GB/T 5121.1-2008 PDF English
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Methods for chemical analysis of copper and copper alloys -- Part 1: Determination of copper content
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Copper and copper alloys--Determination of copper content
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Methods for chemical analysis of copper--The electrolytic method for the determination of copper content
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GB/T 5121.1-2008: Methods for chemical analysis of copper and copper alloys -- Part 1: Determination of copper content
---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT5121.1-2008
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
manganese nitrate solution (2.3.4) dropwise under stirring.
2.6.4.4 Mount the platinum anode and platinum cathode on the electrolyzer.
Soak the net in the solution. Cover the tall beaker with two half-piece watch
dishes.
2.6.4.5 Stir and electrolyze the solution at a current density of about 2.0A/dm2
on the surface of the cathode until the solution is colorless. Use water to wash
the watch glass, beaker wall and electrolysis rod. Reduce the current density to
1.0A/dm2 and continue electrolysis. If there is no copper precipitation in the
newly immersed electrode part, it means that the electrolysis is complete (about
1h).
2.6.4.6 Without cutting off the power, slowly raise the electrode or lower the
beaker. Immediately use two glasses of water to rinse the electrode. Remove
the platinum cathode quickly. And immerse them in two beakers of absolute
ethanol (2.3.1). Immediately put it into a constant temperature drying oven at
105°C to dry for 3min~5min. Take it out and place in a desiccator to cool to
room temperature.
2.6.4.7 Weigh the electrolytically deposited platinum cathode with the original
balance (2.6.4.6).
2.6.4.8 Evaporate the copper solution (2.6.4.5) and the first beaker of electrode
washing water (2.6.4.6) to a volume of about 80mL at low temperature. Cool.
Combine the solutions and transfer to a 200mL volumetric flask. Use water to
dilute to the scale. Mix well. If the residual copper is greater than 0.0005g,
pipette 25.0mL of the solution (2.6.4.8). Put it in a 100mL volumetric flask. Use
water to dilute to the scale. Mix well.
2.6.4.9 Use air-acetylene flame, in atomic absorption spectrometer, at a
wavelength of 324.7nm, with standard solution series at the same time, use
water to zero and adjust the absorbance of the test solution. The measured
absorbance is subtracted from the absorbance of the blank solution with the
test material, and the corresponding copper mass concentration is found from
the working curve.
2.6.5 Drawing of working curve
2.6.5.1 Pipette 0ml, 2.50mL, 5.00mL, 7.50mL, 10.00mL, 12.50mL of copper
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.
3.3.1 Absolute ethanol.
3.3.2 Nitric acid (1+1).
3.3.3 Ammonia (1+1).
3.3.4 Mixed acid. 7 unit-volume of nitric acid (ρ1.42g/mL), 10 unit-volume of
sulfuric acid (ρ1.84g/mL) and 25 unit-volume of water are mixed well. Cool.
3.3.5 Mixed acid. Take 42mL of mixed acid (3.3.4) in a 500mL volumetric flask.
Use water to dilute to the scale. Mix well.
3.3.6 Ammonium citrate solution (500g/L).
3.3.7 Bis (cyclohexanone) oxaldihydrazone (BCO) (1g/L). Weigh 0.5g of BCO
in a 300ml beaker. Add 50mL of absolute ethanol (3.3.1), 200mL of warm water
to dissolve. Move into 500mL volumetric flask. Use water to dilute to the scale.
Mix well.
3.3.8 Neutral red ethanol solution (1g/L).
3.3.9 Copper standard storage solution. Weigh 0.1000g of pure copper (the
mass fraction of copper ≥99.95%) and place it in a 150mL beaker. Add 10mL of
nitric acid (3.3.2). Heat at low temperature to dissolve completely. 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 100μg of copper.
3.3.10 Copper standard solution. Pipette 10.00mL of copper standard stock
solution (3.3.9) into a 100mL volumetric flask. Use water to dilute to the scale.
Mix well. 1mL of this solution contains 10μg of copper.
3.4 Instruments
3.4.1 Electrolyzer equipped with automatic stirring device, precision branch
ammeter and voltmeter.
3.4.2 Electric heating constant temperature drying oven.
3.4.3 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).
3.4.4 Platinum anode. Spiral (see Figure 2).
electrode rod newly submerged in water no longer deposits copper.
3.6.3.5 Without cutting off the power supply, quickly remove the tall beaker and
replace it with a tall beaker containing about 180mL of water. Continue
electrolysis for 15min.
3.6.3.6 Immediately extract the platinum cathode and immerse it in another
250mL beaker filled with water. Move up and down 3 times. Turn off the power
and remove the electrodes. Put it in a beaker that is filled with absolute ethanol.
After taking it out, put it in a 105°C electric heating constant temperature drying
oven to dry for 3min~5min. Take out and place in a desiccator to cool to room
temperature.
3.6.3.7 Weigh the platinum cathode after electrolytic deposition with the original
balance (3.6.3.6).
3.6.3.8 Determine the amount of residual copper in the solution after
electrolysis as follows.
3.6.3.8.1 Blank test
Pipette the same mixed acid (3.3.4) as the test material solution into a 50mL
volumetric flask. Conduct the blank test with test material.
3.6.3.8.2 Combine the electrolyzed electrolyte with a glass of water that has
been electrolyzed for 15min. Place in a 500mL volumetric flask. Use water to
dilute to the scale. Mix well.
3.6.3.8.3 Pipette 10.00mL~20.00mL into a 50mL volumetric flask. Add 2mL of
ammonium citrate solution (3.3.6). Use water to dilute to 25mL. Add 2~3 drops
of neutral red ethanol solution (3.3.8). Neutralize with ammonia solution (3.3.3)
until the red solution fades and there is an excess of 1.0mL. Add 8.0mL of Bis
(cyclohexanone) oxaldihydrazone solution (3.3.7). Use water to dilute to the
scale. Mix well. Place still 20min.
3.6.3.8.4 Transfer part of the solution into a 2cm absorption dish. Take the blank
solution accompanying the test material as a reference. Measure absorbance
at 600nm wavelength of spectrophotometer. Find the mass of the
corresponding copper from the working curve.
3.6.3.9 Drawing of working curve
3.6.3.9.1 Pipet 6 portions of 20.0mL of mixed acid (3.3.5) in a set of 50ml
volumetric flasks. Add 0mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL of
copper standard solution (3.3.10) respectively. The following shall proceed
according to "add 2mL of ammonium citrate solution" in 3.6.3.3.
3.6.3.9.2 Transfer part of the solution into a 2cm absorption dish. Take reagent
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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