CN109580605A - The measuring method of sodium chlorate in sodium hydroxide solution - Google Patents
The measuring method of sodium chlorate in sodium hydroxide solution Download PDFInfo
- Publication number
- CN109580605A CN109580605A CN201811475924.1A CN201811475924A CN109580605A CN 109580605 A CN109580605 A CN 109580605A CN 201811475924 A CN201811475924 A CN 201811475924A CN 109580605 A CN109580605 A CN 109580605A
- Authority
- CN
- China
- Prior art keywords
- sodium hydroxide
- hydroxide solution
- sodium
- added
- measuring method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
-
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Pathology (AREA)
- General Health & Medical Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Immunology (AREA)
- General Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention relates to the measuring methods of sodium chlorate in sodium hydroxide solution, belong to chemical analysis field.To be solved by this invention is the problems such as existing measuring method can not draw qualified standard curve, measurement result accuracy is low, there is provided the measuring methods of sodium chlorate in sodium hydroxide solution for its technical solution, include the following steps: a, take sodium hydroxide solution sample, color developing agent ortho-tolidine is added；B, in 0~10 DEG C of dropwise addition hydrochloric acid to pH=6~8, it is then quickly added into hydrochloric acid hydrogen ion concentration >=6mol/l into solution, the fast added-time maintains the temperature at 20 DEG C hereinafter, shaking up, and standing colour developing measures absorbance；C, the content of sodium chlorate in sodium hydroxide solution sample is calculated according to absorbance measurement result.Measuring method provided by the invention can preferably draw standard curve, and measurement result is stablized, and accuracy is higher.
Description
Technical field
The present invention relates to the measuring methods of sodium chlorate in sodium hydroxide solution, belong to chemical analysis field.
Background technique
Sodium hydroxide, also known as caustic soda, mainly for the production of paper, soap, dyestuff, artificial silk, metal smelting, petroleum refinement,
Cotton goods arrange, the purification of coal tar oil product and food processing, timber processing and mechanical industry etc..Country's hydrogen at present
Sodium oxide molybdena production mainly uses ion film production technique, and wherein the content of ion film caustic soda Chlorine in Solution acid sodium is to measure ionic membrane
One important indicator of performance, accurate detection are of great significance.
The measurement of sodium chlorate uses GB/T11200.1-89 and GB/T11200.1-2006 two in soda bath at present
Kind National Standard Method of Determination, mode of operation are first to be added at one time enough hydrochloric acid (not control temperature during being added dropwise
System), ortho-tolidine indicator solution is then added, sufficiently absorbance is measured after colour developing, so that the content of sodium chlorate be calculated.
However, often occurring related coefficient when drawing standard curve using above two method and there was only the case where 0.6-0.9 (standard song
The basic demand of line is that related coefficient must reach 0.995 or more), standard curve is unqualified, causes accurately calculate at all
The content of sodium chlorate；Moreover, there is also the problem of same sample measurement result variation greatly, inaccurate.
Summary of the invention
The purpose of the present invention is to provide the measuring methods of sodium chlorate in sodium hydroxide solution, to solve existing measurement
The problems such as method can not draw qualified standard curve, measurement result accuracy is low.
The present invention provides the measuring methods of sodium chlorate in sodium hydroxide solution, include the following steps:
A, sodium hydroxide solution sample is taken, color developing agent ortho-tolidine is added；
B, in 0~10 DEG C of dropwise addition hydrochloric acid to pH=6~8, be then quickly added into hydrochloric acid into solution hydrogen ion concentration >=
6mol/l, fast added-time maintain the temperature at 20 DEG C hereinafter, shaking up, and standing colour developing measures absorbance；
C, the content of sodium chlorate in sodium hydroxide solution sample is calculated according to absorbance measurement result.
Preferably, step a is in 0~10 DEG C of dropwise addition hydrochloric acid to pH=7.
Further, step b stands 4~7min colour developing.
Preferably, step b stands 5min colour developing.
Further, step b measures absorbance at wavelength 442nm.
Further, step c presses formulaThe concentration of sodium chlorate in sodium hydroxide solution sample is calculated；Wherein, m is
According to absorbance measurement result from after the deduction blank checked on standard curve in sample the quality of sodium chlorate numerical value, the mark
For directrix curve using sodium chlorate quality contained by 100ml cuvette solution as abscissa, corresponding absorbance is ordinate；V is
The volume of taken sodium hydroxide solution sample.
Further, the standard curve is drawn to obtain by following methods: being by the concentration isometric with measurement sample
The sodium hydroxide solution of 400g/l is respectively placed in 7 100ml volumetric flasks, sequentially adds the chloric acid that concentration is 0.01mg/ml
Sodium standard solution 0.0,1.0,2.0,3.0,4.0,5.0,6.0ml, then sequentially add 10.0,9.0,8.0,7.0,6.0,5.0,
4.0ml water, then each 2.0ml concentration that is added is the ortho-tolidine color developing agent of 1g/l；Hydrochloric acid, side is added dropwise in 0~10 DEG C of water-bath
Edged oscillation, after pH reaches 6~8, then rapidly join 25ml hydrochloric acid, while keeping quick oscillation, control temperature at 20 DEG C hereinafter,
It is quickly shaken up after volumetric flask is removed from water-bath, stands 4~7min colour developing, be then diluted with water to scale, shake up, then is quiet
It sets, suitable cuvette is selected in 10min, measure absorbance, at wavelength 442nm with chlorine contained by 100ml cuvette solution
Sour sodium quality is abscissa, and unit is μ g, and corresponding absorbance is ordinate, draws standard curve.
Further, the measuring method includes the following steps: to take sodium hydroxide solution sample in 100ml volumetric flask
In, 10ml water is added, the ortho-tolidine color developing agent that 2.0ml concentration is 1g/l is added；Hydrochloric acid is added dropwise in 0~10 DEG C of water-bath,
Side edged oscillation, after pH reaches 6~8, then rapidly join 25ml hydrochloric acid, while keeping quick oscillation, control temperature 20 DEG C with
Under, it is quickly shaken up after volumetric flask is removed from water-bath, stands 4~7min colour developing, be then diluted with water to scale, shake up, then
It stands, suitable cuvette is selected in 10min, absorbance is measured at wavelength 442nm；By formulaSodium hydroxide is calculated
The volumetric concentration mg/l of sodium chlorate in solution example, wherein m is from chloric acid in sample after the deduction blank checked on standard curve
The numerical value of the quality of sodium, unit are μ g, volume of the V for taken sodium hydroxide solution sample, unit ml.
Further, the amount of taking of the sodium hydroxide solution sample is 1~5ml.
Further, the sodium hydroxide solution is sodium hydrate aqueous solution.
The present invention provides the measuring methods of sodium chlorate in sodium hydroxide solution.The experimental results showed that using this hair
The measuring method of bright offer can draw out related coefficient in 0.995 or more standard curve, and the measurement knot of sodium chlorate
Fruit is stable, accurate, has good popularization and application foreground.
Specific embodiment
Raw material, equipment used in the specific embodiment of the invention are known product, are obtained by purchase commercial product.
The present invention provides the measuring methods of sodium chlorate in sodium hydroxide solution, include the following steps: a, take hydrogen-oxygen
Change sodium solution sample, color developing agent ortho-tolidine is added；B, it is then quickly added into 0~10 DEG C of dropwise addition hydrochloric acid to pH=6~8
Hydrochloric acid hydrogen ion concentration >=6mol/l into solution, fast added-time maintain the temperature at 20 DEG C hereinafter, shaking up, and standing colour developing, measurement is inhaled
Luminosity；C, the content of sodium chlorate in sodium hydroxide solution sample is calculated according to absorbance measurement result.
Creatively using color developing agent ortho-tolidine is first added, segmentation is added hydrochloric acid and controls reaction acidity the present invention,
And the methods of the reaction temperature of hydrochloric acid is added in control, reduces the volatilization of product and decomposes loss, so that colour developing is more filled
Point, to well solve the problems such as existing measuring method can not draw qualified standard curve, measurement result accuracy is low.
Embodiment 1 is using sodium chlorate in the method for the present invention measurement sodium hydroxide solution
1, the drafting of standard curve: taking 5ml reagent sodium hydroxide (400g/l) to be respectively placed in 7 100ml volumetric flasks, then
Chloric acid sodium standard solution (0.01mg/ml) 0.0,1.0,2.0,3.0,4.0,5.0,6.0ml are sequentially added, is then sequentially added
10.0,9.0,8.0,7.0,6.0,5.0,4.0ml water, then each addition 2.0ml ortho-tolidine developing solution (1g/l)；In 0-10
Hydrochloric acid (analysis is pure) is added dropwise with measuring pipette in DEG C water-bath, edged oscillation in side after pH reaches 7, then rapidly joins 25ml hydrochloric acid extremely
Hydrogen ion degree >=6mol/l, meanwhile, it keeps quick oscillation (temperature does not exceed 20 DEG C), it is fast after volumetric flask is removed from water-bath
Speed shakes up, and stands 5min colour developing, is then diluted with water to scale, shakes up, then stand, suitable cuvette is selected in 10min,
At wavelength 442nm, absorbance is measured, it is corresponding with sodium chlorate quality (μ g) contained by 100ml cuvette solution for abscissa
Absorbance be ordinate, draw standard curve, the related coefficient of standard curve is 0.995 or more；
2, it takes 5ml sample in 100ml volumetric flask, 10ml water is added, 2.0ml ortho-tolidine developing solution (1g/ is added
l)；Hydrochloric acid (analysis is pure) is added dropwise with measuring pipette in 0-10 DEG C of water-bath, edged oscillation in side after pH reaches 7, then rapidly joins
25ml hydrochloric acid to hydrogen ion degree >=6mol/l, meanwhile, keep quick oscillation (temperature does not exceed 20 DEG C), by volumetric flask from water-bath
It is quickly shaken up after middle removal, stands 5min colour developing, be then diluted with water to scale, shake up, then stand, it is suitable to select in 10min
Cuvette, at wavelength 442nm, measure absorbance；
3, formula is pressedThe volumetric concentration (mg/l) of sodium chlorate in sample to be tested is calculated；Wherein, m is from standard song
After the deduction blank checked on line in sample the quality of sodium chlorate numerical value, unit is microgram；V is samples taken volume, unit
For milliliter.
Practical measurement result is as follows:
| Sample ID | Scalar quantity (mg/l) | Measurement result (mg/l) | Recovery of standard addition % |
| Sodium hydroxide solution | — | 12.27 | — |
| Ibid sample mark-on | 5 | 17.19 | 98.4 |
As it can be seen that using measuring method of the present invention, qualified standard curve can not only be drawn out, and measurement result is stablized,
Accuracy is higher.
Claims (8)
1. the measuring method of sodium chlorate in sodium hydroxide solution, it is characterized in that: including the following steps:
A, sodium hydroxide solution sample is taken, color developing agent ortho-tolidine is added；
B, in 0~10 DEG C of dropwise addition hydrochloric acid to pH=6~8, it is then quickly added into hydrochloric acid hydrogen ion concentration >=6mol/l into solution,
The fast added-time maintains the temperature at 20 DEG C hereinafter, shaking up, and standing colour developing measures absorbance；Preferably, extremely in 0~10 DEG C of dropwise addition hydrochloric acid
PH=7；
C, the content of sodium chlorate in sodium hydroxide solution sample is calculated according to absorbance measurement result.
2. measuring method as described in claim 1, it is characterized in that: step b stands 4~7min colour developing；Preferably, step b is quiet
Set 5min colour developing.
3. measuring method as described in claim 1, it is characterized in that: step b measures absorbance at wavelength 442nm.
4. measuring method as described in claim 1, it is characterized in that: step c presses formulaSodium hydroxide solution sample is calculated
The concentration of sodium chlorate in product；Wherein, m is according to absorbance measurement result from after the deduction blank checked on standard curve in sample
The numerical value of the quality of sodium chlorate, the standard curve is using sodium chlorate quality contained by 100ml cuvette solution as abscissa, with it
Corresponding absorbance is ordinate；V for taken sodium hydroxide solution sample volume.
5. measuring method as claimed in claim 4, it is characterized in that: the standard curve is drawn to obtain by following methods: will be with
The sodium hydroxide solution that the isometric concentration of measurement sample is 400g/l is respectively placed in 7 100ml volumetric flasks, is sequentially added
Concentration is the chloric acid sodium standard solution 0.0 of 0.01mg/ml, 1.0,2.0,3.0,4.0,5.0,6.0ml, is then sequentially added
10.0,9.0,8.0,7.0,6.0,5.0,4.0ml water, then each 2.0ml concentration that is added is the ortho-tolidine color developing agent of 1g/l；
Hydrochloric acid is added dropwise in 0~10 DEG C of water-bath, edged oscillation in side after pH reaches 6~8, then rapidly joins 25ml hydrochloric acid to hydrogen ion degree
>=6mol/l, while keeping quick oscillation, controls temperature at 20 DEG C hereinafter, quickly shaking up after volumetric flask is removed from water-bath,
4~7min colour developing is stood, scale is then diluted with water to, shakes up, then stand, suitable cuvette is selected in 10min, in wavelength
Absorbance is measured at 442nm, using sodium chlorate quality contained by 100ml cuvette solution as abscissa, unit is μ g, corresponding
Absorbance be ordinate, draw standard curve.
6. measuring method as claimed in any one of claims 1 to 5, wherein, it is characterized in that: including the following steps: to take sodium hydroxide molten
10ml water is added in 100ml volumetric flask in liquid sample, and the ortho-tolidine color developing agent that 2.0ml concentration is 1g/l is added；0~
Be added dropwise hydrochloric acid in 10 DEG C of water-baths, the oscillation of side edged, after pH reaches 6~8, then rapidly join 25ml hydrochloric acid to hydrogen ion degree >=
6mol/l, while keeping quick oscillation, controls temperature at 20 DEG C hereinafter, quickly shaking up after volumetric flask is removed from water-bath, quiet
4~7min colour developing is set, scale is then diluted with water to, shakes up, then stand, suitable cuvette is selected in 10min, in wavelength
Absorbance is measured at 442nm；By formulaThe volumetric concentration mg/l of sodium chlorate in sodium hydroxide solution sample is calculated,
In, m be from after the deductions blank checked on standard curve in sample the quality of sodium chlorate numerical value, unit be μ g, V is is taken hydrogen
The volume of sodium hydroxide solution sample, unit ml.
7. measuring method as claimed in claim 6, it is characterized in that: the amount of taking of the sodium hydroxide solution sample be 1~
5ml。
8. the measuring method as described in claim 1~7 any one, it is characterized in that: the sodium hydroxide solution is hydroxide
Sodium water solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811475924.1A CN109580605B (en) | 2018-12-04 | 2018-12-04 | Method for measuring sodium chlorate content in sodium hydroxide solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811475924.1A CN109580605B (en) | 2018-12-04 | 2018-12-04 | Method for measuring sodium chlorate content in sodium hydroxide solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109580605A true CN109580605A (en) | 2019-04-05 |
| CN109580605B CN109580605B (en) | 2021-08-13 |
Family
ID=65927531
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811475924.1A Active CN109580605B (en) | 2018-12-04 | 2018-12-04 | Method for measuring sodium chlorate content in sodium hydroxide solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109580605B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110794084A (en) * | 2019-11-19 | 2020-02-14 | 攀枝花钢企欣宇化工有限公司 | Method for measuring calcium chlorate content |
| CN113340834A (en) * | 2021-06-11 | 2021-09-03 | 成都市排水有限责任公司 | Method for rapidly determining content of sodium acetate in industrial-grade sodium acetate solution |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007071377A1 (en) * | 2005-12-20 | 2007-06-28 | Medisynthana Diagnostics Gmbh & Co. Kg | Conversion reagent and method and kit for determining haemoglobin |
| CN103383356A (en) * | 2012-05-02 | 2013-11-06 | 深圳市清时捷科技有限公司 | Method for rapidly determining chlorates in drinking water |
| CN104165888A (en) * | 2014-08-13 | 2014-11-26 | 国家电网公司 | Method for determining content of sodium chlorate in industrial alkali liquor |
| CN106370610A (en) * | 2016-08-31 | 2017-02-01 | 四川北方红光特种化工有限公司 | Method of detecting content of trace phenol in nitro-o-xylene |
-
2018
- 2018-12-04 CN CN201811475924.1A patent/CN109580605B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007071377A1 (en) * | 2005-12-20 | 2007-06-28 | Medisynthana Diagnostics Gmbh & Co. Kg | Conversion reagent and method and kit for determining haemoglobin |
| CN103383356A (en) * | 2012-05-02 | 2013-11-06 | 深圳市清时捷科技有限公司 | Method for rapidly determining chlorates in drinking water |
| CN104165888A (en) * | 2014-08-13 | 2014-11-26 | 国家电网公司 | Method for determining content of sodium chlorate in industrial alkali liquor |
| CN106370610A (en) * | 2016-08-31 | 2017-02-01 | 四川北方红光特种化工有限公司 | Method of detecting content of trace phenol in nitro-o-xylene |
Non-Patent Citations (4)
| Title |
|---|
| 中国国家标准化管理委员会: "《中华人民共和国国家标准》", 14 September 2006, 中国国家标准化管理委员会 * |
| 漆贯荣等: "《理科最新常用数据手册 天文·物理·化学·气象·地理·地质·地震》", 30 November 1983, 陕西人民出版社 * |
| 罗莲英等: "邻-联甲苯胺分光光度法测定氢氧化钠中的氯酸钠", 《氯碱工业》 * |
| 苗凤芹: "邻联甲苯胺比色法测定电解液中氯酸盐", 《氯碱工业》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110794084A (en) * | 2019-11-19 | 2020-02-14 | 攀枝花钢企欣宇化工有限公司 | Method for measuring calcium chlorate content |
| CN113340834A (en) * | 2021-06-11 | 2021-09-03 | 成都市排水有限责任公司 | Method for rapidly determining content of sodium acetate in industrial-grade sodium acetate solution |
| CN113340834B (en) * | 2021-06-11 | 2023-05-16 | 成都市排水有限责任公司 | Method for rapidly determining sodium acetate content in industrial sodium acetate solution |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109580605B (en) | 2021-08-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103323412B (en) | Thiocyanate spectrophotometry method for detecting iron content of high-temperature alloy | |
| CN106290334B (en) | The chemistry in detecting of cobalt and manganese content in cobalt manganese raw material | |
| CN109580605A (en) | The measuring method of sodium chlorate in sodium hydroxide solution | |
| CN106324185B (en) | A kind of assay method of Emulsion of UPR acid value | |
| CN103424443A (en) | Ion-selective electrode method for measuring fluoride content in grains, vegetables and fruits | |
| CN106018672A (en) | Method for determining chlorine ion content in coke | |
| CN104111305B (en) | A kind of potassium bichromate titrimetric method is measured the new method of full iron in iron ore | |
| CN102901765B (en) | Potentiometric titration method for measuring content of Hg<2+> in solution | |
| CN101592644B (en) | Method for detecting barium ions in oil field water | |
| CN103063801A (en) | Rapid online analysis method for main component in alkaline galvanization electroplate liquid | |
| CN109254111A (en) | A kind of detection method and preparation method thereof of Water soluble fertilizer nitrate nitrogen content | |
| CN104886756A (en) | Method for detecting padding calcium carbonate content in paper-making process sheet tobacco basic sheet | |
| CN104280368A (en) | Method for efficiently and accurately detecting main content of industrial magnesium oxide | |
| CN103336004B (en) | A kind of analysis method of sodium carbonate and sodium sulfite | |
| CN113418970A (en) | Method for measuring fluorine in magnesium refractory material | |
| CN102706868A (en) | Quick salt iodine quantitative detection equipment | |
| CN113237994A (en) | Method for rapidly analyzing and detecting impurity sodium sulfide in barium sulfide solution | |
| CN105954262A (en) | {0><}0{>ICP-AES method for measuring sulfur content of lead sulfate in waste storage battery | |
| Tan et al. | Simultaneous and automatic determination of hydroxide and carbonate in aluminate solutions by a micro-titration method | |
| CN108181427A (en) | Calcium ions and magnesium ions assay method in high ph-values water quality | |
| CN111239331A (en) | Method for detecting content of calcium oxide in quick lime | |
| CN107656008A (en) | The assay method of calcium oxide content in a kind of calcium stearate | |
| CN109839474A (en) | The measuring method of fluorine content in a kind of fluorine-containing liquid during tantalum and niobium hydrometallurgy | |
| CN105223200A (en) | A kind of method of content of hydrochloric acid in Accurate Determining iron chloride etchant solution | |
| CN110231435A (en) | A kind of method of chloride content determination in aluminium wastewater |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |