 8 CO 2 − [OH ] = 0 SECTION A6 pH = − log K − log PCO2 + log[HCO [HCO3 ] = [CO3 ]/R (mol/L) - 2- − 3 ] OH − 2− 3 CO HCO − 3 [CO32−] (ppb − )= 0. 42 × Pf [OH − ] [HCO3 ] H2 SO4 [CO 32 −] VER S IO N [CO32−] [ CO 4 – 09 / 13 8 1 pKa1 HCO3 + H ←3→ 3H2 CO3 CO 2 H2 CO 3 (aq 3 H2 2 32→ HCO33 (aq ) + H −(aq ) ) ←pK 8 HCO 2 CO 2− Kaaa12−1 18[ − 2 −] [HCO3+ ] =− 0 − Ka2 2 −−3 2 − ++ K −− − 9 PCO +CO + H +← →5 [OH − ] HCO [ H2 SO4 pK 9f =OH log +(aq H ← → 15 − −pH = − log K − log CO HCO HCO ) ← ) + [HHCO (aq p8HCO (Vol 3 [HCO →HCO ← HCO p3f = HCO ) Vol mL /5 3 ] 3 ]) 32)(3mL 3−3(aq /5 3 3 2 CO 3 a1 2 CO 3 K a1 CO 3 − KKa2→ − + 22 22 [OH ][OH = 0]= 0 2 − + H + ← − H CO ( aq ) ← → HCO 8 a 9 CO → HCO 2 2 3 3 (aq 3 3 K a1→ HCO3 − COCO H )← 6 CO2 ( g ) ← → CO2 (aq )p = 32 − +CO KH H → HCO (aq ) +3 −H +(aq) 89 CO + →3−2HCO 119 +2← a22O (mL) /5 2 32 −3+(aq Vol 6 − CO ( g ) ← → CO ( aq ) f CO + H ← → HCO − 2O N A : C H E 2M 2− I C2A 3 [OH ] = 0 K2 − S E C T I23 L02 D PPH (Ymol P R O −P E R T −I E S 2− 19 32 − [OH ] = 0 9 C A CO B O2T− + H + ← − [CO3[CO ] =3 00−.].02 /S LI C) /A LL )HCO = A0××.N02 23 16 a→ HCO3 →10 H2O(2g3−−)+← f 10 PPff (×mol HCO OH ← 3 K→ 3 + OH ← 6CO 3 +CO → CO ) 32 −− + H2O + a222+(aqCO 2 −(+aq − Ca 9 H ← → HCO CO ) + ( aq ) → ↓ CaCO ( s ) 12 − )OH 23 − (aqO) CO + H2−O← ← →CO H CO 3 7 10 HCO → 23(aq 3 + 2O 10 HCO →20 CO23322−−++3 H H[HCO [CO32 −] = 0. 02 × Pf ( mol / L ) 3− + OH ← 2 ] = [CO32-]/R (mol/L)2 − 2− − − 3 [ ] [ CO 17 ] [ ] [ ] CO + OH = 0 . 02 × P ( mol / L ) CO ( mg / L ) = 1200 × Pf [CO− 3 ] (mol/L) [ CO ] 10 HCO + OH ← → CO + H O 2 − f −2 3 33 − K + 3 − 3 3 2− − − A x2 exp − 2 −− ) + H O ← CO → HCO L ) 3/2 L−+) CO 2 + H 2O 13 ( mol( mol / CO 24 24 [HCO[HCO − HCO ← →=CO 23( g 2+ H O 3 + H (aq) 10 3 ]=3 ]= → 2HCO 11 CO + CO → 2HCO 11 3 + OH 3 +H . . ] (mol/L) [ HCO . . − − 2 − 3 2 2 3 ( ) K ( ) CO ( aq ) + H O ← → H CO ( aq ) − exp A B pH 3 7 + exp A B pH a − − 2 2 − 1 − 2 2 2 3 10 3 HCO + OH ← → CO + H O brine, means the API alkalinity 1. Prepare consisting mL [CO3 2 − ]7 formate H ← H )−(5=aq −of 23−+(aq 3 2HCO CO COa)2sample + H2O→ → 11 [HCO ]((aq CO kg2) /+3m 1.)2 ×fluid Pf sample HCO = 0standard CO/2 L(aq ) + H18 →[that H ) 2 CO 3 3 3 3 2HCO 33](aq 2O ← 2CO CO → 118 [HCO3−] = . ( mol -10 322 −−+ CO 2 + H 2O 3− • 2− [45 HCO =0 • determining 2+ 2 +− 21 carbonate (brine or filtrate) and mL water. = A3.894 10for 25) 25 isAunsuitable + mud 3 ] deionized = 3.894 10-10 12 CO ( aq ) + Ca ( aq ) → ↓ CaCO ( s ) A exp (B . pH )test method ( aq ) + Ca ( aq ) → ↓ CaCO ( s ) [ ] [ ] CO + CO + H O → 2HCO 12 11 ×322O H) + H HCO 3 CO23(22aq → H2CO− 3 (aq)3 7 3 K← 2− a2223+ −− 149 2. Measure K = CO H )+pH ← HCO and bicarbonateKconcentrations in+ this brine system. of this sample a calibrated glass CO → 2H 11 2→ +( aq 2 − ↓with aq + Ca ) CaCO ( s ) 12 − − 2 + H 2O 322 −−(+ 3[→ a1 3 + 2CO -10 3 3 • − − ] (mol/L) CO ( aq ) + Ca ( aq ) → ↓ CaCO ( s ) 12 CO [ ] (mol/L) P A = 3.894 10 H226 CO3 26 (aq ) ← → HCO ( aq ) + H ( aq ) 8 3 3 B K= 2.193 3 22 B = 2.193 − 2 −++ CO CO 2− 2HCO ] = 0 = A x exp( B ×[CO − K11 CO + 2H 22O+ K[ → + a1 − [OH 3=+ 0. 42 × pH3223−−2−)]−](mol/L) = A x exp ] (ppb electrode. +332H((gaq ()aq H2 CO3 (aq )19 ← → HCO (aq) CO2 ( g ) + H2O ←→ CO ) P [OH 3−3] =(aq 8 0 ) + H13 CO 13 HCOCO + 2Ca ( aq )3HCO → ↓ CaCO ( s ) +) 2)H O ←→ + H ( aq ) − 12 [ 3CO f − 2 − − CO − − 3 ]](mol/L) ] (mol/L) 2+ [[2HCO (mol/L) K P +[−HCO [exp CO OHHCl ]3) 12 CO pH =( g−)log KO−K a← log log3=[−−HCO 15 3. Perform CO HCO 3 H ++ ( +3aq − this− are: 323−3 ) + Ca COor (3=aq → K CO 1 → K a−]2OH 13 2− consequences titration toHCO pH − 3 ( aq ]= 0 = AA) xx exp3 =of0HCO B = 2.193 HCO (aq ← ← HCO )8.2 +HH2with aq 22 (−3−g 2O 3 + 27 8 27 + [OH 13 2→ +→ CO ) ++)a)H H HCO (−(aq )0()0.02N 9 The CO [HCO −(aq 2 2 CO 3→ −]](mol/L) (mol/L) −2Ca CO 2 ( aq 3− [+ K a[→ ] CO = . 02 × P ( mol / L ) 23 32 − + H + ← 3− CO + ( aq ) ↓ CaCO s ) 12 3 23 2 K 3 f + ] [ (mol/L) 10 HCO → CO + H O HCO 3 3 + OH ← 3 [HCO ] = [CO ]/R (mol/L) = A x exp( 9 - The CO3phenolphthalein +H ← → HCO 20 3 2 3 + − 13 CO ( g ) + H O ← → HCO + H ( aq ) can be used to[H ] × [HCO 3 ] H2SO endpoint pf − + − the phenolphthalein 3 3 2 − 2 −endpoint 2 4 2 3 [ and ] [report − K (mol/L) ] =3 0] = 30 K 23 − ] [OH −] = 0 − H +× HCO − 28 28 [CO3[CO 13 CO[2[HCO ( gof )2 −3+]] (mol/L) H → HCO3 14 and Kcarbonate = CO + ← 14 K 32=the 2O ← 9 CO +HHvolume, a→ 3 determine the combined hydroxide as V (mL), + required per mL [ +] × [HCO −K]HCO 3 of −titrant 3 = A x exp( 13 CO ←3→ PCO ] HCO3 + H (aq) 16 . 02( g ×[H)P+f] ×HP[CO HCO [CO3 2 − ] [ HCO − ] (mol/L) 2O 14 2− 2− K0 − − − − 2 − + − 14 K ==22 −[sample: [CO32 −] = 0 concentration [−OH −CO ]+322[−CO ]. fluid pK a pK2a 10 HCO − + OH −−OH ← → +− 3HCO HCOHCO 3 [CO −) −] ×P 2[HCO − − 3 −] = − HCO HCO − ( mol 2O 3 3 24 3O ] 3 2 − /L − − 2 −] CO + + H → 2HCO 11 [CO 2 P OH [ ] . − H2 SO[4CO 10 pH = − log K − log P + log HCO 15 CO HCO HCO33 + OH21 ← → CO + H O 3 2 2 3 [ ] HCO = 0 K− −2 log PCO + log[3HCO 3 ] 3A expOH 15CO CO HCO 14 KpH==2 −−3log CO (B−3. pH 3 ] 3 3 2 cannot be used to [)H[3+2HCO ]−× [HCO ]− [CO 2 −3 3 3 - The−methyl orange endpoint − 2− 2− − − 17 2− [ ] [ ] − − CO + OH = 0 . 02 × P ( mol / L ) − + − − − 2 P − [[CO 2− − f log [HCO − ] 14 3 OH −K = CO pH ==3 [+ − OH log KKHCO log 15 ] 3 ] [HCO[HCO ] 3 ] P P H 10 pK[aOH []OH ] [CO3[CO OH ] × [CO CO3 HCO3 2− CO 3+ 3 ] 3 3 ]P ← → CO + H AO(13) 3 SO CO log −/5 log 15H SO HCO CO332 − P HCO HCO33− • =23−(−Haq 2 + P25 f (mL CO + log [2HCO 3− 3 f 214 determine the total buffer concentration (including 3.894 10-10OH− KppH − f =Vol CO 2 ) +K)Ca ( aq )+ → ↓ =CaCO 12 42 4 CO − 2− 22 [ 3= − 3 (s) [ OH ] = 0 OH [ ] CO pH log − log P log HCO 15 CO HCO 2 − − 2 − − − CO 3 P 3] 3 3 CO + CO + H O → 2HCO 11 CO [ − − 2 3 2 2 3 [ ] [ ] [ ] itHis possible to16 detect an endpoint [OH ] HCO = 0 18 CO3 11 HCO − 3 [ Pf if pH[=CO−2log K − log PCO +COlog 15 0. 02 × Pf CO 33 + ). COEven → 16 0. 023× Pf 2 K 26 ] (mol/L) 2 SO4 2HCO3 2 +H 2O − B −=+ 2.193 2 − brine, the use of this OH − CO332− − HCO 3=− A x [exp( ]) CO 3 pH −)Plog KO −← log PCO situations +HCO log[−HCO 15 in a very diluted formate Depending on pH, four exist: 2=− 13 3aq CO ( g + H → + H ( 16 0 . 02 × 2− [ ] 2+ CO = 0 . 02 × P ( mol / L ) 23 2 2 3 CO → 2HCO3 1116 3→ ↓ CaCOf (s) 0. 02 ×− CO Pff 2 + H 2O [ HCO ] (mol/L) 3 + CO 2 −( aq ) + Ca 2 + ( aq ) 12 − endpoint [CO32 −] ( mg /3L ) = 1200 × Pf[CO23−2 − 17 33 (s) [CO32 −]+ [OH2−−] = 0. 02 ( mol /> L3−2)×11.1 CO33 ( aqwould ) + Ca give ( aq )erratic → ↓calculations. CaCO 12 17 × Pf1.pH ]+Pf[OH −] = 0. 0227 × Pf ( mol[OH / L ) ]= 0 16 0[CO . 02 2]− 2 − [[CO − [CO32 − ] (mol/L) 19 [[OH 2 −]2= + −]+0 3 2− 0. 02 × Pf 17 −] = 20 ××) P // LLCaCO )) (14) − K 2− f ((mol 3 H 3 +[HCO Ca aq s16) [CO 12 ] 28 17 = ACO ]−B+P+]×[[)OH ])= 03.(.−02 x[CO exp( pH CO OH 02 P→ mol↓ CO × CO3)2 − ] 13 3 3 ([aq 3 (0 CO2 ( g ) + H2O ←→ HCO− 3− + H ++ ([aq f 2 − − [ CO3 −] (mol/L) 3 [ ] 3 CO = 16 0 . 02 × K 2 − 14 = 2 −3]B+] =×[fOH [CO3 ] ( kg /2m exp( pH [ L0) the] (mol/L) [HCO 13 Another therefore required (15) CO2 ( gmethod ) + H24 ←→ HCO + H . (18 aq)for. measuring HCO 0 −])=2-0. 02 × Pf ( mol / L ) 3 [HCO ( mol 17 18 = A xK[CO − ) = 1. 2 × Pf [CO3 ] 3 ]/=HCO 2O is 3 ]3 = 3 -− 2− 2 − ] (mol/L) [ [ HCO 33− ] (mol/L) − P CO [HCO ] = [CO ]/R (mol/L) (B pH ) 20 CO exp A 3 2 −] 2 − [CO ]+ [OH −] = 0. 02 ×[P K 23 [[HCO (3mo 33 −] = 18 =−pK A a[xCO fexp( 3 HCO bicarbonate concentration. One way of doing this is Unless of3−[+OH have ] 13 )]+=large H002O → HCO H +−(]aq ) 17 been CO CO3 added HCO − amounts 18 CO −2 − 3 2 (2g 322 −− − [ 3−] [CO 17 [CO [OH ]−=← −+log 0. 02 × P+f log ( mol /L) − ] ] (mol/L) HCO [CO [H++] × 25 [HCO 3 −− ] A = 3.894 • 10-10 OH [ 3 − pH = K log P HCO 3 3] 15 CO HCO 3 [ [ ] CO 3 CO 3 3 HCO = 0 18 to this most of22−−this − 3 3 fluid, one can assume that 14 by using K = [Ha Garrett ] × [HCO 3Gas ] Train (GGT). The GGT determines − − − 2− [OH ] 18 [[CO HCO3 )]==[HCO CO33 ]][(ppb 00. 423×] Pf [CO [OH ] =The 0 14 the Ktotal = amount [OH −] =− +0 is from 19 Pf 322−][−C PCO 2 of carbonate and19bicarbonate. [CO −[H] = [[OH ] ×0[HCO 3 − −]carbonate. CO32−] ] 18 21 − alkalinity HCO P26 [ B = 2.193 −]33 CO 2 [ = 0 19 2 − − 2− − − [CO33 ] [OH 19 [= [OH ] [CO ] OHvery CO32 −2- 14 [HCOtherefore H SO CO] =2 −0] [HCO pH = is − log log PCO + logand 15 method timeK −consuming not HCO 3− K0 3− ] 2- 3− 16 .[02 [HCO [CO ]/R19 (mol/L) [OH − ] [CO p = Vol (mL) /5 [CO32−] ( [CO ]/R OH −3-] =CO [HCO 320 ] H22SO44 CO−−]3×=3-]P0]=f P pH = − log K − log PCO + −log 15 HCO 20 CO[HCO [[HCO OH 23 3 ] (mol/L) 33 3 f [ ] OH = 0 − 27 popular on the rig, and does not differentiate between 22 2. pH [OH=]11.1 =- 0= [CO 2-2-]/R (mol/L) 2 − ] = 02 − HCO − [HCO 19 OH −[OH CO 20 [CO 22 − 3− =−233−−-]]log K−−33 log [HCO = [CO ]/RP(mol/L) 15 20 pH CO + log [HCO 3 ] 3(16) 3 [[CO ]( 2− [[HCO ] OH = the different buffer components. 19 -]+0[OH ] = 2- 0. 02 × P ( mol / L ) 17 3 [ CO CO [ ] f 32 − ] = [CO ]/R (mol/L) 3 CO3 = 0 20 3 16 0. 02 × P 28 . 023 × Pf ( mol / L ) 23 (17) [HCO3-] = [CO32-]/R (mol/L) 20 3 ]−]==00 21 2 − [HCO3−] −= 0 16 0. 02 × Pff 21 [[CO HCO − 23-−− ] = [CO ]/R (mol/L) OH concentrations CO3 HCO3 been pK a20 [CO32 −] [[.HCO Carbonate and bicarbonate have 0[HCO (18) 18 33 −]] = 0 3 21 2× − 3]P 16 02 21 [ ] HCO = 0 [ 17 = [CO322 −−]+ [OH −−] = 0. 02 × Pf ( mol / L ) f p ( ) CO ( mg / L ) = 1200 × P Vol mL /5 = 3 p ( ) Vol mL /5 32 − − f using a dual-titration [CO 22 2−] method. [OH −[]HCO = 0 −] 17 measured [CO3 ]+by [OHCabot ] = 0. 02 Pf (−]mol / L ) [CO = 31200 ×f Pff 22 2− ] OH3 −]3]=−(]0mg 21 [[HCO = 0 / L [)CO [×OH ppf ==−Vol ((mL Pf 3 3 H2 SO −2 − ] = [ mol L ( / ) HCO 24 Vol mL)) /5 /5 [ 2 −] 4 − 21 [ ] HCO 3 2 − 22 − − [ OH ] = 0 3 f and more accurate method, based </Am 11.1 3 =0 17 [OH ].exp CO +(0kg =3)0=. 02 CO32− 22 3.9.0 [HCO OH332−< ]−]−=−pH [[CO (1B. 2.×pH [HCO3−a] =simpler ×PfP()fmol / L ) 0 18 Recently = 2− p ( ) /5 [CO Vol mL 2 21 [ ] = 0 ]( − f [[CO OH3 ]]3=]=](0=kg 0 0/. 02 19 [CO3 ] = 0. 02 × Pf 22 [HCO3 ]pH ( mol / L[)CO 23 m ) = 1 . 2 × P = 0measurement and phenolphthalein 3 18 on simple × P ( mol / L ) 23 OH (19) f 32 − -10 f • − 2 − A = 3.894 10 25 − 2 − 22 [OHp ]==Vol 0 (mL ) /5 [CO ] CO 23 3 ]]= = 00..02 18 titration, has been developed. (20) CO 02 2-×× PPff ((mol mol // LL )) 23 [[[[HCO f 3 22 OH23−−2]3−=-]0= [CO [HCO ]/R (mol/L) 20 2− − 3] = 0. 023× P ( mol / L ) [ CO 23 [ CO ] [ ] [ ] 3 f CO From the carbonate 2− (ppb )= 0[CO . 423 2×− ]Pf / bicarbonate [OH −] = 0 CO32− pH relationship 19 2− B 3=2− 2.193 − 326 − [CO3 ] = 0. 02 × Pf ( mol / L ) [HCO3 ] = . . 422×− ]Pf ( mol /[LCO [OH ] =field 0 mol ([CO /2]L−3(ppb )] = )= 0[CO 24 for determining 19 A simple [HCO ) 3 ] 23 the carbonate 24. 3Equation or laboratory method and / .12 − ].Figure [[CO 02 ×[CO Pf3(3B(2 −mol /)L( mol )6, determine A exp (23 B pH ) in exp pH −3−] ]−]==0.A L / ) HCO 24 2[CO32−] ( OH = 0 27 [bicarbonate ] =33−0] = . [ratio, OH 19 [HCO ( mol / L )the bicarbonate 24 [HCOconcentration ] = [CO32- ]/R (mol/L) 20 buffer CO3(B2 − ]..R. Calculate ) 3exp A pH . −] = 0 -10 • -10 21 [ HCO • ( ) [HCO3 ] = [CO3 ]/R (mol/L) exp B pH ( mol / L ) A 10 A = 3.894 10 24 25 20 3 = 3.894 25 [AHCO [CO 2 − ] 3− ] = − .exp . pH ) [ACO=323.894 Laboratory testing of formate brines with known concentration -10as: 28 ( 2(mol/L) - ] = 0A •• 10 2[HCO ]= ( . ) 3 . (m [CO 24 25 -10 3B −] 3 Vol [HCO ] = [CO ]/R 20 − = p A = 3.894 10 25 mL 3 −3 ] = f A exp/5(B pH ) [B[OH ( mol /−L ) HCO 24 additions− of carbonate and bicarbonate B =shown 2.193 26 has 22 ] -10 2 − . = 2.193 3= 0 26 •. − AOH= 3.894 25 pK a exp A 10 CO (B pH ) HCO 21 [HCO =0 – 3− ]buffered B ] = [CO32–3] (mol/L) / R 3 (21) pH of formate brines is dependent on the 26 A = 3.894 • 10-10 25 21 that[HCO B == 2−2.193 2.193 26 [HCO 3 3 ]= 0 [OH −] = 0 -10 2− −= 0 [ ] 27 • OH 27 − −−] = 0. 02 A = 3.894 10 25 [ = CO × P ( mol / L ) 23 p ( ) B = 2.193 Vol mL /5 [ ] [ ] carbonate-to-bicarbonate ratio [6], [7]. The following 26 [OH OH3−−3]]=] =0 0 CO3f HCO3 f 21 [[[HCO P H2 SO4 22 27 [OH −] = 0 ) /5 2 − pf = Vol (mL 2] −= 0 B = 2.193 26 f 27 [COcarbonate ]= 0 22 relationship, 28 [OH −] = 0 R, has been found between [[BOH the 4.pH < CO = 0 28 −3 =]9.0 3 26 OH=− ]22.193 =− 0 27 p = Vol (mL) /5 2 −] = 0 [ 2 − CO 28 [ CO ] bicarbonate molar ratio and brine pH: [[OH 222 −28 − [OHf −] =(22) 23−2 − CO]33−−−2=−−]0= 0 0 − 27 23 and[CO pK 32 −] = 0. 02 × Pf ( mol / L ) OH CO HCO pK OH CO HCO a [ ] 3 3 mol L ( / ) HCO = 24 [[OH a 3− [CO3 ] = 0. 02 × Pf ( mol / L ) 23 27 CO3−−2]−3=]]==0insignificant 0A .exp322(−B− . pH 28 CO insignificant 2 − ) − 2− pK OH 32 − CO3 2− HCO3 − [CO3 ] = 0 2− [CO3 ] (mol/L) pK 28aa −]−−= 3f2 to 3− ] 0. 02CO / LHCO ) [HCO [CO323 ] [[OH [OH −] HCO [×CO ] determine −( mol [CO [CO 3 −23] OH R= = 2A− ]× exp( B × pH ) (12) P-10P ]]=difficult Pf 3− H2 SO4 0 • 10 28 [ CO f 32− H2 SO4HCO pK −− OH CO A = 3.894 25 3 − a 3 3 3 2− − 2−] −] HCO 3 ]] =(mol/L)[CO 2 − ] [[to [[OH −] CO HCO [[HCO ( mol / L ) pH to[[be above 9.0PPwith 24 3 ] H ] ] CO3 HC OHneeds CO233adjusted HCO f 2 SO 4 HOH − 3− −− 2−− f 2 SO4 [HCO33−] = A ..exp 3(B .. pH ) ( mol / L ) 24 pK OH CO HCO [ ] [ ] [ ] OH CO HCO [ CO a ] 3 3 where before concentration B = 2.193 Pfcan Hbe 3 2− 3 26 A exp (B pH ) 2− − the bicarbonate 3 2 SO−4 [CO3 ] [ [OH ] [HCO−3 ] = . ( mol / L ) 24 A = 3.894 • 10-10 25 determined. [CO(3B2−]. pH ) [HCO3−] OH−]]= 0 A exp 25 A = 3.894 • 10-10 Pf H2 SO4 [[OH 27 • B = 2.193 A = 3.894 10-10 25 26 2− ] = 0 amounts of sodium or potassium B = 2.193 equivalent 26 28 The[CO 3 – OH −]2–= 0 27 and[[CO can− easily be calculated B = −2.193and bicarbonate 26 carbonate 2− [OH −3] =‐]0and [HCO3 ] are the molar concentrations of pK a OH 27 CO3 HCO3 2 − carbonate and bicarbonate. This relationship is shown from these molar concentrations. This simple field − [ ] CO32 − = 0 28 [ ] OH = 0 27 2 − − [CO3 7] and = 0 is valid for pH measured with a glass 28 in Figure [CO3 ]in more[HCO ] in Section [OH −]is explained method detail C2.SO P 3 H f 2 4 2− − pK OH − CO 2brine HCO with [CO32 −] = 0 electrode diluted nine − − pK aaparts deionized 28 OH − in formate CO33 HCO33 A6.3.4Buffer requirement for− field use water. used−] to determine buffer − 2− [CO322−−] can be[HCO [OHThis ] relationship pK OH − CO3 HCO3 Pf 3− H2 SO4 − [ ] [ ] [ ] OH CO HCO concentration and buffer capacity3 of buffered The recommended buffer concentrationa required Pf formate 3 H2 SO4 2− − − [COdepends ] [on ] [OH ] brines HCO brines in the field. This means that both carbonate in formate the Pf 3 3 application. HThe 2 SO4 and bicarbonate concentrations can be determined amount of time the brine will be in contact with the just by measuring pH and performing the standard reservoir fluids, and the expected level of acid gas phenolphthalein titration. The method is as follows: influx, are important factors. In well suspension and packer applications where the formate brine may be 5 [HCO3−] = 0 2 2 2 2 2 2 2 2 2 2 2 2 2 V ERSION 4 – 0 9/ 13 SECTION A6 PAGE 9 FORMATE TECHNICAL MANUAL C AB O T 18 H2O NaFo KFo KFo (non-analytical) CsKFo [CO32-]/[HCO3-] (mol/mol) 16 R = [CO32-]/[HCO3-] 14 12 10 8 6 4 2 0 9 9.5 10 pH 10.5 11 Figure 7 Relationship between the carbonate-to-bicarbonate molar ratio (R) and pH in buffered formate brines. The relationship was developed from a range of formate brines and deionized water with known amounts of buffer (carbonate + bicarbonate) added. The carbonate content was measured by titration to endpoint of 8.2, i.e. phenolphthalein endpoint, after dilution with 9 parts deionized water, and pH was measured with a calibrated glass electrode, again after dilution with 9 parts deionized water. 18 [CO32-]/[HCO3-] (mol/mol) K2O3/KHCO3 (wt/wt) Na2CO3/NaHCO3 (wt/wt) 16 R = [CO32-]/[HCO3-] 14 12 10 8 6 4 2 0 9 9.5 10 pH 10.5 11 Figure 8 Relationship between the carbonate-to-bicarbonate ratio (R) and pH for formate brines buffered with carbonate and bicarbonate. The carbonate-to-bicarbonate ratio is given as a) molar ratio of [CO32–] to [HCO3–] (see figure 6 above), b) equivalent potassium carbonate (K2CO3) to potassium bicarbonate (KHCO3) ratio (wt/wt), and c) equivalent sodium carbonate (Na2CO3) to sodium bicarbonate (NaHCO3) ratio (wt/wt). exposed to well conditions for a long time, a high level of buffering is appropriate. In applications where well exposure times are short, and in applications where no acid gas is expected, a smaller buffer concentration will do. In drilling fluids, which can be monitored and conditioned at the surface, less buffer is required. higher than wanted. This problem can be solved by including some bicarbonate. Although addition of bicarbonate does not contribute to buffering at high pH (pKa= 10.2), it contributes to balancing alkalinity of the carbonate as pH is a function of the carbonate-tobicarbonate ratio. (See Equation 12 and Figure 7). Adding only soluble carbonate to the brine provides a high level of buffer capacity, but the pH might become When determining buffer levels for field applications, one needs to consider that some oilfield formate PAGE 10 SECTION A6 VER S IO N 4 – 09 / 13 SECTION A: CHEMICAL AND PHYSICAL PROPERTIES brines come preloaded with buffer and some do not. Cesium formate brine from Cabot delivered by the manufacturing plant typically has a pH of about 10.2 – 10.4 and contains some 0.07 mol/L CO32– and 0.03 mol/L of HCO3–. This corresponds to equivalent potassium carbonate and potassium bicarbonate buffer levels of about 10 kg/m3 / 3.4 lbs/bbl and 3 kg/m3 / 1.0 lbs/bbl respectively. Depending on the application, Cabot might add more buffer to the brine before it is shipped to the field. Potassium formate brine as delivered from the suppliers normally contains none or lower amounts of buffer, typically up to 2.5 kg/m3 / 1 lbs/bbl of potassium carbonate or bicarbonate, and pH can vary considerably. Potassium and sodium formate supplied in solid form (powder) typically contain large amounts of carbonate, which has been added as anti-caking agent. Such material, when dissolved in water, often exhibits a high pH and does not normally require further buffering. Depending on planned use, pH might need to be brought down before such material is used in the field. A buffer level of about 17 to 34 kg/m3 / 6 to 12 lbs/bbl of sodium and / or potassium carbonate / bicarbonate is recommended for most formate brine applications. Cabot normally buffers formate brines to a pH of around 10.0 – 10.5 (measured with 1:10 dilution with deionized water). The amounts of carbonate and bicarbonate required to achieve this depend on the carbonate and bicarbonate levels already in the brine. The graph in Figure 8 shows expected pH for various sodium and potassium carbonate / bicarbonate additions. However, first one always needs to consider the amount of buffer already in the brine. A pH of 10 – 10.5 and a buffer level of about 17 to 34 kg/m3 / 6 to 12 lbs/bbl sodium or potassium carbonate / bicarbonate is ideal for most formate brine applications. The use of cesium carbonate / bicarbonate might be beneficial in certain high-density cesium formate single-salt formulations to achieve higher density. A6.3.5 Maintaining buffer concentration and capacity In order to get the full benefit of the carbonate / bicarbonate buffer in formate brine, both the carbonate concentration and total buffer concentration should be maintained during field use. These concentrations can easily be determined by the simple field method described in Section A6.3.4 above. V ERSION 4 – 0 9/ 13 C A B O T In most field applications, the most practical way to control pH and maintain buffer capacity is by adding carbonate. This method has the advantage that the consequences of over-treatment are not as severe as those from KOH. A potential disadvantage with this method, however, is that it allows the concentration of bicarbonate to build up. Excessive concentrations of bicarbonate are known to cause rheology and fluidloss problems in water-based muds. This has also been experienced in formate-based muds [8]. A good indication that the total buffer concentration is getting low and addition of carbonate is required is that pH drops quickly after it has been adjusted upwards with KOH. References [1] Leth-Olsen, H.: “CO2 Corrosion of Steels in Formate Brines for Well Applications”, 2004 NACE, paper # 04357, New Orleans, USA, March 2004. [2] Prasek, B.B. et al: “A New Industry Standard for Determining the pH in Oilfield Completion Brines,” Paper # SPE 86502, Lafayette, LA, February 2004. [3] Javora P.H. et al: “A New Technical Standard for Testing of Heavy Brines”, paper # SPE 98398, Lafayette, LA, February 2006. [4] “Dilution factors for accurate measurement of formate brine pH”, Cabot laboratory report # LR-050, April 2004. [5] API RP 13B-1: “Standard Procedures for Field Testing Water-Based Drilling Fluids”. [6] “Potassium Formate Titration curve using KCOOH”, report # LR-289, Cabot Operations and Technical Support Laboratory, Aberdeen, UK, February 2009. [7] “Calibration titration for buffer determinations”, report # LR-294, Cabot Operations and Technical Support Laboratory, Aberdeen, UK, March 2009. [8] Berg, P.C., et al.: “Drilling, Completion, and Openhole Formation Evaluation of High-Angle Wells in HighDensity Cesium Formate Brine: The Kvitebjørn Experience, 2004 – 2006,” SPE 105733, Amsterdam, February 2007. SECTION A6 PAGE 11