ISO 17226-1:2021 INTERNATIONAL STANDARDIULTCS/IUC 19-1:2021(E)Leather — Chemical determination of formaldehyde content —Part 1: Method using high-performance liquid chromatography

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INTERNATIONAL STANDARDIULTCS/IUC 19-1:2021(E)Leather — Chemical determination of formaldehyde content —Part 1: Method using high-performance liquid chromatography是于2021-02发布的ISO标准，适用于国际范围。

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INTERNATIONAL STANDARD

IULTCS/IUC 19-1:2021(E)

Leather — Chemical determination of formaldehyde content —

Part 1: Method using high-performance liquid chromatography

1 Scope

This document specifies a method for the determination of free and released formaldehyde in leathers. This method, based on high-performance liquid chromatography (HPLC), is selective and not sensitive to coloured extracts and is intended to be used for precise quantification of formaldehyde.

The formaldehyde content is taken to be the quantity of free formaldehyde and formaldehyde extracted through hydrolysis contained in a water extract from the leather under standard conditions of use.

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 2418, Leather — Chemical, physical and mechanical and fastness tests — Sampling location

ISO 3696, Water for analytical laboratory use — Specification and test methods

ISO 4044, Leather — Chemical tests — Preparation of chemical test samples

ISO 4684, Leather — Chemical tests — Determination of volatile matter

3 Terms a nd definiti ons

No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso. org/ obp

— IEC Electropedia: available at http:// www.e lectropedia. org/ 4 C onform ity

When compared with ISO 17226-2, the two analytical methods should give similar trends but not necessarily the same absolute result. Therefore, in cases of dispute, the method in this document shall be used in preference to ISO 17226-2.

5 Principle

The process is selective. Formaldehyde is separated and quantified as a derivative from other aldehydes and ketones by HPLC. Detected is the free formaldehyde and formaldehyde which is hydrolysed during extraction to yield free formaldehyde.

IULTCS/IUC 19-1:2021(E)

The sample is eluted with a detergent solution at 40 °C. The eluate is mixed with 2,4-dinitrophenylhydrazine (DNPH), whereby aldehydes and ketones react to give the respective hydrazones. These are separated by means of a reversed-phase HPLC with ultraviolet (UV) detector or diode array detector (DAD).

6 Reagents

Use only reagents of recognized analytical grade, unless otherwise stated. All solutions are aqueous solutions.

6.1 Water, grade 3, in accordance with ISO 3696.

6.2 Formaldehyde solution, CAS no. 50-00-0, approximately 37 % (mass fraction).

Certified solutions of formaldehyde or formaldehyde-2,4-DNPH are commercially available. When these solutions are used, the procedure in 9.1 is not required.

6.3 Iodine solution, CAS no. 7553-56-2, 0,05 mol/l, i.e. 12,68 g iodine per litre.

6.4 Sodium hydroxide solution, CAS no. 1310-73-2, 2,0 mol/l.

6.5 Sulfuric acid solution, CAS no. 7664-93-9, 2,0 mol/l.

6.6 Sodium thiosulfate solution, CAS no. 10102-17-7, 0,1 mol/l.

6.7 Starch solution, CAS no. 9005-84-9, 1 %, i.e. 1 g in 100 ml water.

6.8 Acetonitrile, CAS no. 75-05-8, LC grade.

6.9 Sodium dodecylsulfonate, CAS no. 2386-53-0, or sodium dodecylsulfate, CAS no. 151-21-3 (detergent solution), 0,1 %, 1 g in 1 000 ml water.

6.10 Dinitrophenylhydrazine (DNPH) solution, CAS no. 119-26-6, consisting of 0,3 g DNPH (2,4-dinitrophenylhydrazine) dissolved in 100 ml acetonitrile (6.8).

7 Apparatus

Use the usual laboratory equipment and, in particular, the following:

7.1 Volumetric flasks, of capacities 10 ml, 500 ml and 1 000 ml.

7.2 Conical flasks with s topper or screw cap, of capacities 100 ml and 250 ml.

7.3 Strainer with glass f ibre filter, GF8 (or glass filter strainer G 3, diameter 70 mm to 100 mm).

7.4 Water bath, thermostatically controlled to (40 ± 2) °C, fitted with a flask shaker, frequency (50 ± 10) r/min.

7.5 Water bath or oven, thermostatically controlled to (50 ± 2) °C.

7.6 HPLC system with UV or DAD detection.

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