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GB/T 32794-2016 (GB/T32794-2016)

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GB/T 32794-2016: PDF in English (GBT 32794-2016)
GB/T 32794-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.100
H 11
Pig iron contenting nickel - Determination of nickel,
cobalt, chromium, copper, phosphorus content -
Inductively coupled plasma atomic emission
spectrometry
ISSUED ON: AUGUST 29, 2016
IMPLEMENTED ON: JULY 01, 2017
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 Principle ... 5 
4 Reagents ... 5 
5 Instruments ... 7 
6 Sampling and sample preparation ... 9 
7 Analytical procedures ... 9 
8 Calculation of results ... 10 
9 Tolerance ... 11 
10 Test report ... 11 
Appendix A (Normative) Standard operation of measuring instrument ... 13 
Pig iron contenting nickel - Determination of nickel,
cobalt, chromium, copper, phosphorus content -
Inductively coupled plasma atomic emission
spectrometry
Warning -- The personnel using this standard shall have practical
experience in formal laboratory work. This standard does not point out all
possible safety issues. The user is responsible for taking appropriate
safety and health measures AND ensuring compliance with the conditions,
which are stipulated by relevant national laws and regulations.
1 Scope
This standard specifies the determination of nickel, cobalt, chromium, copper,
phosphorus content, by the inductively coupled plasma atomic emission
spectrometry.
This standard applies to the determination of the content of nickel, cobalt,
chromium, copper, phosphorus in pig iron contenting nickel. The content range
of the determined element is as shown in Table 1.
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) is applicable to this standard.
GB/T 4010 Ferroalloys sampling and preparation of samples for chemical
temperature). Place it in a 250 mL beaker. Add 120 mL of nitric acid (2 + 3).
Cover a watch glass. Heat to dissolve completely. Cool to room temperature.
Transfer it into a 1 L volumetric flask. Use water to dilute it to the mark. Mix well.
1 mL of this solution contains 4 mg of nickel.
4.10 Cobalt standard solution:
4.10.1 Cobalt standard solution, 1 mg/mL.
Weigh 1.0000 g of metallic cobalt (above 99.99%) in a 250 mL beaker. Add 40
mL of nitric acid (1 + 1). Heat to dissolve it completely. Cool to room temperature.
Transfer it into a 1 L volumetric flask. Use water to dilute it to the mark. Mix well.
1 mL of this solution contains 1 mg of cobalt.
4.10.2 Cobalt standard solution, 200 μg/mL.
Pipette 20.00 mL of cobalt standard solution (4.10.1) in a 100 mL volumetric
flask. Use water to dilute it to the mark. Mix well. 1 mL of this solution contains
200 μg of cobalt.
4.11 Chromium standard solution, 1 mg/mL.
Weigh 2.8289 g of reference potassium dichromate (baked at 180 °C for 1 h in
advance, placed in a desiccator, cooled to room temperature). Put it in a 250
mL beaker. Add appropriate amount of water to dissolve it. Transfer it into a 1 L
volumetric flask. Use water to dilute it to the mark. Mix well. 1 mL of this solution
contains 1 mg of chromium.
4.12 Copper standard solution:
4.12.1 Copper standard solution, 1 mg/mL.
Weigh 1.0000 g of pure copper (above 99.99%, stored in a desiccator at room
temperature). Place it in a 250 mL beaker. Add 30 mL of nitric acid (1 + 1). Heat
to dissolve it, at low temperature. Cool to room temperature. Transfer it into a 1
L volumetric flask. Use water to dilute it to the mark. Mix well. 1 mL of this
solution contains 1 mg of copper.
4.12.2 Copper standard solution, 100 μg/mL.
Pipette 10.00 mL of copper standard solution (4.12.1), in a 100 mL volumetric
flask. Use water to dilute it to the mark. Mix well. 1 mL of this solution contains
100 μg of copper.
4.13 Phosphorus standard solution:
4.13.1 Phosphorus standard solution, 1 mg/mL.
Weigh 4.3940 g of reference dipotassium hydrogen phosphate (dried in
advance at 105 °C to a constant amount). Place it in a 250 mL beaker. Add an
appropriate amount of water to dissolve it. Transfer it into a 1 L volumetric flask.
Use water to dilute it to the mark. Mix well. 1 mL of this solution contains 1 mg
of phosphorus.
4.13.2 Phosphorus standard solution, 20 μg/mL.
Pipette 2.00 mL of phosphorus standard solution (4.13.1), in a 100 mL
volumetric flask. Use water to dilute it to the mark. Mix well. 1 mL of this solution
contains 20 μg of phosphorus.
4.14 Reagent blank stock solution:
Weigh 2.5 g of ammonium fluoride. Place it in a 500 mL beaker. Add 20 mL of
water and 40 mL of perchloric acid. Heat it, until white smoke is generated.
Remove and cool it. Add 50 mL of hydrochloric acid (1 + 1). Heat to boil.
Remove and cool to room temperature. Transfer it into a 500 mL volumetric
flask. Use water to dilute it to the mark. Mix well.
5 Instruments
In addition to the usual laboratory instruments and equipment, an inductively
coupled plasma atomic emission spectrometer is used in the analysis. A high-
salt atomizer is equipped, if necessary. After optimization, the instrument shall
meet the following requirements:
5.1 General requirements
Initially adjust the inductively coupled plasma atomic emission spectrometer,
according to the recommendations of the instrument manufacturer AND the
requirements of laboratory analysis.
5.2 Actual resolution of instrument
Calculate the bandwidth of each used analysis line; the bandwidth shall be less
than 0.030 nm.
5.3 Analytical spectral lines
This standard does not specify a special analysis line. The recommended
analysis line is as listed in Table 2. During use, it shall check the interference of
the spectral lines.
6 Sampling and sample preparation
Take samples in accordance with the provisions of GB/T 4010. All the easy-to-
break specimens shall pass through 0.125 mm sieve holes. All the hard-to-
break specimens (drilled) shall also pass through 1.60 mm sieve holes; take
the specimens above the 0.154 mm sieve.
7 Analytical procedures
7.1 Sample amount
Weigh 0.20 g of sample, accurate to 0.0001 g.
7.2 Blank test
Pipette an iron solution (4.8), which contains similar amount of iron in the
sample. Do a blank test with the sample.
7.3 Decomposition of sample
7.3.1 Place the sample (7.1) in a 250 mL polytetrafluoroethylene beaker. Add
10 mL of ammonium fluoride solution (4.7). Let it stand for 2 min ~ 3 min. Add
20 mL of nitric acid (4.3) and 10 mL of hydrochloric acid (4.2). Slowly heat to
dissolve. Then add 8 mL of perchloric acid (4.4). Continue to heat, until the
beaker is just filled with white smoke. Immediately remove it and cool it slightly.
Add 20 mL of water and 10 mL of hydrochloric acid (4.6). Heat to boil it. Cool it
to room temperature. Transfer it into a 200 mL volumetric flask. Use water to
dilute it to the mark. Mix well. Filter it under dry state.
7.3.2 If the sample is not completely dissolved, follow step of 7.3.1, until the
procedure that "Add 20 mL of water and 10 mL of hydrochloric acid (4.6). Heat
to boil it. Cool it to room temperature". Use medium-speed quantitative filter
paper to filter it into a 200 mL volumetric flask. Use water to rinse the beaker 2
~ 3 times. Rinse the filter paper 4 ~ 5 times. Retain the filtrate. Move the filter
paper together with the residue into a platinum crucible. Ash it in a low
temperature furnace at 700 °C ~ 750 °C. Take out the crucible. Cool it. Add 1 g
of mixed flux (4.1). Put it in a 700 °C ~ 750 °C low temperature furnace, to melt
for 20 minutes. Then move it into a 900 °C ~ 1000 °C high temperature furnace,
to melt it for 5 ~ 8 minutes. Take out the crucible. Cool it. Leach it in a 250 mL
glass beaker, which contains a small amount of water. Add 5 mL of hydrochloric
acid (4.2). Wash the crucible clean. Heat to boil it. Cool to room temperature.
Move it into a 200 mL volumetric flask, to combine with the original filtrate. Use
water to dilute it to the mark. Mix well.
7.4 Preparation of calibration curve solution
Appendix A
(Normative)
Standard operation of measuring instrument
A.1 Purpose
The purpose of the performance test, which is given in this Appendix, is to use
different types of instruments, to properly determine the performance of the
plasma spectrometer. It allows different instruments to use different operating
conditions, BUT the plasma spectrometer can ultimately produce consistent
results.
The whole performance test procedure is evaluated by three basic parameters:
detection limit (DL), background equivalent concentration (BEC), short-term
precision (RSDN).
A.2 Definition
This standard applies the following definitions:
A.2.1 Detection limit (DL): When an element produces a minimum
concentration signal, it can be considered to exceed any false background
signal with a certain specified level; on the other hand, the element
concentration produces a signal, which is three times the standard deviation of
the background level value.
A.2.2 Background equivalent concentration (BEC): It is the concentration of the
analyte that produces a net intensity equal to the background intensity value; it
is a measure of sensitivity to a given wavelength.
A.2.3 Short-term precision (RSDN): The relative standard deviation of a series
of readings of the instrument, which is obtained under the measurement
conditions.
A.3 Background equivalent concentration and detection limit
Prepare 3 sets of solution, which has the concentration of the measured
substances: 0 concentration level, 10 times the detection limit, 1000 times the
detection limit. These solutions contain acids and matrix elements, at similar
concentrations to the tested samples.
The plasma spectrometer shall be adjusted initially, according to the
manufacturer’s recommendations AND the laboratory’s practical experience in
quantitative analysis. Absorb the blank solution AND take 10 intensity readings.
......
 
(Above excerpt was released on 2021-10-02, modified on 2021-10-02, translated/reviewed by: Wayne Zheng et al.)
Source: https://www.chinesestandard.net/PDF.aspx/GBT32794-2016