INTERNATIONAL ISO

STANDARD 15009

Third edition
2016-02-15

Soil quality — Gas chromatographic

determination of the content of
volatile aromatic hydrocarbons,
naphthalene and volatile halogenated
hydrocarbons — Purge-and-trap
method with thermal desorption
Qualité du sol — Détermination par chromatographie en phase
gazeuse des teneurs en hydrocarbures aromatiques volatils, en
naphtalène et en hydrocarbures halogénés volatils — Méthode par
purge et piégeage avec désorption thermique

Reference number
ISO 15009:2016(E)

© ISO 2016
ISO 15009:2016(E)

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ii © ISO 2016 – All rights reserved

 ISO 15009:2016(E)

Contents Page
Foreword ........................................................................................................................................................................................................................................ iv
1 Scope ................................................................................................................................................................................................................................. 1
2 Normative references ...................................................................................................................................................................................... 1
3 Principle ........................................................................................................................................................................................................................ 2
4 Reagents ........................................................................................................................................................................................................................ 2
4. 1 f f
Water, ree o vo latile aro matic and vo latile halo genated hydro carb o ns ............................................. 2
4.2 Internal standards ................................................................................................................................................................................ 2
4.3 Standard compounds ......................................................................................................................................................................... 3
4. 3 . 1 Vo latile aro matic hydro carb o ns .......................................................................................................................... 3
4. 3 . 2 Vo latile halo genated hydro carb o ns ................................................................................................................. 3
4.4 Methanol....................................................................................................................................................................................................... 4
4.5 Adsorbing agent ..................................................................................................................................................................................... 4
4.6 Cooling water for purge and trap ............................................................................................................................................ 4
4.7 Inert gas for the gas chromatograph .................................................................................................................................... 5
4.8 Nitrogen or helium as inert gas for the purge equipment................................................................................. 5
4.9 Standard solutions ............................................................................................................................................................................... 5
4.9.1 Standard stock solutions for volatile aromatic and halogenated
compounds in methanol, 4 g/l ............................................................................................................................. 5
4.9.2 Internal standard solutions in methanol, 4 g/l ...................................................................................... 5
4.9.3 Calibration solutions .................................................................................................................................................... 5
4.10 Methanol containing internal standards .......................................................................................................................... 6
5 Apparatus ..................................................................................................................................................................................................................... 6
6 Sampling, preservation and sample pretreatment .......................................................................................................... 7
6.1 General ........................................................................................................................................................................................................... 7
6.2 S amp ling us ing vials p re- filled with methano l ............................................................................................................ 8
6.3 Sampling using coring tube method ..................................................................................................................................... 8
7 Procedure ..................................................................................................................................................................................................................... 8
7.1 Blank determination .......................................................................................................................................................................... 8
7.2 Extraction .................................................................................................................................................................................................... 9
7.3 Purge and trap ......................................................................................................................................................................................... 9
7.4 Gas chro mato grap hic analys is ................................................................................................................................................... 9
7.4.1 Gas chromatographic conditions ....................................................................................................................... 9
7.4.2 Calibration .......................................................................................................................................................................... 10
7.4.3 Measurement ................................................................................................................................................................... 11
8 Calculation ............................................................................................................................................................................................................... 12
8.1 Calculation of the concentration of a volatile compound in the water sample ............................ 12
8.2 Calculation of the concentration of a volatile compound in the soil sample .................................. 12
9 Expression of results ..................................................................................................................................................................................... 13
10 Precision .................................................................................................................................................................................................................... 13
11 Test report................................................................................................................................................................................................................ 13
Annex A (informative)
Relative retention time with respect to ethylbenzene-D10 of volatile
aromatic hydrocarbons and volatile halogenated hydrocarbons on following
columns: CP-Sil 5 CB and CP-Sil 13 CB .......................................................................................................................................... 14
Annex B (normative) Check on internal standards ............................................................................................................................ 16
Annex C (informative) Validation .......................................................................................................................................................................... 17
Annex D (informative) Information on purge and trap instruments ............................................................................... 20

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ISO 15009:2016(E)

Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work o f preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters o f
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
di fferent types o f ISO documents should be noted. This document was dra fted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see [Link]/directives).
Attention is drawn to the possibility that some o f the elements o f this document may be the subject o f
patent rights. ISO shall not be held responsible for identi fying any or all such patent rights. Details o f
any patent rights identified during the development o f the document will be in the Introduction and/or
on the ISO list of patent declarations received (see [Link]/patents).
Any trade name used in this document is in formation given for the convenience o f users and does not
constitute an endorsement.
For an explanation on the meaning o f ISO specific terms and expressions related to con formity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical
Barriers to Trade (TBT) see the following URL: Foreword - Supplementary in formation
The committee responsible for this document is ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical
methods and soil characteristics.
This third edition cancels and replaces the second edition (ISO 15009:2012), which has been technically
revised.

iv © ISO 2016 – All rights reserved

INTERNATIONAL STANDARD ISO 15009:2016(E)

Soil quality — Gas chromatographic determination of the

content of volatile aromatic hydrocarbons, naphthalene
and volatile halogenated hydrocarbons — Purge-and-trap
method with thermal desorption

1 Scope
T h i s I nternationa l Sta nda rd s p e c i fie s a me tho d for quantitative ga s- ch romato graph ic de term i nation o f

volati le aromatic hyd ro c arb on s , naphtha lene and volati le ha lo genate d hyd ro c arb on s i n s oi l .

T h i s I nternationa l Standard i s appl ic able to a l l typ e s o f s oi l .

NO TE I n the c a s e o f u n s atu rate d p e aty s o i l s , ab s o r p tion o f the e x trac tion s o lutio n m ay o cc u r.

T he lower l i m it o f quanti fic ation i s dep endent on the e qu ipment u s e d a nd the qua l ity o f the me tha nol

grade used for the extraction of the soil sample.

Under the cond ition s s p e c i fie d i n th i s I nternationa l Standard the fol lowi ng l i m its o f quanti fic ation

app ly (e xpre s s e d on b a s i s o f d r y matter) :

Typic a l l i m it o f quanti fic ation when u s i ng G C-F I D :

— Volati le aromatic hyd ro c arb on s: 0 ,1 mg/ kg

Typic a l l i m it o f quanti fic ation when u s i ng G C-E C D :

— Volati le ha lo genate d hyd ro ca rb on s: 0 , 01 mg/ kg

L ower l i m its o f quanti fic ation for s ome comp ou nd s c an b e ach ieve d b y u s i ng ma s s s p e c trome tr y (M S )

with selected ion detection.

2 Normative references
T he fol lowi ng do c u ments , i n whole or i n p ar t, are normatively re ference d i n th i s do c u ment a nd are

i nd i s p en s able for its appl ic ation . For date d re ference s , on ly the e d ition cite d appl ie s . For u ndate d

re ference s , the late s t e d ition o f the re ference d do c u ment (i nclud i ng any amend ments) appl ie s .

ISO 4799, Laboratory glassware — Condensers

ISO 10381-1, Soil quality — Sampling — Part 1: Guidance on the design of sampling programmes
ISO 10381-2, Soil quality — Sampling — Part 2: Guidance on sampling techniques
ISO 10381-5, Soil quality — Sampling — Part 5: Guidance on the procedure for the investigation of urban
and industrial sites with regard to soil contamination
ISO 11465, Soil quality — Determination of dry matter and water content on a mass basis —
Gravimetric method
ISO 15680, Water quality — Gas-chromatographic determination of a number of monocyclic aromatic
hydrocarbons, naphthalene and several chlorinated compounds using purge-and-trap and thermal
desorption
ISO 18512, Soil quality — Guidance on long and short term storage of soil samples

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ISO 15009:2016(E)

ISO 22892, Soil quality — Guidelines for the identification oftarget compounds by gas chromatography and
mass spectrometry

3 Principle
Test samples are taken from an untreated field moist soil sample. To prevent losses o f the volatiles,
samples are taken as undisturbed as possible in the field with a tube corer or by adding methanol
immediately in the field.
The test sample is extracted with methanol. A fter centri fugation, i f necessary, part o f the methanol
extract is brought into a purge vessel filled with water. The volatile compounds are purged with
nitrogen or helium and adsorbed on a suitable adsorbing agent. The adsorbed compounds are
desorbed thermally and by means o f a carrier gas flow, whether or not via a cold trap, brought into
a gas chromatograph. The various compounds are separated by using a capillary column with an
immobile phase o f low polarity. Volatile organic compounds are detected with appropriate detectors
such as: mass spectrometric detector (MS), flame ionization detector (FID), electron capture detector
(ECD), photo ionization detector (PID) or electrolytic conductivity detector (ELCD). Identification and
quantification takes place by comparison o f retention times and peak heights (or peak areas) towards
internal standard added with the corresponding variables of an external standard solution. The
e fficiency o f the procedure depends on the composition o f the soil that is investigated. The described
procedure does not take into account incomplete extraction caused by structure and composition o f the
soil sample.
When using non-specific detectors such as FID and ECD, the confirmation o f the identity o f the detected
compounds and their concentrations should be done by repeating the gas chromatographic analysis
using a column o f di fferent polarity. When using gas chromatography-mass spectrometry (GC-MS), the
identity confirmation and the quantification can be done in a single run.
NOTE This International Standard follows the description of an ‘off-line purge and trap’ method. The use
o f commercially available online instruments is allowed provided that equivalent results are obtained during
validation o f this equipment. With such an instrument purge and trap occurs on line with gas chromatography
and detection. Follow the manual o f the manu facturer especially regarding the items 5.2.1 to 5.2.9.

4 Reagents
All reagents shall be o f recognized analytical grade. Veri fy whether the reagents are applicable for this
specific purpose and free o f inter fering compounds.

4.1 Water, free of volatile aromatic and volatile halogenated hydrocarbons

Usually boiler water with a temperature o f at least 80 °C and 1 day old can be applied. Purging with
an inert gas, e.g. a flow o f 10 ml/min o f nitrogen for 30 min, is another means o f removing inter fering
compounds from water. A su fficient amount o f water from the same batch should be available to
complete each batch o f analyses, including all preparations.

4.2 Internal standards

4.2.1 For the determination o f volatile aromatic hydrocarbons pre ferably two internal standards shall
be selected from Table 1 . They shall not interfere with compounds present in the sample extract.

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 ISO 15009:2016(E)

Table 1 — Examples of suitable internal standards for the determination of volatile aromatic
hydrocarbons

Compound name CAS-RN a EC-N b

Toluene-D8 2037–26–5 218–009–5
Ethylbenzene-D10 25837–05–2 247–292–8
2-Bromofluorobenzene 1072–85–1 214–018–3
a Chemical Abstracts Service Registry Number
b EC-Number
4.2.2 For the determination o f volatile halogenated hydrocarbons pre ferably two internal standards
shall be selected from Table 2 . They shall not interfere with compounds present in the sample extract.
Table 2 — Examples of suitable internal standards for the determination of volatile
halogenated hydrocarbons

Compound name CAS-RN a EC-N b

1,4-Dichlorobutane 110–56–5 203–778–1
α,α,α-Trifluorotoluene 98–08–8 202–635–0
2-Bromofluorobenzene 1072–85–1 214–018–3
a Chemical Abstracts Service Registry Number
b EC-Number

4.3 Standard compounds

4.3.1 Volatile aromatic hydrocarbons

Table 3 contains volatile aromatic hydrocarbons for use as standard compounds.

Table 3 — Examples of volatile aromatic hydrocarbons suitable as standard compounds

Compound name CAS-RN a EC-N b

Benzene 71–43–2 202–753–7
Toluene 108–88–3 203–625–9
Ethylbenzene 100–41–4 202–849–4
o -Xylene 95–47–6 202–422–2
m -Xylene 108–38–3 203–576–3
p -Xylene 106–42–3 203–396–5
Styrene 100–42–5 202–851–5
Naphthalene 91–20–3 202–049–5
a Chemical Abstracts Service Registry Number
b EC-Number
4.3.2 Volatile halogenated hydrocarbons

Table 4 contains volatile halogenated hydrocarbons for use as standard compounds.

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ISO 15009:2016(E)

Table 4 — Examples of volatile halogenated hydrocarbons suitable as standard compounds

Compound name CAS-RN a EC-N b

Dichloromethane 75–09–2 200–838–9
Trichloromethane 67–66–3 200–663–8
Tetrachloromethane 56–23–5 200–262–8
1,1-Dichloroethane 75–34–3 200–863–5
1,2-Dichloroethane 107–06–2 203–458–1
1,1,1-Trichloroethane 71–55–6 200–756–3
1,1,2-Trichloroethane 79–00–5 201–166–9
1,2-Dichloropropane 78–87–5 201–152–2
1,2,3-Trichloropropane 98–18–4 202–486–1
cis-1,3-Dichloropropene 10061–01–5 233–195–8
trans-1,3-Dichloropropene 10061–02–6 208–826–5
cis-1,2-Dichloroethene 156–59–2 205–859–7
trans-1,2-Dichloroethene 156–60–5 205–860–2
3-Chloropropene 107–05–1 203–457–6
Trichloroethene 79–01–6 201–61–04
Tetrachloroethene 127–18–4 204–825–9
Monochlorobenzene 108–90–7 203–628–5
1,2-Dichlorobenzene 95–50–1 202–425–9
a Chemical Abstracts Service Registry Number
b EC-Number

4.4 Methanol
Methanol (see Table 5) is used as solvent for the extraction of soil samples and for the preparation of
standard solutions.
Table 5 — Registration data

Compound name CAS-RN a EC-N b

Methanol 67–56–1 200–659–6
a Chemical Abstracts Service Registry Number
b EC-Number

4.5 Adsorbing agent

Polymer o f 2,6-diphenyl-p-phenoxide (40 mesh to 60 mesh) o f a grade suitable for thermal desorption.
NOTE 1 2,6-diphenyl-p-phenylene oxide (CAS-RN 24938–68–9) is commercially available as Tenax TA1) .
NOTE 2 Other adsorbing agents may be used provided that their suitability has been tested.

4.6 Cooling water for purge and trap

The temperature of the cooling water depends on the dimensions of the purge and trap equipment (5.2).
A temperature o f about 10 °C is recommended. A cryostat shall be used i f the temperature o f the cooling
water is too high.

1) Tenax TA is an example o f a suitable product available commercially. This information is given for the
convenience o f users o f this International Standard and does not constitute an endorsement by ISO o f this product.
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 ISO 15009:2016(E)

4.7 Inert gas for the gas chromatograph

H el iu m, n itro gen or argon-me tha ne m i x ture u ltra-pu re . O ther ga s e s for gas ch romato graphy sh a l l b e

used in accordance with the instrument manufacturer’s instructions.

4.8 Nitrogen or helium as inert gas for the purge equipment

4.9 Standard solutions

4.9.1 Standard stock solutions for volatile aromatic and halogenated compounds in
methanol, 4 g/l

Weigh about 100 mg of the individual standard compounds (4.3 ) with an acc u rac y o f 0 ,1 mg i nto a

clo s e d s ep tu m fla s k conta i n i ng 2 5 m l me tha nol . Tra n s fer the s ta ndard comp ound s i nto the fla sk b y

u s i ng a s yri nge .

NO TE T he s to ck s olution i s s tab le for ab out 6 mo nth s when s tore d at −1 8 ° C .

4.9.2 Internal standard solutions in methanol, 4 g/l

T he conta i ners contai n i ng the s olution s s ha l l b e ma rke d or weighe d s o that any evap oration lo s s e s o f

the s olvent may b e re co gn i z e d . T he s olution s s ha l l b e s tore d at a temp erature o f (4 ± 2 ) ° C i n the dark.

P rior to u s e, they s ha l l b e brought to a mbient temp erature .

Weigh about 100 mg of the individual internal standards (4.2.1 and 4.2.2) accurate to 0,1 mg into a
clo s e d s ep tu m fla s k contai n i ng 2 5 m l o f me thanol . Us i ng a s yri nge, tra n s fer the s tand ard comp ou nd s

i nto the fla sk.

4.9.3 Calibration solutions

Calibration solutions containing 0 mg/l to 200 mg/l of each standard (4.3) and the selected internal
standards (4.2), 200 mg/l. The calibration solutions are prepared in methanol.
Dilute the amounts indicated in Table 6 of the solutions obtained according to 4.9.2 and 4.9.1 with
methanol (4.4) to 100 ml.
O ther volu me s o f me tha nol may b e u s e d, a s long a s s uitabi l ity i s proven .

Table 6 — Example for preparation of calibration solutions

Calibration Internal standard Standard stock Concentration in the Quantity in µg/5 µl

solution solution (4.9.2) solution (4.9.1) calibration solution calibration solution in
ml ml mg/l 100 ml (sample) water
1 5 0 0 0
2 5 1 40 0,2
3 5 2 80 0,4
4 5 3 120 0,6
5 5 4 160 0,8
6 5 5 200 1,0
The total volume of the methanol used for calibration shall be the same as that which will be taken for
the methanol extract of the soil sample (see 7.3).

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ISO 15009:2016(E)

4.10 Methanol containing internal standards

Prepare methanol containing a suitable concentration of the internal standards (e.g. 0,4 µg/ml). The
concentration shall be such that the end concentration in the water extract in the purge vessel is of the
same level as in the calibration solutions.
5 Apparatus

5.1 General

Usual laboratory glassware, free o f inter fering compounds.

All glassware shall be cleaned according to the usual procedures for this type o f analysis.
5.2 Purge and trap apparatus

The instrument described here is for an off-line purge and trap method. As mentioned in NOTE in
Clause 3 it is allowed to use commercially available automated systems provided that requirements
of this International Standard are met. Annex D gives some considerations for the use of such systems.
5.2.1 Round bottom flask with three angled side necks; volume 100 ml.

5.2.2 Gas inlet tube with a tip of sintered glass.

5.2.3 Ball and cup stopcock with polytetrafluoroethylene (PTFE) ring.

5.2.4 Flow adjustment with a nitrogen flow set to (40 ± 2) ml/min.

5.2.5 Inlet tube for the thermocouple.

5.2.6 Allihn or Graham type condenser (see ISO 4799).

5.2.7 Screw cap with cut-o ff ring made o f silicone rubber with PTFE inlay.

5.2.8 Adsorption tubes made o f glass or stainless steel, filled with at least 240 mg o f adsorbing
agent (4.5).
The adsorbent is kept in place by using inert material, e.g. silanized glass fibre. The tubes shall be
suitable for direct use in connection with the apparatus for thermal desorption. The tubes shall be
marked on one side. The tubes shall be provided with caps o f inert material, e.g. polyethylene or metal,
with screw caps and PTFE ring, allow tight closing after purging.
Be fore use, the adsorbent shall be activated and purified by slowly heating the tubes to 250 °C and
keeping them at that temperature for 3 h while a nitrogen flow o f 10 ml/min is maintained. The
adsorbent shall be cooled under nitrogen and the tubes analysed. The result o f a blank determination
shall not exceed the equivalent o f 1 ng o f a compound to be analysed. When the result is higher than
this, the adsorbent shall be desorbed once more.
The use o f commercially available tubes is recommended.
Tubes that are used should not be used again unless the blank determination meets the above mentioned
requirements.
Care should be taken to avoid cross-contamination. A heavily loaded tube can contaminate a lightly
loaded tube in the sample change platform.

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 ISO 15009:2016(E)

5.2.9 Heating block, with thermocouple, suitable for heating 100 ml flasks.

5.3 Centrifuge , suitable for centri fuging tubes o f 200 ml with such a rotation frequency that the radial
acceleration is 2 000 g to 3 000 g.
5.4 Centrifuge tubes with a volume of 200 ml.
5.5 Capillary columns

Fused silica capillary columns with a non-polar or semipolar stationary phase allowing su fficient
separation o f the compounds o f interest. A thick film o f stationary phase increases the e fficiency o f the
more volatile compounds.
Examples are given in 7.4.1 and Annex A.
5.6 Gas chromatograph , equipped with one or two appropriate detectors. Detectors like flame
ionization detector (FID), electron capture detector (ECD), photo ionization detector (PID) or electrolytic
conductivity detector (ELCD) and mass spectrometer (MS) can be used, depending on the substances to
be analysed and their target level o f contamination. The mass spectrometer should be able o f operating
over the total mass range o f interest and being equipped with a data system capable o f quanti fying ions
using selected m /z values.
5.7 Apparatus for thermal desorption .
The apparatus used shall meet the following requirements:
— a primary desorption oven with adjustable desorption temperature up to 250 °C and adjustable
desorption time;
— a cold trap/ secondary desorption oven;
— a connecting tube to the gas chromatograph, with adjustable heating up to 150 °C;
— adjustable carrier gas flow rate up to 40 ml/min.
NOTE Instruments for thermal desorption are commercially available.

5.8 Electronic integrator or automatic recorder or computer with chromatographic software.

5.9 Syringe , volume 5 µl, readable to 0,1 µl and volume 50 µl, readable to 1 µl.
5.10 Horizontal shaking machine .
A shaking machine with horizontal movement (200 to 300 movements per minute).
6 Sampling, preservation and sample pretreatment

6.1 General
Sampling shall be carried out in accordance with ISO 10381-1 and ISO 10381-5 as appropriate, using
equipment according to ISO 10381-2 a fter coordination with the analytical laboratory.
Samples shall be analysed as soon as possible on their receipt in the laboratory. I f it is necessary to store
samples, they shall be stored cool in accordance with ISO 18512. Samples are not pretreated. Exposure
of samples to air, even during sampling, shall be avoided.

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Samples for the determination of volatile compounds can be obtained using several techniques. It is
strongly recommended to use one o f the procedures described in 6.2 and 6.3.
Determine the dry matter content o f the field-moist sample in accordance with ISO 11465. In case
the sampling method in 6.2 is used, a separate sample should be delivered to the laboratory for
determination o f the dry matter.

6.2 Sampling using vials pre-filled with methanol

Trans fer a defined volume o f soil using an appropriate device into a preweighed vial which is filled
with a defined volume o f methanol already containing internal standards (4.10 ). Prevent leakages by
cleaning the top of the vessel before sealing.
The soil samples should be taken from undisturbed material using an appropriate sample cutter of
known volume, e.g. a modified 20 ml disposable plastic syringe with the tip cut o ff. The soil sample
should be collected immediately a fter exposing a fresh soil sur face o f the drilling core, e.g. o f an open
window sampler or the trial pit wall. The incorporation of material like roots or stones should be
avoided as far as possible.
Make sure that the sample is completely covered with methanol containing internal standards (4.10).
Then close the cap o f the PTFE-coated septum. At least one blank sample on every site shall be prepared
in the field by opening the prepared vial for the same time period as necessary for filling with the soil
sample. Add methanol containing internal standards (4.10) and close the cap of the vial. If blank values
are unusually high (more than 50 % o f the lowest value o f interest) the reason for these high blanks
shall be investigated.
The sampling vials should be kept dark in a cooler (before and after sampling) throughout the whole
transportation. For details see ISO 18512.
NOTE The procedure described here assumes that methanol containing internal standards is used. It is also
acceptable that the internal standards are added in the methanol in the laboratory at the start o f the extraction
procedure.
6.3 Sampling using coring tube method
This method, which consists o f taking an undisturbed sample, greatly reduces or eliminates common
losses (e.g. due to evaporation, diffusion, sorption onto plastics). This method involves a stainless steel
coring tube o f minimal volume 200 ml which is filled in situ, retrieved and capped with a non-permeable
material, e.g. stainless steel, aluminium foil. The tube should be filled totally.
This method is not suitable for very stony soils.
Store in cool conditions at a temperature o f 2 °C to 8 °C for no longer than 4 days; see ISO 18512.
In the laboratory during sub-sampling, take care that no volatile compounds are lost. Start as soon as
possible with the cooled sample. Use the whole content of the coring tube or take a sub-sample with a
suitable instrument, e.g. an apple corer, and put it directly into the vial (see 6.2).

7 Procedure

7.1 Blank determination

For each series o f samples, a blank determination shall be carried out by treating 50 ml water (4.1), to
which 5 µl to 50 µl of methanol containing internal standards (4.10) has been added, as a sample. Ensure
that no contamination occurs from the laboratory atmosphere. I f blank values are unusually high (more
than 50 % o f the lowest value o f interest) the reason for these high blanks shall be investigated.

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7.2 Extraction
Using sampling procedure 6.2 , the addition of methanol is carried out in the field; i f using sampling
procedure 6.3 , the addition of methanol is carried out in the laboratory. In both cases the extraction, i.e.
the shaking, is carried out in the laboratory.
Add a defined amount o f test sample (25 g to 50 g), collected as described during sampling (Clause 6)
with a sampling device into a pre-weighed vial (50 ml to 100 ml) (see 6.2) with a screw cap with PTFE-
coated septum and filled with a defined amount o f methanol containing internal standards (4.10) (25 ml
to 50 ml). Weigh and place the vials on the horizontal shaking machine (5.10) and shake for 30 min.
Take the tube out of the shaking machine and allow it to stand for 10 min to 15 min for the settling of
solid materials. If there is no settling of solid materials on standing, centrifuge for 10 min at a rotation
frequency that results into a radial acceleration o f 2 000 g .

NOTE The procedure described here assumes that methanol containing internal standards is used. It is also
acceptable that the internal standards are added in the methanol at the start of the extraction procedure.
7.3 Purge and trap
Transfer 50 ml water (4.1) into a purge vessel. Inject 5 µl to 50 µl o f the methanol extract, obtained
according to 7.2 , to the bottom of the purge vessel. Heat the sample to 95 °C in about 15 min and then
purge the sample for 30 min with nitrogen at a flow rate o f 40 ml/min.
Remove the adsorption tube from the cooler and close with the cap (5.2.8).
NOTE 1 Automated equipment in which the di fferent steps o f the analytical procedure are combined can
be used.
For dichloromethane, break-through on the adsorption tube (5.2.8) can occur. In that case, the purge
time should be shortened to 15 min. The total purge volume should not exceed 600 ml.
NOTE 2 Other solvent/water ratios can be used i f the validity is proven.
The procedures employed for sample desorption depend on the type o f GC inter face used. Consult the
instructions from the manu facturer o f the purge-and-trap system and the supplier o f the trap packing
material. Trap temperatures up to 220 °C may be employed. However, the higher temperatures will
shorten the use ful li fe o f the trap. Trap temperatures may vary depending on the trap material.

7.4 Gas chromatographic analysis

7.4.1 Gas chromatographic conditions

Example o f gas chromatographic conditions for this analysis:

Stationary phase: low polarity e.g. Restek2) columns: Rxi-5MS, Rtx-1701 or Rxi-624SIL MS
Film thickness: 2 µm to 5 µm
Column length: 50 m to 60 m
Internal diameter: 0,25 mm to 0,32 mm
Oven temperature: 80 °C during 2,5 min
10 °C/min up to 280 °C
280 °C during 10 min
2) Restek Rxi-5MS, Rtx-1701 or Rxi-624SIL MS are examples o f suitable products available commercially.
This information is given for the convenience of users of this International Standard and does not constitute an
endorsement by ISO o f this product.
© ISO 2016 – All rights reserved 9
ISO 15009:2016(E)

Detector temperature: 300 °C (FID)

Carrier gas: helium
Gas flow: 20 cm/s to 30 cm/s
When a column with an internal diameter of 0,53 mm or more is used, the cold trap mentioned in 7.3
can be deleted. Using a thinner film thickness has influence on the starting temperature o f the oven. A
lower temperature will be necessary.
The separation o f the peaks shall be better than 90 % (R = 2). Under the described conditions the critical
pair for separation is ethylbenzene and ethylbenzene-D10 in case o f a non-specific detector, like FID.
Use an electron capture detector (ECD) or an electrolytic conductivity detector (ELCD, hall detector)
to detect halogenated hydrocarbons. The sensitivity o f an ECD varies with the species to be analysed
and can be more sensitive than MS for tri- or tetra-halogenated compounds. A flame ionization detector
(FID) can be used as a universal detector for hydrocarbons (aliphatic, aromatic and some halogenated),
a photo ionization detector (PID) can be used for the detection of aromatic compounds.
When using non-specific detectors as FID and ECD, the confirmation o f the identity o f the detected
compounds and their concentrations should be achieved by repeating the gas chromatographic analysis
using a column o f di fferent polarity.
GC-MS analysis: Mass spectrometers can be used to confirm and detect all the volatile organic
compounds. Compounds are identified on the basis o f their retention times and mass spectra. For the
criteria o f GC-MS identification and mass selective detection ISO 15680 and also ISO 22892 shall be
consulted.
7.4.2 Calibration

Prepare the complete series of calibration solutions according to 4.9.3 . Analyse the solutions
according to 7.3.
As a minimum, per form a five point calibration for each compound by using one or more internal
standards. Based on this, calculate the calibration function for each individual compound.
In this International Standard a linear calibration model is specified. Other calibration models (e.g. a
quadratic calibration function) may be used i f proven to be suitable.
The calibration function is only valid under specific operational conditions and should be re-established
i f these conditions are changed. The calibration function does not need to be renewed for every batch o f
samples. For routine analysis, it is su fficient to check the calibration function by a two-point calibration.
The linear range of each calibration graph is determined as follows.
Calculate, by using linear regression o f peak height (or peak area) over concentration, a straight line
for the range of the complete series of calibration solutions. Determine the deviations between the
measured values and the straight line. When the deviations are less than 5 %, linearity shall be assumed
to exist for the complete range. When these deviations are more than 5 %, the range shall be reduced
by deletion o f the measured value o f the highest concentration and again a straight line is calculated by
linear regression and checked.
Chose for the working standard the calibration solution with the concentration that is closest to the
middle of the linear range. When the range of the samples is lower than the linear range found, a working
standard with a lower concentration may be chosen, corresponding to the middle o f the sample range.
Record the gas chromatogram of the working standard after desorption of the adsorbed compounds
(7.4.3). Determine on the basis of this chromatogram the relative retention times of all volatile aromatic
and halogenated hydrocarbons with respect to the internal standard(s).

10 © ISO 2016 – All rights reserved

 ISO 15009:2016(E)

The relative retention time RRTi of compound with respect to the selected internal standard is
i s

defined in Formula (1):

ti
RRTi = (1)
ts
where
ti is the retention time of compound ;i

ts is the retention time of the internal standard . s

Determine the relative response for all volatile aromatic hydrocarbons with respect to the internal
standard ethylbenzene-D10 or other (see 4.2.1) and for all volatile halogenated hydrocarbons with
respect to the internal standard 1,4-dichlorobutane or other compounds (see 4.2.2).
Establish a linear calibration function for analyte using the pairs of values / and ρ /ρ of the
i yie yse

measured calibration solutions in Formula (2):

ie se

y ie / y se = m ⋅ ρ ie / ρ se + b
is is
(2)
where
yie is the (dependent variable) measured response o f the analyte i in the calibration, depending
on ρ e.g. peak area;
ie

yse is the measured response of the internal standards in the calibration, depending on ρ e.g.
s se

peak area;
ρie is the (independent variable) mass concentration of the substance in the calibration solution,
i

in micrograms per litre, µg/l;

ρ se is the mass concentration of the internal standard in the calibration solution, in micrograms
s

per litre, µg/l;

m is is the slope of the calibration curve from / as a function of the mass concentration ratio
yie yse

ρ /ρ , o ften called the response factor;

ie se

b is is the axis intercept o f the calibration curve on the ordinate;

i re fers to analyte i;
s refers to the internal standard s;
e refers to values connected to the calibration function.
7.4.3 Measurement

Analyse the spiked water samples prepared according to 7.3 in the same manner as described for the
calibration (7.4.2 ). Identi fy the peaks of the internal standards by using the absolute retention times.
Determine for all the other relevant peaks in the gas chromatograms the relative retention times with
respect to the internal standards. Assume that a compound is demonstrated to be present when the
relative retention time does not deviate more than 0,5 % from the relative retention time observed in
7.4.2 . In case of the use of a non-specific detector, confirm the presence o f a compound by repeating the
gas chromatographic analysis using a column with a di fferent polarity.
The volatile compounds shall be quantified with respect to the same selected internal standards used
for calibration, e.g. volatile aromatic hydrocarbons with respect to ethylbenzene-D10 and the volatile
halogenated hydrocarbons with respect to 1,4-dichlorobutane.

© ISO 2016 – All rights reserved 11

ISO 15009:2016(E)

8 Calculation

8.1 Calculation of the concentration of a volatile compound in the water sample

T he volati le aromatic hyd ro c a rb on s a nd volati le ha lo genate d hyd ro c arb on s are quanti fie d b y u s i ng an

internal standard added to the extract. Mistakes can be made when, on the position of the internal
f
s ta nda rd i n the ch romato gram o f the e xtrac t, an i nter eri ng comp ou nd i s pre s ent e s p e ci a l ly when a

Annex B in order to
non- s p e c i fic de te c tor l i ke a FI D or E C D i s u s e d . I n th i s c as e, u s e the pro ce du re i n

determine if interfering compounds are present.

f
C a lc u late the mas s concentration o in the spiked water sample using Formula (3) after solving
ana lyte i

Formula (2):
ρ = (( /
i
− )⋅ ρ )/
y
i
y
s
b
is s
m
is
(3)
where
ρi i s the ma s s concentration o f the a na lyte i in the spiked water sample, in micrograms per litre,
µg/l = ci W;
yi i s the me as u re d re s p on s e o f the a na lyte i i n the water s ample, e . g. p e a k a re a;

ys is the measured response of the internal standard s i n the water s a mp le, e . g. p e a k are a;

ρs is the mass concentration of the internal standard in the water sample, in micrograms per
s

l itre, µg/ l;

m is is the slope of the calibration curve from / as a function of the mass concentration ratio
yie yse

ρ /ρ , often called the response factor, as determined under calibration (7.4.2).

ie se

b is is the axis intercept of the calibration curve on the ordinate, as determined under calibration
(7.4.2).
8.2 Calculation of the concentration of a volatile compound in the soil sample
C a lc u late the content o f a s p e c i fic vol ati le comp ound i n the s oi l s ample b y u s i ng Formu la (4) :

ρi ⋅ ⋅
w
idm
= W

V
V

⋅ m
E
V
W
(4)
a dm

where
wi dm is the content of the individual volatile compound in the sample, in milligrams per kilo-
i

gra m, mg/ kg , o f d r y matter;

ρiW i s the ma s s concentration o f the ana lyte i in the spiked water sample, in micrograms per
l itre, µg/ l;

mdm i s the ma s s o f the te s t s ample o f d r y matter u s e d for ex trac tion, i n gram s , g;

VE is the total volume of the extract i.e. (volume of methanol added to the soil sample + volume
o f water pre s ent i n the field moi s t s a mple ob ta i ne d from the de term i nation o f d r y matter

content accord i ng to I S O 1 14 6 5 ) i n m i l l i l itre s , m l;

V a is the volume of the aliquot of methanol extract used for the spiking of water sample for
he ad s p ace me a s u rement i n m ic rol itre s , µl;

V W is the volume of the spiked water sample for headspace measurement in millilitres, ml.
I n the ca s e where, for one or more volati le aromatic or ha lo genate d hyd ro c arb on comp ou nd s , the

content found is higher than the upper limit of the linear range for that compound, the sample extract
shall be diluted with methanol (4.4 ) and ana lys e d aga i n .

12 © ISO 2016 – All rights reserved

 ISO 15009:2016(E)

9 Expression of results
Rep or t the re s u lts i n m i l l igra m s o f comp ou nd p er ki lo gra m o f d r y s oi l up to two s igni fic a nt figure s .

10 Precision
C ha rac teri s tic s o f the me tho d a re e s tabl i s he d in a va l id ation s tudy. T he re s u lts are pre s ente d in

Annex C.
11 Test report
The test report shall include at least the following information:
a) a re ference to th i s I nternationa l Sta nda rd (I S O 1 5 0 0 9) ;

b) identi fic ation o f the s a mple;

c) s torage ti me o f s ample s;

d) expression of results according to Clause 9 ;

e) a ny de tai l s no t s p e c i fie d i n th i s I nternationa l Sta nda rd or wh ich a re op tiona l, as wel l a s any fac tor
wh ich may h ave a ffe c te d the re s u lts .

© ISO 2016 – All rights reserved 13

ISO 15009:2016(E)

Annex A
(informative)
Relative retention time with respect to ethylbenzene-D10
of volatile aromatic hydrocarbons and volatile halogenated
hydrocarbons on following columns: CP-Sil 5 CB and CP-Sil 13 CB

Table A.1 f
shows e xample s o s u itable ta rge t a nd qua l i fier ion s and rel ative re tention ti me s with re s p e c t

f
to e thylb en zene -D10 o vol ati le aromatic hyd ro c arb on s a nd vol ati le ha lo genate d hyd ro c a rb on s on the

columns CP-Sil 5 CB and CP-Sil 13 CB 3) .

Tab le A .1 — E xa mp le o f s u itab le ta rge t a nd qu a l i fier ion s a nd rel ative re tentio n ti me s with

respect to ethylbenzene-D10 of volatile aromatic hydrocarbons and volatile halogenated

hydrocarbons on following columns: CP-Sil 5 CB and CP-Sil 13 CB

Relative retention time

Compound CP-Sil 5 CB CP-Sil 13 CB
/ /
Qu a l i fier

column column Target m z m z

Dichloromethane 0,212 0,254 129 127
trans-1,2-Dichloroethene 0,253 0,247 96 61
cis-1,2-Dichloroethene 0,312 0,342 96 61
Trichloromethane 0,331 0,360 83 85
1,2-Dichloroethane 0,385 0,404 62 64
1,1,1-Trichloroethane 0,404 0,434 97 99
Benzene 0,441 0,454 78 77
Tetrachloromethane 0,453 0,454 117 119
1,2-Dichloropropane 0,512 0,539 63 62
Trichloroethene 0,536 0,565 130 132
cis-1,3-Dichloropropene 0,625 0,692 75 110
trans-1,3-Dichloropropene 0,684 0,728 75 110
1,1,2-Trichloroethane 0,699 0,740 97 99
Toluene D-8 0,720 0,780 98 100
Toluene 0,731 0,802 91 92
Tetrachloroethene 0,868 0,849 166 164
1,3-Dichlorobutane 0,882 0,961 55 90
Monochlorobenzene 0,956 1,000 112 77
E thylb en z ene D -10 1,000 1,000 101 116
E thylb en z ene 1,014 1,018 106 91
m -Xylene/p -Xylene 1,042 1,034 106 91
S tyrene 1,091 1,113 104 103
o -Xylene 1,106 1,121 106 91
1,2,3-Trichloropropane 1,124 1,188 110 75
NO T E Temp eratu re pro gram me u s e d: 5 m i n at 4 0 ° C , 10 ° C/min to 10 0 °, 2 m i n at 10 0 ° C , 1 5 ° C/min to 2 5 0 ° C , 5 m i n at 2 5 0 ° C .

3) Res tek C P-S il 5 C B and C P-S il 1 3 C B are examp les o f s uitab le p ro ducts availab le co mmercially. This in fo rmatio n

is given f o r the co nvenience o f us ers o f this I nternatio nal S tandard and do es no t co ns titute an endo rs ement by I S O

of these products.
14 © ISO 2016 – All rights reserved
 ISO 15009:2016(E)

Table A.1 (continued)

Relative retention time
Compound CP-Sil 5 CB CP-Sil 13 CB Qualifier
column column Target m z / m /z
Cumene 1,129 1,242 105 120
1,3-Dichlorobenzene 1,380 1,396 146 148
1,4-Dichlorobenzene 1,391 1,412 146 148
1,2-Dichlorobenzene 1,437 1,461 146 148
Naphthalene 1,697 1,744 128 127
NOTE Temperature programme used: 5 min at 40 °C , 10 ° C/min to 100 °, 2 min at 100 °C , 15 ° C/min to 250 °C , 5 min at 250 °C .

© ISO 2016 – All rights reserved 15

ISO 15009:2016(E)

Annex B
(normative)
Check on internal standards

I f a non- s p e c i fic de te c tor i s u s e d the pre s ence o f i nter feri ng comp ou nd s h ave to b e che cke d .

Therefore, two internal standards are added to the extract to determine whether interfering compounds
are present or absent. The presence or absence of interfering compounds can be determined from the
measured responses of the internal standards. When no interfering compounds are present in the
extract, the ratio between the responses of the internal standards is equal to that ratio in the standard
solutions. The quotient of these ratios is called the relative response ratio, RRR. When no interfering
compounds are present in the extract, the value of RRR is in principle 1,00. In this International Standard,
it is assumed that no interfering compounds are present in the extract when RRR = 1 ,0 0 ± 0,05 .

When the value of RRR f

deviate s f
rom 1 , 0 0 ± 0 , 0 5 , a n i nter eri ng comp ou nd pre s ent i n the e xtrac t

i n fluence s the re s p on s e o f one o f the i nterna l s tandard s . I n that c a s e, the hyd ro c arb on s a re quanti fie d

by u s i ng the u nd i s tu rb e d i nterna l s ta ndard . I n prac tice, th i s c a n b e done b y qua nti fyi ng a l l e xtrac ts

with re s p e c t to the s a me i nterna l s tandard and b y c a lc u lati ng the va lue s o f RRR for a l l ex trac ts . O n ly i n
those cases when RRR > 1 , 0 5 i s the re s p on s e o f the i nterna l s tandard cho s en i n fluence d b y a n i nter feri ng

comp ou nd . I n tho s e c a s e s , the qua nti fic ation with re s p e c t to the o ther s tandard c an b e c a rrie d out b y

mu ltiplyi ng the ca lc u late d contents with the va lue o f RRR for the extract considered.
T h i s che ck on the ab s ence o f i nter feri ng comp ound s on ly con s iders the p o s s ible i nter ference on the

position of the internal standards in the chromatogram. The absence of interfering compounds on
f
the p o s ition s o the vol ati le aromatic hyd ro ca rb on s and the ha lo genate d hyd ro c arb on s i s de term i ne d

f
by con fi rmation o f
the pre s ence o 7.4.3). It is assumed that no interfering
the de te c te d comp ou nd s (

f
comp ou nd s a re pre s ent at the p o s ition s o the hyd ro c arb on s i n the ch romato gram when con fi rmation

results in the same contents found.

When the con fi rmation re s u lts i n a lower content, it i s a s s ume d th at the content found e arl ier i s

i n fluence d b y an i nter feri ng comp ound and , i n that c as e, the lower content i s rep or te d as the mo s t

probable true value.

16 © ISO 2016 – All rights reserved

 ISO 15009:2016(E)

Annex C
(informative)
Validation

Annex C gives results of a validation carried out in the Netherlands.

Table C.1 f
s hows the re s u lts or an i ntra lab orator y va l idation u s i ng a n FI D and E C D de te c tor.

Tables C.2 to C.4 f

s how the re s u lts f
or an i nterl ab orator y va l idation or five d i fferent s ample s .

Table C.1 — Results of an intralaboratory test carried out in the Netherlands

Detection limit Repeatability

Compound FID ECD Level CVa FID CVa ECD
mg kg-1 dm mg kg-1 dm mg kg-1 dm % %

Benzene 0,02 – 1 5,0 –

Toluene 0,06 – 130 2,3 –
E thylb en z ene 0,03 – 50 3,5 –
o -Xylene 0,04 – 25 2,5 –
m -Xylene/p -Xylene 0,07 – 25 3,1 –
Styrene 0,05 – 100 3,0 –
Naphthalene 0,09 – 50 9,4 –
Dichloromethane 0,2 0,2 20 5,0 2,7
Trichloromethane 0,1 0,02 10 5,3 –
1,1-Dichloroethane 0,1 – 50 3,5 1,6
1,2-Dichloroethane 0,3 1,1 4 4,2 4,7
1,1,1-Trichloroethane 0,5 0,02 50 2,2 –
1,1,2-Trichloroethane 0,4 0,02 50 4,5 –
1,2-Dichloropropane 0,5 0,1 50 1,4 3,7
1,2,3-Trichloropropane 0,4 0,03 50 9,3 9,7
cis-1,3-Dichloropropene 0,3 0,01 50 4,8 –
trans-1,3-Dichloropropene 0,5 0,04 50 2,6 –
cis-1,2-Dichloroethene 0,4 0,5 50 4,2 2,4
trans-1,2-Dichloroethene 0,4 1,1 50 2,8 2,5
3-Chloropropene 0,2 – 1 18,5 –
Trichloroethene 0,2 0,01 60 3,5 –
Monochlorobenzene 0,5 – 10 3,7 –
1,2-Dichlorobenzene 0,3 0,7 10 3,6 8,0
a C V i s the va r i atio n co e ffic ie nt.

© ISO 2016 – All rights reserved 17

ISO 15009:2016(E)

Table C.2 — Results of an interlaboratory test carried out in the Netherlands (samples 1 and 2)

Sample 1 Sample 2
Compound Number of Average CVra CVRb Number of Average CVra CVRb
laboratories mg kg-1 dm % % laboratories mg kg-1 dm % %
Benzene 18 1,10 15 50 14 0,33 20 28
Toluene 15 9,77 17 33 16 0,20 20 39
E thylb en z ene 15 9,15 24 46 16 0,18 18 34
o -Xylene 15 16,0 7,7 75 15 0,38 20 26
m -Xylene/p -Xylene 16 26,9 9,0 89 15 0,63 22 40
S tyrene 7 0,06 12 54 – – – –
Naphthalene 13 3,87 19 73 11 0,09 64 79
E x p l a n atio n o f s ymb o l s

a CVr i s the re p e atab i l i t y va r i atio n co e ffic ient.

b CVR i s the re p ro duc ib i l i ty va r i atio n co e ffic ient.

Table C.3 — Results of an interlaboratory test carried out in the Netherlands (samples 3 and 4)

Sample 3 Sample 4
Compound Number of Average CVra CVRb Number of Average CVra CVRb
laboratories mg kg-1 dm % % laboratories mg kg-1 dm % %
Dichloromethane 17 5,92 22 88 14 0,16 30 87
Trichloromethane 15 5,56 16 40 – – – –
1,1-Dichloroethane 15 3,18 9,5 45 11 0,06 34 55
1,2-Dichloroethane 17 1,81 20 46 10 0,03 44 63
1,1,1-Trichloroethane 16 0,17 17 39 – – – –
1,1,2-Trichloroethane 14 1,03 15 37 – – – –
cis-1,2-Dichloroethene 13 3,66 8,2 29 9 0,07 16 55
trans-1,2-Dichlo- 13 3,10 10 31 8 0,05 6,3 63
roethane
Trichloroethene 17 0,21 15 73 – – – –
Monochlorobenzene 12 0,13 8,0 35 – – – –
E x p l a n atio n o f s ymb o l s

a CVr i s the re p e atab i l i t y va r i atio n co e ffic ient.

b CVR i s the re p ro duc ib i l i ty va r i atio n co e ffic ient.

Table C.4 — Results of an interlaboratory test carried out in the Netherlands (sample 5)

Sample 5
Compound Number of Average CVra CVRb
laboratories mg kg-1 dm % %

Benzene 13 0,20 9,7 25

Toluene 14 2,00 3,8 31
E thylb en z ene 13 1,69 6,0 23
o -Xylene 15 3,61 7,3 46
m -Xylene/p -Xylene 15 6,25 8,9 53
E xp l a n atio n o f s ymb o l s

a CVr i s the rep e atab i l i ty va r i atio n co e ffic ient.

b CVR i s the re p ro duc ib i l it y va r i atio n co e ffic ie nt.

18 © ISO 2016 – All rights reserved

 ISO 15009:2016(E)

Table C.4 (continued)

Sample 5
Compound Number of Average CVra CVRb
laboratories mg kg-1 dm % %

S tyrene – – – –
Naphthalene 10 0,803 14 66
Dichloromethane 13 12,3 9,5 56
Trichloromethane 15 0,77 9,2 30
1,1-dichloroethane 15 4,48 10 32
1,2-dichloroethane 14 2,38 8,2 18
1,1,1-trichloroethane 14 0,26 17 29
1,1,2-trichloroethane 13 1,32 7,5 55
cis-1,2-dichloroethene 13 5,13 7,5 39
trans-1,2-dichloroethene 12 4,71 9,2 46
Trichloroethene 16 0,30 12 64
Monochlorobenzene 9 0,19 11 57
E x p l a n atio n o f s ymb o l s

a CVr i s the re p e atab i l i t y va r i atio n co e ffic ient.

b CVR i s the re p ro duc ib i l i ty va r i atio n co e ffic ient.

© ISO 2016 – All rights reserved 19

ISO 15009:2016(E)

Annex D
(informative)
Information on purge and trap instruments

See also ISO 15680 for more details.

D.1 Purge and trap apparatus
Purge and trap equipment is commercially available or can be sel f-constructed. This includes fully
automated, online purge and trap GC-equipment with an autosampler and the thermal desorption device
incorporated in the instrument, as well as manually operated, o ff-line equipment. All instruments may
be used that meet the requirements and have proven to give reliable results.
The purge and trap apparatus may include:
a) autosampler;
b) purge vessel, heating mantle and temperature control, purge gas supply, flow controller, timer;
c) condenser and coolant supply or dry purge system;
d) adsorbent trap;
e) thermal desorption device, temperature control, timer;
f ) cold trap, coolant supply, heater, temperature control;
g) GC-MS or a GC with suitable detector(s), GC-auxiliaries, data-system.

D.2 Adsorbent trap

For purge and trap equipment using intermediate trapping on a packed adsorption column, these traps
are o ften home-made or can be obtained in various modifications. As an example, adsorption columns
are made of glass or stainless steel with an internal diameter of 2 mm to 5 mm, appropriate for use in
the apparatus for thermal desorption. Adsorbent traps are packed with a suitable adsorbent (generally
a polymer, a carbonaceous or silica adsorbent is used). Typical dimensions o f the packing are diameter
2 mm to 5 mm, length 10 mm to 50 mm, corresponding to at least 90 mg of adsorbent. The adsorbent is
kept in position by inert material like glass wool plugs or glass screens. This description is an example
and other adsorbent traps can be used as well, provided their performance meets the requirements of
this International Standard.
Prior to their first use, adsorbent traps should be conditioned by heating them above their desorption
temperature for several tens of min while passing a gentle stream of inert gas through them. A blank
procedure should be performed with the conditioned adsorbent trap before using it in routine.
D.3 Special requirements for use in off-line purge and trap equipment
In o ff-line purge and trap equipment, the adsorbent traps are not defined by the instrument in use,
whereas most of the other parts mentioned above [D.1 a) to D.1 f)] are for off-line use. Mark the traps
on one side to allow desorption in a back-flush mode. In case o f o ff-line purge and trap use, for the
adsorbent traps, caps o f inert material, for example polytetrafluoroethylene (PTFE), or o f metal with
screw windings and a PTFE-washer, so, a fter purging, they can be closed leak proo f for storage or
transfer to the apparatus for thermal desorption.

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ISO 15009:2016(E)

I CS 1 3 .080.1 0

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