Links

IAEA Reference Materials

Reference Sheets

REFERENCE MATERIAL
IAEA-408
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
    A large sample of sediment was collected from the mudflats of the Tagus estuary. This sediment was deep-frozen, freeze-dried, ground and sieved through a 150 µm stainless steel sieve.
    The sediment fraction of particle size less than 150 µm was homogenized by mixing in a rotating drum for two weeks. Then, aliquots of about 40 grams were packaged into glass bottles with aluminium screw caps and sealed with Teflon tape.

Date of Release:

November 1999
Unit Price:
130 €
Unit Size:
40 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-408(.pdf)

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

Chlorinated pesticides

alpha- HCH I 0.61 0.21 - 1.5 4

beta- HCH I 0.55 0.38 - 1.7 5

gamma- HCH (Lindane) R 0.19 0.11 - 0.2 14

HCB R 0.41 0.3 - 0.57 25

pp’ DDE R 1.4 0.88 - 2.0 34

pp’ DDD I 0.87 0.56 - 1.7 30

pp’ DDT R 0.67 0.48 - 0.98 21

op DDD I 0.19 0.18 - 0.33 4

op DDT I 0.38 0.09 - 3.8 3

Aldrin I 0.41 0.2 - 2.3 11

Endrin I 0.57 0.14 - 1.2 7

Dieldrin R 0.3 0.3 - 0.48 13

Heptachlor I 0.42 0.23 - 0.7 7

Heptachlor Epoxide I 0.64 0.43 - 1.5 10

alpha- Endosulfan I 1.6 0.3 - 6.2 3

Endosulfan Sulfate I 1.6 0.5 - 8.2 3

alpha- Chlordane I 0.12 0.1 - 0.34 5

gamma- Chlordane I 0.27 0.06 - 0.48 6

Aroclor 1254 I 19 14 - 40 10

Aroclor 1260 I 10 6.8 - 25 11

Hydrocarbons

Total Aliphatics I 120000 81000 - 160000 4

n - C 17 R 74 56 - 140 8

Pristane R 69 50 - 130 10

n - C 18 I 90 60 - 110 7

Phytane R 78 63 - 130 9

SUM n Alkanes (C 14 - C 34) R 8100 4300 -12000 8

Phenanthrene R 35 21 - 43 15

2 Methyl Phenanthrene I 12 12 - 14 4

1 Methyl Phenanthrene I 10 9.2 - 11 6

Anthracene R 9.8 8.0 - 13 9

Chrysene R 35 25 - 56 16

Fluorene I 6.7 4.6 - 24 7

Fluoranthene R 84 53 - 110 18

Pyrene R 77 57 - 93 17

Benzo (b) Fluoranthene R 46 32 - 69 8

Benzo (k) Fluoranthene R 46 26 - 61 8

Benz (a) Anthracene R 53 35 - 60 13

Benzo (e) Pyrene R 55 51 - 81 8

Benzo (a) Pyrene R 48 30 - 63 14

Naphthalene R 27 16 - 47 13

Benzo (ghi) Perylene R 38 20 - 52 12

Indeno (123cd) Pyrene I 51 45 - 53 5

UVF equival. Chrysene I 6000 4600 - 19000 6

UVF equival. ROPME oil I 49000 35000 - 120000 4

Resolved Aliphatics R 11000 6400 - 17000 7

Unresolved Aliphatics I 110000 68000 - 150000 4

Total Aromatics I 3700 1300 -11000 4

Resolved Aromatics I 1900 240- 6800 4

Perylene R 320 140 - 420 7

1 Methyl Naphthalene I 7.5 4.7 - 12 4

2 Methyl Naphthalene I 14 13 - 33 3

Dibenz (ah) Anthracene I 11 7.8 - 14 3

Acenaphthene I 3.3 2.0 - 17 4

Acenaphthylene I 3.6 2.1 - 4.7 4

PCBs

PCB No 8 I 0.24 0.22 - 4.6 3

PCB No 18 I 0.74 0.13 - 1.9 6

PCB No 28 R 0.79 0.35 - 0.98 14

PCB No 31 I 0.43 0.09 - 1.5 3

PCB No 44 I 0.47 0.23 - 3.0 9

PCB No 49 I 0.35 0.22 - 0.38 4

PCB No 52 R 0.6 0.38 - 0.93 18

PCB No 87 I 0.87 0.26 - 1.1 3

PCB No 101 R 1.2 0.81 - 1.7 23

PCB No 105 R 0.57 0.44 - 0.67 9

PCB No 110 R 0.83 0.5 - 0.9 6

PCB No 118 R 1.2 0.9 - 1.6 21

PCB No 128 R 0.33 0.27 - 0.53 10

PCB No 138 R 1.6 1.1 - 2.1 22

PCB No 149 R 1.4 1.3 - 1.6 7

PCB No 153 R 1.9 0.98 - 2.1 20

PCB No 156 I 0.36 0.31 - 0.39 4

PCB No 170 R 0.47 0.34 - 0.59 8

PCB No 174 I 0.34 0.2 - 0.44 4

PCB No 177 I 0.35 0.23 - 0.43 4

PCB No 180 R 1.1 0.85 - 1.2 20

PCB No 183 I 0.32 0.26 - 0.33 3

PCB No 187 R 0.68 0.49 - 0.94 7

PCB No 194 R 0.2 0.2 - 0.23 5

PCB No 195 I 0.12 0.06 - 0.16 4

PCB No 196 I 0.22 0.17 - 0.4 3

Sterols

Coprostanol I 1900 1700^§ 3

Cholesterol I 910 670^§ 3

Cholestanol I 1100 760^§ 3

beta- Sistosterol I 1100 640^§ 3

Campesterol I 2200 2200^§ 2

*
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)

^§ Standard deviation

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 1998 - 1999. The details concerning the criteria for qualification as a recommended or information value can be found in the report (IAEA/AL/121; IAEA/MEL/67), "World-wide and Regional Intercomparison for Determination of Organochlorine Compounds, Petroleum Hydrocarbons and Sterols in Sediment Sample IAEA-408" [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 3.7 %. 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 5 g for petroleum hydrocarbons and 10 g for organochlorines respectively. 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., de Mora S. J., Cattini C. and Carvalho F., World-wide and Regional Intercomparison for Determination of Organochlorine Compounds, Petroleum Hydrocarbons and Sterols in Sediment Sample IAEA-408. IAEA/AL/121 (IAEA/MEL/67), IAEA, Monaco, 1999.

Last updated 30 March 2004

*Date of Release:* November 1999	*Unit Price:* 130 €	*Unit Size:* 40 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-408(.pdf)

Analyte	Status	Concentration [ng/g] *(Based on dry weight)*	95% C. I. [ng/g]	N *
Chlorinated pesticides
alpha- HCH	I	0.61	0.21 - 1.5	4
beta- HCH	I	0.55	0.38 - 1.7	5
gamma- HCH (Lindane)	R	0.19	0.11 - 0.2	14
HCB	R	0.41	0.3 - 0.57	25
pp’ DDE	R	1.4	0.88 - 2.0	34
pp’ DDD	I	0.87	0.56 - 1.7	30
pp’ DDT	R	0.67	0.48 - 0.98	21
op DDD	I	0.19	0.18 - 0.33	4
op DDT	I	0.38	0.09 - 3.8	3
Aldrin	I	0.41	0.2 - 2.3	11
Endrin	I	0.57	0.14 - 1.2	7
Dieldrin	R	0.3	0.3 - 0.48	13
Heptachlor	I	0.42	0.23 - 0.7	7
Heptachlor Epoxide	I	0.64	0.43 - 1.5	10
alpha- Endosulfan	I	1.6	0.3 - 6.2	3
Endosulfan Sulfate	I	1.6	0.5 - 8.2	3
alpha- Chlordane	I	0.12	0.1 - 0.34	5
gamma- Chlordane	I	0.27	0.06 - 0.48	6
Aroclor 1254	I	19	14 - 40	10
Aroclor 1260	I	10	6.8 - 25	11
Hydrocarbons
Total Aliphatics	I	120000	81000 - 160000	4
n - C 17	R	74	56 - 140	8
Pristane	R	69	50 - 130	10
n - C 18	I	90	60 - 110	7
Phytane	R	78	63 - 130	9
SUM n Alkanes (C 14 - C 34)	R	8100	4300 -12000	8
Phenanthrene	R	35	21 - 43	15
2 Methyl Phenanthrene	I	12	12 - 14	4
1 Methyl Phenanthrene	I	10	9.2 - 11	6
Anthracene	R	9.8	8.0 - 13	9
Chrysene	R	35	25 - 56	16
Fluorene	I	6.7	4.6 - 24	7
Fluoranthene	R	84	53 - 110	18
Pyrene	R	77	57 - 93	17
Benzo (b) Fluoranthene	R	46	32 - 69	8
Benzo (k) Fluoranthene	R	46	26 - 61	8
Benz (a) Anthracene	R	53	35 - 60	13
Benzo (e) Pyrene	R	55	51 - 81	8
Benzo (a) Pyrene	R	48	30 - 63	14
Naphthalene	R	27	16 - 47	13
Benzo (ghi) Perylene	R	38	20 - 52	12
Indeno (123cd) Pyrene	I	51	45 - 53	5
UVF equival. Chrysene	I	6000	4600 - 19000	6
UVF equival. ROPME oil	I	49000	35000 - 120000	4
Resolved Aliphatics	R	11000	6400 - 17000	7
Unresolved Aliphatics	I	110000	68000 - 150000	4
Total Aromatics	I	3700	1300 -11000	4
Resolved Aromatics	I	1900	240- 6800	4
Perylene	R	320	140 - 420	7
1 Methyl Naphthalene	I	7.5	4.7 - 12	4
2 Methyl Naphthalene	I	14	13 - 33	3
Dibenz (ah) Anthracene	I	11	7.8 - 14	3
Acenaphthene	I	3.3	2.0 - 17	4
Acenaphthylene	I	3.6	2.1 - 4.7	4
PCBs
PCB No 8	I	0.24	0.22 - 4.6	3
PCB No 18	I	0.74	0.13 - 1.9	6
PCB No 28	R	0.79	0.35 - 0.98	14
PCB No 31	I	0.43	0.09 - 1.5	3
PCB No 44	I	0.47	0.23 - 3.0	9
PCB No 49	I	0.35	0.22 - 0.38	4
PCB No 52	R	0.6	0.38 - 0.93	18
PCB No 87	I	0.87	0.26 - 1.1	3
PCB No 101	R	1.2	0.81 - 1.7	23
PCB No 105	R	0.57	0.44 - 0.67	9
PCB No 110	R	0.83	0.5 - 0.9	6
PCB No 118	R	1.2	0.9 - 1.6	21
PCB No 128	R	0.33	0.27 - 0.53	10
PCB No 138	R	1.6	1.1 - 2.1	22
PCB No 149	R	1.4	1.3 - 1.6	7
PCB No 153	R	1.9	0.98 - 2.1	20
PCB No 156	I	0.36	0.31 - 0.39	4
PCB No 170	R	0.47	0.34 - 0.59	8
PCB No 174	I	0.34	0.2 - 0.44	4
PCB No 177	I	0.35	0.23 - 0.43	4
PCB No 180	R	1.1	0.85 - 1.2	20
PCB No 183	I	0.32	0.26 - 0.33	3
PCB No 187	R	0.68	0.49 - 0.94	7
PCB No 194	R	0.2	0.2 - 0.23	5
PCB No 195	I	0.12	0.06 - 0.16	4
PCB No 196	I	0.22	0.17 - 0.4	3
Sterols
Coprostanol	I	1900	1700^§	3
Cholesterol	I	910	670^§	3
Cholestanol	I	1100	760^§	3
beta- Sistosterol	I	1100	640^§	3
Campesterol	I	2200	2200^§	2

*	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)
^§	Standard deviation