CN105372193A - Detection method of sulfate radical in chromic anhydride - Google Patents
Detection method of sulfate radical in chromic anhydride Download PDFInfo
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- CN105372193A CN105372193A CN201510872588.4A CN201510872588A CN105372193A CN 105372193 A CN105372193 A CN 105372193A CN 201510872588 A CN201510872588 A CN 201510872588A CN 105372193 A CN105372193 A CN 105372193A
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- sulfate radical
- detection method
- chromic
- chromic anhybride
- chromic anhydride
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- 238000001514 detection method Methods 0.000 title claims abstract description 24
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000003381 stabilizer Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 7
- 239000008399 tap water Substances 0.000 claims abstract description 6
- 235000020679 tap water Nutrition 0.000 claims abstract description 6
- 239000008236 heating water Substances 0.000 claims description 10
- 238000001556 precipitation Methods 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 108010010803 Gelatin Proteins 0.000 claims description 3
- 229920000159 gelatin Polymers 0.000 claims description 3
- 239000008273 gelatin Substances 0.000 claims description 3
- 235000019322 gelatine Nutrition 0.000 claims description 3
- 235000011852 gelatine desserts Nutrition 0.000 claims description 3
- 238000012360 testing method Methods 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 238000002798 spectrophotometry method Methods 0.000 abstract description 3
- 238000004806 packaging method and process Methods 0.000 abstract description 2
- 238000012857 repacking Methods 0.000 abstract 1
- NIAGBSSWEZDNMT-UHFFFAOYSA-M tetraoxidosulfate(.1-) Chemical compound [O]S([O-])(=O)=O NIAGBSSWEZDNMT-UHFFFAOYSA-M 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 3
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 3
- 229910001626 barium chloride Inorganic materials 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 239000004305 biphenyl Substances 0.000 description 2
- 235000010290 biphenyl Nutrition 0.000 description 2
- 125000006267 biphenyl group Chemical group 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- XEVRDFDBXJMZFG-UHFFFAOYSA-N carbonyl dihydrazine Chemical compound NNC(=O)NN XEVRDFDBXJMZFG-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000004848 nephelometry Methods 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 241000370738 Chlorion Species 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 238000011481 absorbance measurement Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000004380 ashing Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000004879 turbidimetry Methods 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses a detection method of sulfate radical in chromic anhydride. The method includes the steps of: weighing 15g of chromic anhydride, dissolving in a 100ml flask and adjusting to a constant volume for standby as a solution to be tested; taking 5ml of chromic anhydride solution, adding into a colorimetric tube, then adding 5ml of prepared hydrochloric acid; adding 10ml of absolute ethyl alcohol, shaking evenly, quickly adding into a beaker of 65 DEG C, heating in a water bath for 4 min, taking out the colorimetric tube, showering outer wall of the tube by tap water to reduce the temperature to under 40 DEG C; adding 1ml of a stabilizer, adding 3ml of a precipitant, adding into a beaker of 35 DEG C, heating in a water bath for 8 min, taking out the beaker, shaking slightly, detecting in a spectrophotometer, recording data, and converting by using correlative formula to obtain the content of sulfate radical. The stabilizer can stabilize the sulfate radical ion in chromic anhydride; the spectrophotometric method for determination of the sulfate ion concentration has short testing time; and the method is in full compliance with the demand in packaging production, and reduces the repacking and the detection cost.
Description
Technical field
The invention belongs to sulfate radical content detection technique field, particularly relate to sulfate radical detection method in a kind of chromic anhybride.
Background technology
Current is the gravimetric method that step is various to the sulfate radical detection method in chromic anhybride, this traditional method that production division and detection department are all, although the method detects accurately, but the whole cycle is very long, but in process of production, after chromic anhybride is produced, due to the easy moisture absorption of chromic anhybride, just to encapsulate when therefore dropping to 50 DEG C at temperature, this section of aperture time is about half an hour, the quality of chromic anhybride cannot be detected in short time, and manufacturer uses simple and that error rate is high turbidimetry (range estimation) at present, the method causes later rework serious, and then improve the cost of manufacturer.Thus just start to research and develop this new detection method, this detection method accurately can detect the sulfate radical content in chromic anhybride at short notice.
Existing employing, gravimetric method, reagent: sulfuric acid, 95% ethanol, hydrochloric acid solution (3:7), acetic acid solution (1:1), barium chloride (BCHO) solution (100g/L), liquor argenti nitratis ophthalmicus (17g/L), sulfate standard solution (1mL solution containing sulfate radicals 0.20mg), diphenyl azo carbohydrazide indicator solution (2g/L); Instrument: high temperature furnace (temperature-controllable is built in 700 ± 2 DEG C); Take (about 10g sample, be accurate to 0.01g and be placed in 500mL beaker, add the water-soluble solution of 100mL, add 50ML sulfate standard solution and 100ML hydrochloric acid solution, heating, under agitation drips about 25ML ethanol, heating and thermal insulation 30 points in boiling water bath, as reduced not exclusively, then add ethanol (whether reducing completely with the inspection of diphenyl azo carbohydrazide).Filter with middling speed qualitative filter paper, with hot wash to filter paper redgreen, filtrate and wash pools are in 500ML beaker, be diluted with water to about 300ML, heating is boiled, 50ML barium chloride solution is slowly added while stirring under slight boiling condition, 20ML acetic acid solution and preprepared a little quantitative filter paper paper pulp, abundant stir about 2 points, water-bath heats 30 points, be incubated 2H or at room temperature place 8H, precipitation quantitative filter paper filtration at a slow speed, fully washs with hot water and (checks with liquor argenti nitratis ophthalmicus) to without chlorion; Filter paper and precipitation are placed in advance prior to 700 ± 2 DEG C of calcinations to the porcelain crucible of constant mass, low temperature dry ashing on electric furnace, take off, a sulfuric acid is added after cooling, electric furnace being heated to Mao Baiyan to the greatest extent, moving in 700 ± 2 DEG C of high temperature furnaces calcination to constant mass: do blank test, except not adding except test portion simultaneously, other amount of reagent added is identical with testing liquid, and processes with test portion is simultaneously same.
Gravimetric method accurately can measure sulfate radical content, but needs the quite a long time equally due to the method, still can not go out result in side at short notice, and therefore the method is at present only for encapsulating rear sampling detection up to standard.
Summary of the invention
The object of the present invention is to provide sulfate radical detection method in a kind of chromic anhybride, be intended to solve gravimetric method and can not go out result in side at short notice, only for encapsulating the problem of rear sampling detection up to standard.
The present invention is achieved in that sulfate radical detection method in a kind of chromic anhybride, and in described chromic anhybride, sulfate radical detection method comprises:
Take 15g chromic anhybride, be dissolved in 100ml volumetric flask and constant volume, as solution to be measured;
Measure 5ml chromic anhybride solution in color comparison tube, add 5ml hydrochloric acid; 10ml absolute ethyl alcohol, shakes up and puts into rapidly 65 DEG C of beaker heating water baths 4 minutes, takes out color comparison tube tap water shower outer tube wall, makes its temperature drop to less than 40 DEG C;
Add stabilizing agent 1ml, then add precipitation agent 3ml, shake up and put into 35 DEG C of beaker heating water bath 8min, after taking-up, gently the distant spectrophotometer 880nm that puts into detects, and record data substitute into typical curve calculating just can draw sulfate radical content.
Further, the method for drafting of described typical curve, takes the chromic anhydride 15g of sulfate radical-free, is settled to 100ml, pipettes respectively in 5mll chromic anhybride solution to 7 color comparison tube, adds 5ml hydrochloric acid respectively; 10ml absolute ethyl alcohol, fully shakes up and puts into 65 DEG C of beaker heating water baths 4 minutes, and take out color comparison tube tap water shower outer tube wall, temperature drops to less than 40 DEG C; Add stabilizing agent 1ml respectively, the mass percent interval of sulfate radical in industrial chromic anhydride is: 0.030% ~ 0.110%; Shake up and put into 35 DEG C of beaker heating water bath 8min, the rear jog of taking-up is put into spectrophotometer 880nm and is detected, record data Criterion curve.
Further, the volume ratio of described hydrochloric acid is 1:1.
Further, described precipitation agent collocation method: take 5gBacl
2be dissolved in 100ml volumetric flask, constant volume is to scale mark.
Further, described stabilizing agent collocation method: get 0.1g polyvinyl alcohol (PVA) respectively, 0.1g gelatin, with hot water dissolving, cooling constant volume is to 1000ml.
Sulfate radical detection method in chromic anhybride provided by the invention, stabilizing agent can make the sulfate ion in chromic anhybride stablize, its sulfate ion concentration is measured by spectrophotometric method (nephelometry), whole checkout procedure (not comprising sampling between production) can be obtained a result within half an hour, meet demand during Production and Packaging completely, directly effective minimizing returns bag, reduces testing cost, thus decreases pollution and production cost.
Accompanying drawing explanation
Fig. 1 is sulfate radical detection method process flow diagram in the chromic anhybride that provides of the embodiment of the present invention.
Fig. 2 is sulfate radical examination criteria curve map in the chromic anhybride that provides of the embodiment of the present invention.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The present invention utilizes spectrophotometric method (nephelometry) to measure sulfate radical in chromic anhybride, is to find this all stabilizing agent and spreading agent makes the method measurement result have stability.
Below in conjunction with accompanying drawing, application principle of the present invention is explained in detail.
As shown in Figure 1, in the chromic anhybride of the embodiment of the present invention, sulfate radical detection method comprises the following steps:
S101: take 15g chromic anhybride, is dissolved in 100ml volumetric flask and constant volume, as solution to be measured; Therefrom measure 5ml chromic anhybride solution in color comparison tube, then add the hydrochloric acid (1:1) that 5ml prepares in advance;
S102: add 10ml absolute ethyl alcohol, fully shakes up and puts into rapidly 65 DEG C of beaker heating water baths 4 minutes, takes out color comparison tube tap water shower outer tube wall, makes its temperature drop to less than 40 DEG C;
S103: add stabilizing agent 1ml, add precipitation agent 3ml again, fully shake up and put into rapidly 35 DEG C of beaker heating water bath 8min, after taking-up, gently distant spectrophotometer (880nm) of putting into detects, according to industrial chromic anhydride sulfate radical content Criterion curve record data, the absorbance measurement of sample, substitutes into typical curve and calculates sulfate radical content.
Precipitation agent: accurately take 5gBacl
2be dissolved in 100ml volumetric flask, constant volume is to scale mark, after adding this reagent, generate a kind of water-fast material, stabilizing agent: accurately take 0.1g polyvinyl alcohol (PVA) respectively, 0.1g gelatin, with hot water dissolving, cooling constant volume to 1000ml, make generation water-fast material can long-time stable suspension in the solution.
Below in conjunction with test, effect of the present invention is further described.
Typical curve as shown in Figure 2.
Table one, 1-5 sample are former state (sample provide for * * Chemical Co., Ltd.)
| Sample number into spectrum | Absorbance A 1 | Absorbance A 2 | Absorbance A 3 | SO4 (this method) | SO4 (gravimetric method) |
| 1 | 0.086 | 0.086 | 0.086 | 0.0653％ | 0.063％ |
| 2 | 0.064 | 0.064 | 0.065 | 0.0516％ | 0.054％ |
| 3 | 0.059 | 0.062 | 0.060 | 0.0490％ | 0.051％ |
| 4 | 0.072 | 0.072 | 0.072 | 0.0561％ | 0.054％ |
| 5 | 0.055 | 0.055 | 0.055 | 0.0450％ | 0.045％ |
Table two, No. 1 sample mark-on test result
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. a sulfate radical detection method in chromic anhybride, is characterized in that, in described chromic anhybride, sulfate radical detection method comprises:
Take 15g chromic anhybride, be dissolved in 100ml volumetric flask and constant volume, as solution to be measured;
Measure 5ml chromic anhybride solution in color comparison tube, add 5ml hydrochloric acid; 10ml absolute ethyl alcohol, shakes up and puts into 65 DEG C of beaker heating water baths 4 minutes, takes out color comparison tube tap water shower outer tube wall, makes its temperature drop to less than 40 DEG C;
Add stabilizing agent 1ml, then add precipitation agent 3ml, shake up and put into 35 DEG C of beaker heating water bath 8min, after taking-up, gently the distant spectrophotometer 880nm that puts into detects, and record data substitute into typical curve calculating just can draw sulfate radical content.
2. sulfate radical detection method in chromic anhybride as claimed in claim 1, is characterized in that, the method for drafting of described typical curve, take the chromic anhydride 15g of sulfate radical-free, be settled to 100ml, pipette respectively in 5mll chromic anhybride solution to 7 color comparison tube, add 5ml hydrochloric acid respectively; 10ml absolute ethyl alcohol, fully shakes up and puts into 65 DEG C of beaker heating water baths 4 minutes, and take out color comparison tube tap water shower outer tube wall, temperature drops to less than 40 DEG C; Add stabilizing agent 1ml respectively, the mass percent interval of sulfate radical in industrial chromic anhydride is: 0.030% ~ 0.110%; Shake up and put into 35 DEG C of beaker heating water bath 8min, the rear jog of taking-up is put into spectrophotometer 880nm and is detected, record data Criterion curve.
3. sulfate radical detection method in the chromic anhybride as described in claim 1 and 2, is characterized in that, the volume ratio of described hydrochloric acid is 1:1.
4. sulfate radical detection method in chromic anhybride as claimed in claim 1, is characterized in that, described precipitation agent collocation method: take 5gBacl
2be dissolved in 100ml volumetric flask, constant volume is to scale mark.
5. sulfate radical detection method in chromic anhybride as claimed in claim 1, is characterized in that, described stabilizing agent collocation method: get 0.1g polyvinyl alcohol (PVA) respectively, 0.1g gelatin, and with hot water dissolving, cooling constant volume is to 1000ml.
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| CN201510872588.4A CN105372193A (en) | 2015-12-02 | 2015-12-02 | Detection method of sulfate radical in chromic anhydride |
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| CN201510872588.4A CN105372193A (en) | 2015-12-02 | 2015-12-02 | Detection method of sulfate radical in chromic anhydride |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106908405A (en) * | 2017-03-27 | 2017-06-30 | 中国科学院青岛生物能源与过程研究所 | A kind of hypersensitive sulfate radical nephelometric analysis method and detection means |
| CN109632790A (en) * | 2018-12-11 | 2019-04-16 | 重庆建工建材物流有限公司 | SO in a kind of mixing plant recycle-water42-The rapid detection method of content |
| CN109724912A (en) * | 2019-02-21 | 2019-05-07 | 孙峰 | It is a kind of quickly to measure sulfate ion depth of invasion test method in regeneration concrete test specimen |
| CN112098350A (en) * | 2020-08-28 | 2020-12-18 | 佛山东鹏洁具股份有限公司 | Method for detecting concentration of soluble sulfate ions in sanitary ceramic slurry |
| CN112924400A (en) * | 2019-12-05 | 2021-06-08 | 中粮生物科技股份有限公司 | Method for detecting sulfate content in citric acid sample |
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| CN109724912A (en) * | 2019-02-21 | 2019-05-07 | 孙峰 | It is a kind of quickly to measure sulfate ion depth of invasion test method in regeneration concrete test specimen |
| CN112924400A (en) * | 2019-12-05 | 2021-06-08 | 中粮生物科技股份有限公司 | Method for detecting sulfate content in citric acid sample |
| CN112098350A (en) * | 2020-08-28 | 2020-12-18 | 佛山东鹏洁具股份有限公司 | Method for detecting concentration of soluble sulfate ions in sanitary ceramic slurry |
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Inventor after: Liu Yonggang Inventor after: Su Li Inventor after: Zheng Lei Inventor after: Ma Guohua Inventor after: Zhang Yichuan Inventor after: Zhu Yunyao Inventor before: Liu Yonggang Inventor before: Su Li Inventor before: Ma Guohua Inventor before: Zhang Yichuan Inventor before: Zhu Yunyao |
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