GB/T 223.23-2008 English PDF (GBT223.23-2008)

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GB/T 223.23-2008: Iron, steel and alloy -- Determination of nickel content -- The dimethylglyoxime spectrophotometric method
GB/T 223.23-2008
GB
NATIONAL STANDARD OF
THE PEOPLE’S REPUBLIC OF CHINA
ICS 77.080.01
H 11
Replacing GB/T 223.23~223.24-1994
Iron, steel and alloy - Determination of nickel content -
The dimethylglyoxime spectrophotometric method
ISSUED ON. MAY 13, 2008
IMPLEMENTED ON. NOVEMBER 1, 2008
Issued by. General Administration of Quality Supervision, Inspection
and Quarantine;
Standardization Administration Committee.
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Method One -- Diacetyldioxime Directly Photometric Method ... 5 
4 Method Two -- Extraction Separation - Dimethylglyoxime
Spectrophotometric Method ... 8 
5 Test report ... 12 
Annex A (Informative) Additional Information of Joint Precision Test ... 13 
Foreword
This Part of GB/T 223 is the integral revision of GB/T 223.23-1994 "Methods
for Chemical Analysis of Iron, Steel and Alloy - The Dimethylglyoxime
Spectrophotometric Method for the Determination of Nickel Content" and
GB/T 223.24-1994 "Methods for Chemical Analysis of Iron, Steel and Alloy -
The Extraction Separation - The Dimethylglyoxime Spectrophotometric
Method for the Determination of Nickel Content".
This Part replaced GB/T 223.23-1994 and GB/T 223.24-1994.
Compared with GB/T 223.23-1994 and GB/T 223.24-1994, the main changes
of this Part are listed as follows.
- modified the name to "Iron, Steel and Alloy - Determination of Nickel
Content - The Dimethylglyoxime Spectrophotometric Method";
- merged the previous two standards into one standard, including two
analysis methods;
- added the explanation content for reagents and water in the analysis,
and revised the expression method for solution concentration;
- added the expression for safety notice and specimen quantity weighing;
- revised the result calculation formulae and quantity units in formulae;
- revised and specified the explanation for precision function formula.
Appendix A of this Part is informative.
This Part was proposed by China Iron and Steel Association.
This Part shall be under the jurisdiction of National Technical Committee on
Iron and Steel of Standardization Administration of China.
The drafting organizations of this Part. Baoshan Iron and Steel Co., Ltd. Special
Steel Branch, China Iron and Steel Research Institute Group and Tianjin
Special Steel Factory.
Main drafters of this Part. Wang Yujuan, Cui Qiuhong and Guo Yunshan.
Versions of standard substituted by this Standard are.
- GB 223.23-1982, GB 223.23-1994;
- GB 223.24-1982, GB 223.24-1994.
Iron, steel and alloy - Determination of nickel content -
The dimethylglyoxime spectrophotometric method
WARNING. the personal using this Part shall have the practical
experience of regular laboratory working. This Part does not point out
all possible safety problems. The user is responsible to adopt the
proper safety and health measures and ensure the condition meeting
the requirements of the national relevant regulations.
1 Scope
This Part of GB/T 223 specifies the determination of nickel content with
dimethylglyoxime direct photometric method and extraction separation -
dimethylglyoxime spectrophotometric method.
The method one of this Part is applicable to the determination of nickel
content with mass fraction 0.030% ~ 2.00% in pig iron, iron powder, carbon
steel and alloy steel; the method two of this Part is applicable to the
determination of nickel content with mass fraction 0.010% ~ 0.50% in pig iron,
carbon steel, alloy steel and precious alloy.
2 Normative references
The following standards contain provisions which, through reference in this
text, constitute provisions of this Part of GB/T 223. For dated reference,
subsequent amendments to (excluding correction to), or revisions of, any of
these publications do not apply. However, all parties coming to an agreement
according to this standard are encouraged to study whether the latest edition
of these documents is applicable. For undated references, the latest edition of
the normative document is applicable to this Part.
GB/T 6379.1, Accuracy (Trueness and Precision) of Measurement
Methods and Results - Part 1. General Principles and Definitions
GB/T 6379.2, Accuracy (Trueness and Precision) of Measurement
Methods and Results - Part 2. Basic Method for the Determination of
Repeatability and Reproducibility of a Standard Measurement Method
GB/T 20066, Steel and Iron-Sampling and Preparation of Samples for the
Determination of Chemical Composition
3 Method One -- Diacetyldioxime Directly
Photometric Method
3.1 Principles
Dissolve sample by acid, perchloric acid smokes and oxidize chromium to
hexavalence, screen iron with sodium tartrate; in the strongly alkaline medium,
take ammonium persulfate as the oxidizer; nickel and dimethylglyoxime
generate red complex compound, and measure the absorbance.
The manganese content larger than 1.5 mg, copper content larger than
0.2mg and cobalt content larger than 0.1 mg in the color reagent may
interfere with the determination.
3.2 Reagents and materials
Unless otherwise specified, during the analysis, only confirmed analytical
reagent and distilled water or purity-equivalent water may be used.
3.2.1 Ethanol, more than 95% (volume fraction).
3.2.2 Perchloric acid with ρ 1.67 g/mL.
3.2.3 Nitric acid with ρ 1.42 g/mL, and dilute to 2+3.
3.2.4 Mixed acid of hydrochloric acid-nitric acid; mix one hydrochloric acid
(ρ is about 1.19g/mL), one nitric acid (ρ is about 1.42g/mL) and two waters.
3.2.5 Sodium tartrate solution, 300 g/L.
3.2.6 Sodium hydroxide solution, 100 g/L.
3.2.7 Dimethylglyoxime solution, 10 g/L, prepare with ethanol (3.2.1).
3.2.8 Ammonium persulfate solution, 40 g/L.
3.2.9 Nickel standard solution
3.2.9.1 Nickel stock solution, 100 μg/mL. Weigh 0.1000 g of pure nickel
(mass fraction above 99.99%) into 150-mL conical flask, add 20 mL of nitric
acid (3.2.3), cool to room temperature after heating and dissolution, transfer
into 1000-mL volumetric flask, dilute with water to the scale, and mix well.
3.2.9.2 Nickel standard solution, 10.0 μg/mL. Shift 25.00 mL of nickel stock
solution (3.2.9.1) into 250-mL volumetric flask, add 5 mL of nitric acid (3.2.3),
dilute with water to the scale, and mix well.
3.3 Instruments and equipment
In the analysis, only the general laboratory instruments and equipment as
well as the spectrophotometer are used.
3.4 Sampling and sample preparation
The sampling and sample preparation shall be carried out according to GB/T
20066 or proper national standards.
3.5 Analysis procedures
Warning. when generally existing ammonia, nitrous acid smog or organic
substance, the emission of perchloric acid smoke may cause explosion.
3.5.1 Specimen quantity
Weigh the sample by Table 1 according to the nickel content (mass fraction)
to the accuracy of 0.0001 g.
Table 1
Nickel content (mass fraction) / % Specimen quantity / g
0.03 ~ 0.10 0.50
>0.10 ~ 0.50 0.20
>0.50 ~ 2.00 0.10
3.5.2 Blank test
Carry out the blank test together with the specimen.
3.5.3 Determination
3.5.3.1 Place the specimen (3.5.1) into 150-mL conical flask, add
5mL~10mL of nitric acid (3.2.3) or hydrochloric acid-nitric acid mixed acid
(3.2.4), add 3mL~5mL of perchloric acid (3.2.2) after heating and dissolution,
evaporate to emit perchloric acid smoke and oxidize chromium to
hexavalence, slightly cool.
3.5.3.2 Add a small amou...