🌿 Determination of 4-nonylphenol (mixture of isomers) and 4-(1,1,3,3-tetramethylbutyl)phenol in non-filtered drinking, ground and surface water (0.005–0.2 µg/l and 0.02–0.2 µg/l) and, depending on the matrix, in waste water (0.1–50 µg/l) — 1 l sample acidified to pH 2, internal standard 4-n-nonylphenol(ring-13C6), extraction with 40 ml of toluene for at least 4 h in the sampling bottle, drying with sodium sulfate, concentration to 50–100 µl, clean-up on silica if necessary, GC-MS in EI mode at 70 eV with diagnostic ions m/z 135 and 107 (internal standard 113), calibration of the total procedure with the internal standard; PN-EN ISO 18857-1:2009

Environment PN-EN ISO 18857-1

Overview

WHAT THE STANDARD COVERS. We read the text of the standard in the iTeh sample of ISO 18857-1:2005 (English text) — PN-EN ISO 18857-1:2009 adopts EN ISO 18857-1:2006 and ISO 18857-1:2005 as identical (PKN search): foreword, clauses 1–8 and clause 9 up to 9.3 — the sample ends on page 7. We do not read the rest of calibration (9.3–9.4), calculation (10), expression of results (11), the test report or Annexes A–E (capillary columns, example chromatograms, nonylphenol recoveries, example separator, performance data); we know their titles from the table of contents.

ACCORDING TO THE TEXT OF ISO 18857-1:2005. The standard was prepared by ISO/TC 147 "Water quality", Subcommittee SC 2 "Physical, chemical and biochemical methods"; Part 2 of the series covers filtered samples with solid-phase extraction. Warning: tests must be carried out by suitably qualified staff. Scope (1): determination of 4-nonylphenol (mixture of isomers) and 4-(1,1,3,3-tetramethylbutyl)phenol in non-filtered samples of drinking, ground and surface water, in the range 0.005–0.2 µg/l for 4-(1,1,3,3-tetramethylbutyl)phenol and 0.02–0.2 µg/l for 4-nonylphenol; depending on the matrix also waste water in the range 0.1–50 µg/l; higher concentrations after dilution. References (2): ISO 3696, ISO 5667-1, -2, -3. Principle (3): the compounds are extracted with toluene from the acidified sample, the extract is cleaned on silica if necessary, the alkylphenols are separated on capillary columns, identified by mass spectrometry and quantified with an internal standard over the total procedure; the response factor for 4-(1,1,3,3-tetramethylbutyl)phenol and the technical isomer mixture of 4-nonylphenol is determined daily. Interferences (4): sample-dependent; contamination sources — reagents during storage, reused equipment, carryover from septum seals of bottles, vials and GC septa; organic polymers can form alkylphenols and raise results — avoid direct contact with plastics, which may contain alkylphenols. Reagents (5): with negligible concentrations of target alkylphenols, verified by blanks; grade 1 water; acid (e.g. HCl 37 % or H2SO4 1 mol/l); silica (pore size 6 nm, grain 0.063–0.2 mm) heated for at least 10 h at (550 ± 20) °C, with about 3 % water added, homogenized for 2 h; hexane; toluene (other solvents if they give equivalent recoveries, Annex C); anhydrous sodium sulfate; acetone; internal standard 4-n-nonylphenol(ring-13C6) 1 ng/µl (10 mg in 100 ml acetone, diluted 1:100); other internal standards acceptable if they meet the requirements (stable, non-interfering, structurally as similar to the analyte as possible, absent from the matrix); calibration standards 1 ng/µl: 4-nonylphenol (technical isomer mixture, CAS 84852-15-3) and 4-(1,1,3,3-tetramethylbutyl)phenol (CAS 140-66-9) — 10 mg each in 100 ml toluene, diluted 1:100 with toluene or acetone for calibration of the total procedure; solutions kept in the refrigerator, protected from light, checked weekly; nitrogen of purity ≥ 99.996 %. Apparatus (6): glassware rinsed with acetone (no detergents in a washing machine) or heated for at least 2 h at ≥ 250 °C; volumes chosen for an extraction volume of 1000 ml; shaking device; flat-bottomed 1000 ml bottles, preferably brown glass, with straight shoulders and glass stopper or PTFE-lined screw cap — the bottle must allow direct extraction; quartz wool; clean-up column 8 × 120 mm; quartz beaker; muffle furnace ≥ 600 °C; evaporation device; phase separator (example in Annex D); drying column 600 × 30 mm; 100 ml tapered flask; brown glass vials; gas chromatograph with a mass spectrometric detector operating on selected m/z. Sampling (7): according to ISO 5667-1, -2, -3; bottles acidified to pH 2 and not filled completely (e.g. to the shoulder) to allow addition of the extractant; storage in the refrigerator (2–5 °C), analysis as soon as possible, no later than 2 weeks after sampling; extraction in the bottle, which is weighed to 1 g. Extraction and concentration (8.1): 100–1000 µl internal standard per 1000 ml of sample, so that its concentration is in the middle of the calibration (e.g. 20 ng/l for ground and surface water, 500 ng/l for waste water); 40 ml toluene, shaking for at least 4 h; phase separation in the separator; emulsions broken by centrifuging or sodium sulfate; the extract runs through a column with 1–2 cm of sodium sulfate (pre-washed with 10 ml toluene), rinsed with 10 ml toluene, evaporated to about 2 ml and under a gentle nitrogen stream at < 40 °C to 50–100 µl; if necessary (waste water, polluted surface water) clean-up according to 8.2; without clean-up — into a vial and to 100–500 µl; sample volume = net mass of the bottle before and after (g ≙ ml). Clean-up (8.2): column with quartz wool, sodium sulfate and a slurry of 2 g silica in hexane, conditioned with 5 ml hexane; extract diluted with 1 ml hexane, washed with 10 ml hexane (hexane phase discarded), eluted with 20 ml toluene, concentrated to 50–100 µl. GC-MS (8.3): electron ionization at 70 eV, temperature programme determined experimentally, example conditions in Annex B. Blank (8.4): grade 1 water treated as the sample. Identification (8.5): retention time matching within ± 1 % (maximum ± 6 s) of the latest standard; both diagnostic ions m/z 135 and 107 present; the 4-nonylphenol peak pattern largely matching the technical standard; note: technical 4-nonylphenol usually gives 8–10 main peaks, the pattern may differ between batches, and a fixed ratio of the intensities of ions 135 and 107 is not obtained for the whole peak pattern; Table 1: both alkylphenols — ions 135 and 107, internal standard — 113. Calibration (9.1): solution of both alkylphenols; linearity checked with at least five concentrations (ISO 8466-1); the function is valid only within the range measured and checked regularly, routinely with two points; three variants — GC-MS step only with external standard (9.2), total procedure with external standard (9.3), total procedure with internal standard (9.4); the first two serve to estimate recovery, routine analysis uses only calibration of the total procedure with the internal standard. GC-MS calibration (9.2): at least five points, e.g. 0.005–0.2 µg/l (Table 3: 5–200 µl of the 1 ng/µl solution per 1 l); the same injection volume in calibration and measurement; linear regression y = a·ρ + b. Calibration of the total procedure with external standard (9.3): aliquots of standard solutions are added to 1000 ml of water and treated as a sample.

STATUS (as of 03.10.2026). The PKN search engine (query "PN-EN ISO 18857-1", 03.10.2026) returns two results: PN-EN ISO 18857-1:2009 — Polish version, "Introduces: EN ISO 18857-1:2006 [IDT], ISO 18857-1:2005 [IDT]", without a withdrawal note; and PN-EN ISO 18857-1:2006 — English version, "Withdrawn and replaced by PN-EN ISO 18857-1:2009 - Polish version".

HOW MANY LABORATORIES AND IN WHAT FORM (copy of the accreditation scope database, load up to 17.09.2026, read 03.10.2026). The number 18857-1 appears in 2 records at 2 laboratories: AB 165 and AB 213. In the current PCA documents (read 03.10.2026; AB 213 issue no. 28 of 17.04.2026, AB 165 issue no. 27 of 15.06.2026) the number appears at the same 2 laboratories; in each document the number of page markers equals the number of PDF pages, without duplicates; searching all PCA documents downloaded from the BIP on 03.10.2026 found no laboratories outside the database copy. Forms: "PN-EN ISO 18857-1:2009" (AB 213) and "PN-EN ISO 18857-1" without a year (AB 165). None of these items is suspended. The "Laboratories" tab (query "PN-EN ISO 18857-1") shows both laboratories — checked by a tab query on the labcoda.pl production server on 03.10.2026.

WHAT THE LABORATORIES TEST (PCA items). AB 165: water — concentration of alkylphenols, gas chromatography with mass spectrometric detection (GC-MS), without a numerical range. AB 213: water, water intended for human consumption, waste water — concentration of alkylphenols: 4-nonylphenol (0.02–0.20) µg/l, 4-tert-octylphenol (0.005–0.20) µg/l, gas chromatography with tandem mass spectrometric detection (GC-MS-MS).

WHERE A SEEMINGLY CORRECT RESULT IS EASY TO GET. Contamination: alkylphenols can come from plastics, septa and seals, and polymers can form them (4) — hence glass, PTFE, blanks and reagents checked for analytes (5, 8.4). Sample: the standard covers non-filtered samples extracted entirely in the sampling bottle; the volume is calculated from mass (7, 8.1). Time: no later than 2 weeks after sampling, at 2–5 °C (7). Identification: technical nonylphenol is 8–10 peaks with a variable pattern — a fixed 135/107 ion ratio is not a criterion for the whole pattern (8.5, note); the calibration standard must be the isomer mixture, not 4-n-nonylphenol (5.9). Calibration: routine analysis uses only calibration of the total procedure with the internal standard (9.1). Waste water: the 0.1–50 µg/l range applies "depending on the matrix" (1), and silica clean-up is then needed (8.1); AB 213 gives for waste water the same range as for waters (from 0.005 and 0.02 µg/l). Technique: the standard describes GC with mass selective detection; AB 213 uses GC-MS-MS. Name: AB 213 gives "4-tert-octylphenol" with the range (0.005–0.20) µg/l — this name does not appear in the text of the standard read; the standard gives the same range for 4-(1,1,3,3-tetramethylbutyl)phenol (CAS 140-66-9). AB 165 scope: the item gives neither analytes nor ranges.

WHAT WE DO NOT GIVE. We do not reproduce calculation formulas (10), rules for expressing results (11), example GC-MS conditions and chromatograms (Annexes A, B), recovery results (C) or performance data (E) — they are outside the sample. We do not summarize ISO 18857-2 or legal requirements for nonylphenol and octylphenol in waters in this entry.

Method principle

An internal standard — nonylphenol labelled with the 13C isotope — is added to the acidified water sample (1 l, pH 2), and the alkylphenols are extracted with toluene directly in the bottle. The extract is dried with sodium sulfate, concentrated, cleaned on silica if necessary and separated by gas chromatography; the mass spectrometer records characteristic ions (m/z 135 and 107 for the alkylphenols, 113 for the standard). The concentration is calculated from calibration of the total procedure with the internal standard.

Applications

• Drinking, ground and surface water, non-filtered samples — 4-(1,1,3,3-tetramethylbutyl)phenol 0.005–0.2 µg/l, 4-nonylphenol 0.02–0.2 µg/l (1)
• Waste water, depending on the matrix — 0.1–50 µg/l; higher concentrations after dilution (1)
• Water, water intended for human consumption and waste water — concentration of alkylphenols — 2 accreditation scope records of 2 laboratories in PCA

Key parameters

Standard

Standard number

PN-EN ISO 18857-1:2009

Title (PL)

Jakość wody — Oznaczanie wybranych alkilofenoli — Część 1: Metoda dla próbek niefiltrowanych z zastosowaniem ekstrakcji ciecz-ciecz i chromatografii gazowej z detekcją wybranych mas

Title (EN)

Water quality — Determination of selected alkylphenols — Part 1: Method for non-filtered samples using liquid-liquid extraction and gas chromatography with mass selective detection

Step-by-step procedure

1. Sampling and preservation

   1 l bottle, pH 2, not filled completely; 2–5 °C, up to 2 weeks; weighing the bottle (7). PN-EN ISO 18857-1:2009 — no withdrawal note (PKN, 03.10.2026).

2. Extraction

   Internal standard 100–1000 µl, 40 ml toluene, ≥ 4 h shaking, phase separation (8.1).

3. Drying and concentration

   Sodium sulfate, evaporation to about 2 ml, nitrogen < 40 °C to 50–100 µl (8.1).

4. Clean-up (if necessary)

   2 g silica, washing with hexane, elution with 20 ml toluene (8.2).

5. GC-MS and identification

   EI 70 eV; ions 135, 107 (113); retention time ± 1 %; peak pattern (8.3, 8.5).

6. Calibration

   Routinely total procedure with internal standard; blank with grade 1 water (8.4, 9.1).

Required equipment and apparatus

Reagents, media and consumables

Health and safety (OHS)

• Tests must be carried out by suitably qualified staff; the user establishes safety and health practices (warning)

Frequently asked questions