Method for determination of content of lead in chrome ore

A determination method and technology of lead content, which is applied in the preparation of test samples, fluorescence/phosphorescence, material excitation analysis, etc., can solve the problems that are not suitable for the determination of lead in chrome ore, and achieve stable fusion sample results, ensure stability, well-designed effects

Active Publication Date: 2015-11-18

LIANYUN PORT IMMIGRATION INSPECTION & QUARANTINE BUREAU PEOPLES REPUBLIC OF CHINA

5 Cites 3 Cited by

AI-Extracted Technical Summary

Problems solved by technology

Commonly used methods for the determination of lead in other minerals mostly use acidic systems to digest under normal pressure or microwave high pressure, and use analytical instruments such as ato...

Method used

The boiling point of sodium oxide is 657 ℃, and melting sample temperature is too low, and sample can not be melted completely, and melting sample temperature is too high, and sample splashes easily, and this method is selected at 650 ℃ by test melting sample temperature, and melting sample time is too long If it is too short, the melting will be incomplete, if it is too long, it will waste time and energy. Control the melting time to 20 minutes, which can satisfy the complete melting of the sample and the stability of the melting result.

[0079] Due to laboratory testing...

Abstract

A method for determination of the content of lead in a chrome ore comprises the steps: mixing sodium peroxide with the lead-containing chrome ore in a corundum crucible, melting at the temperature of 600-700 DEG C, then dissolving a precipitate and acidifying the melt with a hydrochloric acid solution and water, diluting with water, mixing evenly, and thus obtaining a sample solution; mixing evenly a hydrochloric acid solution and water with the same volume as that for preparation of the sample solution, to obtain a blank solution; respectively transferring at least five different volumes of lead standard solution with the mass concentration of 0.25 [mu]g/mL in a group of volumetric flasks, adding the blank solution, diluting with water, and thus obtaining the calibration solutions; and finally, testing in an atomic fluorescence spectrometer, to obtain a standard working curve of the calibration solutions, so as to test the content of lead in the chrome ore. With adopting of sodium peroxide to melt the chrome ore, the dissolution time is short, and the determination results are stable; the melting temperature is selected in the range of 600-700 DEG C, so that the sample complete melting can be met, and the molten sample result is stable; and with the calibration solutions as the benchmark, the measurement accuracy is improved.

Application Domain

Preparing sample for investigationFluorescence/phosphorescence

Technology Topic

FluorescenceVolumetric flask +9

Image

Examples

Experimental program(14)
Effect test(1)

Example Embodiment

[0026] Example 1, a method for measuring lead content in chrome ore, the steps are:

[0027] (1) Preparation of sample solution

[0028] Weigh 0.2g of lead-containing chrome ore sample, place it in a corundum crucible pre-added with 0.8g of sodium peroxide, and then cover the sample with 0.8g of sodium peroxide, and place the corundum crucible at 600℃ to melt 15min, take it out and cool to room temperature;

[0029] After cooling, put the corundum crucible with the molten material into the beaker, add 45mL of hot water at 60℃ to soak the molten material, pour the molten material into the beaker, and use the hydrochloric acid solution and water to put the corundum crucible inside and outside Rinse the remaining melt into the beaker, then add 8-12mL hydrochloric acid solution to the beaker, dissolve the precipitate and acidify to obtain the melt solution, cool to room temperature, transfer the melt solution to a 100mL volumetric flask, dilute to the mark with water, Mix well

[0030] Pipette 3mL melt solution from a 100mL volumetric flask to a 50mL volumetric flask, dilute to the mark with water, and mix well to obtain a sample solution;

[0031] (2) Preparation of blank solution

[0032] Weigh the sodium peroxide of the same quality as in step (1), and after melting, follow the same steps as the preparation of the sample solution to obtain a blank solution;

[0033] (3) Preparation of calibration solution

[0034] Pipette 0mL, 5mL, 10mL, 15mL, 20mL, 25mL of the lead standard solution with a mass concentration of 0.25μg/mL into a set of 50mL volumetric flasks, add 8mL blank solution to each volumetric flask, and dilute to the mark with water. Mix well to obtain calibration solution;

[0035] (4) Computer test

[0036] In the atomic fluorescence spectrometer, use the hydrochloric acid solution as the carrier, the potassium borohydride solution as the reducing agent, and the lead hollow cathode lamp as the excitation light source. The calibration solution, the sample solution and the blank solution are sequentially tested for the fluorescence intensity. The lead concentration is the abscissa and the fluorescence intensity is the ordinate. Draw the standard working curve of the calibration solution, and then quantify the lead in the sample according to the fluorescence intensity obtained from the sample solution and refer to the standard working curve of the calibration solution. The content of lead in chrome ore.

Example Embodiment

[0037] Example 2, a method for measuring lead content in chrome ore, the steps are:

[0038] (1) Preparation of sample solution

[0039] Weigh 0.7g of lead-containing chrome ore sample, place it in a corundum crucible pre-added with 1.2g of sodium peroxide, and then cover the sample with 1.2g of sodium peroxide, and place the corundum crucible at 700℃ to melt 25min, take it out and cool to room temperature;

[0040] After cooling, put the corundum crucible with the molten material into the beaker, add 45mL of hot water at 100℃ to soak the molten material, pour the molten material into the beaker, and use the hydrochloric acid solution and water to put the corundum crucible inside and outside Rinse the remaining melt into the beaker, then add 12 mL of hydrochloric acid solution to the beaker, dissolve the precipitate and acidify to obtain the melt solution, cool to room temperature, transfer the melt solution to a 100 mL volumetric flask, dilute to the mark with water, and mix well ;

[0041] Transfer 7 mL of the melt solution from a 100 mL volumetric flask to a 50 mL volumetric flask, dilute to the mark with water, and mix well to obtain a sample solution;

[0042] (2) Preparation of blank solution

[0043] Weigh the sodium peroxide of the same quality as in step (1), and after melting, follow the same steps as the preparation of the sample solution to obtain a blank solution;

[0044] (3) Preparation of calibration solution

[0045] Transfer 1mL, 3mL, 5mL, 7mL, 9mL, 11mL of the lead standard solution with a mass concentration of 0.25μg/mL to a set of 50mL volumetric flasks, add 12mL blank solution to each volumetric flask, dilute to the mark with water, mix Evenly, get the calibration solution;

[0046] (4) Computer test

[0047] In the atomic fluorescence spectrometer, use the hydrochloric acid solution as the carrier, the potassium borohydride solution as the reducing agent, and the lead hollow cathode lamp as the excitation light source. The calibration solution, the sample solution and the blank solution are sequentially tested for the fluorescence intensity. The lead concentration is the abscissa and the fluorescence intensity is the ordinate. Draw the standard working curve of the calibration solution, and then quantify the lead in the sample according to the fluorescence intensity obtained from the sample solution and refer to the standard working curve of the calibration solution. The content of lead in chrome ore.

Example Embodiment

[0048] Example 3, the method for determining the lead content in the chrome ore described in Example 1: In the computer test described in step (4), the fluorescence intensity was tested at a negative high voltage of 230mV, a lamp current of 55mA, and an atomizer height It is performed under the conditions of 6mm, auxiliary gas flow rate of 380mL/min, and shielding gas flow rate of 700mL/min.

PUM

Description & Claims & Application Information

We can also present the details of the Description, Claims and Application information to help users get a comprehensive understanding of the technical details of the patent, such as background art, summary of invention, brief description of drawings, description of embodiments, and other original content. On the other hand, users can also determine the specific scope of protection of the technology through the list of claims; as well as understand the changes in the life cycle of the technology with the presentation of the patent timeline. Login to view more.

Classification and recommendation of technical efficacy words

easy to operate
short dissolution time

Method for determination of content of lead in chrome ore

AI-Extracted Technical Summary

Problems solved by technology

Method used

Abstract

Image

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

Similar technology patents

Household appliance control method and device and mobile terminal

Graphene film and preparation method therefor

Driving working load calculation method of automobile driver

Laser radar optical system with optical axis calibrating function and optical axis calibrating method

Full automatic busbar terminal crimping device and crimping method and terminal crimping machine

Classification and recommendation of technical efficacy words

System and method for information access

Operating mechanism, medical manipulator, and surgical robot system

Lancet device

A method and device for automatic image acquisition

Rapid and non-invasive optical detection of internal bleeding

Qingkailing lyophilized tablet and preparation method thereof

Thickening composition for washing effervescent tablet and washing effervescent tablet