Part B: Test Methods Section, Method C-02.2
Determination of Total Lead in Surface Coating Materials in consumer products 64
1Scope
1.1This method describes a general procedure for the determination of the total
lead content in surface coating materials as applicable to items 2, 9 and 18 of
Part I, and item 31 of Part II of Schedule I to the Hazardous Products Act and
the Surface Coating Materials Regulation (SOR 2005).
2Applicable Documents
2.1N. Ritchot, “Development of a protocol to digest surface coating materiel and
polyvinyl chloride products by block digestion DigiPREP.” Health Canada,
Product Safety Laboratory, Project report no 2008-1046.
2.2 SCP Science DigiPREP instruction manual. Digestion System version 5.
2.3 SCP Science application note: The Determination of Lead, Cadmium and
Cobalt at Low Concentrations in Paint Chips.
3Reagents and Apparatus
3.1Acetone, dichloromethane or other suitable solvent (HPLC grade, Fisher
Scientific)
3.2 Nitric acid 16N, (HNO
3 - Low Trace Metal grade, Fisher Scientific)
3.3Air convection oven
3.4Atomic Absorption Spectrophotometer, SpectrAA 220FS from Varian
3.5Desiccator
3.6Filter paper, Whatman #40 or equivalent
3.7Lead (Pb) certified reference solution, 1000 µg/mL. Certified value (e
Certificate of Analysis)
3.8 Lead (Pb) certified reference solution, 10 µg/mL. Certified value (e
Certificate of Analysis)
3.9 Digestion block SCP Science DigiPREP jr or equivalent
3.10 Scalpel or other suitable scraping tool
3.11 50 mL class A polypropylene DigiTUBE with watch glass
西游记感受3.12 Analytical balance
3.13 NIST2582, Standard Reference Material (SRM). Certified value (e
Certificate of Analysis)
丝毛狗3.14 Foam paint brush or other suitable applicator
3.15 Pipettes, Eppendorf or equivalent
Part B: Test Methods Section, Method C-02.2
Determination of Total Lead in Surface Coating Materials in consumer products 64
3.16 Bottle-top Dispenr 10 mL, Hirschmann Laborgeraete or equivalent春卷的制作方法
4Experimental Procedure
4.1 For liquid paints
4.1.1 Mix the sample thoroughly for at least 5 minutes.
4.1.2 Apply liquid paint on a glass plate with a foam paint brush or other
suitable applicator.
4.1.3 Dry the sample in the convection air oven at 60/C for at least 1 hour.
4.1.4 Scrape off the applied coating from the plate with a scalpel or other
suitable stainless steel blade.
4.1.5 Transfer the recovered coating in a weighing vesl and dry to constant
mass (±2%) in an air convection oven at 60/C for at least 1 hour.
4.1.6 Remove the vesl from the oven and cool to ambient temperature in
a desiccator.
4.2 For applied coatings
4.2.1 Scrape off the applied coating from the article under test with a scalpel
or other suitable scraping tool, being careful not to remove any of the
underlying substrate material. Alternatively, remove the coating with a
suitable solvent2, and collect into a weighing vesl. Evaporate the
心中的你solvent from the removed coating, then dry in an air convection oven
at 60/C for at least 1 hour.
4.2.2 Place the coating in a weighing vesl.
4.2.3 Dry the sample to constant mass (±2%) in an air convection oven at
60°C for at least 1 hour.
4.2.4 Remove the vesl from the oven and cool to ambient temperature in
a desiccator.
4.3 For control samples
Part B: Test Methods Section, Method C-02.2
Determination of Total Lead in Surface Coating Materials in consumer products 64
4.3.1Dry the standard reference material (NIST 2582), as required by the
certificate of analysis, at 60/C for at least 1 hour.
4.3.2 Transfer about 100 mg of the SRM into a digestion tube and weigh to the
nearest 0.1 mg. Prepare this control in duplicate.
4.4For method blanks
4.4.1Prepare a blank sample by adding 2.5 mL of H
2O and 2.5 mL conc.
HNO
3
into a digestion tube.
哥哥的英文4.5DigiPREP digestion
4.5.1 Transfer about 100 mg of the dried coating into a 50 mL DigiTUBE and
weigh to the nearest 0.1 mg.
4.5.2Add 2.5 mL of H
2O, then carefully add 2.5 mL of conc. HNO
3
to the
黑豆功效与作用sample using the Bottle-top dispenr. Cover the tube with a disposable watch glass.
4.5.3 Place the tubes inside the block and install the temperature probe into
the SRM tube.
4.5.4 Digest the sample using the following program variables: PAINT
Time Set point /C
To Temp At temp
1
30
100
4.5.5Following completion of the digestion program, remove the tubes from
the block. Filter the digest solution into a 50 mL polypropylene
DigiTUBE. Rin the digestion tube and the lid into the flask with distilled
water and make up to volume.
4.6 Microwave digestion:
Part B: Test Methods Section, Method C-02.2
Determination of Total Lead in Surface Coating Materials in consumer products 64
4.6.1Transfer about 100 mg of the dried coating into a Teflon ® digestion
vesl and weigh to the nearest 0.1 mg.
4.6.2 Using the Bottle-top dispenr, carefully add 2.5 mL of conc. HNO 3 to
the sample and asmble the digestion vesl and cover fittings with a
single rupture membrane.
4.6.3Place the aled vesl in the turntable inside the microwave cavity and
install the pressure and temperature control system according to the
manufacturer’s instruction.
4.6.4 Ensure that the pressure and temperature nsing tubes do not become
entangled.
4.6.5Digest the sample using the following program variables:Method:
Vesl Type:
哲理诗词
Control style:
PAINT.PGM XP1500Ramp to Temperature Number of Vesls:Volume per Vesl:Sample weight:Acid:122.5 mL 0.1 g HNO 3 , 65%Stage Maximum
Wattage
Power Ramp Time Pressure control Maximum Temp.Stirrer Hold Time 1
1200 W 100%20:00
min 600 psi 210/C 010:00
min 4.6.6 Following completion of the digestion program, allow the vesls to
remain in the microwave oven cavity until the temperature of the sample
is less than 40/C. Direct the vesl vent port away from yourlf and
toward the back of the fume hood, and slowly relea any residual
pressure by gradually looning the vent stem. Carefully open the vesl
and filter the digest solution into a 50 mL class A polypropylene DigiTUBE. Rin the digestion vesl and the lid into the tube with
distilled water and make up to volume.
4.7Prepare an acidic solution of 5% (v/v) of conc. HNO 3. (e.g. 50 mL of conc. HNO 3into a 1 L volumetric flask). Make up to volume with distilled water. This solution
will be ud to prepare standard solutions and dilute samples that are over linear dynamic range.
4.8Prepare a 0.1 µg/mL Pb nsitivity check solution by diluting the 10 µg/mL Pb
standard.
班级德育工作计划Part B: Test Methods Section, Method C-02.2
Determination of Total Lead in Surface Coating Materials in consumer products 64
5Calibration
5.1Prepare a ries of at least three working standard solutions of 0.5, 2.0, 5.0,
10.0 and 20.0 :g/mL Pb by diluting the 1000 :g/mL Pb certified reference
solution in an acidic solution of 5% (v/v) of conc. HNO
3 as prepared in ction
4.6.
5.2Prepare a calibration curve of absorbance versus concentration using the
prepared lead standard solutions.
6Determination
6.1Determine the Pb concentration of the blank solution before and after the
analysis of a digestion batch.
6.2Measure the nsitivity of the instrument with a 0.1 µg/mL Pb before and after
the analysis of a digestion batch.
6.3Measure the Pb concentration for the 10 µg/mL Pb standard before and after the
analysis of each t of 12 digests.
6.4Measure the Pb concentration of the control samples. (NIST 2582)
6.5Determine the Pb concentration in the sample digest solution, as prepared in
ction 4.5.5, using the Atomic Absorption Spectrophotometer operated in flame
mode at a wavelength of 283.3 nm according to the instrument manufacturer's
instructions. If necessary, dilute the sample digest solution with 5% HNO
3, as
prepared in ction 4.6, in order to ensure the measurements are taken within
the range of the calibration curve.
7Calculations and Reporting
