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GB/T 10574.11-2017 (GB/T10574.11-2017)

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GB/T 10574.11-2017: PDF in English (GBT 10574.11-2017)

GB/T 10574.11-2017
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
Issued by. General Administration of Quality Supervision, Inspection and
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
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
--- Part 6. Determination of Copper Content – Flame Atomic Absorption
--- 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
--- 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
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
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 sulfuric acid (4.4), the following procedures
shall take as 6.4.3.
6.5.2 Under the same conditions of measuring the test materials, take reagent blank
as the reference; measure the absorbance of serial standard solutions. Take
phosphorus quantity as abscissa, absorbance as the ordinate, then draw the working
7 Calculation of Analytical Results
The phosphorus quantity shall be calculated by phosphorus mass fraction wp, the value
shall be expressed in %; calculate by Formula (1).
m1 – mass of phosphorus checked from the working curve, in µg;
V – total volume of test solution, in mL;
(Above excerpt was released on 2018-03-30, modified on 2021-06-07, translated/reviewed by: Wayne Zheng et al.)
Source: https://www.chinesestandard.net/PDF.aspx/GBT10574.11-2017