GB/T 17141-1997 PDF English
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| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
| GB/T 17141-1997 | English | 80 |
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Soil quality. Determination of lead, cadmium. Graphite furnace atomic absorption spectrophotometry
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GB/T 17141-1997: Soil quality. Determination of lead, cadmium. Graphite furnace atomic absorption spectrophotometry
---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/GBT17141-1997
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 13.080
Z 18
Soil quality - Determination of lead, cadmium –
Graphite furnace atomic absorption spectrophotometry
Issued on. DECEMBER 8, 1997
Implemented on. MAY 1, 1998
Issued by. Ministry of Environmental Protection of the People’s Republic
of China;
General Administration of Quality Supervision, Inspection and
Quarantine of the People’s Republic of China.
Table of Contents
1 Subject content and scope of application... 3
2 Principle... 3
3 Reagents... 3
4 Instruments... 4
5 Samples... 5
6 Analysis procedures... 5
7 Result representation... 7
8 Precision and accuracy... 7
Annex A (Normative) Determination of the water content in soil sample... 8
Additional information... 9
Soil quality - Determination of lead, cadmium –
Graphite furnace atomic absorption spectrophotometry
1 Subject content and scope of application
1.1 This Standard specifies the graphite furnace atomic absorption
spectrophotometry for determining the lead and cadmium in the soil.
1.2 The detection limit (calculated by digesting 0.5g of test piece to the
constant volume of 50mL) of this Standard is as follows. 0.1 mg/kg, for both
lead and cadmium.
1.3 USE the Zeeman method, self-absorption method and deuterium lamp
method to deduct the background. In the presence of a matrix modifier such as
diammonium hydrogen phosphate or ammonium chloride, directly
DETERMINE the trace lead and cadmium in test solution. There is no
interference.
2 Principle
USE the hydrochloric acid - nitric acid - hydrofluoric acid - perchloric acid full
digestion method to completely destroy the mineral lattices in soil so that all the
elements to be tested in the test pieces can enter into the test solution. INJECT
the test solution into a graphite furnace afterwards. EVAPORATE and REMOVE
the coexisting matrix components by a predetermined temperature rising
program such as drying, ashing and atomization.
3 Reagents
Unless otherwise specified, the analytical reagents and deionized water or
water of equivalent purity, complying with national standards, are used as
reagents in this Standard.
3.1 Hydrochloric acid (HCl), ρ = 1.19 g/mL, guaranteed reagent.
3.2 Nitric acid (HNO3), ρ = 1.42 g/mL, guaranteed reagent.
3.6 Perchloric acid (HClO4), ρ = 1.68 g/mL, guaranteed reagent.
3.7 Aqueous solution of diammonium hydrogen phosphate [(NH4)2HPO4]
(guaranteed reagent), with a weight fraction of 5%.
3.8 Standard lead stock solution, 0.500 mg/mL. Accurately WEIGH 0.5000g
(ACCURATE to 0.0002g) of spectral pure metallic lead. PUT it in a 50mL beaker.
ADD 20mL of nitric acid solution (3.3). Slightly HEAT the solution for dissolution.
After cooling, TRANSFER the solution into a 1,000mL volumetric flask. ADD
water to the scale. SHAKE evenly.
3.9 Standard cadmium stock solution, 0.500 mg/mL. Accurately WEIGH
0.5000g (ACCURATE to 0.0002g) of spectral pure metallic cadmium particles.
PUT them in a 50mL beaker.
3.10 Standard lead and cadmium working mixture, where lead is 250 μg/L and
cadmium is 50 μg/L. Before use, USE nitric acid solution (3.4) to dilute and
prepare the standard lead and cadmium stock solution (3.8) (3.9) step by step.
4 Instruments
4.1 General laboratory instruments and the following instruments.
4.2 Graphite furnace atomic absorption spectrophotometer (with background
subtraction device).
4.3 Lead hollow cathode lamp.
4.4 Cadmium hollow cathode lamp.
4.7 Instrument parameters
The optimal testing conditions for different types of instruments are different. It
is allowed to select by yourselves according to the instrument instruction
manual. For the measurement conditions generally adopted in this Standard,
SEE Table 1.
5 Samples
Evenly MIX the soil samples (generally not less than 500g) taken. USE the
quartering method to divide the samples to 100g or so. CONDUCT air drying
(natural air drying or freeze drying) to the divided soil samples. REMOVE the
foreign matters in the soil, such as stones, animal and plant residues, etc. USE
a wooden stick (or an agate pestle) for milling.
6 Analysis procedures
6.1 Test solution preparation
Accurately WEIGH 0.1g to 0.3g (ACCURATE to 0.0002g) of test pieces. PUT
them in a 50mL teflon crucible. After wetting by using water, ADD 5mL of
hydrochloric acid (3.1). HEAT the test pieces on an electric hot plate in a fume
cupboard at low temperature for preliminary decomposition.
6.2 Determination
ADJUST the instrument to optimal operating conditions according to the
instrument instruction manual. DETERMINE the absorbance of the test solution
afterwards.
6.3 Blank test
USE water to replace the test pieces. USE the same procedures and reagents
as Section (6.1). PREPARE the whole process blank solution. DETERMINE in
accordance with the procedure (6.2). PREPARE at least two portions of blank
solution in each batch of samples.
6.4 Calibration curve
Respectively TRANSFER 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL and
5.00mL of standard lead and cadmium working mixture (3.10) into a 25mL
volumetric flask. ADD 3.0mL of aqueous diammonium hydrogen phosphate
solution (3.7) afterwards.
7 Result representation
The lead and cadmium contents W [Pb (Cd), mg/kg] in soil sample shall be
calculated according to the following equation.
8 Precision and accuracy
Many laboratories use this method to analyze the precision and accuracy of the
lead and cadmium in the ESS series of soil samples. SEE Table 2.
Annex A
(Normative)
Determination of the water content in soil sample
A.1 WEIGH 5g to 10g (ACCURATE to 0.01g) of air-dried soil sample passing
through an 100 mesh sieve. PLACE the soil sample in an aluminum box or
weighing bottle. DRY in a drying oven at 105°C for 4h to 5h, until the soil sample
comes up to constant weight.
A.2 The water content in air-dried soil sample f expressed as percentage shall
be calculated according to the following equation.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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