WO2004031751A1 - Procede pour etalonner le zero d'un appareil determinant la quantite de silice selon une methode colorimetrique - Google Patents
Procede pour etalonner le zero d'un appareil determinant la quantite de silice selon une methode colorimetrique Download PDFInfo
- Publication number
- WO2004031751A1 WO2004031751A1 PCT/FR2003/002917 FR0302917W WO2004031751A1 WO 2004031751 A1 WO2004031751 A1 WO 2004031751A1 FR 0302917 W FR0302917 W FR 0302917W WO 2004031751 A1 WO2004031751 A1 WO 2004031751A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- silica
- solution
- measurement
- sample
- concentration
- Prior art date
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/10—Composition for standardization, calibration, simulation, stabilization, preparation or preservation; processes of use in preparation for chemical testing
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/10—Composition for standardization, calibration, simulation, stabilization, preparation or preservation; processes of use in preparation for chemical testing
- Y10T436/109163—Inorganic standards or controls
Definitions
- the present invention relates to a method for calibrating the zero of an apparatus which determines the quantity of silica according to a colorimetric method.
- silica present in water can precipitate during the expansion of water vapor on the turbine of a power plant or in certain phases of the processing of discs or "Wafers" during the manufacture of semiconductors .
- silica in demineralized water can also serve as an indicator of the end of operation of the deionization resins.
- This presence of silica invariably precedes the release of monovalent ions such as in particular sodium ions, chloride.
- - 1 is the measurement of the quantity of light received through the solution;
- - 1 0 is the quantity of light emitted in the solution;
- - L is the length of the optical path crossed by the light
- Beer-Lambert's law expresses a correlation between concentration and a measure of absorption of a quantity of light. In other words, it expresses the fact that the concentration is related to a measure of absorption of quantity of light by a linear law.
- C C 0 + K.log (1 0/1) (2 )
- - C 0 is called zero of the measurement
- - K is the slope of the measurement
- I 0 is the measurement of the quantity of light as a function of the solution present in the cell
- - 1- is the known concentration of the calibration solution 1;
- - 1 2 is the known concentration of the calibration solution 2;
- the residual silica in the dilution water can be measured by mass spectrometry (ICP-MS: Inductively Coupled Plasma-Mass Spectrometry): this method is difficult to implement and does not seem economically usable in measurement industrial online.
- ICP-MS Inductively Coupled Plasma-Mass Spectrometry
- the slope is determined by measuring a solution of high concentration for which the error on the preparation of this solution and the error on the zero of the measurement will be negligible compared to its concentration.
- two calibration solutions are produced, the most concentrated solution of which is obtained by pre-concentrating the first solution with an N factor of at least 20, by heating and evaporating the latter by controlled microwaves.
- N the pre-concentration factor which is in the ratio of the volumes before and after evaporation.
- NX C 0 + K.log (l 0 / l 2 ) (6) in which the parameters have the same values as in relations (3) and (4).
- This method makes it possible to solve the linear equations (5) and (6) and to deduce therefrom the zero of the apparatus, it being understood that K is known.
- K has the drawback of having an extremely long response time (the pre-concentration process must be slow and controlled) and is also not applicable in an industrial environment and in process control.
- One of the aims of the present invention is therefore to provide a method for calibrating the zero of an apparatus which determines the quantity of silica according to a colorimetric method, making it possible to carry out this calibration within an acceptable time.
- Another object of the invention is to provide such a method which is simple to implement.
- the sample to be analyzed circulates in a rapid loop allowing rapid renewal of the sample.
- the flow rate is adjusted using a needle valve.
- the sample is introduced into the measuring cell using the solenoid valve.
- a molybdate solution is added which reacts with the silica contained in the sample: this gives a silicon-molecular complex.
- the reaction time is relatively long (of the order of 300 s).
- a developer such as oxalic acid, is then added to avoid interference from phosphates and to develop and intensify the color of the silicon-polybdenum complex.
- This silicon-polybdenum complex is finally reduced to a blue molybdenum complex by means of ferrous ions.
- a photometric measurement of light absorption is carried out at the end of the reaction.
- Silica dissolved in solution exists in the form of salicylic acid or various kinds of silicates.
- the acid molybdate reacts with the silica in solution to form a yellow-polyester complex which can be detected by measurement of light absorption to detect a concentration of a few mg / l [ppm: parts per million].
- the yellow compound is transformed into a blue complex which allows a more sensitive detection of the silica concentration at the level of ⁇ g / l [ppb: part per billion].
- a sample of the solution to be analyzed is introduced into oxalic acid (developer), then the molybdate solution and finally the reducing agent.
- the process according to the present invention makes it possible: to compensate for the absorption of light due to the coloring and to the possible turbidity of the reagents,
- a sample present in an overflow tank is introduced into a measuring cell whose volume is approximately 8.5 ml. Then add 250 ⁇ l of a solution of 40 g of 2H20 oxalic acid.
- the measuring cell which is made of a heat conducting material, is kept at a constant temperature of 25 ° C.
- l 0 a first measurement of light absorption in this cell: this measurement, l 0 , is the measurement of intensity of the light emitted in the Beer formula -Lambert mentioned above.
- 250 ⁇ l of a molybdate solution are then introduced, the composition of which for 1 liter is:
- a second light absorption measurement I is carried out one minute after the addition of the reducing agent.
- the zero of the measuring device is determined.
- Zero calibration can be performed using the same process, but with other reagents used to measure silica by colorimetry.
- a mixture of citrates and then a reducing agent such as amino-naphthol sulfonic acid
- the determination of zero according to the present invention will be carried out by introducing into the sample the mixture of citrates, molybdate then the reducer.
Abstract
Description
Claims
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU2003286215A AU2003286215A1 (en) | 2002-10-04 | 2003-10-03 | Method of calibrating the zero point of an apparatus used to determine a quantity of silica using a colorimetric method |
US10/529,754 US7381564B2 (en) | 2002-10-04 | 2003-10-03 | Method of calibrating the zero point of an apparatus used to determine a quantity of silica using a colorimetric method |
EP03776956A EP1546689B1 (fr) | 2002-10-04 | 2003-10-03 | Procede pour etalonner le zero d'un appareil determinant la quantite de silice selon une methode colorimetrique |
CN2003801009056A CN1774625B (zh) | 2002-10-04 | 2003-10-03 | 用于对根据比色法测定二氧化硅量的设备进行零点校准的方法 |
JP2004540894A JP4669286B2 (ja) | 2002-10-04 | 2003-10-03 | 比色定量法によって二酸化珪素の量を測定する装置の目盛りの基点を標準に合致させるための方法 |
HK06107045.4A HK1087177A1 (en) | 2002-10-04 | 2006-06-21 | Method of calibrating the zero point of an apparatus used to determine a quantity of silica using a colorimetric method |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR02/12305 | 2002-10-04 | ||
FR0212305A FR2845477B1 (fr) | 2002-10-04 | 2002-10-04 | Procede pour etalonner le zero d'un appareil determinant la quantite de silice selon une methode colorimetrique |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2004031751A1 true WO2004031751A1 (fr) | 2004-04-15 |
Family
ID=32011386
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/FR2003/002917 WO2004031751A1 (fr) | 2002-10-04 | 2003-10-03 | Procede pour etalonner le zero d'un appareil determinant la quantite de silice selon une methode colorimetrique |
Country Status (8)
Country | Link |
---|---|
US (1) | US7381564B2 (fr) |
EP (1) | EP1546689B1 (fr) |
JP (1) | JP4669286B2 (fr) |
CN (1) | CN1774625B (fr) |
AU (1) | AU2003286215A1 (fr) |
FR (1) | FR2845477B1 (fr) |
HK (1) | HK1087177A1 (fr) |
WO (1) | WO2004031751A1 (fr) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102998271A (zh) * | 2012-12-10 | 2013-03-27 | 天津大学 | 硅片切割废砂浆中二氧化硅、硅和碳化硅的测定方法 |
WO2017021660A1 (fr) * | 2015-08-05 | 2017-02-09 | Deltalys | Procédé et dispositif de quantification du silicium total issu de composes organiques volatils siliciés présents dans un gaz |
Families Citing this family (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101765767B (zh) * | 2007-06-29 | 2013-06-12 | 代表亚利桑那大学的亚利桑那校董会 | 二氧化硅物质的电化学检测 |
US9891162B2 (en) * | 2013-10-03 | 2018-02-13 | Rosemount Analytical Inc. | Photometric measurement cell |
US10788416B2 (en) | 2013-10-03 | 2020-09-29 | Rosemount Inc. | Multiple wavelength light source for colorimetric measurement |
CN105659083B (zh) * | 2014-09-12 | 2018-01-23 | 罗斯蒙特分析公司 | 在线湿法化学分析仪 |
JP6497040B2 (ja) * | 2014-11-21 | 2019-04-10 | 三浦工業株式会社 | シリカ濃度測定装置 |
US9759664B2 (en) | 2015-05-28 | 2017-09-12 | Hamilton Sundstrand Space Systems International, Inc. | Microgravity-compatible analysis |
US9945830B2 (en) | 2016-01-21 | 2018-04-17 | Rosemount Inc. | Standard solution with cleaning reagent for wet chemistry analyzer |
US10677717B2 (en) * | 2016-09-30 | 2020-06-09 | Rosemount Inc. | Colorimetric analyzer with reagent diagnostics |
DE102020129213A1 (de) | 2020-11-05 | 2022-05-05 | Endress+Hauser Conducta Gmbh+Co. Kg | Verfahren zum Kalibrieren eines photometrischen Analysators |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB793792A (en) * | 1955-02-01 | 1958-04-23 | Central Electricity Authority | Improvements in or relating to the determination of impurities in water |
US3015544A (en) * | 1958-05-28 | 1962-01-02 | Milton Roy Co | Method of preparing a chemical blank sample |
US3030192A (en) * | 1958-05-28 | 1962-04-17 | Milton Roy Co | Chemical blank colorimetric analyzer |
JPH04109166A (ja) * | 1990-08-29 | 1992-04-10 | Japan Organo Co Ltd | シリカの定量方法 |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2950396A (en) * | 1960-08-23 | Colorevietric analyzer | ||
US3773423A (en) * | 1972-08-22 | 1973-11-20 | Hach Chemical Co | Automatic analyzer |
US5230863A (en) * | 1987-07-21 | 1993-07-27 | Si Industrial Instruments, Inc. | Method of calibrating an automatic chemical analyzer |
JPH0783833A (ja) * | 1993-09-14 | 1995-03-31 | Dkk Corp | シリカの定量方法 |
US5550053A (en) * | 1995-01-05 | 1996-08-27 | Si Industrial Instruments, Inc. | Method of calibrating an automatic chemical analyzer |
US7416899B2 (en) * | 2002-07-29 | 2008-08-26 | Tohoku Techno Arch Co., Ltd. | Method and apparatus for measuring trace ingredients in water |
-
2002
- 2002-10-04 FR FR0212305A patent/FR2845477B1/fr not_active Expired - Fee Related
-
2003
- 2003-10-03 JP JP2004540894A patent/JP4669286B2/ja not_active Expired - Fee Related
- 2003-10-03 EP EP03776956A patent/EP1546689B1/fr not_active Expired - Lifetime
- 2003-10-03 US US10/529,754 patent/US7381564B2/en not_active Expired - Fee Related
- 2003-10-03 AU AU2003286215A patent/AU2003286215A1/en not_active Abandoned
- 2003-10-03 CN CN2003801009056A patent/CN1774625B/zh not_active Expired - Fee Related
- 2003-10-03 WO PCT/FR2003/002917 patent/WO2004031751A1/fr active Application Filing
-
2006
- 2006-06-21 HK HK06107045.4A patent/HK1087177A1/xx not_active IP Right Cessation
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB793792A (en) * | 1955-02-01 | 1958-04-23 | Central Electricity Authority | Improvements in or relating to the determination of impurities in water |
US3015544A (en) * | 1958-05-28 | 1962-01-02 | Milton Roy Co | Method of preparing a chemical blank sample |
US3030192A (en) * | 1958-05-28 | 1962-04-17 | Milton Roy Co | Chemical blank colorimetric analyzer |
JPH04109166A (ja) * | 1990-08-29 | 1992-04-10 | Japan Organo Co Ltd | シリカの定量方法 |
Non-Patent Citations (1)
Title |
---|
PATENT ABSTRACTS OF JAPAN vol. 016, no. 355 (P - 1394) 30 July 1992 (1992-07-30) * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102998271A (zh) * | 2012-12-10 | 2013-03-27 | 天津大学 | 硅片切割废砂浆中二氧化硅、硅和碳化硅的测定方法 |
WO2017021660A1 (fr) * | 2015-08-05 | 2017-02-09 | Deltalys | Procédé et dispositif de quantification du silicium total issu de composes organiques volatils siliciés présents dans un gaz |
FR3039898A1 (fr) * | 2015-08-05 | 2017-02-10 | Deltalys | Procede de quantification du silicium total issu de composes organiques volatils silicies presents dans un gaz |
Also Published As
Publication number | Publication date |
---|---|
JP2006501459A (ja) | 2006-01-12 |
AU2003286215A1 (en) | 2004-04-23 |
CN1774625B (zh) | 2010-04-28 |
FR2845477B1 (fr) | 2005-02-18 |
US20070037289A1 (en) | 2007-02-15 |
EP1546689B1 (fr) | 2011-11-23 |
JP4669286B2 (ja) | 2011-04-13 |
US7381564B2 (en) | 2008-06-03 |
FR2845477A1 (fr) | 2004-04-09 |
HK1087177A1 (en) | 2006-10-06 |
CN1774625A (zh) | 2006-05-17 |
EP1546689A1 (fr) | 2005-06-29 |
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