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GB/T 10574.11-2017

Chinese Standard: 'GB/T 10574.11-2017'
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GB/T 10574.11-2017English95 Add to Cart 0--15 minutes. Auto immediate delivery. Methods for chemical analysis of tin-lead solders--Part 11: Determination of phosphorus content--Crystal violet phosphorus-vanadium-molybdeum heteropoly acid spectrophotometry Valid GB/T 10574.11-2017
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Detail Information of GB/T 10574.11-2017; GB/T10574.11-2017
Description (Translated English): Methods for chemical analysis of tin-lead solders--Part 11: Determination of phosphorus content--Crystal violet phosphorus-vanadium-molybdeum heteropoly acid spectrophotometry
Sector / Industry: National Standard (Recommended)
Classification of Chinese Standard: H13
Classification of International Standard: 77.120.60
Word Count Estimation: 6,633
Date of Issue: 2017-10-14
Date of Implementation: 2018-05-01
Older Standard (superseded by this standard): GB/T 10574.11-2003
Drafting Organization: Yunnan Tin Industry Co., Ltd., Yunnan Tin Group (Holdings) Co., Ltd., China Nonferrous Guilin Institute of Mineral Geology Co., Ltd., Kunming Institute of Metallurgy, People's Republic of China Bayuquan Exit Inspection and Quarantine
Administrative Organization: National Nonferrous Metals Standardization Technical Committee (SAC/TC 243)
Regulation (derived from): National Standard Announcement 2017 No. 26
Issuing agency(ies): People's Republic of China General Administration of Quality Supervision, Inspection and Quarantine, China National Standardization Administration

GB/T 10574.11-2017
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.60
H 13
Replacing GB/T 10574.11-2003
Methods for Chemical Analysis of Tin-Lead Solders – Part 11.
Determination of Phosphorus Content – Crystal Violet
Phosphorus-Vanadium-Molybdenum Heteropoly Acid
Spectrophotometry
锡铅焊料化学分析方法
第 11 部分. 磷量的测定结晶紫-磷钒钼杂多酸分光光度法
ISSUED ON. OCTOBER 14, 2017
IMPLEMENTED ON. MAY 01, 2018
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of PRC.
Table of Contents
Foreword . 3
1 Scope .. 5
2 Normative References . 5
3 Method Summary .. 5
4 Reagents . 6
5 Specimen .. 7
6 Analytical Procedures .. 7
7 Calculation of Analytical Results .. 8
8 Precision . 9
9 Test Report .. 9
Foreword
GB/T 10574 Methods for Chemical Analysis of Tin-Lead Solders can be divided into
the following 14 parts.
--- Part 1. Determination of Tin Content – Potassium Iodate Titrimetric Method;
--- Part 2. Determination of Antimony Content - Malachite Green
Spectrophotometric Method and Potassium Bromate Titration;
--- Part 3. Determination of Bismuth – Flame Atomic Absorption spectrometry;
--- Part 4. Determination of Iron Content - 1,10-Phenanthroline Spectrophotometry;
--- Part 5. Determination of Arsenic Content – Arseno-Antimono-Molybdenum Blue
Spectrophotometry;
--- Part 6. Determination of Copper Content – Flame Atomic Absorption
spectrometry;
--- Part 7. Determination of Silver Content – Flame Atomic Absorption Spectrometry
and Potassium Thiocyanate Potentiometric Titration;
--- Part 8. Determination of Zinc Content – Flame Atomic Absorption Spectrometry;
--- Part 9. Determination of Aluminum Content – Electrothermal Atomic Absorption
Spectrometry;
--- Part 10. Determination of Cadmium Content – Flame Atomic Absorption
Spectrometry and Na2EDTA Titration;
--- Part 11. Determination of Phosphorus Content – Crystal Violet Phosphorus-
Vanadium-Molybdenum Heteropoly Acid Spectrophotometry;
--- Part 12. Determination of Sulfur Content - High-Frequency Combustion Infrared
Absorption Spectrometry;
--- Part 13. Determination of Antimony, Bismuth, Iron, Arsenic, Copper, Silver, Zinc,
Aluminum, Cadmium, Phosphorous and Gold Contents - Inductively Coupled
Plasma Atomic Emission Spectrometric Method;
--- Part 14. Determination of Tin, Lead, Antimony, Bismuth, Silver, Copper, Zinc,
Cadmium and Arsenic Content - Optical Emission Spectrometry.
This Part belongs to Part 11 of GB/T 10574.
This Part was drafted as per the rules specified in GB/T 1.1-2009.
Methods for Chemical Analysis of Tin-Lead Solders – Part 11.
Determination of Phosphorus Content – Crystal Violet
Phosphorus-Vanadium-Molybdenum Heteropoly Acid
Spectrophotometry
1 Scope
This Part of GB/T 10574 specifies the determination of phosphorus content in the tin-
lead solders.
This Part is applicable to the determination of phosphorus content in the tin-lead
solders. The measurement range is 0.0005% ~ 0.0100%.
This Part belongs to the arbitration analysis method.
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 document.
GB/T 8012 Casting Tin-Lead Solders
3 Method Summary
The test materials shall use nitric acid and hydrochloric acid to decompose; then in the
sulfuric acid medium, use hydrochloric acid-hydrobromic acid to volatilize and remove
the tin, arsenic and antimony, the lead is precipitated as lead sulfate. Take the test
solution separately and adjust the acidity, then in the presence of polyvinyl alcohol,
phosphorus-vanadium-molybdenum heteropoly acid and crystal violet form a purple-
red ion complex; measure its absorbance at a wavelength of 545nm of
spectrophotometer.
the operation for twice. The sulfuric acid continues to smoke till the residual sulfuric
acid volume is 2mL~3mL; take off and cool off. Use small amount of water to wash the
beaker wall, boil for 2min; cool off to the room temperature; use water to transfer into
50mL volumetric flask and dilute to the scale; mix evenly. Use a slow quantitative filter
paper to dry filter in a 100mL beaker; discard the initial portion of the filtrate;
respectively take 10.00mL of filtrate into 100mL volumetric flask.
6.4.3 Add one drop of p-nitrophenol solution (4.7); add 5.0mL of sodium hydroxide
solution (4.6); use sulfuric acid (4.5) to adjust till the yellow color fades; add 10.0mL of
sulfuric acid solution (4.5); dilute with water to about 60mL; mix evenly. Under shaking
condition, slowly add 10mL of molybdenum-ammonium vanadate mixture (4.10); mix
evenly, stand for 10min. Add 2.0mL of polyvinyl alcohol solution (4.11), mix evenly. Add
4.0mL of crystal violet solution (4.12); dilute with water to the scale; mix evenly. Place
for 1h.
6.4.4 Transfer partial test solution into 1cm cuvette; take the blank test solution of the
test materials as the reference; measure its absorbance at the wavelength of 545nm
of the spectrophotometer. Find the corresponding amount of phosphorus from the
working curve.
6.5 Drawing of working curve
6.5.1 Pipette 0mL, 1.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL of
phosphorus standard solution (4.14) into a group of 100mL volumetric flasks; dilute
with water to about 20mL; add 1.2mL of sulf......
Related standard:   GB/T 10574.10-2017  GB/T 10574.12-2017
   
 
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