CN101403700A - Measuring method for background silicon - Google Patents
Measuring method for background silicon Download PDFInfo
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- CN101403700A CN101403700A CNA2008101156581A CN200810115658A CN101403700A CN 101403700 A CN101403700 A CN 101403700A CN A2008101156581 A CNA2008101156581 A CN A2008101156581A CN 200810115658 A CN200810115658 A CN 200810115658A CN 101403700 A CN101403700 A CN 101403700A
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Abstract
The invention provides a measurement method used for substrate silicon, comprising the steps as follows: zero value is measured; chromophoric solution is obtained by inversely added solution; the silicon concentration of the chromophoric solution at the zero value is 0 and the voltage value is V0; two standard solutions 1 and 2 of different concentration, with the consistency C1 and C2 respectively, are prepared; the standard solution 1 and the standard solution 2 are respectively carried out chromophorically operation and subsequently measured according to a photoelectric colorimetry principle; furthermore, the voltage values V1 and V2 are respectively measured; and according to the calculation, the concentration X of the substrate silicon is obtained. An instrument used for measurement is a photometer; the more the consistency of the SiO2 in the chromophoric solution is, the lower the measured voltage value is. The method can precisely measure the concentration of the substrate silicon in silicon-free water, leads the practical concentration of the standard solution of the SiO2 with known concentration to be precise, and has a more precise result measured on the content of the SiO2 during the concentration analysis of the SiO2; and furthermore, the method has simple operation and high precision.
Description
Technical field
The present invention relates to a kind of measuring method of background silicon.
Background technology
At the foundation Beer-Lambert law, carry out with colorimetric method in the process of micro-silica concentration analysis in the water, usually use laboratory or online analyser (also being tintmeter), the accuracy of analyser is to rely on standard solution that usefulness contains concentration known silicon dioxide to calibrate to guarantee.Therefore, the accuracy of the direct impact analysis instrument of the accuracy of standard solution.
Standard solution is to dilute in no silicon water by the mother liquor that contains high concentration silicon dioxide to obtain.Mother liquor is the preparation of national standard material center, belongs to the national standard material.The no silicon water of supposing preparing standard solution is desirable no silicon water, does not contain silicon dioxide, and so, the standard solution that obtains with this water dilution mother liquor should be thought standard.
But in the operating mode of reality, the no silicon water of not silica containing ideal is non-existent, so-called no silicon water refers to and contains the very water of the silicon dioxide of low concentration, and concentration of silicon dioxide should be lower than 5 μ g/L in the no silicon water of requirement usually, and the silicon dioxide in the no silicon water is commonly referred to background silicon.Because the concentration of mother liquor is known, therefore the ideal concentration by the standard solution of acquisition after diluting also is known, but because the content of background silicon is unknown in the needed no silicon water of preparing standard solution, thereby the concentration of the standard solution of the reality that obtains also is unknown, should be that known ideal standard solution concentration adds background silicon concentration in the unknown no silicon water.
At present, in the test analysis of relevant dioxide-containing silica, adopt the mode that adds other reagent zeroing to reduce the influence of background silicon mostly to test result, but this method all will be carried out in each the measurement, make test process complicated, and introduce novel agent and return to zero and handle the precision that has also influenced test.And, just simplified measuring process and accurate measurement result if recorded the content of background silicon in the no silicon water.To obtain concentration of standard solution accurately for this reason, must do not had the concentration of background silicon in the silicon water accurately, have only the content that obtains background silicon in the no silicon water, could improve the accuracy of the concentration of standard solution.
Specifically be for example: the silicon of supposing to contain in the no silicon water 5 μ g/L, we will prepare the standard solution of 80 μ g/L concentration, the concentration of the actual last standard solution that obtains is the concentration of adding background silicon in the no silicon water under ideal concentration, and promptly the concentration of the actual standard solution that obtains is 80+5=85 (μ g/L).When the content of the silicon of measured standard solution seldom the time, the silicone content in the no silicon water will produce a very large impact test result, so to the measurement of background silicon content in the no silicon water be and important.
Summary of the invention
In view of this, the measuring method that the purpose of this invention is to provide a kind of background silicon, by measuring the content of background silicon in the no silicon water, to improve the accuracy of standard solution, thereby can further improve the accuracy of using standard solution calibration analyte instrument, make the result who in the silica concentration analysis, dioxide-containing silica is recorded more accurate.
For reaching above-mentioned purpose, the measuring method of background silicon provided by the invention includes the following step:
A, carry out the zero point value and measure, that is: get an amount of to be measured no silicon water, mode with dosing is handled, obtain the chromophoric solution of value at described zero point, this, silicon concentration of chromophoric solution of value was 0 at zero point, again with photometer to described zero point value chromophoric solution measure, obtain data: output voltage values is V0;
B, get no silicon water same among the step a, use the standard solution that disposes two kinds of variable concentrations with a kind of mother liquor respectively, promptly mark liquid 1, mark liquid 2;
C, will mark liquid 1 and mark liquid 2 and make color operation respectively and handle, the chromophoric solution concentration that obtains described standard solution is respectively C1, C2, with described photometer the chromophoric solution of described two kinds of standard solution is measured again, and the voltage that obtains is respectively V1, V2;
D, according to the photoelectric colorimetry principle, utilize data and the formula record
The concentration that calculates background silicon in the described no silicon water to be measured is X.
Described chromophoric solution is described no silicon water to be measured or described standard solution timesharing successively to be added three kinds of reagent obtain, and described three kinds of reagent are acid ammonium molybdate solution, oxalic acid, scorbic acid.
Adopt described mode of falling dosing to obtain 1 to 2 minute the time of color operation process need of the chromophoric solution of value at described zero point, the described step of dosing comprises:
A1, get no silicon water to be measured;
A2, add described scorbic acid, shake up;
A3, add described oxalic acid, shake up;
A4, the described acid ammonium molybdate solution of adding shake up;
A5, formation chromophoric solution.
14 to 17 minutes the time of color operation process need of described standard solution, the color operation step of described standard solution comprises:
C1, get standard solution to be measured;
C2, the described acid ammonium molybdate solution of adding shake up and wait 5 to 6 minutes;
C3, add described oxalic acid, shake up and wait 1 to 2 minute;
C4, add described scorbic acid, shake up and wait 8 to 9 minutes;
C5, formation chromophoric solution.
Also comprise before the described step a: make blank step of demarcating, promptly described photometric data are proofreaied and correct.
The described photometer that is used to measure described chromophoric solution comprises light source, colorimetric pool and measurement photoelectric cells; Described light source sends stable monochromatic light, described monochromatic light is partly absorbed by chromophoric solution through described colorimetric pool, described monochromatic light remainder is the transmitted light of colorimetric pool, described transmitted light records magnitude of voltage through described measurement photoelectric cells again, silica concentration is high more in the described chromophoric solution, the transmitted light of described colorimetric pool is weak more, and described magnitude of voltage is low more.
The described magnitude of voltage that records all is through the magnitude of voltage to number conversion.
As can be seen from the above technical solutions, the measuring method of background silicon of the present invention has realized the concentration determination to background silicon, make the concentration that under the lower situation of silica concentration, also can measure background silicon in the no silicon water more accurately, accurately the actual concentrations of standard solution of concentration known silicon dioxide, and then more can calibrate the accuracy of analyser, so that the result that analyser records dioxide-containing silica in the silica concentration analysis is more accurate; And the measuring method of background silicon of the present invention is simple to operate, the degree of accuracy height.
Description of drawings
Fig. 1 is the process flow diagram of the measuring method of background silicon among the present invention;
Fig. 2 is the process flow diagram of the color operation process of the chromophoric solution of the usefulness configuration of falling dosing method value at zero point among the present invention;
Fig. 3 is the process flow diagram of the color operation process of the chromophoric solution of configuration standard solution among the present invention.
Embodiment
Below in conjunction with accompanying drawing the specific embodiment among the present invention is described in further detail.
The surveying instrument that measuring method adopted of background silicon is a photometer among the present invention, its measuring principle is according to the photoelectric colorimetry principle dioxide-containing silica in the water to be measured, the solution that contains silicon dioxide is through after developing the color, promptly be configured to chromophoric solution, the absorbance of its chromophoric solution is directly proportional with concentration of silicon dioxide that test solution contains.
The photometer that is used for measuring chromophoric solution among the present invention comprises light source, colorimetric pool, measurement photoelectric cells; During measurement, light source sends stable monochromatic light, and wherein, part monochromatic light is absorbed by chromophoric solution through colorimetric pool, and the monochromatic light of remainder is the transmitted light of colorimetric pool via the colorimetric pool transmission, and this transmitted light records magnitude of voltage again via measurement photoelectric cells; Concentration of silicon dioxide is high more in the measured solution, and the light that chromophoric solution absorbs is many more, and the transmitted light intensity of colorimetric pool is just weak more, and the output signal of measurement photoelectric cells is low more.The immediate data of the magnitude of voltage that is obtained is that promptly the content of silicon dioxide is high more through the magnitude of voltage to number conversion, and magnitude of voltage is low more.
Consult Fig. 1, the measuring method of background silicon may further comprise the steps among the present invention:
A, carry out the zero point value and measure: get an amount of to be measured no silicon water, handle with falling the mode of dosing, obtain the chromophoric solution of value at zero point, this, silicon concentration of chromophoric solution of value was 0 at zero point, again with photometer to zero point value chromophoric solution measure, obtain data: output voltage values V0=3900.
B, get no silicon water same among the step a, use the standard solution that disposes two kinds of variable concentrations with a kind of mother liquor respectively, promptly mark liquid 1, mark liquid 2;
C, will mark liquid 1 and mark liquid 2 and make color operation respectively and handle, the chromophoric solution concentration that obtains two kinds of standard solution is respectively C1, C2, with photometer the chromophoric solution of two kinds of standard solution is measured again, and the voltage that obtains is respectively V1=3760, V2=3270;
If there is not the concentration of background silicon in the silicon water is X (the unknown);
The standard solution that needs two kinds of variable concentrations of configuration, the ideal concentration of promptly marking liquid 1, mark liquid 2 is C1=10, C2=80.
Owing to actually in the to be measured no silicon water that is adopted contain certain silicone content, so the standard solution of actual two kinds of variable concentrations that obtain, the actual concentrations of promptly marking liquid 1, mark liquid 2 is C1+X, and C2+X, the magnitude of voltage that records through photometer is respectively V1=3760, V2=3270;
D, according to the photoelectric colorimetry principle, the concentration of utilizing the data record and formula (as follows) to calculate background silicon in the no silicon water to be measured is X, that is:
The concentration of background silicon
The detailed process of calculating background silicon concentration X is as follows:
The concentration difference of mark liquid 1 and mark liquid 2 is:
Mark liquid 2-mark liquid 1=(C2+X)-(C1+X)=C2-C 1
The measuring voltage difference of mark liquid 1 and mark liquid 2 is:
V1-V2
Silicon dioxide corresponding voltage value that thus can the unit's of calculating concentration is:
The voltage that promptly can be interpreted as the silicon dioxide correspondence of 1 μ g/L is:
Mark liquid 1 and zero point value the concentration difference of chromophoric solution be:
C1+X-0＝C1+X
Mark liquid 1 and zero point value the measuring voltage difference of chromophoric solution be:
V0-V1
Can calculate the concentration difference between mark liquid 1 and the zero point value thus, the actual concentrations of just marking liquid 1 is:
Thereby the concentration that can draw background silicon is exactly: the mark liquid 1 actual concentrations-mark liquid 1 ideal concentration promptly:
The result of calculation that is obtained by above step is as shown in Table 1:
Table one
| Solution | V | C |
| Value at zero point (dosing) | 3900 (measurements) | 0 (known) |
| Mark 1 | 3760 (measurements) | 10 (known) |
| Mark 2 | 3270 (measurements) | 80 (known) |
| Background silicon | (can calculate) | 10 (calculating) |
Among the present invention in the measuring method of background silicon the configuration of chromophoric solution be according to national standard, sample water timesharing is successively added three kinds of reagent and obtain, sample water among the present invention is the standard solution of no silicon water and two kinds of variable concentrations, three kinds of reagent that adopt are respectively acid ammonium molybdate solution, oxalic acid and scorbic acid, also can adopt other reagent, not as limit.
Consult Fig. 2, when carrying out that zero point, value was measured, obtain the chromophoric solution of value at zero point with falling the mode of dosing, the step of its color operation is:
A1, get no silicon water to be measured;
A2, adding scorbic acid shake up;
A3, adding oxalic acid shake up;
A4, add acid ammonium molybdate solution, shake up;
A5, formation chromophoric solution.
Obtain not have time of 1 to 2 minute of whole process need of the chromophoric solution of silicon water with falling the mode of dosing.Zero point, value was meant the magnitude of voltage after the water that do not contain silicon dioxide is through colour developing in theory, and not siliceous water is non-existent, so zero point, value was by falling the method realization of dosing.Because the mode of dosing is also for be worth correcting mode habitual zero point, only do simple description herein.
Consult Fig. 3, the step of the color operation of the chromophoric solution of configuration standard solution is:
C1, get standard solution to be measured;
C2, the described acid ammonium molybdate solution of adding shake up and wait 5 to 6 minutes;
C3, add described oxalic acid, shake up and wait 1 to 2 minute;
C4, add described scorbic acid, shake up and wait 8 to 9 minutes;
C5, formation chromophoric solution.
14 to 17 minutes the time of whole process need of the chromophoric solution of configuration standard solution.
In addition, (referring to Fig. 1) also comprises the steps A of doing blank demarcation before step a, promptly photometric data proofreaied and correct.Make blank timing signal, the no silicon water that does not add chemical reagent is directly poured into photometric colorimetric pool, promptly obtain output voltage V-1, its silicon content can be according to counter the pushing back of curve that zero point, value and mark liquid 1 were determined, with the data that obtain in measuring process as a reference.
The measuring method of background silicon of the present invention has realized the concentration determination to background silicon, make the concentration that under the lower situation of silica concentration, can measure silicon in the no silicon water more accurately, accurately the actual concentrations of standard solution of concentration known silicon dioxide, and then more can calibrate the accuracy of analyser, so that the result that analyser records dioxide-containing silica in the silica concentration analysis is more accurate; And the measuring method of background silicon of the present invention is simple to operate, the degree of accuracy height.
Claims (7)
1, a kind of measuring method of background silicon is characterized in that, includes the following step:
A, carry out the zero point value and measure, that is: get an amount of to be measured no silicon water, mode with dosing is handled, obtain the chromophoric solution of value at described zero point, this, silicon concentration of chromophoric solution of value was 0 at zero point, again with photometer to described zero point value chromophoric solution measure, obtain data: output voltage values is V0;
B, get no silicon water same among the step a, use the standard solution that disposes two kinds of variable concentrations with a kind of mother liquor respectively, promptly mark liquid 1, mark liquid 2; Concentration is respectively C1, C2.
C, will mark liquid 1 and mark liquid 2 and make color operation respectively and handle, the chromophoric solution that obtains described standard solution is measured the chromophoric solution of described two kinds of standard solution with described photometer again, and the voltage that obtains is respectively V1, V2;
D, according to the photoelectric colorimetry principle, utilize data and the formula record
The concentration that calculates background silicon in the described no silicon water to be measured is X.
2, the measuring method of background silicon as claimed in claim 1, it is characterized in that, described chromophoric solution is described no silicon water to be measured or described standard solution timesharing successively to be added three kinds of reagent obtain, and described three kinds of reagent are acid ammonium molybdate solution, oxalic acid, scorbic acid.
3, the measuring method of background silicon as claimed in claim 2 is characterized in that, adopts described mode of falling dosing to obtain 1 to 2 minute the time of color operation process need of the chromophoric solution of value at described zero point, and the described step of dosing comprises:
A1, get no silicon water to be measured;
A2, add described scorbic acid, shake up;
A3, add described oxalic acid, shake up;
A4, the described acid ammonium molybdate solution of adding shake up;
A5, formation chromophoric solution.
4, the measuring method of background silicon as claimed in claim 2 is characterized in that, 14 to 17 minutes the time of color operation process need of described standard solution, the color operation step of described standard solution comprises:
C1, get standard solution to be measured;
C2, the described acid ammonium molybdate solution of adding shake up and wait 5 to 6 minutes;
C3, add described oxalic acid, shake up and wait 1 to 2 minute;
C4, add described scorbic acid, shake up and wait 8 to 9 minutes;
C5, formation chromophoric solution.
5, the measuring method of background silicon as claimed in claim 1 is characterized in that, also comprises before the described step a: make blank step of demarcating, promptly described photometric data are proofreaied and correct.
6, the measuring method of background silicon as claimed in claim 1 is characterized in that, the described photometer that is used to measure described chromophoric solution comprises light source, colorimetric pool and measurement photoelectric cells; Described light source sends stable monochromatic light, described monochromatic light is partly absorbed by chromophoric solution through described colorimetric pool, described monochromatic light remainder is the transmitted light of colorimetric pool, described transmitted light records magnitude of voltage through described measurement photoelectric cells again, silica concentration is high more in the described chromophoric solution, the transmitted light of described colorimetric pool is weak more, and described magnitude of voltage is low more.
As the measuring method of claim 1 or 6 described background silicons, it is characterized in that 7, the described magnitude of voltage that records all is through the magnitude of voltage to number conversion.
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| CN114441460A (en) * | 2020-11-05 | 2022-05-06 | 恩德莱斯和豪瑟尔分析仪表两合公司 | Method for calibrating photometric analyzer |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114441460A (en) * | 2020-11-05 | 2022-05-06 | 恩德莱斯和豪瑟尔分析仪表两合公司 | Method for calibrating photometric analyzer |
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