🌿 Determination of 11 phthalates (e.g. DMP, DEP, DiBP, DBP, BBzP, DEHP, DOP) in groundwater, surface water, wastewater and drinking water — solid phase extraction (RP-C18 in glass cartridges, clean-up on alumina), elution with ethyl acetate, separation on a non-polar capillary column of about 30 m and mass spectrometric detection, quantification with internal standards (e.g. D4-DBP, D4-DOP); special measures against phthalate contamination (no plastics, glassware baked at 400 °C, deactivation with isooctane), maximum blank 80 ng/l for each phthalate; samples in the dark at 4 °C for at most 4 days; PN-EN ISO 18856:2006

Environment PN-EN ISO 18856

Overview

WHAT THE STANDARD COVERS. We read the text of the standard in the iTeh sample of ISO 18856:2004 (English text) — PN-EN ISO 18856:2006 adopts EN ISO 18856:2005 and ISO 18856:2004 as identical (PKN search): contents, foreword, introduction, Clauses 1–7 and Clause 8 up to 8.2.1 b) — the sample ends on page 7. We do not read the rest of extraction and clean-up (8), calibration (9), calculation (10), expression of results (11), precision (12), test report (13) or Annexes A (list of phthalates), B (general remarks, including internal standards), C (precision data, normative), D (examples of solutions), E (equipment to avoid contamination), F (columns) and G (GC conditions); we know the titles from the contents.

ACCORDING TO THE TEXT OF ISO 18856:2004. The standard was prepared by ISO/TC 147 “Water quality”, Subcommittee SC 2 “Physical, chemical and biochemical methods”. Warning: tests are to be carried out by suitably trained staff. Scope (1): determination of phthalates in water after solid phase extraction and GC-MS; groundwater, surface water, wastewater and drinking water; mass concentrations “from above 0.02 µg/l up to 0.150 µg/l” (as in the text), depending on the substance and the blank value; other phthalates — after checking applicability (list in Annex A). Table 1 (11 phthalates, formula, abbreviation, molar mass, CAS number): dimethyl (DMP, 131-11-3), diethyl (DEP, 84-66-2), dipropyl (DPP, 131-16-8), diisobutyl (DiBP, 84-69-5), dibutyl (DBP, 84-74-2), butyl benzyl (BBzP, 85-68-7), dicyclohexyl (DCHP, 84-61-7), di(2-ethylhexyl) (DEHP, 117-81-7), di(n-octyl) (DOP, 117-84-0), didecyl (DDcP, 84-77-5), diundecyl (DUP, 3648-20-2) phthalate. References (2): ISO 5667-1, ISO 5667-2, ISO 5667-3. Principle (3): solid phase extraction, GC separation on capillary columns, identification and quantification by MS. Interferences (4): phthalates as plasticizers are ubiquitous; in sampling — no plastics (tubes etc.); in enrichment — commercial adsorbents vary between batches, recovery depends on concentration: check it regularly at several levels and with each new batch, do calibration and analysis with one batch; laboratory air — remove plastics, do not use cleaning agents (they often contain phthalates); plastic gloves may increase contamination; maximum allowed blank — 80 ng/l for each phthalate with reference to water (Annex C); in GC — phthalates may bleed from injector septa, syringe fittings and vial septa. Reagents (5): with negligibly low phthalate content, checked by blanks; water — sometimes surface water is better than distilled (lower blank); nitrogen ≥ 99.9 %, helium ≥ 99.999 %; ethyl acetate of highest purity, methanol, isooctane; quartz wool and alumina (neutral, 50–200 µm) baked ≥ 4 h at 400 °C, alumina to be used within 5 days (Florisil or silica also possible after checking); RP-C18 sorbent (or commercial glass cartridges), breakthrough checked before analysis and for each batch; internal standards — e.g. diallyl phthalate, D4-DBP, D4-DOP, 13C-labelled standards; single solutions 1 g/l in ethyl acetate, stock solution 10–50 mg/l, solutions for multipoint calibration and recovery; storage at −18 °C in the dark, concentration checked every three months (stock) and every three weeks (calibration); internal standard solutions (e.g. 0.1 mg/l and 10 mg/l). Apparatus (6): everything in contact with the sample or extract free from phthalates; narrow-neck flasks with glass stoppers, preferably brown glass, 1000 and 2000 ml; drying oven (105 ± 10) °C; muffle furnace up to 400 °C, at least 60 l; vacuum SPE device; stainless steel or PTFE cocks; glass vials with PTFE-lined septa; glass cartridges and sample reservoirs (diameter 4 cm, about 35 cm); PTFE frits; baked aluminium foil; GC with capillary column and MS detector; non-polar fused silica columns, diameter ≤ 0.32 mm, about 30 m, film 0.10–0.50 µm. Sampling (7): according to ISO 5667-1, -2, -3; bottles and stoppers pre-treated, filled almost completely; stainless steel or glass containers, no plastics — if plastic parts are unavoidable, flush with at least five times the sample volume and state this in the report; extract as soon as possible, store in the dark at 4 °C for at most 4 days; suspended solids are not removed; homogenize. Procedure (8.1–8.2.1): wash glassware in a dishwasher, dry at 105 °C, bake in the furnace (e.g. to 100 °C at 2.5 °C/min, to 250 °C at 10 °C/min, 400 °C for 75 min, cooling within 12 h) — volumetric glassware may change its properties; close with stoppers or foil; small glassware in baked stainless steel containers; rinse walls with isooctane (deactivation against adsorption); cartridge: PTFE frit, 250 mg RP-C18 …

STATUS (as of 03.10.2026). The PKN search engine (query “PN-EN ISO 18856”, 03.10.2026) lists PN-EN ISO 18856:2006 — Polish version, “Introduces: EN ISO 18856:2005 [IDT], ISO 18856:2004 [IDT]”, without a withdrawal note; PN-EN ISO 18856:2005 (English version) — “Withdrawn and replaced by PN-EN ISO 18856:2006”.

HOW MANY LABORATORIES AND IN WHAT FORM (copy of the accreditation scope database, data up to 17.09.2026, read 03.10.2026). The number 18856 appears in 2 records at 2 laboratories: AB 213 and AB 1095. In the current PCA documents (read 03.10.2026; AB 213 issue no. 28 of 17.04.2026, AB 1095 issue no. 25 of 03.07.2026) the number appears at the same 2 laboratories; in every document the number of page markers equals the number of PDF pages, without repetitions; a search of all PCA documents downloaded from BIP on 03.10.2026 found no laboratories outside the database copy. The form “PN-EN ISO 18856:2006” at both; in the database copy the letter “M” is appended at AB 1095 — in the PCA document it is a separate column identifying the location, not part of the designation. None of these items is suspended. The “Laboratories” tab (query “PN-EN ISO 18856”) shows both laboratories — checked by a tab query on the labcoda.pl production server on 03.10.2026.

WHAT THE LABORATORIES TEST (items in PCA). AB 1095: water, water intended for human consumption, wastewater — dimethyl, diethyl, di-n-butyl, di-n-octyl, bis(2-ethylhexyl) (DEHP) and benzyl butyl phthalate, each (1.0–100) µg/l, and the sum of phthalates by calculation; GC-MS. AB 213: water, drinking water, wastewater — diethyl, DEHP, benzyl butyl, diisobutyl and dibutyl phthalate, each (1.0–100) µg/l, and the sum by calculation; GC-MS.

WHERE A SEEMINGLY CORRECT RESULT IS EASY TO GET. Blank: phthalates are ubiquitous — plastics in the laboratory, cleaning agents, gloves, injector and vial septa raise the result (4); the allowed blank is 80 ng/l for each phthalate (4.2), and the lower limit of the PCA items (1.0 µg/l) is about 12 times higher. Sampling: tubes and plastic parts contaminate the sample — they must be avoided or flushed with five times the volume and this recorded in the report (7). Sorbent: recovery depends on the RP-C18 batch and on concentration — calibration and analysis from the same batch, recovery checked with each new one (4.2, 5.9). Storage: at most 4 days at 4 °C in the dark (7). Glassware: volumetric glassware baked at 400 °C may change its volume (8.1, Note), and non-deactivated walls adsorb phthalates (8.1). Range: the scope text speaks of concentrations from above 0.02 µg/l up to 0.150 µg/l, while PCA items reach 100 µg/l — covering higher concentrations lies in the laboratory’s procedure; the range also depends on the blank value (1). Sum: the “sum of phthalates” in PCA is not a quantity defined in the part of the standard read — it depends on which phthalates the laboratory sums (AB 213 and AB 1095 have different lists).

WHAT WE DO NOT GIVE. We do not quote the rest of extraction and clean-up, calibration, formulae, GC-MS conditions, precision data of Annex C or examples of equipment and solutions — they lie outside the sample. We do not summarize ISO 5667-1, -2 and -3 in this entry. We do not give limit values for phthalates in drinking water or wastewater.

Method principle

Phthalates are isolated from the water sample by solid phase extraction — the sample passes through a cartridge with RP-C18 sorbent that retains them, after which they are eluted with a solvent and cleaned up. The extract is separated on a non-polar capillary column of a gas chromatograph, and the phthalates are identified and quantified by mass spectrometry against added internal standards (e.g. deuterated phthalates). The whole test is carried out in baked glassware without plastics, with control of the blank.

Applications

• 11 phthalates in groundwater, surface water, wastewater and drinking water (1, Table 1)
• Other phthalates — after checking the applicability of the method (1, Annex A)
• Water, water intended for human consumption and wastewater — phthalates (1.0–100) µg/l and sum — 2 accreditation scope records of 2 laboratories in PCA

Key parameters

Standard

Standard number

PN-EN ISO 18856:2006

Title (PL)

Jakość wody — Oznaczanie wybranych ftalanów z zastosowaniem chromatografii gazowej ze spektrometrią mas

Title (EN)

Water quality — Determination of selected phthalates using gas chromatography/mass spectrometry

Step-by-step procedure

1. Glassware preparation

   Dishwasher, drying at 105 °C, baking up to 400 °C, deactivation with isooctane (8.1). PN-EN ISO 18856:2006 — 2005 edition withdrawn and replaced (PKN, 03.10.2026).

2. Sampling

   Pre-treated glass bottles, no plastics; 4 °C in the dark, at most 4 days (7).

3. Extraction

   RP-C18 cartridge, concentration, clean-up (8.2; the rest outside the sample).

4. GC-MS

   Separation on the capillary column, identification and quantification with internal standards (3; Clauses 9–10 outside the sample).

5. Blank control

   Blank ≤ 80 ng/l for each phthalate (4.2).

Required equipment and apparatus

Reagents, media and consumables

Health and safety (OHS)

• The standard does not address all safety problems; tests are carried out by trained staff (warning); deactivation with isooctane in a fume hood (8.1)

Frequently asked questions