CN103323446A - Determination method for arsenic content in gold arsenic alloy target material - Google Patents
Determination method for arsenic content in gold arsenic alloy target material Download PDFInfo
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Abstract
The invention relates to a determination method for the arsenic content in a gold arsenic alloy target material. The determination method employs an inductively coupled plasma atomic emission spectrometry, and includes: (1) dissolving a sample by aqua regia at the low temperature, steaming to nearly dry, and adding hydrochloric acid to remove nitric oxides; (2) diluting with deionized water, and shaking uniformly; (3) starting up a plasma atomic emission spectrometer to pre-heat for half an hour, starting a circulating water pump, opening a analysis control software, setting working parameters, setting the power of 1.0-1.2 Kw, setting the atomization pressure of 46-55 psi, setting the optimum excitation region at a 12-18mm position of a torch, selecting the spectral line of 193.695 nm of arsenic, then clicking an ignition button, and forming a stable plasma torch flame; and (4) successively determining a standard solution and the sample solution to obtain the concentration value of the arsenic element to be measured in a data status bar, and acquiring the percent content of the arsenic element according to a calculation formula of the percent content of an element to be measured. The determination method has the advantages of good accuracy, high precision, and convenient and fast operation.
Description
Technical field
The present invention relates to the assay method of arsenic amount in a kind of gold-arsenic alloy target, be specially a kind of method of utilizing inductively coupled plasma emission spectrography to measure arsenic amount in the gold-arsenic alloy target.
Background technology
Gold-arsenic alloy target (being called for short golden arsenic target) is that a kind of deelectric transferred and anti-electrocorrosion performance is good and have the more stable P.L.S. wave band silicon power transistor metallization material of alloy, and the performance of this target directly affects the quality of components and parts.Along with China's industrial expansion, to the also constantly increase of demand of gold-arsenic alloy target.Arsenic content adds what state in the gold arsenic target, and how homogeneity all can affect the performance of target, therefore accurately, fast detects arsenic content in the gold-arsenic alloy target, is very important for the gold-arsenic alloy target.Because according to testing result, can change the disposal route of technique, finally determine perfect technological process.
The mensuration of arsenic amount in the gold-arsenic alloy target does not also have corresponding chemical analysis method at present, and strong technical support can not be provided for the scientific research of gold-arsenic alloy target.
Summary of the invention
The purpose of this invention is to provide a kind of inductively coupled plasma emission spectrography and measure the method for arsenic amount in the gold-arsenic alloy target, utilize the ICP plasma emission spectrometer to measure arsenic amount in the gold-arsenic alloy target, for the research and production of gold-arsenic alloy target provide strong technical support.This method is measured the scope of arsenic content and is not only saved the loaded down with trivial details step of colourimetry but also save titrimetry and use various reagent, and this method accuracy is good, and precision is high, and is simple and efficient to handle.
For achieving the above object, the present invention takes following technical scheme:
The assay method of arsenic amount in a kind of gold-arsenic alloy target adopts the arsenic amount in the inductively coupled plasma emission spectrography mensuration gold-arsenic alloy target, comprises the steps:
(1) dissolving of sample: with gold-arsenic alloy target sample chloroazotic acid dissolution in low temperature, steam near doing (near wet salt shape), add hydrochloric acid and drive oxides of nitrogen, obtain sample solution;
(2) sample solution is diluted with deionized water, shake up;
(3) plasma atomic emission spectrometer is started shooting preheating half an hour, the ON cycle water pump, open analysis and Control software, running parameter is set, and power is 1.0～1.2Kw, and atomizing pressure is 46～55psi, best lasing region is in torch 12～18mm position, the spectral line of selected arsenic 193.695nm is clicked " igniting " button, forms stable plasmatorch flame;
(4) sequentially determining typical curve solution reaches sample solution, draws the concentration value of element arsenic to be measured on the data mode hurdle, tries to achieve the arsenic element percentage composition according to the computing formula of element percentage composition to be measured.
Step (1), the dissolving of sample: take by weighing 0.1 weight portion gold-arsenic alloy target sample, with the chloroazotic acid of 8～10 weight portions in 50～60 ℃ of dissolvings of low temperature, steam near doing (near wet salt shape), the hydrochloric acid that adds 5 weight portions is driven oxides of nitrogen, and cooling obtains sample solution.
Step (2), arsenic massfraction are transferred to sample solution in the 100mL volumetric flask 0.10%～0.40% the time, are diluted to scale with deionized water, shake up; The arsenic massfraction is transferred to sample solution in the 100mL volumetric flask 0.40%～3.00% the time, is diluted to scale with deionized water, shakes up, and then pipettes the 10.00mL mentioned solution in the 100mL volumetric flask, is diluted to scale with deionized water, shakes up.
Step (3), described power are 1.1Kw, and atomizing pressure is 50psi, and best lasing region is in torch 15mm position.
This method utilizes the ICP plasma emission spectrometer to measure arsenic content in the golden arsenic target, wherein relates to the degree of molten sample, the optimization of light source, and the aspects such as method that wavelength is selected comprise:
1, select the arsenic element analysis spectral line, gold element measures to arsenic whether typical curve influential and arsenic is determined scope in the beta alloy.The method that wavelength is selected, ICP light source usually can produce spectrum and disturb, and main manifestations is the background drift, partially or completely the impact of spectrum covering and matrix.Arsenic element all band scanning in the standard solution of arsenic element and the blank reagent solution is compared and analyzes, in arsenic 193.695nm place blank solution, do not have the strength signal peak of arsenic, do not have matrix to drift about.
2, the mensuration of arsenic element is selected setting and the optimization of various parameters, such as RF power, atomizer pressure, height of observation etc.
3, sequentially determining accuracy and precision have been carried out the test of system, formulate method of testing.
Advantage of the present invention:
1, the inductive coupling plasma emission spectrograph that adopts among the present invention not only can reduce workload, and finding speed is fast, and accuracy is high, and precision is good.
2, the present invention uses reagent to only have hydrochloric acid and nitric acid, does not need other reagent, and bottom line avoids interference material and introduces.
3, the invention provides with inductive coupling plasma emission spectrograph mensuration semimetallic elements instrument condition.
The present invention has carried out experimental study to arsenic amount in the employing inductively coupled plasma emission spectrography mensuration gold-arsenic alloy target, the selection of arsenic element analysis spectral line, the problem that affects of matrix element, definite, the precision of typical curve have been carried out the test of system, formulated method of testing, successfully inductive coupling plasma emission spectrograph is applied in the gold-arsenic alloy target in the Spectrometric Determination Arsenic Content, and in scientific research, production application, has obtained preferably effect.By to a large amount of product analysis testing experiments, the result shows that this method accuracy is good, and precision is high, and is simple and efficient to handle.Precision: RSD＜3.0%, the sample recovery of standard addition exists: 99.2%～100.4%.
The present invention will be further described below by embodiment, but and do not mean that limiting the scope of the invention.
Embodiment
The assay method of arsenic amount in the gold-arsenic alloy target of the present invention utilizes the arsenic amount in the inductively coupled plasma emission spectrography mensuration gold-arsenic alloy target, comprising:
1, the dissolution mechanism of sample:
Sample steams to nearly wet salt shape with chloroazotic acid low temperature (50～60 degree) dissolving, adds hydrochloric acid and drives oxides of nitrogen (add hydrochloric acid and drive nitric acid).The analytical line place that determines at arsenic measures.
2, matrix effect:
Selected arsenic element scanning reagent blank, standard, sample are looked into and are seen if there is the spectrum interference.The matrix gold element does not affect mensuration in the mensuration, does not need Matrix Match, and coexisting substances does not disturb.
3, instrument parameter optimization:
The element arsenic that excites for difficult has carried out the optimization of three aspects:: 1) RF power at light source; 2) atomizer pressure; 3) exposure height.
4, the selection of analytical line:
The selection of analytical line is with highly sensitive, and disturbing is principle less, and all band to arsenic in sample, mark liquid scans, and determines at last optimal analytical line.
5, the drafting of working curve:
The content of determining not only will cover institute's test elements of working curve, be starting point but also will consider that arsenic element that the sample segregation causes is higher or on the low side, in the situation that instrument parameter is optimized, make linear r=0.9995 above for well, tested element true value infinite approach in measured value and sample during r=1 in theory, if it is larger poor that the accuracy of linear differential determination nature and true value have, cause the measurement result distortion.Show that by experiment measurement result can better satisfy the detection needs when linear r=0.9995 was above.The mensuration of method detection limit has been used the measurement and calculation method of the detection limit of ICP-AES.
6, the reliability of method, precision:
The reliability of method mainly adopts the method for reinforced recovery test to verify.The precision work of method is to take the mark liquid of same addition is carried out several mensuration, result of calculation.The result shows after tested, and precision is good.
Embodiment 1
1, sample dissolving
Take by weighing the 0.1000g sample, place the 250mL beaker, add the 8mL chloroazotic acid, cover the table ware, dissolving.Steam to the wet salt shape, add the 5mL concentrated hydrochloric acid and drive oxides of nitrogen, cooling.
2, sample part is got
The arsenic massfraction is transferred in the 100mL volumetric flask＞0.10%～0.40% the time, is diluted to scale with deionized water, shakes up.The massfraction of arsenic is transferred in the 100mL volumetric flask＞0.40%～3.00% the time, is diluted to scale with deionized water, shakes up; Pipette again this solution of 10.00mL in the 100mL volumetric flask, be diluted to scale with deionized water, shake up.
3, Instrument working parameter
Being chosen in of power makes in the situation that sample excites fully, makes lower the stable of plasma that can guarantee like this of power.Prove by experiment power when 1.0～1.2Kw, arsenic element signal intensity trend is identical, and when surpassing 1.3Kw, the arsenic element signal intensity descends.So power selection 1.1Kw.When atomizing pressure was lower than 46psi, the sample atomizing effect was low, was higher than 55psi and can causes again sample residence time in torch short, and atomizing pressure is when 50psi by experiment, and the change in signal strength of arsenic is little.Height of observation is for this difficult element that excites of arsenic, and the best lasing region by debugging it is in torch position on the low side, and such as 12～18mm position, the present embodiment selects best lasing region in torch 15mm position.
4, the selection of analytical line
Highly sensitive according to selected analysis spectral line, disturb few principle, carried out following experiment.The excitation temperature of ICP light source is having less chemistry to disturb more than 6000, usually can produce spectrum and disturb, and main manifestations is the background drift, partially or completely the impact of spectrum covering and matrix.Whether exist, arsenic element all band scanning in the standard solution of arsenic element and the blank reagent solution is compared and analyzes if determining at first that spectrum disturbs, do not have the strength signal peak of arsenic in arsenic 193.695nm place blank solution, do not have matrix to drift about.The strength signal peak of arsenic is fine in the standard solution, so use this spectral line to carry out analytical work.
5, matrix effect
In analytical test, remove arsenic element in the sample and also have the materials such as gold, is there interference in these non-detection elements? done following work for the research of disturbed condition: add respectively identical arsenic mark liquid in the proof gold sample solution neutralization reagent blank solution: 0.10,1.00,3.00 μ g/mL constant volumes are as 100mL, test figure such as following table 1.
Table 1 matrix effect and reagent determination data statistics
By experiment digital proof, arsenic 193.695nm spectral line is fit to, and matrix effect and reagent can not have considerable influence to the testing result accuracy, and graticule does not need Matrix Match.
6, method detection limit
In blank solution, measure 21 times with arsenic 193.695nm spectral line, obtain standard deviation b, use larger than blank value intensity, concentration is 0.05 μ g/mL arsenic mark liquid, records signal intensity X, obtains the signal intensity S=X/C of corresponding unit, with C=2 σ b/S, calculate detection lower limit test figure and see Table 2.
The data statistics of table 2 method detection limit
S＝X/C＝358699.04 C＝2σb/S＝0.0011
The method of arsenic element detects and is limited to 0.0011 μ g/mL, satisfies arsenic element analysis in the gold-arsenic alloy target.
7, method reliability
Because the standard substance of this kind alloy target material does not take the recovery to come the reliability of verification method.Test procedure with working sample is not measured calculate recovery rate in adding 0.10,1.00,3.00 μ g/mL arsenic mark liquid.Test figure sees Table 3.
Table 3 element average recovery rate statistics to be measured
The recovery of arsenic element difference is 99.2%～100.4%.By the test figure result, this method accuracy can be satisfied the detection needs.
8, the precision of method
To golden arsenic target sample, to carry out 10 times according to analytical procedure and measure, measurement result sees Table 4.
Table 4 precision
Relative standard deviation (RSD) is 0.70%.
9, the drafting of working curve:
Pipette 0,0.50,1.00,3.00,5.00mL arsenic standard solution (1.3.5) and place respectively one group of 100mL volumetric flask, each adds 8mL hydrochloric acid, is diluted to scale with deionized water, shakes up.
10, the calculating of analysis result
In the formula:
M: test portion weight (g);
m
1: tested element checks in a milligram number (μ g);
v
Always: overall solution volume (mL).
Embodiment 2
AuAs
0.3The mensuration of middle As:
With reference to the step among the embodiment 1.Take by weighing three parts on 0.1000g sample, place the 250mL beaker, add the 8mL chloroazotic acid, cover the table ware, dissolving.Steam to the nearly dried 5mL of adding hydrochloric acid and drive nitric acid, cool off.Transfer in the 100mL volumetric flask, be diluted to scale with deionized water, shake up.Sequentially determining arsenic typical curve under selected good Instrument working parameter, sample.Recording concentration value is: 3.02 μ g/ml, 2.86 μ g/ml, 2.94 μ g/ml, substitution formula gained sample result is respectively: 0.30%, 0.29%, 0.29%.
Claims (4)
1. the assay method of arsenic amount in the gold-arsenic alloy target adopts inductively coupled plasma emission spectrography to measure arsenic amount in the gold-arsenic alloy target, comprises the steps:
(1) dissolving of sample: with gold-arsenic alloy target sample chloroazotic acid dissolution in low temperature, steam near and do, add hydrochloric acid and drive oxides of nitrogen, obtain sample solution;
(2) sample solution is diluted with deionized water, shake up;
(3) plasma atomic emission spectrometer is started shooting preheating half an hour, the ON cycle water pump, open analysis and Control software, running parameter is set, and power is 1.0～1.2Kw, and atomizing pressure is 46～55psi, best lasing region is in torch 12～18mm position, the spectral line of selected arsenic 193.695nm is clicked " igniting " button, forms stable plasmatorch flame;
(4) sequentially determining typical curve solution reaches sample solution, draws the concentration value of element arsenic to be measured on the data mode hurdle, tries to achieve the arsenic element percentage composition according to the computing formula of element percentage composition to be measured.
2. the assay method of arsenic amount in the gold-arsenic alloy target according to claim 1, it is characterized in that: being dissolved as of described sample: take by weighing 0.1 weight portion gold-arsenic alloy target sample, with the chloroazotic acid of 8～10 weight portions 50～60 ℃ of dissolvings, steam near and do, the hydrochloric acid that adds 5 weight portions is driven oxides of nitrogen, cooling obtains sample solution.
3. the assay method of arsenic amount in the gold-arsenic alloy target according to claim 1 is characterized in that: the arsenic massfraction is transferred to sample solution in the 100mL volumetric flask 0.10%～0.40% the time, is diluted to scale with deionized water, shakes up; The arsenic massfraction is transferred to sample solution in the 100mL volumetric flask 0.40%～3.00% the time, is diluted to scale with deionized water, shakes up, and then pipettes the 10.00mL mentioned solution in the 100mL volumetric flask, is diluted to scale with deionized water, shakes up.
4. the assay method of arsenic amount in the gold-arsenic alloy target according to claim 1, it is characterized in that: described power is 1.1Kw, and atomizing pressure is 50psi, and best lasing region is in torch 15mm position.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103558209A (en) * | 2013-11-13 | 2014-02-05 | 北京达博有色金属焊料有限责任公司 | Method for measuring arsenic content of gold through plasma atomic emission spectrometry |
| CN112147209A (en) * | 2020-09-21 | 2020-12-29 | 中化地质矿山总局地质研究院 | Method for measuring arsenic in geochemical sample by ICP-MS |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101349646A (en) * | 2007-07-19 | 2009-01-21 | 北京有色金属与稀土应用研究所 | Method for measuring impurity in high pure gold by plasma atomic emission spectrometer |
| CN101748307A (en) * | 2008-12-19 | 2010-06-23 | 北京有色金属与稀土应用研究所 | Gold-arsenic alloy material and preparation method thereof |
-
2012
- 2012-03-23 CN CN201210080945XA patent/CN103323446A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101349646A (en) * | 2007-07-19 | 2009-01-21 | 北京有色金属与稀土应用研究所 | Method for measuring impurity in high pure gold by plasma atomic emission spectrometer |
| CN101748307A (en) * | 2008-12-19 | 2010-06-23 | 北京有色金属与稀土应用研究所 | Gold-arsenic alloy material and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| 中华人民共和国国家质量监督检验检疫总局 中国国家标准化管理委员会: "《中华人民共和国国家标准 GB/T 15072.11-2008》", 30 June 2008, article "贵金属合金化学分析方法 金合金中钆和铍量的测定 电感耦合等离子体原子发射光谱法", pages: 7.3 * |
| 中华人民共和国国家质量监督检验检疫总局 中国国家标准化管理委员会: "《中华人民共和国国家标准 GB/T 15072.18-2008》", 30 June 2008, article "贵金属合金化学分析方法 金合金中锆和镓量的测定 电感耦合等离子体原子发射光谱法", pages: 7.3 * |
| 中华人民共和国国家质量监督检验检疫总局 中国国家标准化管理委员会: "《中华人民共和国国家标准 GB/T 15072.7-2008》", 30 June 2008, article "贵金属合金化学分析方法 金合金中铬和铁量的测定 电感耦合等离子体原子发射光谱法", pages: 7.3 * |
| 郅富国: "电感耦合等离子体发射光谱法测定金砷靶材中砷量", 《有色金属与稀土应用》, no. 3, 31 December 2011 (2011-12-31), pages 1 - 4 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103558209A (en) * | 2013-11-13 | 2014-02-05 | 北京达博有色金属焊料有限责任公司 | Method for measuring arsenic content of gold through plasma atomic emission spectrometry |
| CN112147209A (en) * | 2020-09-21 | 2020-12-29 | 中化地质矿山总局地质研究院 | Method for measuring arsenic in geochemical sample by ICP-MS |
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Application publication date: 20130925 |