CN102564984A - Method for measuring and analyzing Ni (nickel) content in carbon material - Google Patents

Abstract

The invention relates to a method for measuring and analyzing the Ni (nickel) content in a carbon material. The method is characterized in that anhydrous sodium carbonate or/and boric acid is/are adopted as a fluxing agent(s), the ash of the burned carbon material is melted, then a test solution is leached by the use of a dilute hydrochloric acid solution, and Ni measurement is carried out through an air-acetylene lean-burn flame. The method for measuring and analyzing the Ni content in the carbon material has the advantages of simple operation method and high accuracy.

Description

Ni Determination on content analytical approach in a kind of carbon materials

One, technical field

The present invention relates to Ni Determination on content analytical approach in a kind of carbon materials, especially adopt the method for Ni content in the atomic absorption spectroscopy determination carbon materials.

Two, background technology

At present, Ni analysis on Content method in the unified carbon materials in the industry, some is more loaded down with trivial details to the processing of sample.The determination and analysis method of prior art Ni constituent content mainly adopts the principle of atomic emission spectrum; Utilization is seen general appearance and with reference to spectrogram and analysis mark; To the evaluation of testing oneself of the spectrum of sample emission; The undue on the one hand spectrogram that relies on of this method is if the spectrogram distortion is very big to result's influence; On the other hand, the matrix line of Ni constituent content and element line seldom, for the subtle change of constituent content, the evaluation of corresponding line strength is than can not embody, and makes that to measure result error very big.Therefore, invent that a kind of accuracy is high, Ni method for measuring and analyzing content simple to operate is the active demand of industry.

Three, summary of the invention

Technical matters to be solved by this invention provides Ni Determination on content analytical approach in the carbon materials that a kind of method of operating is simple, accuracy is high.

For realizing technical matters of the present invention; Concrete technical scheme is: Ni Determination on content analytical approach in a kind of carbon materials; With natrium carbonicum calcinatum or/and boric acid is made flux; After ash content after the carbon materials calcination carried out fusion, leach test solution, carry out the mensuration of nickel at the poor combustion property flame of air-acetylene with dilute hydrochloric acid solution.

The further technical scheme of the present invention is also to comprise carbon materials high temperature cineration step, takes by weighing an amount of carbon materials through grinding and is tiled in the porcelain boat, places the high temperature baking box slowly to rise to 750～900 ℃ by room temperature, and calcination is 1～3 hour under this temperature.

The further technical scheme of the present invention is with in the carbon materials of ashing is packed platinum crucible into, adds an amount of natrium carbonicum calcinatum or/and boric acid stirs afterwards 800～900 ℃ of fusions.

The further technical scheme of the present invention is with the cooling of the carbon materials after the fusion, adds dissolving with hydrochloric acid, moves in the volumetric flask and processes Sample A.

The further technical scheme of the present invention is that Ni Determination on content analytical procedure is in the Sample A:

A, obtain 25.00ml Sample A solution in the 100ml volumetric flask, add hydrochloric acid 2ml, be diluted to scale with water, mixing;

B, with test solution in (a) in atomic absorption spectrophotometer (AAS) wavelength 232.0nm place, with the poor combustion property flame of air-acetylene, return to zero with sample blank, the absorbance of measurement nickel is found corresponding nickel amount from working curve;

C, calculate Ni content by following formula:

$\mathrm{Ni}(\%)=\frac{m_1}{m}\×100$

In the formula: m ₁: nickel amount in the test solution that on working curve, checks in, g; M: take by weighing the quality of carbon materials, g.

The further technical scheme of the present invention is that said concentration of hydrochloric acid solution is 1+1.

The invention has the beneficial effects as follows:

1, assay method usable range of the present invention is wide, comprises nickel Determination on content and analysis in all carbon materialses such as petroleum coke, charcoal piece, pitch.

2, the method for the invention need be to pre-service such as sample filter, measures after can directly adding corresponding reagent.

3, the method for the invention is easy and simple to handle, developing time is short, and the deviation of measuring the result is little.

Four, embodiment

Describe embodiment of the present invention in detail below in conjunction with concrete experimental data.

The instrument and equipment that the present invention need use: disk mill, high temperature furnace, balance (0.1mg), porcelain boat, platinum crucible (with cover, 30ml), atomic absorption spectrophotometer (AAS), attach nickel hollow cathode lamp, graduated cylinder.

The configuration of main agents and sample:

1, natrium carbonicum calcinatum.

2, boric acid.

3, hydrochloric acid, 3mol/L, 1+1.

4, hydrogen peroxide, 1.10g/ml.

5, the preparation of Sample A: a, get tested carbon materials sample m in the disk grinding alms bowl, be ground into powder; B, accurately take by weighing, be put in the porcelain boat, pave through air dried ground sample 2.0000g (m); C, porcelain boat is put on the porcelain boat frame, frame is put in the high temperature box furnace fire door, fire door is left the into slit of air, slowly rise to 750～900 ℃, in calcination under this temperature 1～3 hour (pitch should keep about 20 minutes at low thermophase when burning) by room temperature; D, take out the porcelain boat cooling, the ash content in the porcelain boat is swept in the platinum crucible that 2.5g natrium carbonicum calcinatum and 0.5g boric acid are housed, carefully stir, cover and be placed in 800～900 ℃ of high temperature furnaces fusion 20 minutes; E, the crucible that will melt sample take out cooling from high temperature furnace, add the hydrochloric acid 30ml of 3mol/L, and sample is all dissolved, and are placed on the electric furnace and boil a few minutes fully like dissolving; In f, the test solution cooling immigration 100ml volumetric flask with dissolving, clean crucible, washing lotion moves in the volumetric flask, and constant volume shakes up and processes Sample A; G, do blank test in company with Sample A.

6, the preparation of nickel standard stock solution: take by weighing 1.0000g nickel, place the 400ml beaker, the cover upper surface ware; Add 50ml hydrochloric acid (1+1), drip an amount of hydrogen peroxide, slowly heating is dissolved nickel fully; Boil the several minutes hydrogen peroxide with decomposing excessive, cooling moves into solution in the 1000ml volumetric flask; Be diluted to scale with water, mix, this solution 1ml contains 1.0mg nickel.

7, the preparation of nickel standard solution: pipette 50.00ml nickel standard stock solution in the 1000ml volumetric flask, be diluted with water to scale, mix, this solution 1ml contains 50ug nickel.

8, the drafting of working curve:

Pipette 0,1.00,2.00,3.00; 4.00 5.00ml nickel standard solution respectively adds 2ml hydrochloric acid (1+1) in one group of 100ml volumetric flask, be diluted to scale with water; Mix, above-mentioned solution in atomic absorption spectrophotometer (AAS) wavelength 232.0nm place, with the poor combustion property flame of air-acetylene, is returned to zero so that standard is blank; With the absorbance of measuring measurement standard solution series under sample the same terms, be horizontal ordinate with the mass percent of nickel, absorbance is an ordinate, the drawing curve.

Concrete determination step and analytical approach:

Obtain 25.00ml Sample A solution in the 100ml volumetric flask, add hydrochloric acid (1+1) 2ml, be diluted to scale with water; Mixing; Above-mentioned test solution in atomic absorption spectrophotometer (AAS) wavelength 232.0nm place, with the poor combustion property flame of air-acetylene, is returned to zero with sample blank; Measure the absorbance of nickel, find corresponding nickel amount from working curve.

Be calculated as follows the percentage composition of nickel

$\mathrm{Ni}(\%)=\frac{m_1}{m}\×100$

In the formula, m ₁: m ₁: nickel amount in the test solution that on working curve, checks in, g; M: take by weighing the quality of carbon materials, g.

Tolerance between the laboratory: %

ω(Ni)	Tolerance
		0.0010～0.0050	0.0005
0.0050～0.0100	0.0010
		0.0100～0.0500	0.0050

Claims (6)

1. Ni Determination on content analytical approach in the carbon materials; It is characterized in that, with natrium carbonicum calcinatum or/and boric acid is made flux, the ash content after the carbon materials calcination carried out fusion after; Leach test solution with dilute hydrochloric acid solution, carry out the mensuration of nickel at the poor combustion property flame of air-acetylene.

2. Ni Determination on content analytical approach in a kind of carbon materials according to claim 1; It is characterized in that; Also comprise carbon materials high temperature cineration step; Take by weighing an amount of carbon materials through grinding and be tiled in the porcelain boat, place the high temperature baking box slowly to rise to 750～900 ℃ by room temperature, calcination is 1～3 hour under this temperature.

3. Ni Determination on content analytical approach is characterized in that in a kind of carbon materials according to claim 2, will in the carbon materials of ashing is packed platinum crucible into, add an amount of natrium carbonicum calcinatum or/and boric acid stirs afterwards 800～900 ℃ of fusions.

4. Ni Determination on content analytical approach is characterized in that in a kind of carbon materials according to claim 3, with the cooling of the carbon materials after the fusion, adds dissolving with hydrochloric acid, moves in the volumetric flask and processes Sample A.

5. Ni Determination on content analytical approach is characterized in that in a kind of carbon materials according to claim 4, and Ni Determination on content analytical procedure is in the Sample A:

A, obtain 25.00ml Sample A solution in the 100ml volumetric flask, add hydrochloric acid 2ml, be diluted to scale with water, mixing;

B, with test solution in (a) in atomic absorption spectrophotometer (AAS) wavelength 232.0nm place, with the poor combustion property flame of air-acetylene, return to zero with sample blank, the absorbance of measurement nickel is found corresponding nickel amount from working curve;

C, calculate Ni content by following formula:

$\mathrm{Ni}(\%)=\frac{m_1}{m}\×100$

In the formula: m ₁: nickel amount in the test solution that on working curve, checks in, g; M: take by weighing the quality of carbon materials, g.

6. Ni Determination on content analytical approach is characterized in that in a kind of carbon materials according to claim 5, and said concentration of hydrochloric acid solution is 1+1.