The U.S. Consumer Product Safety Commission (CPSC) published the standard “CPSC-CH-C1001-09 Standard Operating Procedure for Determination of Phthalates,” which describes test methods to be used to analyze phthalate content in children’s toys and child care products covered by the Consumer Product Safety Improvement Act, Part 108, and the standard specified in 16 CFR Part 1307. It has been determined that using an appropriate combination of extraction and analysis methods presented herein is sufficient to determine the concentration of eight regulated phthalates in most consumer products. Adjustments may be required for products made from certain materials and should be based on sound chemistry and materials science knowledge and appropriate solvents for the materials. The general approach is to completely dissolve the sample in tetrahydrofuran, precipitate any dissolved polymer with a second solvent, and then analyze by gas chromatography-mass spectrometry (GC-MS).
The procedure for measuring phthalate concentration consists of three parts: sample preparation, extraction, and analysis. In addition to the procedure described here, certain alternative methods listed below are acceptable for phthalate content certification testing. However, some methods may require adaptation to be adequate. Most importantly, some methods do not specifically include all phthalates regulated for use in children's toys and child care products in the United States. Therefore, the methods should be modified to include all phthalates of concern.
The following independent methods are acceptable for phthalate content certification testing and require no adaptation beyond including all phthalates of interest:
The following methods are only suitable for the extraction part of the certification test. They should be combined with an independent method listed above or with an analysis method only in the following standards:
These methods require the use of hazardous materials. It is extremely important that all hazardous materials are handled properly and safely in a ventilated extractor cabinet with adequate personal protective equipment.
Phthalates are a common contaminant. Even low levels of contamination can affect quantitative results. Plastics should be avoided and only meticulously cleaned glassware and equipment should be used. All solvents should be tested for any phthalate content. Solvent blanks should be subjected to periodic GC-MS to monitor for possible contamination. Disposable glassware is recommended whenever possible.
Before analysis, each piece of plasticized component shall be cut into small pieces (not larger than 2 mm in size) or ground into a representative powder. Each piece of plasticized component that is cut or ground shall be considered a sample for testing. At least the amount required to form a sufficient sample size shall be prepared.
In the phthalate removal method, the testing laboratory determines how many replicate samples are needed to meet quality assurance requirements. A laboratory reagent blank is prepared simultaneously with the samples. Benzyl benzoate is added directly to the precipitation solvent (choice of acetonitrile or hexane) to obtain a concentration of 30 μg/mL for use as an internal standard.
A minimum of 0,05 g plus/minus 0,005 g of sample is weighed into a sealable glass vial (to an accuracy of plus/minus 0,5 percent); if the sample is not uniform, more is collected to reduce sample variance.
Add 5 mL of tetrahydrofuran to the sample. For samples greater than 0,05 g, add 0,1 mL of tetrahydrofuran for every 10 g of sample (or a reasonable amount to dissolve the sample). Shake or stir the sample for at least 30 minutes to ensure dissolution. Some materials may not dissolve completely. In this case, add another 2 hours to the mixing time and then continue.
Precipitate any PVC polymer with 5 mL of acetonitrile or hexane for every 10 mL of tetrahydrofuran used. Shake vigorously and wait at least 5 minutes for the polymer to precipitate.
Transfer the supernatant solution to a GC vial for analysis. If hexane was used in the above step, it is recommended to filter the supernatant solution through a 0,45 pm PTFE (teflon) filter before transfer.
A GC-MS system with an autosampler is recommended for sample analysis. Corresponding instrumentation such as GC or liquid chromatography (LC) with advanced MS options (e.g. ion trap or tandem mass spectrometry) can be used for qualitative assessment. GC conditions are shown in the table provided in the standard.
Our organization, which has been trying to support businesses from every sector with its testing, measurement, analysis and evaluation studies carried out in a wide range for years, has a strong staff that closely follows the developments in the world in the field of science and technology and constantly improves itself. In this context, testing services in accordance with the "CPSC-CH-C1001-09 Standard Operating Procedure for the Determination of Phthalates" standard are also provided to businesses.
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