CN204789319U - Detection apparatus for total phosphorus content in short -term test water sample - Google Patents

Detection apparatus for total phosphorus content in short -term test water sample Download PDF

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Publication number
CN204789319U
CN204789319U CN201520553050.2U CN201520553050U CN204789319U CN 204789319 U CN204789319 U CN 204789319U CN 201520553050 U CN201520553050 U CN 201520553050U CN 204789319 U CN204789319 U CN 204789319U
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China
Prior art keywords
room
water sample
color comparison
total phosphorus
phosphorus content
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Expired - Fee Related
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CN201520553050.2U
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Chinese (zh)
Inventor
蒋然
梁志宏
刘艺斯
郭伟
朱小平
叶伟聪
雷列辉
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Pearl River Hydraulic Research Institute of PRWRC
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Pearl River Hydraulic Research Institute of PRWRC
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Abstract

The utility model discloses a detection apparatus for total phosphorus content in short -term test water sample, including light source room, color comparison room and the detection room that connects gradually, the both sides of color comparison room be equipped with 2 respectively with the light source room with detect the communicating logical unthreaded hole in room, still include colour comparison tube and mount, the mount is installed in the color comparison indoorly, the colour comparison tube inserts the color comparison room, and the mount is fixed in to the bottom of colour comparison tube, simultaneously, 2 it is located same straight line with the colour comparison tube to lead to the unthreaded hole. The utility model discloses reduced the drip washing process before the water sample detection that awaits measuring, simplified detect operation, improved detection efficiency, can generally popularize and apply in the laboratory simultaneously.

Description

The pick-up unit of total phosphorus content in a kind of quick detection water sample
Technical field
The utility model relates to detection technique, specifically the pick-up unit of total phosphorus content in a kind of quick detection water sample.
Background technology
Phosphorus is the important indicator of the reflection contaminated degree of water body and body eutrophication, and the enforcement of Ye Shi China is to one of leading indicator of pollutant emission factor.Phosphorus be mainly derived from industrial waste water and sanitary wastewater, a large amount of discharges of these phosphorus-containing wastewaters, the phosphorus content in water body is increased and causes body eutrophication, fish and other biological mass mortality, water quality deterioration and have stench.In recent years, along with improving and strengthening of national environmental protection regulation, require that comprising total phosphorus to all kinds of waste water and urban river water carries out strict monitoring in internal contamination thing index.Obviously, easy, fast and efficiently detection method total phosphorus carried out for sampling in enormous quantities detect that to analyze be very important.
At present, the main method measuring total phosphorus has spectrophotometric method, flow injection analysis, the chromatography of ions.Although the chromatography of ions has clearing up the sample solution after process without the need to adding the advantage of chemical reagent, flow injection analyzer method combines pre-service, precession sample introduction, detecting unit, fast easy to operate, suitable in enormous quantities test, but the expense of the purchasing of its instrument, use and maintenance be the 5-10 of visible spectrophotometer doubly.Visible spectrophotometric instrument have cheap, detect the advantages such as sensitive, become the conventional analytical instruments of all kinds of testing laboratory.Existing spectrophotometer adopts a light source that can produce multiple wavelength, by serial light-dividing device, thus produces the light source of specific wavelength, after the sample of light therethrough test, some light is absorbed, the light absorption value of calculation sample, thus the concentration changing into sample.Based on spectrophotometer method in the water such as the day water, all kinds of sewage and industrial waste water total phosphorus detect and obtain general employing, as GB " ammonium molybdate spectrophotometric method ".Compared with other analytical instrument (as gas chromatography, liquid chromatography), spectrophotometer does not have the device that can carry out the automatic sampler of continuous detecting operation.Therefore, need the test solution after to colour developing in color comparison tube to transfer to cuvette (material is glass or quartz), the mensuration of absorbance is carried out in the colorimetric room putting into spectrophotometer.Obviously, the drip washing of the cuvette done before each test solution detection is a loaded down with trivial details process consuming time.For the detection of batch sample, this step have impact on the efficiency of detection.For this reason, the total phosphorus detecting instrument that HACH company of the U.S. produces adopts same customization test tube to carry out clearing up and colorimetric detection thereupon, with the direct-detection of test solution absorbance after realizing developing the color.But the test tube of this kind of customization is not easily at laboratory popularity.Therefore, develop the detection that a kind of direct employing color comparison tube easily used on conventional spectrophotometer carries out absorbance, it is necessary for carrying out detecting analysis for batch samples.
Utility model content
The purpose of this utility model is to overcome the deficiency that above prior art exists, and provides that a kind of structure is simple, cost is low, can popularity application and the pick-up unit of total phosphorus content in the high quick detection water sample of accuracy.
In order to achieve the above object, the utility model is by the following technical solutions: the pick-up unit of total phosphorus content in a kind of quick detection water sample, comprise connect successively light source chamber, colorimetric room and sensing chamber, the both sides of described colorimetric room are provided with 2 light holes communicated with light source chamber and sensing chamber respectively; Also comprise color comparison tube and fixed mount, described fixed mount is installed on colorimetric indoor, and described color comparison tube inserts colorimetric room, and fixed mount is fixed in the bottom of color comparison tube; Meanwhile, 2 described light holes and color comparison tube are positioned at same straight line.
Preferably, the upper end open place of described colorimetric room is provided with capping, and described capping is provided with the patchhole inserting color comparison tube, and the upper end cover of described color comparison tube has shading sleeve.
Preferably, described fixed mount comprises base plate and fixed block, and described base plate is installed on the bottom surface of colorimetric indoor, and described fixed block is fixed on base plate, and described fixed block is provided with hole clipping, and hole clipping is inserted in the bottom of described color comparison tube.
Preferably, be provided with light source and monochromator in described light source chamber, described monochromator is between light source and light hole, and described light source, monochromator and be located along the same line by light.
Preferably, be provided with detecting device in described sensing chamber, this detecting device is just to light hole, and described detecting device is connected with display, and this display is installed on the outer wall of sensing chamber.
Adopt a detection method for the pick-up unit of total phosphorus content in above-mentioned quick detection water sample, comprise the following steps:
(1) slope value s is determined: configure one group of known total phosphorus content standard solution, be placed in color comparison tube and carry out spectral detection; Thus detect that to obtain in one group various standard solution be the absorbance of 400nm and 700nm at wavelength respectively, again with often kind of standard solution respectively in the wavelength difference that is the absorbance of 400nm and 700 for ordinate, again with the total phosphorus content of various standard solution for horizontal ordinate, form a coordinate axis; Then make fitting a straight line with the total phosphorus content of the difference of the absorbance at wavelength 400nm and 700nm and standard solution in coordinate axis, the slope value of gained straight line is s;
(2) sample pretreatment: getting volume is V 1water sample to be measured be placed in digestion tube, first water sample to be measured is added potassium persulfate solution, then closes digestion tube, then digestion tube is put the 20min ~ 40min that to be hydrolyzed at the temperature of 120 ± 2 DEG C, total phosphorus absorbance measurement in supplying water after cooling;
(3) light absorption value is detected: be drawn in color comparison tube by cooled water sample to be measured, and water sample to be measured is diluted, then add ascorbic acid and ammonium molybdate solution to the water sample to be measured after dilution, shake up rear standing 10min ~ 20min, the volume recording now water sample to be measured is V 2, then color comparison tube being inserted in colorimetric room fixing, after covering color comparison tube upper end, utilizing pick-up unit to detect water sample to be measured through the leaving standstill light absorption value A when two different wavelength of light 1and A 2;
(4) total phosphorus content is determined: according to data s, V in step (1), (2) and (3) 1, V 2, A 1and A 2, then obtain computing formula in conjunction with langbobier law:
c=(A 2-A 1)V 2/(sV 1),
The total phosphorus content c in water sample to be measured is obtained according to computing formula.
Preferably, in step (3), light absorption value A 1and A 2be record in 400nm and 700nm in wavelength of light respectively.
Preferably, in step (2), the volume of described potassium persulfate solution and concentration are respectively 4ml and 5%.
The utility model, relative to prior art, has following advantage and effect:
1, of the present utility model colorimetric room in existing spectrophotometer to be transformed, color comparison tube is utilized to instead of traditional cuvette, fixed mount is set in colorimetric indoor simultaneously, by fixed mount, color comparison tube is fixed on colorimetric indoor, this configuration reduces the drip washing operation before water sample detection to be measured, simplify detection operation, improve detection efficiency.
2, the utility model by arranging fixed mount in colorimetric room, and this fixed mount can fix general color comparison tube, and it is applied widely, easily applies in common lab.
3, in quick detection water sample of the present utility model, the pick-up unit of total phosphorus content can carry out batch testing, and its cost is low, and color comparison tube can directly in market buying, thus make this pick-up unit can apply at laboratory popularity.
When 4, utilizing the utility model pick-up unit to detect total phosphorus content, have employed double-wavelength method, namely detect the light absorption value at two different wave lengths, then obtain the total phosphorus content in water sample to be measured by langbobier law, this method is simple, and precision and accuracy high.
Accompanying drawing explanation
Fig. 1 is the structural representation of the pick-up unit of total phosphorus content in a kind of quick detection water sample.
Fig. 2 is spectrum spectrogram after the colour developing of standard phosphate solution.TP in Fig. 2 represents standard solution.
Fig. 3 is the graph of a relation of standard phosphate solution light absorption value and phosphoric acid solution concentration when optical wavelength is 700nm.
Fig. 4 is the graph of a relation of standard phosphate solution light absorption value and phosphoric acid solution concentration when dual wavelength.
Embodiment
For ease of it will be appreciated by those skilled in the art that the utility model is described in further detail below in conjunction with drawings and Examples.
As shown in Figure 1, detect fast the pick-up unit of total phosphorus content in water sample, comprise connect successively light source chamber 1, colorimetric room 2 and sensing chamber 3, the both sides of described colorimetric room 2 are provided with 2 light holes 4 communicated with light source chamber 1 and sensing chamber 3 respectively; Also comprise color comparison tube 5 and fixed mount 6, described fixed mount 6 is installed in colorimetric room 2, and described color comparison tube 5 inserts colorimetric room 2, and fixed mount 6 is fixed in the bottom of color comparison tube 5; Meanwhile, 2 described light holes 4 are positioned at same straight line with color comparison tube 5.Concrete, the monochromatic light that light source chamber 1 sends passes rear penetration ratio colour tube 5 from the light hole 4 between colorimetric room 2 and light source chamber 1, and then arrives in detecting device through the light hole 4 colorimetric room 2 and sensing chamber 3, thus completes the detection of light absorption value.And the both sides of described colorimetric room 2 are established and 2 light holes 4 communicated with light source chamber 1 and sensing chamber 3 respectively, in these 2 light holes, one is light well, another is light hole, namely the light hole 4 between colorimetric room 2 and light source chamber 1 is light well, and the light hole 4 between colorimetric room 2 and sensing chamber 3 is light hole.
The upper end open place of described colorimetric room 2 is provided with capping 7, and described capping 7 is provided with the patchhole 8 inserted by color comparison tube 5, and the upper end cover of described color comparison tube 5 has shading sleeve 9.Shading sleeve 9 can avoid extraneous light on the impact of testing result, improves accuracy of detection and accuracy.
Described fixed mount 6 comprises base plate 10 and fixed block 11, and described base plate 10 is installed on the bottom surface in colorimetric room 2, and described fixed block 11 is fixed on base plate 10, and described fixed block 11 is provided with hole clipping, and hole clipping is inserted in the bottom of described color comparison tube 5.This structure is simple, easy to operate, and the stability of fixing color comparison tube is strong.Concrete fixed mount 6 is adopted made of plastic.
For guarantee work is effectively carried out, be provided with light source 12 and monochromator 13 in described light source chamber 1, described monochromator 13 between light source 12 and light hole 4, namely, described monochromator 13 between light source 12 and light well, and described light source 12, monochromator 13 and by light be positioned at same directly on.
Be provided with detecting device 14 in described sensing chamber 3, this detecting device 14 is just to light hole 4, and described detecting device 14 is connected with display 15, and this display 15 is installed on the outer wall of sensing chamber 3.
Adopt a detection method for the pick-up unit of total phosphorus content in above-mentioned quick detection water sample, comprise the following steps:
(1) slope value s is determined: configure one group of known total phosphorus content standard solution, be placed in color comparison tube and carry out spectral detection; Thus detect that to obtain in one group various standard solution be the absorbance of 400nm and 700nm at wavelength respectively, again with often kind of standard solution respectively in the wavelength difference that is the absorbance of 400nm and 700 for ordinate, again with the total phosphorus content of various standard solution for horizontal ordinate, form a coordinate axis; Then make fitting a straight line with the total phosphorus content of the difference of the absorbance at wavelength 400nm and 700nm and standard solution in coordinate axis, the slope value of gained straight line is s;
(2) sample pretreatment: getting volume is V 1water sample to be measured be placed in digestion tube, first water sample to be measured is added potassium persulfate solution, then close digestion tube, then hydrolysis pipe is put the 20min ~ 40min that to be hydrolyzed at the temperature of 120 ± 2 DEG C, then the water sample to be measured in order hydrolysis pipe cools;
(3) light absorption value is detected: be drawn in color comparison tube by cooled water sample to be measured, and water sample to be measured is diluted, then add ascorbic acid and ammonium molybdate solution to the water sample to be measured after dilution, shake up rear standing 10min ~ 20min, the volume recording now water sample to be measured is V 2, then color comparison tube being inserted in colorimetric room fixing, after covering color comparison tube upper end, namely covers color comparison tube shading sleeve, utilizing pick-up unit to detect water sample to be measured through the leaving standstill light absorption value A when two different wavelength of light 1and A 2;
(4) total phosphorus content is determined: according to data s, V in step (1), (2) and (3) 1, V 2, A 1and A 2, then obtain computing formula in conjunction with langbobier law:
c=(A 2-A 1)V 2/(sV 1),
The total phosphorus content c in water sample to be measured is obtained according to computing formula.
Concrete, standard solution is placed in color comparison tube when carrying out spectral detection, obtain spectrogram as shown in Figure 2, each lines of Fig. 2 show absorbance is the absorbance that phosphorus concentration distinguishes the standard solution of 0.02mg/L, 0.04mg/L, 0.12mg/L, 0.2mg/L, 0.4mg/L, 0.6mg/L.Institute Fig. 3 and Fig. 4 is obtained again according to the institute's value in Fig. 2.Wherein, Fig. 3 is traditional direct color comparison pipe absorbance measurement, namely utilizes single wavelength, this wavelength be 700nm absorbance and and standard solution in the related coefficient of normal linearity curve between phosphorus concentration be only R 2=0.991, therefore traditional direct direct color comparison pipe absorbance measurement is the accurate quantitative analysis that can not realize total phosphorus content in sample; Utilizing double-wavelength method to obtain the related coefficient that wavelength is the normal linearity curve in 700nm absorbance and standard solution between phosphorus concentration in the utility model is R 2=0.999, therefore the method for the dual wavelength adopted in the utility model substantially improves the response relation of light absorption value to total phosphorus content, thus improve the accuracy rate detected.
In step (3), light absorption value A 1and A 2be record in 400nm and 700nm in wavelength of light respectively.
In step (2), the volume of described potassium persulfate solution and concentration are respectively 4ml and 5%.
When this pick-up unit detecting total phosphorus content in water sample fast carries out total phosphorus content detection to four kinds of water samples, the numerical value obtained is as following table 1:
The reappearance of table 1 method
RSD in table 1 is expressed as relative standard deviation.The reappearance that this speed detects the detection method replicate determination of the pick-up unit of total phosphorus content in water sample is fine, and relative standard deviation (RSD) is less than 0.85%, can meet the accurate requirement of spectrophotometry completely.
The numerical value that in quick detection water sample of the present utility model, the detection method of the pick-up unit of total phosphorus content detects water sample total phosphorus content and standard method to the contrast of the numerical value that water sample total phosphorus content detects as following table 2:
Table 2
From the data in above-mentioned table 2, detection method error of the present utility model is little, and accuracy is high.
Above-mentioned embodiment is preferred embodiment of the present utility model; can not limit the utility model; the any of other does not deviate from the technical solution of the utility model and the substitute mode of the change made or other equivalence, is included within protection domain of the present utility model.

Claims (5)

1. detect fast a pick-up unit for total phosphorus content in water sample, comprise connect successively light source chamber, colorimetric room and sensing chamber, the both sides of described colorimetric room are provided with 2 light holes communicated with light source chamber and sensing chamber respectively; It is characterized in that: also comprise color comparison tube and fixed mount, described fixed mount is installed on colorimetric indoor, and described color comparison tube inserts colorimetric room, and fixed mount is fixed in the bottom of color comparison tube; Meanwhile, 2 described light holes and color comparison tube are positioned at same straight line.
2. the pick-up unit of total phosphorus content in quick detection water sample according to claim 1, is characterized in that: the upper end open place of described colorimetric room is provided with capping, and described capping is provided with the patchhole inserting color comparison tube, and the upper end cover of described color comparison tube has shading sleeve.
3. the pick-up unit of total phosphorus content in quick detection water sample according to claim 1, it is characterized in that: described fixed mount comprises base plate and fixed block, described base plate is installed on the bottom surface of colorimetric indoor, described fixed block is fixed on base plate, described fixed block is provided with hole clipping, and hole clipping is inserted in the bottom of described color comparison tube.
4. the pick-up unit of total phosphorus content in quick detection water sample according to claim 1, it is characterized in that: in described light source chamber, be provided with light source and monochromator, described monochromator is between light source and light hole, and described light source, monochromator and be located along the same line by light.
5. the pick-up unit of total phosphorus content in quick detection water sample according to claim 1, it is characterized in that: be provided with detecting device in described sensing chamber, this detecting device is just to light hole, and described detecting device is connected with display, and this display is installed on the outer wall of sensing chamber.
CN201520553050.2U 2015-07-27 2015-07-27 Detection apparatus for total phosphorus content in short -term test water sample Expired - Fee Related CN204789319U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104964940A (en) * 2015-07-27 2015-10-07 珠江水利委员会珠江水利科学研究院 Detection device and method for rapidly detecting content of total phosphorus in water sample
CN109060692A (en) * 2018-09-13 2018-12-21 厦门大学 Active phosphorus automatic analyzer and its measuring method based on syringe pump

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104964940A (en) * 2015-07-27 2015-10-07 珠江水利委员会珠江水利科学研究院 Detection device and method for rapidly detecting content of total phosphorus in water sample
CN109060692A (en) * 2018-09-13 2018-12-21 厦门大学 Active phosphorus automatic analyzer and its measuring method based on syringe pump

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Granted publication date: 20151118

Termination date: 20160727