CN101609047A - The assay method of antimony in a kind of electric equipment products - Google Patents
The assay method of antimony in a kind of electric equipment products Download PDFInfo
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- CN101609047A CN101609047A CNA2009100878388A CN200910087838A CN101609047A CN 101609047 A CN101609047 A CN 101609047A CN A2009100878388 A CNA2009100878388 A CN A2009100878388A CN 200910087838 A CN200910087838 A CN 200910087838A CN 101609047 A CN101609047 A CN 101609047A
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Abstract
The present invention relates to a kind of by the assay method of inductively coupled plasma atomic emission spectrometer to antimony in the electric equipment products.Be to add nitric acid in the metal species sample, hydrogen peroxide and hydrochloric acid solution, the plastics sample adds sulfuric acid, nitric acid and superoxol heating are cleared up, antimony extracts from electric equipment products with the form of ion under acid condition, uses inductively coupled plasma atomic emission spectrometer that sample treatment solution is measured then.Adopt the content of antimony in the method detected electrons electric equipment products of the present invention, fast effectively, relative average debiation is less than 5%, this shows, method of the present invention, be the content of antimony in the detected electrons product, a kind of method of implementing be convenient to reliably is provided, can satisfy of the management and control of electronic apparatus manufacturing enterprise for objectionable impurities antimony and compound thereof.
Description
Technical field
The present invention relates to a kind of assay method, particularly relate to a kind of by the assay method of inductively coupled plasma atomic emission spectrometer to antimony in the electric equipment products to antimony in the electric equipment products.
Background technology
Antimony can stimulate people's eye, nose, throat and skin, and lasting contact can destroy heart and liver function, and the antimony of suction high-load can cause the antimony acute poisoning, causes after the suction that the upper respiratory tract stimulates, has a headache, feels sick, vomits, has difficulty in breathing.Eyes and skin there is pungency.Cause GI irritation after the absorption, feel sick, vomiting, oral cavity and throat burn and central nervous system suppress.Severe patient may be dead.Slow poisoning can cause liver, renal damage.Blood pressure change and electrocardiographic abnormality appear in long-term contact.Can cause skin lesion, cause dry skin, chap, also dermatitis or eczema can occur.
2008, Green Peace uses according to stricter chemical substance and electronic waste reclaims standard (comprising new standard) and newly-installed standard of energy is marked, and a newly-increased key name is the standard of " progressively eliminating additive material and timetable thereof ".So-called additive material comprises much being defined as the superseded suspicious noxious material of needs in the future by some brand, comprising antimony and antimonial.Electronic apparatus enterprise bears the financial responsibility of the electronic waste of handling its brand, and is responsible for being responsible for reclaiming reject product at the All Countries of selling its product, and is re-used or recycle.Electric equipment products is of a great variety, the material complexity, do not have good check and analysis method for antimony at present, thus the utmost point be necessary to set up a kind of fast, accurately, convenient and economic detection method, satisfy of the management and control of electronic apparatus manufacturing enterprise for objectionable impurities antimony and compound thereof.Stop using noxious material, and then reduce processing cost.
Summary of the invention
Technical matters to be solved by this invention is, a kind of assay method to antimony in the electric equipment products is provided.
For achieving the above object, the present invention takes following design proposal:
What the present invention relates to is a kind of by the assay method of inductively coupled plasma atomic emission spectrometer to antimony in the electric equipment products, comprises the steps:
Sample is crossed 80 mesh sieves after pulverizing evenly.
The metal species sample takes by weighing 0.5g ± 0.1g and prepares sample, place the 250ml triangular flask, add the nitric acid of 10ml (1+1), bottleneck is put little funnel and is added a cover surface plate, is placed on 200 ℃ of heating on the electric hot plate, digestion solution reduces to about 5ml and takes off, be cooled to room temperature, carefully add the 5ml red fuming nitric acid (RFNA), continue to clear up, repeat this step and add red fuming nitric acid (RFNA) 15ml altogether, do not have brown cigarette up to sample.After treating that sample cools off fully, slowly add 2ml hydrogen peroxide (the bubbling phenomenon will appear in the adding of hydrogen peroxide).Taking off cooling fully when clearing up sample to the 5ml left and right sides, carefully add the 3ml hydrogen peroxide and continue to clear up, is that 5ml takes off cooling (annotating: add the hydrogen peroxide cumulative volume and must not surpass 10ml) to liquor capacity.Carefully add hydrochloric acid 5ml again, heated 15 minutes.Sample should dissolve or be out of shape this moment.Cooling is settled in the 50ml volumetric flask to be measured with deionized water, if any the residue filter paper filtering, blank assay is made in the machine test simultaneously on the filtrate.
The plastics sample accurately takes by weighing 0.5g ± 0.1g and prepares sample, place the 250ml triangular flask, slowly add the 10ml concentrated sulphuric acid, bottleneck is put little funnel and is added a cover surface plate, being placed on the electric furnace 400 ℃ heats and clears up, sample dissolution sulfuric acid cigarette is caught up with to the greatest extent, takes off cooling, carefully adds the 5ml red fuming nitric acid (RFNA), substantially clarify until sample and to take off, cooling adds the 5ml hydrogen peroxide, continues to be heated to the sample clarification and takes off.(do not clarify as sample, need add equivalent nitric acid and continue to clear up, clarify to solution.) cooling is settled in the 50ml volumetric flask to be measuredly with deionized water, if any the residue filter paper filtering, machine is tested on the filtrate, makes blank assay simultaneously.
Press concentration gradient order from low to high with inductively coupled plasma atomic emission spectrometer, measure the spectral emissions intensity of object element in the serial solution of calibration, concentration with calibration solution is horizontal ordinate, is that ordinate is drawn calibration curve with the signal intensity of element to be measured.Calibration curve detects blank solution and sample treatment solution after setting up.
Result of calculation, the computing formula of antimony is in the sample:
The content of antimony in the X-sample, unit are every kilogram (mg/kg) of milligram;
C
0-blank solution concentration, unit is every liter (mg/l) of milligram;
C
1-sample solution concentration, unit is every liter (mg/l) of milligram;
V-constant volume, unit are milliliter (ml);
F-sample solution extension rate;
The m-sample quality, unit is gram (g).
Preferably, sample is crossed 80 mesh sieves after pulverizing evenly, take by weighing 0.5g ± 0.1g.
Preferably, the metal species sample adds the 15ml red fuming nitric acid (RFNA) altogether, 10ml hydrogen peroxide, 5ml hydrochloric acid; The plastics sample adds the 10ml concentrated sulphuric acid, 5ml red fuming nitric acid (RFNA), 5ml hydrogen peroxide.
Preferably, 200 ℃ of heating of metal species sample electric hot plate are cleared up; 400 ℃ of heating of plastics sample electric furnace are cleared up.
The described condition of utilizing inductively coupled plasma atomic emission spectrometer to detect is:
Incident power: 1200W
Atomization gas pressure: 0.18Mpa
Secondary air amount: 0.5L/min
Observed altitude: 12mm
Pump speed: 30rpm
And according to the typical curve standard measure.
Advantage of the present invention is: adopt the content of antimony in the method detected electrons electric equipment products of the present invention, effectively, RSD detects and is limited to 1mg/kg less than 5% fast, and concentration limit is 0.01mg/l.This shows that method of the present invention is the content of antimony in the detected electrons product, a kind of method of implementing be convenient to reliably is provided, can satisfy of the management and control of electronic apparatus manufacturing enterprise for objectionable impurities antimony and compound thereof.
Embodiment
Embodiment 1, and the precision of antimony content and the recovery detect in the alloy material:
The testing sample of crossing 80 mesh sieves after the drying and crushing takes by weighing 0.5025g, place the 250ml triangular flask, the nitric acid that adds 10ml (1+1), bottleneck is put little funnel and is added a cover surface plate, is placed on 200 ℃ of heating on the electric hot plate, and digestion solution reduces to about 5ml and takes off, be cooled to room temperature, the careful 10ml red fuming nitric acid (RFNA) that adds continues to clear up, and does not have brown cigarette up to sample.After treating that sample cools off fully, slowly adding the 2ml hydrogen peroxide, take off cooling fully when clearing up sample to the 5ml left and right sides, carefully add the 3ml hydrogen peroxide and continue to clear up, is that 5ml takes off cooling to liquor capacity.Carefully add hydrochloric acid 5m l again, heated 15 minutes, sample dissolves.Cooling is settled in the 50ml volumetric flask to be measured with deionized water, make blank assay simultaneously.
Use the antimony standard reserving solution: single element solution composition analytical standard material antimony, 500mg/L, medium 25%H
2SO
4Preparation antimony working solution, concentration gradient 0.0mg/L, 0.1mg/L, 0.5mg/L, 1.0mg/L, 5.0mg/L, 10.0mg/L:5%H
2SO
4Medium.
Detecting instrument is existing THERMO iCAP6300 inductively coupled plasma atomic emission spectrometer;
Testing conditions is:
Incident power: 1200W
Atomization gas pressure: 0.18Mpa
Secondary air amount: 0.5L/min
Observed altitude: 12mm
Pump speed: 30rpm
According to the typical curve standard measure.
Result of calculation, the computing formula of antimony is in the sample:
The content of antimony in the X-sample, unit are every kilogram (mg/kg) of milligram;
C
0-blank solution concentration, unit is every liter (mg/l) of milligram;
C
1-sample solution concentration, unit is every liter (mg/l) of milligram;
V-constant volume, unit are milliliter (ml);
F-sample solution extension rate;
The m-sample quality, unit is gram (g).
Through calculating, the result is:
The content of antimony by formula calculates in the sample, and the result is as follows:
Embodiment 2, and the precision of antimony content and the recovery detect in the plastic sheet:
The testing sample of crossing 80 mesh sieves after the drying and crushing takes by weighing 0.5002g, place the 250ml triangular flask, slowly add the 10ml concentrated sulphuric acid, bottleneck is put little funnel and is added a cover surface plate, being placed on the electric furnace 400 ℃ heats and clears up, the sulfuric acid cigarette is caught up with most sample dissolution, takes off cooling, carefully adds the 5ml red fuming nitric acid (RFNA), substantially clarify until sample and to take off, cooling adds the 5ml hydrogen peroxide, continues to be heated to the sample clarification and takes off.Cooling is settled in the 50ml volumetric flask to be measured with deionized water, make blank assay simultaneously.
Use the antimony standard reserving solution: single element solution composition analytical standard material antimony, 500mg/L, medium 25%H
2SO
4Preparation antimony working solution, concentration gradient 0.0mg/L, 0.1mg/L, 0.5mg/L, 1.0mg/L, 5.0mg/L, 10.0mg/L:5%H
2SO
4Medium.
Detecting instrument is existing THERMO iCAP6300 inductively coupled plasma atomic emission spectrometer;
Testing conditions is:
Incident power: 1200W
Atomization gas pressure: 0.18Mpa
Secondary air amount: 0.5L/min
Observed altitude: 12mm
Pump speed: 30rpm
According to the typical curve standard measure.
Result of calculation, the computing formula of antimony is in the sample:
The content of antimony in the X-sample, unit are every kilogram (mg/kg) of milligram;
C
0-blank solution concentration, unit is every liter (mg/l) of milligram;
C
1-sample solution concentration, unit is every liter (mg/l) of milligram;
V-constant volume, unit are milliliter (ml);
F-sample solution extension rate;
The m-sample quality, unit is gram (g).
The content of antimony by formula calculates in the sample, and the result is as follows:
Obviously, those of ordinary skill in the art can be with of the present invention a kind of by the assay method of inductively coupled plasma atomic emission spectrometer to antimony in the electric equipment products.
The foregoing description is only for the usefulness that the present invention is described; and be not to be limitation of the present invention; the those of ordinary skill in relevant technologies field; without departing from the present invention; can also make various variations and modification; therefore all technical schemes that are equal to also should belong to category of the present invention, and scope of patent protection of the present invention should be limited by each claim.
Claims (7)
1, the present invention relates to a kind ofly by the assay method of inductively coupled plasma atomic emission spectrometer to antimony in the electric equipment products, it is characterized in that: described assay method comprises the steps:
1. specimen preparation:
Sample is crossed 80 mesh sieves after pulverizing evenly.
The metal species sample takes by weighing 0.5g ± 0.1g and prepares sample, place the 250ml triangular flask, add the nitric acid of 10ml (1+1), bottleneck is put little funnel and is added a cover surface plate, is placed on 200 ℃ of heating on the electric hot plate, digestion solution reduces to about 5ml and takes off, be cooled to room temperature, carefully add the 5ml red fuming nitric acid (RFNA), continue to clear up, repeat this step and add red fuming nitric acid (RFNA) 15ml altogether, do not have brown cigarette up to sample.After treating that sample cools off fully, slowly add 2ml hydrogen peroxide (the bubbling phenomenon will appear in the adding of hydrogen peroxide).Taking off cooling fully when clearing up sample to the 5ml left and right sides, carefully add the 3ml hydrogen peroxide and continue to clear up, is that 5ml takes off cooling (annotating: add the hydrogen peroxide cumulative volume and must not surpass 10ml) to liquor capacity.Carefully add hydrochloric acid 5ml again, heated 15 minutes.Sample should dissolve or be out of shape this moment.Cooling is settled in the 50ml volumetric flask to be measured with deionized water, if any the residue filter paper filtering, blank assay is made in the machine test simultaneously on the filtrate.
The plastics sample accurately takes by weighing 0.5g ± 0.1g and prepares sample, place the 250ml triangular flask, slowly add the 10ml concentrated sulphuric acid, bottleneck is put little funnel and is added a cover surface plate, being placed on the electric furnace 400 ℃ heats and clears up, sample dissolution sulfuric acid cigarette is caught up with to the greatest extent, takes off cooling, carefully adds the 5ml red fuming nitric acid (RFNA), substantially clarify until sample and to take off, cooling adds the 5ml hydrogen peroxide, continues to be heated to the sample clarification and takes off.(do not clarify as sample, need add equivalent nitric acid and continue to clear up, clarify to solution.) cooling is settled in the 50ml volumetric flask to be measuredly with deionized water, if any the residue filter paper filtering, machine is tested on the filtrate, makes blank assay simultaneously.
2. go up the machine test: utilize inductively coupled plasma atomic emission spectrometer that standard solution, blank solution and sample treatment solution are detected.
2, according to claim 1 a kind of by the assay method of inductively coupled plasma atomic emission spectrometer to antimony in the electric equipment products, it is characterized in that: sample is crossed 80 mesh sieves after pulverizing evenly, have the best under this condition and clear up effect.
3, according to claim 1 a kind of by the assay method of inductively coupled plasma atomic emission spectrometer to antimony in the electric equipment products, it is characterized in that: with nitric acid, hydrogen peroxide and hydrochloric acid solution system are cleared up in the metal species sample; The plastics sample is with sulfuric acid, and nitric acid and superoxol system are cleared up, and have the best under this condition and clear up effect.
4, according to claim 1 a kind of by the assay method of inductively coupled plasma atomic emission spectrometer to antimony in the electric equipment products, it is characterized in that: the metal species sample adds the 15ml red fuming nitric acid (RFNA) altogether, 10ml hydrogen peroxide, 5ml hydrochloric acid; The plastics sample adds the 10ml concentrated sulphuric acid, 5ml red fuming nitric acid (RFNA), 5ml hydrogen peroxide.
5, according to claim 1 a kind of by the assay method of inductively coupled plasma atomic emission spectrometer to antimony in the electric equipment products, it is characterized in that: 200 ℃ of heating of metal species sample electric hot plate are cleared up; 400 ℃ of heating of plastics sample electric furnace are cleared up.
6, according to claim 1 a kind of by the assay method of inductively coupled plasma atomic emission spectrometer to antimony in the electric equipment products, it is characterized in that: the described condition of utilizing inductively coupled plasma atomic emission spectrometer to detect is:
Incident power: 1200W
Atomization gas pressure: 0.18Mpa
Secondary air amount: 0.5L/min
Observed altitude: 12mm
Pump speed: 30rpm
7, according to claim 1 a kind of by the assay method of inductively coupled plasma atomic emission spectrometer to antimony in the electric equipment products, it is characterized in that: antimony extracts from electric equipment products with the form of ion under acid condition, uses inductively coupled plasma atomic emission spectrometer that sample treatment solution is measured then.Adopt the content of antimony in the method detected electrons electric equipment products of the present invention, fast effectively, relative average debiation is less than 5%, this shows, method of the present invention, be the content of antimony in the detected electrons product, a kind of method of implementing be convenient to reliably is provided, can satisfy of the management and control of electronic apparatus manufacturing enterprise for objectionable impurities antimony and compound thereof.
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| CN2009100878388A CN101609047B (en) | 2009-06-24 | 2009-06-24 | Method for measuring stibium in electronic and electrical products |
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| CN2009100878388A CN101609047B (en) | 2009-06-24 | 2009-06-24 | Method for measuring stibium in electronic and electrical products |
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| CN101609047B CN101609047B (en) | 2011-04-13 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101963594A (en) * | 2010-08-13 | 2011-02-02 | 同济大学 | Method for analyzing trace antimony in solid environmental sample |
| CN102393387A (en) * | 2011-11-10 | 2012-03-28 | 西安航空动力股份有限公司 | Method for analyzing surface silver coating components of high-temperature alloy GH4169 part |
| CN108318476A (en) * | 2018-05-09 | 2018-07-24 | 郭秀娟 | The ICP-AES measurement methods of micro- antimony content in a kind of ferro-molybdenum |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102323130A (en) * | 2011-08-30 | 2012-01-18 | 上海华碧检测技术有限公司 | Pre-processing method of rubber material element detection |
-
2009
- 2009-06-24 CN CN2009100878388A patent/CN101609047B/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101963594A (en) * | 2010-08-13 | 2011-02-02 | 同济大学 | Method for analyzing trace antimony in solid environmental sample |
| CN102393387A (en) * | 2011-11-10 | 2012-03-28 | 西安航空动力股份有限公司 | Method for analyzing surface silver coating components of high-temperature alloy GH4169 part |
| CN102393387B (en) * | 2011-11-10 | 2013-04-24 | 西安航空动力股份有限公司 | Method for analyzing surface silver coating components of high-temperature alloy GH4169 part |
| CN108318476A (en) * | 2018-05-09 | 2018-07-24 | 郭秀娟 | The ICP-AES measurement methods of micro- antimony content in a kind of ferro-molybdenum |
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| CN101609047B (en) | 2011-04-13 |
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