CN108458918A - A kind of method that micro-wave digestion-ICP-OES measures copper, lead, zinc, cadmium element in ion type rareearth slag - Google Patents
A kind of method that micro-wave digestion-ICP-OES measures copper, lead, zinc, cadmium element in ion type rareearth slag Download PDFInfo
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- CN108458918A CN108458918A CN201810665179.0A CN201810665179A CN108458918A CN 108458918 A CN108458918 A CN 108458918A CN 201810665179 A CN201810665179 A CN 201810665179A CN 108458918 A CN108458918 A CN 108458918A
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- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
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Abstract
The present invention relates to the assay methods of copper, lead, zinc, cadmium content in a kind of ion type rareearth slag.Ion type rareearth ore slag specimen product after the hydrofluoric acid micro-wave digestion of the inverse chloroazotic acid+2mL of inverse 8mL, 2mL HClO are added into counteracting tank by a kind of method that micro-wave digestion ICP OES measure copper, lead, zinc, cadmium content in ion type rareearth slag, method4It is placed in and catches up in sour instrument, acid is caught up with to be done to close at 160 DEG C, 5mL HCl (1+1), which are added, after cooling shifts and with water constant volume in the volumetric flask of 50mL.Sample blank and solution are passed through into inductively coupled plasma atomic emission spectrometer atomizer, form aerosol, high-temperature high-frequency plasma is loaded by argon gas, occur to ionize and generates characteristic spectral line, the intensity of spectral line of copper, lead, zinc, cadmium element in determination sample blank and solution, the intensity of each element is directly proportional to the content of the element, therefore is quantitative determined using calibration curve, and the content of copper in cosmetics, lead, zinc, cadmium element is calculated.This method has the characteristics that good measurement stability, high sensitivity, result are accurate.
Description
Technical field
The invention belongs to analyze testing field, it is related to the measurement of copper, lead, zinc, cadmium element in a kind of ion type rareearth slag
Method, it is especially a kind of that ion type rareearth is measured using micro-wave digestion-inductively coupled plasma emission spectrography (ICP-OES)
The detection method of copper, lead, zinc, cadmium element in slag.
Background technology
Southern ion type rareearth ore commercial reserves explored at present is 1,500,000 tons, and prospective reserves is 50,000,000 tons, accounts for generation
The 80% of heavy rare earth reserves in boundary.The exploitation of ion type rareearth ore experienced leaching process, dump leaching process and in_situ leaching technique 3
For evolution.In_situ leaching technique is currently to open because of the advantages that its production has cost of winning relatively low, and yield is big, and speed is fast
The ripe production practice of ion adsorption type rare earth ore is adopted, but still will produce slag in recovery process.
Ion type rareearth slag refers to the slag that ion type rareearth mother liquor is generated through removing impurity by means of precipitation, essential element be calcium,
Magnesium, aluminium, iron, silicon, ammonium salt and other impurity elements, and with a small amount of rare earth element.
Ammonium ion in rare earth mother solution can change the chemical form of heavy metal and cause heavy metal accumulation in slag, wherein
Copper, lead, the enrichment pollution of zinc and cadmium are more serious.
Ion type rareearth slag is one of Heavy Metal in Soil of Mining source.Through inquiry, the existing measurement rare earth in China and its
The concerned countries standard of non-rare earth impurity element in oxide, but there is no the state for measuring heavy metal element in ion type rareearth slag
Family's standard and professional standard.Currently without find related micro-wave digestion-ICP-OES measure copper in ion type rareearth slag, lead,
The document report of zinc, rapid determination of content of cadmium element.
Invention content
The present invention is directed to fill up the technological gap for measuring copper, lead, zinc, cadmium element in ion type rareearth slag.
The present invention provides the detections that a kind of micro-wave digestion-ICP-OES measures copper, lead, zinc, cadmium in ion type rareearth slag
Method.Method is quick, stablizes, is accurate, is reliable, can be widely applied to the heavy metal analysis of ion type rareearth slag.
To achieve the above object, the present invention provides a kind of micro-wave digestion-ICP-OES to measure in ion type rareearth slag
The detection method of copper, lead, zinc, cadmium, method mainly include the following steps：
1) experiment weighs 0.5g samples (being accurate to 0.0001g) and is placed in counteracting tank, and a little distilled water is blown into along tank skin, will
Sample is blown into tank bottom
2) inverse chloroazotic acid (HCl: HNO is added3=1: 3) 8mL, HF 2mL are added, resolution cover is tightened and shakes up, will clear up
Tank is put into resolution turntable, is cleared up by setting resolution program.
3) counteracting tank is taken out when resolution terminates and temperature is less than 50 DEG C, unscrews counteracting tank under draught cupboard, uses distilled water
Cover is purged, 2mL HClO are added into counteracting tank4It is placed in and catches up in sour instrument, catch up with acid to be done to close at 160 DEG C, be added after cooling
5mL HCl (1+1) are shifted and with water constant volume in the volumetric flask of 50mL, while doing blank test.
4) standard curve configures：Using copper, lead, zinc, cadmium single element standard solution, diluted step by step with 5% HCl,
Make a concentration of 0,0.1,1,5,10 μ g/mL of each element, shakes up spare.
5) Specification Curve of Increasing：It is measured under the inductively coupled plasma atomic emission spectrometer operating condition of setting
The intensity of spectral line of copper, lead, zinc and cadmium, with a concentration of abscissa of each element, intensity is ordinate, is painted automatically by instrument software
Copper, lead, zinc and cadmium element calibration curve processed.
6) step 5) method determination step 3 is pressed) intensity of copper, lead, zinc and cadmium in sample solution, according to each element of measurement
Intensity, the content of each element in cosmetic sample is calculated using the calibration curve of gained in step 5), it is corresponding to count
It calculates as follows：
Copper in ion type rareearth slag, lead, zinc and cadmium content indicated with ω, calculated by formula (1)：
In formula：
ω --- the content of copper, lead, zinc and cadmium in ion type rareearth slag, unit 10-6；
C --- the concentration that element is tested in solution is measured, unit is μ g/mL；
C0--- the concentration of element is tested in blank solution, unit is μ g/mL；
V --- measure solution constant volume, unit mL；
The quality of m --- sample, unit g.
Preferably, being formed for following three steps the step of the resolution sample of microwave dissolver in step 2)：
Preferably, in step 5) inductive coupling plasma emission spectrograph running parameter and measure each element selected by
Wavelength it is as follows：
The method that a kind of micro-wave digestion-ICP-OES of the present invention measures copper, lead, zinc, cadmium in ion type rareearth slag, with
Inverse chloroazotic acid-hydrofluoric acid is digestive reagent, and resolution sample is complete, more easy compared with the molten sample method of traditional battery plate tetracid, quick,
It can will shorten to processing time 2 hours, and reagent consumption is few, measurement result is accurate.Method detection is limited to 0.0021~0.0039 μ
G/mL, Determination Limit are：0.0070~0.0130 μ g/mL；Relative standard deviation (RSD) is：0.23%~2.52%；Method
Relative error is：1.68%~1.90%, recovery of standard addition is 88.46%~102.50%.
The present invention has filled up the detection that domestic micro-wave digestion-ICP-OES measures copper, lead, zinc, cadmium in ion type rareearth slag
Technological gap can be widely applied to the heavy metal analysis of ion type rareearth slag, data reference be provided for the disposition of slag, to ring
Border protection has very real meaning.
Description of the drawings
Fig. 1 is the copper standard curve of wavelength 327.393nm, y=548774.35x+6731.26, related coefficient 0.9999.
Fig. 2 is the lead standard curve of wavelength 220.353nm, y=2575.30x+74.28, related coefficient 0.9999.
Fig. 3 is the zinc standard curve of wavelength 206.200nm, y=23432.80x+1053.77, related coefficient 0.9999.
Fig. 4 is the cadmium standard curve of wavelength 228.802nm, y=49749.90x+553.49, related coefficient 0.9999.
Specific implementation mode
The present invention is elaborated below by way of example.
1. the instrument that the present invention uses
8000 type inductive coupling plasma emission spectrographs of Optima, PerkinElmer companies of the U.S.；
Touchwin2.0 type high throughput intelligent microwaves clear up instrument, Ao Pule science and technology group (Chengdu) Co., Ltd；AL204 electronic balances,
Mettler-Toledo Instrument (Shanghai) Co., Ltd..
2. testing agents useful for same
Single standard reserving solution of copper, lead, zinc and cadmium, 1000 μ g/mL；Hydrochloric acid, nitric acid, perchloric acid and hydrofluoric acid, top pure grade；
Experimental water is redistilled water.
3. experimental procedure
3.1 sample treatment
It weighs 0.5005g samples to be placed in counteracting tank, a little distilled water is blown into along tank skin, sample is blown into tank bottom, be added
Inverse chloroazotic acid (HCl: HNO3=1: 3) 8mL, adds HF 2mL, tightens resolution cover and shakes up, counteracting tank is put into resolution turntable
In, it is cleared up by above-mentioned micro-wave digestion program.Counteracting tank is taken out when resolution terminates and temperature is less than 50 DEG C, under draught cupboard
Counteracting tank is unscrewed, cover is purged with distilled water, 2mL HClO is added into counteracting tank4It is placed in and catches up in sour instrument, caught up at 160 DEG C
Acid is done to close, and 5mLHCl (1+1), which is added, after cooling shifts and with water constant volume in the volumetric flask of 50mL, while doing blank test.
3.2 standard curves configure
Using copper, lead, zinc, cadmium single element standard solution, each element singly mark solution 0,10,100,500,1000 is pipetted respectively
μ L are placed in 5 100mL volumetric flasks, and constant volume is carried out with 5% HCl, are made a concentration of 0,0.1,1,5,10 μ g/mL of each element, are shaken
It is even spare.
3.3 Specification Curve of Increasing
The spectrum of copper, lead, zinc and cadmium is measured under the inductively coupled plasma atomic emission spectrometer operating condition of setting
Line intensity, with a concentration of abscissa of each element, intensity is ordinate, draws copper, lead, zinc and cadmium member automatically by instrument software
Plain calibration curve.Each element calibration curve equation is as follows：
Copper standard curve：Y=548774.35x+6731.26, related coefficient 0.9999.
Lead standard curve：Y=2575.30x+74.28, related coefficient 0.9999.
Zinc standard curve：Y=23432.80x+1053.77, related coefficient 0.9999.
Cadmium standard curve：Y=49749.90x+1053.49, related coefficient 0.9999.
3.4 results calculate
The intensity of blank sample and sample to be tested is measured using ICP-OES, instrument is automatically according to the standard curve drawn
The concentration of equation calculation object elements calculates the content of each element in sample further according to formula (1), is the accuracy of verification method
And stability, instrument have carried out 12 measurement, measurement result such as following table to sample.This method measurement result as can be seen from the table
Deviation is small, and relative standard deviation is 0.23%~2.52%, and numerical stability is reliable.Meet correlation in GB/T 27404-2008 to want
It asks, is suitable for the detection of ion type rareearth slag.
Claims (9)
1. a kind of method that micro-wave digestion-ICP-OES measures copper, lead, zinc, cadmium element in ion type rareearth slag, feature exist
In this method comprises the following steps：
(1) sample weighing：Experiment weighs 0.5g samples (being accurate to 0.0001g) and is placed in counteracting tank, and a little steaming is blown into along tank skin
Sample is blown into tank bottom by distilled water
(2) Specimen eliminating：Inverse chloroazotic acid (HCl: HNO is added3=1: 3) 8mL, HF 2mL are added, resolution cover is tightened and shakes up,
Counteracting tank is put into resolution turntable, is cleared up by setting resolution program.
(3) acid is caught up with：Counteracting tank is taken out when resolution terminates and temperature is less than 50 DEG C, counteracting tank is unscrewed under draught cupboard, with distillation
Water purges cover, and 2mL HClO are added into counteracting tank4It is placed in and catches up in sour instrument, acid is caught up with to be done to close at 160 DEG C, add after cooling
Enter 5mL HCl (1+1) transfers and with water constant volume in the volumetric flask of 50mL, while doing blank test.
(4) standard curve configures：It using copper, lead, zinc, cadmium single element standard solution, is diluted, is made each step by step with 5% HCl
Concentration of element is 0,0.1,1,5,10 μ g/mL, is shaken up spare.
(5) Specification Curve of Increasing：Under the inductively coupled plasma atomic emission spectrometer operating condition of setting measure copper,
The intensity of spectral line of lead, zinc and cadmium, with a concentration of abscissa of each element, intensity is ordinate, is drawn automatically by instrument software
Copper, lead, zinc and cadmium element calibration curve.
(6) sample measures：By the intensity of copper, lead, zinc and cadmium in step (5) method determination step (3) sample solution, according to measurement
Each element intensity, the content of each element in cosmetic sample is calculated using the calibration curve of gained in step (5),
Corresponding calculating is as follows：
Copper in ion type rareearth slag, lead, zinc and cadmium content indicated with ω, calculated by formula (1)：
In formula：
ω --- the content of copper, lead, zinc and cadmium in ion type rareearth slag, unit 10-6
C --- the concentration that element is tested in solution is measured, unit is μ g/mL
C0--- the concentration of element is tested in blank solution, unit is μ g/mL；
V --- measure solution constant volume, unit mL；
The quality of m --- sample, unit g.
2. a kind of micro-wave digestion-ICP-OES according to claim 1 measures copper, lead, zinc, cadmium in ion type rareearth slag
The method of element, it is characterised in that sample sample weighting amount is 0.5g (being accurate to 0.0001g) in the step (1).
3. a kind of micro-wave digestion-ICP-OES according to claim 1 measures copper, lead, zinc, cadmium in ion type rareearth slag
The method of element, it is characterised in that inverse chloroazotic acid addition is 8mL in the step (2), and hydrofluoric acid addition is 2mL.
4. a kind of micro-wave digestion-ICP-OES according to claim 1 measures copper, lead, zinc, cadmium in ion type rareearth slag
The method of element, it is characterised in that micro-wave digestion program following steps in the step (2)：
5. a kind of micro-wave digestion-ICP-OES according to claim 1 measures copper, lead, zinc, cadmium in ion type rareearth slag
The method of element, it is characterised in that it is 160 DEG C to catch up with sour instrument to catch up with the temperature of acid in the step (3).
6. a kind of micro-wave digestion-ICP-OES according to claim 1 measures copper, lead, zinc, cadmium in ion type rareearth slag
The method of element, it is characterised in that the HClO being added when catching up with acid in the step (3)4Amount is 2mL.
7. a kind of micro-wave digestion-ICP-OES according to claim 1 measures copper, lead, zinc, cadmium in ion type rareearth slag
The method of element, it is characterised in that step (4) the Plays solution allocation step is：Use copper, lead, zinc, cadmium single element mark
Quasi- solution is diluted step by step with 5% HCl, makes a concentration of 0,0.1,1,5,10 μ g/mL of each element.
8. a kind of micro-wave digestion-ICP-OES according to claim 1 measures copper, lead, zinc, cadmium in ion type rareearth slag
The method of element, it is characterised in that inductively coupled plasma atomic emission spectrometer (ICP-OES) works in the step (5)
Parameter is as follows：
9. a kind of micro-wave digestion-ICP-OES according to claim 1 measures copper, lead, zinc, cadmium in ion type rareearth slag
The method of element, it is characterised in that hydrochloric acid, nitric acid, perchloric acid and hydrofluoric acid used must be top pure grade；It is secondary steaming with water
Distilled water；Instrument sample introduction and atomization system should be thoroughly cleaned before detection.
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|---|---|---|---|---|
| CN109142004A (en) * | 2018-09-21 | 2019-01-04 | 吉林大学 | The detection method of biologically effective state cadmium in a kind of soil |
| CN109827952A (en) * | 2019-02-25 | 2019-05-31 | 滕亚君 | The ICP-AES detection method of micronutrient levels in a kind of lead concentrate |
| CN110057791A (en) * | 2019-02-25 | 2019-07-26 | 滕亚君 | The measuring method of arsenic, mercury, bismuth, lead, cadmium content in a kind of eucalyptus oil |
| CN110320264A (en) * | 2019-08-09 | 2019-10-11 | 福建省农业科学院农业质量标准与检测技术研究所 | Inductively coupled plasma mass spectrometry measure marine sediment in lead, cadmium, chromium, copper, zinc, nickel content detection method |
| CN110595851A (en) * | 2019-09-12 | 2019-12-20 | 中国地质科学院矿产综合利用研究所 | Method for rapidly decomposing sedimentary rare earth ore |
| CN110658095A (en) * | 2019-11-11 | 2020-01-07 | 北方工业大学 | Method for determining molybdenum in molybdenum concentrate by microwave-sealed ore-dissolving lead molybdate gravimetric method |
| CN111392761A (en) * | 2020-04-20 | 2020-07-10 | 中稀(宜兴)稀土新材料有限公司 | Rare earth solution preparation process capable of quickly and efficiently dispelling acid |
| CN112630175A (en) * | 2020-12-22 | 2021-04-09 | 江苏微谱检测技术有限公司 | Method for determining heavy metals in soil |
| CN113109323A (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 sediments |
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| CN116223486A (en) * | 2023-03-31 | 2023-06-06 | 浙江国检检测技术股份有限公司 | Analysis method for yttrium content in yttrium-containing glass microsphere material |
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| CN109142004A (en) * | 2018-09-21 | 2019-01-04 | 吉林大学 | The detection method of biologically effective state cadmium in a kind of soil |
| CN109827952A (en) * | 2019-02-25 | 2019-05-31 | 滕亚君 | The ICP-AES detection method of micronutrient levels in a kind of lead concentrate |
| CN110057791A (en) * | 2019-02-25 | 2019-07-26 | 滕亚君 | The measuring method of arsenic, mercury, bismuth, lead, cadmium content in a kind of eucalyptus oil |
| CN110320264A (en) * | 2019-08-09 | 2019-10-11 | 福建省农业科学院农业质量标准与检测技术研究所 | Inductively coupled plasma mass spectrometry measure marine sediment in lead, cadmium, chromium, copper, zinc, nickel content detection method |
| CN110595851B (en) * | 2019-09-12 | 2022-03-18 | 中国地质科学院矿产综合利用研究所 | Method for rapidly decomposing sedimentary rare earth ore |
| CN110595851A (en) * | 2019-09-12 | 2019-12-20 | 中国地质科学院矿产综合利用研究所 | Method for rapidly decomposing sedimentary rare earth ore |
| CN110658095A (en) * | 2019-11-11 | 2020-01-07 | 北方工业大学 | Method for determining molybdenum in molybdenum concentrate by microwave-sealed ore-dissolving lead molybdate gravimetric method |
| CN111392761A (en) * | 2020-04-20 | 2020-07-10 | 中稀(宜兴)稀土新材料有限公司 | Rare earth solution preparation process capable of quickly and efficiently dispelling acid |
| CN112630175A (en) * | 2020-12-22 | 2021-04-09 | 江苏微谱检测技术有限公司 | Method for determining heavy metals in soil |
| CN113109323A (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 sediments |
| CN113984740A (en) * | 2021-09-22 | 2022-01-28 | 湖南省药品检验研究院(湖南药用辅料检验检测中心) | Method for rapidly analyzing eight trace elements in patrinia scabiosaefolia |
| CN116223486A (en) * | 2023-03-31 | 2023-06-06 | 浙江国检检测技术股份有限公司 | Analysis method for yttrium content in yttrium-containing glass microsphere material |
| CN116223486B (en) * | 2023-03-31 | 2023-08-29 | 浙江国检检测技术股份有限公司 | Analysis method for yttrium content in yttrium-containing glass microsphere material |
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Application publication date: 20180828 |