CN101109700A - Method for measuring ruthenium content using ethyne-air flame atomic absorption spectrometry - Google Patents
Method for measuring ruthenium content using ethyne-air flame atomic absorption spectrometry Download PDFInfo
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Abstract
The invention provides a method for determining ruthenium content by acetylene-air flame atom absorption spectrum method, the procedures for which are: a sample is dried under 100-120 centigrade, burned under 400-600 centigrade, residual ash is removed; potassium hydroxide is added in a reference pure ruthenium powder and sample, which is heated under 360-390 centigrade to dissolve; surplus chlorhydric acid is added, so that the solution is acid; some de-saline water is added in the solution to prepare standard mother solution and sample solution; standard solutions of different concentrations are prepared by taking sample blank liquid as thinner; the spectrometer wavelength is adjusted to 344.9 nm, the acetylene flow 65 l/h, lamp current 10 mA; the zero is calibrated by using sample blank liquid, the standard solution is determined, and a standard work curve is established, parameters of the sample are input, the concentration and content of the ruthenium are measured in the sample. The invention has a rapid measuring speed, high accuracy, low harm on the operator, and is applicable for determining the ruthenium content in various solid or liquid multi-component substances, especially the ruthenium content in ruthenium/carbon catalyzer.
Description
Technical field
The present invention relates to the method for a kind of acetylene-air flame aas determination ruthenium content, particularly measure the method for ruthenium content in the ruthenium-containing catalyst.
Background technology
Ruthenium is a kind of precious metal, is widely used in fields such as medical treatment, chemical industry, metallurgy.In order to prepare, use ruthenium catalyst effectively, make full use of or reclaim the ruthenium metal, need to measure the content of ruthenium in multi-component material.The method of known mensuration ruthenium content has, and tube sealing chloridising dissolving reference material and sample are with thiocarbamide spectrophotometry ruthenium content.Promptly reference material or sample are placed tube sealing respectively, add hydrochloric acid and hydrogen peroxide, heating for dissolving in special steel bomb, make standard solution and sample solution, add the thiocarbamide developer, select wavelength 602nm, make the light absorption value of reference liquid measurement standard solution with reagent blank with spectrophotometer, the drawing standard curve, working sample calculates ruthenium content then.The deficiency of this method is that the heating of (1) hydrogen peroxide is easily blasted, the personal safety of harm testing crew; (2) test period is long, and reference material and sample dissolution need 24 hours.
Chinese patent CN1030799C discloses the assay method of osmium, ruthenium in a kind of complex component.Method comprises with reductive agent carries out pre-service to detected solution, adds proper amount of oxidant and distills absorption, measures the content of ruthenium in the absorption liquid then with conventional method.The method is defined as the mensuration of ruthenium content in the polycomponent solution, and the content＜200mg/l of ruthenium in the measured object.
Summary of the invention
The method that the purpose of this invention is to provide acetylene-air flame aas determination ruthenium content is particularly measured the method for ruthenium content in the ruthenium-containing catalyst.Wherein, the carrier of ruthenium catalyst can be activated charcoal, aluminium oxide, titania, monox etc.Measured matter involved in the present invention can be solid-state or liquid, and the scope of measuring ruthenium content is 0～100%.
Characteristics of the present invention are: use potassium hydroxide at high temperature to dissolve reference material and sample, with the content of ruthenium in acetylene-air flame atomic absorption spectrometry multi-component material.Determination step is as follows:
1, standard solution configuration
A, take by weighing quantitative spectroscopic pure ruthenium powder and place nickel crucible, add 5～1 5 times of (weight) potassium hydroxide, 360～390 ℃ of following heating for dissolving.
Move to beaker after b, the ruthenium dissolving cooling, add excessive hydrochloric acid (hydrochloric acid: water=1: 1), make solution be acid, add demineralized water constant volume in volumetric flask, be the standard mother liquor.
C, be the standard solution that thinning agent is configured to the standard mother liquor respectively variable concentrations with sample blank liquid.
2, sample solution configuration
A, with sample 100～120 ℃ of down oven dry, remove moisture.
B, take by weighing quantified sample and place nickel crucible, calcination in muffle furnace, temperature is controlled at 400～600 ℃, eliminates residual ash.
C, take out sample crucible from muffle furnace, the cooling back adds 2～12 times of (weight) potassium hydroxide, 360～390 ℃ of following heating for dissolving.
Move to beaker after d, the cooling, add excessive hydrochloric acid (hydrochloric acid: water=1: 1), make solution be acid, add demineralized water constant volume in volumetric flask, be sample solution.
E, use and the potassium hydroxide of preparing sample equivalent and hydrochloric acid, add demineralized water and make sample blank liquid (as thinning agent configuration standard solution and alignment light spectrometer zero point).
The preparation of standard solution and sample solution can be carried out simultaneously.
3, instrument condition
Use NOVAA300 or other Atomic Absorption Spectrometers of the same type, the hollow lamp of ruthenium negative electrode, measure with acetylene-air flame.Regulating the spectrometer condition is: wavelength 344.9nm, acetylene flow 65l/hr, slit 0.2nm, lamp current 10mA, combustion head specification 50mm, height 7mm, 5 Blind Test of measurement are once.
4, sample determination
With sample blank liquid calibration Atomic Absorption Spectrometer zero point, measuring the light absorption value of variable concentrations standard solution, is horizontal ordinate with concentration, and light absorption value is an ordinate, draw the natural working curve of standard specimen, import working sample solution behind the data message of sample under the same conditions.Instrument is measured the concentration and the ruthenium content of sample automatically.If the concentration of being surveyed is higher than the upper limit of typical curve, sample solution suitably is diluted in the standard curve range measures again.
Measuring the used standard solution of ruthenium content prepares with spectroscopic pure ruthenium powder, also can prepare with commercially available ruthenium standard solution, another program of the present invention is to make mother liquor with commercially available ruthenium standard solution, with the test standard solution of sample blank liquid dilution configuration variable concentrations, measures.
Ruthenium/carbon the promotor of use such as benzoic acid hydrogenation process is made carrier with activated charcoal in the caprolactam production, analyzes preparation, use, recovery and chemical process that the content of ruthenium in the ruthenium/carbon catalyst is convenient to control catalyst exactly.As introducing, the measured matter in the method for the invention is a ruthenium/carbon catalyst.
The present invention compares the advantage that has with existing assay method: with potassium hydroxide dissolving ruthenium reference material and sample, potassium does not form ruthenium in the atomic absorption analysis process and disturbs; The analysis precision height, its accuracy is higher by about 3% than thiocarbamide spectrophotometry ruthenium content; Analysis time is short, can finish test in 10 hours; Little to testing crew health harmfulness; The content of ruthenium in the various liquid state of adaptation mensuration 0～100% concentration or the solid-state multi-component material.
Embodiment
Embodiment 1
With spectroscopic pure ruthenium powder configuration standard solution, measure the content of following closely in the ruthenium/carbon catalyst.
The ruthenium/carbon catalyst sample 105 times oven dry 4 hours, is removed moisture; Take by weighing 0.4064 gram (butt) sample and place nickel crucible, calcination is 6 hours in muffle furnace, and the control temperature eliminates residual ash for 500 ℃, takes out the crucible cooling; Take by weighing 0.1025 gram spectroscopic pure ruthenium powder and place nickel crucible; Prepare sample solution and standard solution when as follows: in ruthenium powder and sample, add 1.0 gram potassium hydroxide respectively, heating for dissolving, 380 ℃ of control temperature.Be cooled to room temperature after the dissolving.Sample and reference material are transferred to beaker respectively, add 20ml hydrochloric acid (hydrochloric acid: water=1: 1; Hydrochloric acid is commercially available hydrochloric acid), change the 250ml volumetric flask over to, add the demineralized water constant volume, be mixed with standard mother liquor and sample solution.
Get 1 gram potassium hydroxide and 20ml hydrochloric acid (hydrochloric acid: water=1: 1), change the 250ml volumetric flask over to, add the demineralized water constant volume, again as sample blank liquid.Get 5,10,15,20,25ml standard mother liquor places the 50ml volumetric flask, with sample blank liquid dilution constant volume, is standard solution.
Regulate Atomic Absorption Spectrometer, wavelength: 344.9nm, slit: 0.2nm, deuterium lamp electric current: 10mA, acetylene flow: 65l/hr, combustion head specification: 50nm, highly: 7nm, measure 5 Blind Test 1 time.
Elder generation's working sample blank solution is proofreaied and correct spectrometer zero point, again bioassay standard solution.Instrument is measured the light absorption value of variable concentrations solution automatically, and the drawing standard working curve.The information such as weight of input sample under identical condition, working sample solution.Measurement result is:
Light absorption value: 0.5633
The concentration of sample solution: 94.95%
Ruthenium content in the catalyzer: 59130mg/kg
RSD：0.141％
Embodiment 2
With commercially available ruthenium standard solution is mother liquor configuration standard solution, measures the content of ruthenium in the ruthenium/carbon catalyst.
The ruthenium/carbon catalyst sample 110 ℃ of down oven dry 3 hours, is removed moisture, take by weighing 0.3831 gram (butt) sample, place nickel crucible, 550 ℃ of calcinations are 5 hours in muffle furnace, eliminate residual ash.The cooling back adds 1.0 gram potassium hydroxide, heating for dissolving, 370 ℃ of control temperature.Add 25ml hydrochloric acid (hydrochloric acid: water=1: 1), change the 250ml volumetric flask over to, add the demineralized water constant volume, be sample solution.(be numbered GSB G62037-90, concentration is 1000 μ g/mg, and medium is: 10% hydrochloric acid) be mother liquor, be diluted to 10mg/l, 30mg/l, 50mg/l, 70mg/l and 100mg/l test standard solution with sample blank liquid with the national standard ruthenium solution.
Regulate Atomic Absorption Spectrometer with the step identical, rectify an instrument zero point with embodiment 1, bioassay standard solution drawing standard curve, and working sample, the result is:
Light absorption value: 0.5538
Sample solution concentration: 95.33%
Ruthenium content in the catalyzer: 58435mg/kg
RSD：0.21％
Embodiment 3
The replica test of standard sample
Get 0.1035 gram, 0.09958 gram, 0.1058 gram spectroscopic pure ruthenium powder adding, 1.0 gram potassium hydroxide respectively, heat 380 ℃ of dissolvings, the cooling back adds 25ml hydrochloric acid (hydrochloric acid: water=1: 1), change the 250ml volumetric flask over to, add the demineralized water constant volume, make 1#, 2#, 3# sample.
With the method among the embodiment 2, be mother liquor configuration test standard solution with commercially available national standard ruthenium solution, regulate the spectrometer parameter, with the zeroing of sample blank liquid, bioassay standard solution, drawing standard curve.Import the data of each sample respectively, working sample solution.In order to contrast, utilize tube sealing chlorination-thiocarbamide spectrophotometric method to do the mensuration of one group of pure ruthenium powder simultaneously.Two kinds of method measurement results see Table 1.
Table 1
| Acetylene-air atomic absorption method | The thiocarbamide spectrophotometric method |
| 100.5％ | 102.3 |
| 101.0％ | 103.8 |
| 100.8％ | 102.5 |
Good reproducibility of the present invention as can be seen from Table 1, accuracy are better than tube sealing chlorination-thiocarbamide spectrophotometric method.
Claims (3)
1. the method for acetylene-air flame aas determination ruthenium content, measurement range is a ruthenium content 0～100%, its mensuration process comprises:
A. dry sample down at 100～120 ℃, remove moisture.
B. take by weighing quantified sample, calcination in muffle furnace, temperature is controlled at 400～600 ℃, eliminates residual ash.
C. preparation standard mother liquor and sample solution promptly add 2～12 times of (ruthenium grain weight amount) potassium hydroxide in the pure ruthenium powder of reference material, add 5～15 times of (butt example weight) potassium hydroxide in sample, dissolve ruthenium down at 360～390 ℃; The cooling back adds excessive hydrochloric acid, makes solution be acid, adds the demineralized water constant volume, is mixed with standard mother liquor and sample solution.
D. be thinning agent with sample blank liquid, mother liquor be mixed with the standard solution of variable concentrations.
E. the spectrometer condition enactment is: wavelength 344.9nm, acetylene flow 651/hr, lamp current 10mA.
F. with sample blank liquid calibration Atomic Absorption Spectrometer zero point, the absorbance of bioassay standard solution and sample solution, the drawing standard curve is measured the content of ruthenium.
2. press the method for claim 1 described mensuration ruthenium content, it is characterized in that: standard solution is made mother liquor preparation test standard solution with commercially available ruthenium standard solution in the described method.
3. press claim 1 or 2 described mensuration ruthenium content methods, it is characterized in that: the determined material in the described method is a ruthenium/carbon catalyst.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102353637A (en) * | 2011-06-16 | 2012-02-15 | 山东正元地质资源勘查有限责任公司烟台分公司 | Method of determining silver content in rock minerals |
| CN102706815A (en) * | 2012-05-25 | 2012-10-03 | 中国航空工业集团公司北京航空材料研究院 | Method for determination of trace element Na in pure Hf (hafnium) |
| CN102706816A (en) * | 2012-05-25 | 2012-10-03 | 中国航空工业集团公司北京航空材料研究院 | Method for determination of trace element Na and K in pure Re |
| CN110146490A (en) * | 2019-06-14 | 2019-08-20 | 北京北达智汇微构分析测试中心有限公司 | A method of with micro ruthenium element in ICP-OES measurement drug |
| CN111289498A (en) * | 2020-03-26 | 2020-06-16 | 福州大学 | Method for determining ruthenium content in supported ruthenium catalyst |
| CN111855595A (en) * | 2020-08-24 | 2020-10-30 | 四川长虹电器股份有限公司 | Spectral data calibration method based on black and white calibration plate |
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2007
- 2007-08-22 CN CNB2007101392448A patent/CN100523785C/en active Active
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102353637A (en) * | 2011-06-16 | 2012-02-15 | 山东正元地质资源勘查有限责任公司烟台分公司 | Method of determining silver content in rock minerals |
| CN102706815A (en) * | 2012-05-25 | 2012-10-03 | 中国航空工业集团公司北京航空材料研究院 | Method for determination of trace element Na in pure Hf (hafnium) |
| CN102706816A (en) * | 2012-05-25 | 2012-10-03 | 中国航空工业集团公司北京航空材料研究院 | Method for determination of trace element Na and K in pure Re |
| CN102706815B (en) * | 2012-05-25 | 2014-07-02 | 中国航空工业集团公司北京航空材料研究院 | Method for determination of trace element Na in pure Hf (hafnium) |
| CN102706816B (en) * | 2012-05-25 | 2014-07-02 | 中国航空工业集团公司北京航空材料研究院 | Method for determination of trace element Na and K in pure Re |
| CN110146490A (en) * | 2019-06-14 | 2019-08-20 | 北京北达智汇微构分析测试中心有限公司 | A method of with micro ruthenium element in ICP-OES measurement drug |
| CN111289498A (en) * | 2020-03-26 | 2020-06-16 | 福州大学 | Method for determining ruthenium content in supported ruthenium catalyst |
| CN111289498B (en) * | 2020-03-26 | 2021-06-22 | 福州大学 | Method for determining ruthenium content in supported ruthenium catalyst |
| CN111855595A (en) * | 2020-08-24 | 2020-10-30 | 四川长虹电器股份有限公司 | Spectral data calibration method based on black and white calibration plate |
| CN111855595B (en) * | 2020-08-24 | 2022-04-05 | 四川长虹电器股份有限公司 | Spectral data calibration method based on black and white calibration plate |
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