🌿 Determination of 17 organochlorine pesticides (HCB, HCH, aldrin, dieldrin, endrin, heptachlor and its epoxides, α-endosulfan, DDT, DDD, DDE) and 7 polychlorinated biphenyls (PCB 28, 52, 101, 118, 138, 153, 180) in soil — extraction with a hydrocarbon solvent, clean-up on aluminium oxide, removal of sulfur with tetrabutylammonium sulfite, gas chromatography with electron capture detection and confirmation on a column of different polarity; detection limits 0.1–4 µg/kg d.m., PN-ISO 10382

Environment PN-ISO 10382

Overview

WHAT THE STANDARD COVERS. Scope from the PKN catalogue card of PN-ISO 10382:2007 (Polish version), in full (our translation): “A method is given for the quantitative determination of seven polychlorinated biphenyls and seventeen organochlorine pesticides in soil. The method is applicable to all soils. Under the conditions given in this standard detection limits of 0.1 microg/kg to 4 microg/kg (expressed on soil dry matter) can be achieved”. We read the text of the standard in the iTeh sample of ISO 10382:2002 (French version): from the title page through the foreword and Clauses 1–5 up to and including Clause 6 (preparation of standard solutions). Outside the sample remain Clauses 7 (sampling, storage and pre-treatment of samples), 8 (blank test, extraction and concentration, clean-up, separation of PCB from polar pesticides, GC analysis), 9 (test report) and 10 (accuracy) and Annexes A (retention times on two columns), B (scheme of standard solutions), C (interlaboratory trial in the Netherlands) and D (removal of sulfur and certain organic sulfur compounds).

ACCORDING TO THE TEXT OF ISO 10382:2002 (Clauses 1–6). The standard was prepared by ISO/TC 190 “Soil quality”, subcommittee SC 3; Annexes A–D are informative. References (2): ISO 10381-1 and -2 (soil sampling), ISO 11465:1993 (dry matter), ISO 14507 (pre-treatment of samples for determination of organic contaminants). Principle (3): the sample after pre-treatment is extracted with a hydrocarbon solvent, the extract is concentrated, polar compounds are removed on an aluminium oxide column, and elemental sulfur — with tetrabutylammonium sulfite reagent; separation on a capillary column with a stationary phase of low polarity and electron capture detection (ECD); identification and quantification on the basis of relative retention times and relative peak heights or areas against internal standards. The standard notes that the efficiency depends on the composition of the soil, and the procedure does not account for incomplete extraction due to the structure and composition of the sample. Notes: confirmation of identity and concentration requires re-analysis on a column of different polarity or by GC-MS; other non-volatile organochlorine compounds, e.g. chlorobenzenes, can also be determined by this method. Reagents (4): petroleum ether 40–60 °C, acetone, diethyl ether (checked for peroxides, e.g. with a fresh 10 % KI solution), anhydrous sodium sulfate heated at least 6 h at 550 °C ± 20 °C, basic or neutral aluminium oxide (200 m2/g, Brockmann activity Super I) deactivated with 10 % water and left about 16 h, silica gel 60–200 µm dried at least 24 h at 150 °C and deactivated with 5 % water; for each new batch of adsorbent the elution pattern is checked with a standard solution of PCB and pesticides. Standards: PCB 28, 52, 101, 118, 138, 153, 180 and pesticides: hexachlorobenzene (HCB), α-, β- and γ-hexachlorocyclohexane, aldrin, dieldrin, endrin, heptachlor, two heptachlor epoxides (isomer A and B), α-endosulfan, p,p′-DDE, o,p′-DDD, o,p′-DDT, p,p′-DDD, o,p′-DDE, p,p′-DDT; internal standard PCB 155 and a second one chosen from PCB 143, PCB 207 or mirex. TBA reagent: tetrabutylammonium hydrogen sulfate 0.1 mol/l in a mixture of equal volumes of water and isopropanol, saturated with sodium sulfite (about 25 g per 100 ml); n-heptane. Apparatus (5): glassware washed and rinsed with acetone and petroleum ether or hexane; 1 l glass bottles with PTFE-lined screw caps; horizontal shaker 200–300 strokes per minute; water bath up to 100 °C; 2 l separating funnels; Kuderna-Danish evaporator (or another equivalent, e.g. a rotary evaporator); quartz wool or silanised glass wool — with a warning against inhaling quartz dust; gas chromatograph with a non-discriminating injector, capillary column and a 63Ni ECD (the radioactive source requires a licence under national regulations); fused silica column 50 m × about 0.25 mm with cross-linked polysiloxane, and for confirmation — a column of medium polarity (e.g. CP-Sil 19, OV 1701); chromatographs with two detectors and two columns connected to one injector work well — confirmation then takes place in the same injection. Standard solutions (6): about 10 mg of each standard in 25 ml n-heptane (about 0.4 mg/ml), purity checked by GC with FID or TCD, mixture with internal standards according to Annex B, storage in the dark below 4 °C, stability at least one year.

STATUS (as of 03.10.2026). The card of PN-ISO 10382:2007 (Polish version, published 13-02-2007, 26 pages, price group M) has no “Withdrawn” header: Health, Environment and Medicine Sector, KT 191 Soil Chemistry, ICS 13.080.10, “Introduces: ISO 10382:2002 [IDT]”; the card has no “Replaces” or “Replaced by” fields. In the iTeh catalogue (read on 03.10.2026) ISO 10382:2002 has the status “Withdrawn” (stage 95.99, completed 29.08.2026), and in the field “Revised” two standards: ISO 23646:2022 “Soil quality — Determination of organochlorine pesticides by gas chromatography with mass selective detection (GC-MS) and gas chromatography with electron-capture detection (GC-ECD)” and ISO 18475:2023 “Environmental solid matrices — Determination of polychlorinated biphenyls (PCB) by GC-MS or GC-ECD”. The ISO standard has thus split into two — separately for pesticides and separately for PCB; the Polish national standard adopting ISO 10382 remains in the PKN catalogue without annotation. The PCB part already has a counterpart in the PKN catalogue: the card of PN-EN ISO 18475:2026-01 (English version, published 08-01-2026, KT 191, “Introduces: EN ISO 18475:2025 [IDT], ISO 18475:2023 [IDT]”) — seven PCB in soil, sewage sludge, sludge, treated biowaste and solid waste by GC-MS and GC-ECD, from 1 µg/kg d.m. (soil, sewage sludge, biowaste) to 10 µg/kg d.m. (solid waste); it replaced PN-EN 17322:2021-01, which was withdrawn on 08-01-2026 (cards as of 03.10.2026). We did not find a standard adopting ISO 23646 (pesticides) in the PKN search engine (term “ISO 23646”, 03.10.2026).

HOW MANY LABORATORIES AND IN WHAT FORM (copy of the accreditation scope database, data up to 17.09.2026, read on 03.10.2026). The number 10382 appears in 6 records at 5 laboratories: AB 165, AB 213 (2), AB 322, AB 418, AB 1095. In the current PCA documents (read on 03.10.2026, issues from 17.11.2025 to 03.07.2026) the number appears in 6 items of the same 5 laboratories. Notation “PN-ISO 10382:2007”, at AB 165 “PN-ISO 10382” without the year (together with PN-EN 17322); AB 213 cites the standard as the basis of its in-house procedure (“EFO/PB/24/A z dnia 18.09.2023 r. na podstawie normy: PN-ISO 10382:2007”). The “Laboratories” tab (“PN-ISO 10382”) shows the same 5 laboratories — checked with the tab query on the production server labcoda.pl on 03.10.2026.

WHAT THE LABORATORIES TEST (items in PCA). Only two items correspond directly to the subject and technique of the standard: AB 322 — pesticides in soil by GC-ECD (aldrin (0.2–120) µg/kg, dieldrin and endrin (0.2–400) µg/kg, p,p′-DDE, p,p′-DDD (0.2–120) µg/kg, p,p′-DDT and o,p′-DDT (0.2–250) µg/kg, “total DDT” (0.2–250) µg/kg, α-HCH (0.2–400) µg/kg, β-HCH and γ-HCH (0.2–300) µg/kg) — the lower limits lie within the detection limits of Clause 1; AB 1095 — seven PCB in soil (PCB 28, 52, 101, 118, 138, 153, 180, each (0.020–2.0) mg/kg) by GC-ECD and the sum of PCB by calculation. The others reach beyond the standard: AB 418 — chlorobenzenes in soil and ground by GC-ECD (the standard allows chlorobenzenes in Note 2 to Clause 3); AB 165 — PCB in soil by GC-MS, together with PN-EN 17322 (withdrawn by PKN on 08.01.2026 and replaced by PN-EN ISO 18475:2026-01); AB 213 — two items “pesticide content” in bottom sediments and soil by GC-MS/MS according to an in-house procedure, with a list that besides compounds of the standard includes many outside it, also from other pesticide groups (e.g. trifluralin, chlorfenvinphos, cypermethrin, dichlorvos, terbutryn, cybutryne, alachlor, δ-HCH, isodrin, hexachlorobutadiene, methoxychlor, endosulfan II, endosulfan sulfate, chlordane), in ranges from 0.0001 to 5.0 mg/kg.

WHERE A SEEMINGLY CORRECT RESULT IS EASY. In identification: a peak at the right retention time on one column is not enough — the standard requires confirmation on a column of different polarity (e.g. CP-Sil 19, OV 1701) or by GC-MS (3, Note 1; 5.13). In extraction: the procedure does not account for incomplete extraction due to the structure and composition of the soil (3) — good recoveries of internal standards do not prove that compounds bound to the soil have been extracted. With reagents: diethyl ether containing peroxides may oxidise some of the analytes (4.4); for each new batch of aluminium oxide and silica gel the standard requires checking the elution pattern with a standard solution and adjusting the deactivation if necessary (4.8) — without this check it is not known whether all analytes reach the collected fraction. With sums: “total DDT” and “sum of PCB” depend on which compounds the laboratory includes — the standard lists six forms of DDT and seven PCB, and accreditation scopes do not always say which components went into the sum.

WHAT WE DO NOT GIVE. We have not read Clauses 7–10 or the annexes, so we do not give the sample mass, solvent volumes, the course of extraction and clean-up, the separation of PCB from polar pesticides on silica gel, the chromatographic conditions, the calculation or accuracy data. Nor do we give the differences between ISO 10382 and ISO 23646 and ISO 18475 — we have not read the texts of those standards — or limit values in soil.

Method principle

A pre-treated soil sample is extracted with a hydrocarbon solvent (petroleum ether with acetone) with addition of internal standards (PCB 155 and a second one — PCB 143, PCB 207 or mirex), the extract is concentrated, polar compounds are removed on an aluminium oxide column and elemental sulfur — with tetrabutylammonium sulfite reagent. Organochlorine pesticides and PCB are separated on a capillary column of low polarity and detected with an electron capture detector (63Ni); identity and concentration are confirmed on a column of different polarity or by GC-MS.

Applications

• All types of soil — 7 PCB and 17 organochlorine pesticides, detection limits 0.1–4 µg/kg d.m. (1)
• Other non-volatile organochlorine compounds, e.g. chlorobenzenes (3, Note 2)
• Soil and bottom sediments — pesticides, PCB and chlorobenzenes in the accreditation scopes of 5 laboratories in PCA (GC-ECD, GC-MS, GC-MS/MS)

Key parameters

Standard

Standard number

PN-ISO 10382:2007

Title (PL)

Jakość gleby — Oznaczanie zawartości pestycydów chloroorganicznych i polichlorowanych bifenyli — Metoda chromatografii gazowej z detekcją wychwytu elektronów

Title (EN)

Soil quality — Determination of organochlorine pesticides and polychlorinated biphenyls — Gas-chromatographic method with electron capture detection

Step-by-step procedure

1. Sampling and pre-treatment

   Glass bottles with PTFE liner; sampling according to ISO 10381, pre-treatment according to ISO 14507, dry matter according to ISO 11465. PN-ISO 10382:2007 without “Withdrawn” header on the PKN card, ISO 10382:2002 withdrawn (as of 03.10.2026).

2. Extraction

   Hydrocarbon solvent with addition of internal standards; we do not give the sample mass and volumes (Clause 8).

3. Clean-up

   Aluminium oxide column (removal of polar compounds), concentration, TBA reagent (removal of elemental sulfur); if necessary separation on silica gel.

4. GC-ECD

   Capillary column of low polarity; identification by relative retention times against internal standards.

5. Confirmation

   Re-analysis on a column of different polarity or GC-MS — a single ECD peak is no proof of identity.

Required equipment and apparatus

Reagents, media and consumables

Health and safety (OHS)

• The ECD contains a sealed radioactive 63Ni source — its use requires a licence under national regulations (5.12, Note 1)
• Dust from quartz wool is harmful if inhaled — work in a hood and wear a dust mask (5.8)
• Diethyl ether forms peroxides — check before use (4.4); organochlorine pesticides and PCB are toxic and persistent — treat standard solutions and waste as hazardous

Frequently asked questions