bionad 18 month meeting july 7th, 2015, inescop premises, elda (e) life12 env/it/352 determination...
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BIONAD 18 Month Meeting July 7th, 2015, Inescop Premises , Elda (E)
LIFE12 ENV/IT/352
Determination of trace elements in traditional dyes, naturalized dyes and commercial dyes
Alessandro D’Ulivo
BIONAD 18 Month Meeting July 7th, 2015, Inescop Premises , Elda (E)
LIFE12 ENV/IT/352
Dyes Type Notes
Disperse Blue 27Blue Teratop
Commercial ~ 90% Additives~ 10% Dye
Disperse Red 202 Traditional Acid Dye
Disperse Yellow 42 Traditional Acid Dye
Disperse Blue 27, Purified
Traditional Acid Dye Extracted from Blue Teratop
Disperse Orange 30 Traditional Acid Dye
Red Nat Naturalized Dye Naturalized Red 202
Blue Nat Naturalized Dye 18C UNIFI, DB27
Yellow Nat Naturalized Dye 17D UNIFI, DY42
Orange Nat Naturalized Dye 12D UNIFI, D030
Analized Dyes
Trace element Determination • Pressurized MW Digestion, HNO3 + H2O2
• Determination by Inductively Coupled PlasmaOptical Emission Spectrometry (ICP-OES)Perkin Elmer Optima 8000Elements: Hg, Cd, Pb, Tl
Mn, Cr, V, Co, Ni, Cu, Zn B, As, Sb, Se
Be, Ba Al, Fe
LIFE12 ENV/IT/352
BIONAD 18 Month Meeting July 7th, 2015, Inescop Premises , Elda (E)
Direct Determination of Mercury
• Direct determination of Hg in solid and liquid samples• Digestion not required• No Hg losses• No Hg contamination• Typical Sample size 100 - 500 mg • L.O.Q < 20 pg Hg (< 0.2 ppb)• DMA-80: fully compliant with US EPA method 7473 and with ASTM method D-6722-01.
Mercury Determination at sub p.p.b. Level
LIFE12 ENV/IT/352
BIONAD 18 Month Meeting July 7th, 2015, Inescop Premises , Elda (E)
Direct Determination of MercuryResults
LIFE12 ENV/IT/352
BIONAD 18 Month Meeting July 7th, 2015, Inescop Premises , Elda (E)
Hg Tl Cd Se As Co Pb Cr V Be Ni Mn Zn Al Cu Fe B Ba
1E-3
0,01
0,1
1
10
DECRETO MINISTERIALE 12 giugno 2003, n. 185«Regolamento recante norme tecniche per il riutilizzodelle acque reflue in attuazione dell’articolo26, comma 2, del D.Lgs. 11 maggio 1999, n. 152».(G.U. 23 luglio 2003, n. 169)
Max
imun
Con
cent
ratio
n (m
g/L)
Metal
Concentration Limits for reusing waste waters
Detected Elements inat least one of the Dyes
Hg, Se, Pb, Cr, V, Be, Ni, Mn, Zn, Al, Cu, Fe, B, Ba
Above Limit of quantification L.O.Q. = 10 s
Elements Non-Detectedin any dyes
Tl 0.17 ; Cd 0.1; As 1.0; Co 0.17 [Sb 1.7 ] (mg/kg)
Below the reported L.O.Q.
Indicators of potential hazard level
Direct Determination of Mercury
LIFE12 ENV/IT/352
BIONAD 18 Month Meeting July 7th, 2015, Inescop Premises , Elda (E)
Red202 Yell 42 Blue27
Orang 30
Red Nat
Yell Nat
Blue Nat
Orang Nat
Blue COM
LOQ mg/kg
Hg 0,089 0,056 0,003 0,011 0,013 0,012 0,022 0,019 0,66 0,0002
Se - (*) 2,4 - - - - - - - 1,7
Pb 1,3 2,0 3,7 1,5 - 2,2 - - 3,5 0,8
Cr 0,6 0,6 1,1 - 4,5 0,8 2,1 0,4 2,8 0,17
V - 0,7 - 1,1 1,2 1,2 1,0 1,3 1,8 0,4
Be - - - 0,3 0,27 0,31 - 0,3 0,07
Ni - - 0,5 - 2,1 - 1,2 2,1 0,42
Mn 0,3 0,9 - 0,25 0,56 - 0,25 0,19 59,1 0,08
Zn 1,6 4,6 1,7 0,6 6,4 17,7 15,5 2,8 10,6 0,17
Al - 64,3 - - 6,6 - - 0,9 26,1 0,8
Cu 1,4 0,4 1,0 - - - - - 11,4 0,3
Fe 33,7 29,2 2,0 1,8 49,7 1,7 2,1 1,0 112,4 0,08
B 29 3,6 - - - - - - 64 0,83
Ba - 1,705 - - 0,170 - 0,186 0,025 2,991 0,02
(*) LOQ ; Below LOQ in all samples: Co 0.17; Sb 1.7; As 1.0; Tl 1.7; Cd 0.1 mg/kg
Direct Determination of MercuryTotal Metal Content
LIFE12 ENV/IT/352
BIONAD 18 Month Meeting July 7th, 2015, Inescop Premises , Elda (E)
1 2 3 4 5 6 7 8 90
50
100
150
200
250
300Total Metal Content B-Comm
Met
als
(mg/
kg)
Dyes
Traditional Naturalized
1 2 3 4 5 6 7 8 90
20
40
60
80
100
120
140
160
B-Comm
RN YN BN ONOB*Y
Tot
al M
etal
s (m
g/kg
)
Dyes
RTraditional Naturalized
Total Metal Content
Al and Fe not included
Hg, Cd, Pb, TlMn, Cr, V, Co, Ni, Cu, Zn
B, As, Sb, SeBe, Ba
+ Al, Fe
160 mg/kg 298 mg/kgCommercialDisperse Blue27Blue Teratop
Direct Determination of MercuryMercury and Lead
LIFE12 ENV/IT/352
BIONAD 18 Month Meeting July 7th, 2015, Inescop Premises , Elda (E)
1 2 3 4 5 6 7 8 90,0
0,1
0,2
0,3
0,4
0,5
0,6
0,7
B-Comm
Naturalized
Traditional
Hg
(mg/
kg)
Dyes
MercuryLOQ=0.0002 mg/kg
1 2 3 4 5 6 7 8 90
1
2
3
4
5
6
7
L e a dLOQ=0.83 mg/kg
B-Comm
Pb
(mg/
kg)
Dyes
Traditional
Naturalized
(1) Red202 (2) Yellow (3) Blue 27 (purified)) (4) Orange30
(5) Red202Nat (6) Yellow Nat ( 7) Blue Nat (8) OrangeNat
(9) Disperse Blue 27 – Blue Teratop
Direct Determination of MercuryChromium and Vanadium
LIFE12 ENV/IT/352
BIONAD 18 Month Meeting July 7th, 2015, Inescop Premises , Elda (E)
1 2 3 4 5 6 7 8 90
1
2
3
4
5
6
ChromiumLOQ = 0.17 mg/kg
B-Comm
Cr (m
g/kg
)
Dyes
Traditional
Naturalized
1 2 3 4 5 6 7 8 90,0
0,5
1,0
1,5
2,0B-Comm
V (m
g/kg
)
Dyes
VanadiumLOQ=0.4 mg/kg
Traditional
Naturalized
(1) Red202 (2) Yellow (3) Blue 27 (purified)) (4) Orange30
(5) Red202Nat (6) Yellow Nat ( 7) Blue Nat (8) OrangeNat
(9) Disperse Blue 27 – Blue Teratop
Direct Determination of MercuryNickel and Manganese
LIFE12 ENV/IT/352
BIONAD 18 Month Meeting July 7th, 2015, Inescop Premises , Elda (E)
1 2 3 4 5 6 7 8 90,0
0,5
1,0
1,5
2,0
B-Comm
Ni (
mg/
kg)
Dyes
NickelLOQ=0.4 mg/kg
Traditional
Naturalized
1 2 3 4 5 6 7 8 90
10
20
30
40
50
60
B-Comm ManganeseLOQ=0.08 mg/kg
Naturalized
Mn
(mg/
kg)
Dyes
Traditional
(1) Red202 (2) Yellow (3) Blue 27 (purified)) (4) Orange30
(5) Red202Nat (6) Yellow Nat ( 7) Blue Nat (8) OrangeNat
(9) Disperse Blue 27 – Blue Teratop
Direct Determination of MercuryZinc and Copper
LIFE12 ENV/IT/352
BIONAD 18 Month Meeting July 7th, 2015, Inescop Premises , Elda (E)
1 2 3 4 5 6 7 8 90
2
4
6
8
10
12
14
16
18
20
22 ZincLOQ=0.2 mg/kg
B-CommZn
(mg/
kg)
Dyes
Traditional
Naturalized
1 2 3 4 5 6 7 8 90
2
4
6
8
10
12 CopperLOQ=0.3 mg/kg B-Comm
Cu
(mg/
kg)
Dyes
Traditional
Naturalized
(1) Red202 (2) Yellow (3) Blue 27 (purified)) (4) Orange30
(5) Red202Nat (6) Yellow Nat ( 7) Blue Nat (8) OrangeNat
(9) Disperse Blue 27 – Blue Teratop
Direct Determination of MercuryAluminum and Iron
LIFE12 ENV/IT/352
BIONAD 18 Month Meeting July 7th, 2015, Inescop Premises , Elda (E)
1 2 3 4 5 6 7 8 90
10
20
30
40
50
60
70
80
90
100 AluminumLOQ=0.83 mg/kg
B-Comm
Al (
mg/
kg)
Dyes
Traditional
Naturalized
1 2 3 4 5 6 7 8 90
20
40
60
80
100
120 B-Comm I r o nLOQ=0.08 mg/kg
Fe
(mg/
kg)
Dyes
Traditional
Naturalized
(1) Red202 (2) Yellow (3) Blue 27 (purified)) (4) Orange30
(5) Red202Nat (6) Yellow Nat ( 7) Blue Nat (8) OrangeNat
(9) Disperse Blue 27 – Blue Teratop
Direct Determination of MercuryBoron and Barium
LIFE12 ENV/IT/352
BIONAD 18 Month Meeting July 7th, 2015, Inescop Premises , Elda (E)
1 2 3 4 5 6 7 8 90
10
20
30
40
50
60 BoronLOQ=0.83 mg/kg
B-Comm
B (m
g/kg
)
Dyes
Traditional
Naturalized
1 2 3 4 5 6 7 8 90,0
0,5
1,0
1,5
2,0
2,5
3,0
Ba
(mg/
kg)
Dyes
BariumLOQ=0.02 mg/kg
Traditional
Naturalized
(1) Red202 (2) Yellow (3) Blue 27 (purified)) (4) Orange30
(5) Red202Nat (6) Yellow Nat ( 7) Blue Nat (8) OrangeNat
(9) Disperse Blue 27 – Blue Teratop
BIONAD 18 Month Meeting July 7th, 2015, Inescop Premises , Elda (E)
LIFE12 ENV/IT/352
Commercial Dye mixture containing additves present a much higher content of hazardous elements with respect to both traditional acid and naturalized dyes.
Contamination in commercial dyes is probably due to use of additives with low degree of purity.
Naturalized dyes, needing none additives, present a much lower environmental impact for hazardous elements with respect to traditional acid dyes.
Conclusion
BIONAD 18 Month Meeting July 7th, 2015, Inescop Premises , Elda (E)
LIFE12 ENV/IT/352
Screening of hazardous elements will be expanded to more samples:
Commercial Dyes (containing additives) Acid Dyes (Extracted from Commercial)
- Teratop Yellow GWL - Yellow DY42- Terasil Brown 2RFL - Orange D030- Foron Bruno Giallo S-2RFL - Red 202- Foron Rosso Brillante
Future Activities
Toxic metals /elements (mg/kg or ppm) con ICP-OESTraditional Dyes Naturalized Dyes Commercial Dyes
Disperse RED 202
Disperse Yellow 42
Disperse Blue 27
(purified)
Disperse Orange
30Red 202 Red nat
17D Unifi DY42 Yellow
nat
18 C Unifi DB27
Blue nat
12D Unifi D030
Orange natDisperse Blue 27
Blue TeratopL.O.Q .
mg/kg Dyes
Hg (*) 0,089 0,056 0,003 0,011 0,022 0,012 0,019 0,013 0,66 0,0002
B 29,0 3,6 - - - - - - 64,0 0,83
V - 0,7 - 1,1 1,2 1,2 1,1 1,3 1,8 0,42
Cr 0,6 0,6 1,1 4,5 0,8 2,1 0,4 2,8 0,17
Mn 0,3 0,9 - 0,3 0,6 - 0,3 0,2 59,0 0,08
Ni - - 0,5 - 2,1 - 1,2 - 2,2 0,42
Cu 1,4 0,4 1,0 - - - - - 12,0 0,33
Zn 1,6 4,6 1,7 0,6 6,4 17,7 15,5 2,8 11,0 0,17
Be - - - 0,3 0,3 0,3 - 0,3 - 0,07
Ba - 1,7 - - 0,2 - 0,2 0,0 3,0 0,02
Pb 1,3 2,0 3,7 1,5 - 2,2 - - 3,5 0,83
Se - 2,4 - - - - - - - 1,67
Total Me 34,4 18,0 8,0 3,8 15,2 22,3 20,4 5,0 160,0
In all samples : Co 0.17; Sb 1.7; As 1.0; Tl 1.7; Cd 0.1 mg/kg . (*) Direct mercury analysis, DMA80
BIONAD 18 Month Meeting July 7th, 2015, Inescop Premises , Elda (E)
LIFE12 ENV/IT/352
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