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Determination of lead, iron, titanium, copper, manganese, zinc, chromium, aluminium content in quartz sand. Inductively couple plasma atomic emission spectrometric method
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SN/T 3365-2012: PDF in English (SNT 3365-2012) SN/T 3365-2012
SN
ENTRY & EXIT INSPECTION & QUARANTINE STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
Determination of lead, iron, titanium, copper,
manganese, zinc, chromium, aluminum content in
quartz sand - Inductively couple plasma atomic
emission spectrometric method
ISSUED ON: DECEMBER 12, 2012
IMPLEMENTED ON: JULY 01, 2013
Issued by: General Administration of Quality Supervision Inspection and
Quarantine of PRC
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Method summary ... 4
4 Reagents and materials ... 4
5 Instruments and equipment... 5
6 Specimen ... 6
7 Analytical procedures ... 6
8 Result calculation ... 7
9 Precision ... 7
Appendix A (Informative) Instrument working conditions and element analysis
line wavelength parameters ... 8
Determination of lead, iron, titanium, copper,
manganese, zinc, chromium, aluminum content in
quartz sand - Inductively couple plasma atomic
emission spectrometric method
1 Scope
This standard specifies the inductively coupled plasma emission spectrometry
method for the determination of lead, iron, titanium, copper, manganese, zinc,
chromium, aluminum in quartz sand.
This method is suitable for the determination of lead, iron, titanium, copper,
manganese, zinc, chromium, and aluminum in quartz sand. The detection limits
of each element are: lead 0.57 μg/g; iron 0.67 μg/g, titanium 0.88 μg /g; copper
0.24 μg/g; manganese 0.25 μg/g; zinc 0.35 μg/g; chromium 0.29 μg/g;
aluminum 0.56 μg/g.
2 Normative references
The following documents are essential to the application of this document. For
the dated documents, only the versions with the dates indicated are applicable
to this document; for the undated documents, only the latest version (including
all the amendments) are applicable to this standard.
GB/T 6682 Water for analytical laboratory use - Specification and test
methods
3 Method summary
The sample is dissolved with hydrofluoric acid and perchloric acid, heated and
evaporated to dryness until the white smoke of perchloric acid is exhausted; the
residue is dissolved with dilute nitric acid, measured by inductively coupled
plasma emission spectrometer.
4 Reagents and materials
Unless otherwise specified, only use premium grade pure reagents and grade-
5.2 Crucible: Platinum crucible or platinum-gold crucible (95% Pt + 5% Au).
5.3 Electric heating plate: It can be heated to 300 °C; temperature control
accuracy is ±5 °C.
5.4 Analytical balance: Sensitivity is 0.1 mg.
5.5 Agate mortar.
6 Specimen
Weigh about 20 g of specimen in a weighing bottle. Place the specimen in an
oven at 105 °C for 2 hours. Take it out. Cool in a desiccator. Use an agate
mortar (5.5) to grind the dried specimen, until all specimen passes through a
0.08 mm (200 mesh) square-hole sieve. Put the specimen into a sample bottle
for analysis.
7 Analytical procedures
7.1 Sample digestion
Accurately weigh 1.0 g of sample (accurate to 0.1 mg) into the crucible (5.2).
Add 15 mL of hydrofluoric acid (4.3) and 0.5 mL of perchloric acid (4.1). Use
the temperature-controlled electrical heating plate to heat it. Set the
temperature to 250 °C. When it evaporates to near dryness, remove it and cool
it slightly. Add 3 mL of hydrofluoric acid (4.3). Heat and evaporate until the
perchloric acid white smoke is exhausted. Remove it and cool it slightly. Use 10
mL of diluted nitric acid (4.4) to rinse the inner wall of the crucible. Place it on
an electrical heating plate and heat it until it boils. Take it off. Cool it to room
temperature. Transfer the solution to a 50 mL volumetric flask. Use water to
dilute it. Mix it uniformly to prepare for determination.
Carry out a blank test together with the sample.
7.2 Determination
Use the 5% nitric acid solution (4.5) to dilute the mixed standard working
solution (4.14) gradually to a series of standard solutions which have
concentration of 0.0 μg/mL, 0.5 μg/mL, 2.0 μg/mL, 5.0 μg/mL, 10.01 μg/mL.
Refer to Appendix A to set the working conditions of the instrument. After the
instrument is stable, measure the spectral intensity of each element to be tested
in the series of standard solutions in the order of concentration from low to high
at the corresponding wavelength. Use the spectral intensity as the ordinate and
element concentration as the abscissa, to draw a working curve.
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Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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