TestingofHeavyBrines

APIRECOMMENDEDPRACTICE13JSIXTHEDITION,JANUARY2023

AmericanPetroleumInstitute

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Copyright◎2023AmericanPetroleumInstitute

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Foreword

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Contents

Page

1Scope 1

2NormativeReferences 1

3Terms,Definitions,Acronyms,Abbreviations,andSymbols 1

3.1TermsandDefinitions 1

3.2Acronyms,Abbreviations,andSymbols 3

4Requirements 7

4.1QualityControlInstructions 7

4.2RecordsRetention 7

5CalibrationofEquipment 7

5.1GeneralRequirements 7

5.2ReagentsandMaterialsforCalibrationandVerification 7

5.3GeneralRequirementsforCalibrationofParticularApparatus 8

5.4FrequencyofCalibration/Verification 8

5.5Calibration/Verification—Temperature-measuringDevice 9

5.6Calibration/Verification-Density-measuringDevice 9

6Density 11

6.1General 11

6.2Apparatus 12

6.3MeasurementofRelativeDensityorDensityUsingaHydrometer 14

6.4DensityCorrectionsforHydrometersandBrines 15

6.5CalculationofDensityinUnitsOtherthang/mLorkg/m3 22

6.6CalculationsforPressureandTemperatureCompensation 24

7CrystallizationTemperature 28

7.1Principle 28

7.2Apparatus 33

7.3DeterminationofCrystallizationTemperatureofHalideBrines 35

8BrineClarity 35

8.1Principle 35

8.2Apparatus 36

8.3DeterminationofBrineClarity 36

9SolidsEvaluationbyGravimetricProcedure 37

9.1Principle 37

9.2Apparatus 37

9.3PreparationofGlass-fiberFilterDisk 38

9.4SelectionofSampleVolume 39

9.5DeterminationofTotalSuspendedSolids 39

9.6CalculationofTotalSuspendedSolids 40

9.7CalculationofPrecisionandBias 40

9.8DeterminationofVolatileandNon-volatileSolids 41

9.9CalculationofNon-volatileandVolatileSolids 41

Contents

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Page

10pH 41

10.1Principle 41

10.2ReagentsandMaterials 42

10.3Apparatus 43

10.4MeasurementofpHofHalideBrines 44

10.5PrecisionStatement 45

10.6CareoftheElectrode 45

11IronContamination 45

11.1Principle 45

11.2ReagentsandMaterials 46

11.3Apparatus 46

11.4PreparationofColorimetricStandards 47

11.5MeasurementofIronContamination 47

11.6PrecisionStatement 48

12BufferingCapacityofBrines 48

12.1Principle 48

12.2Equipment 49

12.3ReagentsandMaterials 50

12.4Procedure—DeterminationofBufferConcentrationsofHalideBrines 51

12.5Calculation—FirstpHEndpoint 53

12.6Calculation—SecondpHEndpoin 55

13DailyCompletionFluidReport 56

13.1Principle 56

13.2DailyReportHeader 57

13.3WellboreGeometry,Pumps,andZoneData 57

13.4CompletionFluidProperties 58

13.5FluidsandProductsAccounting 59

13.6Usageand/orCostAccounting 59

13.7DailyOperationalCommentary 59

13.8VendorRepresentativeldentification 59

13.9EnvironmentalandSafetyInformation 60

AnnexA(informative)ExampleofDailyCompletionFluidReport 61

AnnexB(informative)GasHydrates 62

AnnexC(informative)PressureCrystallizationofBrines 64

AnnexD(informative)BrineViscosity 66

AnnexE(informative)PrincipleofCorrosionTesting 67

Bibliography 80

Figures

1HydrometerReadingatBottomofMeniscus 15

2CalciumChlorideCrystallizationTemperature 29

3TypicalCrystallizationCurveforBrine 33

Contents

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Page

4TypicalCrystallizationTemperatureMeasurementSetup 34

5ExampleofpHvsVolumeofHCIAcidAdded 52

6Exampleof△pH/△VHClvspHforMoreAccurateDeterminationofTitrationEndpoint 53

Tables

1TemperatureCorrectionFactorsforHydrometersduetoGlassExpansion

andContraction 17

2EstimatedBrineThermalExpansion/ContractionFactors(ConversionFactors) 21

3PressureCompensationFactorinSIUnits 25

4TemperatureCompensationFactorinSIUnits 25

5PressureCompensationFactorsinUSCUnits 27

6TemperatureCompensationFactorsinUSCUnits 27

7CalciumChlorideSolutions—CrystallizationTemperature 30

8SodiumChlorideSolutions—CrystallizationTemperature 31

E.1MechanicalPropertiesofSelectedOilCountryTubularGoods 70

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Introduction

ThisstandardisbasedonAPISpecification13J,5thEditionandcoversthetestingofheavybrinescommonlyusedinpetroleumandnaturalgascompletion,fracturing,workover,anddrill-influids.Thesebrinescanbepurchasedorrentedfrommultiplesourcesandareavailableworldwide.Nosinglesourceorlimitedsourceofsupplyisincluded,eitherbyinferenceorreference.

AnnexesAthroughEaregivenforinformation.

Inthisstandard,quantitiesareexpressedintheInternationalSystem(SI)ofunitsandarealso,wherepractical,expressedinU.S.Customary(USC)unitsinparentheses.

NOTETheunitsdonotnecessariyrepresentadirectconversionofSlunitstoUSCunits,orofUSCunitstoSlunits.

Considerationhasbeengiventotheprecisionoftheinstrumentmakingthemeasurement.Forexample,thermometersaretypicallymarkedinone-degreeincrements;therefore,temperaturevalueshavebeenroundedtothenearestdegree.However,forcertaincriticalmeasurements(suchasbrinecrystallization),thermometersaretypicallycalibratedandusedto0.05℃(0.1°F).

Calibratinganinstrumentreferstoassuringtheaccuracyofthemeasurement.Accuracyisthedegreeofconformityofameasurementofaquantitytoitsactualortruevalue.Accuracyisrelatedtoprecision,orreproducibilityofameasurement.Precisionisthedegreetowhichfurthermeasurementsorcalculationswillshowthesameorsimilarresults.Precisionischaracterizedintermsofthestandarddeviationofthemeasurement.Theresultsofcalculationsorameasurementcanbeaccuratebutnotprecise;precisebutnotaccurate;neither;orboth.Aresultisvalidifitisbothaccurateandprecise.

ThisdocumentusesaformatfornumbersthatfollowstheexamplesgivenintheAPIDocumentFormatandStyleManual,October2020.Inthisdocument,thedecimalmarkisaperiodandseparatesthewholepartfromthefractionalpartofanumber.Nospacesareusedinthenumberingformat.Thethousandsseparatorisacommaandisonlyusedfornumbersgreaterthan10,000(i.e.5000items,12,500bags)

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TestingofHeavyBrines

1Scope

Thisstandardcoversthephysicalproperties,potentialcontaminants,andtestproceduresforheavybrinefluidsmanufacturedforuseinoilandgaswelldrilling,completion,fracturing,andworkoverfluids.

Thisstandardprovidesmethodsforassessingtheperformanceandphysicalcharacteristicsofheavybrinesforuseinfieldoperations.Itincludesproceduresforevaluatingthedensityorspecificgravity,theclarityoramountofparticulatemattercarriedinthebrines,thecrystalizationpointorthetemperatureatwhichthebrinesmakethetransitionbetweenliquidandsolidatatmosphericpressure(adiscussionofcrystallizationtemperatureunderpressureisprovidedAnnexC),thepH,ironcontamination,andbufferingcapacity.Thisstandardalsocontainsadiscussionofgashydrateformationandmitigation(AnnexB),brineviscosity(AnnexD),corrosiontesting(AnnexE),andadailycompletionfluidsreportwithexample(AnnexA).

NOTEProceduresforevaluatingthecrystallizationpoint,pH,andbuffercapacityofbrinesarenotapplicabletoformatebrines.ProceduresapplicabletoformatebrinesarefoundinISO13503-3:2022[4].

Thisstandardisintendedfortheuseofmanufacturers,servicecompanies,andendusersofheavybrines.

2NormativeReferences

Thefollowingreferenceddocumentsareindispensablefortheapplicationofthisdocument.Fordatedreferences,onlytheeditioncitedapplies.Forundatedreferences,theatesteditionofthereferenceddocument(includinganyamendments)applies.

APIRecommendedPractice13B-1,FieldTestingWater-basedDrillingFluids

ASTME771,StandardTestMethodforInspectionandVerificationofThermometers

ASTME617,StandardSpecificationforLaboratoryWeightsandPrecisionMassStandards

NISTSRM185h2,PotassiumHydrogenPhthalate,pHStandardNISTSRM186g,PotassiumDihydrogenPhosphate,pHStandardNISTSRM191C,pHStandards

NISTSRM3126a,Iron(Fe)StandardSolution

3Terms,Definitions,Acronyms,Abbreviations,andSymbols

3.1TermsandDefinitions

Forthepurposesofthisstandard,thefollowingtermsanddefinitionsapply.

3.1.1

ACSreagentgrade

GradeofchemicalthatmeetspuritystandardsasspecifiedbytheAmericanChemicalSociety(ACS).

1ASTMInternational.POBoxC700.100BarrHarborDrive.WestConshohocken.PA19428.

www.astm.ora.

2NationalInstituteofStandardsandTechnology.100BureauDrive,Gaithersburg.MD20899.

www.nist.qov.

2APIRECOMMENDEDPRACTICE13J

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3.1.2

calibration

Theverificationofaninstrumentortotheadjustmentsmadetotheinstrumentifitisoutofcalibration.

NOTETheterm"calibrate"alsoreferstoinstrumentsthatcannotbeadjustediftheyareinaccurateandtodeterminetheircorrectionfactors.

3.1.3

converteddensity

Densityofthebrineatthereportingtemperature,calculatedfromabrinedensitymeasuredatatemperatureotherthanthereportingtemperatureusingadensity-temperatureconversionfactor(conversionfactor).

3.1.4

correcteddensity

correctedrelativedensity

Measureddensityorrelativedensityofthefluidcorrectedforglassexpansion/contraction(correctionfactor)whenthemeasurementismadeatatemperatureotherthanthesamplereferencetemperature.

3.1.5

density

massdensity

Massofaspecifiedmaterialpervolumeofthespecifiedmaterial,ataspecifiedtemperature.

3.1.6

measureddensity

measuredrelativedensity

Densityorrelativedensityofafluidatitsmeasuredtemperature.

3.1.7

relativedensity

Dimensionlessratioofthemassofavolumeofaparticularsubstancetothemassofthesamevolumeofareferencesubstance,i.e.theratiooftheirrespectivemassdensities.

NOTE1Generallyspeaking,thereferencesubstanceispurewater.

NOTE2Relativedensityiscommonlyknownasspecificgravity

3.1.8

samplereferencetemperature

Thetemperatureatwhichmeasurementsmadedonotrequireacorrectionfactor.

3.1.9

specificgravity(SG)hydrometer

relativedensityhydrometer

Commonhydrometermeasuringtherelativedensity(specificgravity)ofaliquid:thedensityoftheliquidatareferencetemperature(60F)tothedensityofdistlledwateratareferencetemperature(60F)(ie.relativedensity60°F/60°F).

NOTE1Thestandardreferencetemperaturecanbetakenat15.56℃.

NOTE2Densityhydrometersprovideadirectmeasurementofthedensityofaliquidatareferencetemperature.

3.1.10

user

Manufacturer,servicecompany,enduser,oroperatorapplyingthetestingofthispartofthisstandard.

TESTINGOFHEAVYBRINES3

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3.2Acronyms,Abbreviations,andSymbols

3.2.1AcronymsandAbbreviations

ACSAmericanChemicalSociety

AISIAmericanIronandSteelInstitute

BHPbottomholepressure

BHTbottomholetemperature

CASChemicalAbstractsService

CRAcorrosion-resistantalloy

CWcold-worked

DSSduplexstainlesssteelFCTAfirstcrystaltoappear

ISOInternationalOrganizationforStandardizationJSAjobsafetyassessments

LCTDlastcrystaltodissolve

meqACIDmilliequivalentsofhydrochloricacid

MICmicrobiologicallyinducedcorrosionmLBRINEmillilitersofbrine

MSSmartensiticstainlesssteel

MTALCmaximumtemperatureafterlastcrystal

NACEFormerlyNACEInternational,nowknownasTheAssociationforMaterialsProtection

andPerformance(AMPP)

NTUnephelometricturbidityunit

PCTpressurecrystallizationtemperaturePPEpersonalprotectiveequipment

psipound-forcepersquareinch

RTDresistancetemperaturedetectorSCCstresscorrosioncracking

SEMscanningelectronmicroscope

SGrelativedensity(specificgravity)hydrometerSImetric(unit)

SSstainlesssteel

SSCsulfidestresscracking

TCTtruecrystallizationtemperatureTDtodeliver

TVDtrueverticaldepthUSCU.S.customary(unit)

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4APIRECOMMENDEDPRACTICE13J

3.2.2Symbols

Be

density-measuringdevice-correctioncurveintercept,expressedinmeasuring-devicedensityunit

C

brinedensityconversionfactor,expressedingramspermilliliterandperdegreesCelsius

Cp.sI

pressurecompensationfactor,expressedin(kilogramspercubicmeterandpermegapascal[(kg/m3)/MPa]

Cp,uSC

pressurecompensationfactor,expressedinpoundspergallonandper1000pounds-forcepersquareinch([Ib/gal)/kpsi]

CsI

brinedensityconversionfactor,expressedinkilogramspercubicmeterandperdegreesCelsius

Cusc

brinedensityconversionfactor,expressedinpoundspergallonsandperdegreesFahrenheit

Cg

glassexpansion/contractioncorrectionfactor,expressedingramspermililiterordimensionless

Ce,si

temperaturecompensationfactor,expressedin(kilogramspercubicmeterandper100degreesCelsius[(kg/m3)/100℃]

Ce,Usc

temperaturecompensationfactorexpressedinpoundspergallonandper100degreesFahrenheit[(lb/ga)/100°F]

CB1

firstbufferconcentration,expressedinmilliequivalentsofacidpermilliliterofbrine(meqACID/mLBRINE)

CB2

secondbufferconcentration,expressedinmilliequivalentsofacidpermililiterofbrine(meqACID/mLBRINE)

CKHCO;

concentrationoftitratablebasicspecies,expressedinkilogramspercubicmeterorinpoundsperbarrelofpotassiumbicarbonate

CK?CO

concentrationoftitratablebasicspecies,expressedinkilogramspercubicmeterorinpoundsperbarrelofpotassiumcarbonate

CNa?CO?

concentrationoftitratablebasicspecies,expressedinkilogramspercubicmeterorinpoundsperbarrelofsodiumcarbonate

CNaHCO

concentrationoftitratablebasicspecies,expressedinkilogramspercubicmeterorinpoundsperbarrelofsodiumbicarbonate

Fe

density-measuringdevice-correctionfactor,expressedinmeasuring-devicedensityunit

hTvD,S

trueverticaldepth,expressedinmeters

hTVD,USC

trueverticaldepth,expressedinfeet

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MHCl

molartyofthehydrochloricacidused,expressedinmolesperliter

ms

massoftotalsuspendedsolidsexpressedinmilligramsperliter

mS-nv

ms-v

massoftotalnon-volatilesolidsorresidue,expressedinmilligramsperlitermassoftotalvolatilesolids,expressedinmilligramsperliter

m1

originalmassofpanandglass-fiberfilter,expressedinmilligrams

m2

finalmassofpan,glass-fiberfilterandresidue,expressedinmilligrams

m3

massofporcelainevaporatingdishandfiltermedium,expressedinmilligrams

m4

massofporcelainevaporatingdishandfilteredsampleafterdryingat105℃(220°F),expressedinmilligrams

m?

massofporcelainevaporatingdishandfilteredsampleafterauto-ignitionat550℃(1000°F),expressedinmilligrams

PhydSI

hydrostaticpressureinthewellbore,expressedinkilopascals

Phyd,USc

hydrostaticpressure,inthewellbore,expressedinpounds-forcepersquareinch

R

RsG

densityhydrometercorrectedreadingatmeasuredtemperature,expressedingramspermilliliter

SGhydrometercorrectedreadingatmeasuredtemperature,dimensionless

R?

averagedensityreadingatthelowerbathtemperature

R?

VA-HCl

averagedensityreadingatthehigherbathtemperature

volumeofhydrochloricacidusedtothefirstpHendpoint,expressedinmilliliters

VB-HC

volumeofhydrochloricacidusedtoreachthesecondpHendpoint,expressedinmilliliters

VHC

volumeofhydrochloricacidadded,expressedinmilliliters

Vs

volumeofbrinesample,expressedinmilliliters

Zc

IDFG,SI

density-measuringdevice-correctioncurveslope,expressedinmeasuringdeviceunitpereitherdegreesCelsiusorperdegreesFahrenheit

drillingfluidgradientexpressedinkilopascalspermeter

DFG,USC

drilingfluidgradientexpressednponds-forcepersquareinchandperfoot(psi/t)calculatedfromdensityexpressedinpoundspergallon

DFG,USC-2

drillingfluidgradient,expressedinpoundspersquarefoot,calculatedfromdensityinpoundspercubicfoot

ApH

changeinpHafteradditionofhydrochloricacidaliquot(dimensionless)

6APIRECOMMENDEDPRACTICE13J

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△VHC

volumeofhydrochloricacidaliquotaddition,expressedinmililiters

θBH,SI

brinetemperaturemeasuredatbottomhole,expressedindegreesCelsius

θBH,USC

brinetemperature,measuredatbottomhole,expressedindegreesFahrenheit

θRef

samplereferencetemperatureofhydrometer,expressedindegreesCelsiusorFahrenheit

θsurf,SI

brinetemperaturemeasuredatthesurfaceorassumedtobe20℃,expressedindegreesCelsius

θsur,USC

brinetemperaturemeasuredatthesurfaceorassumedtobe70F,expressedindegreesFahrenheit

0m

measurementtemperature,expressedindegreesCelsiusorFahrenheit

θm,sI

measuredtemperature,expressedindegreesCelsius

θm,USC

measuredtemperature,expressedindegreesFahrenheit

θ?

averagetemperatureatthe