Natural dyes from food processing wastes representative examples

The extract quality of selected examples is discussed in Section 19.5.1, sources presented in more detail are onion peels (19.5.2), nuts (19.5.3), berries (19.5.4), grape pomace (19.5.5) and tea residues (19.5.6).

19.5.1 Colour strength of extract

A comparison of the amount of extracted dyestuff can be made by comparison with commercial reactive dyes. In the literature, Reactive Red 4 (Cibacron Brillant Red 3B-A, Ciba, Basel) was taken as a representative dyestuff.19 Based on the absorbance of this dye, the absorbance of plant material extracts can be used to calculate an equivalent concentration of reactive dye ceq, which will show the same absorbance in solution.29 The calculation can be performed according to equation 19.1:

tRR4d

Table 19.7 Berries and grapes: results of screening for natural dyes, selected colour and fastness properties and assessment of properties as pass/fail

Raw material

Part of plant

Source

Representative data

Pass/fail

Substrate

Mordant

Colour

L*

a*

b*

LF

WF

Black chokeberry

Berries

Conc. juice

Wool

_

Rose

46.22

+13.47

+6.25

2

4-5

Passf

Blackberry

Berries

Pomace

Wool

-

Beige

63.83

+5.28

+14.51

-

5

f

Cherry

Cherries

Distiller's wash

Wool

-

Rose

56.39

+6.43

+6.48

2

4-5

Fail

Sour cherries

Berries

Pomace

Wool

Fe

Beige

55.44

-0.56

+10.27

2

4-5

Fail

Raspberry

Berries

Pomace

Wool

Fe

Grey

52.70

-2.02

+7.85

3

4-5

Pass

Raspberry

Berries

Distiller's wash

Wool

Fe

Grey

40.74

+1.86

+3.40

3-4

5

Pass

Elder

Berries

Pomace

Wool

-

Red-brown

54.36

+4.70

+5.29

2

4-5

Pass*

Elder

Berries

Distiller's wash

Wool

-

Rose

37.13

+13.69

+8.66

2

3-4

Passf

Elder

Berries

Conc. juice

Wool

Al

Violet

41.60

+21.25

+3.27

3

4

Passf

Blackcurrant

Berries

Pomace

Wool

Al

Grey

53.92

-0.40

-4.08

2-3

5

Pass

Blackcurrant

Berries

Conc. juice

Wool

Al

Pink

51.45

+14.94

+6.55

2-3

3-4

Passf

Grapes

Berries

Pomace

Wool

-

Mauve

59.91

+6.76

+5.32

2

3-4

LF, light fastness; WF, water fastness. Water fastness: 1 = poor; 5 = excellent. Light fastness: 1 = poor; 8 = excellent. * Further research needed, improvement of fastness. f Model tests, not real waste.

LF, light fastness; WF, water fastness. Water fastness: 1 = poor; 5 = excellent. Light fastness: 1 = poor; 8 = excellent. * Further research needed, improvement of fastness. f Model tests, not real waste.

Table 19.8 Vegetables: results of screening for natural dyes, selected colour and fastness properties and assessment of properties as pass/fail

Raw material

Part of plant

Source

Representative data

Red cabbage

Leaves of

fruit

Blue potato

Potato

Beans

Crop

Peas

Crop

Onion

Peels

Spinach

Plant

Carrots

Plant

Black carrots

Crop

Beetroot

Crop

Rhubarb

Conc. juice Farming

Representative data

Substrate

Mordant

Colour

L*

a*

b*

LF

WF

Wool

Fe

Olive

47.66

-1.68

+11.61

2-3

5

Pass*f

Wool

Fe

Beige

72.91

+3.27

-0.77

2

-

Failf

Wool

Fe

Beige

78.28

+3.33

+13.67

3

4

Failf

Wool

Fe

Brown

68.48

+4.81

+25.05

4

-

Failf

Wool

-

Orange

52.96

+16.17

+46.58

3

4-5

Pass

Wool

Al

Light yellow

84.31

-5.63

+28.34

1-2

4-5

Failf

Wool

Fe

Beige

67.51

+5.30

+25.98

2-3

-

Failf

Wool

Al

Violet

44.92

+22.85

+1.67

3

4

Passf

Wool

-

Red

47.80

+25.69

+14.64

1

4-5

Pass*f

Wool

Fe

Olive

28.99

-0.29

+19.75

2-3

5

Wastes

Conc. juice Farming

LF, light fastness; WF, water fastness. * Further research needed, improvement of fastness. f Model tests, not real waste.

Table 19.9 Tea, fruits and nuts: results of screening for natural dyes, selected colour and fastness properties and assessment of properties as pass/fail

Part of plant Source

Representative data

Pass/fail

Table 19.9 Tea, fruits and nuts: results of screening for natural dyes, selected colour and fastness properties and assessment of properties as pass/fail

Part of plant Source

Representative data

Pass/fail

material

Substrate

Mordant

Colour

L*

a*

b*

LF

WF

Walnut

Green shell

Processing of green nuts

Wool

Al

Brown

43.28

+9.59

+17.62

4

3-4

Pass

Walnut

Brown shell

Processing of

Wool

-

Beige

68.65

+3.67

+17.35

3-4

4-5

Pass

walnut

Walnut

Young shoot

-

Wool

Fe

Beige

52.29

-0.57

+7.53

3-4

4

Pass

Tea

Leaves

Pomace from ice-tea

Wool

-

Beige

64.94

+4.13

+18.12

3

5

Pass

Hollyhock

Buds

-

Wool

Fe

Green

29.48

-1.87

+2.16

2-3

4-5

Passf

Barberry

Branch, roots

-

Wool

Al

Yellow

79.97

-8.25

+43.37

1

4

Failf

Pomegranate

Peels

-

Wool

Al

Yellow

66.88

+0.98

+40.55

1

4-5

Pass*

LF, light fastness; WF, water fastness. * Further research needed, improvement of fastness. f Model tests, not real waste.

LF, light fastness; WF, water fastness. * Further research needed, improvement of fastness. f Model tests, not real waste.

where ceq is the equivalent concentration of Reactive Red 4 (in g/L), Eextr is the absorbance of the extract, eRR4 is the extinction coefficient of commercial Reactive Red 4 (9.7 L/cm g at l = 508 nm), d is the path length of the cuvette (in cm).

The equivalent concentration ceq - calculated as the mass (in g) of Reactive Red 4 dye per 1 litre of extract - obtained from different materials is given in Table 19.10. Depending on the material used for extraction the maximum absorbance obtained during extraction of the different samples ranges from 0.7 (grapes) to 28.1 (rhubarb), which corresponds to a dyestuff concentration ceq of 0.62-2.9 g/L (calculated as commercial reactive dye). The theoretical equivalence between 1 kg of plant material and the commercial reactive dye Cibacron Brillant Red 3B-A is also shown in Table 19.10. Provided a comparable degree of dyestuff fixation is achieved on the textile substrate, equivalence in colour strength to commercial reactive dyes can be calculated. Extraction of 1 kg of plant waste yields solutions containing natural dyestuff, equivalent to an amount of 0.62-57.9 g of commercial Reactive Red 4. These values indicate substantial potential for application of the extracts as a source for natural dyes.

19.5.2 Flavonoid dyes - onion peels (Allium cepa L.)

The peels of onions, particularly red onion peels, are wildly used for egg coloration at home, but they are also applicable for textile dyeing. The outermost dry papery skins of onions contain different colouring substances. In addition to the flavonoid dyes, for example quercetin, its glucosides and cempferol, the extract also contains tannins (see Fig. 19.4 for the structure of quercetin).2,50 As shown in Table 19.10 the high absorbance of the extracts indicates the remarkable colouristic potential of onion peels; 1 kg of dried

Table 19.10 Dyestuff extraction: maximum absorbance E obtained during extraction using a liquor ratio of 1 : 20, colour yield calculated as equivalent concentration of commercial reactive dye ceq and equivalence mass meq given as mass of commercial reactive dyestuff Reactive Red 4 equivalent to the extract of 1 kg of plant residue

Table 19.10 Dyestuff extraction: maximum absorbance E obtained during extraction using a liquor ratio of 1 : 20, colour yield calculated as equivalent concentration of commercial reactive dye ceq and equivalence mass meq given as mass of commercial reactive dyestuff Reactive Red 4 equivalent to the extract of 1 kg of plant residue

Source

Physical state

Major class of dye component

(wavelength) (nm)

(g/L)

meq (g/kg)

Raspberries

Pomace

Solid

Anthocyan

2.25 (437)

0.23

4.7

Black elder

Pomace

Solid

Anthocyan

1.05 (523)

0.11

2.2

Blackcurrant

Pomace

Solid

Anthocyan

1.15 (519)

0.12

2.4

Grapes

Pomace

Solid

Anthocyan

0.7 (519)

0.07

1.4

Onions

Peels

Solid

Flavonoid

15.5 (450)

1.60

32.0

Rhubarb

Roots

Solid

Anthraquinone

28.1 (405)

2.90

57.9

Black tea

Pomace

Solid

Tannins

1.56

0.16

3.2

Fig. 19.4 Structure of quercetin as a representative for flavenoid dyes.

onion peels corresponds to an equivalent amount of 32 g of commercial reactive dye. The annual amount of onions harvested in Austria is about 100 000 tonnes51 and 10% of this amount is red skin onions.20,51 Onions lose their outermost papery skin during handling or the peels are removed before final use. Traditionally the peels are wastes that are collected and released to farming areas for composting (K. Wais, Karl Wais GmbH (large-scale vegetable merchandising company, personal communication, 2005).20 Thus the material is available in considerable amounts and at low costs. The low specific weight of onion peels may require compression to lower volumes for transportation. Dyeing experiments showed a wide variety of orange/brown/olive shades depending on substrate, mordant and dyeing technology. The substrate's influence on the shade and fastness can be seen more clearly in Table 19.11.

For all types of mordant shown, dyeings on wool and polyamide exhibit darker shades, while for cellulose fibres (flax) lighter shades are observed. The possibility of changing the shade of a dyeing by the changing the mordant is demonstrated for all three types of fibres. Mordanting with alum results in orange shades whereas addition of iron2+/3+ salt changes colour towards olive shades. In the case of onion peels, the use of iron mordant increases light fastness by at least one mark. Water fastness is hardly dependent on the type of substrate, however on flax a remarkable decrease in light fastness from 3 to 1-2 can be observed for direct dyeing and alum mordant. Onion peel extracts are thus only recommended on cellulose textiles when an iron mordant is used.

19.5.3 Naphtoquinone dyes - nuts (Juglans regia L.) In the colour index (C.I.), natural dyes extracted from walnuts are identified as C.I. Natural Brown 7. Walnuts (Juglans Regia L.) have been widely used for dyeing textiles and hair since the middle ages. Some of the oldest still-available recipes are collected in the Innsbrucker Handschrift that were written in 1330 in Tyrol and can now be seen in the library of the University of Innsbruck.52 The tree species was imported from Asia 100 years before Christ. Marcus Terentius Varro brought Juglans Regia L. to Italy where it was re-cultivated.2,53 Traditionally the green shells and young leaves are used for dyeing purposes and beige to brown shades are obtained on wool,

Table 19.11 Onion peels - representative dyeings on different substrates; influence of substrate on colour and fastness properties

Substrate

Mordant

Colour

L*

a*

b*

LF

WF

Wool

-

Orange

49.53

+19.29

+33.06

3

4

Polyamide

-

Brown

48.64

+13.91

+33.64

3

4-5

Flax

-

Brown

68.02

+8.14

+22.73

1-2

4

Wool

Al

Orange

52.96

+16.17

+46.58

3

4-5

Polyamide

Al

Orange

54.10

+15.53

+54.90

3

4-5

Flax

Al

Orange

62.73

+11.20

+54.49

1-2

5

Wool

Fe

Olive

35.57

+0.28

+12.44

4

3-4

Polyamide

Fe

Olive

29.66

+4.57

+18.49

4

4-5

Flax

Fe

Olive

43.74

+0.12

+13.91

3

5

LF, light fastness; WF, water fastness.

LF, light fastness; WF, water fastness.

Table 19.12 Walnut, C.I. Natural Brown 7 - results of dyeings obtained with different parts of walnut trees

Plant material

Substrate

Mordant

L*

a*

b*

DE

LF

WF

Green shells

Wool

-

43.2

+10.04

+21.18

0

4

3-4

Al

44.82

+11.25

+23.28

2.9

3-4

3

Fe

35.65

+3.53

+11.36

14.0

3-4

3-4

Cotton

-

65.35

+0.79

+15.35

0

4

2-3

Al

63.21

+2.04

+14.79

2.5

4

3-4

Fe

57.54

+0.36

+9.66

9.7

3-4

4-5

Brown shells

Wool

-

68.65

+3.67

+17.35

0

3-4

4-5

Al

70.05

+2.66

+21.55

4.5

4

4-5

Flax

Fe

49.03

-0.62

+6.82

22.7

3-4

4-5

-

80.77

+0.53

+10.41

0

4

4

Al

72.45

+2.34

+13.52

9.1

3-4

4

Fe

71.39

-0.89

+5.83

10.5

3-4

4

Young shoots

Wool

-

69.93

+2.87

+16.5

0

3-4

4-5

Al

71.62

-1.2

+29.66

13.9

3-4

4-5

Fe

39.04

-0.48

+6.7

32.6

3-4

5

Cotton

-

86.78

-0.88

+6.75

0

4

4-5

Al

81.74

-2.7

+14.99

9.8

3-4

4-5

Fe

72.84

-1.66

+3.89

14.3

3-4

4-5

DE, CIELab colour difference between direct dyeing and mordant dyeing.

DE, CIELab colour difference between direct dyeing and mordant dyeing.

flax, cotton and polyamide (Table 19.12). In Table 19.12 a comparison of the different dyeings obtained from the various sources of walnut-based plant material is shown.

Walnut leaves contain juglon precursor molecules that change easily to juglon, a quinone compound (see Fig. 19.5). The relative unstable juglon polymerises and results in brown pigments. Besides flavone glycosides, 9-11% o.w. tannins have been identified. The green shells of walnut mainly contain juglon, juglon derivatives and tannin. Collection of green nuts

Fig. 19.5 Structure of juglon as a representative for naphthoquinone dyes.

requires harvesting the complete crop and thus green nuts cannot be said to be real waste. However, considerable numbers of green nuts fall off the trees during the ripening period, and can be seen as a waste product from walnut growth. The potential of walnuts to serve as a source for natural dyes can be estimated from the volume of walnuts harvested in Austria. In 2003, approximately 20 300 tonnes of walnuts were collected and approximately 50% of the weight can be assumed to be released as wastes (mainly dried shells).20 Green nut shells are rather expensive. The price of 1 kg of green dried nut shells differs wildly from €3 to €10 depending on the company's location, distance of transportation and quality.6,20

Alternatively, brown shells from ripe walnuts can be collected and used for dyeing purposes. The material is cheaper and is released as waste, however the colour depths are much lighter (Table 19.12). Green walnut shells are preferable but young shoots and brown shells still contain enough colouring matter to give reasonable results.

Mordanting with iron salt causes remarkable colour changes due to complex formation. While colour differences between direct dyeing and alum mordanting are quite small, iron salt mordanting increases colour depth significantly. On cellulose substrates and wool, good light fastness values near 4 are observed. Results on polyamide fibres are disappointing (light fastness 1-2). Water fastness is not affected as much by the type of substrate. The distinct dependence of light fastness on substrate indicates the need to determine the fastness properties for any selected source on the chosen substrate.

There are other kinds of nut species that can serve as a source for natural dye extraction. Hazel (Corylus avellana L.) leaves contain the colouring substance myricitrin, a flavonoid dye. The extract of the leaves, and fixation with alum, leads to yellow colour shades. In Scotland, hazel willows have been used for dyeing using various recipes, e.g. ripe willows were extracted and dyeing was performed adding alum and ammonium hydroxide to obtain a dark yellow shade.2

19.5.4 Anthocyanin dyes - berries

Anthocyanin dyes are present in many intensively coloured parts of plants like fruits and blossoms. Anthocyanins are glycoside derivatives of

OH O

OH O

Fig. 19.6 Structure of cyanidin as a representative for anthocyanine dyes.
Table 19.13 Representative examples for berry wastes released in Austria

Berries

Latin name

Residue

Physical form

Blackberry

Rubus fruticous L.

Pomace

Solid

Blackcurrant

Ribes nigrum L.

Pomace

Solid

Elder

Sambucus nigra L.

Pomace

Solid

Distiller's wash

Pulp

Conc. juice

Liquid

Raspberry

Rubus idaeus L.

Pomace

Solid

Distiller's wash

Pulp

anthocyanidins (see Fig. 19.6). The glycosidic group increases solubility in water. Depending on the position and number of glycosidic groups, shades vary from orange-red to blue. A mixture of anthocyanin compounds can be extracted from ripe berries, however cultivation of berries exclusively for dyestuff production is prohibited by the high costs of the material. Wastes released from the beverage industry and strong liquor production are available at low costs and could serve as possible sources for natural dyes.

Table 19.13 gives several examples of berry wastes released in Austrian companies.

In the case of the beverage industry, the major part of the colouring matter is intended to be transferred into the juice fraction. However, useful amounts of extractable dyestuff remain in the pressed residue, the so-called 'pomace' (Table 19.10). These residues are released in the wet state and extraction has to follow immediately or stabilisation by drying or freezing is required.20 When the extraction is done exclusively with water, no changes in the further handling of the extracted wastes are required; the wastes can be used, for example, as animal feed.

Another source for dye-containing waste is the well-known strong liquor production in Austria. Plant material (berries, fruits and vegetables) that contains sugar or starch is fermented and high-quality spirit is obtained by distillation. After distillation the remaining plant residue, so-called 'distiller's wash', contains considerable amounts of anthocyanin dyes. Due to the high water content of the waste, immediate use is recommended or possible microbial growth has to be hindered. Residues from the beverage industry and from spirit production are non-hazardous wastes. Thus at present there is only limited information available about amounts and classification of such wastes. Some limited data about agricultural production and processed amounts of berries are available.51 Approximately 10-15% of the processed crop are released in the form of pressed solid wastes. In Europe, the average amount of waste released for certain types of berries can be estimated at 200-500 tonnes per year.19

The shade of anthocyanin dyes is very sensitive to the pH value. To avoid undesired changes of colour, the dyeing conditions, use of mordants and planned applications of the textiles have to be considered carefully. In a scientific study, concentrated juice from different berries were included in the tests to evaluate the potential of such materials for textile dyeing at optimum conditions with regard to the plant material. These results can be used to estimate the potential of a certain type of waste. Table 19.14 shows the results obtained with wastes from the processing of elder berries and with the use of the concentrated juice. Dyeings with concentrated juice exhibit violet shades while application of berry wastes predominantly leads to grey and beige shades.

While dried pomace was extracted with water, the liquid products (concentrated juice and distiller's wash) were just filtered before use. Considering the L values (lightness), as expected the exhaustion of dyestuff on wool is higher than on cotton. Normal standard dyeing procedures were performed at 95 °C. However in case of anthocyan-containing sources, lower dyeing temperatures were found favourable in terms of the shade of the dyeings

Table 19.14 Elder residues - results of dyeings obtained with different wastes from elder processing

Raw material

Substrate

Mordant

Colour

L*

a*

b*

LF

WF

Distiller's

Wool

-

Brown

37.13

+13.69

+8.66

2

4-5

wash

Al

Olive

35.38

+2.75

+7.40

1-2

4-5

Fe

Dark grey

22.68

-0.65

+2.77

2-3

5

Cotton

-

Brown

58.97

+9.32

+2.37

2

3-4

Al

Grey

55.46

+4.24

+1.24

2

4-5

Fe

Dark grey

51.27

-0.48

-2.10

2

4-5

Pomace

Wool

-

Rose

61.06

+4.64

+8.34

2

4-5

Al

Light grey

60.33

-0.02

+2.33

2-3

4-5

Fe

Grey

46.78

-2.98

+2.06

1-2

4-5

Cotton

-

Light rose

82.12

+4.11

+1.86

3

3-4

Al

Light grey

78.13

+0.08

+0.27

2-3

3-4

Fe

Light grey

73.77

-1.59

+0.48

2-3

4-5

Conc.

Wool

Al

Violet

33.07

+10.86

+4.83

2-3

4

juice

Fe

Brown-

43.14

+19.17

+4.93

1

(see Section 19.5.5). In the case of residues from strong liquor production, dyeings were performed at room temperature. Dyeing at room temperature does not change light fastness but wash fastness decreases. The shade obtained with anthocyanin dyes is promising, however light fastness and pH dependence of colour will require further improvement.

19.5.5 Anthocyan dyes - grape peels from vine production

(Vitis vinifera L.)

Production of red vines is quite an important part of agricultural production in Austria. Various sorts of vine grapes are cultivated in the eastern regions of Austria, for example: Zweigelt, Blauer Portugieser, Blauer Burgunder and Cabernet Sauvignon. The pressed grapes contain considerable amounts of red-violet anthocyan dyes, which can be extracted and used for dyeing purposes. An estimation of the amount of grapes harvested for vine production in Austria comes near 100 000 tons per year, and approximately 2025% of the mass will be released as waste. From these residues anthocyan dyes can be extracted with hot water. The red-violet shade of the extract-able dyes in particular, makes them highly interesting for natural dyeing processes. The aqueous extract contains considerable amounts of red dyes, but dyeings obtained on cellulose or woollen samples using the standard dyeing process at 95 °C only showed disappointing colour. Satisfying results could be obtained after the introduction of pre-mordanting based on tannin mordant and lowering dyeing temperature.

Table 19.15 shows dyeing results given as CIELab-values for dyeing obtained with extracted pressed Zweigelt and Blauer Portugieser grapes using the standard process (95 °C) and the modified pre-mordant process. The considerable increase in the a value (red axis) and blue axis (negative b value) demonstrate the positive results. Dried grape pomace was used for

Table 19.15 Dyeing results obtained with extracts from pressed Zweigelt and Blauer Portugieser grapes

Material

Substrate

Mordant

(°C)

L*

a*

b*

LF

WF

Zweigelt

Wool

-

95

60.17

+2.97

+7.10

1

4-5

Wool

Al (meta-)

95

64.15

+3.65

+8.78

1

4-5

Cotton

Tannin (pre-)

RT

60.54

+15.32

-5.44

1-2

3-4

Blauer

Portugieser

Wool

-

95

66.31

+3.40

+9.56

1-2

4-5

Cotton

-

95

76.71

+4.62

-1.81

1

4-5

Cotton

Tannin (pre-)

RT

63.80

+12.01

-3.53

1

3-4

RT, room temperature.

RT, room temperature.

the examples given in Table 19.15. The wet residue after extraction showed an approximately three-fold increase in mass due to water uptake.

Analytical methods to determine the content of dyestuff in the extract are of importance to standardise a raw material for commercial use. In the case of grape extracts, ultraviolet spectroscopy can be applied to determine the concentration of anthocyanins in the extracted material.54 A direct correlation between the analytically determined anthocyanin concentration calculated as monomer anthocyanin pigment and the Kubelka-Munk K/S value of the dyed fabric, measured at 550 nm, proves the suitability of the photometric method for standardising plant residues.55

19.5.6 Condensed tannins - tea (Theaceae)

Particularly in Far Eastern countries tea plants have been used for textile dyeing purposes and research is in progress (see Fig. 19.7). The dyeing of cotton and jute with tea as a natural dye - using alum, copper sulphate or ferrous sulphate mordants - has been studied by Deo and Desai.22 Ice-tea holds a remarkable share in the market of soft drinks. Considerable amounts of residues from industrial production are available. In Austria the amount of wastes released from industrial tea production can be estimated at 200300 tonnes per year. The colour strength of the residues is low, because the majority of the hot-water-soluble coloured components have been extracted during the ice-tea production. One kilogram of dried tea residues is equivalent to 3.3 g of commercial dyestuff.19 Relevant data for colour, i.e. CIELab-coordinates, and fastness properties are summarised in Table 19.16.

The colour of dyeings based on tea residues ranges from beige to grey. The high level of colour fastness and production under quite standardised conditions make these residues very interesting for future use as a source for natural dyes.

OH

Fig. 19.7 Structure of theaflavin as a representative for condensed tannin dyes.

Fig. 19.7 Structure of theaflavin as a representative for condensed tannin dyes.

Table 19.16 CIELab-colour coordinates and selected fastness properties for dyeings obtained with black-tea residues from ice-tea production

Material

Mordant

L*

a*

b*

LF

WF

Wool

-

64.64

+3.72

+17.60

3-4

4-5

Fe

41.54

+0.79

+5.06

3

5

Al

67.55

+2.S4

+21.79

4

5

Cotton (bleached)

-

S5.19

+0.75

+9.12

3-4

4-5

Fe

75.38

-0.62

+2.55

3

4-5

Al

7S.07

+2.04

+12.56

3

4-5

Flax (unbleached)

Al

57.53

+3.64

+16.05

4

-

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