GMW-15635-2007.pdf
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1、 WORLDWIDE ENGINEERING STANDARDS Test Procedure Materials GMW15635 Determination of Aldehyde and Ketone Emissions from Interior Materials Copyright 2007 General Motors Corporation All Rights Reserved December 2007 Originating Department: North American Engineering Standards Page 1 of 8 1 Scope Note:
2、 Nothing in this standard supersedes applicable laws and regulations. Note: In the event of conflict between the English and domestic language, the English language shall take precedence. 1.1 Purpose. This test procedure describes a measuring process for determining the aldehyde and ketone emissions
3、 from vehicle interior materials. 1.1.1 For this test, test pieces are fastened above demineralized water in a sealed bottle and stored in an oven for a specific period. Afterwards, the bottles are cooled, and the aldehydes and ketones absorbed in the demineralized water are determined. 1.1.2 The co
4、ncentrations of aldehydes and ketones are determined by derivatization with 2,4-dinitrophenylhydrazine (DNPH) followed by high performance liquid chromatography (HPLC) with ultraviolet (UV) detection. 1.1.3 The quantity of aldehydes and ketones are ascertained as a proportion of the dry weight g/g o
5、f the test piece. 1.2 Foreword. The determination of aldehydes and ketones in vehicle materials and components is essential to meet customer requirements and regulatory requirements in some global markets. 1.3 Applicability. This test procedure is applicable to all solid polymer materials and compon
6、ents used in vehicle interiors. The results will provide complementary information to GMW14444. 2 References Note: Only the latest approved standards are applicable unless otherwise specified. 2.1 External Standards/Specifications. DIN 55531 ISO/IEC 17025 ISO 16979 2.2 GM Standards/Specifications. G
7、MW14444 3 Resources 3.1 Facilities. Not applicable. 3.2 Equipment. This test procedure utilizes commonly available equipment and instrumentation. Specific instrumentation and test conditions are noted in the Appendix. 3.2.1 Test Apparatus. 3.2.1.1 Precision weighing device with scale gradation 1 mg.
8、 3.2.1.2 Air circulating oven capable of maintaining the required temperature to within 2C. 3.2.1.3 1 L polyethylene bottle with hook implement integrated in the lid (see Figure 1). 3.2.1.4 High performance liquid chromatograph with binary pump, solvent degasser, heated column compartment, autosampl
9、er (optional), variable wavelength or diode array detector, and PC-based controller and data evaluation. System must be capable of gradient operation to 3.5 mL/minute and 350 bar (max), and UV detection at 360 to 365 nm. 3.2.1.5 HPLC column capable of separating the 2,4-dinitrophenylhydrazine (DNPH)
10、 derivatives of the specified aldehydes/ketones using gradient elution conditions. The column is critical for this procedure. (e.g., Agilent 1100 Series and Agilent ChemStation for system control and data evaluation, ). 3.2.2 Reagents. 3.2.2.1 Acetonitrile. HPLC grade 3.2.2.2 Tetrahydrofuran. HPLC g
11、rade, no antioxidant 3.2.2.3 Water. HPLC grade 3.2.2.4 Phosphoric Acid. Concentrated, reagent grade 3.2.2.5 Derivatizing Reagent. 3.2.2.5.1 DNPH-Solution. Approximately 250 mg of 2,4-dinitrophenylhydrazine (DNPH) are dissolved in 50 mL of acetonitrile. 3.2.2.6 Calibration standards containing the co
12、mponents of interest already derivatized in appropriate concentration range, typically 0.1 g/mL to 15 g/mL in acetonitrile. GMW15635 GM WORLDWIDE ENGINEERING STANDARDS Copyright 2007 General Motors Corporation All Rights Reserved Page 2 of 8 December 2007 3.2.2.6.1 Calibration standards are availabl
13、e from: Cerilliant: ERA-037, ERA-13K, ERA-028, 13 components in acetonitrile, 1 g/mL to 15 g/mL of each component as aldehyde/ketone, () Supelco: TO11/IP-6-A Carbonyl-DNPH-Mix, 15 components in acetonitrile, 15 g/mL of each component (aldehyde equivalent), Sigma-Aldrich (Supelco), 47285-U. 3.3 Test
14、Vehicle/Test Piece. 3.3.1 Test Sample handling and preparation. If possible, shall be taken out of the finished part of the material or the component. 3.3.1.1 In exceptional cases (e.g., if only one material of a component is to be tested, or if the complete component is not available) tests can be
15、conducted on specially prepared parts. 3.3.1.2 The sample should be taken within 7 days after production. Date of production and sampling should be documented. Care should be taken to prevent material from thermal desorption before analysis (package, refrigerate). 3.3.1.3 Representative sample of th
16、e material is to be used (smaller samples have to cut out from large components to a size of 10 cm x 15 cm. The sample shall be handled with protective gloves and the cutting shall be done with an oil-free tool such as a disposable razor blade. The sample should be packed by aluminum composite films
17、 (e.g,. VACUPAC, or any other material according to DIN 55531) prior to shipping. In the exceptional case, the sample can be packed twice into thick silicone-free aluminum foil (cleaned with n- pentane). The edges should be folded multiple times to prevent contamination from outside and to ensure an
18、 air-tight packing. The aluminum foil packed sample should than be packed additionally and placed in a polyethylene bag. The bag shall be labelled with sample ID number; final sample name (cannot be changed afterwards), production date and date of sampling shall be record in the data sheet in Append
19、ix D. If this information is missing, the sample should not be analyzed. 3.3.2 Taking of Test Pieces. The test pieces shall be taken from suitable and representative points spread evenly across the width of the part. They must be taken 50 mm from the edge of the part. 3.3.3 The size of each test pie
20、ce is nominally 40 mm x 100 mm x thickness. If the size of the molded part is smaller or the distance of 50 mm to the edge of the part is not possible, this test may also be performed using smaller test pieces. Here, care must be taken to ensure that all the edges of test pieces are freshly cut. To
21、fasten the test piece, a hole corresponding to the diameter of the hook is drilled near its center, 10 mm from the upper edge. 3.3.3.1 For small parts, at least three (3) samples must be taken from each part. Two (2) parts are used for determining aldehydes/ketones and one (1) part is used to determ
22、ine the moisture content. 3.3.4 If the testing of the sample cannot take place immediately, they must be stored in cool, air-tight conditions with a minimal air volume. Storage time should not exceed 5 days. 3.4 Test Time. Sampling of the test pieces requires 3 h in the oven and 1 h of cool down. Sa
23、mpling is best conducted for several materials in parallel in individual bottles in the oven. The determination of aldehydes/ketones by derivatization and HPLC is conducted serially with each sample requiring 30 5 minutes. Calendar time: Not applicable Test hours: Not applicable Coordination hours:
24、Not applicable 3.5 Test Required Information. Material component information such as vendor name, production date, pretreatment, etc., should be recorded in the data report sheet in Appendix D. 3.6 Personnel/Skills. Proper training is required to process the samples and operate the HPLC instrument.
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