GB/T 23276-2009 English PDF (GBT23276-2009)

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GB/T 23276-2009: Method for chemical analysis of palladium compounds -- Determination of palladium content -- Complexometric titration using butanedione dioxide releasing EDTA
GB/T 23276-2009
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 68
Method for chemical analysis of palladium compounds -
Determination of palladium content - Complexometric
titration using butanedione dioxime releasing DETA
ISSUED ON: JANUARY 05, 2009
IMPLEMENTED ON: NOVEMBER 01, 2009
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of PRC;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Principles of the method ... 4 
4 Reagents ... 5 
5 Specimen ... 7 
6 Analytical procedures ... 7 
7 Calculation of analytical results ... 9 
8 Precision ... 9 
Method for chemical analysis of palladium compounds -
Determination of palladium content - Complexometric
titration using butanedione dioxime releasing DETA
1 Scope
This standard specifies the method for the determination of palladium content in
palladium compounds.
This standard applies to the determination of palladium content, in such compounds as
palladium dichloride (PdCl2), palladium bromide (PdBr2), palladium nitrate dihydrate
(Pd(NO3)2 • 2H2O), palladium sulfate (PdSO4), palladium sulfate dihydrate (PdSO4 •
2H2O), chlorodiamine palladium (Pd(NH3)2Cl2), dichlorotetraammonium palladium
(Pd(NH3)4Cl2), potassium chloropalladite (K2PdCl4), dinitrosodiammonia palladium
(Pd(NO2)2(NH3)2), dinitrosotetraammine palladium (Pd(NO2)2(NH3)4), palladium
acetate ([Pd(CH3COO)2]3), bis(acetylacetonate) palladium (Pd(C5H7O2)2), tetra
(triphenylphosphine) palladium (Pd[P(C6H5)3]4), bis(triphenylphosphine) palladium
dichloride (PdCl2[P(C6H5)3]2), 1,2-bis(diphenylene)
(PdCl2[(C6H5)2PCH2CH2P(C6H5)2]), bis[1,2-bis(diphenylphosphine)ethane]palladium
dichloride (PdCl2[(C6H5)2PCH2CH2P(C6H5)2]2). The measurement range is 5% ~ 70%.
2 Normative references
The provisions in following documents become the provisions of this Standard through
reference in this Standard. For the dated references, the subsequent amendments
(excluding corrections) or revisions do not apply to this Standard; however, parties who
reach an agreement based on this Standard are encouraged to study if the latest versions
of these documents are applicable. For undated references, the latest edition of the
referenced document applies.
YS/T 371 Methods for chemical analysis of precious metals alloys - General rules
and regulations
3 Principles of the method
PdCl2 sample is dissolved in hydrochloric acid; PdBr2, Pd(NO3)2 • 2H2O, PdSO4, PdSO4
• 2H2O, Pd(NH3)2Cl2, Pd(NH3)4Cl2, K2PdCl4, Pd(NO2)2(NH3)2, Pd(NO2)2(NH3)4,
Heat at low temperature, until it is completely dissolved. Use water to rinse the watch
glass and the wall of the beaker. Add 5 mL of sodium chloride solution (4.12).
Evaporate at low temperature to wet salt. Add 5 mL of hydrochloric acid (4.5).
Evaporate at low temperature to wet salt. Repeat three times and remove it. Add 250
mL of hydrochloric acid (4.3). Transfer it into a 500 mL volumetric flask. Use water to
dilute it to the mark. Mix well. 1 mL of this solution contains 1 mg of palladium.
4.14 Xylenol orange solution (2 g/L).
4.15 Zinc standard titration solution
4.15.1 Preparation
4.15.1.1 Zinc standard titration solution (0.005 mol/L): Weigh 0.655 g of metallic zinc
(the mass fraction of zinc is not less than 99.99%). Put it in a 150 mL beaker. Add 10
mL of nitric acid solution (4.6). Cover a watch glass. Heat at low temperature, until it
is completely dissolved. Evaporate to about 2 mL. Use water to rinse the watch glass
and the wall of the beaker. Use water to transfer it to a 2000 mL volumetric flask. Use
water to dilute it to the mark. Mix well.
4.15.1.2 Zinc standard titration solution (0.008 mol/L): Weigh 1.048 g of metallic zinc
(with a mass fraction of not less than 99.99%). Place it in a 150 mL beaker. Add 10 mL
of nitric acid solution (4.6). Cover a watch glass. Heat at low temperature, until it is
completely dissolved. Evaporate to about 2 mL. Use water to rinse the watch glass and
beaker wall. Use water to transfer it to a 2000 mL volumetric flask. Use water to dilute
it to the mark. Mix well.
4.15.2 Calibration
Calibration is performed in parallel with the titration of the sample.
Pipette 10.00 mL ~ 20.00 mL of palladium standard solution. Place it in a 300 mL beaker.
Add 2 mL of sodium chloride solution (4.12). Evaporate it to about 1 mL at low
temperature. Add 100 mL of water and 20 mL of EDTA. Add 20 mL of acetic acid-
sodium acetate buffer solution and 7 drops of xylenol orange solution, whilst stirring it.
Add dropwise sodium hydroxide solution, to adjust the pH to about 5.8. Use zinc
standard titration solution (when Pd amount is 10 mg, use 0.005 mol/L zinc standard
titration solution; when Pd amount is 20 mg, use 0.008 mol/L zinc standard titration
solution) for titration, until the solution changes from yellow to red, which is the end
point. Do not count.
Add 7 mL of dimethylglyoxal oxime ethanol solution to the solution, whilst stirring.
Continue stirring for 1 min. Let it stand for 15 min. Add 7 mL of chloroform under
stirring (when the amount of Pd is 20 mg, add 10 mL of chloroform). Continue to stir,
until the solution is clear. Use zinc standard titration solution to titrate it, until the
solution turns from yellow to red, which is the end point.
6.2.1 Dissolution
6.2.1.1 Put the PdCl2 sample in a 150 mL beaker. Add 10 mL of hydrochloric acid
solution (4.5). Cover a watch glass. Heat at low temperature, until it is completely
dissolved. Remove and cool it. Use water to rinse the watch glass and beaker walls.
6.2.1.2 Put the PdBr2, Pd(NO3)2 • 2H2O, PdSO4, PdSO4 • 2H2O, Pd(NH3)2Cl2,
Pd(NH3)4Cl2, K2PdCl4, Pd(NO2)2(NH3)2, Pd(NO2)2(NH3)4, [Pd(CH3COO)2]3,
Pd(C5H7O2)2 samples in a 300 mL beaker. Add 5 mL of nitric acid (4.4). Cover a watch
glass. Heat it at low temperature for about 1 min. Add 10 mL of hydrochloric acid (4.3).
Continue to heat until it is completely dissolved. Use water to rinse the watch glass and
beaker wall.
6.2.1.3 Put the Pd[P(C6H5)3]4, PdCl2[P(C6H5)3]2, PdCl2[(C6H5)2PCH2CH2P(C6H5)2],
PdCl2[(C6H5)2PCH2CH2P(C6H5)2]2 sample in a 300 mL beaker. Add 3 mL of nitric acid
(4.4). Cover a watch glass. Heat at low temperature for 1 min. Add 10 mL of
hydrochloric acid (4.3). Continue to heat, until it is completely dissolved. Use water to
rinse the watch glass and beaker wall.
6.2.2 Treatment of test solution
6.2.2.1 Transfer the test solution (6.2.1.1) into a 100 mL volumetric flask. Use water to
dilute it to the mark. Mix well. Pipette the test solution, which contains 10 mg ~ 20 mg
of palladium. Place it in a 300 mL beaker.
6.2.2.2 Add 2 mL of sodium chloride solution to the test solution (6.2.1.2). Evaporate
at low temperature, until it becomes wet salt. Add 5 mL of hydrochloric acid solution
(4.5). Evaporate it, until it becomes wet salt. Repeat 2 times. When the amount of
palladium is not more than 20 mg, the residue is kept in the original beaker. Add 5 mL
of hydrochloric acid (4.3) to the residue, which has a palladium content not less than
20 mg. Transfer it into a volumetric flask. Use water to dilute it to the mark. Mix well.
Pipette the test solution, which contains 10 mg ~ 20 mg of palladium. Place it in a 300
mL beaker.
6.2.2.3 Add 2 mL of sodium chloride solution to the test solution (6.2.1.3). Evaporate
to about 3 mL at low temperature. Transfer it to a 120 mL separatory funnel. Use 20 mL
of di...