ForewordHauptteilScopeNormative referencesTypesRequirementsAllowable limits of extractable substances from the glovesHeavy metalsPhthalate contentSample preparationDetermination of heavy metalsDetermination of potassium permanganate consumption and the evaporation residueDetermination of the phthalate contentProvision for useLabelling and markingDetermination of heavy metals (normative)PrincipleApparatusReagentsStandard solutionsLaboratory reagent blankDeterminationGeneralSet up the instrument with proper operating parameters established from the manufacturer’s instruction manual. Allow the instrument to achieve thermal stability before beginning. Instructions provided by the manufacturer should be followed.Initiate the appropriate operating configuration of the computer.Profile and calibrate the instrument according to the manufacturer’s recommended procedures using the standard solutions (A.4).Begin the sample run by flushing the system with the reagent blank (A.5) between each sample.Recommended wavelengths and important spectral interferencesLimit of detectionThe limit of detection, expressed as the concentration or the quantity, is derived from the smallest measure that can be detected with reasonable certainty for a given analytical procedure (IUPAC).The limit of detection (LOD) shall be calculated using Formula (A.1):Actual working detection limits are dependent on the type of instrumentation, detection device and sample introduction system used, and on the sample matrix. Therefore, these concentrations can vary between different instruments.Expression of resultsDetermination of potassium permanganate consumption (normative)PrincipleApparatusReagentsStandard solutionsDeterminationExpression of resultDetermination of evaporated residue (normative)PrincipleApparatus ReagentsDeterminationExpression of resultDetermination of phthalate content (normative)PrincipleApparatusReagentsStandard solutionsDeterminationSampling, extraction, and gravimetric analysis for phthalate plasticisersPlace the sample in a pre-weighed 150 ml flat bottom flask and heat in an oven at (105 ± 5) °C for (30 ± 5) min. Allow to cool in a desiccator.Weigh the flask and sample. Use a scalpel or other appropriate cutting utensil to cut a representative portion from the sample into small pieces, Φ < 5 mm.Weigh accurately (2 ± 0,2) g of the pieces into a Soxhlet thimble and add cotton wool to the top of the thimble.Add approximately (50 ± 10) ml of diethyl ether into the flask. Reflux gently for 6 h ± 30 min. Allow sufficient time for the diethyl ether to cool.Evaporate the diethyl ether completely by mean of steam bath.Place the flask in an oven at (105 ± 5) °C for (30 ± 5) min. Allow to cool in a desiccator and weigh.Repeat the drying and cooling cycles until the difference between two consecutive weighings are not more than 0,0005 g. A blank solution shall be run consecutively.Preparation of sample extract solution for gas chromatography-mass spectrometry (GC-MS)To the weighed extract (D.5.1), add (50 ± 2) ml of n-hexane.Place a stopper to the flask and swirl to completely dissolve the extract.Decant the solution into a 200 ml volumetric flask, repeatedly rinsing the flask with n-hexane.Add n-hexane to the volumetric flask to bring the total volume to 200 ml.Prepare (if necessary) further diluted solutions using n-hexane such that the final concentration in solution is within the linear calibration concentration for phthalate present.Transfer a portion of the n-hexane solution into a capped vial for GC-MS analysis.The samples can be analysed for phthalate plasticisers by conditioning the GC-MS as follows.Expression of resultsPrecision (informative)GeneralDetails of test programmesPrecision resultsBibliography