CN101571478B - Method for analyzing and detecting potassium and sodium impurity elements in vanadium carbide - Google Patents
Method for analyzing and detecting potassium and sodium impurity elements in vanadium carbide Download PDFInfo
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Abstract
The invention discloses a method for analyzing and detecting potassium and sodium impurity element in vanadium carbide, which comprises a step of adding cesium chloride solution when vanadium carbide test solution and standard solution series are prepared. The method comprises the following steps: (1) putting vanadium carbide test material in a quartz beaker, using deionized water to blow and washthe wall of the beaker, sequentially adding hydrochloric acid and nitric acid at the volume ratio of 3:1, mixing the materials well, covering the beaker with a lid and heating the beaker for dissolut ion; (2) moving the completely dissolved vanadium carbide test solution into a plastic volumetric flask, using the deionized water to dilute the vanadium carbide test solution to a scale, mixing the two well and filtering the obtained product; (3) preparing the standard solution series which is matched with a vanadium matrix and mixed with potassium and sodium; and (4) simultaneously putting the vanadium carbide test solution and the mixed standard solution series on an atomic absorption spectrophotometer under the condition of selected instruments to determine the absorbance of potassium and sodium element, looking up the concentration of corresponding detected elements in a standard curve and calculating analysis results. The method has a lower analysis-detection limit up to 10 ppm and has a content determination range between 0.0010 and 0.10 percent.
Description
Technical field
The present invention relates to the analyzing detecting method of potassium, sodium impurity elements in the analyzing and testing of potassium, sodium element, particularly vanadium carbide.
Background technology
Because vanadium carbide has the performance of a lot of excellences, in recent years, in the wimet new product development, often vanadium carbide is added in the alloy as adjuvant, the grain growth that suppresses alloy, and the height of impurity content directly affects the performance of wimet in the vanadium carbide, in order to guarantee the quality of hart metal product, and must be to carrying out check and analysis as impurity elements such as potassium, sodium in the vanadium carbide of wimet crystallizing inhibitor.In existing vanadium carbide chemical analysis method, potassium, sodium impurity elements do not have corresponding chemical analysis method.Owing to need potassium, the sodium impurity elements content of mensuration lower in the vanadium carbide, should select for use atomic absorption spectrophotometry to carry out assay determination, this is industry technician's a common recognition.Yet, vanadium carbide sample utmost point indissoluble is separated, though can decompose with the potassium pyrosulfate fusion method, or dissolve with sulfuric acid nitric acid nitration mixture, but may there be the problem of introducing a large amount of impurity elements to be measured in the skip test liquid of above-mentioned molten (molten) agent, and sulfuric acid can produce molecule absorption in the mensuration of atomic absorption spectrophotometry, influences the absorbance of element to be measured, thereby influence the accuracy of testing result, be not suitable for atomic absorption spectroscopy determination.Therefore, vanadium carbide is decomposed fully, artificially not introduce impurity element to be measured and the generation of avoiding the molecule absorption phenomenon again, become one technical barrier that must solve with potassium, sodium impurity elements in the atomic absorption spectroscopy determination vanadium carbide.
Summary of the invention
Purpose of the present invention just be to solve in the above-mentioned vanadium carbide potassium, sodium impurity elements still do not have analyzing detecting method and vanadium carbide extremely difficulty decompose technical matters completely, the analyzing detecting method of potassium, sodium impurity elements in a kind of vanadium carbide is provided, it does not artificially introduce the foreign impurity element, be suitable for potassium, sodium impurity elements in the atomic absorption spectroscopy determination vanadium carbide, and measurement result is accurate, fills up in the prior art blank of potassium, sodium impurity elements analyzing detecting method in the vanadium carbide.
For realizing purpose of the present invention, select for use hydrochloric acid and nitric acid acid mixture (chloroazotic acid) to make solvent, heating and decomposition vanadium carbide sample, sample can decompose fully, can not separate out V again
2O
5Crystallization; Simultaneously, adopt potassium, the sodium mixed standard solution series drawing standard curve of vanadium matrix coupling, can on atomic absorption spectrophotometer (AAS), directly measure potassium in the vanadium carbide, sodium impurity elements exactly.Concrete technical scheme comprises the steps:
(1) the vanadium carbide test portion is placed quartz beaker, behind deionized water purge wall of cup, add hydrochloric acid and nitric acid successively, the volume ratio that adds hydrochloric acid and nitric acid is 3: 1, hydrochloric acid purity is that MOS level, mass concentration are 1.19 grams per milliliters, addition is 7.5～15 milliliters, and nitric acid purity is that MOS level, mass concentration are 1.42 grams per milliliters, and addition is 2.5～5 milliliters, mixing then, cover bowl cover, heating for dissolving, heating for dissolving temperature are 60～80 ℃;
(2) consoluet vanadium carbide test solution is moved in the plastics volumetric flask, be diluted to scale with deionized water, mixing filters;
(3) the standard solution series of the potassium of preparation vanadium matrix coupling, sodium mixing;
(4) under selected instrument condition of work, vanadium carbide test solution and the mixed standard solution series of (3) preparation are measured the absorbance of potassium, sodium element simultaneously on atomic absorption spectrophotometer (AAS), find the concentration of corresponding tested element again from typical curve, Calculation results.
When above-mentioned vanadium carbide test solution of preparation and standard solution series, also should add the cesium chloride solution of coupling by the conventional way of potassium, sodium element in the test samples, to guarantee analyzing and testing result's precision.
The present invention is when implementing, the vanadium matrix solution that need add when the potassium of preparation vanadium matrix coupling, sodium mixed standard solution series is suitable with the test portion amount that takes by weighing, when taking by weighing sample size was 0.1250～0.2500 when gram, added mass concentration and be 5～10 milliliters of the vanadium matrix solution of 20.0 grams per liters.
Analysis detecting data collection of enforcement the inventive method and result calculate basic close with the analysis result computing method with conventional atomic absorption spectrophotometry data acquisition, and computational analysis testing result concrete grammar is:
Look into typical curve (1) result of calculation as follows,
In the formula:
X represents tested element (potassium, sodium);
ρ represents the mass concentration that checks in tested element in the sample solution that blank correction is crossed on the typical curve, (μ g/mL, mcg/ml);
V represents the volume of tested sample solution, (mL, milliliter);
M represents the quality of test portion, (g, gram).
Advantage of the present invention is to adopt highly purified MOS grade hydrochloric acid and nitric acid nitration mixture (chloroazotic acid) dissolving vanadium carbide sample, potassium in the vanadium carbide, sodium impurity elements analyzing and testing lower limit (reaching 10ppm) have been improved, with vanadium matrix match-on criterion curve, make that potassium, sodium impurity elements become possibility in the analyzing and testing vanadium carbide, thereby filled up the blank of potassium, sodium impurity elements analyzing detecting method in the vanadium carbide.And to the accuracy of measurement height of potassium, sodium impurity elements in the vanadium carbide, precision is good, can satisfy the requirement of quality inspection.Potassium, sodium element content range that analyzing detecting method of the present invention is measured are 0.0010%～0.10%, are highly suitable for the assay determination of potassium in the vanadium carbide, sodium impurity elements, and the result is stable, consistent, favorable reproducibility.
Description of drawings
Fig. 1 adopts the typical curve of the present invention with atomic absorption spectrophotometer.
Embodiment
Analyzing detecting method to potassium, sodium impurity elements in the vanadium carbide of the present invention is described in further detail below.
1. standard solution preparation
The sodium standard solution preparation: take by weighing 0.2543g sodium chloride (99.99%) and place quartz beaker, use deionized water dissolving, move in the 1000mL plastics volumetric flask, be diluted to scale with deionized water, mixing is stored in the plastics volumetric flask.This solution quality concentration is the sodium of 0.100mg/mL (mg/ml).
The preparation of potassium standard solution: take by weighing 0.1907g potassium chloride (99.99%) and place quartz beaker, use deionized water dissolving, move in the 1000mL plastics volumetric flask, be diluted to scale with deionized water, mixing is stored in the plastics volumetric flask.This solution quality concentration is the potassium of 0.100mg/mL (mg/ml).
The preparation mass concentration is potassium, the sodium mixed standard solution of 10 μ g/mL (mcg/ml): pipette the above-mentioned sodium standard solution 10mL and the potassium standard solution 10mL that prepare respectively, place 100mL plastics volumetric flask, be diluted to scale with deionized water, mixing is stored in the plastics volumetric flask.
The preparation mass concentration is the vanadium matrix solution of 20.0g/L (grams per liter): take by weighing 3.5705g vanadium pentoxide (99.99%), place the 150ml quartz beaker, add 40ml chloroazotic acid (hydrochloric acid: the nitric acid volume ratio is 3: 1), place on the electric hot plate, slowly be heated to dissolving fully, take off cooling, with deionized water purge wall of cup, move in the 100ml plastics volumetric flask, be diluted to scale with deionized water, mixing is stored in the plastics volumetric flask.
The mixed standard solution series of preparation vanadium matrix coupling: pipette potassium, sodium mixed standard solution 0 that the above-mentioned mass concentration for preparing is 10 μ g/mL respectively, 1.00mL, 2.00mL, 3.00mL, 4.00mL in one group of (5) 50mL plastics volumetric flask, (the concrete addition of vanadium matrix solution should be suitable with test portion amount to be detected to add above-mentioned mass concentration and be the vanadium matrix solution 10mL of 20.0g/L (grams per liter), such as: when taking by weighing sample size was 0.2500 when gram, and adding mass concentration is 20.0g/L vanadium matrix solution 10mL; When taking by weighing sample size was 0.1250 when gram, adding mass concentration is 20.0g/L vanadium matrix solution 5mL), adding purity then is high-purity (MOS level), and mass concentration is the hydrochloric acid 12mL of 1.19g/mL (grams per milliliter), and purity is that high-purity (MOS level), mass concentration are the nitric acid 4mL of 1.42g/mL.Precision in order to ensure the analyzing and testing result, conventional way by potassium, sodium element in the test samples, adding mass concentration again is that 10g/L (gets 5g and analyzes pure cesium chloride, be dissolved in the 500mL plastics volumetric flask with deionized water, mixing) ionization buffer (ionization in the time of can preventing potassium, sodium element atomization) cesium chloride solution 2.0ml, be diluted to scale with deionized water, mixing, promptly be mixed with every milliliter (mL) and contain 0,0.20 μ g (microgram), 0.40 μ g, 0.60 μ g, potassium, the sodium mixed standard solution series of the vanadium matrix coupling of 0.80 μ g.
2. press the step measurements drawing standard working curve of the inventive method
When adopting the inventive method to measure the potassium of vanadium matrix coupling, the potassium in the sodium mixed standard solution series, sodium element on AA-220 type atomic absorption spectrophotometer (AAS), the condition of work of atomic absorption spectrophotometer (AAS) is listed in table 1 (embodiment below the wavelength of listed condition of work and element to be measured is all identical).
The condition of work of table 1 AA-220 type atomic absorption spectrophotometer (AAS)
| Element | Wavelength nm | Lamp current mA | Spectral band-width nm | Burner height mm | Air mass flow L/min | Acetylene flow L/min |
| Na? | 589.0? | 2? | 0.5? | 6? | 10? | 2.0? |
| K? | 766.5? | 2? | 1.0? | 6? | 10? | 2.0? |
Under the listed condition of work of table 1, potassium, sodium mixed standard solution series that the vanadium matrix that has prepared mates are measured (carrying out blank determination simultaneously) on atomic absorption spectrophotometer (AAS), mass concentration with tested element is a horizontal ordinate, and the absorbance of mensuration is that ordinate is drawn out typical curve (as shown in Figure 1).
3. sample determination
Embodiment 1: the mensuration of potassium, sodium element in the vanadium carbide (sample y-1)
Take by weighing 0.2500 gram vanadium carbide test portion and place the 150mL quartz beaker, with deionized water purge wall of cup, adding purity then successively is high-purity (MOS level), mass concentration is hydrochloric acid (following examples the are identical) 9.0mL (milliliter) of 1.19g/mL (grams per milliliter), purity is high-purity (MOS level), mass concentration is nitric acid (following examples the are identical) 3.0mL of 1.42g/mL, mixing, cover bowl cover, place on the electric hot plate, 60～80 ℃ are heated to dissolving fully, take off cooling, solution is moved in the 50ml plastics volumetric flask, in order to ensure analyzing and testing result's precision, by potassium in the test samples, the conventional way of sodium element, adding mass concentration again is that 10g/L (gets 5g and analyzes pure cesium chloride, be dissolved in the 500mL plastics volumetric flask with deionized water, mixing) ionization buffer cesium chloride solution (following examples are identical) 2.0ml is diluted to scale with deionized water, mixing, and with the test solution filtration, to remove the uncombined carbon that may exist in the test portion.By the listed instrument condition of work of above-mentioned table 1, with the potassium of blank, vanadium carbide test solution and vanadium matrix coupling, sodium mixed standard solution series is measured its potassium, sodium element simultaneously on atomic absorption spectrophotometer (AAS) absorbance.
Absorbance according to potassium, sodium element in the vanadium carbide test solution of measuring, find the mass concentration of corresponding tested element from aforementioned typical curve when being 20.0g/L vanadium matrix solution 10mL (add mass concentration draw), by aforementioned formula (1) Calculation results.Measure carry out repeatedly (more than five times, following examples are identical) with a collection of vanadium carbide sample, the mean value of measurement result, standard deviation, relative standard deviation see Table 2.
Table 2 analysis result and precision
| Element | Measurement result mean value (%) | Standard deviation (%) | Relative standard deviation (%) |
| Potassium | 0.0012? | 0.000060? | 5.00? |
| Sodium | 0.0017? | 0.000084? | 4.94? |
Embodiment 2: the mensuration of potassium, sodium element in the vanadium carbide (sample y-2)
Take by weighing 0.2500 gram vanadium carbide test portion and place the 150mL quartz beaker,, add hydrochloric acid 12.0mL (milliliter) then successively with deionized water purge wall of cup, nitric acid 4.0mL, mixing covers bowl cover, place on the electric hot plate, 60～80 ℃ are heated to dissolving fully, take off cooling, and solution is moved in the 50ml plastics volumetric flask, add ionization buffer cesium chloride solution 2.0ml, be diluted to scale with deionized water, mixing, test solution filters.Under the instrument condition of work identical, with the potassium of blank, vanadium carbide test solution and vanadium matrix coupling, the sodium mixed standard solution series absorbance of its potassium of mensuration, sodium element on atomic absorption spectrophotometer (AAS) simultaneously with embodiment 1.
Absorbance according to potassium, sodium element in the vanadium carbide test solution of measuring, find the mass concentration of corresponding tested element from aforementioned typical curve (add and draw when mass concentration is 20.0g/L vanadium matrix solution 10mL), and press aforementioned formula (1) Calculation results.To repeatedly measuring with a collection of vanadium carbide sample, the mean value of measurement result, standard deviation, relative standard deviation see Table 3.
Table 3 analysis result and precision
| Element | Measurement result mean value (%) | Standard deviation (%) | Relative standard deviation (%) |
| Potassium | 0.0019? | 0.000071? | 3.74? |
| Sodium | 0.0030? | 0.000084? | 2.80? |
Embodiment 3: the mensuration of potassium, sodium element in the vanadium carbide (sample y-3)
Take by weighing 0.2500 gram vanadium carbide test portion and place the 150mL quartz beaker,, add hydrochloric acid 15mL (milliliter) then successively with deionized water purge wall of cup, nitric acid 5mL, mixing covers bowl cover, place on the electric hot plate, 60～80 ℃ are heated to dissolving fully, take off cooling, and solution is moved in the 50ml plastics volumetric flask, add ionization buffer cesium chloride solution 2.0ml, be diluted to scale with deionized water, mixing, test solution filters.Under the instrument condition of work identical, with the potassium of blank, vanadium carbide test solution and vanadium matrix coupling, the sodium mixed standard solution series absorbance of its potassium of mensuration, sodium element on atomic absorption spectrophotometer (AAS) simultaneously with embodiment 1.
Absorbance according to potassium, sodium element in the vanadium carbide test solution of measuring, find the mass concentration of corresponding tested element from aforementioned standard working curve (add and draw when mass concentration is 20.0g/L vanadium matrix solution 10mL), and press aforementioned formula (1) Calculation results.
The potassium in the vanadium carbide sample of surveying, sodium element measurement result are generally all less than 0.010%, for potassium, sodium element content are checked greater than precision of carrying out method under 0.010% the condition and accuracy, take by weighing with a collection of vanadium carbide sample, add a certain amount of potassium, sodium mixed standard solution respectively, carry out mark-on and reclaim experiment, also repeatedly measure by above-mentioned sample determination step, mean value, standard deviation, relative standard deviation and the recovery data of calculating measurement result see Table 4.
Table 4 analysis result and precision
| Element | Measurement result mean value (%) | Standard deviation (%) | Relative standard deviation (%) | The recovery (%) |
| Potassium | 0.010? | 0.00057? | 5.67? | 105.0? |
| Sodium | 0.013? | 0.00055? | 4.23? | 95.5? |
[0052]Embodiment 4: the mensuration of potassium, sodium element in the vanadium carbide (sample y-4)
Take by weighing 0.1250 gram vanadium carbide test portion and place the 150mL quartz beaker,, add hydrochloric acid 9mL (milliliter) then successively with deionized water purge wall of cup, nitric acid 3mL, mixing covers bowl cover, place on the electric hot plate, 60～80 ℃ are heated to dissolving fully, take off cooling, and solution is moved in the 50ml plastics volumetric flask, add ionization buffer cesium chloride solution 2.0ml, be diluted to scale with deionized water, mixing, test solution filters.Under the instrument condition of work identical, with the potassium of blank, vanadium carbide test solution and vanadium matrix coupling, the sodium mixed standard solution series absorbance of its potassium of mensuration, sodium element on atomic absorption spectrophotometer (AAS) simultaneously with embodiment 1.
Absorbance according to potassium, sodium element in the vanadium carbide test solution of measuring, find the mass concentration of corresponding tested element from aforementioned standard working curve (add and draw when mass concentration is 20.0g/L vanadium matrix solution 5mL), and press aforementioned formula (1) Calculation results.
The general potassium in the vanadium carbide sample of surveying, sodium element measurement result are generally all less than 0.010%, but also there is content high slightly, for to impurity content at 0.05%～0.10% o'clock, carry out the precision and the accuracy check of method, take by weighing with a collection of vanadium carbide sample, add a certain amount of potassium, sodium mixed standard solution respectively, carry out mark-on and reclaim experiment, repeatedly measure by above-mentioned sample determination step, the mean value of Calculation results, standard deviation, relative standard deviation and the recovery, data see Table 5.
Table 5 analysis result, precision and the recovery
| Element | Measurement result mean value (%) | Standard deviation (%) | Relative standard deviation (%) | The recovery (%) |
| Potassium | 0.051? | 0.00114? | 2.24? | 98.0? |
| Sodium | 0.056? | 0.00148? | 2.64? | 101.5? |
Above embodiment explanation: according to the analyzing detecting method of potassium, sodium impurity elements in the vanadium carbide of the present invention, sample is carried out mark-on reclaim experiment, the recovery is all between 95%～105%; Sample is carried out independent mensuration more than five times, and the relative standard deviation of method illustrates that all less than 5.7% the inventive method has good accuracy and precision, is accurately feasible.
Claims (2)
1. the analyzing detecting method of potassium, sodium impurity elements in the vanadium carbide adds the ionization buffer cesium chloride solution when being included in preparation vanadium carbide test solution and standard solution series, it is characterized in that it comprises the steps:
(1) the vanadium carbide test portion is placed quartz beaker, behind deionized water purge wall of cup, add volume ratio successively and be 3: 1 hydrochloric acid and nitric acid, hydrochloric acid purity is that MOS level, mass concentration are 1.19 grams per milliliters, and addition is 7.5～15 milliliters, nitric acid purity is that MOS level, mass concentration are 1.42 grams per milliliters, addition is 2.5～5 milliliters, and mixing covers bowl cover, heating for dissolving, heating for dissolving temperature are 60～80 ℃;
(2) consoluet vanadium carbide test solution is moved in the plastics volumetric flask, be diluted to scale with deionized water, mixing filters;
(3) the standard solution series of the potassium of preparation vanadium matrix coupling, sodium mixing;
(4) under selected instrument condition of work, vanadium carbide test solution and the mixed standard solution series of (3) preparation are measured the absorbance of potassium, sodium element simultaneously on atomic absorption spectrophotometer (AAS), find the concentration of corresponding tested element again from typical curve, Calculation results.
2. the analyzing detecting method of potassium, sodium impurity elements in the vanadium carbide according to claim 1, the potassium, the sodium mixed standard solution that it is characterized in that preparing vanadium matrix coupling need add the vanadium matrix solution suitable with the test portion amount when serial, when taking by weighing sample size was 0.1250～0.2500 when gram, added mass concentration and be 5～10 milliliters of the vanadium matrix solution of 20.0 grams per liters.
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| CN102539362B (en) * | 2010-12-30 | 2013-10-16 | 中国科学院金属研究所 | Ultraviolet quantitative determination method for concentration of electrolyte of positive electrode of vanadium battery and application thereof |
| CN102735638A (en) * | 2012-07-12 | 2012-10-17 | 南南铝业股份有限公司 | Method for analyzing and determining potassium and sodium contents in aluminum alloy smelting agent |
| CN103575669B (en) * | 2012-08-08 | 2016-05-04 | 四川奇力制药有限公司 | The potassium chloride of potassium chloride in sodium chloride inj and the assay method of sodium chloride content |
| CN102954941A (en) * | 2012-10-24 | 2013-03-06 | 中国航空工业集团公司北京航空材料研究院 | Method for determining sodium and potassium in tantalum-containing high-temperature alloy by atomic absorption spectrometry |
| CN102914513A (en) * | 2012-11-06 | 2013-02-06 | 长沙伟徽高科技新材料股份有限公司 | Analysis detection method of iron element in vanadium carbide |
| CN110567944A (en) * | 2019-09-11 | 2019-12-13 | 自贡硬质合金有限责任公司 | Method for measuring trace iron, aluminum, silicon and calcium in vanadium carbide |
| CN111257097A (en) * | 2020-01-20 | 2020-06-09 | 攀枝花学院 | Vanadium carbide sample to be tested manufacturing method and impurity content analysis method thereof |
| CN113029987A (en) * | 2021-03-30 | 2021-06-25 | 上海耀大生物科技有限公司 | Method for measuring total sodium content in compound polyethylene glycol electrolyte powder |
| CN114324306B (en) * | 2021-12-14 | 2024-05-28 | 武汉钢铁有限公司 | Combined measuring method for phosphorus and arsenic content in gas mud and gas ash |
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