ISO 5120:2023

Soil quality — Determination of perchlorate in soil using liquid chromatography-tandem mass spectrometry (LC-MS/MS)

This document specifies a method for determining of perchlorate in soil and soil-like materials using liquid chromatography connected to a tandem mass spectrometry (LC-MS/MS). It defines pretreatment (including drying and sieving) of sample, extraction, clean-up, analysis using LC-MS/MS, and calculation of perchlorate content in dry soil. Under the conditions specified in this document, the limit of quantitation (LOQ) is approximately 4,6 μg/kg-dry soil.

Qualité du sol — Détermination du perchlorate dans le sol par chromatographie en phase liquide couplée à la spectrométrie de masse en tandem (CL-SM/SM)

General Information

• Status: Published
• Publication Date: 03-Jul-2023
• ICS: 13.080.10 - Chemical characteristics of soils
• Technical Committee: ISO/TC 190/SC 3 - Chemical and physical characterization
• Drafting Committee: ISO/TC 190/SC 3/WG 6 - Organic analysis
• Current Stage: 6060 - International Standard published
• Start Date: 04-Jul-2023
• Due Date: 14-Jul-2023
• Completion Date: 04-Jul-2023

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 5120
First edition
2023-07
Soil quality — Determination of
perchlorate in soil using liquid
chromatography-tandem mass
spectrometry (LC-MS/MS)
Qualité du sol — Détermination du perchlorate dans le sol par
chromatographie en phase liquide couplée à la spectrométrie de
masse en tandem (CL-SM/SM)
Reference number
ISO 5120:2023(E)
© ISO 2023

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ISO 5120:2023(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2023
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
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Published in Switzerland
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ISO 5120:2023(E)
Contents Page
Foreword .v
Introduction . vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Interferences . 2
6 Reagents . 2
6.1 Eluents . 2
6.2 Extractant . 2
6.3 Reagents for standard solutions . 3
6.4 Standard solutions . 3
−
6.4.1 Stock standard solution, c (ClO ) = 1 000 mg/l . 3
4
−
6.4.2 Working standard solution, c (ClO ) = 10 mg/l . 3
4
6.4.3 Calibration standards . 3
18 −
6.4.4 Internal standard stock solution, c (Cl O ) = 10 mg/l . 3
4
18 −
6.4.5 Internal standard spiking solution, c (Cl O ) = 1 000 μg/l . 3
4
7 Apparatus . 3
7.1 Centrifuge tube . 3
7.2 Equipment for extraction . 3
7.2.1 Horizontal mechanical shaker . 3
7.2.2 Centrifuge . 3
7.3 Filtration device . 4
7.4 Membrane filter . 4
7.5 Clean-up cartridge. 4
7.6 Micro pipette and Pasteur pipette . 4
7.7 Liquid chromatograph/tandem mass spectrometer . 4
7.7.1 Liquid chromatograph. 4
7.7.2 Mass spectrometer . 4
8 Procedure .5
8.1 Sampling and storage . 5
8.2 Pretreatment . 5
8.2.1 Drying . 5
8.2.2 Sieving . . 5
8.3 Extraction . 5
8.3.1 Mechanical shaking . 5
8.3.2 Centrifuge . 5
8.3.3 Filter and clean-up . 5
8.4 Liquid chromatography-Tandem mass spectrometry (LC-MS/MS) . 5
8.4.1 Liquid chromatography . . . 5
8.4.2 Tandem mass spectrometry . 5
8.4.3 Calibration using internal standard material . 6
9 Quality control . 6
10 Calculation . 7
11 Expression of results . 7
12 Test report . 7
Annex A (informative) Examples of Liquid chromatography – tandem mass spectrometry
(LC-MS/MS) conditions . . 8
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ISO 5120:2023(E)
Annex B (informative) Performance data .10
Bibliography .12
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ISO 5120:2023(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
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electrotechnical standardization.
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described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO document should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
ISO draws attention to the possibility that the implementation of this document may involve the use
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This document was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3
Chemical and physical characterization.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.
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ISO 5120:2023(E)
Introduction
-
Although perchlorate (ClO ) occurs naturally, it is mainly considered a manmade anion. Usually, it is
4
+ + +
combined with NH , Na , and K to form ammonium perchlorate, potassium perchlorate, and sodium
4
perchlorate, respectively. It has been reported that more than 90 % of manufactured perchlorate is
used in military activities. Due to the outstanding oxidizing capacity of perchlorate, it is added to
propellant for rockets, missiles, and satellites. Various routes of manmade perchlorate exposure to
soil can be assumed. For example, complete or incomplete explosion of a signal bomb in a target or
impact area, an oversupply of perchlorate for complete combustion at firing points, and large-scale
fireworks display can be sources of perchlorate exposure to soil. Additionally, other routes could
come from waste treatment processes. Because perchlorate in missiles naturally deteriorates over
time, they need to be recharged. In the past, incineration was the preferred treatment for deteriorated
perchlorate. When the incineration process is carried out in an open space and kept as ash onsite
without caution, this becomes a detrimental route for soil contamination. Perchlorate is very stable in
water and is not strongly retained by soil particle. As such, surface water or groundwater can become
easily contaminated by the surface runoff or the leaching process. Perchlorate in growth medium also
contaminates vegetation. This kind of pathway could subsequently affect higher level organisms through
the food chain. Perchlorate contamination of drinking water and the food chain can potentially affect
human health through interfering with iodide uptake by the thyroid gland. This kind of interference
causes a decrease in thyroid hormone production and leads to hyperthyroidism. The permitted level
of perchlorate concentration in drinking water is below 15 ppb in South Korea. Although some states
in the USA have an advisory level for perchlorate in drinking water, it is very difficult to find a country
which regulates the perchlorate level in soil as perchlorate contamination of soil is rare in normal
circumstances. However, perchlorate is considered a major contaminant in military fields and so the
management of perchlorate in soil is necessary. Accordingly, ISO 20295 proposes a standard method
for determining perchlorate in soil using ion chromatography. For the standard method of ISO 20295,
the limit of quantitation of perchlorate is 0,1 mg/kg soil. However, since perchlorate in soil is frequently
found to be lower than the designated level, an analytical method for determining perchlorate at ppb
levels is required. For this purpose, a standard method for analysing the trace level of perchlorate in
soil has been developed.
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INTERNATIONAL STANDARD ISO 5120:2023(E)
Soil quality — Determination of perchlorate in soil using
liquid chromatography-tandem mass spectrometry (LC-
MS/MS)
1 Scope
This document specifies a method for determining of perchlorate in soil and soil-like materials using
liquid chromatography connected to a tandem mass spectrometry (LC-MS/MS). It defines pretreatment
(including drying and sieving) of sample, extraction, clean-up, analysis using LC-MS/MS, and calculation
of perchlorate content in dry soil.
Under the conditions specified in this document, the limit of quantitation (LOQ) is approximately
4,6 μg/kg-dry soil.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 11464, Soil quality — Pretreatment of samples for physico-chemical analysis
ISO 8466-1, Water quality — Calibration and evaluation of analytical methods — Part 1: Linear calibration
function
ISO 8466-2, Water quality — Calibration and evaluation of analytical methods and estimation of
performance characteristics — Part 2: Calibration strategy for non-linear second-order calibration
functions
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
4 Principle
The soil and soil-like materials to be analysed are used for the experiment after pretreatment, air-
drying and sieving. Perchlorate in soil and soil like materials is extracted by distilled or deionized
water. Extraction of perchlorate is done by mechanical shaking and centrifugation.
After filtering the extract using 0,2 μm to 0,45 μm membrane filter (e.g. cellulose acetate, hydrophilic
polypropylene or polyethersulphone filter), the internal standard solution is spiked into the filtrate.
The filtrate is analysed by LC-MS/MS for the determination of perchlorate.
If the adverse effects of other anions (e.g. sulfate, chloride, and bicarbonate), cations, or organic
matter are not negligible, appropriate pretreatment for the elimination of these effects should be
applied. Selective removal of interfering elements with cartridge or column is one of the applicable
pretreat
...