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REFERENCE MATERIAL
IAEA-383
ORGANOCHLORINE COMPOUNDS, PETROLEUM HYDROCARBONS AND STEROLS
IN
SEDIMENT

Intended Use
This sample is intended to be used as a reference material for the determination of chlorinated compounds, petroleum hydrocarbons and sterols in sediment samples. It can also be used as a quality control material for the assessment of a laboratory's analytical work, for the validation of analytical methods and for quality assurance within a laboratory.

Origin and preparation of the material
    About 30 kg of sediment from the Lagoon of Venice (Italy) was collected. This sediment was deep-frozen, freeze-dried, ground and sieved to pass through a 250 µm stainless steel sieve. This powder, with a particle size of less than 250 µm was homogeneized by mixing in a rotating drum for two weeks. Then, aliquots of about 35 grams were packed into glass bottles with aluminium screw caps and sealed with teflon tape.

Date of Release:

November 1998
Unit Price:
130 €
Unit Size:
35 g

Producer:
Marine Environment Laboratory (MEL)
International Atomic Energy Agency
B.P. No 800
MC-98012 Monaco Supplier:
Analytical Quality Control Services
Agency's Laboratories, Seibersdorf
A-2444 Seibersdorf, Austria

Reference Sheet: IAEA-383(.pdf)

Analyte Status Concentration
[ng/g] (Based on dry weight) 95% C. I.
[ng/g] N *

Chlorinated pesticides

alpha- HCH I 0.29 0.13 - 3.7 8

beta- HCH I 0.57 0.26 - 9.7 5

gamma- HCH (Lindane) I 0.46 0.16 - 1.1 23

HCB I 38 17 - 57 35

pp’ DDE R 1.2 0.75 - 1.8 30

pp’ DDD I 1.8 0.8 - 3.6 28

pp’ DDT I 2.4 0.86 - 6.1 24

op DDE I 0.21 0.062 - 0.73 3

op DDD I 1.2 0.54 - 2.5 6

op DDT I 0.39 0.067 - 0.82 3

Aldrin I 1.4 0.84 - 5.9 8

Endrin I 1.1 0.4 - 1.8 8

Dieldrin I 0.27 0.1 - 0.57 13

Heptachlor I 1 0.51 - 2.5 9

Heptachlor Epoxide I 1.5 0.42 - 5.9 8

alpha- Endosulfan I 0.31 0.15 - 0.57 6

Endosulfan Sulfate I 1.7 0.92 - 7.1 3

alpha- Chlordane I 0.47 0.06 - 0.73 3

gamma- Chlordane I 1.4 0.8 - 1.9 3

Aroclor 1254 R 36 24 - 48 10

Aroclor 1260 I 22 14 - 34 10

Hydrocarbons

Total Aliphatics I 52000 14000 - 85000 6

n - C 17 R 380 330 - 470 11

Pristane I 87 36 - 240 10

n - C 18 I 83 42 - 230 10

Phytane I 57 43 - 150 9

SUM n Alkanes (C 14 - C 34) I 6100 5300 - 6800 8

Phenanthrene R 160 140 - 190 17

2 Methyl Phenanthrene R 31 24 - 38 7

1 Methyl Phenanthrene R 24 18 - 28 10

Anthracene R 30 25 - 34 9

Chrysene R 170 120 - 220 16

Fluorene R 27 24 - 34 9

Fluoranthene R 290 260 - 350 16

Pyrene R 280 210 - 350 19

Benzo (k) Fluoranthene R 73 48 - 76 8

Benz (a) Anthracene R 105 83 - 130 16

Benzo (e) Pyrene R 160 120 - 210 12

Benzo (a) Pyrene R 120 77 - 140 16

Naphthalene R 96 52 - 110 12

Benzo (ghi) Perylene R 190 69 - 230 16

Indeno (123cd) Pyrene I 150 130 - 160 8

UVF equival. Chrysene I 13000 1800 - 28000 6

UVF equival. ROPME oil I 96000 12000 - 225000 7

Resolved Aliphatics I 9600 6700 - 24000 9

Unresolved Aliphatics I 52000 11000 - 79000 7

Total Aromatics I 8800 1500 - 22000 5

Resolved Aromatics I 2500 400- 6000 7

Unresolved Aromatics I 6600 1100 - 16000 5

Benzo (b) Fluoranthene R 150 96 - 190 8

Perylene R 58 41 - 130 7

1 Methyl Naphthalene R 14 11 - 28 6

2 Methyl Naphthalene I 36 26 - 43 4

2,6 Dimethyl Naphthalene I 13 7.1 - 23 4

Dibenz (ah) Anthracene I 20 18 - 41 5

Acenaphthene R 16 13 - 21 8

Acenaphthylene R 47 31 - 59 8

Biphenyl I 29 19 - 30 3

PCBs

PCB No 18 I 1.5 1.2 - 1.9 4

PCB No 28 R 1.7 1.3 - 2.5 17

PCB No 31 R 1.8 1.7 - 2.1 5

PCB No 44 I 2 1.9 - 2.1 4

PCB No 49 R 1.6 1.1 - 1.9 6

PCB No 52 R 3.8 2.6 - 4.9 24

PCB No 66 I 0.89 0.65 - 1.1 4

PCB No 87 I 1.8 1.1 - 4.0 4

PCB No 95 I 0.19 0.04 - 6.9 4

PCB No 97 I 1.6 1.2 - 2.0 4

PCB No 99 I 0.9 0.75 - 1.4 4

PCB No 101 R 2.4 1.9 - 3.2 24

PCB No 105 R 0.49 0.4 - 0.7 13

PCB No 110 R 1.0 0.97 - 1.10 10

PCB No 118 R 1.7 1.2 - 2.6 24

PCB No 128 R 1.2 1.1 - 1.6 6

PCB No 137 R 1.7 1.3 - 3.1 27

PCB No 138 R 0.17 0.08 - 0.36 7

PCB No 141 I 0.21 0.16 - 0.76 7

PCB No 149 R 0.43 0.38 - 0.52 17

PCB No 151 I 0.58 0.37 - 1.1 3

PCB No 153 R 4.3 2.3 - 5.4 17

PCB No 156 I 0.47 0.24 - 0.78 7

PCB No 158 I 0.39 0.18 - 0.57 4

PCB No 170 R 0.82 0.62 - 1.3 11

PCB No 174 I 0.67 0.42 - 0.92 4

PCB No 177 I 0.56 0.35 - 0.73 4

PCB No 180 R 2.5 1.9 - 3.4 17

PCB No 183 R 0.47 0.34 - 0.57 6

PCB No 185 I 0.14 0.073 - 0.18 3

PCB No 187 R 1.3 0.63 - 1.5 10

PCB No 189 I 0.07 0.041 - 1.4 4

PCB No 194 R 0.54 0.31 - 0.73 7

PCB No 195 I 0.24 0.13 - 0.29 5

PCB No 199 I 0.091 0.01 - 0.35 3

PCB No 200 I 0.16 0.051 - 0.22 3

PCB No 201 I 0.71 0.28 - 0.74 3

PCB No 205 I 0.033 0.027 - 0.05 3

PCB No 206 I 0.48 0.44 - 1.1 5

PCB No 207 I 0.094 0.05 - 0.19 3

PCB No 209 R 2.1 1.2 - 3 7

Sterols

Coprostanol I 590 420 - 940 4

Cholesterol I 1200 1030 - 1215 3

Cholestanol I 840 580 - 1100 3

beta- Sistosterol I 700 570 - 950 3

Campesterol I 270 140 -510 3

*
Number of accepted laboratory results which were used to calculate the recommended or information values and their respective confidence intervals about the median value.

(R/I) Classification assigned to the property value for Analyte (Recommended/Information)

The values listed above were established on the basis of statistically valid results submitted by laboratories which had participated in an international intercomparison exercise conducted between 1997 - 1998. The details concerning the criteria for qualification as a recommended or information value can be found in the report (IAEA/AL/115; IAEA/MEL/65), "World-wide and Regional Intercomparison for Determination of Organochlorine Compounds, Petroleum Hydrocarbons and Sterols in Sediment Sample IAEA-383" [1]. This report is available free of charge upon request.

Homogeneity
    The homogeneity of the material for organochlorine compounds, petroleum hydrocarbons and sterols was checked by determining the concentration of some compounds (chlorinated pesticides, petroleum hydrocarbons and sterols) in 10 replicate analyses taken at random from the bulk material. A one-way variance analysis indicated that the material could be considered homogeneous.

Dry weight determination
    The moisture content of the lyophilized sample as determined by drying to a constant weight at 105°C, was found to be 2.0 %. Since the moisture content can change with the ambient humidity and temperature, it was recommended that the water content of this material always be determined in a separate sub-sample (not that taken for analysis) by drying to a constant weight (~24 hours) at 105°C. Results should always be reported on a dry weight basis.

Instructions for use
The recommended sample size for analysis is 10 g. Analysts are reminded to take appropriate precautions in order to avoid contamination of the material during handling. The material should be stored in the dark and kept in a refrigerator.

References:

[1]
Villeneuve J. P., Carvalho F. and Cattini C., World-wide and Regional Intercomparison for Determination of Organochlorine Compounds, Petroleum Hydrocarbons and Sterols in Sediment Sample IAEA-383. IAEA/AL/115 (IAEA/MEL/65), IAEA, Monaco, 1998.

Last updated 30 March 2004

*Date of Release:* November 1998	*Unit Price:* 130 €	*Unit Size:* 35 g
*Producer:* Marine Environment Laboratory (MEL) International Atomic Energy Agency B.P. No 800 MC-98012 Monaco	*Supplier:* Analytical Quality Control Services Agency's Laboratories, Seibersdorf A-2444 Seibersdorf, Austria
Reference Sheet: IAEA-383(.pdf)

Analyte	Status	Concentration [ng/g] *(Based on dry weight)*	95% C. I. [ng/g]	N *
Chlorinated pesticides
alpha- HCH	I	0.29	0.13 - 3.7	8
beta- HCH	I	0.57	0.26 - 9.7	5
gamma- HCH (Lindane)	I	0.46	0.16 - 1.1	23
HCB	I	38	17 - 57	35
pp’ DDE	R	1.2	0.75 - 1.8	30
pp’ DDD	I	1.8	0.8 - 3.6	28
pp’ DDT	I	2.4	0.86 - 6.1	24
op DDE	I	0.21	0.062 - 0.73	3
op DDD	I	1.2	0.54 - 2.5	6
op DDT	I	0.39	0.067 - 0.82	3
Aldrin	I	1.4	0.84 - 5.9	8
Endrin	I	1.1	0.4 - 1.8	8
Dieldrin	I	0.27	0.1 - 0.57	13
Heptachlor	I	1	0.51 - 2.5	9
Heptachlor Epoxide	I	1.5	0.42 - 5.9	8
alpha- Endosulfan	I	0.31	0.15 - 0.57	6
Endosulfan Sulfate	I	1.7	0.92 - 7.1	3
alpha- Chlordane	I	0.47	0.06 - 0.73	3
gamma- Chlordane	I	1.4	0.8 - 1.9	3
Aroclor 1254	R	36	24 - 48	10
Aroclor 1260	I	22	14 - 34	10
Hydrocarbons
Total Aliphatics	I	52000	14000 - 85000	6
n - C 17	R	380	330 - 470	11
Pristane	I	87	36 - 240	10
n - C 18	I	83	42 - 230	10
Phytane	I	57	43 - 150	9
SUM n Alkanes (C 14 - C 34)	I	6100	5300 - 6800	8
Phenanthrene	R	160	140 - 190	17
2 Methyl Phenanthrene	R	31	24 - 38	7
1 Methyl Phenanthrene	R	24	18 - 28	10
Anthracene	R	30	25 - 34	9
Chrysene	R	170	120 - 220	16
Fluorene	R	27	24 - 34	9
Fluoranthene	R	290	260 - 350	16
Pyrene	R	280	210 - 350	19
Benzo (k) Fluoranthene	R	73	48 - 76	8
Benz (a) Anthracene	R	105	83 - 130	16
Benzo (e) Pyrene	R	160	120 - 210	12
Benzo (a) Pyrene	R	120	77 - 140	16
Naphthalene	R	96	52 - 110	12
Benzo (ghi) Perylene	R	190	69 - 230	16
Indeno (123cd) Pyrene	I	150	130 - 160	8
UVF equival. Chrysene	I	13000	1800 - 28000	6
UVF equival. ROPME oil	I	96000	12000 - 225000	7
Resolved Aliphatics	I	9600	6700 - 24000	9
Unresolved Aliphatics	I	52000	11000 - 79000	7
Total Aromatics	I	8800	1500 - 22000	5
Resolved Aromatics	I	2500	400- 6000	7
Unresolved Aromatics	I	6600	1100 - 16000	5
Benzo (b) Fluoranthene	R	150	96 - 190	8
Perylene	R	58	41 - 130	7
1 Methyl Naphthalene	R	14	11 - 28	6
2 Methyl Naphthalene	I	36	26 - 43	4
2,6 Dimethyl Naphthalene	I	13	7.1 - 23	4
Dibenz (ah) Anthracene	I	20	18 - 41	5
Acenaphthene	R	16	13 - 21	8
Acenaphthylene	R	47	31 - 59	8
Biphenyl	I	29	19 - 30	3
PCBs
PCB No 18	I	1.5	1.2 - 1.9	4
PCB No 28	R	1.7	1.3 - 2.5	17
PCB No 31	R	1.8	1.7 - 2.1	5
PCB No 44	I	2	1.9 - 2.1	4
PCB No 49	R	1.6	1.1 - 1.9	6
PCB No 52	R	3.8	2.6 - 4.9	24
PCB No 66	I	0.89	0.65 - 1.1	4
PCB No 87	I	1.8	1.1 - 4.0	4
PCB No 95	I	0.19	0.04 - 6.9	4
PCB No 97	I	1.6	1.2 - 2.0	4
PCB No 99	I	0.9	0.75 - 1.4	4
PCB No 101	R	2.4	1.9 - 3.2	24
PCB No 105	R	0.49	0.4 - 0.7	13
PCB No 110	R	1.0	0.97 - 1.10	10
PCB No 118	R	1.7	1.2 - 2.6	24
PCB No 128	R	1.2	1.1 - 1.6	6
PCB No 137	R	1.7	1.3 - 3.1	27
PCB No 138	R	0.17	0.08 - 0.36	7
PCB No 141	I	0.21	0.16 - 0.76	7
PCB No 149	R	0.43	0.38 - 0.52	17
PCB No 151	I	0.58	0.37 - 1.1	3
PCB No 153	R	4.3	2.3 - 5.4	17
PCB No 156	I	0.47	0.24 - 0.78	7
PCB No 158	I	0.39	0.18 - 0.57	4
PCB No 170	R	0.82	0.62 - 1.3	11
PCB No 174	I	0.67	0.42 - 0.92	4
PCB No 177	I	0.56	0.35 - 0.73	4
PCB No 180	R	2.5	1.9 - 3.4	17
PCB No 183	R	0.47	0.34 - 0.57	6
PCB No 185	I	0.14	0.073 - 0.18	3
PCB No 187	R	1.3	0.63 - 1.5	10
PCB No 189	I	0.07	0.041 - 1.4	4
PCB No 194	R	0.54	0.31 - 0.73	7
PCB No 195	I	0.24	0.13 - 0.29	5
PCB No 199	I	0.091	0.01 - 0.35	3
PCB No 200	I	0.16	0.051 - 0.22	3
PCB No 201	I	0.71	0.28 - 0.74	3
PCB No 205	I	0.033	0.027 - 0.05	3
PCB No 206	I	0.48	0.44 - 1.1	5
PCB No 207	I	0.094	0.05 - 0.19	3
PCB No 209	R	2.1	1.2 - 3	7
Sterols
Coprostanol	I	590	420 - 940	4
Cholesterol	I	1200	1030 - 1215	3
Cholestanol	I	840	580 - 1100	3
beta- Sistosterol	I	700	570 - 950	3
Campesterol	I	270	140 -510	3

*	Number of accepted laboratory results which were used to calculate the recommended or information values and their respective confidence intervals about the median value.
(R/I)	Classification assigned to the property value for Analyte (Recommended/Information)