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GB/T 5121.1-2008 English PDF (GBT5121.1-2008)

GB/T 5121.1-2008 English PDF (GBT5121.1-2008)

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GB/T 5121.1-2008: Methods for chemical analysis of copper and copper alloys -- Part 1: Determination of copper content
GB/T 5121.1-2008
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.30
H 13
Replacing GB/T 5121.1-1996
Methods for chemical analysis of copper and copper
alloys - Part 1: Determination of copper content
(ISO 1554:1976, ISO 1553:1976, Wrought and cast copper alloys and
unalloyed copper containing not less than 99.90% of copper – Determination
of copper content - Electrolytic method, MOD)
ISSUED ON: JUNE 17, 2008
IMPLEMENTED ON: DECEMBER 01, 2008
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3 
1 Method One - Direct electrolysis-atomic absorption spectrometry ... 6 
2 Method Two - Potassium permanganate oxidation of tellurium-electrolysis-
atomic absorption spectrometry ... 11 
3 Method Three - Electrolysis-spectrophotometry ... 16 
Annex A (informative) Control table on clause numbers between Method One
of this Part and ISO 1554:1976 ... 22 
Annex B (informative) Technical differences between Method One of this Part
and ISO 1554:1976 and reasons ... 23 
Annex C (informative) Control table on clause numbers between Method Three
of this Part and ISO 1553:1976 ... 24 
Annex D (informative) Technical differences between Method Three of this Part
and ISO 1553:1976 and reasons ... 25 
Table D.1 -- Technical differences between Method Three of this Part and ISO
1553:1976 and reason ... 25 
Methods for chemical analysis of copper and copper
alloys - Part 1: Determination of copper content
1 Method One -- Direct electrolysis-atomic absorption
spectrometry
1.1 Scope
This Method specifies the determination method of copper content in copper
and copper alloys.
This Method is applicable to the determination of copper content in copper and
copper alloys. The determination range: 50.00%~99.0%.
1.2 Method principle
After the test material is dissolved by nitric acid and hydrofluoric acid, use
hydrogen peroxide to reduce nitrogen oxides. Add lead to reduce the loss of
platinum on the anode. Electrolysis causes copper to precipitate on the
platinum cathode. Weigh after drying the cathode. The amount of copper
remaining in the electrolyte is determined by flame atomic absorption
spectrometry.
1.3 Reagents
Unless otherwise specified, only reagents and distilled water or deionized water
or equivalently pure water that are confirmed as analytically pure are used in
the analysis.
1.3.1 Absolute ethanol.
1.3.2 Hydrofluoric acid (ρ1.13g/mL).
1.3.3 Nitric acid (1+1).
1.3.4 Hydrogen peroxide (1+9).
1.3.5 Ammonium chloride solution (0.02g/L).
1.3.6 Lead nitrate solution (10g/L).
1.3.7 Copper standard stock solution: Weigh 1.0000g of pure copper (the mass
1.6 Analysis steps
1.6.1 Test material
Weigh 2.000g of sample (1.5), to the nearest of 0.0001g.
1.6.2 Determination times
Perform the secondary determination independently. Take the average value.
1.6.3 Blank experiment
Do a blank test with the sample (electrolysis is not necessary).
1.6.4 Determination
1.6.4.1 Place the test material (1.6.1) in a 250mL Teflon beaker. Add 2mL of
hydrofluoric acid (1.3.2), 30mL of nitric acid (1.3.3). Cover the watch glass.
When the reaction is close to the end, heat at no higher than 80°C until the test
material is completely dissolved.
1.6.4.2 Add 25mL of hydrogen peroxide (1.3.4), 3mL of lead nitrate solution
(1.3.6). Use ammonium chloride solution (1.3.5) to wash the watch glass and
beaker wall and dilute to a volume of about 150mL.
1.6.4.3 Mount the platinum anode and the precisely weighed platinum cathode
on the electrolyzer. Soak the net in the solution. Cover the beaker with a split
Teflon dish or polypropylene dish.
1.6.4.4 Electrolyze under stirring (current density 1.0A/dm2) until the color of
copper fades. Use water to wash the watch glass, beaker wall and electrode
rod. Continue electrolysis for 30min. If there is no copper precipitation in the
newly submerged electrode part, it means that the electrolysis is complete.
1.6.4.5 Without cutting off the power, slowly raise the electrode or lower the
beaker. Immediately use two glasses of water to rinse the electrodes in
sequence. Remove the platinum cathode quickly. Dip into two beakers of
absolute ethanol (1.3.1) in turn. Immediately put it into a constant temperature
drying oven at 105°C to dry for 3min~5min. Take it out and put it in a desiccator.
Cool to room temperature and weigh.
1.6.4.6 Transfer the solution (1.6.4.5) after electrolysis of copper and the first
beaker of water (1.6.4.5) that washed the electrode into two 300mL beakers
respectively. Cover the watch glass. Evaporate at low temperature to a volume
of about 80mL. Cool. Combine the solutions and transfer to a 200mL volumetric
flask. Use water to dilute to the scale. Mix well. If the amount of residual copper
is greater than 0.0005g, pipette 25.0ml of solution (1.6.4.6) and place in a 100ml
volumetric flask. Use water to dilute to the scale. Mix well.
The test material is dissolved in nitric acid. Add lead to reduce the loss of
platinum on the anode. Use potassium permanganate to oxidize all tellurium to
hexavalent to prevent tellurium precipitation at the cathode. Electrolyze at
2.0A/dm2. Precipitate copper on the platinum cathode. Weigh after drying the
cathode. The mass of residual copper in the electrolyte is determined by flame
atomic absorption spectrometry.
2.3 Reagents
Unless otherwise specified, only reagents and distilled water or deionized water
or equivalently pure water that are confirmed as analytically pure are used in
the analysis.
2.3.1 Absolute ethanol.
2.3.2 Nitric acid (1+1).
2.3.3 Potassium permanganate solution (20g/L).
2.3.4 Manganese nitrate solution (20g/L).
2.3.5 Lead nitrate solution (10g/L).
2.3.6 Ammonium chloride solution (0.02g/L).
2.3.7 Copper standard stock solution: Weigh 1.0000g of pure copper (the mass
fraction of copper is ≥99.95%) and place it in a 250mL beaker. Add 40mL of
nitric acid (2.3.2). Cover the watch glass. Heat till it is completely dissolved. Boil
to remove nitrogen oxides. Use water to wash the watch glass and beaker wall.
Cool. Move into a 1000mL volumetric flask. Use water to dilute to the scale. Mix
well. 1mL of this solution contains 1mg of copper.
2.3.8 Copper standard solution: Pipette 10.00mL of copper standard stock
solution (2.3.7) and place it in a 500mL volumetric flask. Use water to dilute to
the scale. Mix well. 1mL of this solution contains 20μg of copper.
2.4 Instruments
2.4.1 Electrolyzer equipped with automatic stirring device, precision branch
ammeter and voltmeter.
2.4.2 Electric heating constant temperature drying oven.
2.4.3 Platinum cathode: A platinum wire with a diameter of about 0.2mm is
woven into a mesh of about 36μg per square centimeter. Make it into a net of
cylindrical shape (see Figure 1).
2.4.4 Platinum anode: Spiral (see Figure 2).
oxides. Take it down and cool for a while. Use a small amount of water to wash
the beaker wall and watch glass. Add 3mL of lead nitrate (2.3.5). Dilute the
solution volume with ammonium chloride solution (2.3.6) to about 150mL.
2.6.4.3 Put the magnetic stirring rod into the beaker (2.6.4.2). Place on the
electrolysis instrument tray. Start the mixing device. Stir the solution uniformly
and add 3mL of potassium permanganate solution (2.3.3) and 5mL of <...
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