CN102590130A - Method for quantificationally and rapidly detecting content of silicon in quartz sand by infrared method - Google Patents

Abstract

The invention discloses a method for quantificationally and rapidly detecting the content of silicon in quartz sand by an infrared method. According to the method, the content of the silicon in a quartz sand sample is determined by using an infrared instrument, and a solid phase of the quartz sand is directly determined and is not required to be dissolved and volatilized by using hydrofluoric acid, so that the disadvantages that the time is consumed, steps are fussy, toxic solvents such as the hydrofluoric acid are required in other methods are overcome, the method is environment-friendly, and an analysis result is more accurate and time-saving; and aims of economy and practicability are expected to be fulfilled, and the method has a good application prospect.

Description

The method of silicone content in the quantitative fast detecting silica sand of infrared method

Technical field

The invention discloses the detection method of silicone content in the quantitative fast detecting silica sand of a kind of infrared method, specifically relate to the method for silicone content in the quantitative fast detecting silica sand of a kind of infrared method.

Background technology

The mensuration accuracy of silicon content and ageing in the silica sand is utilization factor and the added value that directly has influence on silica sand, need to set up save time, environmental protection, the easy and detection method that is easy to promote.

The method (National Standard Method) that detects silicone content at present in the production is to adopt gravimetric method, promptly uses hydrofluoric acid dissolution and heated volatile, asks the of poor quality of its dissolving volatilization front and back.But there are many problems in this National Standard Method: the one, and the detection method complicated operating process needs heating for dissolving, during consumption energy consumption; The 2nd, the poisonous and hazardous chemical reagent hydrofluorite amount of using in the course of dissolution is very big, and the silicon tetrafluoride of hydrofluorite and generation will inevitably cause the pollution of environment, if ventilation condition is bad even can cause the infringement of testing staff's health.

Summary of the invention

In order to solve the technical matters that exists in the prior art, the object of the present invention is to provide the infrared appearance of a kind of usefulness rapidly and efficiently to detect the method for silicon content in the silica sand, silica sand solid phase detection by quantitative is further studied.

The technical scheme that the present invention adopts is following:

The method of silicone content is characterized in that in the quantitative fast detecting silica sand of infrared method, and the assay of elemental silicon adopts infrared appearance internal standard method or infrared appearance rule of three to carry out quantitative measurement in the silica sand.

Further, be added with solid brominated potassium or potassium rhodanide in the silica sand.

Comparatively perfect is that infrared appearance rule of three comprises the steps:

Take by weighing 0.0005～0.0030g standard sample (99.80%) and 0.0500～0.4000g potassium bromide with electronic balance; In mortar, grind till particle grinds and evenly mixes the back; Carry out then all and quantitative compressing tablet; Compressing tablet is put into infrared spectrometer with the mixing sheet compressing tablet of gained and is tested after accomplishing, and obtains infrared spectrum;

Take by weighing 0.0005～0.0030g with electronic balance and treat test sample and 0.0500～0.4000g potassium bromide; In mortar, grind till particle grinds and evenly mixes the back; Carry out then all and quantitative compressing tablet; Compressing tablet is put into infrared spectrometer with the mixing sheet compressing tablet of gained and is tested after accomplishing, and obtains infrared spectrum;

By comparing the absorbance of representing the independent peak of each component in the infrared spectrum,, obtain relative content between the component according to Lambert-Beer's law.

Comparatively perfect is that infrared appearance internal standard method comprises the steps:

0.0005g～0.0030g standard sample (99.80%) and 0.0006g～0.0030g potassium rhodanide have been taken by weighing with electronic balance; In mortar, being ground to does not have particle and mixes; Carry out then all and quantitative compressing tablet; Compressing tablet puts it in the infrared spectrometer and tests after accomplishing, and obtains infrared spectrum;

Taken by weighing the test sample of treating of 0.0010g～0.0060g again with electronic balance, 0.0015g～0.0070g potassium rhodanide, in mortar, being ground to does not have particle and mixes; Carry out then all and quantitative compressing tablet; Compressing tablet puts it in the infrared spectrometer and tests after accomplishing, and obtains infrared spectrum;

Characteristic absorption peak area and interior mark characteristic absorption peak area with testing sample compare, and be so same under the situation of unknown sample thickness, can directly determine the content of silicon components in sample.

Further, the particle diameter of said silica sand is more than 40 orders.

For other trace element beyond the silica removal in the silica sand, though also can adopt existing infrared detection technology to detect, the error of its detection is bigger.

The present invention is according to the abundant quartz sand resources in Fengyang, and contrived experiment uses infrared appearance solid phase quantitative methods to detect, to save time and to protect environment, in the hope of reaching not only economy but also practical purpose.

The present invention carries out the silica sand solid phase and directly measures, need not with hydrofluoric acid dissolution and volatilization, has overcome consuming time in the additive method, and complex steps needs the deficiency with toxic solvents such as hydrofluorite, and both environmental protections make analysis result more accurately, more save time again.

Embodiment

One, infrared appearance rule of three detects

Take by weighing 0.0005～0.0030g standard sample (99.80%) and 0.0500～0.4000g potassium bromide with electronic balance; In mortar, grind till particle grinds and evenly mixes the back; Carry out then all and quantitative compressing tablet, compressing tablet is put into infrared spectrometer with the mixing sheet compressing tablet of gained and is tested after accomplishing; Obtain infrared spectrum, carry by spectrometer and ask peak area software to try to achieve wave number at 1100cm ^-1The peak area of (silicon oxygen bond goes out the peak position) is 809～822.

Take by weighing 0.0005～0.0030g with electronic balance and treat test sample and 0.0500～0.4000g potassium bromide; In mortar, grind till particle grinds and evenly mixes the back; Carry out then all and quantitative compressing tablet, compressing tablet is put into infrared spectrometer with the mixing sheet compressing tablet of gained and is tested after accomplishing; Obtain infrared spectrum, obtain treating that the peak area of test sample is 812～825.

If the absorbance of standard sample is A _M, the absorbance of treating test sample is A _N, know by the Lambert-Beer law:

A _M＝a _Mb _MC _M A _N＝a _Nb _NC _N

Owing under same condition, measure then: a _M=a _N, b _M=b _NSo,

Substitution data (replacing absorbance etc. accurately with peak area in the experimentation) must treat that the silicone content of test sample is 98.60%～99.50%.

The content that records this sample through gravimetric method is 99.10%～99.30%, and using rule of three gained result to compare its relative error with it is-0.70%～0.30%.

Two, infrared appearance internal standard method detects

0.0005g～0.0030g standard sample (99.80%) and 0.0006g～0.0030g potassium rhodanide have been taken by weighing with electronic balance; In mortar, being ground to does not have particle and mixes; Carry out then all and quantitative compressing tablet; Compressing tablet puts it in the infrared spectrometer and tests after accomplishing, and obtains infrared spectrum.

Taken by weighing the test sample of treating of 0.0010g～0.0060g again with electronic balance, 0.0015g～0.0070g potassium rhodanide, in mortar, being ground to does not have particle and mixes; Carry out then all and quantitative compressing tablet; Compressing tablet puts it in the infrared spectrometer and tests after accomplishing, and obtains infrared spectrum.

In drawing, the calculated by peak area software that is carried by the spectrogram software for drawing is marked on 2048cm ^-1Place's peak area is 36.60～36.90 and 76.70～76.95, sample and treat that test sample is at 800cm ^-1Peak area be 3.5～8.50 and 7.7～11.5, at 1085cm ^-1The place is because the peak has overlapping the needs to proofread and correct, owing to be same substance, so three places have the overlapping peak area sum and the ratio of place's independence peak-to-peak area wherein to should be a constant, can obtain this ratio through the independent spectrogram of potassium rhodanide, with this ratio to 1085cm ^-1The peak area at place is proofreaied and correct.

At 1085cm ^-1The place is by the internal standard method computing formula $C_{1M}=\frac{A_{1M}}{A_M}\·\frac{A_K}{A_{1K}}\·\frac{C_{1K}}{C_K}\·C_M$ With $M_1=\frac{C_{1M}}{W_1}\×100\%,$ The substitution data are calculated, and must record the silicone content of treating test sample is 98.70%～99.40%.

The content that records this sample through gravimetric method is 99.10%～99.30%, and using rule of three gained result to compare its relative error with it is-0.50%～0.20%.

Three, infrared method detects the advantage of silicone content in the silica sand

Single detects index	Conventional (GB) method	Infrared method
			Detection time	3～6 hours	0.5～1 hour
The HF consumption	15～25mL	0mL
			SiF 4Volatile quantity	0.01～0.03mol	0mol
The value of promoting	Though accurately, time-consuming, pollution weighs	Environmental protection accurately, fast,

Four, conclusion

Through measuring; Come directly to measure the method for the content of silicon dioxide in the solid silica sand through having adopted infrared spectrum rule of three and internal standard method; Need not with hydrofluoric acid dissolution and volatilization; Not only solved the complicated problem during with consumption energy consumption of gravimetric method testing process, and solved toxic gases such as no hydrofluorite and silicon tetrafluoride and produce, have with infrared quantitative detection detection silica sand save time, environmental protection, easy and the characteristics and the superiority that are easy to promote.

Above content only is to give an example and explanation to what structure of the present invention was done; Under the technician in present technique field various modifications that described specific embodiment is made or replenish or adopt similar mode to substitute; Only otherwise depart from the structure of invention or surmount the defined scope of these claims, all should belong to protection scope of the present invention.

Claims (5)

1. the method for silicone content in the quantitative fast detecting silica sand of infrared method is characterized in that, the assay of elemental silicon adopts infrared appearance internal standard method or infrared appearance rule of three to carry out quantitative measurement in the silica sand.

2. the method for silicone content is characterized in that in the quantitative fast detecting silica sand of infrared method according to claim 1, is added with solid brominated potassium or potassium rhodanide in the silica sand.

3. the method for silicone content is characterized in that in the quantitative fast detecting silica sand of infrared method according to claim 2, and infrared appearance rule of three comprises the steps:

Take by weighing 0.0005～0.0030g standard sample (99.80%) and 0.0500～0.4000g potassium bromide with electronic balance; In mortar, grind till particle grinds and evenly mixes the back; Carry out then all and quantitative compressing tablet; Compressing tablet is put into infrared spectrometer with the mixing sheet compressing tablet of gained and is tested after accomplishing, and obtains infrared spectrum;

Take by weighing 0.0005～0.0030g with electronic balance and treat test sample and 0.0500～0.4000g potassium bromide; In mortar, grind till particle grinds and evenly mixes the back; Carry out then all and quantitative compressing tablet; Compressing tablet is put into infrared spectrometer with the mixing sheet compressing tablet of gained and is tested after accomplishing, and obtains infrared spectrum;

By comparing the absorbance of representing the independent peak of each component in the infrared spectrum,, obtain relative content between the component according to Lambert-Beer's law.

4. the method for silicone content is characterized in that in the quantitative fast detecting silica sand of infrared method according to claim 2, and infrared appearance internal standard method comprises the steps:

0.0005g～0.0030g standard sample (99.80%) and 0.0006g～0.0030g potassium rhodanide have been taken by weighing with electronic balance; In mortar, being ground to does not have particle and mixes; Carry out then all and quantitative compressing tablet; Compressing tablet puts it in the infrared spectrometer and tests after accomplishing, and obtains infrared spectrum;

Taken by weighing the test sample of treating of 0.0010g～0.0060g again with electronic balance, 0.0015g～0.0070g potassium rhodanide, in mortar, being ground to does not have particle and mixes; Carry out then all and quantitative compressing tablet; Compressing tablet puts it in the infrared spectrometer and tests after accomplishing, and obtains infrared spectrum;

Characteristic absorption peak area and interior mark characteristic absorption peak area with testing sample compare, and be so same under the situation of unknown sample thickness, can directly determine the content of silicon components in sample.

5. according to the method for silicone content in the quantitative fast detecting silica sand of each described infrared method of claim 1～4, it is characterized in that the particle diameter of said silica sand is more than 40 orders.