CN101349646B - Method for measuring impurity in high pure gold by plasma atomic emission spectrometer - Google Patents
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Abstract
The invention relates to a method for using a plasma atomic emission spectrometer to measure impurities in high-purity gold, which comprises the following steps: weighing one unit of sample in a bunsen beaker, adding aqua regia to dissolve, replenishing hydrochloric acid deionized water to do constant volume to a scale after dissolving, respectively getting sample solution in more than two colorimetric tubes, solution in each tube is 15ml, adding gold standard solution which is mixed by elements according to a multiple relation in turn, doing constant volume by deionized water, starting the plasma atomic emission spectrometer, starting a circulating water pump, opening analytic control software, entering a 'standard addition method' control procedure, choosing a spectral line for measuring in a spectral line base, setting the concentration value of curved lines, scanning a whole band, sucking sample solution in each colorimetric tube in an instrument in turn according to the sequence that the concentration is from low to high, clicking a feeler switch to get an initial curve point of the point after sucking in each time, assuring curved lines, and leading the linear coefficient to be more than 0.99, outputting the concentration value result of each determined element, and calculating the result of the percentage content of each determined element according to the calculating formula.
Description
Technical field
The present invention relates to a kind of determination techniques of precious metal material, relate in particular to a kind of method of measuring impurity in the High Purity Gold with plasma atomic emission spectrometer.
Background technology
Development along with domestic and international analysis and detection technology, each detects enterprise for adapting to the also corresponding analyzing and testing level that has improved its product of market cut-throat competition, the analytical approach (mainly measuring Ag in the High Purity Gold, Bi, Cr, Pb, Sb, Pd, Si, Mg, Cu, Fe, Ni, Mn, As, the Sn content of totally 14 kinds of impurity) of China's High Purity Gold is carried out according to standard GB/T11066-89 at present, its analytical instrument is mainly Atomic Absorption Spectrometer and arc source emission spectrometer, the sample analysis complex disposal process, length consuming time, it is more to consume reagent and glassware.
In the assay method of impurity element, spectrophotometric method, atomic absorption spectrography (AAS) and arc excitation, spectrographic analysis method all have application in gold and alloy thereof.But these assay methods all have defective: the defective of preceding 2 kinds of assay methods is to remove to measure various impurity one by one, and total measurement result speed is slow; Arc excitation, taking the photograph spectrum, to measure the involutory golden composition influence of rule bigger, and the preparation standard sample needs matrixes such as High Purity Gold, and goldstandard and sample loss are relatively large.
The pre-treatment work of the assay method of High Purity Gold is a step very crucial in the whole analytical work, accounts for more than 2/3 time of whole mensuration process.Be easy to make sample to be subjected to " staining " by in the past assay method pattern in this course, thereby influence the authenticity of determination data.
Summary of the invention
The purpose of this invention is to provide a kind of method with impurity in the plasma atomic emission spectrometer mensuration High Purity Gold, but the suffered outside contamination of minimizing sample of its maximum possible, the authenticity height of detection.
For achieving the above object, the present invention takes following design proposal:
A kind of method with impurity in the plasma atomic emission spectrometer mensuration High Purity Gold, its method step is as follows:
1) presets clean test environment;
2) get High Purity Gold sample and clean sample, dried for standby;
3) sample that takes by weighing a unit adds chloroazotic acid in the 200ml quartz beaker, and the heating dissolution in low temperature is treated to change in the 100ml volumetric flask after sample dissolves fully, adds hydrochloric acid, to scale, obtains sample solution with the deionized water constant volume;
4) divide solution each 15ml in the 25ml color comparison tube more than two that materialses, become the multiple relation to add the goldstandard solution that each element to be measured mixes successively, use the deionized water constant volume; Obtain concentration sample solution from low to high;
5) plasma atomic emission spectrometer is started shooting preheating half an hour, the ON cycle water pump is opened analysis and Control software, and running parameter is set, and clicks " igniting " button, forms stable plasmatorch flame; Selection enters " standard addition method " control program, selects the spectral line be used to measure in the spectral line storehouse of 24 kinds of elements to be measured, and the concentration value of input curve each point carries out all band scanning, after finishing light path and proofreading and correct, sets the duplicate measurements number of times;
6) by the order of concentration from low to high the sample to be tested solution in each color comparison tube is sucked instrument successively, each time point " test " key that sucks, obtain the initial curve point of each element, after the curve affirmation to each curve point formation, click " result's output ", can draw the concentration value C of element to be measured on the data mode hurdle
n, try to achieve element percentage composition result to be measured according to the computing formula of element percentage composition to be measured.
Step 6) is confirmed to be meant selected curve linear coefficient more than 0.99 to curve, when the curve of measuring meets the requirements, can draw the concentration value of element to be measured, measures otherwise reselect the element that curve do not reach requirement.
Described constant volume is that dosing is reached normal capacity full scale (as using the 100ml volumetric flask, dosing is to 100ml).
Successfully (ICP-OES) is applied in the impurity determination method in the High Purity Gold with inductive coupling plasma emission spectrograph in the present invention.
Inductive coupling plasma emission spectrograph (hereinafter to be referred as ICP-OES) with inductively coupled plasma as excitaton source, be topmost, the most widely used analysis light source in Atomic Emission Spectral Analysis field, being applied in the assay method of High Purity Gold is innovation of the present invention, can play extraordinary mensuration effect.
Adopting " standard addition method " is to eliminate matrix to disturb the most effective way.
Goldstandard solution used in the determination test is:
Au standard 1:15% hydrochloric acid medium:
Ag、Cu、Fe、Be、Ca、Cd、Mg、Ni、Zn、Co、La、Pd、Si、Mn 10.0μg/ml
Pb、Sb、Bi、Cr、Al、As、Pt、Ce、Ge、Sn 20.0μg/ml
Au standard 2:10% hydrochloric acid medium
Ag、Cu、Fe、Be、Ca、Cd、Mg、Ni、Zn、Co、La、Pd、Si、Mn 0.50μg/ml
Pb、Sb、Bi、Cr、Al、As、Ce、Pt、Ge、Sn 1.00μg/ml
Because of the concentration height of Au standard 1, performance is more stable, easily stores, and generally stores for future use with Au standard 1 liquid, during mensuration Au standard 1 liquid is prepared into Au standard 2 liquid.
Advantage of the present invention is:
1, because the inductive coupling plasma emission spectrograph ICP-OES that is adopted in the inventive method has the higher detection limit, can accurately, accurately measure impurity in the high-purity material in conjunction with Chemical Decomposition and beneficiation technologies, the present invention has selected suitable spectral line, make inductive coupling plasma emission spectrograph under the prerequisite of eliminating the spectral line interference, the content of 24 kinds of trace impurity in can the single-time measurement High Purity Gold, not only can reduce workload, and finding speed is fast, the accuracy height, precision is good.
2, the minimizing of pre-treating method used in the present invention and experiment condition maximum possible the suffered outside contamination of sample, so detect the authenticity height.
3, assay method process of the present invention is short, and needs the High Purity Gold matrix of samples loss of detection usefulness little, has avoided the huge waste that causes economically.
Description of drawings
Fig. 1 is an affirmation curve map of measuring impurity Ca in the High Purity Gold with plasma atomic emission spectrometer
Embodiment
The method concrete steps that the present invention measures impurity in the High Purity Gold with plasma atomic emission spectrometer are as follows:
1, preset test environment:
Test experiments of the present invention should carry out in ten thousand grades of Clean Operating Labs.
2, cleaning sample:
Except that the High Purity Gold of sponge attitude, need sample to be boiled with hydrochloric acid, rinse dried for standby under infrared lamp well with deionized water.
It is good that used hydrochloric acid reagent answers top grade pure, and used deionized water is 18.2 mega-ohms, and the dried operation will be carried out in the organic glass glove box.
3, sample dissolution:
The sample that takes by weighing a unit adds chloroazotic acid in the 200ml quartz beaker, cover surface plate, is positioned over to heat low temperature (below 100 ℃) dissolving on the electric hot plate.Change in the 100ml volumetric flask when treating to be cooled to room temperature after sample dissolves fully, add a certain amount of hydrochloric acid, to scale, this moment, sample concentration was C with the deionized water constant volume.
4, the sample branch is got and the standard adding:
Divide solution each 15ml in some (more than two) 25ml color comparison tubes that materialses, become the multiple relation to add the goldstandard solution that each element mixes successively, use the deionized water constant volume; Obtain concentration sample solution from low to high.
Prove through repetition test, select four test points preferable, can satisfy fast measuring and measure accurately accordingly again.
5, use Instrument measuring:
A) plasma atomic emission spectrometer is started shooting preheating half an hour the ON cycle water pump;
Open analysis and Control software, running parameter be set:
Plant capacity: (1.0～1.3) Kw; Cooling gas flow (15～20) L/min; Secondary air amount: (1.0～2.0) L/min; Atomizing pressure: 50～60psi (1psi=6.89kPa); Sample pulling speed: (1.0～1.5) ml/min; Measure integral time: (2～6) s;
B) click " igniting " button, form stable plasmatorch flame;
C) select to enter " standard addition method " control program, in the spectral line storehouse of 24 kinds of elements to be measured, select to be applicable to the spectral line of mensuration, import the concentration value that each concentration of element goldstandard solution from low to high adds.
Prove that through repetition test it is preferable selecting as the spectral line in the following table 1:
Table 1--element wavelength to be measured:
| Element | Ag | Cu | Fe | Pb | Bi | Sb | Si | Pd |
| Wavelength nm | 328.0 | 324.7 | 259.9 | 220.3 | 223.0 | 217.5 | 251.6 | 324.2 |
| Element | Mg | As | Sn | Cr | Ni | Mn | Al | Be |
| Wavelength nm | 279.5 | 193.6 | 189.9 | 283.5 | 231.6 | 257.6 | 396.1 | 313.0 |
| Element | Ca | Cd | Co | Ce | La | Ge | Pt | Zn |
| Wavelength nm | 393.3 | 214.4 | 228.6 | 413.7 | 333.7 | 265.1 | 214.4 | 213.8 |
Select the spectral line in the table 1 for use, instrument signal to noise ratio is better, and the data of mensuration are accurate.
D) carry out all band scanning, after finishing light path and proofreading and correct, set duplicate measurements number of times (the measurement number of times of setting in the instrument mostly is 10 times most, generally is determined as 2 times～4 times and gets final product); The liquid to be measured (concentration from low to high) of each color comparison tube is sucked instrument successively by pump line, generate test point, each back point that sucks starts feeler switch; After these several test points are confirmed, make its linear coefficient, click " result's output ", can draw the concentration value C of each element to be measured respectively on the data mode hurdle more than 0.99
n(n is various impurity elements to be measured).
The principle of work of ICP-OES test is to be brought in the inductively coupled plasma after by control of computer software the sample solution that sucks being atomized into gasoloid earlier, molten through the past, evaporate, dissociate, ionization, excite, process such as radiation handles, by the signals collecting and the conversion of signals of light path system, just can sequentially determining go out the concentration value of tested element.
Wherein the Computer Processing Calculation Method is:
That is:
In assay method of the present invention, to measure with the point of the adding more than 2 o'clock, these add point and are the integral multiple of sample size.First of standard addition method is primary sample, second standard solution that adds the certain volume concentration known, and the addition of back is the integral multiple of second addition, by that analogy.The measurement of tested concentration of element in the primary sample, its data result key is this slope of a curve and intercept, and the absolute value of curve intercept is the concentration of tested element in the sample, and slope is 45 minimums when spending.So when obtaining curve, revise its curve, make linear coefficient more than 0.99, can reach the purpose of accurate mensuration.
Adopt the assay method of the invention described above, the impurity content in can the rapid and accurate determination High Purity Gold.
The present invention is described further below in conjunction with specific embodiment
Embodiment 1:
Impurity to a kind of high-purity spun gold material detects:
Concrete assay method step is as follows:
1, cleaning sample
Take by weighing high-purity spun gold of about 2g, boil sample 15min, rinse well, in having the organic glass glove box of infrared lamp, carry out drying with deionized water with (1+1) hydrochloric acid.
2, sample dissolution
Take by weighing high-purity spun gold sample 1.000g after the above-mentioned cleaning in the 100ml quartz beaker, add chloroazotic acid 15ml and cover surface plate and be positioned over low-temperature heat on the electric hot plate (about 60～80 ℃) dissolving.After treating that sample dissolves fully, change over to when being cooled to room temperature in the 100ml volumetric flask, add the hydrochloric acid of 5ml, to scale, the solution concentration value is C (C=0.01g/ml) with the deionized water constant volume.
3, the sample branch is got and the standard adding
Divide solution each 15ml in four 25ml color comparison tubes that materialses, add goldstandard 2 solution 0.00,1.00,2.00,4.00ml at four color comparison tubes successively.With deionized water constant volume (promptly reaching the 25ml full scale).
4, instrumentation
With after instrument preheating half an hour, the ON cycle water pump is opened analysis and Control software, it is 1.0Kw that plant capacity is set, cooling gas flow 18L/min, secondary air amount 1.0L/min, atomizing pressure 50psi (1psi=6.89kPa), sample pulling speed 1.0ml/min measures 3s integral time.Click " igniting " button, form stable plasmatorch flame.Selection enters the standard addition method control model, selects the spectral line of 24 kinds of elements to be measured, and choice of spectrum is pressed selected (i.e. the table 1) in the technical scheme,
Input curve concentration data value:
Ag, Cu, Fe, Be, Ca, Cd, Mg, Ni, Zn, Co, La, Pd, Si, Mn are 0.00,0.02,0.04,0.08 μ g/ml
Pb, Sb, Bi, Cr, Al, As, Ce, Pt, Ge, Sn are 0.00,0.04,0.08,0.16 μ g/ml
Carry out all band scanning then, the manganese mark liquid with 10 μ g/ml carries out the light path system correction again.Setting the duplicate measurements number of times again is 2 times, clicks the liquid of measuring four color comparison tubes to be measured (concentration from low to high) and sucks successively by pump line, generates four test points, and the curve of this some formation is proofreaied and correct affirmation, makes linear coefficient more than 0.99.
What Fig. 1 showed is the affirmation curve that obtains when measuring the Ca impurity element, and its linear coefficient is 0.998, clicks result's output, can draw the concentration value C of Ca element on the data mode hurdle
Ca
Respectively the element curve that will survey is confirmed that it is as follows to obtain concentration of element to be measured:
Table 2
| Element | Ag | Cu | Fe | Pb | Bi | Sb | Si | Pd |
| Concentration C n(μg/ml) | 0.0107 | 0.0072 | 0.0052 | 0.0061 | 0.0025 | 0.0012 | 0.0018 | 0.0025 |
| Element | Mg | As | Sn | Cr | Ni | Mn | Al | Be |
| Concentration C n (μ g/ml) | 0.0031 | 0.0011 | 0.0019 | 0.0028 | 0.0016 | 0.0024 | 0.0019 | 0.0052 |
| Element | Ca | Cd | Co | Ce | La | Ge | Pt | Zn |
| Concentration C n(μg/ml) | 0.0009 | 0.0025 | 0.0028 | 0.0012 | 0.0019 | 0.0031 | 0.0072 | 0.0022 |
According to computing formula
The content that obtains various elements to be measured at last is as follows:
| Element | Ag | Cu | Fe | Pb | Bi | Sb | Si | Pd |
| Percentage composition % | 1.8×10 -4 | 12×10 -4 | 8.7×10 -5 | 1.0×10 -4 | 4.2×10 -5 | 2.0×10 -5 | 3.0×10 -5 | 4.2×10 -5 |
| Element | Mg | As | Sn | Cr | Ni | Mn | Al | Be |
| Percentage composition % | 5.2×10 -5 | 1.8×10 -5 | 3.2×10 -5 | 4.7×10 -5 | 2.7×10 -5 | 4.0×10 -5 | 3.2×10 -5 | 8.7×10 -5 |
| Element | Ca | Cd | Co | Ce | La | Ge | Pt | Zn |
| Percentage composition % | 1.5×10 -5 | 4.2×10 -5 | 4.7×10 -5 | 2.0×10 -5 | 3.2×10 -5 | 5.2×10 -5 | 1.2×10 -4 | 3.7×10 -5 |
Claims (6)
1. measure the method for impurity in the High Purity Gold with plasma atomic emission spectrometer for one kind, it is characterized in that method step is as follows:
1) presets the laboratory of ten thousand grades of cleanings;
2) get the High Purity Gold sample, the High Purity Gold sample is boiled with hydrochloric acid, clean with 18.2 mega-ohms deionized water rinsings, dried for standby;
3) sample that takes by weighing a unit adds chloroazotic acid in the 200ml quartz beaker, and the heating dissolution in low temperature is treated to change in the 100ml volumetric flask after sample dissolves fully, adds hydrochloric acid, to scale, obtains sample solution with the deionized water constant volume;
4) divide solution each 15ml in the 25ml color comparison tube more than two that materialses, become the multiple relation to add the goldstandard solution that each element to be measured mixes successively, use the deionized water constant volume; Obtain concentration sample solution from low to high;
5) plasma atomic emission spectrometer is started shooting preheating half an hour, the ON cycle water pump is opened analysis and Control software, and running parameter is set, and clicks " igniting " button, forms stable plasmatorch flame; Selection enters " standard addition method " control program, selects the spectral line be used to measure in the spectral line storehouse of 24 kinds of elements to be measured, and the concentration value of input curve each point carries out all band scanning, after finishing light path and proofreading and correct, sets the duplicate measurements number of times;
6) by the order of concentration from low to high the sample to be tested solution in each color comparison tube is sucked instrument successively, each time point " test " key that sucks, obtain the initial curve point of each element, after the curve affirmation to each curve point formation, click " result's output ", can draw the concentration value C of element to be measured on the data mode hurdle
n, try to achieve element percentage composition result to be measured according to the computing formula of element percentage composition to be measured.
2. the method with impurity in the plasma atomic emission spectrometer mensuration High Purity Gold according to claim 1, it is characterized in that: all reagent are top grade purity, and sample adopts the infrared lamp drying, and drying process is carried out in the organic glass glove box.
3. the method with impurity in the plasma atomic emission spectrometer mensuration High Purity Gold according to claim 1 is characterized in that: divide solution each 15ml in 4 25ml color comparison tubes that materialses in the step 4), become the multiple relation to add goldstandard solution successively.
4. the method with impurity in the plasma atomic emission spectrometer mensuration High Purity Gold according to claim 1 is characterized in that the spectral line of selecting in the step 5) to be used for measuring is the spectral line of following table in the spectral line storehouse of 24 kinds of elements to be measured:
。
5. the method for measuring impurity in the High Purity Gold with plasma atomic emission spectrometer according to claim 1, it is characterized in that the running parameter that is provided with in the step 5): plant capacity is 1.0Kw, cooling gas flow 18L/min, secondary air amount 1.0L/min, atomizing pressure 50psi, sample pulling speed 1.0ml/min measures 3s integral time.
6. the method for measuring impurity in the High Purity Gold with plasma atomic emission spectrometer according to claim 1, it is characterized in that: step 6) is confirmed to be meant that selected curve linear coefficient is more than 0.99 to curve, when the curve of measuring meets the requirements, can draw the concentration value of element to be measured, measure otherwise reselect the element that curve do not reach requirement.
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| CN102565028A (en) * | 2010-12-31 | 2012-07-11 | 北京有色金属与稀土应用研究所 | Method for measuring impurities in 4-5N high-purity tin by plasma atomic emission spectrometer |
| CN103323446A (en) * | 2012-03-23 | 2013-09-25 | 北京有色金属与稀土应用研究所 | Determination method for arsenic content in gold arsenic alloy target material |
| CN102749320A (en) * | 2012-07-18 | 2012-10-24 | 西安航空动力股份有限公司 | Method for determining impurities in magnesium-neodymium alloy |
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| CN104677883A (en) * | 2015-02-02 | 2015-06-03 | 海南中航特玻科技有限公司 | Analytical method for measuring impurity content in tin sample |
| CN105372230A (en) * | 2015-09-30 | 2016-03-02 | 遵宝钛业有限公司 | Method for measuring tin in titanium tetrachloride through ICP-AES |
| CN105866102B (en) * | 2016-03-28 | 2019-03-08 | 超威电源有限公司 | A method of lanthanum element content in lead or metal is measured with plasma emission spectrum |
| CN106018382A (en) * | 2016-05-17 | 2016-10-12 | 深圳市宁深检验检测技术有限公司 | Method for rapidly testing impurity elements in high-purity gold |
| CN109374599A (en) * | 2018-10-30 | 2019-02-22 | 金川集团股份有限公司 | The rapid assay methods of 20 kinds of impurity elements in a kind of ingot casting bronze |
| CN110907527A (en) * | 2019-12-16 | 2020-03-24 | 重庆市计量质量检测研究院 | Method for measuring content of impurity elements in high-purity gold jewelry |
| CN110987907A (en) * | 2019-12-18 | 2020-04-10 | 北京达博有色金属焊料有限责任公司 | Method for simultaneously measuring cerium content and lanthanum content in gold alloy by using plasma atomic emission spectrometry |
| CN113109322A (en) * | 2021-04-15 | 2021-07-13 | 山东省海洋资源与环境研究院(山东省海洋环境监测中心、山东省水产品质量检验中心) | Method for determining main heavy metal elements in marine organisms |
| CN115112520B (en) * | 2022-07-07 | 2023-09-29 | 山东招金金银精炼有限公司 | Analysis method for gold content in cyanide-free hard gold |
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Assignee: Beijing Doublink Solders Co., Ltd. Assignor: Beijing Non-ferrous Metal and Rare-earth Application Inst. Contract record no.: 2010110000199 Denomination of invention: Method for measuring impurity in high pure gold by plasma atomic emission spectrometer Granted publication date: 20100908 License type: Exclusive License Open date: 20090121 Record date: 20101111 |
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Assignee: Beijing Doublink Solders Co., Ltd. Assignor: Beijing Non-ferrous Metal and Rare-earth Application Inst. Contract record no.: 2010110000199 Date of cancellation: 20140917 |
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