加拿大玩具安全C03 Leachable Metals Applied Coatings 2014-02-20

加拿大消费品安全法案-玩具条例 SOR/2011-17, 测试方法：加拿大产品安全参考手册第5卷,C03：2014版

1 SCOPE 1.1

This method describes a general procedure for the determination of leachable arsenic, selenium, cadmium, antimony and barium in decorative or surface coatings materials applicable to item 23 of the Toys Regulation (SOR/2011-17).

2 APPLICABLE DOCUMENTS 2.1

Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods. Volume 14.02, ASTM E177-90a (1996), pp.79-90.

Standard Practice for Intra laboratory quality Control Procedures and a Discussion on Reporting Low-Level Data. Volume 11.01, ASTM D4210-89, pp.412-419, 1998.

John Keenan Taylor, Quality Assurance of Chemical Measurements. Lewis Publishers, INC. 328 pages, 1987.

National Standard of Canada - Methods of test for toxic trace elements in protective coatings. CGSB Standard Test Method 1-GP-500.2, 1-GP-500.3, 1-GP-500.4, 1-GP-500.5, 1-GP-500.7. Specifications Board. (December, 1973). CGSB Standard Test Method 1-GP-500.2 (December, 1973).

S. Krushkova, “Update of Method C-03, Determination of Leachable Arsenic (As), Selenium (Se), Cadmium (Cd), Antimony (Sb), and Barium (Ba) in Applied Coatings”. Product Safety Laboratory, Project Report No. 2010-1226.

2.2

2.3

2.4

2.5

2.6 A. Babcock, “Development of a Standard Operating Procedure for the Agilent 7700x ICP-MS”

Project Report No. 2010-1249. 2.7

Logbook LBC-55, “Agilent 7500ce ICP-MS with Cetac ASX-500 series Auto Sampler”, and Logbook LBC-56, “Agilent ICP-MS 7700x”.

S. Krushkova, “Update of Method C-03, Determination of Leachable Arsenic (As), Selenium (Se), Cadmium (Cd), Antimony (Sb), and Barium (Ba) in Applied Coatings.” Product Safety Laboratory, Project Report No. 2013-1521.

2.8

加拿大消费品安全法案-玩具条例 SOR/2011-17, 测试方法：加拿大产品安全参考手册第5卷,C03：2014版

3

REAGENTS AND APPARATUS (Note 1)_ 3.1 3.2 3.3

3.4 3.5 3.6 3.7 3.8 3.9 3.10 3.11 3.12 3.13 3.14 3.15 3.16 3.17 3.18 3.19 3.20 3.21 3.22 3.23 3.24 3.25 3.26

Inductively coupled plasma mass spectrometer (ICP-MS), Agilent 7500ce or Agilent 7700x equipped with an internal standards addition Tee/ mixer.

As, Se, Cd, Sb, Ba (+ others) Multi-element Calibration Standard 10.0 ppm ± 0.5%, High Purity or equivalent, traceable to NIST, for calibration.

As, Se, Cd, Sb, Ba (+ others) Multi-element Verification Standard, High Purity

or equivalent traceable t NIST. The calibration and verifications standards should have different lot numbers or manufacturer.

Gallium, Indium and Bismuth standards, 1000 ppm (nominal), SCP Science or equivalent, traceable to NIST, for internal standards Ultra-pure (18.2 MΩ) water

Hydrochloric acid, concentrated (～ 37% w/w), Trace Metal Grade, Fisher Scientific Nitric acid, concentrated (～ 69% w/w), Trace Metal Grade, Fisher Scientific Tetrahydrofuran (THF) HPLC Grade, Caledon Laboratories, Ltd. Scalpel or other suitable scraping tool Electric grinder Mortar and pestle

Air convection oven (60 ± 3 °C) Desiccator

Sieves, 250 and 500μm mesh, Certified service by W.S. Tyler or equivalent. Sample bottles for sieved paint.

Analytical Balance, with a precision of 0.1mg. Weighing vessels. Glass beakers, 50 Ml.

Digital shaker or magnetic stirrer. Filter paper, Whatman No. 40.

Funnels to fit 50 mL flasks or tubes. Volumetric flasks, 50 mL, 2 L.

Sample tubes, screw cap 50mL certified volume.

Pipettes adjustable 10 - 100μL, 100 - 1000μL, 0.500 - 2.50mL, 1.00 - 10.00mL.

NIST SRM 2710 (Montana Soil) or NIST SRM 1633c (Coal Fly Ash), used as a control or equivalent.

Aqua-regia solution for trace metal glassware cleaning.

Note 1: Equivalent materials and apparatus may be used.

加拿大消费品安全法案-玩具条例 SOR/2011-17, 测试方法：加拿大产品安全参考手册第5卷,C03：2014版

4

EXPERIMENTAL PROCEDURE 4.1

Scrape off the applied coating from the test sample with a scalpel, or other suitable scraping tool, being careful not to remove any of the underlying substrate material. Alternatively, the coating (for example: paint on metal surface) can be removed with tetrahydrofuran (THF) or a suitable solvent. Collect into an appropriate weighting vessel, evaporate the solvent from the removed coating and dry in an air convection oven at 60°C ± 3°C for at least 1 hour. This may take several hours. Record the drying time in the oven Log book. Remove the vessel from the oven and cool in a desiccator.

Transfer the removed coating to a mortar and grind the sample with a pestle. An electric grinder may be used when the sample is too difficult to grind with a pestle and a mortar. Sieve the ground coating with a 500μm sieve. The sample passing through the 500μm sieve is then sieved through a 250μm sieve. The portion of the ground coating that passes the

500μm and does not pass the 250μm is used for the leaching test. Place the sieved portion in a weighing vessel and dry to constant weight (to the nearest 1 mg) in an air convection oven at 60°C ± 3°C. This may take about an hour. Record the drying time on the Results of Analysis data sheet (Form C03 F1.1 Sample Data.doc) and on the Constant Weight form (C03 F3.0 Constant Weight.xls). Remove the vessel from the oven and cool in a desiccator. Transfer a sufficient amount (i.e. 5g) of the standard reference material (NIST 2710 or NIST 1633c) to an appropriate vessel. Dry it as required by the certificate of analysis, in an air

convection oven at 60°C ± 3°C for at least 1 hour. Remove the vessel from the oven, cool and store in a desiccator.

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