enm 233 coursework

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Due Date Date Submitted For official use only

13th April 2014

10th April 2014 LATE DATE

MATRIC No 1300000

SURNAME ANTOINE

FIRST NAME(S) GERARD

COURSE & STAGE

MSc Oil & Gas Engineering

MODULE NUMBER & TITLE ENM233 Materials & Corrosion INDIVIDUAL COURSEWORK

ASSIGNMENT TITLE Corrosiveness of Bottled Mineral Water (Rusty Nail Experiment)

LECTURER ISSUING COURSEWORK Owen Jenkins

I confirm: (a) That the work undertaken for this assignment is entirely my own and that I have not made use of any unauthorised assistance.

(b) That the sources of all reference material have been properly acknowledged. [NB: For information on Academic Misconduct, refer to

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Signed Gerard Natoine............................ Date ............13th/04/2014........................

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Materials and Corrosion Science 2014


RUSTY NAIL CORROSION EXPERIMENT

NAME : Gerard Antoine STUDENT ID : 1300000 COURSE CODE: ENM 233 DATE : 13th/04/2014


TABLE OF CONTENTS

GLOSSARY ............................................................................................................................ 1

LIST OF FIGURES .............................................................................................................. 1

LIST OF TABLES ................................................................................................................. 1

EXECUTIVE SUMMARY ..................................................................................................... 2

1.0 INTRODUCTION ......................................................................................................... 2

2.0 OBJECTIVES ................................................................................................................ 2

3.0 METHOD and MATERIALS ....................................................................................... 3

3.1 Materials ................................................................................................................. 3

3.2 Method .................................................................................................................... 3

4.0 RESULTS ....................................................................................................................... 5

5.0 ANALYSIS ................................................................................................................... 10

5.1 Still Water (SMW) Corrosion Cell ......................................................................... 11

5.2 Brackish Water Corrosion Cell .............................................................................. 12

5.3 Carbonated Water Corrosion Cell ........................................................................ 13

6.0 CONCLUSION ............................................................................................................ 14

APPENDIX 1 – THREE (3) DAY INTERVAL PHOTOGRAPHIC RECORD OF

EXPERIMENT OBSERVATIONS GIVEN IN TABLE 1 (A-E) ........................................... 16

APPENDIX 2 – ORIGINAL COMPOSITION AND PH OF STILL AND CARBONATED

WATER USED IN THE EXPERIMENT ................................................................................ 17


1

GLOSSARY

BW Brackish Water

SMW Still Mineral Water CW Carbonated Water Fe Iron

LIST OF FIGURES

Figure 1.0: Summary of procedure for rusty nail experiment Figure 2.0: pH changes of brackish, still and carbonated water solutions Figure 3.0: Pourbaix diagram for iron- water system at 25°C and 1 atm.

Figure 4.0: Physical condition of nail after removed from still water Figure 5.0: Physical condition of nail after removed from brackish water

Figure 6.0: Physical condition of nail from carbonated water Figure 7.0: Permanent orange stain on glass jar

LIST OF TABLES

Table 1.0: Corrosive effects of brackish, still and carbonated water (a-e) on steel nails Table 2.0: Initial compositions and pH of the Still Mineral Water solution

Table 3.0: Initial compositions and pH of the Carbonated Water solution


2

EXECUTIVE SUMMARY

This report examined the effects of corrosion mechanisms on steel nails

immersed in aqueous environments.

Methods of analysis included visual observations and measurements of

pH and temperature over a fifteen day duration.

The report found that corrosion had occurred in each test solution.

However, due to the parameters measured no definite conclusions with

respect to corrosion rate and overall effect on the steel nail could be

ascertained.

1.0 INTRODUCTION

In general, corrosion can be regarded as the degradation of metals via

chemical and electrochemical reactions with its environment (Bardal

2004). The cost of corrosion in the oil and gas industry is high in terms of

prevention and maintenance overheads and can have disastrous effects

on production, people and the environment if not properly controlled. As

a result, acquiring an understanding of the mechanisms which support or

prevent corrosion is important. In this report an experiment was

conducted under controlled conditions in order to ascertain the cause and

effects of corrosion on three mild steel nails placed in different wet

environments.

2.0 OBJECTIVES

The objectives of this report are as follows:

1. Outline and explain the chemical and electrochemical reactions

behind the physical changes observed with the nail and its

environment;

2. Demonstrate the thermodynamics and electrode kinetics involved

in the observed reaction through the use of Pourbaix or Evans

diagrams;

3. Recommend further test that could be implemented to support

deductions and conclusions made.


3

3.0 METHOD and MATERIALS

The following is an overview of the procedures and materials used to

establish three wet environments in which steel nails were submerged,

and monitored.

3.1 Materials – Materials used to conduct this experiment were;

1. A 550 ml measuring bottle

2. A graduated tea spoon (5.0 ml)

3. A room temperature thermometer range -40 to +50 °C

4. Two 250ml glass jars

5. One 1L glass jar

6. A digital pH meter with acid/alkali calibration solution

range 4.0 to 10 on the pH scale.

7. Three steel nails

8. One jar of sea salt

9. One bottle of carbonated water

10.One bottle of still mineral water

3.2 Method – A 500ml bottled sample of carbonated and still

mineral water were obtained randomly from a commercial

outlet. The bottled carbonated water was placed to stand

undisturbed for 24 hours. During this period 550ml of tap

water was measured using a measuring bottle and placed in

the 1L glass jar. One teaspoon of sea salt (5.0ml) was then

added to the jar containing the tap water and mixed vigorously

for five minutes. The 1L jar containing the salt water was then

closed and left to stand. Subsequently, a second test solution

was prepared. Here the still mineral water was used to fill one

of the 250ml glass jars. Both jars were immediately covered

and labelled based on content and date. Finally, after 24 hours

had expired, the remaining 250ml glass jar was prepared with

the carbonated water in a similar fashion to that described for

mineral water. However additional care was taken not to

severely agitate the carbonated water whilst pouring.

With the three solutions prepared the entire surface area of

each of the three steel nails were thoroughly polished using


4

very fine sand paper. Care was taken not to contaminate the

polished surfaces by handling with a tweezers and dry paper

towels.

The pH of each of the three prepared solutions were checked

with a calibrated digital pH meter and recorded. The ambient

room temperature was recorded using a room thermometer

and a freshly polished nail subsequently immersed into each of

the three jars containing the salt, carbonated and still mineral

water test solutions. All three jars were subsequently observed

continuously for 25 minutes and observations noted.

The pH test, observation notes and room temperature

recordings were then repeated daily for eleven days after

which each sample solution was vigorously shaken and re-

observed daily for an additional four days (see figure 1).

At the end of a fifteen day period the contents of each test jar

was poured into large white ceramic bowls and closely

observed to gauge the overall effect of corrosion mechanisms.

Figure 1: Summary of procedure described for the rusty nail experiment

SH

AK

EN

AF

TE

R

11

DA

YS


5

4.0 RESULTS

In this section the results of all observations made over the fifteen day

duration of the experiment would be presented. The tabulated daily

records shown in table 1.0 revealed that corrosive reactions were not

confined to the surface of the steel nails but also caused changes to the

pH of the solutions and transparency of the glass containers respectively.

See Appendix 1 for the corresponding photographic record.

Table 1a: Corrosive effects of brackish (BW), still (SMW) and carbonated water (CW) on steel nails.

Date Temp.

(°C)

I.D. PH Physical Observations

22/03/14

(Day 1)

25 BW 7.9 After 25 minutes a slight greenish brown tinge

was seen forming on a small are of the nail

surface. Water remained clear.

SMW 7.0 No visible change in nail, water remained clear

CW 5.3 Carbonated water fizzed violently on adding the

nail. Gas bubbles approximately 2mm in

diameter were seen quickly forming on the

surface of the nail before floating up

(Appendix1). After 25 minutes no visible

change was seen, however size of bubbles

decreased to approx. 1.5 mm.

23/03/14

(Day 2)

24 BW 7.6 Water appeared slightly cloudy. A light red

brown oxide layer formed on sides and upward

facing surface of nail with the exception of an

area approximately 5mm below the nail head

which remained silver. A thin brown film was

also seen at the base of the jar surrounding the

nail in an irregular fashion. Directly below the

outer edges of the nail small piles of oxide

flakes were seen deposited. The base of the

nail in contact with the jar did not develop any

oxide film.

SMW 7.2 Water transparency reduced slightly. 50%

upward nail surface covered with a brown oxide

film, sides and base of nail unaffected. A thin

brown film was also seen surrounding nail at

base of jar in a semi-circular shape.

CW 5.3 Oxide film at surface of nail looked dark

grey/black in colour. No film was seen on the

base of jar and bubbles forming on nail surface

was reduced in size to approximately 1 mm.

Water remained clear.

24/03/14

(Day 3)

24 BW 7.5 Thickness of oxide layer on upward side of nail

noticeably thicker. Spread of brown film on jar

had increased and solution transformed from

murky white to slightly brown in colour.


6

Table 1b: Corrosive effects of brackish (BW), still (SMW) and carbonated Water (CW) on steel nails.

Date Temp.

(°C)


24/03/14 24 SMW 7.2 Brown oxide film now spread uniformly

throughout upward nail surface. Sides of nail

showed patches of film developing but silver

surface remained largely visible. The brown

film surrounding the nail at the base had

increased in thickness but had not spread

giving a dark brown appearance.

CW 5.5 Water remained clear. Oxide film colour on

upward nail surface increased in intensity and

seemed black. No film seen at base of jar or

underside of nail. Bubbles forming on surface

of nail had reduced in rate of formation,

quantity as well as diameter.

25/03/14

(Day 4)

24 BW 7.5 Upward and side of nail with the exception of

nail head and strip 5mm below was now

completely covered by a thick oxide layer

(Appendix1). Brown thin film at base of jar no

longer looked uniform in texture but was

speckled by solid oxide flakes. A small pocket

of water condensation was seen on the wall of

the jar.

SMW 7.3 No major change in condition of nail. Water

seemed to have developed a light brown tinge.

CW 5.7 Water seemed slightly murky and had

developed a translucent greenish red slightly

oily film at the surface. No change on the

surface of the nail was observed.

26/03/14

(Day 5)

24 BW 7.5 The region near the nail head remained

seemingly untouched by the surrounding brown

oxide layer had noticeably reduced by the

oxide film. The quantity of oxide flakes present

at the base of the jar however had increased

and a transparent brown film had formed on

the vertical walls of the jar covering a height of

approximately 20mm from the base.

SMW 7.5 The brown oxide layer on the upward surface

of the nail had noticeably increased in

thickness. The sides of the nail were almost

completely covered by patches of oxide film.

CW 5.9 A uniform finely powdered brown oxide film

now covered the top and sides of the nails as

well as the entire base of the jar. Bubbles

resting on the surface of the nail had reduced

in size and quantity. Only very small bubbles

now rose to the surface from around the edges

of the nail. The translucent oily film was still

present but the colour reflected was changing

from light reddish brown to a darker shade.


7

Table 1c: Corrosive effects of brackish (BW), still (SMW) and carbonated water (CW) on steel nails.

Date Temp.

(°C)


27/03/14

(Day 6)

24

BW 7.5 No noticeable change observed

SMW 7.7 No major changes with the exception that the

sides of the nail were now completely covered

with a brown oxide layer.

CW 6.0 Water appeared to now have a distinct orange/

brown colour. The fine uniform brown film on

the nail and at the base of the jar had increase

in thickness. Most of the nail surface was now

bubble free with minor exceptions, Barely

noticeable bubbles were seen rising from the

edges of the nail

28/03/14

(Day 7)

24 BW 7.5 No noticeable change observed

SMW 7.7 No noticeable change observed

CW 6.2 Water appeared to be a darker shade of

orange/brown colour (Appendix 1). Bubbles

now seldomly seen either on the nail surface or

rising.

29/03/14

(Day 8)

25 BW 7.5 Deposition of oxides flakes at base of jar

seemed to increase. The thin transparent

brown film on the walls of the jar had also

increased slightly in height.

SMW 7.6 Water seemed murkier in appearance. Larger

piles of oxide flakes had accumulated directly

below the edges of the nail.

CW 6.3 Brown film at the base of the jar increased in

thickness and became opaque. No noticeable

change in the nail surface.

31/03/14

(Day 9)

24 BW 7.4

No noticeable change observed

SMW 7.7

CW 6.4

1/04/14

(Day 10)

25 BW 7.3

SMW 7.7 Small reddish brown oxide flakes now seen

sparsely scattered on the once uniformly

textured brown film at base of jar

CW 6.5 Increase in the intensity of the orange brown

colour of the water observed.


8

Table 1d: Corrosive effects of brackish (BW), still (SMW) and carbonated water (CW) on steel nails.

Date Temp.

(°C)


3/04/14

(Day 11

Shaken)

24 BW 7.4 Pre-Shake: Noticeable increase in the build-up

of brown oxide layer on upward face of nail and

in the immediate vicinity at an approximate

radius of 3mm.

Post Shake: Water now an opaque light brown

colour nail no longer visible from surface. At

base of jar reddish brown oxide flakes were not

suspended and accumulated in centre of jar.

SMW 7.7 Pre-Shake: No change in water colour but

oxide layer on the nail surface transitioned

from a light brown to a reddish brown colour.

Post Shake: Solution became cloudy with a

substantial amount of dark red oxide flakes

accumulating at the base of the jar. The oxide

layer that previously coated the nail was

completely dislodged and a dull grey gleam

throughout the surface of the nail was seen.

CW 6.4 Pre-Shake: Film at the base of jar had

become completely opaque. Water colour still

appeared to be a dark reddish/brown shade. No

bubbles were observed on or around the nail.

Post Shake: Water colour remained the same.

Solution no longer transparent. Insoluble fairly

big oxide flakes were seen swirling in the

mixture. The opaque brown film at the base of

the jarl had remained intact. As a result the

nail was not visible (Appendix 1)

4/04/14

(Day 12)

24 BW 7.4 Transparency of water had improved and was

now comparable to initial experiment state.

Oxide film looked very similar in composition

and texture to pre-shaken conditions. However

the brown film at the base of the jar had now

been dispersed and replaced by fairly large

quantities of brown flaky crumb like oxide

solids. These brown oxides particle

accumulated in small mounds throughout the

base of the jar. The reddish brown oxides

flakes apparent immediately after shaking the

sample was now sparsely distributed amongst

these mounds.

SMW 7.7 Water seemed cloudier than the pre-shaken

sample reducing the visibility of the nail.

However the nail seemed totally covered by a

loose looking brown oxide layer.

CW 6.5 Visibility of nail was reduced as water became

less transparent. However the nail seemed to

be free of any noticeable oxide layer as a dull

grey gleam was seen throughout the surface.

The reddish brown oily film at the surface of

the water had completely dissipated.


9

Table 1e: Corrosive effects of brackish (BW), still (SMW) and carbonated water (CW) on steel nails.

Date Temp.

(°C)


5/04/14

(Day 13)

25

BW 7.3

No apparent change was observed SMW 7.6

CW 6.8 A uniform finely textured reddish brown

oxide film had reformed on the exposed

surfaces of the nail. The opaque film at the

base of the jar was no longer uniform but

was speckled with small thin glossy looking

flakes.

7/04/14

(Day 14)

25 BW 7.4

No apparent change was observed

SMW 7.6

CW 7.3

8/04/14

(Day 15)

24 BW 7.3 The height of the transparent brownish film

on the vertical walls of the jar had

increased from 20 to 35mm.

SMW 7.6 The transparency of solution remained

murky however short piles of oxide flakes

was seen on the base of the jar around the

edges of the nail (Appendix 1).

CW 7.9 No apparent change was observed

The observations presented in tables 1(a-d) were taken at fairly

consistent ambient room temperatures which varied mostly between +/-

1°C giving a mean temperature of 24.4 °C. This allowed trends in the pH

of the three test solutions to be identified.

5.0

6.0

7.0

8.0

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15

PH

No. of Days

BW (pH)

SMW (pH)

CW (pH)

Figure 2: pH changes for the brackish, still and carbonated test solutions

SMW

AG

ITATED


10

As shown in figure 2 the pH of the Brackish Water (BW) decreased

steadily whilst the Still Mineral (SMW) and Carbonated Water (CW) pH

values increased. The reasons for this and its relationship to ongoing

corrosion mechanisms would be explained in the following section of this

report.

5.0 ANALYSIS

In this experiment the corrosive mechanisms was largely attributed to

wet corrosion which, according to Garverick 1994, can be defined

typically by electrochemical processes in the presence of water containing

corrosion products of various solubility’s and concentrations.

Another significant consideration was the metallurgy of the material

tested. Here the metal used was steel which consisted primarily of iron

(Fe). In addition, the experiments were conducted at a mean

temperature of 24.4°C under atmospheric conditions. As a result, the

Pourbaix diagram for iron at 25°C (298K) and 1 atmosphere (see figure

3) was used to predict and explain reactions such as corrosion, non-

corrosion and passivation of the steel nails whilst immersed in their

respective aqueous environments.

Figure 3: Pourbaix diagram for an iron-water system at

1atm and 25°C (298K) (Pourbaix and Verink 1971)

ACTIVE

CORROSION

PASSIVITY

IMMUNITY

CORROSION


11

5.1 Still Water (SMW) Corrosion Cell

Figure 4: Physical condition of nail after removed from still water

In describing the corrosion mechanism that resulted in the corroded

effects on the steel nail shown in figure 4, it is best to first examine

the least highly oxidised form of iron given by equation 1.

Fe Fe2+ + 2e- (1)

This mechanism whereby iron is dissolved is considered active

corrosion and is outlined in the Pourbaix diagram between line 23,

26, 28 and 20 for ionic Fe concentrations greater than 10-6. This

system is analogous to day 1 observations where no physical changes

were evident. However this reaction was affected by the increasing

pH of the SMW shown in figure 2. At the measured pH of 7.2 on day

2 (see table 1a), the reaction reached the region bounded by line 26

on the Pourbaix diagram. Here ferric hydroxide Fe(OH)3 (rust) was

observed in the form of a red brown film that appeared on the

upward facing surface of the nail and at the base of the jar. The

chemical equation for this reaction is given below.

4Fe + 3O2 +6H2O 4 Fe(OH)3 (2)

As time progressed during the experiment, the iron in the steel nail

formed a passive Magnetite oxide layer Fe3O4.

3Fe + 4H2O Fe3O4 + 8H+ + 8e- (3)

Evidence of this reaction was confirmed by the dark grey black

patches shown on the nail in figure 4 which appeared to be greenish

black when initially removed from solution but quickly turned into

black patches when dried of with paper towels (dehydrated Fe3O4).

This differentiated Magnetite from the other stable passive layer

Haematite (Fe2O3) which is red brown in colour. In addition, due to

Area with a light reddish/brown stain

Black/dark grey patches spotted on upper and

lower area of nail


12

the production of hydrogen ions, this reaction would account for the

decrease in pH values after day 7(see figure 2).

The initial composition and pH of the SMW used in this experiment

was also examined to deduce if any additional passive or corrosive

mechanisms could be identified (see Appendix 2). Two compounds of

interest were identified namely chlorides and bicarbonates in

concentrations of less than 240 and less than 11 mg/l. The chloride

content was thought to have a negligible effect due to the small

quantities, and considering that the pH at source was 7.4, the

possibility that the concentration of carbonic ions from dissolved

bicarbonate was high enough to create acidic conditions was

dismissed.

5.2 Brackish Water Corrosion Cell

Figure 5: Physical condition of nail after removed from brackish water

As shown in figure 5 the steel nail was covered in a passive uniform

layer of Magnetite oxide layer Fe3O4. The chemical reactions were

similar to that described by equations 1 – 3. The major difference

was the higher concentration of chloride ions (Cl-) which increased

the conductivity of the electrolyte and the rate of corrosive reactions.

This was evident by the large quantities of ferric hydroxide or brown

rust particles that accumulated in the jar over the duration of the

experiment compared to the other test solutions. Another indicator of

the increased reaction rate of reaction was the speed at which

physical changes were observed (see table 1) and the sharp rate of

Uniform

black/dark grey film


13

initial decline in pH value (see figure 2) before the passive oxide layer

(Fe3O4 ) was formed.

5.3 Carbonated Water Corrosion Cell

Figure 6: Physical condition of nail after removed from carbonated water

The carbonic acid theory stipulates that carbonic acid reacts with iron to

form carbonates whilst releasing hydrogen which bonds with oxygen in

the air to breakdown ferrous carbonate to ferric hydroxide (Sang 1910).

The equations describing these processes are given below:

2Fe + 2CO2 + 2H2O 2FeCO3 + 4H+ (4)

4H + 2FeCO3 +3O Fe2O3 + 2CO2 +2H2O (5)

Fe +2CO2 + H2O + ½ O2 Fe(HCO3)2 (6)

2Fe(HCO3) + H2O + ½ O2 2Fe(OH)CO3 + 2CO2 +2H2O (7)

2Fe(OH)CO3 +2H2O 2Fe(OH)3 + 2CO2 (8)

2CO2 + 2H2O 2H2CO3 (9)

H2CO3 H+ + HCO3

- (10)

From examination of equation 5 above, it can be seen that the reddish

brown oxide film on the surface of the nail shown in figure 6 was

Haematite (Fe2O3). According to Bardal 2004 Haematite is known for its

non-porous stable and good adherence to substrate abilities. These

properties were proven by the fact that the oxide layer which

accumulated on the nail and at the base of the jar did not totally detach

after the sample was vigorously shaken.

Reddish brown film


14

Figure 7: Permanent orange stain on glass jar that contained the nail and carbonated water.

The effect of glass corrosion was seen on the surface of glass after the

test solution was poured out. This was attributed to sharp increases in pH

which caused leaching of alkali ions from the surface of the glass into the

carbonated water (Perkoff and Beyers 2001). As a result the

concentrations of silica on the surface of the glass increased changing its

colour to orange as shown in figure 7.

6.0 CONCLUSION

In conclusion all three samples showed signs of corrosion and

development of passive layers. However some ambiguity existed with

respect to the determination of the rate and quantity of corrosion that

occurred in each test. From a visual perspective (see Appendix1) the rate

of corrosion seemed to be fastest with the brackish water sample,

however when considering the electrochemical/chemical reactions

reflected in the pH measurements (see figure 2) the carbonated water

test solution seemed to be most active. Therefore a recommendation

could be to include measurements of mass and potentials in future

experiments. This would make the effect of corrosion on each metal

quantifiable as well as allow for the practical use of the Evans diagram in

determining the reaction kinetics.


15

REFERENCES

BARDAL, E., 2004. Corrosion and Protection. London, UK. Technomic Publishing Company, Inc.

GARVERICK, L., 1994. Corrosion in the Petrochemical Industry. ASM

International.

POURBAIX, M. and VERINK, E., 2011. Pourbaix diagram for Iron and Water system at 1atm and 25°C 1971. In: R. W. REVIE, 2011. Uhlig’s Corrosion Handbook: 3rd Edition: New York:John Wiley and Sons. P. 107.

PERKOFF and BEYERS, 2001. Destruction of Glass surfaces: Inevitable or

Preventable?. [online]. Ritech International ltd. Available from

http://www.ritec.co.uk/cmsfiles/International_Glass_Review.pdf

[Accessed 5 April 2014].

SANG, A., 1910. The Corrosion of Iron and Steel. New York, USA. Mc Graw Hill Book Comoany.

http://www.ritec.co.uk/cmsfiles/International_Glass_Review.pdf


16

APPENDIX 1 – THREE (3) DAY INTERVAL PHOTOGRAPHIC RECORD OF

EXPERIMENT OBSERVATIONS GIVEN IN TABLE 1 (A-E)

DAY 1

BRACKISH CARBONATED STILL MINERAL

DAY 4

DAY 7

DAY 11 (AGITATED SOLUTION)

DAY 15 (Final Day)


17

APPENDIX 2 – ORIGINAL COMPOSITION AND PH OF STILL AND

CARBONATED WATER USED IN THE EXPERIMENT

Original composition and pH of the Still Mineral Water (SMW)

Composition Quantity (mg/litre)

Calcium <55.0

Magnesium <16.0

Potassium <2.0

Sodium <15.0

Bicarbonate <240.0

Sulphate <28.0

Nitrate <6.0

Chloride <11.0

pH at source 7.4

Original composition and pH of the Carbonated Water (CW)

Composition Quantity (mg/litre)

Calcium 55.0

Magnesium 19.0

Potassium 1.0

Sodium 15.0

Bicarbonate 248.0

Sulphate 13.0

Nitrate <0.1

Chloride 37.0

pH at source 7.4

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