🌿 Determination of 15 chlorophenols (six dichlorophenols, six trichlorophenols, 2,3,4,5- and 2,3,4,6-tetrachlorophenol and pentachlorophenol) in soil, sediments and solid waste — at least 10 g of soil with an internal standard (2,4,6-tribromophenol) is extracted with 75 ml of acetone–hexane 1 : 1 with hydrochloric acid using ultrasound, the chlorophenols are transferred to NaOH, after acidification to hexane and to potassium carbonate solution, acetylated with acetic anhydride, the acetates are extracted with hexane and determined by GC-ECD on two columns of different polarity (or GC-MS); from about 0.01–0.05 mg/kg, PN-ISO 14154

Environment PN-ISO 14154

Overview

WHAT THE STANDARD COVERS. We read the text of the standard in the iTeh sample of SIST ISO 14154:2006 (English text of ISO 14154:2005): from the contents through the foreword, warning and Clauses 1–7 to 8.8 (calibration) on page 5. Outside the sample remain the rest of calibration, calculation (9), precision (10), quality assurance (11), test report (12), Annexes A (typical concentrations of standard solutions), B (example gas chromatographic conditions) and C (results of the interlaboratory test) and the bibliography.

ACCORDING TO THE TEXT OF ISO 14154:2005. The standard was prepared by ISO/TC 190 “Soil quality”, Subcommittee SC 3 “Chemical methods and soil characteristics”. Warning: chlorophenols are toxic and some are even carcinogenic — avoid skin contact, use gloves and protective clothing, and if large amounts of aerosols and dust are produced during sampling, breathing protection may be necessary. Scope (1): gas chromatographic determination of 15 chlorophenols in soil samples — 2,3-, 2,4-, 2,5-, 2,6-, 3,4- and 3,5-dichlorophenol, 2,3,4-, 2,3,5-, 2,3,6-, 2,4,5-, 2,4,6- and 3,4,5-trichlorophenol, 2,3,4,5- and 2,3,4,6-tetrachlorophenol and pentachlorophenol; the method can also be applied to other solid samples such as sediments and solid wastes; acid–base liquid extraction, acetylation, liquid/liquid extraction and determination by GC with electron-capture detection; lowest concentrations about 0.01–0.05 mg/kg depending on the component sensitivity and the sample quantity; when isomers cannot be completely separated, the sum is reported (e.g. 2,4- and 2,5-dichlorophenol). References (2): ISO 3696:1987, ISO 10381-1, ISO 11465:1993, ISO 14507. Term (3.1): chlorophenol — aromatic hydroxy compound (phenol) carrying one to five chlorine atoms. Principle (4): two steps — solid/liquid extraction with acetone–hexane at low pH, then purification by successive extractions in basic and acidic aqueous media and hexane; the chlorophenols in a carbonate solution are derivatized with acetic anhydride, the derivatives extracted with hexane, and the hexane fraction analysed by gas chromatography with electron capture or mass detection. Reagents (5): analytical grade, gases as recommended by the chromatograph manufacturer, only certified high-purity standards; water of grade 1; ethanol 99.5 %; hexane; acetone; hydrochloric acid 37 %; sodium hydroxide; potassium carbonate; acetic anhydride; anhydrous sodium sulfate (2 g portions in tubes with PTFE-lined caps, dried for 4 h at (500 ± 20) °C); internal standard 2,4,6-tribromophenol (according to a note, 2,4- or 2,6-dibromophenol can also be used); 15 chlorophenol standards with CAS numbers; NaOH 0.1 and 0.5 mol/l, K2CO3 0.1 and 5.2 mol/l; stock solutions of internal standard and chlorophenols in ethanol, portioned in 1.5 ml, at −18 °C (stable at least one year; at 4 °C in the dark at least half a year), working solutions diluted with water with a few drops of NaOH against precipitation; acetone–hexane 1 : 1. Apparatus (6): clean glassware free of interfering compounds — no plastics containers, since chlorophenols may adsorb to them and plastics may contribute impurities; capillary gas chromatograph, preferably with two electron-capture detectors and two columns connected to the same injector or two injectors — results from a single-column GC-ECD are confirmed on a second column of different polarity or by GC-MS; at least two capillary columns of different polarity; ultrasonic bath. Sampling (7): warning — soil contaminated with commercial chlorophenol mixtures often contains impurities of polychlorinated phenoxyphenols, dioxins and furans and PCBs, creating a contamination risk in the laboratory; sampling according to ISO 10381-1, pretreatment according to ISO 14507; glass bottles with PTFE caps, filling completely is recommended; storage in the dark at −18 °C or +4 °C; chlorophenols may undergo microbial conversion, so freezing is recommended for storage longer than 2 days. Procedure (8): field-moist soil is mixed with a spoon or spatula and at least 10 g taken from the bottle to 0.01 g; dry matter is determined in a subsample according to ISO 11465; blank — 10 g of matrix free of chlorophenols; standard sample — 50 µl of working solution and 10 g of such matrix. Extraction (8.5): in a fume hood, solvent wastes treated as hazardous; to the portion 50 µl of internal standard working solution, 75 ml of acetone–hexane and 0.5 ml of hydrochloric acid (more internal standard at high concentrations); ultrasound 2 min every 10 min for 1 h; the solution is extracted twice with 40 ml of 0.1 mol/l NaOH; for acidic, carbonate-containing or highly buffered soils, check that pH is < 3 in extraction and > 12 after adding NaOH; the combined NaOH extracts are acidified with hydrochloric acid to pH < 3 and extracted twice with 50 ml of hexane, and the hexane twice with 35 ml of 0.1 mol/l K2CO3. Acetylation (8.6): to the combined carbonate solution 1 ml of acetic anhydride, vigorous shaking for 2 min (releasing CO2), 10 min with occasional shaking, 5 ml of hexane, the hexane phase onto 2 g of Na2SO4, then into a second vial with Na2SO4, storage at 4 °C; acetates hydrolyse easily, so analysis as soon as possible, within 48 h; control samples — 50 µl of working solution in 100 ml of water with 2 ml of 5.2 mol/l K2CO3, acetylated as above. GC analysis (8.7): columns according to the manufacturer’s instructions, gas flows optimized for separation, stable conditions; example in Annex B. Calibration (8.8): extracted and acetylated standard samples with different volumes of working solution serve as calibration solutions; for each compound a separate calibration function of at least five points; several compounds may be examined in one calibration.

STATUS (as of 03.10.2026). The PKN search (query “PN-ISO 14154”, 03.10.2026) shows PN-ISO 14154:2008 (Polish version, “Wprowadza: ISO 14154:2005 [IDT]”) without a withdrawal note; the other results are PN-EN 14154 standards on water meters. In the iTeh catalogue (read on 03.10.2026) ISO 14154:2005 has the status “Published”, stage 90.93 (standard confirmed).

HOW MANY LABORATORIES AND IN WHAT FORM (copy of the accreditation scope database, load up to 17.09.2026, read on 03.10.2026). The number 14154 appears in 4 records at 4 laboratories: AB 213, AB 300, AB 418, AB 1095. In the current PCA documents (read on 03.10.2026, issues from 26.01.2026 to 08.09.2026) the number appears in 4 rows — one at each; in each of the four documents the number of page markers equals the number of PDF pages, without repetitions; a search of all 1291 PCA documents downloaded from BIP on 03.10.2026 found no laboratories outside the database copy (17 laboratories in the register have no link to a scope document on BIP). Form “PN-ISO 14154:2008” together with procedure EFO/I/45/2 of 17.09.2025 (AB 213), “PN-ISO 14154:2008” marked “M” for a modified method (AB 1095), “PN-ISO 14154” without year (AB 418) and “PN ISO 14154:2008” without the hyphen, together with instruction IN-172 issue 3 of 18.03.2019 (AB 300). None of these items is suspended. The “Laboratories” tab (query “PN-ISO 14154”) shows 3 laboratories — all except AB 300, where the number is written “PN ISO” without the hyphen — checked with a tab query on the labcoda.pl production server on 03.10.2026.

WHAT THE LABORATORIES TEST (items in PCA). Test object: bottom sediments, soil, ground (AB 213); soil (AB 300, AB 1095); soil, ground (AB 418, item in a flexible accreditation scope). Characteristic: chlorophenol content — at AB 213 and AB 1095 with a list: 2-, 3- and 4-chlorophenol, dichlorophenols (at AB 213 2,4- and 2,5- as a sum), trichlorophenols, 2,3,4,5-, 2,3,4,6- and 2,3,5,6-tetrachlorophenol, pentachlorophenol and calculated sums; at AB 418 without a list; AB 300 — phenol and cresol (o,m,p-cresol) content. Ranges: (0.010–5.0) mg/kg, for the sum of 2,4- and 2,5-dichlorophenol (0.010–10.0) mg/kg (AB 213), (0.010–1.0) mg/kg (AB 1095), (0.020–100) mg/kg for phenol and cresols (AB 300). Technique: GC-MS (AB 300, AB 418, AB 1095), GC-MS-MS (AB 213).

WHERE A SEEMINGLY CORRECT RESULT IS EASY TO GET. At the scope: the standard covers 15 chlorophenols from dichloro- to pentachlorophenol (1) — monochlorophenols and 2,3,5,6-tetrachlorophenol (AB 213, AB 1095) and phenol and cresols (AB 300) are not in it. At detection: GC-ECD in the title, but the principle allows mass detection, and a single-column ECD result is confirmed on a second column or by GC-MS (4, 6.2) — all four laboratories state GC-MS or GC-MS-MS. At pH: for acidic, carbonate or buffering soils check pH < 3 and > 12 (8.5). At vessels: glass only, no plastics (6.1). At the sample: freezing for storage longer than 2 days, because chlorophenols undergo microbial conversion (7). At derivatives: acetates hydrolyse — analysis within 48 h (8.6). At isomers: unseparated ones are reported as a sum, e.g. 2,4- and 2,5-dichlorophenol (1). At the laboratory: soils contaminated with chlorophenol mixtures may bring in dioxins, furans and PCBs (7).

WHAT WE DO NOT GIVE. We did not read the calculation, precision data, quality assurance rules, typical standard concentrations and chromatographic conditions (9–12, Annexes A–C). We do not give limit values for chlorophenols in soil.

Method principle

At least 10 g of field-moist soil with an internal standard (2,4,6-tribromophenol) is extracted with acetone–hexane 1 : 1 with hydrochloric acid in an ultrasonic bath for 1 h. The chlorophenols pass into NaOH, after acidification into hexane, and from it into potassium carbonate solution, where they are acetylated with acetic anhydride; the acetates are extracted with hexane, dried over sodium sulfate and determined within 48 h by GC with an electron-capture detector on two columns of different polarity or by GC-MS, with calibration on extracted standard samples.

Applications

• Soil — 15 chlorophenols (di-, tri-, tetra- and pentachlorophenol) from about 0.01–0.05 mg/kg (1)
• Other solid samples, e.g. sediments and solid wastes (1)
• Soil, ground and bottom sediments — chlorophenols, at one laboratory phenol and cresols — items in the accreditation scopes of 4 laboratories in PCA

Key parameters

Standard

Standard number

PN-ISO 14154:2008

Title (PL)

Jakość gleby — Oznaczanie zawartości niektórych wybranych chlorofenoli — Metoda chromatografii gazowej z detekcją wychwytu elektronów

Title (EN)

Soil quality — Determination of some selected chlorophenols — Gas-chromatographic method with electron-capture detection

Step-by-step procedure

1. Sample

   Glass with PTFE, dark, −18 °C or +4 °C (freezing > 2 days); ≥ 10 g of moist soil, dry matter according to ISO 11465 (7, 8.1, 8.2). PN-ISO 14154:2008 without a withdrawal note (03.10.2026).

2. Extraction

   Internal standard, acetone–hexane with HCl, ultrasound 1 h; blank and standard samples alike (8.3–8.5).

3. Clean-up

   NaOH → acidification to pH < 3 → hexane → K2CO3 (8.5).

4. Acetylation

   Acetic anhydride, hexane, drying over Na2SO4, 4 °C, analysis within 48 h (8.6).

5. GC and calibration

   GC-ECD on two columns or GC-MS; ≥ 5 calibration points per compound (8.7, 8.8).

Required equipment and apparatus

Reagents, media and consumables

Health and safety (OHS)

• Chlorophenols are toxic, some carcinogenic — gloves and protective clothing, breathing protection with dust (warning)
• Extraction in a fume hood, solvent wastes treated as hazardous (8.5)
• Soils contaminated with chlorophenol mixtures may contain dioxins, furans and PCBs — risk of laboratory contamination (7)

Frequently asked questions