CN109211718B - K in potassium dichromate production2Method for measuring O content - Google Patents
K in potassium dichromate production2Method for measuring O content Download PDFInfo
- Publication number
- CN109211718B CN109211718B CN201811258910.4A CN201811258910A CN109211718B CN 109211718 B CN109211718 B CN 109211718B CN 201811258910 A CN201811258910 A CN 201811258910A CN 109211718 B CN109211718 B CN 109211718B
- Authority
- CN
- China
- Prior art keywords
- precipitate
- solution
- potassium
- washing
- tetraphenylborate
- 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.)
- Active
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/42—Low-temperature sample treatment, e.g. cryofixation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- 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
- G01N31/02—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using precipitation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
- G01N2001/386—Other diluting or mixing processes
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Biomedical Technology (AREA)
- Engineering & Computer Science (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses K in potassium dichromate production2Taking potassium dichromate reaction solution V to be measured, adding a reducing agent under an acidic condition to completely reduce hexavalent chromium into trivalent chromium, adding alkali to neutralize the solution until the solution is neutral, preserving the temperature for 1-2h at 90-100 ℃, filtering and washing until no K exists+Collecting the washing liquid; precipitation of potassium tetraphenylborate: heating the obtained washing liquid to boiling, dropwise adding a sodium tetraphenylborate solution under the stirring condition until potassium tetraphenylborate precipitate is generated, and cooling and standing; transferring the cooling liquid obtained in the step 2 to G which is baked to constant weight at 120 DEG C4Carrying out suction filtration in a glass sand core funnel, washing the obtained precipitate by using tetraphenyl boron potassium washing liquid, and finally placing the precipitate in a drying oven to dry to constant weight W; k2The O content was calculated as 0.1314 × W × 1000/V.
Description
Technical Field
The invention belongs to the technical field of chemical engineering, and particularly relates to K in potassium dichromate production2And (4) a method for measuring the content of O.
Background
In the industrial production of potassium dichromate, in order to ensure that KCl is utilized 100%, the addition amount of KCI is 98% of the theoretical amount, and Na2Cr2O7A slight excess. After a period of time of production according to the proportion, the 'deficiency' K appears in the system+Phenomena or K caused by metering+/Cr6+The ratio is out of balance, thereby affecting production. Therefore, the K in the production system is periodically paired2Cr2O7、K2The content of O is measured to guide the production.
In the system K2Cr2O7The content determination is performed by using ferrous ammonium sulfate for redox determination, and is a more classical method, which is not described herein again.
And K2The principle of the determination of the O content is K+Reacting with sodium tetraphenylboron solution to generate potassium tetraphenylboron, washing, drying, weighing, and calculating to obtain K2The content of O. The traditional method is that after hexavalent chromium is reduced and neutralized to remove hexavalent chromium, 10 percent acetic acid is added to adjust the solution to be weakly acidic, 0.1mol/L sodium tetraphenylboron ethanol solution is added for precipitation, after the precipitation is transferred and washed by potassium tetraphenylboron saturated solution, the solution is dried to constant weight at 120 ℃, K is calculated according to a formula2The content of O.
However, in the actual testing process, the condition of the potassium tetraphenylborate precipitate is difficult to control, and when the potassium tetraphenylborate precipitate is measured in parallel, the amount of the generated potassium tetraphenylborate precipitate is different, so that the analysis result has a large error. In order to improve the precision and accuracy of the inspection and better serve the production, it is imperative to develop more reasonable inspection methods.
Disclosure of Invention
The invention aims to make more reasonable K2The method for measuring the content of O improves the precision and the accuracy of the detection and better serves the production.
In order to achieve the purpose, the technical scheme is as follows:
k in potassium dichromate production2The method for measuring the content of O comprises the following steps:
1) removing chromium: taking potassium dichromate reaction liquid V to be detected, adding a reducing agent under an acidic condition to completely reduce hexavalent chromium into trivalent chromium, adding alkali to neutralize the solution until the solution is neutral, preserving heat for 1-2h at the temperature of 90-100 ℃, filtering and washing until no K exists+Collecting the washing liquid;
2) precipitation of potassium tetraphenylborate: heating the obtained washing liquid to boiling, dropwise adding a sodium tetraphenylborate solution under the stirring condition until potassium tetraphenylborate precipitate is generated, and cooling and standing;
3) and (3) precipitation transfer: transferring the cooling liquid obtained in the step 2 to G which is baked to constant weight at 120 DEG C4Carrying out suction filtration in a glass sand core funnel, washing the obtained precipitate by using tetraphenyl boron potassium washing liquid, and finally placing the precipitate in a drying oven to dry to constant weight W;
4)K2the O content is calculated as follows:
A＝0.1314×W×1000/V；
wherein, A: k2O content, g/L; w: dry weight of the precipitate obtained in step 3, g; v: the potassium dichromate reaction solution, L, to be tested.
In the above scheme, step 1 uses a diphenylcarbodihydrazide indicator for checking to determine that the hexavalent chromium is completely reduced into trivalent chromium.
According to the scheme, the sodium tetraphenylborate solution is mixed with a small amount of washing liquid tail liquid in the step 1, no white precipitate is generated, and no K is generated in the precipitate obtained by filtering+。
Compared with the prior art, the invention has the following beneficial effects:
the pretreatment adopts the traditional method, and the potassium chloride method is adopted for determination after the treatment, which proves that the method is feasible, the operation method is simpler than the traditional method, the result reproducibility is good, the accuracy is high, the method is basically consistent with the theoretical result, and the method is the heavy chromiumPotassium system Cr6 +/K+The balance provides the basis.
Detailed Description
The following examples further illustrate the technical solutions of the present invention, but should not be construed as limiting the scope of the present invention.
Example 1
50g (to 0.0001g) of standard potassium dichromate was weighed in a 250ml beaker, and dissolved by heating on an electric furnace with an appropriate amount of water. Cooling, transferring into a 250ml volumetric flask, adding water to dilute to the scale, shaking up, at which time K2The O content was about 63.9 g/L.
25.00ml of the mixture is respectively put into 4 250ml beakers of A, B, C and D. Adding 10ml hydrochloric acid (1+1) and appropriate amount of ethanol and water, respectively, placing in 100 deg.C water bath, and maintaining for 1-2 hr until Cr is6+After complete reduction (detected by diphenyl carbonyl dihydrazide indicator), adding liquid alkali to adjust the solution to be neutral, preserving the temperature for 1 hour in boiling water bath, filtering by slow quantitative filter paper, washing by hot water until no K exists+Until then (checked with sodium tetraphenylborate solution), the filtrate was collected in a 250ml beaker.
The first sample and the second sample are carried out according to a traditional method: adding 1 drop of methyl orange indicator into each of the two samples, adjusting the mixture to be just red by using 10% acetic acid solution, and heating the mixture to 60 ℃ for taking down. Adding 10ml sodium tetraphenylborate solution dropwise under stirring, stirring for 1 min, standing for 10 min, and adding G with constant weight at 120 deg.C4The glass crucible is filtered by suction, the precipitate is transferred by using a potassium tetraphenylborate ethanolate saturated solution, and the precipitate is washed 3 to 4 times by 15ml, and is dried by suction each time. The crucible was taken down, washed once along the crucible wall with 2ml of absolute ethanol, and drained. G is to be4The glass crucible was dried at 120 ℃ to a constant weight, placed in a desiccator to cool to room temperature, and weighed. According to the formula of the traditional method, the method comprises the following steps:
jia bottle, K2O content 58.31g/L
B bottle, K2O content 55.28g/L
Respectively heating the C and the D to about 70 ℃, respectively dropwise adding 10ml of sodium tetraphenylborate solution under stirring, continuously stirring for 1 minute, rapidly cooling to below 20 ℃ in running water, and standing for 10 minutes. By using a precedingG dried to constant weight at 120 deg.C4And (3) carrying out suction filtration on the glass crucible, transferring the precipitate into the glass crucible by using a tetraphenylboron potassium washing liquid, and continuously washing the precipitate for about 12 times by using a washing liquid, wherein the dosage of each time is about 5 ml. G is to be4The glass crucible is placed in a drying oven at 120 ℃ and dried to constant weight, and then placed in a dryer to be cooled to room temperature and weighed. Calculating according to the formula:
third sample K2The O content is 63.82g/L
D sample K2O content 63.78g/L
K determined according to the method2The average O content is 63.8g/L, which is close to the true value, and both the precision and the accuracy meet the requirements, and can provide reliable basis for production.
According to the traditional detection method, the absolute error of the parallel result reaches 3.03g/L, and deviates from the true value, and the precision and the accuracy of the parallel result do not meet the detection requirements.
Claims (1)
1. K in potassium dichromate production2The method for measuring the content of O is characterized by comprising the following steps of:
1) removing chromium: taking a potassium dichromate reaction solution V to be detected, adding a reducing agent under an acidic condition to completely reduce hexavalent chromium into trivalent chromium, and checking by using a diphenylcarbonyldihydrazide indicator to determine that the hexavalent chromium is completely reduced into the trivalent chromium; adding alkali to neutralize until the solution is neutral, keeping the temperature at 90-100 ℃ for 1-2h, filtering and washing until no K exists+Collecting the washing liquid; mixing sodium tetraphenylborate solution with small amount of washing solution tail solution to ensure no white precipitate and no K in precipitate obtained by filtering+；
2) Precipitation of potassium tetraphenylborate: heating the obtained washing liquid to boiling, dropwise adding a sodium tetraphenylborate solution under the stirring condition until potassium tetraphenylborate precipitate is generated, and cooling and standing;
3) and (3) precipitation transfer: carrying out suction filtration on the cooling liquid obtained in the step 2, washing the obtained precipitate by using tetraphenylboron potassium washing liquid, and finally placing the precipitate in a drying oven to dry to constant weight W;
4)K2the O content is calculated as follows:
A＝0.1314×W×1000/V；
wherein, A:K2o content, g/L; w: dry weight of the precipitate obtained in step 3, g; v: the potassium dichromate reaction solution, L, to be tested.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811258910.4A CN109211718B (en) | 2018-10-26 | 2018-10-26 | K in potassium dichromate production2Method for measuring O content |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811258910.4A CN109211718B (en) | 2018-10-26 | 2018-10-26 | K in potassium dichromate production2Method for measuring O content |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109211718A CN109211718A (en) | 2019-01-15 |
| CN109211718B true CN109211718B (en) | 2021-03-19 |
Family
ID=64997092
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811258910.4A Active CN109211718B (en) | 2018-10-26 | 2018-10-26 | K in potassium dichromate production2Method for measuring O content |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109211718B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113233507B (en) * | 2021-06-15 | 2022-09-13 | 湖北振华化学股份有限公司 | Method for preparing basic chromium sulfate from residual liquid in menadione production |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102331384A (en) * | 2011-07-07 | 2012-01-25 | 内蒙古包钢钢联股份有限公司 | Determination method of content of potassium in mud with iron |
| CN104849181A (en) * | 2015-06-09 | 2015-08-19 | 中蓝连海设计研究院 | Method for rapidly distinguishing potassium chloride particles and sodium chloride particles |
| CN105466802A (en) * | 2014-08-11 | 2016-04-06 | 宋淑芹 | Detection method for potassium in organic fertilizer |
| CN106277053A (en) * | 2016-07-25 | 2017-01-04 | 中国科学院过程工程研究所 | A kind of preparation method of chromium oxide |
| CN106353218A (en) * | 2016-11-17 | 2017-01-25 | 江南工业集团有限公司 | Continuous determination method of potassium nitrate and sodium nitrate mixed salt bath |
-
2018
- 2018-10-26 CN CN201811258910.4A patent/CN109211718B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102331384A (en) * | 2011-07-07 | 2012-01-25 | 内蒙古包钢钢联股份有限公司 | Determination method of content of potassium in mud with iron |
| CN105466802A (en) * | 2014-08-11 | 2016-04-06 | 宋淑芹 | Detection method for potassium in organic fertilizer |
| CN104849181A (en) * | 2015-06-09 | 2015-08-19 | 中蓝连海设计研究院 | Method for rapidly distinguishing potassium chloride particles and sodium chloride particles |
| CN106277053A (en) * | 2016-07-25 | 2017-01-04 | 中国科学院过程工程研究所 | A kind of preparation method of chromium oxide |
| CN106353218A (en) * | 2016-11-17 | 2017-01-25 | 江南工业集团有限公司 | Continuous determination method of potassium nitrate and sodium nitrate mixed salt bath |
Non-Patent Citations (3)
| Title |
|---|
| 四苯硼酸钠重量法测定氯化钾中钾含量结果不确定度的评定探讨;高云龙等;《化学分析计量》;20031231;第12卷(第2期);第10-12页 * |
| 四苯硼酸钾重量法测定氟硼酸钾含量;施建忠，叶闻俊，陈晓青;《浙江化工》;20090930;第40卷(第9期);第33-34页 * |
| 四苯硼钠滴定法快速测定钾;晏华中;《理化检验-化学分册》;20010131;第37卷(第1期);第39、42页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109211718A (en) | 2019-01-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104034722B (en) | Content of material assay method in a kind of complex silicon carbide | |
| CN108344789B (en) | Method for measuring fluorine content in continuous casting mold flux | |
| CN111830106A (en) | Method for measuring content of fluorine ions in serpentine | |
| CN107132219A (en) | A kind of method for continuously measuring of Zinc in Zinc Concentrates and iron content | |
| CN101334365A (en) | Determination method for chloride ion content of temper rolling liquor for steel plate rolling | |
| CN104181118A (en) | Method for measuring phosphorus content in chromite | |
| CN109211718B (en) | K in potassium dichromate production2Method for measuring O content | |
| CN102331385A (en) | Method for determining tungsten content in impure tungsten product | |
| CN105973822A (en) | Method for determining content of silver, copper, lead and zinc elements in gold concentrate | |
| CN100386617C (en) | Method for measuring alumina in aluminium fluoride | |
| CN105044275B (en) | The method of testing of alumina content in aluminium metaphosphate | |
| CN104458609B (en) | Method for auxiliary determination of substitution degree of water-soluble food-grade sodium carboxymethylcellulose by microwaves | |
| CN101140242A (en) | Application of | |
| CN100367025C (en) | Method for measuring alumina in cryolite | |
| CN108680562A (en) | The assay method of copper-lead zinc-manganese cadmium chromium in a kind of cyaniding tail washings | |
| CN111650194A (en) | Method for determining phosphorus content in iron ore by bismuth-phosphorus-molybdenum blue | |
| CN104062252A (en) | Method for measuring content of phosphorus pentoxide in glass | |
| CN107655886B (en) | Method for measuring silicon dioxide content in phosphorite by potassium fluosilicate volumetric method | |
| CN103983737A (en) | Method for analyzing composite type sodium polysulfide in aluminum alloy alkalization milling liquid | |
| CN103808708A (en) | Method for detecting components of industrial ammonium sulfate product | |
| CN112697952A (en) | Method for converting and measuring barium sulfate content in barite by adopting ammonium dihydrogen phosphate | |
| CN106353218A (en) | Continuous determination method of potassium nitrate and sodium nitrate mixed salt bath | |
| CN109387450B (en) | Method for measuring platinum content in platinum-palladium alloy ornament | |
| CN109596607A (en) | A kind of method of chloride ion in measurement silver cyanide | |
| CN104142283A (en) | Method for measuring barium titanate content |
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 |