CN101923049A - Quick detection of nickel plating waste water in production before discharge - Google Patents

Abstract

The invention relates to a test method which uses a special reagent (dimethyl glyoxime) to analyze a specific metal ion (nickel) for identifying the content phase of the nickel ion in a waste liquid and finally judging whether the content phase is in an allowable standard section. Compared with a common flame atomic absorption spectrophotometric method, the method has the characteristics of simplicity, practicability and economy. The technique is particularly suitable for standards detection of waste water in medium and small electronickelling industries before discharge, and belongs to the environmental protection scope. The method adopts the principle that the dimethyl glyoxime is both a color developing agent and a precipitant for the nickel ion. The detection method comprises the step of comparing a detection result with a segment standard sample to judge the content range of the nickel ion. The method has the technical points that 1. the pH value of a liquid to be detected is 7.5-8.0 preferably; and 2. after being mixed in a colorimetric tube, the color developing agent and the liquid to be detected need to be shaken for more than 200 times continuously to develop color as quickly as possible so as to compare with a standard sample.

Description

Aborning fast detecting before the nickel-plating waste water discharging

One, technical field: the environmental protection of electroplating (casting) industry production

Two, suitable application area: the wastewater treatment of industrial electro nickel plating detects

Three, background technology

Nickel-plating waste water discharging detection method generally adopts atomic absorption spectrophotometry to detect, and the method is with high content of technology, and expense is big, (one-time detection need 4000 surplus yuan) is uneconomical; General enterprise does not possess testing conditions, can not realize timely detection.New detection method has well solved this problem.

Four, Fa Ming motivation and result

Hebei province's Zhuozhou City three ring textile equipment company limiteds that I am employed are the whole nation nearly 50 professional production textile printing and dyeings one of producers bigger in the printed nickel net.This factory produces per year surplus printed nickel net 100,000, and ton surplus the 1# nickel 100 is separated in a year power consumption, 10 of 1000L nickel baths is arranged, 5 of 1500L nickel baths.Detected the discharge of wastewater severe overweight by environmental administration in 2004, if this problem does not solve the danger that enterprise faces closure.For this reason, we have visited many colleagues enterprise business organization, and visited Hebei province's Environmental Science Institute, and they have proposed the new concept of recycling economy, cleaner production, this theory is implemented in my unit, thereby makes the heavy metal in the water---and nickel ion content reduces greatly.Companies in 2005 have carried out the sewage water treatment method and the detection method up to standard of my invention again, and succeed, thereby authorized cleaner production demonstration enterprise by higher level department, and become sewage discharge enterprise up to standard, my invention moved 5 years continuously extremely now from 2005, and up to standard every year.Through higher level specialized department selective examination, detect with atomic absorption spectrophotometry, 5 years maximal values of outer draining are 0.27mg/L, (the national standard permissible value is 1mg/L), enterprise is survived like this, and has created condition for sustainable development.

Five, summary of the invention:

Aborning fast detecting before the nickel-plating waste water discharging

1, test item: the judgement that the nickel plating wastewater disposition is up to standard

2, test philosophy: dimethylglyoxime promptly is a developer to nickel ion in assay, also is organic precipitant, or extractant.Utilize developer to carry out the segmentation contrast to determine that it is below certain section content to nickel ion content and standard specimen in the solution; Utilize its final quantity that continues precipitation to carry out the segmentation contrast, just declare the result to verify its colour developing back.Facts have proved that the two was practical in conjunction with judging in the detection of producing in 5 years

3, detection method, principle and explanation:

Owing to be detection up to standard,, be qualified as long as can affirm in standard-required value section with regard to decidable so the detection method that adopts is non-accurate sizing technique.Block several sections at certain again below the section, be judged to be certain section with next can tell again excellent (matter), good (good), can class such as (qualified).Because concrete my Zhuozhou City three of institute's inventive method of implementing encircles the relatively good of textile equipment company limiteds nickel-plating waste waters processing.What carry out is to be qualified away from the bigger 0.5mg/L of standard value 1mg/L.Increase by 1 0.3mg/L again for good following.If other enterprises or unit relax this method of employing, as being fully passable between＞1mg/L～0.5mg/L.

4, reagent and key instrument:

Reagent: 0.2% dimethylglyoxime solution

The reagent compound method: claim 0.2g with analytical balance, dimethylglyoxime adds water 100ml, gets final product after the heated and boiled.

Instrument: one on the special-purpose frame of color comparison tube that has six color comparison tubes.

5, analyze preceding preliminary work:

1., configuration detection reagent

2., the reagent calibration is equipped with and the test solution preparation

The titer of a, preparation 0.3mg/L: get nickelous sulfate 150mg (nickeliferous 30mg), be dissolved in the 1L pure water, get this solution 5ml and be dissolved in the 500ml dissolve measuring bottle, this solution then is 0.3mg/L.It is standby to the 100ml position afterwards this liquid to be taken into the 100ml color comparison tube

B, prepare the titer of 0.5mg/L: get nickelous sulfate 250mg (nickeliferous 50mg), be dissolved in the 1L pure water, get this solution 5ml and be dissolved in the 500ml volumetric flask, this solution then is 0.5mg/L, after the 100ml color comparison tube of packing into standby to the 100ml position

C, get handle back water one plastic cup (about 500～600m1), the 100ml color comparison tube of packing into is to the 100ml position, adorn altogether two standby

6, analyze contrast:

Get one of 0.3mg/L titer color comparison tube, transfer pH value to 7.5～8 after, add dimethylglyoxime reagent 3～5ml after, add a cover and insert in the colorimetric shelf after shaking 200～300 times; Get to be equipped with and handle one of back water color comparison tube, add dimethylglyoxime 3～5ml after transferring pH value 7.5～8, also insert in the Colorimetric cylinder holder after shaking 200～300 times after adding a cover and compare, quite or more develop the color shallow with the titer color with the titer pipe.Be judged to≤0.3mg/L, then do the 0.5mg/L standard specimen with the liquid sample quite contrasts when heavy with said method as look, as liquid sample and standard specimen quite or summary look shallow is≤0.5mg/L; Look then is defective when heavy.Control methods is: at first observe contrast from horizontal direction, and then look down directly over color comparison tube, further contrast.The above-mentioned observation for first step colourity contrasts, substantially like this, just can determine its paragraph scope, in order further to determine, can further observe again, Here it is: the liquid in the color comparison tube is continued to leave standstill a period of time in color comparison tube, treat that heavy wadding thing precipitates fully substantially, and after concentrating on the bottom, also can sink what the contrast of wadding thing, more can further determine its judgement.If will precipitate with after ashless filter paper filtration, the dry also calcination, can get the actual weight of nickel.

7, the concrete image of comparative analysis visible " Figure of description "-test nickeliferous sewage figure with colourimetry.

8, the point that should note:

A, the liquid pH value when judging colourity are 7.5～8.5 better.Because this value is outstanding fast.

Can directly dissolve when b, preparation dimethylglyoxime solution, needn't add ethanol again, directly the solution after the heating can directly use, needn't use filter paper filtering again, because of the chelate molecule of dimethylglyoxime and the generation of Ni++ ionic reaction is big, not handy on the contrary after the filtration, even can not use.

Six, description of drawings:

Fig. 1 tests nickeliferous sewage figure with colourimetry.Code name is among its figure:

1. be color comparison tube; 2. be pipe close; 3. be reflex reflector lens; 4. be wallboard; 5. be crossbeam; 6. be base plate.

1., a 2. ratio of components colour tube complete set, be outsourcing piece; 3.-6. being the Colorimetric cylinder holder assembly, also is outsourcing piece

Seven, embodiment:

The method Hebei province's Zhuozhou City three ring textile equipment company limiteds implement 5 years respond well and up to standard every year.The existing whole nation also has nearly 50 families with the product industry, and this patent is once ratifying again to its popularization.Other electronickelling industries can be adopted equally.

Claims (3)

1. principle one dimethylglyoxime of fast detecting is developer, precipitation agent to nickel ion.

2. detection method:

A, the non-accurately quantitative card piecewise analysis determining method of employing

B, detection nickel ion are analyzed the operational process of craft of pairing comparision

C, technical essential: the best pH value of side colourity and dimethylglyoxime reagent join method

3. Figure of description.

Images