CN102374989A - Automatic analyzer for determining ammonia nitrogen in water and automatic analytic method thereof - Google Patents
Automatic analyzer for determining ammonia nitrogen in water and automatic analytic method thereof Download PDFInfo
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- CN102374989A CN102374989A CN2010102585492A CN201010258549A CN102374989A CN 102374989 A CN102374989 A CN 102374989A CN 2010102585492 A CN2010102585492 A CN 2010102585492A CN 201010258549 A CN201010258549 A CN 201010258549A CN 102374989 A CN102374989 A CN 102374989A
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Abstract
The invention relates to an automatic analyzer for determining the content of ammonia nitrogen in water and sewage through a flow injection colorimetric process and an automatic analytic method thereof. The automatic analyzer for determining the content of ammonia nitrogen in water and sewage comprises an automatic injection device, a peristaltic pump, a detector, and an online processing assembly, wherein the online processing assembly comprises a sample injection valve, braided reactors, three-way valves, a four-way valve, online heating modules, an online distillation module, an online degasser, and capillary connecting tubes. According to the automatic analyzer of the invention, samples can be continuously and automatically tested, the test speed is fast, fifty samples can be tested each hour, the test sensitivity is high, and the test accuracy is good; and according to the method of the invention, the liner range is 0.02-4.0mg/L, the liner correlation coefficient r is equal to or more than 0.999, the detection limit is 2.49mug/L, the standard addition recovery rate of practical water samples is 90-110%, the precision is high, and the repeatability is good.
Description
Technical field
The present invention relates to the automatical analysis of ammonia nitrogen in water and the sewage, the automatic analysis method of ammonia nitrogen in particularly a kind of automatic analyzer and water with ammonia nitrogen in the flow injection colorimetric method for determining water.
Background technology
Ammonia nitrogen exists with the form of free ammonia or ammonium salt in natural water, and both ratio of componentss depend on the pH value of water body.Its main source is that itrogenous organic substance receives microbial action to decompose generation in the sanitary sewage, also contains ammonia nitrogen in some industrial waste water.When ammonia-nitrogen content is higher in the water body, can produce eutrophication, the dissolved oxygen DO in the consume water causes the fish anoxia asphyxia in the water.Measure at present ammonia nitrogen and adopt manual analytical approach more, disturb morely, need distill pre-treatment, complex operation.
Flow Injection Analysis is simple, convenient with it, realize robotization and can the online characteristics that sample is carried out pre-treatment easily, is widely used in (Ruzicka J, Hansen E H in the chemical analysis at present; Flow Injection Analysis; Wiley, New York, 1981; Fang Zhaolun (Fang Zhaolun) .Flow injection analysis method (flow injection analysis) .Beijing (Beijing): Science Press (Science Press), 1999).Can use the method for flow injection (FI) to survey ammonia nitrogen, the online pre-treatment of sample, on-line determination, accuracy is high.
Summary of the invention
The object of the present invention is to provide a kind of mensuration sensitivity and accuracy high, and simple to operate, and analysis speed is fast, the automatic analytical instrument of ammonia nitrogen in water steady in a long-term and the sewage.
Another object of the present invention has provided the automatic analysis method of ammonia nitrogen in a kind of water.
The fully-automatic analyzer of ammonia nitrogen in a kind of water; Wherein, Comprise automatic sampling apparatus, peristaltic pump, online treatment assembly, detecting device, computer processing system; Automatic sampling apparatus comprises sample introduction needle; The online treatment assembly comprises sample fillup valve, online distillation module, three knitting reactor, two online degassers of online heating module of five threeways, and the sample fillup valve has A, B, C, D, E, six interfaces of F, and online distillation module has upper left mouthful of A, upper right mouth B, left end opening C, bottom right mouth D; Sample introduction needle links to each other through the capillary connecting pipe with the first peristaltic pump pump line, first threeway, first inlet successively; First threeway outlet links to each other through the capillary connecting pipe with the first online heating module, online distillation module left side end opening C successively, and online distillation module bottom right mouth D links to each other through the capillary connecting pipe with first back pressure regulator, waste liquid bottle successively, and the distilling reagent bottle links to each other through the capillary connecting pipe with the second peristaltic pump pump line, first threeway, second inlet successively; Sulfuric acid absorption liquid bottle links to each other through the capillary connecting pipe with the upper left A mouth of the 3rd peristaltic pump pump line, online distillation module successively; The upper right B mouth of online distillation module links to each other through the capillary connecting pipe with the interface F of online degasser, sample fillup valve successively; The interface B of sample fillup valve is connected with the two ends of sampling ring respectively with interface E; The interface D of sample fillup valve is communicated with the capillary connecting pipe with the 4th peristaltic pump pump line, current-carrying container bottle successively; The interface A of sample fillup valve links to each other through the capillary connecting pipe with waste liquid tank through second back pressure regulator; The interface C of sample fillup valve links to each other through the capillary connecting pipe with second threeway, first inlet; Second threeway outlet links to each other through the capillary connecting pipe with first knitting reactor, the 3rd threeway first inlet successively; The 3rd threeway outlet links to each other through the capillary connecting pipe with second knitting reactor, the 4th threeway inlet successively; The 4th threeway outlet links to each other through the capillary connecting pipe with the 3rd knitting reactor, the 5th threeway first inlet successively; The 5th threeway outlet successively with the second online heating module, detecting device in flow cell, the 3rd back pressure regulator, waste liquid tank be communicated with the capillary connecting pipe; Second threeway, second inlet is connected through the capillary connecting pipe with the 5th peristaltic pump pump line, buffer reagent container bottle successively, and second inlet of the 3rd threeway is connected through the capillary connecting pipe with the 6th peristaltic pump pump line, phenol sodium reagent container bottle successively, and the 4th threeway second inlet is connected through the capillary connecting pipe with the 7th peristaltic pump pump line, sodium nitroprusside reagent container bottle successively; Second inlet of the 5th threeway is connected through the capillary connecting pipe with the 8th peristaltic pump pump line, sodium hypochlorite reagent container bottle successively, and detecting device is connected with computer processing system through signal wire.
Automatic analyzer of the present invention; Wherein, online distillation module comprises] fixed block of shape, in the fixed block groove, be disposed with lower lock block, phase separation membrane, upper holder block and briquetting from lower to upper; On a wing plate of fixed block, bolt is installed; Bolt withstands briquetting, has groove at lower lock block and upper holder block and the contacted side of phase separation membrane, and the relative phase separation membrane symmetry of the groove of lower lock block, upper holder block is offered the stream that constitutes fluid; Both ends of the surface at lower lock block and upper holder block are provided with the threaded hole that communicates with groove, are respectively upper left mouthful of A, upper right mouth B, left end opening C, bottom right mouth D.
Automatic analyzer of the present invention, wherein, online distillation module stream form is shaped form, linear pattern or broken line type; The height of its stream is 0.5～3mm; The width of stream is 0.5～3mm, and the length of stream is 0.1～10m, and its material is chemically inert fluorine material.
Automatic analyzer of the present invention; Wherein, Online heating module comprises heating rod, is sleeved on the outer good aluminium body of heat transfer property of heating rod, is wrapped in the polytetrafluoroethylene capillary and the thermometric thermal resistance that form the reaction pipeline of online heating on the aluminium body; The thermometric thermal resistance is ceramic platinum resistance Pt100 or copper resistance Cu 50 etc., the external muff that is surrounded by of aluminium.
Automatic analyzer of the present invention, wherein, online degasser adopts the tubular membrane degassing, and the tubular membrane length of the tubular membrane degassing is 8-30cm.
Automatic analyzer of the present invention, wherein, the length capillaceous of first knitting reactor be 1-10m; The capillary pipe length of second knitting reactor is 1-9m; The capillary pipe length of the 3rd knitting reactor is 1-9m, and the length of capillary connecting pipe is 0.1-1m, and the length of sampling ring is 1-4m; Length capillaceous is 10-20m in the first online heating module, and length capillaceous is 10-20m in the second online heating module.
Automatic analyzer of the present invention, wherein, the light path of flow cell be 10～50mm.
The method of using the fully-automatic analyzer of ammonia nitrogen in a kind of water of the present invention to divide ammonia nitrogen in the bleed, wherein, step comprises:
(1) after filtering with sample; Utilizing automatic sampler that sample is sent into first threeway makes the sample that contains ammonia nitrogen mix with distilling reagent; Through online heating arrangement, ammonia gets into online distilling apparatus with gas form, and the ammonia that distills out is absorbed through online degasser by sulfuric acid absorption liquid and gets into sampling ring;
(2) current-carrying is released sample in the sampling ring and is mixed with buffer reagent;
(3) mixed solution of gained mixes with phenol sodium in the step (2);
(4) mixed solution of gained mixes with sodium nitroprusside in the step (3);
(5) mixed solution and the sodium hypochlorite reaction of gained in the step (4);
(6) colorimetric estimation is carried out at 600～700nm place in the online heating of mixed solution of the gained pond that circulates in the step (5), and institute's value transfers to computer processing system and calculates ammonia nitrogen value in the water.
The method of ammonia nitrogen in of the present invention minute bleed, wherein, current-carrying is a deionized water, and in the distilling reagent, the mass concentration of sodium borate decahydrate is 1-10g/L, and sodium hydroxide concentration is 0.1-10g/L, and in the sulfuric acid absorption liquid, the concentration of sulfuric acid is 0.1-10mL/L; In the phenol sodium solution, phenol sodium mass concentration is 10-100g/L, and sodium hydroxide concentration is 10-50g/L, and in the sodium hypochlorite reagent, the concentration of sodium hypochlorite is 100-550ml/L; In the damping fluid reagent, the mass concentration of ethylenediamine tetraacetic acid is 20-150g/L, and sodium hydroxide concentration is 5-50g/L; In the sodium nitroprusside reagent, the mass concentration of sodium nitroprusside is 1-10g/L, and sodium hydroxide concentration is 1-10g/L.
Beneficial effect of the present invention is: the principle that this analyser adopts flow injection to combine with the indophenol blue AAS; Removing the interference in the water body through an online distilling apparatus, so, can test sample continuously and automatically; Test speed is fast, and the sample determination frequency is 50 kinds/hour; That tests is highly sensitive, accuracy good; The range of linearity of method is 0.02～4.0mg/L, and linearly dependent coefficient r >=0.999 detects and is limited to 2.49 μ g/L, and the recovery of standard addition of actual water sample is 90%～110%; Precision is high, good reproducibility.
Description of drawings
Fig. 1 is the structure diagram of the automatic analyzer of ammonia nitrogen in the water provided by the invention;
Fig. 2 a is online distillation module diagram;
Fig. 2 b is the stream form that goes up lower lock block: shaped form;
The online heating module synoptic diagram of Fig. 3.
Embodiment
Further the present invention will be described through embodiment below.
The structure of the fully-automatic analyzer of ammonia nitrogen in the water of the present invention
The automatic analyzer of ammonia nitrogen in the water as shown in Figure 1, the flow cell 44 in the peristaltic pump pump line 12-19 in automatic sampling apparatus 1, the peristaltic pump 11, online treatment assembly, the detecting device 45 links to each other successively, and the light path of flow cell 28 is 10～50mm; Detecting device 45 is connected with computer processing system 47 through signal wire 46.
The online treatment assembly comprises:
(1) the sample fillup valve 31, and fillup valve 31 has A, B, C, D, E, six interfaces of F;
(2) online distillation module 23; Shown in Fig. 2 a, online distillation module 23 comprises] fixed block 56 of shape, in fixed block 56 grooves, be disposed with lower lock block 60, phase separation membrane 59, upper holder block 58 and briquetting 57 from lower to upper; On a wing plate of fixed block 42, bolt 55 is installed; Bolt 55 withstands briquetting 57, has groove in lower lock block 60 and upper holder block 58 and phase separation membrane 59 contacted sides, and relative phase separation membrane 59 symmetries of the groove of lower lock block 60, upper holder block 58 are offered the stream that constitutes fluid; Both ends of the surface at lower lock block 60 and upper holder block 58 are provided with the threaded hole that communicates with groove, are respectively upper left mouthful of A, upper right mouth B, left end opening C, bottom right mouth D; Shown in Fig. 2 b, online distillation module 23 stream forms are shaped form, and the height of its stream is 0.5～3mm, and the width of stream is 0.5～3mm, and the length of stream is 0.1～10m, and its material is chemically inert fluorine material;
(3) two online heating modules 21,43; As shown in Figure 3; Online heating module comprises heating rod 63, is sleeved on the good aluminium body 61 of heat transfer property outside the heating rod 63, is wrapped in the polytetrafluoroethylene capillary 65 and thermometric thermal resistance 62 of the reaction pipeline that forms online heating on the aluminium body 61; Thermometric thermal resistance 62 is ceramic platinum resistance Pt100 or copper resistance Cu 50 etc.; Aluminium body 61 is outer to be surrounded by that length capillaceous is 10-20m in muff 64, the first online heating modules 14, and length capillaceous is 10-20m in the second online heating module 27;
(4) three knitting reactor 37,39,41, the capillary pipe length of first knitting reactor 37 be 1-10m, the capillary pipe length of second knitting reactor 39 is 1-9m, the capillary pipe length of the 3rd knitting reactor 41 is 1-9m;
(5) five threeways 20,36,38,40,42;
(6) online degasser 25, online degasser 25 adopts the tubular membrane degassing, and the tubular membrane length of the tubular membrane degassing is 8-30cm;
(7) sampling ring 30, and its length is 1-4m;
(8) capillary connecting pipe, the length of capillary connecting pipe are 0.1-1m.
The sample introduction needle 2 of automatic sampling apparatus 1 links to each other through the capillary connecting pipe with the first peristaltic pump pump line 12, first threeway, 20 first inlets successively; First threeway 20 outlet links to each other through the capillary connecting pipe with the first online heating module 21, online distillation module 23 left end opening C successively; Online distillation module 23 bottom right mouth D link to each other through the capillary connecting pipe with first back pressure regulator 28, waste liquid bottle 51 successively, and distilling reagent bottle 4 links to each other through the capillary connecting pipe with the second peristaltic pump pump line 13, first threeway, 20 second inlets successively; Sulfuric acid absorption liquid bottle 5 links to each other through the capillary connecting pipe with the upper left A mouth of the 3rd peristaltic pump pump line 14, online distillation module 23 successively; The upper right B mouth of online distillation module 23 links to each other through the capillary connecting pipe with the interface F of online degasser 25, sample fillup valve 31 successively; The interface B of sample fillup valve 31 is connected with the two ends of sampling ring 30 respectively with interface E; The interface D of sample fillup valve 31 is communicated with the 4th peristaltic pump pump line 15, current-carrying container bottle 6 usefulness capillary connecting pipes successively; The interface A of sample fillup valve 31 links to each other through the capillary connecting pipe with waste liquid tank 51 through second back pressure regulator 33; The interface C of sample fillup valve 31 links to each other through capillary connecting pipe 35 with second threeway, 36 first inlets; Second threeway 36 outlet links to each other through the capillary connecting pipe with first knitting reactor 37, the 3rd threeway 38 first inlets successively; The 3rd threeway 38 outlet links to each other through the capillary connecting pipe with second knitting reactor 39, the 4th threeway 40 inlets successively; The 4th threeway 40 outlet links to each other through the capillary connecting pipe with the 3rd knitting reactor 41, the 5th threeway 42 first inlets successively; The 5th threeway 42 outlet is communicated with the second online heating module 43, flow cell 44, the 3rd back pressure regulator 49, waste liquid tank 51 usefulness capillary connecting pipes successively; Second threeway 36 second inlet is connected through the capillary connecting pipe with the 5th peristaltic pump pump line 16, buffer reagent container bottle 7 successively; Second inlet of the 3rd threeway 38 is connected through the capillary connecting pipe with the 6th peristaltic pump pump line 17, phenol sodium reagent container bottle 8 successively, and the 4th threeway 40 second enters the mouth successively and to be connected through the capillary connecting pipe with the 7th peristaltic pump pump line 18, sodium nitroprusside reagent container bottle 9, and second of the 5th threeway 42 enters the mouth successively and to be connected through the capillary connecting pipe with the 8th peristaltic pump pump line 19, sodium hypochlorite reagent container bottle 10.
The course of work of the fully-automatic analyzer of ammonia nitrogen in the water of the present invention:
Sample is mixed with distilling reagent 4 through first threeway 20 by automatic sampling apparatus 1 warp first pump line 12 under the effect of peristaltic pump 11, gets in the first online heating module 21; Sample and distilling reagent 4 are heated, and the gas-liquid mixed after the heating gets into online distillation module 23 mutually, and wherein ammonia carries out gas-liquid separation through the online distillation module 23 that has microporous membrane; Direct waste discharges get into waste liquid bottles 51 to liquid through first back pressure regulator 28 after through the reacting pipe of online distillation module 23; And ammonia gas is passed through microporous membrane, and ammonia gas is absorbed through the sulfuric acid absorption liquid 5 that the 3rd pump line 14 pumps into down by the effect by peristaltic pump 11, gets into online degasser 25; Get into six-way valve 31 after removing the bubble in the liquid; At this moment, when A interface and B interface connection, C interface and D interface connection, E interface and F interface are communicated with, be the sample introduction state; Liquid gets into sampling ring 30, and sampling ring is full of after the 33 direct waste discharges of second back pressure regulator get into waste liquid bottle 51.After sampling process finished, six-way valve 31 turned to the state shown in the dotted line among the figure, when A interface and F interface connection, B interface and C interface connection, D interface and E interface are communicated with; Be detected state, this moment, peristaltic pump 11 pumped into deionized water current-carrying solution 6, and the sample in the sampling ring 30 is released; In second threeway 36, converge with buffer solution 7, in first knitting reactor 37, mix, mixed solution converges with phenol sodium solution 8 in the 3rd threeway 38; In second knitting reactor 39, mix; Mixed solution converges with sodium nitroprusside solution 9 in the 4th threeway 40, in the 3rd knitting reactor 41, mixes, and mixed solution converges with time acid sodium solution 10 in the 5th threeway 42; Get into mixed liquor reacting by heating in the second line heating module 43; The pond 44 that circulates is carried out colorimetric estimation by detecting device 45 at 600～700nm place, and the liquid that flows out directly gets into waste liquid bottles 51 through the 3rd back pressure regulator 49.Colorimetric institute value transfers to computer processing system (47) and calculates ammonia nitrogen value in the water.
Standard solution and sample are poured into respectively in the sample hose of automatic sampling apparatus; The fully-automatic analyzer that starts ammonia nitrogen in the water can be analyzed automatically; Absorbance peak height or peak area according to the standard solution that writes down are done typical curve, and absorbance peak height value per sample or peak area value can calculate the content of ammoniacal nitrogen in the sample on typical curve.
Specify the course of work of using ammonia nitrogen in automatic analyzer test water of the present invention and the sewage below:
1, the preparation of standard specimen and reagent
11 sal-ammoniac standard reserving solution: 100mg/L: take by weighing 0.3819g sal-ammoniac NH
4Cl is transferred in the 1000ml volumetric flask after the water dissolving, and the nitrogen content of this standard solution is that 1.00ml contains 100.0 μ g nitrogen, is stored in the Brown Glass Brown glass bottles and jars only subsequent use.
1.2 with the ammonia nitrogen standard reserving solution with deionized water be mixed with 0.02,0.05,0.1,0.2,0.5,1.0,2.0 successively, the 4.0mg/L standard series.
1.3 in the distilling reagent, the mass concentration of sodium borate decahydrate is 4.76g/L, sodium hydroxide concentration is 0.272g/L.
1.4 in the absorption liquid, the concentration of sulfuric acid is 0.1mL/L.
1.5 in the damping fluid, the mass concentration of disodium ethylene diamine tetraacetate is 50.0g/L, sodium hydroxide concentration is 1.8mol/L.
1.6 in the developer, the mass concentration of phenol sodium is 83.0g/L, sodium hydroxide concentration is 32.0g/L.
1.7 in the sodium nitroprusside solution, the mass concentration of sodium nitroprusside is 3.5g/L, sodium hydroxide concentration is 5.5g/L.
1.8 among the liquor natrii hypochloritis, the volume ratio of sodium hypochlorite is 1: 1NaOCl effective chlorine 7-10%, sodium hydroxide concentration is 10.0g/L.
1.9 current-carrying is a deionized water.
Agents useful for same all adopts domestic reagent, and the purity of reagent is minimum pure for analyzing.
Adopt automatic analyzer shown in Figure 1 to test, shown in Fig. 2 b, online dialysis module adopts broken line type; The mechanical dimension head of stream * wide * height is 5m * 0.003m * 0.002m, and its material is PTFE, the phase separation membrane that it is used; The capillary inner diameter of stream is 0.6mm; The capillary pipe length of three knitting reactor 37,39,41 is 70cm in the online treatment assembly, and the length of other capillary connecting pipe is 0.5m, and the length of sampling ring 30 is 1.5m.The light path of flow cell is 10mm, and capillary pipe length is 6m in the first online heating module, and capillary pipe length is 6m in the second online heating module, measures at the 630nm place.
2, sample online treatment
Sample mixes 20 with distilling reagent in first threeway and mixes, and gets into the first online heating 21, and ammonia gets into online distilling apparatus 23 with gas form, and the ammonia that distills out is absorbed after online degasser 25 degassings by sulfuric acid absorption liquid through phase separation membrane and gets into sampling ring 30.
3, response measurement
Current-carrying is released the sample in the sampling ring 30, mixes in second threeway 36 with buffer reagent, and first knitting reactor 37 of flowing through is then further mixed; Mix with the phenol sodium reagent in the 3rd threeway 38 with the mixed test solution of buffer reagent; Further mixes through second knitting reactor 39, with the mixed test solution of phenol sodium reagent in the 4th threeway 40 and nitrous matrix sodium cyanide reagent mix, warp the 3rd knitting reactor 41 is further mixed; With test solution after the sodium nitroprusside reagent mix in the 5th threeway 42 and sodium hypochlorite reagent mix; Get into second online heating module 43 reacting by heating, the pond 44 that circulates is again detected, and the spectrogram of generation can be surveyed and drawn.The absorbance peak height value or the peak area value of standard solution according to record done typical curve, the content that on typical curve, calculates ammoniacal nitrogen according to the absorbance peak height value or the peak area value of sample.
The test result of table 1 standard model:
Table 1 result can prove that fully-automatic analyzer of the present invention and method can be surveyed the content of ammoniacal nitrogen accurately.
Above embodiment describes preferred implementation of the present invention; Be not that scope of the present invention is limited; Design under the prerequisite of spirit not breaking away from the present invention; Various distortion and improvement that those of ordinary skills make technical scheme of the present invention all should fall in the definite protection domain of claims of the present invention.
Claims (9)
1. the fully-automatic analyzer of ammonia nitrogen in the water; It is characterized in that; Comprise automatic sampling apparatus (1), peristaltic pump (11), online treatment assembly, detecting device (45), computer processing system (47); Said automatic sampling apparatus (1) comprises sample introduction needle (2); Said online treatment assembly comprises sample fillup valve (31), online distillation module (23), three knitting reactor (37,39,41), five threeways (20,36,38,40,42), two online heating modules (21,43), online degasser (25); Sample fillup valve (31) has A, B, C, D, E, six interfaces of F; Online distillation module (23) has upper left mouthful of A, upper right mouth B, left end opening C, bottom right mouth D; Sample introduction needle (2) links to each other through the capillary connecting pipe with the first peristaltic pump pump line (12), first threeway (20) first inlets successively; First threeway (20) outlet links to each other through the capillary connecting pipe with the first online heating module (21), the left end opening C of online distillation module (23) successively, and online distillation module (23) bottom right mouth D links to each other through the capillary connecting pipe with first back pressure regulator (28), waste liquid bottle (51) successively, and distilling reagent bottle (4) links to each other through the capillary connecting pipe with the second peristaltic pump pump line (13), first threeway (20) second inlets successively; Sulfuric acid absorption liquid bottle (5) links to each other through the capillary connecting pipe with the upper left A mouth of the 3rd peristaltic pump pump line (14), online distillation module (23) successively; The upper right B mouth of online distillation module (23) links to each other through the capillary connecting pipe with the interface F of online degasser (25), sample fillup valve (31) successively; The interface B of sample fillup valve (31) is connected with the two ends of sampling ring (30) respectively with interface E; The interface D of sample fillup valve (31) is communicated with the capillary connecting pipe with the 4th peristaltic pump pump line (15), current-carrying container bottle (6) successively; The interface A of sample fillup valve (31) links to each other through the capillary connecting pipe with waste liquid tank (51) through second back pressure regulator (33); The interface C of sample fillup valve (31) links to each other through capillary connecting pipe (35) with second threeway (36) first inlets; Second threeway (36) outlet links to each other through the capillary connecting pipe with first knitting reactor (37), the 3rd threeway (38) first inlets successively; The 3rd threeway (38) outlet links to each other through the capillary connecting pipe with second knitting reactor (39), the 4th threeway (40) inlet successively; The 4th threeway (40) outlet links to each other through the capillary connecting pipe with the 3rd knitting reactor (41), the 5th threeway (42) first inlets successively; The 5th threeway (42) outlet is communicated with the capillary connecting pipe with the second online heating module (43), interior flow cell (44), the 3rd back pressure regulator (49), the waste liquid tank (51) of detecting device (45) successively; Second threeway (36) second inlets are connected through the capillary connecting pipe with the 5th peristaltic pump pump line (16), buffer reagent container bottle (7) successively; Second inlet of the 3rd threeway (38) is connected through the capillary connecting pipe with the 6th peristaltic pump pump line (17), phenol sodium reagent container bottle (8) successively; The 4th threeway (40) second inlets are connected through the capillary connecting pipe with the 7th peristaltic pump pump line (18), sodium nitroprusside reagent container bottle (9) successively; Second inlet of the 5th threeway (42) is connected through the capillary connecting pipe with the 8th peristaltic pump pump line (19), sodium hypochlorite reagent container bottle (10) successively, and detecting device (45) is connected with computer processing system (47) through signal wire (46).
2. automatic analyzer as claimed in claim 1; It is characterized in that; Said online distillation module (23) comprises] fixed block (56) of shape; In fixed block (56) groove, be disposed with lower lock block (60), phase separation membrane (59), upper holder block (58) and briquetting (57) from lower to upper, on a wing plate of fixed block (42), bolt (55) be installed, bolt (55) withstands briquetting (57); Has groove at lower lock block (60) and upper holder block (58) with the contacted side of phase separation membrane (59); The relative phase separation membrane of groove (59) symmetry of lower lock block (60), upper holder block (58) is offered the stream that constitutes fluid, is provided with the threaded hole that communicates with groove in the both ends of the surface of lower lock block (60) and upper holder block (58), is respectively upper left mouthful of A, upper right mouth B, left end opening C, bottom right mouth D.
3. automatic analyzer as claimed in claim 2; It is characterized in that; Online distillation module (23) stream form is shaped form, linear pattern or broken line type, and the height of its stream is 0.5～3mm, and the width of stream is 0.5～3mm; The length of stream is 0.1～10m, and its material is chemically inert fluorine material.
4. automatic analyzer as claimed in claim 3; It is characterized in that; Said online heating module comprises heating rod (63), is sleeved on the outer good aluminium body of heat transfer property (61) of heating rod (63), is wrapped in polytetrafluoroethylene capillary (65) and thermometric thermal resistance (62) that aluminium body (61) is gone up the reaction pipeline that forms online heating; Said thermometric thermal resistance (62) is ceramic platinum resistance Pt100 or copper resistance Cu 50 etc., the outer muff (64) that is surrounded by of aluminium body (61).
5. automatic analyzer as claimed in claim 4 is characterized in that, said online degasser (25) adopts the tubular membrane degassing, and the tubular membrane length of the tubular membrane degassing is 8-30cm.
6. automatic analyzer as claimed in claim 5 is characterized in that, described first knitting reactor (37) length capillaceous is 1-10m; The capillary pipe length of second knitting reactor (39) is 1-9m; The capillary pipe length of the 3rd knitting reactor (41) is 1-9m, and the length of capillary connecting pipe is 0.1-1m, and the length of sampling ring (30) is 1-4m; Length capillaceous is 10-20m in the first online heating module (14), and length capillaceous is 10-20m in the second online heating module (27).
7. automatic analyzer as claimed in claim 6 is characterized in that, the light path of described flow cell (28) is 10～50mm.
8. the method for using the fully-automatic analyzer like ammonia nitrogen in any one water of claim 1 to 7 to divide ammonia nitrogen in the bleed is characterized in that step comprises:
(1) after filtering with sample; Utilizing automatic sampler that sample is sent into first threeway (20) makes the sample that contains ammonia nitrogen mix with distilling reagent; Through online heating arrangement (21); Ammonia gets into online distilling apparatus (23) with gas form, and the ammonia that distills out is absorbed through online degasser (25) by sulfuric acid absorption liquid and gets into sampling ring;
(2) current-carrying is released sample in the sampling ring and is mixed with buffer reagent;
(3) mixed solution of gained mixes with phenol sodium in the step (2);
(4) mixed solution of gained mixes with sodium nitroprusside in the step (3);
(5) mixed solution and the sodium hypochlorite reaction of gained in the step (4);
(6) colorimetric estimation is carried out at 600～700nm place in the online heating of mixed solution of the gained pond that circulates in the step (5), and institute's value transfers to computer processing system (47) and calculates ammonia nitrogen value in the water.
9. like the method for ammonia nitrogen in the claim 8 minute bleed; It is characterized in that said current-carrying is a deionized water, in the said distilling reagent; The mass concentration of sodium borate decahydrate is 1-10g/L; Sodium hydroxide concentration is 0.1-10g/L, and in the said sulfuric acid absorption liquid, the concentration of sulfuric acid is 0.1-10mL/L; In the said phenol sodium solution, phenol sodium mass concentration is 10-100g/L, and sodium hydroxide concentration is 10-50g/L, and in the said sodium hypochlorite reagent, the concentration of sodium hypochlorite is 100-550ml/L; In the said damping fluid reagent, the mass concentration of ethylenediamine tetraacetic acid is 20-150g/L, and sodium hydroxide concentration is 5-50g/L; In the said sodium nitroprusside reagent, the mass concentration of sodium nitroprusside is 1-10g/L, and sodium hydroxide concentration is 1-10g/L.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010102585492A CN102374989A (en) | 2010-08-20 | 2010-08-20 | Automatic analyzer for determining ammonia nitrogen in water and automatic analytic method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010102585492A CN102374989A (en) | 2010-08-20 | 2010-08-20 | Automatic analyzer for determining ammonia nitrogen in water and automatic analytic method thereof |
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| CN102374989A true CN102374989A (en) | 2012-03-14 |
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| CN102734529A (en) * | 2012-07-13 | 2012-10-17 | 深圳市理邦精密仪器股份有限公司 | Linkage control device and blood gas analyzer adopting same |
| CN103048481A (en) * | 2013-01-17 | 2013-04-17 | 北京吉天仪器有限公司 | Automatic analyzer for detecting ammonia nitrogen in environmental water and method for detecting ammonia nitrogen in environmental water |
| CN103376239A (en) * | 2012-04-12 | 2013-10-30 | 株式会社岛津制作所 | Injection pump type ammonia nitrogen analyzer |
| CN103592413A (en) * | 2013-11-08 | 2014-02-19 | 山东益源环保科技有限公司 | Reagent and method for quickly testing content of ammonia and nitrogen in water sample |
| CN104360090A (en) * | 2014-11-13 | 2015-02-18 | 北京吉天仪器有限公司 | Automatic soil analyzer and method for measuring trace elements in soil by using automatic soil analyzer |
| CN105510325A (en) * | 2015-12-08 | 2016-04-20 | 浙江省嘉兴市农业科学研究院（所） | Semiquantitative determination method of concentration of ammonium nitrogen in agricultural biogas fluid |
| CN107024441A (en) * | 2017-05-03 | 2017-08-08 | 厦门大学 | The assay method of ammonia-nitrogen content a kind of water body suitable for different salinity |
| CN108444994A (en) * | 2018-03-18 | 2018-08-24 | 北京宝德仪器有限公司 | The automatic analysing apparatus and method of formaldehyde in water |
| CN108732162A (en) * | 2018-05-29 | 2018-11-02 | 四川理工学院 | The device for fast detecting and detection method of arsenic concentration in a kind of water |
| CN108872420A (en) * | 2018-05-18 | 2018-11-23 | 同济大学 | A kind of instrument and method detecting soluble organic nitrogen |
| CN109342159A (en) * | 2018-09-30 | 2019-02-15 | 中国科学院水生生物研究所 | A kind of separation of close and distant water component and collection device and method based on on-line checking |
| CN115784456A (en) * | 2022-12-02 | 2023-03-14 | 江南大学 | Application of sodium nitroprusside in improving purification of eutrophic water body by water hyacinth |
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| CN103376239A (en) * | 2012-04-12 | 2013-10-30 | 株式会社岛津制作所 | Injection pump type ammonia nitrogen analyzer |
| CN102734529A (en) * | 2012-07-13 | 2012-10-17 | 深圳市理邦精密仪器股份有限公司 | Linkage control device and blood gas analyzer adopting same |
| CN103048481A (en) * | 2013-01-17 | 2013-04-17 | 北京吉天仪器有限公司 | Automatic analyzer for detecting ammonia nitrogen in environmental water and method for detecting ammonia nitrogen in environmental water |
| CN103048481B (en) * | 2013-01-17 | 2013-12-04 | 北京吉天仪器有限公司 | Automatic analyzer for detecting ammonia nitrogen in environmental water and method for detecting ammonia nitrogen in environmental water |
| CN103592413A (en) * | 2013-11-08 | 2014-02-19 | 山东益源环保科技有限公司 | Reagent and method for quickly testing content of ammonia and nitrogen in water sample |
| CN104360090A (en) * | 2014-11-13 | 2015-02-18 | 北京吉天仪器有限公司 | Automatic soil analyzer and method for measuring trace elements in soil by using automatic soil analyzer |
| CN104360090B (en) * | 2014-11-13 | 2016-03-02 | 北京吉天仪器有限公司 | Soil automatic analyzer and the method with this analysis-e/or determining Trace Elements in Soil |
| CN105510325A (en) * | 2015-12-08 | 2016-04-20 | 浙江省嘉兴市农业科学研究院（所） | Semiquantitative determination method of concentration of ammonium nitrogen in agricultural biogas fluid |
| CN107024441A (en) * | 2017-05-03 | 2017-08-08 | 厦门大学 | The assay method of ammonia-nitrogen content a kind of water body suitable for different salinity |
| CN107024441B (en) * | 2017-05-03 | 2019-06-14 | 厦门大学 | A kind of measuring method of the ammonia-nitrogen content suitable for different salinity water body |
| CN108444994A (en) * | 2018-03-18 | 2018-08-24 | 北京宝德仪器有限公司 | The automatic analysing apparatus and method of formaldehyde in water |
| CN108444994B (en) * | 2018-03-18 | 2021-11-05 | 北京宝德仪器有限公司 | Automatic analysis device and method for formaldehyde in water |
| CN108872420A (en) * | 2018-05-18 | 2018-11-23 | 同济大学 | A kind of instrument and method detecting soluble organic nitrogen |
| CN108872420B (en) * | 2018-05-18 | 2019-06-11 | 同济大学 | A kind of instrument and method detecting soluble organic nitrogen |
| CN108732162A (en) * | 2018-05-29 | 2018-11-02 | 四川理工学院 | The device for fast detecting and detection method of arsenic concentration in a kind of water |
| CN109342159A (en) * | 2018-09-30 | 2019-02-15 | 中国科学院水生生物研究所 | A kind of separation of close and distant water component and collection device and method based on on-line checking |
| CN115784456A (en) * | 2022-12-02 | 2023-03-14 | 江南大学 | Application of sodium nitroprusside in improving purification of eutrophic water body by water hyacinth |
| CN115784456B (en) * | 2022-12-02 | 2023-08-25 | 江南大学 | Application of sodium nitroprusside in improving purification of eutrophic water body of water hyacinth |
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