CN103323402A - Portable chromium liquor components detection device and detection method - Google Patents
Portable chromium liquor components detection device and detection method Download PDFInfo
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- CN103323402A CN103323402A CN201310118196XA CN201310118196A CN103323402A CN 103323402 A CN103323402 A CN 103323402A CN 201310118196X A CN201310118196X A CN 201310118196XA CN 201310118196 A CN201310118196 A CN 201310118196A CN 103323402 A CN103323402 A CN 103323402A
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Abstract
The invention discloses a portable chromium liquor components detection device. The device comprises a shell consisting of an upper shell and a bottom shell, a circuit board and a colorimetric ware are disposed on the bottom shell; a photoelectric sensor and a LED light source are respectively disposed on the two sides of the colorimetric ware, and the wavelength of the LED light source is 580 nm; the circuit board is provided with a one-chip microcomputer and a processing circuit of the one-chip microcomputer; the photoelectric sensor and the LED light source are connected with the circuit board via wires; the upper shell is fixedly connected with a touch-control display screen, and the touch-control display screen is connected with the circuit board via a data flat cable; and the colorimetric ware is exposed through the upper surface shell. According to the portable chromium liquor components detection device, 580 nm monochromatic wavelength design, Bouguer-Beer law, and the one-chip microcomputer as a control conversion unit are all employed, so that the detection device is fast in detection speed, high in stability, low in detection result error rate, high in precision, less in detection personel workload, short in detection time and low in detection cost.
Description
Technical field
The present invention relates to electrodeposited chromium industry detection technique field, be specifically related to a kind of chrome liquor component detection apparatus and detection method thereof.
Background technology
In the electrodeposited chromium industry, solution composition mainly is made up of chromic anhydride, trivalent chromium, sulfate radical, and the detection of chromic anhydride and trivalent chromium content detects by titrimetry, and sulfuric acid utilizes centrifuge method to detect.Since titration chemical examination to operator's competency profiling than higher, simultaneously because of in the titration chemical examination process, the preparation of standard solution, demarcate, move links such as liquid process, titration end-point judgement and all easily produce error, so the accuracy of chemical examination is not high always, often because of the inaccurate quality fault that occurs of composition chemical examination.
Specifically, the shortcoming of traditional titration mainly embodies as follows: to laboratory personnel's technical requirement height, the beginner is difficult to grasp at short notice; Chemical examination speed is relatively slow, and the most of the time is wasted on the preliminary works such as standard solution preparation, demarcation, and the man-hour of expending is bigger, and a duty multipotency is not realized in the post; Addition and the order of the preparation of standard solution, demarcation, plating bath dilution, auxiliary reagent, and the error that endpoint exists is relatively large, causes the chemical examination accuracy not high; Assay step is loaded down with trivial details, not only needs in the chemical examination process plating bath is diluted, and the reagent of Tian Jiaing is more simultaneously, also needs activated carbon filtration in the project analysis process that has and boils, and operation is loaded down with trivial details, inefficiency; Chemical examination cost height, the chemical examination medicine that uses in traditional titration process more (chemical examination such as copper sulphate needs the chemical examination of 4 kinds of reagent, nickelous sulfate to need 5 kinds of reagent, and chromic chemical examination needs the reagent more than 5 kinds), consumption is also bigger, causes the chemical examination cost bigger; The utility appliance of using is more, such as analytical balance, electric furnace, a large amount of transfer pipet, reagent bottle, volumetric flask, buret etc.Therefore, the precision that traditional titrimetry does not detect is not high, and required time is long, workload is big, cost is high, can not adapt to the requirement of modern production.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of detection efficiency height, precision height, portable chrome liquor composition pick-up unit and detection method thereof that cost is low.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: a kind of portable chrome liquor component detection apparatus, it is characterized in that: comprise the shell that is constituted by upper casing and drain pan, at drain pan circuit board and cuvette are arranged fixedly, fixedly there are photoelectric sensor and led light source in the cuvette both sides, the wavelength of led light source is 580nm, and single-chip microcomputer and treatment circuit thereof are arranged on the circuit board, and photoelectric sensor and led light source are by lead connecting circuit plate; Upper casing fixedly has the touch-control display screen, and the touch-control display screen is by data winding displacement connecting circuit plate; Circuit board is provided with switch, data communication interface and power interface, and switch, data communication interface and power interface all expose in enclosure; Cuvette exposes the upper casing surface, is stamped the cuvette lid on it.
The detection method of this portable chrome liquor component detection apparatus,
A, chromic anhydride, sulfuric acid, chromic detection:
1), to the detection of chromic anhydride, getting No. 8 reagent of 0.3g is put in the 50ml color comparison tube, add deionized water to the 25ml scale, add No. 5 reagent of 2.5ml again, suitably concussion shakes up, getting the 0.5ml chrome liquor again adds in the color comparison tube, add water to the 50ml scale, turn upside down 3-5 times behind the jam-pack bottle cap, leave standstill 3min, treat that chrome liquor fully reacts and finish, get liquid and measure to 4/5 place of cuvette internal height; Shake up again before getting liquid, cuvette transparent surface paper handkerchief wiped clean, transparent surface is facing to light source;
2), to the detection of sulfuric acid, getting about 0.3g8 reagent is put in the 50ml color comparison tube, add deionized water to the 25ml scale, add No. 5 reagent of 2.5ml again, suitably concussion shakes up, get the 0.5ml chrome liquor again in color comparison tube, shake up the back and add No. 6 reagent of 2.5ml, add deionized water to the 50ml scale, leave standstill 5min behind the jam-pack bottle cap thermal agitation 20s, treat that chrome liquor fully reacts and finish, get liquid and measure to 4/5 place of cuvette internal height; Shake up again before getting liquid, cuvette transparent surface paper handkerchief wiped clean, transparent surface is facing to light source;
3), to chromic detection, get the 2.5ml chrome liquor in the 50ml color comparison tube, add No. 7 reagent of 2.5ml, add deionized water to the 25ml scale, turn upside down 3-5 times behind the jam-pack bottle cap, leave standstill 3min, treat that chrome liquor fully reacts and finish, get liquid and measure to 4/5 place of cuvette internal height; Shake up again before getting liquid, cuvette transparent surface paper handkerchief wiped clean, transparent surface is facing to light source;
No. 5 reagent: the PH correctives prevents the generation of subsidiary reaction;
No. 6 reagent: the characteristic precipitation reagent, selectively precipitate specific ion;
No. 7 reagent: developer, impel the easier colour developing of relevant ions, be easy to measure;
No. 8 reagent: reductive agent, reduce extraordinary composition, and it quantitatively detected.
The using method of B, this pick-up unit:
1), start, system host preheating 500 seconds, countdown end equipment reaches stable, enters to detect the interface, detects the interface and divides three: chromic anhydride, sulfuric acid, trivalent chromium;
2), enter this detection interface by chromic anhydride, sulfuric acid, chromic sequential touches options menu, carry out coherent detection; Detect the interface four operations are arranged: sky is calibrated, please be detected, calibrate, return, and wherein " empty calibration " and " please detect " are for detection of composition, and " calibration " is used for the correction-compensation to testing result, and " returning " returned for detection of the interface;
3), touch " result's calibration " key and calibrate the interface to testing result, also there are four operations at this interface: ++ key,--key, preserve, return; " ++ key " and "--key " be used for the correction-compensation to calibration result, " preservation " key is used for the preservation to correction result; Enter this interface at every turn, all must carry out " preservation " operation after, carry out again " returning " operation;
4), testing process: it is empty 1. detecting in the cuvette, builds the cuvette lid, by " the empty calibration ", waits to be calibrated finishing, and " empty calibration " becomes " calibration is finished ", and calibration is finished; 2. open cuvette lid, it is clean to wipe examination, gets the liquid to be detected for preparing to cuvette, put into groove also transparent area be parallel to light path, build the cuvette lid, by " please detect ", to be detected finishing, " please detect " and become " detect and finish ", detection is finished, and the touch-control display screen shows testing result;
5), detect to finish after, close main frame, clean color comparison tube and cuvette, wiped clean is put into casing.
This pick-up unit and detection method are based on " lambert-law of Beer ", utilize the monochromatic light of fixed wave length that solution composition is tested, utilize the monochromatic light of the specific wavelength that polariscope or special light sources provide by standard specimen and analyzed sample, relatively both light intensities are come the amalyzing substances composition, by measuring the absorbance log of measured matter light in certain wave strong point or certain wavelength coverage, this material is carried out quantitative test.
When measured matter solution was passed in the monochromatic light radiation, the thickness of the amount that is absorbed by this material and the concentration of this material and liquid layer (be light path, also in optical path length) was directly proportional, its relation as shown in the formula:
A=-log(Ι/Ι。)=-lgT=kLc
In the formula: A is absorbance log;
Ι。Monochromatic light intensity for incident;
Ι is the monochromatic light intensity of transmission;
T is the transmittance of material;
K is absorption coefficient;
L is the light path of analyte;
C is the concentration of material.
Here it is lambert-law of Beer.
Material is to the selectivity absorbing wavelength of light, and its corresponding absorption coefficient k is the physical constant of this material.Behind known certain pure material absorption coefficient under certain condition, available similarity condition is measured its absorbance log with this sample wiring solution-forming, can calculate the content of this material in the sample according to lambert-law of Beer.At visible region, except some material has the absorption light, a lot of materials itself do not absorb, but can add chromogenic reagent under certain condition or make after its colour developing mensuration again through handling, and claim colorimetric analysis again.
According to above-mentioned theory, be written into the concentration that corresponding calculation procedure just can detect each composition of chrome liquor at single-chip microcomputer.
In sulphur phosphorus mixed acid solution, trivalent chromium is blue solution, its maximum absorbance is at the 58Onm place, do blank to eliminate background interference with the pure chromic acid solution identical with the sample hexavalent chromium concentration, add phosphoric acid and shelter ferric interference, utilize this pick-up unit test, according to test absorbance size, directly calculate chromic content by single-chip microcomputer.
Sexavalent chrome exists with the form that chromic acid is followed or dichromic acid is followed in plating bath, can not directly measure with spectrophotometer, at first need the sexavalent chrome in the electroplating solution is reduced into trivalent chromium with reductive agent, in sulphur phosphorus mixed acid solution, trivalent chromium is blue solution, its maximum absorbance is at the 58Ohm place, do blank to eliminate background interference with the pure chromic acid solution identical with the sample hexavalent chromium concentration, add phosphoric acid and shelter ferric interference, utilize this pick-up unit test, according to test absorbance size, directly be converted into the content of chromic anhydride by single-chip microcomputer;
The method of testing of sulfate radical in the chromium plating solution, the sexavalent chrome Restore All in the plating bath at first, in acid medium, add barium chloride and handle sample solution, sulfate ion and barium chloride effect generate the very little barium sulphate white precipitate of solubleness, make the solution muddiness, under the situation of the existence of spreading agent, the solution of precipitation can the short-term layering, but form the solution with even turbidity, when sulfate ion concentration in 1-10g/L scope, its turbidity is directly proportional with sulfate ion concentration in the solution, tests its absorbance by this pick-up unit, according to test absorbance size, directly be converted into the content of sulfate radical by single-chip microcomputer; Thereby calculate the content of sulfate ion in the solution.
The present invention adopts the monochromatic wavelength design of 580nm, avoids the degree of stability of optical source wavelength to the influence of test result, and as the control scaling unit, stability is high by single-chip microcomputer for equipment, test result repeatability, and error rate can both guarantee; Technical requirement to the beginner is not high, only needs the operator can use simple tool such as pipettor that plating bath is diluted, and simply understands the use computer, just can finish the chemical examination work of relevant composition; Chemical examination speed is fast, does not need to prepare any standard solution, and direct reading in the chemical examination process does not need relevantly manually to convert again, and the chemical examination of a project only needed just can finish in 1-2 minutes, and speed also can increase after the skilled operation; The chemical examination initial stage does not need to use producer's configuration standard solution, and there has been the preprepared typical curve in device interior, and each manufacturer's standard curve unanimity, so the examination criteria unanimity, and the data error that obtains has just dropped to minimum; Assay step is simple, grasps easily, only the plating bath dilution need be moved in the cuvette before the chemical examination to get final product, and follow-up work only needs shirtsleeve operation equipment to finish; Do not need utility appliance such as Allocation Analysis balance, electric furnace, conical flask, beaker, only need several volume weight tubes and reagent bottle to get final product, therefore the equipment that needs is considerably less.
Description of drawings
Fig. 1 is one-piece construction synoptic diagram of the present invention;
Fig. 2 is inner structure synoptic diagram of the present invention.
Among the figure, 1 is upper casing, and 2 is the touch-control display screen, and 3 is drain pan, and 4 is circuit board, and 5 is cuvette, and 6 is led light source, and 7 are the cuvette lid, and 8 is attaching plug, and 9 is photoelectric sensor.
Embodiment
In the present embodiment, see figures.1.and.2, described portable chrome liquor component detection apparatus, comprise the shell that is constituted by upper casing 1 and drain pan 3, at drain pan 3 circuit board 4 and cuvette 5 are arranged fixedly, fixedly there are photoelectric sensor 9 and led light source 6 in cuvette 5 both sides, and the wavelength of led light source 6 is 580nm, single-chip microcomputer and treatment circuit thereof are arranged on the circuit board 4, and photoelectric sensor 9 and led light source 6 are by lead connecting circuit plate 4; Upper casing 1 fixedly has touch-control display screen 2, and touch-control display screen 2 is by data winding displacement connecting circuit plate 4; Circuit board 4 is provided with switch, data communication interface and power interface, and switch, data communication interface and power interface all expose in enclosure, and power interface connects power supply adaptors by attaching plug 8; Cuvette 5 exposes upper casing 1 surface, is stamped cuvette lid 7 on it.
The detection method of this portable chrome liquor component detection apparatus,
A, chromic anhydride, sulfuric acid, chromic detection:
1), to the detection of chromic anhydride, getting No. 8 reagent of 0.3g is put in the 50ml color comparison tube, add deionized water to the 25ml scale, add No. 5 reagent of 2.5ml again, suitably concussion shakes up, getting the 0.5ml chrome liquor again adds in the color comparison tube, add water to the 50ml scale, turn upside down 3-5 times behind the jam-pack bottle cap, leave standstill 3min, treat that chrome liquor fully reacts and finish, get liquid and measure to 4/5 place of cuvette 5 internal height; Shake up again before getting liquid, cuvette 5 transparent surfaces paper handkerchief wiped clean, transparent surface is facing to light source;
2), to the detection of sulfuric acid, getting about 0.3g8 reagent is put in the 50ml color comparison tube, add deionized water to the 25ml scale, add No. 5 reagent of 2.5ml again, suitably concussion shakes up, get the 0.5ml chrome liquor again in color comparison tube, shake up the back and add No. 6 reagent of 2.5ml, add deionized water to the 50ml scale, leave standstill 5min behind the jam-pack bottle cap thermal agitation 20s, treat that chrome liquor fully reacts and finish, get liquid and measure to 4/5 place of cuvette 5 internal height; Shake up again before getting liquid, cuvette 5 transparent surfaces paper handkerchief wiped clean, transparent surface is facing to light source;
3), to chromic detection, get the 2.5ml chrome liquor in the 50ml color comparison tube, add No. 7 reagent of 2.5ml, add deionized water to the 25ml scale, turn upside down 3-5 times behind the jam-pack bottle cap, leave standstill 3min, treat that chrome liquor fully reacts and finish, get liquid and measure to 4/5 place of cuvette 5 internal height; Shake up again before getting liquid, cuvette 5 transparent surfaces paper handkerchief wiped clean, transparent surface is facing to light source;
The using method of B, this pick-up unit:
1), start, system host preheating 500 seconds, countdown end equipment reaches stable, enters to detect the interface, detects the interface and divides three: chromic anhydride, sulfuric acid, trivalent chromium;
2), enter this detection interface by chromic anhydride, sulfuric acid, chromic sequential touches options menu, carry out coherent detection; Detect the interface four operations are arranged: sky is calibrated, please be detected, calibrate, return, and wherein " empty calibration " and " please detect " are for detection of composition, and " calibration " is used for the correction-compensation to testing result, and " returning " returned for detection of the interface;
3), touch " result's calibration " key and calibrate the interface to testing result, also there are four operations at this interface: ++ key,--key, preserve, return; " ++ key " and "--key " be used for the correction-compensation to calibration result, " preservation " key is used for the preservation to correction result; Enter this interface at every turn, all must carry out " preservation " operation after, carry out again " returning " operation;
4), testing process: it is empty 1. detecting in the cuvette, builds the cuvette lid, by " the empty calibration ", waits to be calibrated finishing, and " empty calibration " becomes " calibration is finished ", and calibration is finished; 2. open cuvette lid, it is clean to wipe examination, gets the liquid to be detected for preparing to cuvette, put into groove also transparent area be parallel to light path, build the cuvette lid, by " please detect ", to be detected finishing, " please detect " and become " detect and finish ", detection is finished, and the touch-control display screen shows testing result;
5), detect to finish after, close main frame, clean color comparison tube and cuvette, wiped clean is put into casing.
Below the present invention is described in detail, the above only is the present invention's preferred embodiment, when not limiting the scope of the present invention, namely allly does impartial change and modify according to the application's scope, all should still belong in the covering scope of the present invention.
Claims (2)
1. portable chrome liquor component detection apparatus, it is characterized in that: comprise the shell that is constituted by upper casing and drain pan, at drain pan circuit board and cuvette are arranged fixedly, fixedly there are photoelectric sensor and led light source in the cuvette both sides, single-chip microcomputer and treatment circuit thereof are arranged on the circuit board, and photoelectric sensor and led light source are by lead connecting circuit plate; Upper casing fixedly has the touch-control display screen, and the touch-control display screen is by data winding displacement connecting circuit plate; Circuit board is provided with switch, data communication interface and power interface, and switch, data communication interface and power interface all expose in enclosure; Cuvette exposes the upper casing surface, is stamped the cuvette lid on it.
2. the detection method of the described portable chrome liquor component detection apparatus of claim 1 is characterized in that:
A, chromic anhydride, sulfuric acid, chromic detection:
1), to the detection of chromic anhydride, getting No. 8 reagent of 0.3g is put in the 50ml color comparison tube, add deionized water to the 25ml scale, add No. 5 reagent of 2.5ml again, suitably concussion shakes up, getting the 0.5ml chrome liquor again adds in the color comparison tube, add water to the 50ml scale, turn upside down 3-5 times behind the jam-pack bottle cap, leave standstill 3min, treat that chrome liquor fully reacts and finish, get liquid and measure to 4/5 place of cuvette internal height; Shake up again before getting liquid, cuvette transparent surface paper handkerchief wiped clean, transparent surface is facing to light source;
2), to the detection of sulfuric acid, getting about 0.3g8 reagent is put in the 50ml color comparison tube, add deionized water to the 25ml scale, add No. 5 reagent of 2.5ml again, suitably concussion shakes up, get the 0.5ml chrome liquor again in color comparison tube, shake up the back and add No. 6 reagent of 2.5ml, add deionized water to the 50ml scale, leave standstill 5min behind the jam-pack bottle cap thermal agitation 20s, treat that chrome liquor fully reacts and finish, get liquid and measure to 4/5 place of cuvette internal height; Shake up again before getting liquid, cuvette transparent surface paper handkerchief wiped clean, transparent surface is facing to light source;
3), to chromic detection, get the 2.5ml chrome liquor in the 50ml color comparison tube, add No. 7 reagent of 2.5ml, add deionized water to the 25ml scale, turn upside down 3-5 times behind the jam-pack bottle cap, leave standstill 3min, treat that chrome liquor fully reacts and finish, get liquid and measure to 4/5 place of cuvette internal height; Shake up again before getting liquid, cuvette transparent surface paper handkerchief wiped clean, transparent surface is facing to light source;
The using method of B, this pick-up unit:
1), start, system host preheating 500 seconds, countdown end equipment reaches stable, enters to detect the interface, detects the interface and divides three: chromic anhydride, sulfuric acid, trivalent chromium;
2), enter this detection interface by chromic anhydride, sulfuric acid, chromic sequential touches options menu, carry out coherent detection; Detect the interface four operations are arranged: sky is calibrated, please be detected, calibrate, return, and wherein " empty calibration " and " please detect " are for detection of composition, and " calibration " is used for the correction-compensation to testing result, and " returning " returned for detection of the interface;
3), touch " result's calibration " key and calibrate the interface to testing result, also there are four operations at this interface: ++ key,--key, preserve, return; " ++ key " and "--key " be used for the correction-compensation to calibration result, " preservation " key is used for the preservation to correction result; Enter this interface at every turn, all must carry out " preservation " operation after, carry out again " returning " operation;
4), testing process: it is empty 1. detecting in the cuvette, builds the cuvette lid, by " the empty calibration ", waits to be calibrated finishing, and " empty calibration " becomes " calibration is finished ", and calibration is finished; 2. open cuvette lid, it is clean to wipe examination, gets the liquid to be detected for preparing to cuvette, put into groove also transparent area be parallel to light path, build the cuvette lid, by " please detect ", to be detected finishing, " please detect " and become " detect and finish ", detection is finished, and the touch-control display screen shows testing result;
5), detect to finish after, close main frame, clean color comparison tube and cuvette, wiped clean is put into casing.
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| CN201310118196XA CN103323402A (en) | 2013-04-07 | 2013-04-07 | Portable chromium liquor components detection device and detection method |
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| CN201310118196XA CN103323402A (en) | 2013-04-07 | 2013-04-07 | Portable chromium liquor components detection device and detection method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108572153A (en) * | 2017-03-07 | 2018-09-25 | 泰安市康宇医疗器械有限公司 | A kind of portable breast milk analyser |
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| CN202041501U (en) * | 2011-02-24 | 2011-11-16 | 张天洪 | Electroplating liquid analyzer |
| CN102564968A (en) * | 2010-12-31 | 2012-07-11 | 东莞市常晋凹版模具有限公司 | Plating solution component analysis method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN200982951Y (en) * | 2006-06-21 | 2007-11-28 | 中国人民解放军军事医学科学院卫生学环境医学研究所 | Intelligent hand-held photoelectrical color contrast device |
| CN102564968A (en) * | 2010-12-31 | 2012-07-11 | 东莞市常晋凹版模具有限公司 | Plating solution component analysis method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108572153A (en) * | 2017-03-07 | 2018-09-25 | 泰安市康宇医疗器械有限公司 | A kind of portable breast milk analyser |
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Owner name: ZHANG GUIMING Free format text: FORMER OWNER: DONGGUAN CHANGJIN GRAVURE MOULD CO., LTD. Effective date: 20150819 Free format text: FORMER OWNER: ZHANG GUIMING Effective date: 20150819 |
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