PROCEDURE

CORROSION INHIBITOR SCREENING TEST

LABORATORIUM PENGUJIAN INHIBITOR KOROSI - ITB

LAPI ITB May 2016

Content

1. Introduction

2. Test Procedure

2.1.
2.2.
2.3.
2.4.
2.5.
2.6.

Bubble test3
Jet impingement test5
Thermal Stability Test 6
Foaming Tendency Test
Emulsion Stabilization Test
FTIR Finger Printed Spectra8

3. Test Procedure Reference

6
7


1. Introduction
The following are the testing type to be carried out:
1. Bubble Testing
2. Jet impingement Testing
3. Thermal stability Testing
4. Emulsion stabilizing testing
5. Foaming tendency
6. IR Spectroscopy

2. The Corrosion Inhibitor Test procedure

2.1.

Bubble Testing

The bubble test is a flexible laboratory procedure for monitoring corrosion rates and inhibitor
performance. In the bubble test cell, the composition and temperature of the fluids in the field
can be simulated. The bubbles of the purging gas and very slowly stirred of magnetic bar
generate the fluid movement, so that no hydrodynamics correlation exists between the flow
condition in the test and those in pipelines.
The objective of this test is to provide the efficiency of corrosion inhibitor under low shear
stress condition. The corrosion inhibitors will be tested at 50 ppm/brine volume. The test will
be carried out in a sweet environment saturated with CO2 and a temperature of 50C in the
absence and in the presence of 20% hydrocarbon ( cyclohexane or kerosene) phase.
The testing glass cell consist of three electrodes system (Working Electrode = mild carbon
steel, Auxiliary Electrode = Pt, Reference electrode = saturated calomel) is filled with 1600 mL
of synthetic brine solution (1.9% NaCl, water analysis composition as Tabel 1) is exposed to
continuous CO2 bubbling with constant magnetic stirring. Figure 1 represent the cell set up for
bubble testing. Pre-corrosion time is 4 hours followed by LPR measurement to obtain the
baseline of corrosion rate. The inhibitors will be tested is injected to the testing solution (50
ppm/brine volume) after four hours LPR measurement of the baseline corrosion rate relatively
constant. Duration of the LPR measurement on the presence of 50 ppm corrosion inhibitor
would be carried out along 16 hours. pH and dissolved oxygen of testing solution will be
recorded at the beginning and at the end of LPR measurement. The bubble test shall be done
in duplicate.

Tabel 1.Water analysisof of the synthetic brine test solution

CationWater
in1litersolution:
19,459gNaCl
2,058gCaCl2.2H2O,
5,284gMgCl2.6H2O
0,082gBasCl2.2H2O,

AnionWater
in1litersolution:
19,459gNaCl
0,067gNa2SO4.10H2O;

SyntheticBrine
(2L)
38,919gNaCl
2,058gCaCl2.2H2O,
5,284gMgCl2.6H2O
0,082gBaCl2.2H2O,
.
0,067gNa2SO4 10H2O;

Figure1.Schematicdiagramoftheelectrochemicalcellusedforthebubbletest

Resultingdatafromthetestshallcover:
1) Plot of the corrosion rate and the polarization resistance versus time of each corrosion
inhibitorproduct.
2) Calculationofefficiencyofthecorrosioninhibitorbasedoncorrosionrateandpolarization
resistance.
Optionaltestingrequirementtothetestingprocedure:
1) The fluid composition in the bubble cell is 80% v/v brine: 20% v/v hydrocarbon. Brine
compositionis1.9%NaCl.
2) Hydrocarbon is saturated with CO2 (at least 1 hour continuous CO2 bubbling before it is
transferredtothebubblecell.Nocontaminationwithairduringtransferthehydrocarbonto
bubblecell).
3) BrineissaturatedwithCO2(atleast12hourscontinuousCO2 bubblinginthestoragetank,
beforethebrineistransferredtothebubblecell).
4) Durationofprecorrosionis4hours.
5) Durationofcorrosionmeasurementis16hours.
6) The bubble test shall be done in duplicate for each corrosion inhibitor product .and the
resultwillbetheaverageofthetwotestresults.

% CPE =

Rpi Rp0

x 100

(1)

Rpi
Rpi =polarization resistance in the presence of 50 ppm corrosion inhibitor
Rp0 =polarization resistance) of blank solution
or
% CPE =

CR0 CRi

x 100

( 2)

Rp0
CRi =corrosion rate in the presence of 50 ppm corrosion inhibitor
CR0 =corrosion rate of blank solution

2.2. Jet impingement test

Jet impingement is a widely used test methodology to study flowaccelerated corrosion for
evaluatingtheperformanceofcorrosioninhibitors.Thistestcouldbeusedtocompareamongthe
successful candidates from the previous electrochemical tests in term of its rate and strength of
adsorption under a varying high shear stress flow condition. The electrochemical measuring
techniques used in this type of testing is linear Polarization Resistance (LPR) techniques which is
undertakenonmildsteelelectrodeinsidealooptestchamber.Ajetofbrineisimpingeduponthe
working electrode while charge transfer resistance is monitored electrochemically in real time,
workingelectrodesassociatedwithturbulentflowregionswhichrepresentaworstsituationmeetin
service.Figure 2 (a) and Figure 2(b) represent respectively a schematic diagram of the
electrochemicalcellusedforjetimpingementtest,andschematicofringworkingelectrodeusedfor
jetimpingementtest.

The objective of this test is to evaluate the efficiency of corrosion inhibitor performance under a
known shear stress.The inhibitor concentration is 100 ppm/brinevolume. The testwill becarried
outinasweetenvironmentsaturatedwithCO2andatemperatureof40C.Thecalculatedwallshear
stressduringeachtypicalexperimentare150250Paforjetflowrateofapproximately500liters
/hour. The change in corrosion rate is followed with the progression of time as the adsorption
develop during the increase in inhibitor concentration of 100 ppm through a direct titration with
1275ppmofaninhibitorsolutionattheadditionrateofaround16.7mL/min.thepossibledecrease
in transfer resistance is followed with time of aging at constant shear stress level. Very persistent
monolayer will remain adsorbed and provide protection as shown by slow drop of transfer
resistance.Themeasurementisundertakenunderconstant150ml/minflowrateofcarbondioxide
gas at the temperature of around 400C in the absence of any hydrocarbon phase (kerosene).The
corrosionratesmeasurementwasconductedusingPotentiostat/GalvanostatVoltaLab30,PGZ301
RadiometerandcontrolledwithcorrosionanalysissoftwaremodelVoltaMaster4.Jet impingement
testing shall be done once only.

ThechangesofcorrosionratemonitoredbyLPRmeasurement
Thejetimpingementtestareundertakenonmildsteelelectrode(workingelectrode,surfacearea=
2.355cm2),auxiliaryplatinumelectrode(surfacearea=0.785cm2),andsaturatedcalomelreference
electrode.Thejetimpingementtestconditionwastemperatureof55oCof5000mLsyntheticbrine
(plusaddedvolumeofcorrosioninhibitorsolution)weresaturatedwithCO2(CO2pressureof1020
mbar above atmospheric pressures as a deoxygenated continuous purging gas inside the jet
impingementtestchamber).Onthistestcondition,Protectionefficiencyfactor(in%)forcorrosion
inhibitorcouldbecalculatedbyusingformulae:
%CPE=

Rp Rp0
x 100
Rp

Rp=polarizationresistancewithcorrosioninhibitor
Rp0=polarizationresistanceofblanksolution

Electricalwireof
workingelectrode

(a)

(b)

Figure2.(a)Schematicdiagramoftheelectrochemicalcellusedforjetimpingementtest,
(b)Schematicofringworkingelectrodeusedforjetimpingementtest

Data and data presentation resulting from the test shall cover at the minimum:
1) Corrosion inhibitor efficiency calculation.
2) Plot of corrosion inhibitor efficiency versus time of each corrosion inhibitor product.

2.3 Thermal Stability Test

The objective of this test is to evaluate the influence of thermal treatment on the corrosion inhibitor
stability. Thermal treatment is heating of corrosion inhibitor at 100C for 24 hours. Corrosion
inhibitor aging of heating treatment shall be done once only.After aging, the corrosion inhibitor
product is subject to observe visually and scanning its FTIR spectra .
Data and data presentation resulting from the test shall cover at the minimum:
1) The results are of a qualitative nature and provide information on the evolution of the corrosion
inhibitor solution against temperature and the blank sample (without corrosion inhibitor).
2) Photograph and FTIR spectra before and after heating treatment.

2.4 Foaming Tendency

The objective of this test is to assess the foaming tendency of brine/hydrocarbon emulsion in the
presence of corrosion inhibitor. The inhibitor concentration is 100 ppm/brine volume. The amount of
foam formed and foam life time is recorded and compared to a baseline obtained without addition of
the corrosion inhibitor (blank). Gas (air or nitrogen) flow for foaming the emulsion shall be measured
and recorded. Figure 3. Represent a schematic diagram of the set up.
The testing shall be done in duplicate. The test result is the average of the duplicate test. If the test
result from the duplicate test shows strong deviation (difference more than 20%), then the third test
shall be done, and he result will be the average of the three test results.

Figure 3. Schematic diagram of the set up

The resulting data obtained from the test shall cover at the minimum:
1) Table of result showing volume increase and foam life time.

2.5 Emulsion stabilizing tendency

The objective of this test is to assess the brine/hydrocarbon emulsion stabilizing tendency in the
presence of corrosion inhibitor. The inhibitor concentration is 100 ppm/brine volume. Evaluation of
emulsion forming tendency is carried out by comparing the decanting rates at ambient temperature of
brine/hydrocarbon mixtures emulsified in the volumetric cylinder. The results give the volumes of brine
decanted with time, and are compared to a blank with no addition of corrosion inhibitor. Figure 4
representing a schematic diagram of the set up. The testing shall be done in duplicate. The test result
is the average of the duplicate test. If the test result from the duplicate test shows strong deviation
(difference more than 20%), then the third test shall be done, and the result will be the average of the
three test results.
Equipment:
2 volumetric cylinder of 100 and 250 mL
1 sample bottle of 250 mL equipped with a lid
1 micro syringe of 100 L
1 stopwatch and a ruler

Figure 4.Schematic diagram of the set up.

Test procedure:
This test procedure will be first carried out in absence of corrosion inhibitor in order to obtain a
reference line.
1. Preparing the emulsion
In the 250 mL sample bottle, add 145 mL of brine and 55 mL of hydrocarbon.
Measure with the ruler the height of the brine and hydrocarbon phase.
Inject the corrosion inhibitor in its more soluble phase (145 L of inhibitor to be tested).
Place the lid of he sample bottle and mixed vigorously during 1 minute in order to create an
emulsion. After the mixing step leave the sample bottle on a flat surface and start the
stopwatch.
2. Measurements.
Using the ruler, measure against time:
The height of the brine decanted
The height of the decanted hydrocarbon layer
After 10 minutes of settling, the test is finished.
3. Results:
The test will first be carried out in the absence of inhibitor
The test will be repeated 3 times and the final result will be an average of the three
measurements.
The results will be expressed as a percentage of each phase decanted versus time from the
initial volume (i.e. % of brine decanted, % hydrocarbon decanted, % remaining emulsion).
The percentage volume of the remaining emulsion is calculated by substracting the brine from
the initial total volume.
An histogram representation versus time will be drawn
Data and data presentation resulting from the test shall cover at the minimum:
1) Histogram of the emulsion separation process.
2) Bar diagram of the final results at time = 10 minutes.
3) Photograph of brine/hydrocarbon emulsion at time = 10 minutes.

2.6 IR Spectroscopy
The objective of this test is to obtain fingerprint of the tested corrosion inhibitor product. It is carried
out with common IR spectrometric methods.The testing shall be done in once only.
Data and data presentation resulting from the test shall cover at the minimum:
1) Plot of fingerprint obtained from common IR Spectroscopy, transmitans vs wave number plot.

3. Test Procedure Reference

1. ASTM G 1 -2004, Standard PracticeforPreparing, Cleaning, and EvaluatingCorrosion Test
Speciment,ASTM International, PA, USA.
2. ASTM G 5-2004, Standard References Test MethodforMakingPotentiostatic and
PotentiodynamicAnodicPolarizationMeasurement, ASTM Inrternational PA, USA.
3. ASTM G 170 2006, Standards, Standard Guide for Evaluation and Qualifying Oilfield and
Refinery Corrosion Inhibitors in the Laboratory, ASTM Inrternational PA, USA.
4. ASTM
G
59-2009,
Standard
Test
MethodforConductingPotentiodynamicPolarizationResistanceMeasurement,
ASTM
Inrternational PA, USA
5. TOTALFINAs Procedure for Screening Corrosion Inhibitors (A.HOULIER, G. GAZUC AND
A. BELGHAZI, Process and Refining Department, Electrochemistry-Corrosion Section,
August 2000 and Emetteur 20/04/2009