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GB/T 223.31-2008 English PDF (GBT223.31-2008)

GB/T 223.31-2008 English PDF (GBT223.31-2008)

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GB/T 223.31-2008: Iron, steel and alloy -- Determination of arsenic content -- Distillation-molybdenum blue spectrophotometric method
GB/T 223.31-2008
Iron, steel and alloy. Determination of arsenic content. Distillation-molybdenum blue spectrophotometric method
ICS 77.080.01
H11
National Standards of People's Republic of China
GB/T 223.31-2008/ISO 17058..2004
Replacing GB/T 223.31-1994
Iron, steel and alloy - Determination of arsenic content
Distillation separation - molybdenum blue spectrophotometry
(ISO 17058..2004, IDT)
2008-05-13 released
2008-11-01 implementation
General Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
China National Standardization Administration released
Foreword
This part of GB/T 223 is equivalent to using ISO 17058..2004 "Determination of arsenic content of steel spectrophotometry."
For ease of use, this section made the following editorial changes.
a) Replace "this International Standard" with "this Part";
b) Use the decimal "." instead of the comma "," as the decimal point;
c) delete the preface to international standards;
d) In the "normative references", the referenced international document or the quoted specific clause is exactly the same as the domestic document,
In the document instead.
This Part Replaces GB/T 223.31-1994 "Methods for Chemical Analysis of Iron, Steel and Alloy Distillation - Determination of molybdenum blue spectrophotometry
Arsenic content. "
This section compared with GB/T 223.31-1994, the main changes made to the following.
--- Reducing agent "20mL sulfuric acid trap - potassium bromide mixed solution" to "2g sulfuric acid trap - potassium bromide mixture", while reducing the increase
Into the distillation flask acid volume, shorten the distillation time;
--- Calibration curve by the uniform use of 10μg/mL arsenic standard solution formulated for different content of the calibration curve using different concentrations
Degree of arsenic standard solution preparation;
--- Increased 2.0μg/mL arsenic standard solution.
This part of the Appendix A, Appendix B is an informative annex.
This part is proposed by China Iron and Steel Association.
This part of the National Standardization Technical Committee Steel centralized.
This section mainly drafted by. China Steel Research Technology Corporation.
The main drafters of this section. Luo Qianhua, Yu Dingzhi, Ge Ru Bin.
This part of the standard replaces the previous editions are.
--- GB/T 223.31-1984, GB/T 223.31-1994.
GB/T 223.31-2008/ISO 17058..2004
Iron, steel and alloy - Determination of arsenic content
Distillation separation - molybdenum blue spectrophotometry
Warning. Personnel using this section should have practical experience in formal laboratory work. This section does not indicate all possible security issues.
It is the user's responsibility to take appropriate safety and health measures and to ensure compliance with the requirements of the relevant state laws and regulations.
1 range
This section GB/T 223 specifies the distillation separation - molybdenum blue spectrophotometric determination of arsenic content.
This section applies to the determination of arsenic content of 0.0005% ~ 0.10% in steel and alloy.
2 Normative references
The following documents contain provisions that, through reference in this section, become the provisions of this part of GB/T 223. Any reference to the date of the citation
All subsequent amendments (not including errata content) or revisions do not apply to this section, however, encouraged to be reached under this section
The parties to the agreement study whether the latest versions of these documents are available. For undated references, the latest version applies to this book
section.
GB/T 6379.1 Accuracy (accuracy and precision) of measurement methods and results - Part 1. General and definitions
(GB/T 6379.1-2004, ISO 5725-1..1994, IDT)
GB/T 6379.2 Accuracy (accuracy and precision) of measurement methods and results - Part 2. Determination of the weight of standard measurement methods
Fundamentals of renaturation and reproducibility (GB/T 6379.2-2004, ISO 5725-2..1994, IDT)
GB/T 20066-2006 Sampling and sample preparation methods for the determination of chemical compositions of steel and iron (ISO 14284..1996, IDT)
ISO 385-1. 1984 Laboratory glassware burets - Part 1. Basic requirements
Laboratory glassware single standard pipette
ISO 1042..1998 Laboratory glassware Monoscript wire capacity bottles
ISO 3696. 1987 Analysis of laboratory water specifications and test methods
ISO 5725-3 Accuracy (accuracy and precision) of measurement methods and results - Part 3. Standard measurement methods Precision
Interval measurement
3 principle
The sample was dissolved in hydrochloric acid, nitric acid mixed acid, adding sulfuric acid, continue to heat to take sulfuric acid white smoke. In sulfuric acid and hydrochloric acid medium, add sulfuric acid
Hydrazine and potassium bromide reduce arsenic and separate it by distillation in the form of AsCl3. The distillate is absorbed by nitric acid and As (III) is oxidized to As (V). To
Hydrazine sulfate as a reducing agent, arsenic and ammonium molybdate blue molybdenum complexes formed. Spectrophotometry was performed at a wavelength of 840 nm.
4 Reagents and materials
In the analysis, unless otherwise stated, only certified analytical reagents and Grade III water as defined in ISO 3696. 1987 are used.
4.1 Hydrochloric acid, p approximately 1.19 g/mL.
4.2 nitric acid, p about 1.40 g/mL.
4.3 Nitric acid, ρ approximately 1.40 g/mL, diluted to 3 + 1.
4.4 Mixed acids. A volume of nitric acid (4.2) is added to four volumes of hydrochloric acid (4.1).
4.5 sulfuric acid, p about 1.84 g/mL.
4.6 sulfuric acid, ρ about 1.84g/mL, diluted to 1 +1. While cooling in the water and stirring constantly, a certain volume of sulfuric acid (4.5) min
GB/T 223.31-2008/ISO 17058..2004
Several times to join an equal volume of water.
4.7 sulfuric acid, ρ about 1.84g/mL, diluted to 1 +6. While cooling in the water and stirring constantly, a certain volume of sulfuric acid (4.5) min
Several times into six times the volume of water.
4.8 reductant powder mixture. According to a certain percentage, weighed 2.5g of hydrazine sulfate and 10g of potassium bromide, placed in a mortar, with research sticks fine, and
Mix well, spare.
4.9 ammonium molybdate solution, (NH4) 6Mo7O24 4H2O, 10 g/L.
4.10 hydrazine sulfate solution, N2H6SO4, 0.6g/L.
4.11 arsenic standard solution
4.11.1 stock solution, equivalent to 0.20g of arsenic per liter. Weigh 0.1320g arsenic trioxide (As2O3), accurate to 0.0001g, placed
100mL beaker, slowly add 10mL nitric acid (4.2), cover the watch glass, slowly heated until completely dissolved. Add 2 mL of sulfuric acid
(4.6), slowly heat up, get rid of nitrogen oxides, continue to evaporate to take a large amount of white smoke. Remove the cold, rinse the watch glass and cup wall with a little water, again
Evaporation to take a lot of white smoke. Remove the cooling, add about 10mL of water, slightly heated until the salts dissolved, the solution becomes clear so far. Cool to room temperature,
The solution was quantitatively transferred to 500mL single-labeled volumetric flask, diluted with water to the mark, and mix. This stock solution 1 mL contains 0.2 mg of arsenic.
4.11.2 Standard solution A, equivalent to 0.01g of arsenic per liter. Pipette 25.00mL stock solution (4.11.1), in 500mL single-standard line capacity
Bottle, diluted with water to the mark, mix well. When used with the time. This standard solution 1mL containing 10μg arsenic.
4.11.3 Standard solution B, equivalent to 0.002g a liter per liter. Pipette 50.00mL standard ...
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