GB/T 22105.3-2008 English PDF (GB/T22105.3-2008)

GB/T 22105.3-2008: Soil quality -- Analysis of total mercury, arsenic and lead contents -- Atomic fluorescence spectrometry -- Part 3: Analysis of total lead contents in soils
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GB/T 22105.3-2008
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 13.080.05
Z 18
Soil quality - Analysis of total mercury, arsenic and lead
contents - Atomic fluorescence spectrometry - Part 3:
Analysis of total lead contents in soils
ISSUED ON: JUNE 27, 2008
IMPLEMENTED ON: OCTOBER 1, 2008
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 Principles ... 4
3 Reagents ... 4
4 Instruments and equipment ... 6
5 Analysis steps ... 6
6 Result presentation ... 7
7 Precision and accuracy ... 8
8 Notes ... 8
Soil quality - Analysis of total mercury, arsenic and lead
contents - Atomic fluorescence spectrometry - Part 3:
Analysis of total lead contents in soils
1 Scope
This part of GB/T 22105 specifies the atomic fluorescence spectrometry method for the
determination of total lead content in the soil.
This part applies to the determination of total lead content in the soil.
The detection limit of the method of this part is 0.06 mg/kg.
2 Principles
The hydrochloric acid-nitric acid-hydrofluoric acid-perchloric acid total digestion
method is used; the lead in the digested sample reacts with the reducing agent
(potassium borohydride) to generate volatile lead hydride (PbH4). The argon is used as
a carrier to introduce the hydride into an electrothermal quartz atomizer for atomization.
Under the irradiation of a special lead hollow cathode lamp, the lead atoms in the
ground state are excited to a high-energy state; when deactivated and returned to the
ground state, they emit fluorescence at a characteristic wavelength. The fluorescence
intensity is proportional to the content of lead, and finally, the content of lead is
quantitatively calculated according to the standard series.
3 Reagents
Unless otherwise specified, the reagents used in this part are analytical reagents, and
the test water is deionized water.
3.1 Hydrochloric acid (HCl): ρ=1.19 g/mL, guarantee reagent.
3.2 Nitric acid (HNO3): ρ=1.42 g/mL, guarantee reagent.
3.3 Hydrofluoric acid (HF): ρ=1.49 g/mL, guarantee reagent.
3.4 Perchloric acid (HClO4): ρ=1.68 g/mL, guarantee reagent.
3.5 Potassium hydroxide (KOH): guarantee reagent.
3.6 Potassium borohydride (KBH4): guarantee reagent.
3.7 Potassium ferricyanide (K3Fe(CN)6): guarantee reagent.
3.8 Hydrochloric acid solution (1+1): Take a certain volume of hydrochloric acid (3.1)
and add the same volume of water to prepare the solution.
3.9 Hydrochloric acid solution (1+66): Take 1.5 mL of hydrochloric acid (3.1), add
water to make up to 100 mL and mix well.
3.10 Nitric acid solution (1+1): Take a certain volume of nitric acid (3.2) and add the
same volume of water to prepare the solution.
3.11 Oxalic acid solution (100 g/L): Weigh 10 g of oxalic acid, dissolve it in water and
dilute it to 100 mL.
3.12 Potassium ferricyanide solution (100 g/L): Weigh 10 g of potassium ferricyanide
(3.7), dissolve it in water and dilute it to 100 mL.
3.13 Reducing agent [2% potassium borohydride (KBH4) + 0.5% potassium hydroxide
(KOH) solution]: Weigh 0.5 g of potassium hydroxide (3.5), put it into a beaker, and
dissolve it with a small amount of water; weigh 2.0 g of potassium borohydride (3.6),
put it into the potassium hydroxide solution, dissolve it and dilute to 100 mL with water;
prepare this solution for current use.
3.14 Carrier solution: Take 3 mL of hydrochloric acid solution (3.8), 2 mL of oxalic
acid solution (3.11), and 4 mL of potassium ferricyanide solution (3.12), put them into
a beaker, dilute the solution to 100 mL with water, and mix well.
3.15 Lead standard stock solution: Weigh 0.5000 g of spectroscopically pure metal lead,
add a small amount of (1+1) nitric acid solution (3.10) a few times, and if necessary,
heat it until the lead dissolves completely. Transfer the solution to a 500 mL volumetric
flask, dilute to the mark with water, and shake well. The concentration of lead in this
standard solution is 1.00 mg/mL (the able organizations can directly purchase the
standard stock solution from the department recognized by the country).
3.16 Lead standard intermediate solution: Pipette 10.00 mL of lead standard stock
solution (3.15) into a 1000 mL volumetric flask, dilute to the mark with the hydrochloric
acid solution (3.9), and shake well. The concentration of lead in this standard solution
is 10.00 μg/mL.
3.17 Lead standard working solution: Pipette 2.00 mL of lead standard intermediate
solution (3.16) into a 100 mL volumetric flask, dilute to the mark with the hydrochloric
acid solution (3.9), and shake well. The concentration of lead in this standard solution
is 0.20 μg/mL.
GB/T 22105.3-2008
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 13.080.05
Z 18
Soil quality - Analysis of total mercury, arsenic and lead
contents - Atomic fluorescence spectrometry - Part 3:
Analysis of total lead contents in soils
ISSUED ON: JUNE 27, 2008
IMPLEMENTED ON: OCTOBER 1, 2008
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 Principles ... 4
3 Reagents ... 4
4 Instruments and equipment ... 6
5 Analysis steps ... 6
6 Result presentation ... 7
7 Precision and accuracy ... 8
8 Notes ... 8
Soil quality - Analysis of total mercury, arsenic and lead
contents - Atomic fluorescence spectrometry - Part 3:
Analysis of total lead contents in soils
1 Scope
This part of GB/T 22105 specifies the atomic fluorescence spectrometry method for the
determination of total lead content in the soil.
This part applies to the determination of total lead content in the soil.
The detection limit of the method of this part is 0.06 mg/kg.
2 Principles
The hydrochloric acid-nitric acid-hydrofluoric acid-perchloric acid total digestion
method is used; the lead in the digested sample reacts with the reducing agent
(potassium borohydride) to generate volatile lead hydride (PbH4). The argon is used as
a carrier to introduce the hydride into an electrothermal quartz atomizer for atomization.
Under the irradiation of a special lead hollow cathode lamp, the lead atoms in the
ground state are excited to a high-energy state; when deactivated and returned to the
ground state, they emit fluorescence at a characteristic wavelength. The fluorescence
intensity is proportional to the content of lead, and finally, the content of lead is
quantitatively calculated according to the standard series.
3 Reagents
Unless otherwise specified, the reagents used in this part are analytical reagents, and
the test water is deionized water.
3.1 Hydrochloric acid (HCl): ρ=1.19 g/mL, guarantee reagent.
3.2 Nitric acid (HNO3): ρ=1.42 g/mL, guarantee reagent.
3.3 Hydrofluoric acid (HF): ρ=1.49 g/mL, guarantee reagent.
3.4 Perchloric acid (HClO4): ρ=1.68 g/mL, guarantee reagent.
3.5 Potassium hydroxide (KOH): guarantee reagent.
3.6 Potassium borohydride (KBH4): guarantee reagent.
3.7 Potassium ferricyanide (K3Fe(CN)6): guarantee reagent.
3.8 Hydrochloric acid solution (1+1): Take a certain volume of hydrochloric acid (3.1)
and add the same volume of water to prepare the solution.
3.9 Hydrochloric acid solution (1+66): Take 1.5 mL of hydrochloric acid (3.1), add
water to make up to 100 mL and mix well.
3.10 Nitric acid solution (1+1): Take a certain volume of nitric acid (3.2) and add the
same volume of water to prepare the solution.
3.11 Oxalic acid solution (100 g/L): Weigh 10 g of oxalic acid, dissolve it in water and
dilute it to 100 mL.
3.12 Potassium ferricyanide solution (100 g/L): Weigh 10 g of potassium ferricyanide
(3.7), dissolve it in water and dilute it to 100 mL.
3.13 Reducing agent [2% potassium borohydride (KBH4) + 0.5% potassium hydroxide
(KOH) solution]: Weigh 0.5 g of potassium hydroxide (3.5), put it into a beaker, and
dissolve it with a small amount of water; weigh 2.0 g of potassium borohydride (3.6),
put it into the potassium hydroxide solution, dissolve it and dilute to 100 mL with water;
prepare this solution for current use.
3.14 Carrier solution: Take 3 mL of hydrochloric acid solution (3.8), 2 mL of oxalic
acid solution (3.11), and 4 mL of potassium ferricyanide solution (3.12), put them into
a beaker, dilute the solution to 100 mL with water, and mix well.
3.15 Lead standard stock solution: Weigh 0.5000 g of spectroscopically pure metal lead,
add a small amount of (1+1) nitric acid solution (3.10) a few times, and if necessary,
heat it until the lead dissolves completely. Transfer the solution to a 500 mL volumetric
flask, dilute to the mark with water, and shake well. The concentration of lead in this
standard solution is 1.00 mg/mL (the able organizations can directly purchase the
standard stock solution from the department recognized by the country).
3.16 Lead standard intermediate solution: Pipette 10.00 mL of lead standard stock
solution (3.15) into a 1000 mL volumetric flask, dilute to the mark with the hydrochloric
acid solution (3.9), and shake well. The concentration of lead in this standard solution
is 10.00 μg/mL.
3.17 Lead standard working solution: Pipette 2.00 mL of lead standard intermediate
solution (3.16) into a 100 mL volumetric flask, dilute to the mark with the hydrochloric
acid solution (3.9), and shake well. The concentration of lead in this standard solution
is 0.20 μg/mL.