CN103412028B - Method for testing content of sodium oxide in silica sol - Google Patents

Abstract

The invention belongs to the technology of sol elements, and relates to an improvement on the method for testing the content of sodium oxide in silica sol. The method is characterized by comprising the following steps: diluting a sample; fixing the volume of a silica sol sample dilute; performing the pH value calibration on an automatic potentiometic titrator; titrating silica sol sample to-be-tested solution; calculating the content of sodium oxide. The invention provides a method for testing the content of sodium oxide in silica sol, reduces the testing error, and improves the testing repeatability.

Description

A kind of method measuring sodium oxide content in silicasol

Technical field

The invention belongs to colloidal sol element analysis technology, relating to the improvement to measuring sodium oxide content method in silicasol.

Background technology

Silicasol is at present conventional a kind of binder product, because the silica aqueous solution of neutrality is very unstable, and its pH value will be made to be greater than more than 8.5 just can reach steady state (SS).So neutral silicasol is by adding stabilizing agent NaOH, and then concentratedly just industrial requirements can be reached.Thus Na ₂o content is the important indicator characterizing silicasol product quality.Therefore, must the strict content controlling sodium oxide molybdena in silicasol.At present, the method measuring sodium oxide content in silicasol is: employing methyl red is indicator, by the method for sodium oxide molybdena in watery hydrochloric acid standard solution titration silicasol sample liquid to be measured.See navigation mark HB5346-86, its shortcoming is: employing methyl red is indicator, and titration end-point sudden change is not obvious, and titration end-point not easily judges, causes error at measurment large, the poor repeatability of mensuration.In production practices, the relative standard deviation of said method is 4.26%.

Summary of the invention

The object of the invention is: the assay method proposing sodium oxide content in a kind of silicasol of easy judgement titration end-point, to reduce error at measurment, improve the repeatability measured.

Technical scheme of the present invention is: a kind of method measuring sodium oxide content in silicasol, is characterized in that, the step of mensuration is as follows:

1, sample is diluted: taking 1g ~ 5g silicasol sample in volume is in 150mL ~ 300mL beaker, and add secondary deionized water, secondary deionized water consumption is 20mL ~ 80mL, becomes silicasol sample dilution after being mixed evenly;

2, silicasol sample dilution constant volume: silicasol sample dilution is transferred in 100mL ~ 200mL volumetric flask, adds secondary deionized water constant volume and shake up, then refund in former beaker and become silicasol sample liquid to be measured;

3, pH value demarcation is carried out to automatical potentiometric titrimeter: use pH combination electrode, adopt phthalate standard buffer solution, phosphate standard buffer solution, borate standard buffer solution to carry out pH value demarcation to automatical potentiometric titrimeter;

4, titration is carried out to silicasol sample liquid to be measured: adopt automatical potentiometric titrimeter, with the silicasol sample liquid to be measured in watery hydrochloric acid standard solution titrating beaker, the substance withdrawl syndrome of watery hydrochloric acid standard solution is 0.05mol/L ~ 0.5mol/L, till the pH=7 of silicasol sample liquid to be measured, the volume of the watery hydrochloric acid standard solution that record titration consumes;

5, the content of sodium oxide molybdena is calculated: the content being calculated sodium oxide molybdena in silicasol by following formula:

${\mathrm{Na}}_{2}0\%=\frac{V*N*0.031}{G}\×100$ ..........................................(1)

In formula:

V: titration consume the volume of watery hydrochloric acid standard solution, Unit/mL;

N: the substance withdrawl syndrome of watery hydrochloric acid standard solution, unit mol/L;

G: silicasol sample mass, unit g.

Advantage of the present invention is: the assay method proposing sodium oxide content in a kind of silicasol of easy judgement titration end-point, reduces error at measurment, improve the repeatability of mensuration.Test proves, adopt the inventive method, the relative standard deviation of the sodium oxide content of mensuration is 1.08%.

Embodiment

Below the present invention is described in further details.Measure a method for sodium oxide content in silicasol, it is characterized in that, the step of mensuration is as follows:

1, sample is diluted: taking 1g ~ 5g silicasol sample in volume is in 150mL ~ 300mL beaker, and add secondary deionized water, secondary deionized water consumption is 20mL ~ 80mL, becomes silicasol sample dilution after being mixed evenly;

2, silicasol sample dilution constant volume: silicasol sample dilution is transferred in 100mL ~ 200mL volumetric flask, adds secondary deionized water constant volume and shake up, then refund in former beaker and become silicasol sample liquid to be measured;

3, pH value demarcation is carried out to automatical potentiometric titrimeter: use pH combination electrode, adopt phthalate standard buffer solution, phosphate standard buffer solution, borate standard buffer solution to carry out pH value demarcation to automatical potentiometric titrimeter;

4, titration is carried out to silicasol sample liquid to be measured: adopt automatical potentiometric titrimeter, with the silicasol sample liquid to be measured in watery hydrochloric acid standard solution titrating beaker, the substance withdrawl syndrome of watery hydrochloric acid standard solution is 0.05mol/L ~ 0.5mol/L, till the pH=7 of silicasol sample liquid to be measured, the volume of the watery hydrochloric acid standard solution that record titration consumes;

5, the content of sodium oxide molybdena is calculated: the content being calculated sodium oxide molybdena in silicasol by following formula:

${\mathrm{Na}}_{2}0\%=\frac{V*N*0.031}{G}\×100$ ...........................................(1)

In formula:

V: titration consume the volume of watery hydrochloric acid standard solution, Unit/mL;

N: the substance withdrawl syndrome of watery hydrochloric acid standard solution, unit mol/L;

G: silicasol sample mass, unit g.

Principle of work of the present invention is: the present invention adopts automatical potentiometric titrimeter to judge titration end-point, and titration end-point can accurately judge, avoids the error at measurment caused due to the collimation error when adopting indicator method.

Embodiment 1, measures the sodium oxide content of 01 batch of silicasol.

1, sample is diluted: taking 3.0997g silicasol sample in volume is in 150mL beaker, and add secondary deionized water, secondary deionized water consumption is 50mL, becomes silicasol sample dilution after being mixed evenly;

2, silicasol sample dilution constant volume: silicasol sample dilution is transferred in 100mL volumetric flask, adds secondary deionized water constant volume and shake up, then refund in former beaker and become silicasol sample liquid to be measured;

3, pH value demarcation is carried out to automatical potentiometric titrimeter: use pH combination electrode, adopt phthalate standard buffer solution, phosphate standard buffer solution, borate standard buffer solution to carry out pH value demarcation to automatical potentiometric titrimeter;

4, titration is carried out to silicasol sample liquid to be measured: adopt automatical potentiometric titrimeter, with the silicasol sample liquid to be measured in watery hydrochloric acid standard solution titrating beaker, the substance withdrawl syndrome of watery hydrochloric acid standard solution is 0.1038mol/L, till the pH=7 of silicasol sample liquid to be measured, the volume 2.930mL of the watery hydrochloric acid standard solution that record titration consumes;

5, the content of sodium oxide molybdena is calculated: the content being calculated sodium oxide molybdena in silicasol by following formula:

${\mathrm{Na}}_{2}0\%=\frac{V*N*0.031}{G}\×100$ ..........................................(1)

In formula:

V: titration consume the volume of watery hydrochloric acid standard solution, Unit/mL;

N: the substance withdrawl syndrome of watery hydrochloric acid standard solution, unit mol/L;

G: silicasol sample mass, unit g.

The sodium oxide content recorded in sample is 0.30%.

Embodiment 2, measures the sodium oxide content of 02 batch of silicasol.

1, sample is diluted: taking 3.0176g silicasol sample in volume is in 150mL beaker, and add secondary deionized water, secondary deionized water consumption is 50mL, becomes silicasol sample dilution after being mixed evenly;

2, silicasol sample dilution constant volume: silicasol sample dilution is transferred in 100mL volumetric flask, adds secondary deionized water constant volume and shake up, then refund in former beaker and become silicasol sample liquid to be measured;

3, pH value demarcation is carried out to automatical potentiometric titrimeter: use pH combination electrode, adopt phthalate standard buffer solution, phosphate standard buffer solution, borate standard buffer solution to carry out pH value demarcation to automatical potentiometric titrimeter;

4, titration is carried out to silicasol sample liquid to be measured: adopt automatical potentiometric titrimeter, with the silicasol sample liquid to be measured in watery hydrochloric acid standard solution titrating beaker, the substance withdrawl syndrome of watery hydrochloric acid standard solution is 0.1038mol/L, till the pH=7 of silicasol sample liquid to be measured, the volume 1.502mL of the watery hydrochloric acid standard solution that record titration consumes;

5, the content of sodium oxide molybdena is calculated: the content being calculated sodium oxide molybdena in silicasol by following formula:

${\mathrm{Na}}_{2}0\%=\frac{V*N*0.031}{G}\×100$ ..........................................(1)

In formula:

V: titration consume the volume of watery hydrochloric acid standard solution, Unit/mL;

N: the substance withdrawl syndrome of watery hydrochloric acid standard solution, unit mol/L;

G: silicasol sample mass, unit g.

The sodium oxide content recorded in sample is 0.16%.

Embodiment 3, measures the sodium oxide content of 03 batch of silicasol.

1, sample is diluted: taking 3.0119g silicasol sample in volume is in 150mL beaker, and add secondary deionized water, secondary deionized water consumption is 50mL, becomes silicasol sample dilution after being mixed evenly;

2, silicasol sample dilution constant volume: silicasol sample dilution is transferred in 100mL volumetric flask, adds secondary deionized water constant volume and shake up, then refund in former beaker and become silicasol sample liquid to be measured;

3, pH value demarcation is carried out to automatical potentiometric titrimeter: use pH combination electrode, adopt phthalate standard buffer solution, phosphate standard buffer solution, borate standard buffer solution to carry out pH value demarcation to automatical potentiometric titrimeter;

4, titration is carried out to silicasol sample liquid to be measured: adopt automatical potentiometric titrimeter, with the silicasol sample liquid to be measured in watery hydrochloric acid standard solution titrating beaker, the substance withdrawl syndrome of watery hydrochloric acid standard solution is 0.1038mol/L, till the pH=7 of silicasol sample liquid to be measured, the volume 4.127mL of the watery hydrochloric acid standard solution that record titration consumes;

5, the content of sodium oxide molybdena is calculated: the content being calculated sodium oxide molybdena in silicasol by following formula:

${\mathrm{Na}}_{2}0\%=\frac{V*N*0.031}{G}\×100$ ..........................................(1)

In formula:

V: titration consume the volume of watery hydrochloric acid standard solution, Unit/mL;

N: the substance withdrawl syndrome of watery hydrochloric acid standard solution, unit mol/L;

G: silicasol sample mass, unit g.

The sodium oxide content recorded in sample is 0.44%.

Claims (1)

1. measure a method for sodium oxide content in silicasol, it is characterized in that, the step of mensuration is as follows:

1.1, sample is diluted: taking 1g ~ 5g silicasol sample in volume is in 150mL ~ 300mL beaker, and add secondary deionized water, secondary deionized water consumption is 20mL ~ 80mL, becomes silicasol sample dilution after being mixed evenly;

1.2, silicasol sample dilution constant volume: silicasol sample dilution is transferred in 100mL ~ 200mL volumetric flask, adds secondary deionized water constant volume and shake up, then refund in former beaker and become silicasol sample liquid to be measured;

1.3, pH value demarcation is carried out to automatical potentiometric titrimeter: use pH combination electrode, adopt phthalate standard buffer solution, phosphate standard buffer solution, borate standard buffer solution to carry out pH value demarcation to automatical potentiometric titrimeter;

1.4, titration is carried out to silicasol sample liquid to be measured: adopt automatical potentiometric titrimeter, with the silicasol sample liquid to be measured in watery hydrochloric acid standard solution titrating beaker, the substance withdrawl syndrome of watery hydrochloric acid standard solution is 0.05mol/L ~ 0.5mol/L, till the pH=7 of silicasol sample liquid to be measured, the volume of the watery hydrochloric acid standard solution that record titration consumes;

1.5, the content of sodium oxide molybdena is calculated: the content being calculated sodium oxide molybdena in silicasol by following formula:

${\mathrm{Na}}_{2}0\%=\frac{V*N*0.031}{G}\×100$ ..........................................(1)

In formula:

V: titration consume the volume of watery hydrochloric acid standard solution, Unit/mL;

N: the substance withdrawl syndrome of watery hydrochloric acid standard solution, unit mol/L;

G: silicasol sample mass, unit g.