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Method for measuring content of tin in crude lead

A determination method, crude lead technology, applied in the preparation of test samples, thermal excitation analysis, material excitation analysis, etc., can solve the problems of difficult device fabrication, difficult operation, high color temperature and condition requirements of photometric method, and achieve Effects of increasing accuracy, adding correction steps, and widening the detection range

Active Publication Date: 2020-02-04
CHANGCHUN GOLD RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Standard method, YS / T 248.2-2007, this standard contains two methods, one of which is phenylfluorone spectrophotometry, and the other is potassium bromate titration ; wherein the phenylfluorone spectrophotometric measurement range is too narrow, only 0.01%-0.2%, and the photometric method has higher requirements on the color temperature and conditions, poor reproducibility, and is difficult to operate; and the potassium bromate titration method needs to use aluminum Chip reduction requires a specific reduction device, which is not easy to manufacture and increases the cost and difficulty of analysis.
[0005] Use dilute nitric acid to dissolve, or dissolve the crude lead sample with nitric acid and hydrochloric acid, but both methods have their own disadvantages; if dilute nitric acid is used alone, it will cause In the hydrolysis of tin, it can be seen in the experiment that a large amount of white matter appears, which is the product of tin hydrolysis

Method used

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  • Method for measuring content of tin in crude lead
  • Method for measuring content of tin in crude lead
  • Method for measuring content of tin in crude lead

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] Weigh m as 4.9970g (accurate to 0.001) sample and measure according to the above method;

[0075] In Step 1, add 130 mL of dissolving acid, heat and dissolve on a hot plate at 220°C, add 97.5 mL of hydrochloric acid with a density ρ of 1.19 g / mL and 3 mL of potassium sodium tartrate with a concentration of 200 g / L,

[0076] Wash the original beaker 3 times and the filter paper 3 times with aqua regia with a mass concentration of 1% after the filtration is completed in step 2;

[0077] In step 3, put the zirconium crucible into the muffle furnace and raise it from low temperature to 650°C for ashing. After the ashing is complete, take it out and cool it, add 2g of sodium peroxide, cover with 0.5g of sodium peroxide, and put it in the muffle furnace at Melt at 680°C for 10 minutes, take it out and cool to room temperature;

[0078] Add 50mL water in step 4, add 10mL hydrochloric acid and 5mL potassium sodium tartrate;

[0079] In step 5, the mass fraction range of tin i...

Embodiment 2

[0083] Weigh m as 4.9980g (accurate to 0.001) sample and measure it according to the above method;

[0084] In step 1, add 150 mL of dissolving acid, heat and dissolve on a hot plate at 250°C, add 97.5 mL of hydrochloric acid with a density ρ of 1.19 g / mL and 4 mL of potassium sodium tartrate with a concentration of 200 g / L,

[0085] After the filtration in step 2 is completed, wash the original beaker 3 times and the filter paper 3 times with aqua regia with a mass concentration of 1.5% respectively;

[0086] In step 3, put the zirconium crucible into the muffle furnace and raise it from low temperature to 700°C for ashing. After the ashing is complete, take it out and cool it, add 3g of sodium peroxide, cover with 1g of sodium peroxide, and put it in the muffle furnace at 700°C Melt at ℃ for 15 minutes, take out and cool to room temperature;

[0087] Add 60mL water in step 4, add 15mL hydrochloric acid and 6mL potassium sodium tartrate;

[0088] The mass fraction range of ...

Embodiment 3

[0092] Weigh m as 4.9990g (accurate to 0.001) sample and measure it according to the above method;

[0093] In step 1, 140 mL of dissolving acid was added, heated and dissolved on a hot plate at 250°C, 97.5 mL of hydrochloric acid with a density ρ of 1.19 g / mL and 5 mL of potassium sodium tartrate with a concentration of 200 g / L were added,

[0094] Wash the original beaker 3 times and the filter paper 3 times with aqua regia with a mass concentration of 1.2% after the completion of the filtration in step 2;

[0095] In step 3, put the zirconium crucible into the muffle furnace and raise it from low temperature to 700°C for ashing. After the ashing is complete, take it out and cool it, add 2.5g of sodium peroxide, cover with 0.8g of sodium peroxide, and put it into the muffle furnace Melt at 700°C for 15 minutes, take out and cool to room temperature;

[0096] Add 50mL water in step 4, add 12mL hydrochloric acid and 5.5mL potassium sodium tartrate;

[0097] The mass fraction...

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Abstract

The invention belongs to the technical field of measurement of tin elements in metals, and particularly relates to a method for measuring the content of tin in crude lead. The method comprises the steps of: firstly, dissolving metal lead with nitric acid and potassium sodium tartrate, adding hydrochloric acid to inhibit tin hydrolysis, after a white precipitate disappears, taking off the lead forcooling, performing filtering by using medium-speed quantitative filter paper, ashing residues together with the filter paper in a muffle furnace, melting the ash with sodium peroxide, leaching in hotwater, performing acidification, merging the solution with the filtrate, and measuring the tin in ICP. According to the method, the applicability of the sample is fully considered, the experimental process is greatly simplified, the analysis efficiency is improved, and the detection range of the experiment is expanded; at the same time, the disadvantages of simultaneous addition of nitric acid and hydrochloric acid in other methods are fully considered, the method of firstly adding the nitric acid and the potassium sodium tartrate to dissolve the metal lead, and then adding the hydrochloric acid to inhibit tin hydrolysis is invented, this change effectively solves the problem of the formation of a dense oxide film on the metal lead in an aqua regia system, meanwhile, a step of correctinginsoluble residues is increased to further improve the accuracy of the experiment.

Description

technical field [0001] The invention belongs to the technical field of tin element determination in metals, and in particular relates to a method for determining tin content in crude lead. Background technique [0002] Crude lead is lead that contains 1% to 4% (mass fraction) impurities and precious metals from ore smelted in a blast furnace. Tin is a common element in crude lead. During the refining process of lead, the precipitation potential of tin is very close to that of lead , tin dissolves with lead and precipitates out on the cathode. The existence of tin element in crude lead seriously affects the quality of electric lead products and reduces the purity of crude lead. Therefore, the determination of tin content in crude lead is particularly important. [0003] At present, the determination of tin content in crude lead mainly has the following methods: [0004] The industry standard method, YS / T 248.2-2007, contains two methods in this standard, one is phenylfluoro...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N21/73
CPCG01N1/28G01N21/73Y02P10/20
Inventor 张越陈永红洪博苏广东高振广穆岩关国军杨星
Owner CHANGCHUN GOLD RES INST
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