CN104359903A - Novel method for measuring iron content in waste mortar - Google Patents
Novel method for measuring iron content in waste mortar Download PDFInfo
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- CN104359903A CN104359903A CN201410655680.0A CN201410655680A CN104359903A CN 104359903 A CN104359903 A CN 104359903A CN 201410655680 A CN201410655680 A CN 201410655680A CN 104359903 A CN104359903 A CN 104359903A
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Abstract
The invention relates to a novel method for measuring iron content in waste mortar. The method comprises the following steps: (1) performing acid leaching treatment: drying and grinding waste mortar to powder, adding deionized water, adding a sulfuric acid solution under continuous stirring for acid leaching treatment (the mass ratio of the waste mortar to concentrated sulfuric acid is 1.0: (1.2-2.0), stirring for reacting at 35-80 DEG C, then, filtering an acid leaching waste solution, then washing for 3-5 times by using deionized water, transferring the acid leaching waste solution and the washing liquid to a volumetric flask, making the volume constant by deionized water, and standing for 1-3 hours for later use; and (2) transferring a to-be-measured liquid obtained in the step (1) into the volumetric flask, sequentially adding 0.5-3ml of a 10% hydroxylamine hydrochloride solution, 10mg/L of a phenanthroline developing liquid and 3-8mL of a sodium acetate-acetic acid buffer solution, making the volume constant by distilled water, and after standing and developing, measuring the absorbancy at 500-520nm. The method is strong in anti-interference on heavy metal chromium in the waste mortar, high in accuracy and precision, simple to operate and relatively low in cost, thereby facilitating recycle of scrap iron in the waste iron.
Description
Technical field
The present invention relates to a kind of new method measuring iron content in waste mortar, the method is to the heavy metal chromium strong interference immunity contained in powder of stainless steel in waste mortar, and accuracy, precision are high, simple to operate, cost is lower, is conducive to the recycling of iron filings in waste mortar, belongs to environmental technology field.
Background technology
In photovoltaic industry and semiconductor manufacturing industry, usually adopt line cutting technology that highly purified monocrystalline silicon and polycrystalline silicon rod are cut into satisfactory silicon chip, in the process, a large amount of waste mortars can be produced.Main containing polyglycol, silicon carbide micro-powder, simple substance silica flour, iron and stainless steel powder etc. in this mortar.If directly discharged by waste mortar, not only to environment, and the serious waste of resource can be caused.Therefore, silicon cutting waste mortar is recycled, there is higher environmental protection and economy and be worth.
At present polyglycol, silicon and silit are only limitted to the research of the recycling of waste mortar.Comparatively considerable based on the iron content in mortar, can pickling be passed through, the ferrous iron solution of generation is applied in the purified treatment of process water, thus reach the recycling of iron filings in waste mortar, thus be necessary to measure the iron content in waste mortar.Traditional waste mortar componential analysis is gravimetric method, and technique is more loaded down with trivial details, and accuracy is low.Also have some relevant reports, its common ground mainly by first being separated by the iron in waste mortar, then carries out assay.These existing methods have complex process, are easy to the interference being subject to heavy metal chromium, and accuracy and precision are not high, and the shortcoming that consuming cost is high is unfavorable for the mensuration of iron content in waste mortar.
Summary of the invention
The object of the invention is to overcome traditional waste mortar component analyzing method and the deficiencies in the prior art, ferrous ion and Phen is utilized to generate stable comple, the character of characteristic absorption is had in visible region, establish the method for iron content in a kind of Accurate Measurement waste mortar, the method is simple and direct, strong interference immunity to heavy metal chromium in powder of stainless steel in waste mortar, accuracy and precision high, be suitable for the quantitative test of iron content in waste mortar.
The invention provides a kind of new method measuring iron content in waste mortar, it is characterized in that, comprise the following steps:
(1) acidleach process: by waste mortar dry, be ground to Powdered, add deionized water, under Keep agitation, add sulfuric acid solution wherein and carry out cleanup acid treatment (waste mortar and concentrated sulphuric acid mass ratio are 1.0:1.2 ~ 2.0), stirring reaction under 35 ~ 80 DEG C of conditions, then pickle liquor is filtered, then spend deionized water 3 ~ 5 times, pickle liquor and cleansing solution are transferred in volumetric flask, use deionized water constant volume, after shaking up, leave standstill 1 ~ 3h, stand-by;
(2) liquid to be measured will obtained in step (1), move in volumetric flask, add 10% hydroxylamine hydrochloride solution of 0.5 ~ 3mL more successively, the o-phenanthrolin nitrite ion of 10mg/L, sodium acetate-the hac buffer of 3 ~ 8mL, shaking up with distilled water constant volume, after leaving standstill colour developing, is 500 ~ 520nm place its absorbance of mensuration at maximum absorption wavelength.
Further, in described step (1), the concentration of sulfuric acid solution is 0.01 ~ 0.1mol/L.
Further, in described step (1), the time of acid-leaching reaction is 0.5 ~ 2h.
Further, in described step (2), the consumption of the o-phenanthrolin nitrite ion of 10mg/L is 1 ~ 3.5mL.
Further, in described step (2), the pH value of sodium acetate-hac buffer is 2 ~ 7.
Further, in described step (2), standing developing time is 5 ~ 120min.
Beneficial effect of the present invention comprises:
(1) technique is simple, with low cost;
(2) strong interference immunity of heavy metal chromium, accuracy and precision is high;
(3 measure process cleans environmental protection, meet green requirement of producing.
Accompanying drawing explanation
Technical scheme of the present invention is described in detail referring to accompanying drawing, wherein:
Fig. 1 shows the typical curve of ferric ion, and with iron concentration (mg/L) for horizontal ordinate X, take absorbance A as ordinate Y, Criterion curve, curvilinear equation is Y=0.19445X+0.022, R
2=0.9996.Shown by figure, iron concentration meets Beer law within the scope of 0 ~ 2mg/L.
Fig. 2 shows the method anti-interference, and namely chromium measures the impact of iron content on spectrophotometer method.As seen from the figure, along with the increase of chromium addition, less on the impact of absorbance, therefore in spectrophotometry waste mortar, the anti-interference of iron content to crome metal a small amount of in powder of stainless steel is stronger.
Embodiment
Below in conjunction with specific embodiment and accompanying drawing, the invention will be further described.
According to a kind of new method measuring iron content in waste mortar provided by the invention, its measuring principle is as follows: under certain acidity condition, Fe
2 +can generate stable orange-red complex compound with Phen, this complex compound has characteristic absorption peak near 510nm, Fe
2 +concentration and absorbance meet langbobier law, are applicable to Iron Measurement.Shown in reaction equation following (I):
Embodiment one: a kind of new method measuring iron content in waste mortar, comprises the following steps:
(1) acidleach process: by waste mortar dry, be ground to Powdered, add deionized water, under Keep agitation, the sulfuric acid solution adding 0.01mol/L wherein carries out cleanup acid treatment (waste mortar and concentrated sulphuric acid mass ratio are 1.0:1.2), stirring reaction 0.5h under 35 DEG C of conditions, then pickle liquor is filtered, then spend deionized water 3 times, pickle liquor and cleansing solution are transferred in volumetric flask, use deionized water constant volume, after shaking up, leave standstill 1h, stand-by;
(2) liquid to be measured will obtained in step (1), move in volumetric flask, add 10% hydroxylamine hydrochloride solution of 0.5mL more successively, the 10mg/L o-phenanthrolin nitrite ion of 1mL, the pH of 3mL is the sodium acetate-hac buffer of 2, shaking up with distilled water constant volume, after leaving standstill colour developing 5min, is 500nm place its absorbance of mensuration at maximum absorption wavelength.
Embodiment two: a kind of new method measuring iron content in waste mortar, comprises the following steps:
(1) acidleach process: by waste mortar dry, be ground to Powdered, add deionized water, under Keep agitation, the sulfuric acid solution adding 0.03mol/L wherein carries out cleanup acid treatment (waste mortar and concentrated sulphuric acid mass ratio are 1.0:1.4), stirring reaction 1h under 40 DEG C of conditions, then pickle liquor is filtered, then spend deionized water 3 times, pickle liquor and cleansing solution are transferred in volumetric flask, use deionized water constant volume, after shaking up, leave standstill 2h, stand-by;
(2) liquid to be measured will obtained in step (1), move in volumetric flask, add 10% hydroxylamine hydrochloride solution of 1mL more successively, the 10mg/L o-phenanthrolin nitrite ion of 2mL, the pH of 4mL is the sodium acetate-hac buffer of 3, shaking up with distilled water constant volume, after leaving standstill colour developing 45min, is 511nm place its absorbance of mensuration at maximum absorption wavelength.
Embodiment three: a kind of new method measuring iron content in waste mortar, comprises the following steps:
(1) acidleach process: by waste mortar dry, be ground to Powdered, add deionized water, under Keep agitation, the sulfuric acid solution adding 0.06mol/L wherein carries out cleanup acid treatment (waste mortar and concentrated sulphuric acid mass ratio are 1.0:1.8), stirring reaction 1h under 65 DEG C of conditions, then pickle liquor is filtered, then spend deionized water 4 times, pickle liquor and cleansing solution are transferred in volumetric flask, use deionized water constant volume, after shaking up, leave standstill 2h, stand-by;
(2) liquid to be measured will obtained in step (1), move in volumetric flask, add 10% hydroxylamine hydrochloride solution of 2mL more successively, the 10mg/L o-phenanthrolin nitrite ion of 3mL, the pH of 6mL is the sodium acetate-hac buffer of 5, shaking up with distilled water constant volume, after leaving standstill colour developing 80min, is 511nm place its absorbance of mensuration at maximum absorption wavelength.
Embodiment four: a kind of new method measuring iron content in waste mortar, comprises the following steps:
(1) acidleach process: by waste mortar dry, be ground to Powdered, add deionized water, under Keep agitation, the sulfuric acid solution adding 0.1mol/L wherein carries out cleanup acid treatment (waste mortar and concentrated sulphuric acid mass ratio are 1.0:2.0), stirring reaction 2h under 80 DEG C of conditions, then pickle liquor is filtered, then spend deionized water 5 times, pickle liquor and cleansing solution are transferred in volumetric flask, use deionized water constant volume, after shaking up, leave standstill 3h, stand-by;
(2) liquid to be measured will obtained in step (1), move in volumetric flask, add 10% hydroxylamine hydrochloride solution of 3mL more successively, the 10mg/L o-phenanthrolin nitrite ion of 3.5mL, the pH of 8mL is the sodium acetate-hac buffer of 7, shaking up with distilled water constant volume, after leaving standstill colour developing 120min, is 520nm place its absorbance of mensuration at maximum absorption wavelength.
Adopt the accuracy analysis of iron content in determined by ultraviolet spectrophotometry waste mortar:
Get 6 100mL volumetric flasks, add the waste mortar filtrate 5mL after acidleach process respectively, add iron ammonium sulfate standard solution 2mL, 4mL, 6mL, 8mL, 10mL, 12mL that iron-holder is 100mg/L more respectively, shake up with deionized water constant volume, the iron concentration of sampling and measuring solution, measurement result is as shown in table 1 below.
Table 1 accuracy experimental result
As shown in Table 6, the average recovery rate of mensuration is 98.92%, illustrates that spectrophotometric method is used for iron content accuracy of measurement in waste mortar higher.
The present invention utilizes ferrous ion and Phen to generate stable comple, provide the new method of iron content in a kind of Accurate Measurement waste mortar, the method is simple and direct, strong interference immunity to heavy metal chromium in powder of stainless steel in waste mortar, accuracy and precision high, be suitable for the quantitative test of iron content in waste mortar.
Although above in conjunction with the embodiments to invention has been detailed description; but; the present invention is not limited to above-mentioned embodiment; in the ken that those of ordinary skill in the art possess; under not departing from the prerequisite of present inventive concept; can also in claims, above-described embodiment is changed or change etc.
Claims (6)
1. measure a new method for iron content in waste mortar, it is characterized in that, comprise the following steps:
(1) acidleach process: by waste mortar dry, be ground to Powdered, add deionized water, under Keep agitation, add sulfuric acid solution wherein and carry out cleanup acid treatment (waste mortar and concentrated sulphuric acid mass ratio are 1.0:1.2 ~ 2.0), stirring reaction under 35 ~ 80 DEG C of conditions, then pickle liquor is filtered, then spend deionized water 3 ~ 5 times, pickle liquor and cleansing solution are transferred in volumetric flask, use deionized water constant volume, after shaking up, leave standstill 1 ~ 3h, stand-by;
(2) liquid to be measured will obtained in step (1), move in volumetric flask, add 10% hydroxylamine hydrochloride solution of 0.5 ~ 3mL more successively, the o-phenanthrolin nitrite ion of 10mg/L, sodium acetate-the hac buffer of 3 ~ 8mL, shaking up with distilled water constant volume, after leaving standstill colour developing, is 500 ~ 520nm place its absorbance of mensuration at maximum absorption wavelength.
2. measure the new method of iron content in waste mortar as claimed in claim 1, it is characterized in that: in described step (1), the concentration of sulfuric acid solution is 0.01 ~ 0.1mol/L.
3. measure the new method of iron content in waste mortar as claimed in claim 1, it is characterized in that: in described step (1), the time of acid-leaching reaction is 0.5 ~ 2h.
4. measure the new method of iron content in waste mortar as claimed in claim 1, it is characterized in that: in described step (2), the consumption of the o-phenanthrolin nitrite ion of 10mg/L is 1 ~ 3.5mL.
5. measure the new method of iron content in waste mortar as claimed in claim 1, it is characterized in that: in described step (2), the pH value of sodium acetate-hac buffer is 2 ~ 7.
6. measure the new method of iron content in waste mortar as claimed in claim 1, it is characterized in that: in described step (2), standing developing time is 5 ~ 120min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107561025A (en) * | 2017-07-20 | 2018-01-09 | 武汉纺织大学 | A kind of method of quantitative determination iron-oxidizing bacteria to iron oxidability |
| CN111077036A (en) * | 2019-12-30 | 2020-04-28 | 广州傲农生物科技有限公司 | Rapid determination method for detecting content of ferrous iron in various iron additives |
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| CN101738391A (en) * | 2008-11-12 | 2010-06-16 | 中国科学院沈阳应用生态研究所 | Mensuration method for amorphous Fe in soil |
| CN103439213A (en) * | 2013-09-02 | 2013-12-11 | 武汉钢铁(集团)公司 | System detection method for components in industrial silicon carbide |
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2014
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| CN101738391A (en) * | 2008-11-12 | 2010-06-16 | 中国科学院沈阳应用生态研究所 | Mensuration method for amorphous Fe in soil |
| CN103439213A (en) * | 2013-09-02 | 2013-12-11 | 武汉钢铁(集团)公司 | System detection method for components in industrial silicon carbide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107561025A (en) * | 2017-07-20 | 2018-01-09 | 武汉纺织大学 | A kind of method of quantitative determination iron-oxidizing bacteria to iron oxidability |
| CN111077036A (en) * | 2019-12-30 | 2020-04-28 | 广州傲农生物科技有限公司 | Rapid determination method for detecting content of ferrous iron in various iron additives |
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