Method for improving accuracy and precision of trace amount antimony in metal lead measuring

A metal lead, precision technology, used in the preparation of test samples, measurement of color/spectral properties, etc., can solve problems such as instability, poor linearity of the standard curve, lack of control methods, etc.

A metal lead, precision technology, used in the preparation of test samples, measurement of color/spectral properties, etc., can solve problems such as instability, poor linearity of the standard curve, lack of control methods, etc.

CN103076293AInactive Publication Date: 2013-05-01WESTERN MINING CO LTD

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for improving accuracy and precision of trace amount antimony in metal lead measuring
  • Method for improving accuracy and precision of trace amount antimony in metal lead measuring
  • Method for improving accuracy and precision of trace amount antimony in metal lead measuring

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] This implementation example illustrates the determination result of this method to low content antimony in metallic lead.

[0036] The solution preparation and the drawing of the standard solution working curve are completely operated according to the contents of the invention (1) and (2).

[0037] Sample analysis: Weigh the national standard substance GB469-83 1 # Sample 5.0000 grams, GB469-83 2 # Sample 4.0000 grams of sample in a series of 250mL beaker, add 40mL of 1+3 nitric acid, heat at low temperature to dissolve, boil to remove nitrogen oxides, cool, rinse the watch glass and cup wall with water, add 8mL of 1+3 sulfuric acid solution, heat and evaporate to Emit white smoke and nearly dry, cool, add 10mL 1+1 hydrochloric acid, the following operations are completed according to the steps in the sample analysis (3) of the content of the invention. The obtained measurement results are shown in Table 1.

[0038] Table 1 Determination results of low content antimo...

Embodiment 2

[0042] This implementation example illustrates the determination results of this method to the lower content of antimony in metallic lead.

[0043] The solution preparation and the drawing of the standard solution working curve are completely operated according to the contents of the invention (1) and (2).

[0044] Sample analysis: Weigh the national standard substance GB469-83 3 # Sample 2. Put 0000 grams of sample in a 250mL beaker, add 20mL of 1+3 nitric acid, heat at low temperature to dissolve, boil to remove nitrogen oxides, cool, rinse the watch glass and the wall of the cup with water, and transfer it into a 50mL volume filled with 20mL1+3 sulfuric acid solution in advance. In the bottle, make up to volume with water and let stand.

[0045] Take 20 mL of the supernatant, add 8 mL of 1+3 sulfuric acid solution, heat and evaporate until white smoke is emitted and nearly dry, and then cool. Add 10mL 1+1 hydrochloric acid, and the following operations are completed accor...

Embodiment 3

[0050] This implementation example illustrates this method to the determination result of relatively high content antimony in metallic lead.

[0051]The solution preparation and the drawing of the standard solution working curve are completely operated according to the contents of the invention (1) and (2).

[0052] Sample analysis: Weigh the national standard substance GB469-83 5 # Sample 0.5000 grams of sample in a 250mL beaker,

[0053] Heat at low temperature to dissolve, boil to remove nitrogen oxides, cool, rinse the watch glass and cup wall with water, transfer to a 50mL volumetric flask filled with 20mL 1+3 sulfuric acid solution in advance, dilute to volume with water, and let stand.

[0054] Separate 10 mL of the supernatant into a 250 mL beaker, add 8 mL of 1+3 sulfuric acid solution, heat and evaporate until white smoke is emitted and nearly dry, then cool. Add 10mL 1+1 hydrochloric acid, and the following operations are completed according to the steps in the sa...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention belongs to the field of nonferrous metallurgy, in particular to a method for improving the accuracy and precision of trace amount antimony in metal lead measuring. The method comprises the following steps: (1), preparing the following solution; (2), drawing the standard solution working curve; and (3), analyzing samples and finding out corresponding antimony concentration from the working curve. The method has the following advantages: (1), a technology is provided for improving the accuracy and precision of trace amount antimony in metal lead measuring; (2), full amount extraction is realized; (3), the method has high result accuracy, high precision and good repeatability; no light absorption value variation triggered by diversity of the extraction sequence or storage period during the measurement between standard curve series point solution and sample solution is caused; (4), the method is also suitable for the measurement of antimony in lead alloy; and (5), only simple and convenient spectrophotometer is used, the cost is low, and the method is particularly suitable for production units.

Description

technical field [0001] The invention belongs to the field of nonferrous metallurgy, and in particular relates to a method for improving the accuracy and precision of determining trace antimony in metallic lead. Background technique [0002] The content of antimony in metallic lead is very small, usually in the range of 0.000X to 0.0X%. At present, the main methods of determination are direct reading spectroscopy, plasma emission spectrometry, hydride-atomic fluorescence method, spectrophotometry and so on. Although the results of direct reading spectroscopy and plasma emission spectroscopy are relatively accurate, the equipment is expensive, and high-purity nitrogen gas is required, which is high in cost; although the hydride-atomic fluorescence method has high sensitivity and precision of measurement results, the results are reliable, but it requires It is equipped with a hydride generating device, and the operation is tedious and the cost of use is high; the latest effect...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
01 May 2013
Publication
CN103076293A
IPC
G01N21/31; G01N1/28
Inventors
吴敏; ζ’ι‡‘ι£Ž