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Method for continuously measuring tungsten and molybdenum by using citric acid and hydrogen peroxide as complexing agents

A technology of hydrogen peroxide and citric acid, which is applied in the field of chemical analysis, can solve the problems of high measurement cost, slow measurement speed, and narrow measurement range, and achieve the effects of simple method, promoting sample dissolution, and improving mineral processing efficiency

Active Publication Date: 2012-11-21
NORTHWEST RES INST OF MINING & METALLURGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] The present invention provides a method for the continuous determination of tungsten and molybdenum using citric acid and hydrogen peroxide as complexing agents to solve the problem of narrow determination range and poor process flow caused by traditional determination methods. Long time, slow measurement speed and high measurement cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Dissolution of the sample

[0038] Step 1: Weigh 0.2000g of GBW07238 standard sample into a polytetrafluoroethylene beaker, the addition amount of hydrochloric acid, nitric acid, hydrofluoric acid and sulfuric acid is shown in Table 1:

[0039] Table 1 The amount of inorganic acid added in the examples (mL)

[0040] Sample serial number hydrochloric acid nitric acid hydrofluoric acid sulfuric acid GBW07238 15 5 8 8

[0041] Add 15mL of analytically pure concentrated hydrochloric acid (commercially available), boil for 3-5min, add 5mL of analytically pure concentrated nitric acid (commercially available), boil for a while, add 8mL of analytically pure hydrofluoric acid (commercially available), 8mL of sulfuric acid with a volume fraction of 50%, Continue to heat until the white smoke of sulfur trioxide exhausts, remove and cool, and rinse the wall of the cup with water.

[0042] Step 2: Add 2mL of concentrated hydrochloric acid (comme...

Embodiment 2

[0058] (1) Dissolution of the sample

[0059] Step 1: Weigh 0.2000 g of the GBW07238 standard sample in a polytetrafluoroethylene beaker, add hydrochloric acid, nitric acid, hydrofluoric acid, and sulfuric acid according to step 1 in Example 1, and the amounts added are as shown in Table 3:

[0060] Table 3 The amount of inorganic acid added in the examples (mL)

[0061] Sample serial number hydrochloric acid nitric acid hydrofluoric acid sulfuric acid GBW07238 20 7 15 10

[0062] The sample dissolution method is the same as that in Example 1, the sample is dissolved until the white smoke is exhausted, cooled, and the cup wall is washed with water;

[0063] Step 2 is the same as step 2 in Example 1.

[0064] (2) The preparation of the standard solution is the same as the preparation of the standard solution in Example 1.

[0065] (3) The instrument conditions are the same as those in Example 1.

[0066] The comparison between the standard val...

Embodiment 3

[0070] (1) Decomposition of samples

[0071] Step 1: Weigh 0.2000 g of GBW07238 standard sample in a polytetrafluoroethylene beaker, add hydrochloric acid, nitric acid, hydrofluoric acid, and sulfuric acid according to step 1 of Example 1, and the addition amount is as shown in Table 5:

[0072] Table 5 The amount of inorganic acid added in the examples (mL)

[0073] Sample serial number hydrochloric acid nitric acid hydrofluoric acid sulfuric acid GBW07238 30 10 20 15

[0074] Dissolving the sample is the same as in Example 1, dissolving the sample until the white smoke is exhausted, cooling, and washing the cup wall with water;

[0075] Step 2 is the same as step 2 in Example 1.

[0076] (2) The preparation of the standard solution is the same as the preparation of the standard solution in Example 1.

[0077] (3) The instrument conditions are the same as those in Example 1.

[0078] The standard value and comparison between the tungsten and...

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Abstract

The invention discloses a method for continuously measuring tungsten and molybdenum by using citric acid and hydrogen peroxide as complexing agents. By the method, the problems of narrow measuring range, long flow path, slow measuring speed and high measuring cost caused by the traditional measuring method are solved. The method comprises the following steps of: weighing a sample and placing the sample into a polytetrafluoroethylene beaker; performing treatment by adding concentrated hydrochloric acid, pure nitric acid, hydrofluoric acid and sulfuric acid; adding 1 to 5 milliliters of analytic pure concentrated hydrochloric acid (commercial) and 2 to 6 milliliters of citric acid with mass fraction of 10 g / L; boiling to dissolve the soluble salt; taking down and cooling for a moment; adding 10 to 50 milliliters of analytic pure strong ammonia water (commercial); adjusting the pH value of the solution to 8 to 10; heating to volatilize excessive ammonia water; adding 4 to 40 millimeters of analytic pure concentrated hydrochloric acid (commercial) and 2 milliliters of hydrogen peroxide with the volume fraction of 30 percent; heating to dissolve the soluble salt and decompose the excessive hydrogen peroxide; taking down, cooling and entering a volumetric flask; diluting to 100 to 1,000 milliliters; filtering; and performing inductively coupled plasma-atomic emission spectrometry (ICP-AES) measurement. By the method, the tungsten and the molybdenum are measured at the same time by dissolving the sample at one step. The method is simple, rapid and convenient. By the method, resources are saved.

Description

technical field [0001] The invention belongs to chemical analysis technology, in particular to a method for chemical analysis of tungsten and molybdenum in samples. Background technique [0002] (1) Determination of tungsten [0003] At present, most of the decomposition of tungsten ore adopts alkali fusion method. Alkali fusion method is very efficient in decomposing tungsten minerals. The commonly used fluxes are sodium hydroxide, potassium hydroxide, sodium peroxide, etc. Among them, sodium hydroxide has the strongest decomposition ability. Both the acid dissolution method and the alkali fusion method are widely used in the actual analysis of tungsten ore, and the alkali fusion method is more widely used. [0004] Tungsten can be determined by gravimetry, photometry, XRF spectroscopy, atomic absorption, polarography and neutron activation. Different methods need to be selected according to the content of tungsten in the sample and the nature of the sample itself, such ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/73G01N1/28G01N1/38
Inventor 齐白羽赵海军王同敏方彦霞王红燕郑省政路军兵庞振业许素敏
Owner NORTHWEST RES INST OF MINING & METALLURGY INST