A Comparative Study on the Sieve Size Effects on the X-Ray and Microscopy of Spent Foundry Sand-Admixed Concrete

Shuaibu SI and Elinwa AU

Published on: 2023-12-30

Abstract

Morphological changes that occurred during the hydration of concrete containing spent foundry sand (SFS) and gum Arabic) admixture (GA) were observed using the X-ray analyses and the scanning electron microscopy. The XRD was used to identify the crystalline and mineral phases while, the scanning electron microscope (SEM) was used for the corresponding changes in microstructure. Sieve sizes of 120 µm and 212 µm apertures were used to compare their effects with and without SFS and GA admixture on concrete. SFS at 10 % by wt. % of the fine aggregate, and GA admixture dosage of 0.5 % by wt. % of cement were used. The water-to-cement ratio was 0.5.

The results showed the morphological changes, and the specific influences of SFS and GA, with the sieve sizes of 120 µm and 212 µm, respectively. The results showed additions of SFS with GA-admixture and the sieve sizes modified the pore network and the composition of the main hydration product.

Keywords

Sieve sizes Gum Arabic admixture Spent foundry sand Crystalline and mineral phases Microstructure of concrete

Introduction

The use of SCMs in cement-based materials is becoming an interesting topic in the construction industry. This is because of the numerous benefits. These benefits are contained in many literatures. Incorporating SCMs in cement-based materials modify the pore network and composition of the main hydration product, calcium (-aluminate)-silicate-hydrate (C (-A)-S-H) [1]. It also offers sustainability, environmental-friendly, and energy-saving alternatives of cement, and enhances the use of recycled wastes as construction materials [2]. There are many classes of SCMs of which spent foundry sand (SFS) is one of them. The by-product of the foundry industry is spent foundry sand (SFS). One of the advantages of SFS to the construction industry for its use as building materials will safeguard the ecosystem and environmental assets, while also providing durable construction. The use of industrial waste in concrete offsets a shortage of environmental sources, solves the waste dumping trouble and provides another method of protecting the environment. Several researchers have investigated the suitability of this material, SFS in concrete production as a partial replacement of fine aggregate. This has been held as a disposal method for SFS in the foundry industry, and thus, accomplish its recycling in concrete production [3].

Carried out an experimental investigation to study the influence of spent foundry sand (SFS) as partial replacement for fine aggregate on two grades of concrete mixtures. They used two control concrete mixtures M20 and M30, designed to have compressive strengths of 30 MPa and 40 MPa at 28 days of curing. The fine aggregate was replaced by SFS in proportions of 0 % to 20 % by wt. % of fine aggregate and compared with the originals (M20 and M30), cured for 365 days. They concluded that the test results showed marginal increase in strength and durability properties [4]. Investigated the durability and microstructure properties of concrete with gum biopolymer admixture.

The X-ray diffraction and SEM tests were to determine the rate of hydration and expose the microstructure properties of AGB cement mix and help explain its macroscopic behaviour, respectively. Some of the findings were that the XRD results showed almost similar hydration pattern of AGB cement relative to the OPC cement, and. the scanning electron microscopy (SEM) of AGB concrete showed less voids dispersed in the AGB mix microstructure. They, therefore, concluded that the use of AGB can be beneficial as a water-reducing admixture in the construction sector, resulting in decreasing the chemical admixture demand [5]. Research was on the effects of waste foundry sand on the strength and microstructural properties of concrete. They used concrete cubes, cylinders, and unreinforced beams to test and assess the mechanical properties of concrete made with waste foundry sand and manufactured sand as fine aggregate. The tensile, splitting, and flexural strengths of the concrete were determined after curing for 90 days. The micro-structural analyses were conducted on the control mixture and mixtures containing 10, 20, 30, 40, and 50% waste foundry sand using the SEM, EDS, and TGA/DCs methods of analyses. They concluded that the strength differences that occurred when fine aggregates were replaced with waste foundry sand in different proportions were better understood. An evaluation on the use of SFS in the production of concrete was undertaken by [6], using SFS in proportions of 10 % to 40 % by wt. % of fine aggregate to produce concrete samples that were cured for up to 90 days. The results confirmed the suitability of SFS for concrete productions and is pozzolanic. It also confirmed SFS reduced water as the replacement level increased absorption by about 8 % to 28 % at 90 days, but the compressive strength decreased [7]. Studied the effect of used foundry sand on the mechanical properties of concrete using 10 %, 20 %, and 30 % to replace fine aggregate by wt. %, and cured for up to 365 days. Results showed marginal increase in the strength properties of plain concrete by inclusion of UFS as partial replacement of fine aggregate and can be effectively used in making quality concrete and construction material. The influence of GA admixture on the mechanical properties of lime-metakaolin paste used as binder in hemp concrete was undertaken by [8]. The paste was modified with powdered gum Arabic at 1 %, 3 %, and 5 %, by mass as a partial replacement for the binder mix. The influence of the admixture on the pore size distribution as well as flexural and compressive strengths were investigated. The admixture enhanced the total porosity of the paste and the compressive and flexural strengths. Gum Arabic and sawdust ash (SDA) have been used by [9] to address some of the gaps between pozzolanic and conventional concretes. He used concrete mixtures designated as M_00, M-00GA, M-10GAS, and M-30GAS with a GA dosage of 0.5 % by wt. 5 of cement and SDA replacement by wt. % of 10 %, and 30 %, respectively, and cured for 28 days. The results showed that 28 days of curing used for the conventional concrete in stripping the formwork, may not be appropriate for use on pozzolanic concrete. Therefore, he proposed for a strength beyond the 28 days of curing to carter for the pozzolanic effects which starts well above 28 days.

However, a lack of proper knowledge about the progress of waste foundry sand (WFS) in concrete production have been stressed [10]. The current paper examines two materials of interest, GA-admixture and SFS, whose performances are still in the forming stages in the research on cement and construction materials because of lack of adequate information needed in the literature on their performances. The thrust, therefore, is to build understanding on their characteristics using X-ray diffraction analysis to study the crystalline and mineral phases and scanning electron microscopy for the morphology and structure of the micrographs. These were carried out using crushed compressive cube samples which were cured for 28 days and derived from sieve sizes of 150 µm and 212 µm, respectively. These were used to assess the effects of GA and sieve size effects on concrete.

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2.0 Materials

The proper understanding the composition of a material before use is important because mmaterials are made up of atoms which are arranged in crystal microstructures, while the mminerals are crystalline inorganic solids which possess well-defined chemical composition and are formed through natural processes. Minerals, therefore, are usually classified and characterized based on their physical properties.

2.1- Physical and Chemical Properties, and Sieve Analysis of the Concrete Materials

The materials used for the investigation are Ashaka Portland cement conforming [11], fine and coarse aggregates conforming [12], spent foundry sand (SFS) and gum Arabic which is an emulsifier and superplasticizer. The characteristics of these materials are shown in Tables 1 to 3. Table1is the physical and chemical properties of the ‘Ashaka’ cement used. Table 2 shows the physical characteristics of the fine and coarse aggregates, while the sieve analyses for the fine and coarse aggregates and spent foundry sand are shown in Table 3. Tables 4 and 5 are the physical and chemical characteristics of the two (2) additive materials of interest added to the cement materials. The physical and chemical properties of SFS and the oxide composition of GA are shown in Tables 4 and 5, respectively. The values in Table 5 were derived using the X-ray Fluorescence method of analysis as shown in Figure 1.

Table 1: Physical and Chemical Properties of Cement.

Physical Property

Parameter

Value

Specific gravity

3.15

Blaine fineness (m2kg-1

375

Loss on Ignition (%)

1

Soundness (mm)

8

Consistency (%)

33

Initial Setting Time (min.)

143

Final Setting Time (min.)

196

Chemical Property

Oxide Composition

Weight (%)

SiO2

19.68

Al2O3

6.44

Fe2O3

3.32

CaO

60.92

MgO

0.97

SO3

2.28

K2O

0.85

Na2O

0.12

Table 2: Physical Properties of Fine and Coarse Aggregate.

Parameter

Aggregate/Value

Fine

Coarse

Specific gravity

2.48

2

Silt content (%)

4.32

-

Bulk Density (kgm-3)

1648

1607

Aggregate crushing value (%)

-

16

Table 3: Sieve Analysis of the Fine and Coarse Aggregate.

Sieve Size (mm)

Fine Aggregate (%)

Coarse Aggregate (%)

Spent Foundry Sand (%)

Retained

Passing

Retained

Passing

Retained

Passing

75

-

-

0

100

-

-

63

-

-

0

100

-

-

50

-

-

0

100

-

-

37

-

-

25

75

-

-

28

-

-

24.1

50.92

-

-

20

-

-

21.96

28.96

-

-

14

-

-

17.04

11.92

-

-

10

-

-

6.36

5.56

-

-

6

-

-

4.08

1.48

-

 

5

0

100

1.1

0.39

0

100

3.35

0

100

0.39

0

0

100

2

13.96

86.04

-

-

0

100

1.18

11.44

74.59

-

-

0.54

99.46

0.6

40.31

34.29

-

-

1.54

97.92

0.425

18.8

15.49

-

-

2.17

95.75

0.3

5.18

10.31

-

-

6.21

89.54

0.212

6.74

3.57

-

-

29.8

59.74

0.15

1.1

2.47

-

-

32.5

27.24

0.075

0.7

1.77

-

-

16.8

10.44

Receiver

1.77

0

-

-

10.44

0

Table 4: Physical and Chemical Properties of Spent Foundry Sand.

Physical Properties

Parameter

Value

Specific Gravity

2.54

Bulk Density (kg/m3)

2589

Moisture Content (%)

3.11

LOI

0.93

Chemical Properties

Oxide Composition

Spent Foundry Sand

SiO2

82.71

Al2O3

10.2

Fe2O3

3.92

CaO

0.98

MgO

0.15

SO3

1.32

K2O

-0.06

Na2O

0.29

P2O5

-

Mn2O3

-

TiO2

-

CaCO3

-

Figure 1: X-Ray Fluorescence of Gum Arabic.

Table 5: Oxide Composition of Gum Arabic.

Oxide

Content

SiO2

8.36

K2O

0.76

CaO

3.47

MnO

0.07

Fe2O3

0.22

NiO

0.03

SrO

0.06

Y2O3

0.003

Nb2O5

0.05

MoO3

0.26

Ag2O

0.02

2.2 X-Ray Diffraction and Microscopy Characteristics of the Materials

X-ray diffraction technique was used to determine the SFS and GA composition and their crystalline structure. The x-ray study was by irradiating the materials with incident x-rays and then measuring the intensities and scattering angles of the x-rays that leave the materials. The XRD diffractograms of the SFS and GA samples and their characteristics compositions are shown in Figures 2 and 3, Tables 6, respectively. The scanning electron microscopy was used to study the morphology (texture), chemical composition, and crystalline structure and orientation of the materials making up the SFS and GA, respectively. The microscopy of the SFS and GA morphologies and their structural compositions are shown in Figures 4 (a, b), 6. For SFS and GA, respectively. These show the morphologies (texture), while Figures5 and 7 with the accompanying Tables 6 and 7 are the EDS elemental analysis showing the structural structure of the SFS and GA, respectively.

Figure 2: X-ray Diffraction of Spent Foundry Sand.

Table 6: XRD Peaks of Spent Foundry Sand.

Pos. [°2Th.]

Height [cts]

FWHM Left [°2Th.]

d-spacing [Å]

Rel. Int. [%]

20.0892

53.34

0.1574

4.23553

0.3

26.7624

17500.36

0.4723

3.33121

100

39.5255

38.28

0.4723

2.28003

0.22

49.9133

89.55

0.0984

1.84524

0.51

55.0237

67.76

0.4723

1.70876

0.39

60.6416

51.24

0.0787

1.52709

0.29

68.1389

73.63

0.096

1.37847

0.42

Figure 3: X-Ray Diffractogram of Gum Arabic.

Table 7a: Elemental Composition of SS.

Element Name

Element Symbol

Weight Conc.

Carbon

C

45.18

Silicon

Si

13.89

Iron

Fe

12.4

Oxygen

O

10.75

Aluminium

Al

7.4

Tantalum

Ta

5.42

Lead

Pb

2.86

Calcium

Ca

1.57

Magnesium

Mg

0.4

Titanium

Ti

0.14

Table 7b: SFS Particle Size.

Measurement

Diameter (µm)

L1

189.4

L2

205.7

L3

326.5

L4

142.8

L5

96.6

L6

129.1

L7

124

a) Microscopy of SFS Material.

b) Particle Size of SFS Material.

Figure 4: Microscopy of Spent Foundry Sand.

Figure 5: Energy Disperse X-Ray Spectrum of SFS.

Figure 6: Micrograph of Gum Arabic.

Table 8: Elemental Composition of Gum Arabic.

Element

Symbol

Weight Conc

Carbon

C

59.61

Oxygen

O

25.64

Boron

B

4.4

Tellurium

Te

2.3

Nitrogen

N

2.24

Gallium

Ga

1.25

Calcium

Ca

1.07

Bromine

Br

0.83

Arsenic

As

0.6

Potassium

K

0.46

Silicon

Si

0.41

Rubidium

Rb

0.35

Phosphorus

P

0.31

Magnesium

Mg

0.31

Fluorine

F

0.22

Figure 7: Energy Disperse X-Ray Spectrum of Gum Arabic.

 

 

4.0. Discussions

4.1. Characteristics of the Materials

From Tables 1, 4 and 5 of physical and chemical properties of the materials, the CaO content of the cement was approximately 61 % and therefore classified as having cementing effect with SiO2 content of approximately 20 %. As earlier stated, this conformed to BS 12. The SiO2 in the SFS used was approximately 83 % and the CaO, 1 %. Studies on the physical and chemical properties of SFS have shown some variability which are due to some factors which may depend on the environment and condition of use [7]. Gave factors such as type of casting process and the industrial sector from which it originated. With the values of SiO2 + Al2O3 + Fe2O3 greater than 70 %, against the stipulated in ASTM [13 of 70 %, it could be concluded that SFS has pozzolanic characteristics with high affinity for water [6]. The specific gravity of spent foundry sand (SFS), the LOI and the fineness passing are 2.54, 0.91 and 27 % respectively. These are somewhat in agreement with the findings of [6, 7], who gave them as 2.2, 5.15, 8 % and 3.15, 1.0, 8.2 %, respectively. The bulk density is 2589 kg/m3. The XRF for the gum Arabic is shown in Figure 1, and has oxide compositions of K, Ca, Mn, Fe, Ni, Sr, Y, Nb, Mo, and Ag (Table 5).

The XRD diffractogram of the SFS is shown in Figure 2. This has a peak which showed it has a crystalline structure with the peak intensity reflecting the amount of this structure in the SFS. The dominant mineral is Quartz, a hard crystalline mineral composed of silica (silicon dioxide), whose atoms are linked in a continuous framework of SiO4 silicon–oxygen tetrahedra. Each oxygen is shared between two tetrahedra giving an overall chemical formula of SiO2 in which magnesium, iron, aluminum, and silicon substitute for each other in the crystal structure. Table 6 showed the peaks of the crystalline phase and mineral compositions. Figure 3 showed the XRD diffractogram for GA. This is amorphous with no distinct peak structure [14].

The morphology (Texture) and particle dimensions of the SFS sample are shown in Figure 4 (a, b). The EDS elemental spectrogram and the structural values are shown in Figure 5, and Table 7a, while the particle diameters are shown in Table 7b. The microstructure showed that the SFS particles were generally irregular in shape (205.7 µm to 96.0 µm). These contain micro-porous surfaces, and discreet widely. The dominant oxides are C, Si, Fe, O, Ta, Pb, and Ca with trace oxides of Mg and Ti Table 7 (a, b). GA, which is an emulsifier, was used as the superplasticizer and conformed to BN EN 480-1 [15]. Figure 6, the morphology (texture) of the GA showed the GA internal structure consisted of different layers with clear lines of separation with hair cracks appearing on them. The EDS elemental result as shown in Figure 6 and Table 8 showed that the dominant oxides are C, O, B, Te, N, Ga, and Ca, with minor oxides as Br, As, K, and Si, respectively.

4.2. X-Ray Diffraction and Scanning Electron Microscopy of Concrete Samples

4.2.1. X-Ray Diffraction

The X-ray characterization of the various diffractograms (Figures 8-10 and Tables 10-16) showed the pattern, crystalline peaks, and the mineral compounds in the hydrated products, respectively. Figures 8-10 present the different patterns of the control concrete, and concrete samples containing 10 % SFS but with sieve sizes 212 µm and 150 µm, respectively, with or without gum Arabic (GA) added as an emulsifier. The peaks indicate the existence of crystalline structures of the material, and the intensities of these peaks reflected the amount of these structures in the concrete samples. It is evident from Tables 10-13 that both GA and SFS samples showed distinct differences in peak intensities of SiO2 and Ca (OH) 2, respectively. The concrete samples with GA addition had peaks that were much reduced. The reasons adduced for the reduced peaks have been tied to the pH value of the GA which is approximately 4.0 [6], and the emulsifying effects of GA. This is constituted of sugars that made it react as an admixture [16]. It is also observed that some new peaks appeared with small intensities of CuFe detected in both samples of the control concrete (with and without GA), and only in SFS concrete samples with both sieve sizes (150 µm and 212µm) without GA, respectively. Peaks of CuFe were also detected in the works of [17]. Studies conducted on SDA and GA confirmed the concentrations of hydration process were determined through the length intensity of Ca (OH) 2 and C-S-H, collected by X-ray scans which were recorded as intensity counts [18]. These were detected at several locations along the 2 Theta at the 28 days of curing. This signified that at 28 days of curing the hydration of the concrete mix was still much in progress.

Tables 14-16 showed the quantitative analysis of the concrete samples with or without GA, using sieve sizes of 150 µm and 212 µm, respectively. From the results, all the concrete samples contained the same crystalline phases and minerals but of various weight percentages. They are Hillebrandite (SiO2, CaO and H2O), Quartz (SiO2), Brownmillerite (Al2O3, Fe2O3, CaO), Portlandite and Tricalcium aluminate. The oxides enclosed in brackets are the dominant constituent of the mineral oxide.

4.2.2. Scanning Electron Microscopy

The analysis of the results obtained from the scanning electron microscopy (SEM) were used to support the characteristic behavior observed in the interpretations of the crystalline and mineral phases of the Xray diffraction results. These observations were used in the interpretation of the transformational effects of SFS material and GA admixture on one hand, and the sieve size effects of 212 µm and 150 µm on the other hand, on the concrete properties. These were used to examine the morphology (texture) and structure of the concrete samples. Figure 11 (a and b) showed the morphology of the control concrete with that of 0.5 % GA. Figure 11a depicted C-S-H gels with nodules and vast areas of somehow chalky gel over the whole micrograph, dotted with voids. Figure 11b containing 0.5 % GA showed a well distributed gel of C-S-H and reduced void sizes. Patches of aggregates and unhydrated cement were noticed with the control concrete but disappeared with the addition of GA. The differences in the characteristic features, and the effectiveness of the GA as an admixture were observed in the level of compactness and internal arrangements using the results of the water absorption and density (Table 9). These were 1.56 % for the water absorption and 2516 kg/m3 for the density, without the addition of GA. The water absorption was reduced by 49.7 % and density increased by approximately 4.4 %. Therefore, the addition of GA admixture would reduce the water absorption and increase the density of concrete. Examining the EDS spectrogram results, the mineral oxides with wt. % ≥ 3% were considered as having significant impact on the internal rearrangement of the mineral composition, and therefore, responsible for the observed characteristic developments (Table 9). Figure 12 (a, b) and Table 17 (a, b) showed that Ca, Si, Fe, K, and Ag were the dominant mineral oxides in the control concrete (Figure 12a and Table 17a), and Ca and Fe as the dominant mineral oxides in Figure 12b and Table 17b, respectively. The GA admixture as an emulsifier can act on silica. Silica in concrete coagulates due to the presence of hydroxide ions on its surface. Therefore, the action of GA was to reverse this action to allow better workability and flow of the control concrete with GA.

The effects of SFS material and GA were evaluated using the morphology (Texture) of the concrete sample shown in Figure 13 (a, b). This contained partial replacement of fine aggregate with SFS at 10 % by wt. % of the fine aggregate (Figure 13a). The second sample (Figure 13b) included 0.5 % GA by wt. % of cement in the SFS-concrete sample used for the evaluation of the contribution of GA in the modification of the concrete morphology. Their EDS Spectrograms and the structural characterizations are shown in Figure14 (a, b) and Table 18 (a, b), respectively. The formation of C-S-H with reduced pores sizes than the control concrete and some unreacted SFS were noticed. Comparing the control concrete with the mix to which SFS was added had tremendous effect on the water absorption and density of the concrete were improved. These were 24.34 % and 3.86 % respectively. It also showed that the internal grain structure was more compact and better dispersed than the control concretes. Therefore, SFS addition reduced the water absorption and increased the density of the concrete. The same observations could be said for the SFS concrete mix with GA. Both the water absorption and density were reduced and increased respectively. Therefore, SFS and material and GA admixture are compatible. However, the unreacted SFS noticed in the SFS concrete mix without GA disappeared. The EDS spectrogram results shown in Figure 14 (a and b) were the same as the EDS spectrogram for the control concrete in Figure 12 (a and b). Figure 14a and Table 18a showed the dominance of the mineral oxides of Ca, Si, Al, and Fe. The same observations made for the control concrete (Figure 11a and 11b) were made for the SFS concrete mix, both with and without GA (Figure 14a and14b). The peaks of Ca and Si appeared strong in SFS-concrete mix but almost disappeared when GA was added for the same reason raised earlier. That of reversing the coagulation and making the concrete more flow able. The SFS concrete mix with GA had mineral oxides of Ca, Fe, Si, K, C, Ag, and Al.

The sieve size effects of 150 µm and 212 µm with and without GA were compared and evaluated. The SFS mix with and without GA and having sieve size 212 µm are shown in Figures 15 (a and b), 16 (a and b), and Table 19 (a and b). Both are showing the morphology, ED’s spectrogram, and structural characterization of the microstructure. The mix without the GA, showed large particles and very rough textures in the internal grain structure of the microstructure. Aggregates and some unreacted SFS were also noticed. The values obtained on the mechanical characteristics (Table 9) showed better structuring of the microstructure than the control concrete. The water absorption was reduced by 22.2 % and the density increased by 5.6 %. However, comparing this with sieve size 150 µm showed more porous structure by 2.6 %. Therefore, sieve size 150 µm showed more refined structure than sieve size 212 µm. Again, the peaks of sieves 150 µm and 212 µm had the same strong appearances of Ca and Si. The EDS spectrogram (Figure 16a and Table 19a) showed the same dominant mineral oxides (≥ 3 %) as sieve size 150 µm which are Ca, Si, Fe and Al but with varying wt. %. The addition of GA had a better effect with more flow ability on the texture giving a more compact and well distributed internal grains. Also, C-S-H gel was formed with voids dotted around the gel with a water absorption of approximately 10.9 % and a reduction in density of 1.2 %. Compared to sieve size 150 µm with GA, the water absorption increased to 17.9 % signifying more porous structure. The peaks of 212 µm remained very strong when GA was introduced unlike the peaks of sieve 150 µm which flattened off. Therefore, it can be said that GA has more compatible behavior with sieve sizes greater than 150 µm. More work is advocated on this. The EDS spectrogram (Figure 16b and Table 19b) showed Ca, Si, Ag and Fe were the dominant mineral oxides. Comparing this with the microstructure of SFS concrete with sieve 150 µm (Figure 14b and Table 18b), the mineral oxides K, C, and Al were not found. This may also confirm that sieve 150 µm is more plastic than sieve size 212 µm.

Conclusion

A comparison of the effects of two sieve sizes 150 µm and 212 µm, and the use of SFS and GA additions, have been carried out and conclusions drawn as shown.

  • The microstructure of SFS showed it is irregular in shape with a crystalline nature with micro-porous surfaces. The dominant oxides are C, Si, Fe, O, Ta, Pb, and Ca with some trace elements.
  • The texture of GA have internal structure which consisted of layers with clear lines of cleaverages with hair cracks with dominant oxides of C, O, B, Te, N, Ga and Ca, with minor oxides.
  • The results of the investigation showed SFS and GA have marked effects in the transformation of the morphology of the concrete characteristics. SFS acts as a pozzolanic material, and the GA as an admixture and an emulsifier due to its pH and sugar content. SFS reduces water absorption while, the GA increased water absorption.
  • The investigation showed that sieve size affects the refinement and performance of the concrete mixture. The peaks of the crystalline phases showed marked difference with the addition of SFS and GA, and after 28 days of curing Ca (OH) 2
  • The use of SFS and GA are compatible, complimenting the deficiencies in each other. The SFS can substitute for fine aggregate in making quality concrete and construction materials.

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