CN103645174A - Method for determining content of lead in Pt950 jewelry through microwave digestion-inductively coupled plasma-atomic emission spectrometry (ICP-AES) - Google Patents
Method for determining content of lead in Pt950 jewelry through microwave digestion-inductively coupled plasma-atomic emission spectrometry (ICP-AES) Download PDFInfo
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- CN103645174A CN103645174A CN201310688887.3A CN201310688887A CN103645174A CN 103645174 A CN103645174 A CN 103645174A CN 201310688887 A CN201310688887 A CN 201310688887A CN 103645174 A CN103645174 A CN 103645174A
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Abstract
The invention relates to a method for determining the content of lead in Pt950 jewelry through microwave digestion-inductively coupled plasma-atomic emission spectrometry (ICP-AES). The method comprises the following steps: digesting a to-be-tested sample through a microwave digester by using hydrochloric acid, nitric acid and hydrogen peroxide as digestion agents; diluting the to-be-tested sample to a certain volume to obtain a to-be-tested solution; performing a test on an ICP instrument according to an established method; performing calculation to obtain the content of the lead in the to-be-tested solution. According to the method, the sample can be easily treated, element loss in a digestion process is avoided, an analysis result is accurate, analysis requirements for the content of the lead in the Pt950 jewelry can be well met, and guarantee is provided for improvement of the quality of the Pt950 jewelry and control of the content of lead elements through a Pt950 jewelry processing enterprise.
Description
Technical field
The present invention relates to the detection method of lead content in Pt950 jewellery, relate in particular to the detection method that a kind of use micro-wave digestion-inductively coupled plasma atomic emission spectrum (ICP-AES) method is measured lead content in Pt950 Jewelry product.
Background technology
The toxic metals such as lead in Pt950 jewellery can be by the sweat etch of human body, slowly diffuse in skin, lead is general on the impact of human body, even the lead of Long Term Contact low concentration, also can cause the infringement of the systems such as immunity, reproduction, nerve, even cause canceration.Domestic jewellery during the safe association of U.S.'s consumer goods repeatedly requires to recall, recall that reason relates generally to lead, cadmium content exceeds standard.(particularly European Union) pays much attention to the harm of harmful element in the world, and WEEE instruction (2002/96EC), the RoHS instruction (2002/95/EC) of European Union all make strict rules and limit harmful element kind and content.The regulation > > standard (GB28480-2012) that China < < ornaments harmful element is limited the quantity of has made to lead element the regulation of limiting the quantity of, require content plumbous in jewellery must be less than 0.1%, in jewellery, the detection of harmful element more and more causes people's concern.
At present, people generally detect the lead content in ornaments according to the mensuration spectroscopic methodology > > standard (GB/T28021-2011) of the mensuration x ray fluorescence spectrometry > > standard (GB/T28020-2011) of < < ornaments harmful element and < < ornaments harmful element.X ray fluorescence spectrometry is subject to sample surfaces to have coating or affects greatly through factors such as chemical treatment, detection time, shape, area of detection, degree of uniformity, spectrum interference, to chemical sample preparation, requires difficulty high; While utilizing inductive coupling emission spectrometry (ICP-AES) to test to cadmium element, what use is to take the method for chloroazotic acid as the common electric hot plate heating of digestion agent, do not provide concrete micro-wave digestion condition, not only labour intensity is large, and reagent dosage is many, the length that expends time in, and lead element is easily lost, the accuracy of impact analysis result, in addition, what mensuration was selected is comparison method with standard, and precision of analysis is not as calibration curve method.
Summary of the invention
For existing deficiency in prior art, the present invention is proposed.
The object of the present invention is to provide the detection method that a kind of sample pretreating is simple, analysis result is measured lead content in Pt950 jewellery accurately.
To achieve these goals, the invention provides the method that a kind of micro-wave digestion-ICP-AES measures lead content in Pt950 jewellery, described method comprises the steps:
1) take the sample 0.05-0.15g shredding; be accurate to 0.1mg; be placed in micro-wave diminishing pot; add 2-4mL red fuming nitric acid (RFNA), 3-8mL concentrated hydrochloric acid and 2-5mL hydrogen peroxide, standing reaction 5-10min, builds lid; insert in protective sleeve and put safety spring sheet; compress whole counteracting tank, prepare blank sample simultaneously, then put into microwave dissolver and clear up.Clear up after EOP (end of program), be cooled to below 30 ℃, digestion solution is transferred in 100ml volumetric flask, with ultrapure water, repeatedly clean on a small quantity inner canister, washing lotion is incorporated in volumetric flask, with ultrapure water, is settled to scale, shakes up;
2) open ICP, after instrument igniting complete stability is good, according to the condition of work of ICP, set up the analytical approach of this sample,
According to formula:
In formula: the massfraction of this metallic element in w-sample, unit is ug/g
C
ithe mass concentration of this metallic element in-Specimen eliminating liquid, unit is ug/mL
C
0the mass concentration of this metallic element in-blank solution, unit is ug/mL
Constant volume after V-Specimen eliminating, unit is mL
M-takes sample quality, and unit is g
Can be calculated the lead content in Pt950 jewellery.
As preferably, described step 1) in, micro-wave digestion program is specially: clear up power 1000-1500W, temperature 120-170 ℃, heating-up time 5-10min, constant temperature time 10-20min.
As preferably, described step 2) in, inductive coupling plasma emission spectrograph condition of work is specially: emissive power is that 1100-1200W, argon pressure are that 0.4-0.6MPa, atomization gas pressure are that 24.0-28.0L/min, flushing pump speed are that 90-110r/min, analysis pump speed are that 90-110r/min, carrier gas flux are 0.8-1.2Lmin
-1, lead element analytical wavelengths is 220.315nm.
A kind of micro-wave digestion of the present invention-ICP-AES measures the method for lead content in Pt950 jewellery, with red fuming nitric acid (RFNA), concentrated hydrochloric acid and hydrogen peroxide are digestion agent, clear up ability strong, sample preparation is simple, the 7-8 hour sample preparation time of common electric hot plate method can be shortened to 1-2 hour, and use acid solution to reduce, be conducive to environmental protection and operator's safety, avoided the loss of lead element in digestion process, analysis result is accurate, be well positioned to meet the analysis requirement of lead content in Pt950 jewellery, the content of controlling lead element for improving Pt950 jewellery quality and Pt950 processing of ornament enterprise provides guarantee.
Embodiment
Further illustrate by the following examples the present invention.
A kind of micro-wave digestion of the present invention-ICP-AES measures the method for lead content in Pt950 jewellery, and described method comprises the steps:
1. test instrument and equipment
Italy MILESTONE ETHOSA microwave dissolver
U.S.'s Thermo IRIS Intrepid II type inductive coupling plasma emission spectrograph (ICP-AES)
The T-214 of U.S. Denver electronic balance.
2. test agents useful for same
Nitric acid (top grade is pure)
Hydrochloric acid (top grade is pure)
Hydrogen peroxide (top grade is pure)
Ultrapure water (self-control)
Lead element standard reserving solution: 1000ppm, Beijing NaKe Analytical Instrument Co., Ltd.
3. experimental procedure
3.1 micro-wave digestion processing samples
Take the Pt950 jewellery sample 0.10402g shredding, be placed in 50mL micro-wave diminishing pot, add 2mL red fuming nitric acid (RFNA), 6mL concentrated hydrochloric acid and 2mL hydrogen peroxide; standing reaction 10min; build lid, insert in protective sleeve and put safety spring sheet, compress whole counteracting tank; prepare blank sample simultaneously; then putting into microwave dissolver, is 1200W according to clearing up power, 150 ℃ of temperature; heating-up time 10min, the condition of constant temperature time 15min is cleared up.Clear up after EOP (end of program), be cooled to below 30 ℃, digestion solution is transferred in 100ml volumetric flask, with ultrapure water, repeatedly clean on a small quantity inner canister, washing lotion is incorporated in volumetric flask, with ultrapure water, is settled to scale, shakes up.
The condition of work of 3.2 instruments
Emissive power is that 1150W, argon pressure are that 0.5MPa, atomization gas pressure are that 24.0L/min, flushing pump speed are that 100r/min, analysis pump speed are that 100r/min, carrier gas flux are 1.0Lmin
-1, lead element analytical wavelengths is 220.315nm.
3.3 matrix interference experiments
This research specimen in use is Pt950 jewellery, if exist matrix to disturb, mainly from Pt950 matrix and Pd, Zn, Fe, Co etc., mixes the interference that ion produces, and conventionally to having higher-energy spectrum line, disturbs comparatively serious.But by sxemiquantitative, scan, in conjunction with sampling amount, calculate total ion concentration and be less than 1gL
-1, the interference of matrix is negligible.
3.4 linear relationships and detection limit
In experiment, lead element standard solution is to be formed by plumbous standard reserving solution stepwise dilution, concrete preparation method is: draw the plumbous standard inventory solution of 5.0mL in 100mL volumetric flask, with 5% salpeter solution dilution, be settled to scale, first be mixed with the standard operation solution that is equivalent to every milligram of 50ug lead, draw respectively more plumbous standard solution 0.0,1.0,2.0,10.0mL is in 100mL volumetric flask, with 5% salpeter solution dilution, be settled to scale, in volumetric flask, solution concentration is equivalent to every milliliter 0.00,0.50,1.00,5.00ug is plumbous.Under the inductive coupling plasma emission spectrograph condition of work of setting, measure plumbous line strength, the concentration of lead element of take is horizontal ordinate, and the intensity of lead element of take is ordinate, instrument computer automatic drafting lead element calibration curve.Plumbous standard working curve linear equation, related coefficient and detection limit are in Table 1.
Standard working curve equation, related coefficient and the detection limit of table 1 lead
3.5 sample determinations and recovery experiment
By ICP-AES instrument condition of work described in 3.2, draw successively blank solution, sample, record its intensity, the test result of the direct display element of computing machine, adds the standard solution 5uL of 1000ug/mL, and addition is equivalent to 0.5ug/mL, do recovery test, result shows that the recovery is good.
Table 2 measured value and recovery test result
3.6 result of calculation
According to formula:
In formula: the massfraction of this metallic element in w-sample, unit is ug/g
C
ithe mass concentration of this metallic element in-Specimen eliminating liquid, unit is ug/mL
C
0the mass concentration of this metallic element in-blank solution, unit is ug/mL
Constant volume after V/ Specimen eliminating, unit is mL
M-takes sample quality, and unit is g
The lead content can be calculated in Pt950 jewellery is 375.9ug/g.
Claims (3)
1. micro-wave digestion-ICP-AES measures a method for lead content in Pt950 jewellery, it is characterized in that, described method comprises the steps:
1) take the sample 0.05-0.15g shredding; be accurate to 0.1mg; be placed in micro-wave diminishing pot; add 2-4mL red fuming nitric acid (RFNA), 3-8mL concentrated hydrochloric acid and 2-5mL hydrogen peroxide, standing reaction 5-10min, builds lid; insert in protective sleeve and put safety spring sheet; compress whole counteracting tank, prepare blank sample simultaneously, then put into microwave dissolver and clear up.Clear up after EOP (end of program), be cooled to below 30 ℃, digestion solution is transferred in 100ml volumetric flask, with ultrapure water, repeatedly clean on a small quantity inner canister, washing lotion is incorporated in volumetric flask, with ultrapure water, is settled to scale, shakes up;
2) open ICP, after instrument igniting complete stability is good, according to the condition of work of ICP, set up the analytical approach of this sample,
According to formula:
In formula: the massfraction of this metallic element in w-sample, unit is ug/g
C
ithe mass concentration of this metallic element in-Specimen eliminating liquid, unit is ug/mL
C
0the mass concentration of this metallic element in-blank solution, unit is ug/mL
Constant volume after V-Specimen eliminating, unit is mL
M-takes sample quality, and unit is g
Can be calculated the lead content in Pt950 jewellery.
2. a kind of micro-wave digestion-ICP according to claim 1-AES measures the method for lead content in Pt950 jewellery, it is characterized in that described step 1) in micro-wave digestion program be specially: clear up power 1000-1500W, temperature 120-170 ℃, heating-up time 5-10min, constant temperature time 10-20min.
3. a kind of micro-wave digestion-ICP according to claim 1-AES measures the method for lead content in Pt950 jewellery, it is characterized in that described step 2) in inductive coupling plasma emission spectrograph condition of work be specially: emissive power is that 1100-1200W, argon pressure are that 0.4-0.6MPa, atomization gas pressure are that 24.0-28.0L/min, flushing pump speed are that 90-110r/min, analysis pump speed are that 90-110r/min, carrier gas flux are 0.8-1.2Lmin
-1, lead element analytical wavelengths is 220.315nm.
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| CN104075933A (en) * | 2014-06-27 | 2014-10-01 | 国家黄金钻石制品质量监督检验中心 | Method for determining content of Ir in gold jewelry by microwave digestion ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) |
| CN106153417A (en) * | 2016-06-24 | 2016-11-23 | 安徽创新检测技术有限公司 | A kind of digestion procedure of water quality total metal content |
| CN109324036A (en) * | 2018-10-29 | 2019-02-12 | 湖南航天磁电有限责任公司 | The method that ICP measures lanthanum, cobalt, strontium, barium, calcium content in permanent-magnet ferrite |
| CN109655448A (en) * | 2019-01-07 | 2019-04-19 | 安徽铜冠有色金属（池州）有限责任公司 | The method of inductively coupled plasma atomic emission spectrometry survey lead in urine |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104075933A (en) * | 2014-06-27 | 2014-10-01 | 国家黄金钻石制品质量监督检验中心 | Method for determining content of Ir in gold jewelry by microwave digestion ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) |
| CN104075933B (en) * | 2014-06-27 | 2016-06-15 | 国家黄金钻石制品质量监督检验中心 | Micro-wave digestion ICP-AES measures the method for Ir content in gold jewelry |
| CN106153417A (en) * | 2016-06-24 | 2016-11-23 | 安徽创新检测技术有限公司 | A kind of digestion procedure of water quality total metal content |
| CN109324036A (en) * | 2018-10-29 | 2019-02-12 | 湖南航天磁电有限责任公司 | The method that ICP measures lanthanum, cobalt, strontium, barium, calcium content in permanent-magnet ferrite |
| CN109655448A (en) * | 2019-01-07 | 2019-04-19 | 安徽铜冠有色金属（池州）有限责任公司 | The method of inductively coupled plasma atomic emission spectrometry survey lead in urine |
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Application publication date: 20140319 |