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Corrosion Science 50 (2008) 2493–2497

Corrosion Science 50 (2008) 2493–2497 Contents lists available at <a href=ScienceDirect Corrosion Science journal homepage: www.elsevier.com/locate/corsc i Quantitative analysis of iron oxides using Fourier transform infrared spectrophotometry H. Namduri, S. Nasrazadani * College of Engineering, University of North Texas, Denton, TX-76207, USA article info abstract Article history: Received 14 August 2007 Accepted 17 June 2008 Available online 4 July 2008 In this study, a systematic approach based on the application of Fourier transform infrared spectropho- tometry (FTIR) was taken, in order to quantitatively analyze the corrosion products formed in the sec- ondary cycle of pressurized water reactors (PWR). Binary mixtures of iron oxides were prepared with known compositions containing pure commercial magnetite (Fe O ), maghemite ( -Fe O ), and hematite ( -Fe O ) for calibration purposes. Calcium oxide (lime) was added to all samples as a standard reference Keywords: in obtaining the calibration curves. Using regression analysis, relationships were developed for intensity versus concentration for absorption bands cor responding to each of the phases in their corresponding A. Steel B. FTIR spectrum. Correlation coe ffi cients, R , of 0.82, 0.87, and 0.86 were obtained for maghemite–magne- IR spectroscopy C. tite, hematite–magnetite, and hematite–maghemite systems, respectively. The calibration curves gener- Rust C. ated were used to quantify phases in multi-component unknown field samples that were obtained from Oxidation C. different components (moisture separators, condensers, and high and low pressure heaters) of the two units (units 1 and 2) of the secondary cycle of the Comanche Peak PWR. © 2008 Elsevier Ltd. All rights reserved. Passivity 1. Introduction Formation and transformation of iron oxides is of interest to a wide variety of industries including steel making, power generat- ing, paint systems, pharmaceutical, and petrochemical, to name a few. The thermal hydraulic performance and integrity of the steam generators in nuclear power plants may be compromised due to the presence of cor rosion deposits. The amount of iron transported in a steam generator is dependent on the composition of iron oxide formed in the feed train. Deposits that contain well crystallized magnetite and maghemite are more stable than deposits contain- ing a combination of oxides and oxyhydroxides [1] . Therefore, it is very important to quantitatively understand the composition of the deposits. Standard methods for identifications and characterizations of iron oxides have traditionally used either X-ray diffraction (XRD) or Mössbauer spectroscopy (MS) [2] . XRD has been widely used in characterizing cor rosion products. Although these techniques have served industry well in the past, they suffer from shortcom- ings that could be replaced by Fourier transform infrared spectro- photometry (FTIR). MS is a technique that utilizes a live radioactive source, which makes the technique relatively unsafe from an oper- ational point of view, since it poses a potential health risk to the operator. The main limitations of MS technique include the level * Corresponding author. Tel.: +1 940 565 4052; fax: +1 940 565 2666. E-mail address: nasr@unt.edu (S. Nasrazadani). 0010-938X/$ - see front matter © 2008 Elsevier Ltd. All rights reserved. doi:10.1016/j.corsci.2008.06.034 of operator expertise requirements and the complexity of spectral interpretation. Even though XRD is easier to operate and interpret, its spectra is limited in its ability in differentiating magnetite and maghemite. On the other hand, FTIR instrumentation is simple and spectra interpretation is relatively easy [3] . In the past, it has been estab- lished that the FTIR technique can be routinely used to e ffi ciently differentiate and quantify different iron oxides and oxyhydroxides. To the best knowledge of the authors, no attempts have been made in using FTIR for quantitative analysis of iron oxides formed in the power plants. The main objective of this research is to quantify iron oxide phases formed in the secondary side of the steam gener- ator units at Comanche peak steam electric station (CPSES). Such analysis will allow better interpretation and control of the cor ro- sion process. 2. Literature review Magnetite is a well-known form of iron oxide that forms at room temperature in crevices between steel plates and at elevated temperature inside boiler tubes, heat exchangers etc. The oxida- tion product of Fe O is either -Fe O or -Fe O depending on the oxidation temperature and/or possibly the crystallite size of the starting magnetite [4–5] . Studies performed by Nasrazadani and Raman [4] have shown that transformation of magnetite to hematite goes through the for- mation of maghemite. The production of maghemite begins with " id="pdf-obj-0-5" src="pdf-obj-0-5.jpg">

Contents lists available at ScienceDirect

Corrosion Science

Corrosion Science 50 (2008) 2493–2497 Contents lists available at <a href=ScienceDirect Corrosion Science journal homepage: www.elsevier.com/locate/corsc i Quantitative analysis of iron oxides using Fourier transform infrared spectrophotometry H. Namduri, S. Nasrazadani * College of Engineering, University of North Texas, Denton, TX-76207, USA article info abstract Article history: Received 14 August 2007 Accepted 17 June 2008 Available online 4 July 2008 In this study, a systematic approach based on the application of Fourier transform infrared spectropho- tometry (FTIR) was taken, in order to quantitatively analyze the corrosion products formed in the sec- ondary cycle of pressurized water reactors (PWR). Binary mixtures of iron oxides were prepared with known compositions containing pure commercial magnetite (Fe O ), maghemite ( -Fe O ), and hematite ( -Fe O ) for calibration purposes. Calcium oxide (lime) was added to all samples as a standard reference Keywords: in obtaining the calibration curves. Using regression analysis, relationships were developed for intensity versus concentration for absorption bands cor responding to each of the phases in their corresponding A. Steel B. FTIR spectrum. Correlation coe ffi cients, R , of 0.82, 0.87, and 0.86 were obtained for maghemite–magne- IR spectroscopy C. tite, hematite–magnetite, and hematite–maghemite systems, respectively. The calibration curves gener- Rust C. ated were used to quantify phases in multi-component unknown field samples that were obtained from Oxidation C. different components (moisture separators, condensers, and high and low pressure heaters) of the two units (units 1 and 2) of the secondary cycle of the Comanche Peak PWR. © 2008 Elsevier Ltd. All rights reserved. Passivity 1. Introduction Formation and transformation of iron oxides is of interest to a wide variety of industries including steel making, power generat- ing, paint systems, pharmaceutical, and petrochemical, to name a few. The thermal hydraulic performance and integrity of the steam generators in nuclear power plants may be compromised due to the presence of cor rosion deposits. The amount of iron transported in a steam generator is dependent on the composition of iron oxide formed in the feed train. Deposits that contain well crystallized magnetite and maghemite are more stable than deposits contain- ing a combination of oxides and oxyhydroxides [1] . Therefore, it is very important to quantitatively understand the composition of the deposits. Standard methods for identifications and characterizations of iron oxides have traditionally used either X-ray diffraction (XRD) or Mössbauer spectroscopy (MS) [2] . XRD has been widely used in characterizing cor rosion products. Although these techniques have served industry well in the past, they suffer from shortcom- ings that could be replaced by Fourier transform infrared spectro- photometry (FTIR). MS is a technique that utilizes a live radioactive source, which makes the technique relatively unsafe from an oper- ational point of view, since it poses a potential health risk to the operator. The main limitations of MS technique include the level * Corresponding author. Tel.: +1 940 565 4052; fax: +1 940 565 2666. E-mail address: nasr@unt.edu (S. Nasrazadani). 0010-938X/$ - see front matter © 2008 Elsevier Ltd. All rights reserved. doi:10.1016/j.corsci.2008.06.034 of operator expertise requirements and the complexity of spectral interpretation. Even though XRD is easier to operate and interpret, its spectra is limited in its ability in differentiating magnetite and maghemite. On the other hand, FTIR instrumentation is simple and spectra interpretation is relatively easy [3] . In the past, it has been estab- lished that the FTIR technique can be routinely used to e ffi ciently differentiate and quantify different iron oxides and oxyhydroxides. To the best knowledge of the authors, no attempts have been made in using FTIR for quantitative analysis of iron oxides formed in the power plants. The main objective of this research is to quantify iron oxide phases formed in the secondary side of the steam gener- ator units at Comanche peak steam electric station (CPSES). Such analysis will allow better interpretation and control of the cor ro- sion process. 2. Literature review Magnetite is a well-known form of iron oxide that forms at room temperature in crevices between steel plates and at elevated temperature inside boiler tubes, heat exchangers etc. The oxida- tion product of Fe O is either -Fe O or -Fe O depending on the oxidation temperature and/or possibly the crystallite size of the starting magnetite [4–5] . Studies performed by Nasrazadani and Raman [4] have shown that transformation of magnetite to hematite goes through the for- mation of maghemite. The production of maghemite begins with " id="pdf-obj-0-16" src="pdf-obj-0-16.jpg">

Quantitative analysis of iron oxides using Fourier transform infrared spectrophotometry

  • H. Namduri, S. Nasrazadani *

College of Engineering, University of North Texas, Denton, TX-76207, USA

article

info

abstract

Article history:

Received 14 August 2007 Accepted 17 June 2008 Available online 4 July 2008

In this study, a systematic approach based on the application of Fourier transform infrared spectropho- tometry (FTIR) was taken, in order to quantitatively analyze the corrosion products formed in the sec- ondary cycle of pressurized water reactors (PWR). Binary mixtures of iron oxides were prepared with known compositions containing pure commercial magnetite (Fe 3 O 4 ), maghemite ( -Fe 2 O 3 ), and hematite ( -Fe 2 O 3 ) for calibration purposes. Calcium oxide (lime) was added to all samples as a standard reference

Keywords:

in obtaining the calibration curves. Using regression analysis, relationships were developed for intensity

versus concentration for absorption bands cor responding to each of the phases in their corresponding
A.

Steel

  • B. FTIR spectrum. Correlation coecients, R 2 , of 0.82, 0.87, and 0.86 were obtained for maghemite–magne-

IR spectroscopy

  • C. tite, hematite–magnetite, and hematite–maghemite systems, respectively. The calibration curves gener-

Rust

  • C. ated were used to quantify phases in multi-component unknown field samples that were obtained from

Oxidation

  • C. different components (moisture separators, condensers, and high and low pressure heaters) of the two units (units 1 and 2) of the secondary cycle of the Comanche Peak PWR. © 2008 Elsevier Ltd. All rights reserved.

Passivity

1. Introduction

Formation and transformation of iron oxides is of interest to a wide variety of industries including steel making, power generat- ing, paint systems, pharmaceutical, and petrochemical, to name a few. The thermal hydraulic performance and integrity of the steam generators in nuclear power plants may be compromised due to the presence of cor rosion deposits. The amount of iron transported in a steam generator is dependent on the composition of iron oxide formed in the feed train. Deposits that contain well crystallized magnetite and maghemite are more stable than deposits contain- ing a combination of oxides and oxyhydroxides [1]. Therefore, it is very important to quantitatively understand the composition of the deposits. Standard methods for identifications and characterizations of iron oxides have traditionally used either X-ray diffraction (XRD) or Mössbauer spectroscopy (MS) [2]. XRD has been widely used in characterizing cor rosion products. Although these techniques have served industry well in the past, they suffer from shortcom- ings that could be replaced by Fourier transform infrared spectro- photometry (FTIR). MS is a technique that utilizes a live radioactive source, which makes the technique relatively unsafe from an oper- ational point of view, since it poses a potential health risk to the operator. The main limitations of MS technique include the level

* Corresponding author. Tel.: +1 940 565 4052; fax: +1 940 565 2666. E-mail address: nasr@unt.edu (S. Nasrazadani).

0010-938X/$ - see front matter © 2008 Elsevier Ltd. All rights reserved.

doi:10.1016/j.corsci.2008.06.034

of operator expertise requirements and the complexity of spectral interpretation. Even though XRD is easier to operate and interpret, its spectra is limited in its ability in differentiating magnetite and maghemite. On the other hand, FTIR instrumentation is simple and spectra interpretation is relatively easy [3]. In the past, it has been estab- lished that the FTIR technique can be routinely used to eciently differentiate and quantify different iron oxides and oxyhydroxides. To the best knowledge of the authors, no attempts have been made in using FTIR for quantitative analysis of iron oxides formed in the power plants. The main objective of this research is to quantify iron oxide phases formed in the secondary side of the steam gener- ator units at Comanche peak steam electric station (CPSES). Such analysis will allow better interpretation and control of the cor ro- sion process.

2. Literature review

Magnetite is a well-known form of iron oxide that forms at room temperature in crevices between steel plates and at elevated temperature inside boiler tubes, heat exchangers etc. The oxida- tion product of Fe 3 O 4 is either -Fe 2 O 3 or -Fe 2 O 3 depending on the oxidation temperature and/or possibly the crystallite size of the starting magnetite [4–5]. Studies performed by Nasrazadani and Raman [4] have shown that transformation of magnetite to hematite goes through the for- mation of maghemite. The production of maghemite begins with

  • 2494 H. Namduri, S. Nasrazadani / Corrosion Science 50 (2008) 2493–2497

nucleation and growth of goethite or lepidocrocite, followed by dehydration to hematite, and then reduction to magnetite. The deposition rate of hematite is an order of magnitude greater than magnetite. As seen from the Pourbaix diagram of iron, it is important that the reducing conditions be maintained in the steam generators during operation, so as to facilitate formation of magnetite. Turner and Klimas showed that lowering the concentra- tion of hematite relatively to magnetite in the fee dwater will signif- icantly lower the rate of tube bindle fouling [6]. Theoretical studies by Jobe showed that hematite has a very low solubility and a much smaller dissolution rate than magnetite and lepidocrocite in the presence of 5 ppb of dissolved oxygen. Formation of thin layer of maghemite/magnetite is known to act as a very good passive film

[7].

FTIR spectra of iron oxides are well established. It is been observed that the absorption band at a high wavenumber region is due to OH stretching, and at lower wavenumber as a result of Fe-O lattice vibration. FTIR spectrum of magnetite exhibits two strong infrared absorption bands at 570 cm ¡1 ( 1 ) and 390 cm ¡1 ( 2 ) [8]. According to Ishii et al, these bands can be assigned to the Fe-O stretching mode of the tetrahe dral and octahe dral sites for the 1 band at 570 cm ¡1 and the Fe-O stretching mode of the octahe- dral sites for the 2 band at 390 cm ¡1 , provided that Fe 3+ ion dis- placements at tetrahe dral sites are negligible [8]. FTIR spectrum of magnetite exhibits two other absorption bands at 268 cm ¡1 and 178 cm ¡1 which were beyond the detection limit of our instru- ment. Maghemite, a defective form of magnetite, has absorption bands at 630 cm ¡1 , 590 cm ¡1 , and 430 cm ¡1 . Table 1 summarizes possible FTIR peak s for different iron oxides. Legodi and his group performed quantitative analysis on cal- cium carbonate present in different cement blends using FTIR [9]. Reig and group performed quantitative FTIR analysis on calcium

Table 1 Infrared bands of different iron oxides [4,13]

Iron oxide/hydroxide

Wave numbers of bands (cm ¡1 )

Magnetite (Fe 3 O 4 ) Maghemite ( -Fe 2 O 3 ) Hematite ( -Fe 2 O 3 ) Goethite ( -FeOOH) Lepidocrocite ( -FeOOH)

Broad bands at 570 and 400 cm ¡1 700, 630–660, 620 range (Fe-O range) 540, 470 and 352 cm ¡1 1124, 890 and 810 cm ¡1 for OH stretch 1018 cm ¡1 (in plane vibration) and 750 cm ¡1 (out of plane vibration)

carbonate and silica (quartz) using the constant ratio method. The group used potassium ferricynaide as standard and successfully showed the accuracy of quantifying the concentration of silica and quartz in geological samples using FTIR [10]. The same group also successfully showed that FTIR can be used to quantify butyl acetate and toluene in binary and ternary mixtures using constant method ratio. They used valeronitrile as the standard and they also showed that the above method is independent of optical path length [11]. The Xu group showed that FTIR can be eciently used for quan- tifying minerals. They used a multifunctional analysis, which is based on Beer’s law to quantify different minerals present in oil wells. In this method, the absorbance at a specific wave number is equal to the sum of the absorbance of all sample components at that wavenumber [12].

3. Experimental proce dure

Commercially available powders of magnetite (puratronic 99.999% purity), maghemite (99+% purity), and hematite (99.99% purity) were obtained. Three binary sets of sample mixtures with known concentrations of maghemite and magnetite, hematite and magnetite, and hematite and maghemite were prepared. All the samples were added to KBr powder and compressed into pellets using hydraulic press. Magnitude of compression applied in KBr pellet preparation needs to be kept constant to avoid variance in absorbance intensity from one sample to the next. Nicolet Avatar 370 DTGS FTIR was used to quantify iron oxides. FTIR spectra collec- tion was done for 32 scans with 2 cm ¡1 resolutions. Three equiva- lent runs of each of the three sets of the samples were made on the FTIR spectrometer. The average values of background subtracted peak intensity results were used for obtaining calibration curve. Once all of the spectra for the samples were obtained, three cal- ibration curves were drawn for the three sets of samples. To set the calibration curve for known amounts of iron oxide (magnetite, maghemite and hematite) in each mixture, I/I o ratio was used. The intensity of the iron oxide peak (magnetite 570 cm ¡1 , hematite- 540 cm ¡1 and maghemite 630 cm ¡1 ) is represented by I and I o rep- resents, the intensity of the 3640 cm ¡1 peak of CaO. This calibration curve was used to quantify the amount of iron oxides present in the field samples collected from the secondary side of CPSES. The most readily available samples of the secondary system were obtained from the fee dwater heaters (FW HTR-low pressure and high pressure fee dwater heaters), condenser, and moisture separator-reheater (MSR), as these components are rou-

2494 H. Namduri, S. Nasrazadani / Corrosion Science 50 (2008) 2493–2497 nucleation and growth of goethite

Fig. 1. Simplified schematic of secondary system sample locations.

H. Namduri, S. Nasrazadani / Corrosion Science 50 (2008) 2493–2497

2495

tinely opened during outages and represent major temperature locations of the system as illustrated by Fig. 1. The CaO absorption band was used primarily as a reference because it does not interfere with any of the iron oxide phases. Even though an absorption band of 3640 cm ¡1 is close to the OH band, it has a very distinct peak and can be easily discerned (Fig. 2). CaCO 3 (894–865 cm ¡1 peak) has been previously used as a standard reference in quantifying the amount of limestone in different cement blends [9]. A linear fit was used to obtain the calibration curve.

4. Results and conclusions

Fig. 3 shows FTIR spectra of single phases of hematite, mag- netite, and maghemite. A sharp peak at 3640 cm ¡1 belonging to calcium oxide is shown in all of the spectra of iron oxides. The peak intensity of CaO was fairly constant in all the spectra. Cali- bration curves were obtained for combinations of two phases of iron oxides. Correlation factors of 0.822 (magnetite added to maghemite, Fig. 4), 0.8584 (maghemite added to hematite, Fig. 5), and 0.8708 (magnetite added to hematite, Fig. 6) were obtained.

H. Namduri, S. Nasrazadani / Corrosion Science 50 (2008) 2493–2497 2495 tinely opened during outages and

Fig. 2. FTIR spectra of 100% CaO showing 3640 cm ¡1 peak .

H. Namduri, S. Nasrazadani / Corrosion Science 50 (2008) 2493–2497 2495 tinely opened during outages and

Fig. 3. FTIR spectra of 100% hematite, maghemite and magnetite.

  • 2496 H. Namduri, S. Nasrazadani / Corrosion Science 50 (2008) 2493–2497

Table 2

Fig. 4. FTIR calibration for mixture containing magnetite and maghemite.

FTIR intensities for different known concentrations of iron oxides used in calibra-

tion curves (I = intensity of iron oxide mixture, and I o = intensity of 3640 cm ¡1 peak

of CaO)

Hematite (%)

Magnetite (%)

Maghemite (%)

I/I o

100

1.30

100

1.13

100

1.02

80

20

1.01

60

40

0.98

40

60

0.82

20

80

0.81

80

20

1.13

60

40

1.02

40

60

0.91

20

80

0.95

20

80

0.86

40

60

0.81

60

40

0.75

80

20

0.76

  • most intense peak of maghemite) was used for I values in the case
    The main fee dwater heater sample showed 96% magnetite and

of mixtures containing magnetite and maghemite. No peak inter-

ferences of any phases were observed in all of the mixtures since

FTIR spectra of all iron oxides are well resolved and spectra resolu-

tion of most FTIR instruments is 2 cm ¡1 . These calibration curves

were then used to quantify the iron oxide phases present in the

field samples collected from the secondary side of unit 1 and unit

2 of CPSES.

The percentage concentrations of the iron oxides present in

the selected field samples is given in Table 3. The samples from

the moisture separator mainly show hematite and magnetite.

Fig. 5. FTIR calibration for mixture containing hematite and magnetite.

about 4% maghemite. The high-pressure fee dwater heater sam- ple showed mostly hematite; whereas, low-pressure fee dwater heater sample showed hematite and magnetite. The presence of magnetite and hematite is expected in fee dwater systems due to the transformation of hydroxides and other hydrated iron species, which move through the fee dwater system into stable iron oxides (Schikorr reaction). The two samples form the main condenser

mainly consisted of hematite with traces of magnetite and maghe-

mite. Detection limits determination for iron oxides quantification

using FTIR was not done in this study and is planned for future

5. Summary and conclusions

A quantitative determination of iron oxides can be quickly per-

formed relatively accurately using FTIR technique. The technique

involves taking mid infrared measurements with samples in the

form of KBr pellets. By using a standard reference like CaO, nor-

malization can be performed. The peak of 3450 cm ¡1 is free from interference with any of the major iron oxide peak s considered in

this study. This method makes it a very suitable method in quickly determining the concentrations of major iron oxides in the power industry. The FTIR technique was reconfirmed to be a valuable tool to dif- ferentiate between Fe 3 O 4 and -Fe 2 O 3 . It is also been shown that this technique can be used in quantifying iron oxides. It has also been shown that the infrared active mode of calcium oxide can be eciently used in the quantification process. The FTIR quantification method performed in this study can be further fine- tuned and extended to other major metallic oxides including: chro- mium oxide, nickel oxide, lead oxide, and silicon dioxide. This will prove valuable for studying cor rosion deposits formed in nuclear power plants.

work .

Fig. 6. FTIR calibration for mixture containing maghemite and hematite.

A confidence limit of 95% was used in the calculations. The aver- age values of I/I o for three runs made with mixtures with different concentrations of iron oxides are shown in the Table 2. Hematite peak at 540 cm ¡1 intensity (the most intense peak for hematite) was used for the I value for mixtures containing hematite and mag- netite, and maghemite and hematite. The peak at 630 cm ¡1 (the

H. Namduri, S. Nasrazadani / Corrosion Science 50 (2008) 2493–2497

Table 3

2497

Concentration of field sample collected from different components of secondary side of unit 1 and unit 2 steam generator system of CPSES

Field samples

Sample description

Oxides present

I o

Maghemite (I)

Hematite (I)

I/I o

Final concentrations

  • 1 Moisture separator

Magnetite and hematite

3.02

2.85

0.94

52% Hematite and 48% magnetite

  • 2 Main feedwater heater

Magnetite and maghemite

4.29

2.81

0.66

96% magnetite and 4% maghemite

  • 3 Main condenser, hotwell

Magnetite and hematite

3.08

4.01

1.3

Mostly hematite a

  • 4 Main condenser

Maghemite and hematite

0.28

0.49

1.74

Mostly hematite b

  • 5 High pressure feedwater heater

Maghemite and hematite

0.75

1.03

1.37

Mostly hematite b

  • 6 Low pressure feedwater heater

Magnetite and hematite

5.81

5.37

0.92

52% magnetite and 48% hematite

Amount of magnetite was below the detection limit. b Amount of maghemite was below the detection limit.

a

Acknowledgement

Authors would like to thank both Mr. Jim Stevens and Mr. Rob- ert Theimer for providing field samples.

References

[6] Turner, Klimas, “The Effect of Alternative Amines on the Rate of Boiler Tube Fouling”, Final Report, TR-108004, EPRI Report, September 1997. [7] David Jobe, “The calculated solubilities of hematite, magnetite and lepidocro- cite in steam generator feed trains”, AECL, 1997. [8] M. Ishii, M. Nakahira, Infrared absorption spectra and cation distribution in (Mn,Fe) 3 O 4 , Solid State Communications 11 (1972) 209–212. [9] Legodi, D. De Waal, J.H. Potgieter, Quantitative determination of CaCO 3 in cement blends by FT-IR, Society for Applied Spectroscopy 55 (3) (2001) 361–

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