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REFERENCE MATERIAL
IAEA-417
ORGANOCHLORINE COMPOUNDS AND PETROLEUM HYDROCARBONS
IN
SEDIMENT

Intended Use
This sample is intended to be used as a reference material for the determination of chlorinated compounds and petroleum hydrocarbons 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 Venice Lagoon, Italy. This sediment was deep-frozen, dried, ground and sieved through a 250 µm stainless steel sieve.
    The sediment fraction of particle size less than 250 µm was homogenized by mixing it 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:

May 2004
Unit Price:
90 €
Unit Size:
40 g

Producer:
Marine Environment Laboratory (MEL)
International Atomic Energy Agency
4 Quai Antoine 1er
MC-98000 Monaco Supplier:
Analytical Quality Control Services
Agency's Laboratories, Seibersdorf
A-2444 Seibersdorf, Austria

Reference Sheet: IAEA-417(.pdf)

Analyte Status Concentration
[ng/g] (Based on dry weight) Standard deviation
[ng/g]
N *

Chlorinated pesticides

alpha- HCH I 0.28 0.19 5

beta- HCH I 2.8 2.3 4

gamma- HCH (Lindane) R 0.54 0.35 24

HCB I 1.2 0.8 30

pp’ DDE R 14 6.9 55

pp’ DDD R 21 11 57

pp’ DDT I 19 12 57

op DDD I 11 5.0 5

op DDT I 2.5 2.6 4

Aldrin I 1.6 1.1 14

Endrin I 7.1 6.4 22

Dieldrin I 2.3 2.5 23

Heptachlor I 2.0 2.0 20

Heptachlor Epoxide I 4.8 4.3 11

alpha- Endosulfan I 14 19 15

beta- Endosulfan I 5.1 3.7 9

Endosulfan Sulfate I 8.4 7.6 6

alpha- Chlordane I 1.8 1.7 11

gamma- Chlordane I 1.2 0.72 9

Cis Nonachlor I 1.7 1.3 3

Trans Nonachlor R 0.32 0.19 5

Aroclor 1254 I 410 270 28

Aroclor 1260 I 170 140 22

Hydrocarbons

Total Aliphatics I 230000 1910000 13

Resolved Aliphatics I 14000 5200 9

Unresolved Aliphatics
I 230000 150000 10

n - C 17 R 200 140 14

Pristane I 420 630 14

n - C 18 I 230 200 14

Phytane I 370 330 15

SUM n Alkanes (C 14 - C 34) I 9500 6800 15

Phenanthrene R 3900 1500 43

1 Methyl Phenanthrene R 320 150 12

2 Methyl Phenanthrene I 580 230 6

Acenaphthylene
R 42 35 5

Acenaphthene
R 180 62 8

Anthracene R 630 240 20

Dibenz (ah) Anthracene
I 1100 1100 16

Biphenyl
I 42 4.0 3

Chrysene R 3600 1700 42

Dibenzothiophene
R 280 16 4

Fluoranthene R 7700 3000 47

Fluorene
R 230 110 11

Pyrene R 6000 2200 43

Benzo (b) Fluoranthene R 4100 2000 17

Benzo (k) Fluoranthene R 2000 300 12

Benz (a) Anthracene R 3200 1200 40

Benzo (a) Pyrene R 2800 1200 44

Benzo (e) Pyrene
R 3000 830 18

Benzo (ghi) Perylene
R 2300 1300 43

Indeno (123cd) Pyrene
R 2700 370 14

Naphthalene I 150 110 22

Perylene R 1200 460 4

UVF equival. Chrysene
I 110000 110000 5

UVF equival. ROPME oil I 820000 840000 5

Total Aromatics I 130000 87000 4

Resolved Aromatics I 48000 25000 12

Unresolved Aromatics
I 220000 230000 4

1 Methyl Naphthalene I 53 21 4

2 Methyl Naphthalene I 81 44 4

PCBs

PCB No 8
I 1.8 1.2 5

PCB No 18 I 3.7 2.4 10

PCB No 22
I 1.0 0.36 3

PCB No 28 R 5.7 2.8 31

PCB No 31 R 4.1 1.5 12

PCB No 40
I 0.98 0.57 3

PCB No 44 R 9.7 4.6 16

PCB No 45
I 0.46 0.056 3

PCB No 49 R 7.8 2.9 8

PCB No 52 R 17 7.9 41

PCB No 66 I 23 16 8

PCB No 70 I 20 9.9 7

PCB No 74
R 5.1 2.1 5

PCB No 87
R 19 6.0 9

PCB No 91
I 3.6 1.3 3

PCB No 95
I 20 1.5 4

PCB No 97 I 9.1 1.3 3

PCB No 99 R 19 7.8 7

PCB No 101 R 42 15 39

PCB No 105 R 22 4.5 19

PCB No 110 R 42 15 13

PCB No 114
I 25 40 3

PCB No 118 I 43 18 42

PCB No 128 R 12 4.2 14

PCB No 138 R 45 22 46

PCB No 141 I 5.2 2.1 3

PCB No 149 R 25 11 13

PCB No 151 I 3.9 0.18 3

PCB No 153 I 39 20 49

PCB No 156 R 5.9 1.2 12

PCB No 158
I 6.0 2.8 4

PCB No 170 R 8.1 4.3 17

PCB No 174 R 3.1 0.97 5

PCB No 177 R 1.8 0.61 5

PCB No 180 I 16 7.4 47

PCB No 183 R 3.4 1.4 10

PCB No 185
I 1.6 0.98 3

PCB No 187 R 8.1 3.3 10

PCB No 189 I 0.41 0.23 3

PCB No 194 R 2.7 1.3 12

PCB No 195 R 1.2 0.53 6

PCB No 199
I 1.2 0.79 5

PCB No 200
I 7.8 11 3

PCB No 201
I 3.8 2.8 3

PCB No 206
R 1.8 0.96 7

PCB No 209
R 1.2 0.7 6

*
Number of accepted laboratory results which were used to calculate the recommended or information values and their respective confidence intervals about the mean 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 in 2001. The details concerning the criteria for qualification as a recommended or information value can be found in the report (IAEA/AL/131; IAEA/MEL/71), "World-wide and Regional Intercomparison for Determination of Organochlorine Compounds and Petroleum Hydrocarbons in Sediment Sample IAEA-417" [1]. This report is available free of charge upon request.

Homogeneity
    The homogeneity of the material for organochlorine compounds and petroleum hydrocarbons was checked by determining the concentration of some compounds (chlorinated pesticides and petroleum hydrocarbons) in 10 replicate sub-samples taken at random from the bulk material. A one-way analysis of variance 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 1.6 %. Since the moisture content can change with the ambient humidity and temperature, it is recommended that the water content of this material always be determined in a separate sub-sample (not that taken for analysis) by drying it 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 2 g for petroleum hydrocarbons and 5 g for organochlorine pesticides and PCBs. Analyst 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. and Cattini C., World-wide and Regional Intercomparison for Determination of Organochlorine Compounds and Petroleum Hydrocarbons in Sediment Sample IAEA-417; IAEA/AL/131 (IAEA/MEL/71), IAEA, Monaco, 2002.

Last updated 7 May 2004

*Date of Release:* May 2004	*Unit Price:* 90 €	*Unit Size:* 40 g
*Producer:* Marine Environment Laboratory (MEL) International Atomic Energy Agency 4 Quai Antoine 1er MC-98000 Monaco	*Supplier:* Analytical Quality Control Services Agency's Laboratories, Seibersdorf A-2444 Seibersdorf, Austria
Reference Sheet: IAEA-417(.pdf)

Analyte	Status	Concentration [ng/g] *(Based on dry weight)*	Standard deviation [ng/g]	N *
Chlorinated pesticides
alpha- HCH	I	0.28	0.19	5
beta- HCH	I	2.8	2.3	4
gamma- HCH (Lindane)	R	0.54	0.35	24
HCB	I	1.2	0.8	30
pp’ DDE	R	14	6.9	55
pp’ DDD	R	21	11	57
pp’ DDT	I	19	12	57
op DDD	I	11	5.0	5
op DDT	I	2.5	2.6	4
Aldrin	I	1.6	1.1	14
Endrin	I	7.1	6.4	22
Dieldrin	I	2.3	2.5	23
Heptachlor	I	2.0	2.0	20
Heptachlor Epoxide	I	4.8	4.3	11
alpha- Endosulfan	I	14	19	15
beta- Endosulfan	I	5.1	3.7	9
Endosulfan Sulfate	I	8.4	7.6	6
alpha- Chlordane	I	1.8	1.7	11
gamma- Chlordane	I	1.2	0.72	9
Cis Nonachlor	I	1.7	1.3	3
Trans Nonachlor	R	0.32	0.19	5
Aroclor 1254	I	410	270	28
Aroclor 1260	I	170	140	22
Hydrocarbons
Total Aliphatics	I	230000	1910000	13
Resolved Aliphatics	I	14000	5200	9
Unresolved Aliphatics	I	230000	150000	10
n - C 17	R	200	140	14
Pristane	I	420	630	14
n - C 18	I	230	200	14
Phytane	I	370	330	15
SUM n Alkanes (C 14 - C 34)	I	9500	6800	15
Phenanthrene	R	3900	1500	43
1 Methyl Phenanthrene	R	320	150	12
2 Methyl Phenanthrene	I	580	230	6
Acenaphthylene	R	42	35	5
Acenaphthene	R	180	62	8
Anthracene	R	630	240	20
Dibenz (ah) Anthracene	I	1100	1100	16
Biphenyl	I	42	4.0	3
Chrysene	R	3600	1700	42
Dibenzothiophene	R	280	16	4
Fluoranthene	R	7700	3000	47
Fluorene	R	230	110	11
Pyrene	R	6000	2200	43
Benzo (b) Fluoranthene	R	4100	2000	17
Benzo (k) Fluoranthene	R	2000	300	12
Benz (a) Anthracene	R	3200	1200	40
Benzo (a) Pyrene	R	2800	1200	44
Benzo (e) Pyrene	R	3000	830	18
Benzo (ghi) Perylene	R	2300	1300	43
Indeno (123cd) Pyrene	R	2700	370	14
Naphthalene	I	150	110	22
Perylene	R	1200	460	4
UVF equival. Chrysene	I	110000	110000	5
UVF equival. ROPME oil	I	820000	840000	5
Total Aromatics	I	130000	87000	4
Resolved Aromatics	I	48000	25000	12
Unresolved Aromatics	I	220000	230000	4
1 Methyl Naphthalene	I	53	21	4
2 Methyl Naphthalene	I	81	44	4
PCBs
PCB No 8	I	1.8	1.2	5
PCB No 18	I	3.7	2.4	10
PCB No 22	I	1.0	0.36	3
PCB No 28	R	5.7	2.8	31
PCB No 31	R	4.1	1.5	12
PCB No 40	I	0.98	0.57	3
PCB No 44	R	9.7	4.6	16
PCB No 45	I	0.46	0.056	3
PCB No 49	R	7.8	2.9	8
PCB No 52	R	17	7.9	41
PCB No 66	I	23	16	8
PCB No 70	I	20	9.9	7
PCB No 74	R	5.1	2.1	5
PCB No 87	R	19	6.0	9
PCB No 91	I	3.6	1.3	3
PCB No 95	I	20	1.5	4
PCB No 97	I	9.1	1.3	3
PCB No 99	R	19	7.8	7
PCB No 101	R	42	15	39
PCB No 105	R	22	4.5	19
PCB No 110	R	42	15	13
PCB No 114	I	25	40	3
PCB No 118	I	43	18	42
PCB No 128	R	12	4.2	14
PCB No 138	R	45	22	46
PCB No 141	I	5.2	2.1	3
PCB No 149	R	25	11	13
PCB No 151	I	3.9	0.18	3
PCB No 153	I	39	20	49
PCB No 156	R	5.9	1.2	12
PCB No 158	I	6.0	2.8	4
PCB No 170	R	8.1	4.3	17
PCB No 174	R	3.1	0.97	5
PCB No 177	R	1.8	0.61	5
PCB No 180	I	16	7.4	47
PCB No 183	R	3.4	1.4	10
PCB No 185	I	1.6	0.98	3
PCB No 187	R	8.1	3.3	10
PCB No 189	I	0.41	0.23	3
PCB No 194	R	2.7	1.3	12
PCB No 195	R	1.2	0.53	6
PCB No 199	I	1.2	0.79	5
PCB No 200	I	7.8	11	3
PCB No 201	I	3.8	2.8	3
PCB No 206	R	1.8	0.96	7
PCB No 209	R	1.2	0.7	6

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