CN102411001A - Method for rapid detection of hexavalent chromium ions in sewage - Google Patents

Method for rapid detection of hexavalent chromium ions in sewage Download PDF

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Publication number
CN102411001A
CN102411001A CN2011102255942A CN201110225594A CN102411001A CN 102411001 A CN102411001 A CN 102411001A CN 2011102255942 A CN2011102255942 A CN 2011102255942A CN 201110225594 A CN201110225594 A CN 201110225594A CN 102411001 A CN102411001 A CN 102411001A
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hexavalent chromium
detection
water
add
standard
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CN2011102255942A
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高鹏文
张剑锋
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Shandong Foreign Exchange Cai Gang Co Ltd
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Shandong Foreign Exchange Cai Gang Co Ltd
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Priority to CN2011102255942A priority Critical patent/CN102411001A/en
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Abstract

The invention specifically relates to a method for rapid detection of hexavalent chromium ions in sewage, which belongs to the field of detection of metal ions. The method comprises the following steps: adding 100 ml of distilled water or deionized water into a wash bottle; sequentially adding 1 ml of 1+1 sulfuric acid and 1 ml of 1+1 phosphoric acid and shaking up an obtained mixture; adding 4 ml of a prepared diphenylcarbazide solution and shaking up an obtained mixture; adding 100 ml of distilled water or deionized water and shaking up an obtained mixture for usage in subsequent detection; taking 2 to 5 ml of a water sample to be detected, adding 2 to 5 ml of a hexavalent chromium ion detection reagent with a wash bottle, shaking up an obtained mixture, observing the color of mixed liquor and determining the range of the content of chromium ions in detection liquid by observing whether the mixed liquor has a color or by observing the color which the mixed liquor displays. Application of the method provided in the invention for detection of hexavalent chromium ions enables detection time to be saved and on-site detection to be realizable; the method has the advantages of simpleness, easy operation and strong practicality.

Description

The method of hexavalent chromium in a kind of fast detecting sewage
Technical field
[0001] the invention belongs to the metal ion detection field, be specifically related to the method for hexavalent chromium in a kind of fast detecting sewage.
Background technology
In testing process to sewage; Whether the hexavalent chromium that can detect usually in the sewage exceeds standard, and the detection method in common for hexavalent chromium is the method GB7467-87 of national standard at present, this method ability detection by quantitative; But adopt the required consumed time of this method to be about 30min~60min; And in the production run of reality, to the sewage detection at scene the time, only need carry out qualitative detection to the hexavalent chromium in the sewage; And often need when detecting at the scene will obtain testing result at short notice, so the method for national standard is applicable to that not too on-site qualitative detects.Particularly for the sewage-treatment plant of continuous operation, abnormal conditions all might take place at any time.Utilize national standard method monitoring sewage-treatment plant operation conditions; Be difficult to timely unusual circumstance; Because utilize national standard method; Generally need 40 minutes from sampling, sample preparation, dosing set by step, standing and reacting, start detection, cleaning apparatus etc., if operating personnel are unfamiliar with the flow process of the whole series, the time of detection can be longer.In the long time interval, in case take place will pollute water body in many ways unusually, the operation of processing and recovery device needs 4 hours, the wasting manpower and material resources at least again.In more than 4 hours time, sewage-treatment plant can not be disposed of sewage, and must handle the water that pollutes pumpback again, has increased the burden of sewage-treatment plant.In addition, national standard method needs instrument, and operating personnel are inconvenient to be with instrument to do detection to the scene, also is a big defective.
Summary of the invention
In order to solve above-mentioned technical matters, the invention provides the method for hexavalent chromium in a kind of ability fast detecting sewage.
The method of hexavalent chromium comprises following step in a kind of fast detecting sewage of the present invention:
(1) preparation or reagent preparation: the 1+1 phosphoric acid solution, mix phosphoric acid with the water equal-volume; The 1+1 sulfuric acid solution mixes sulfuric acid with the water equal-volume; Distilled water or deionized water; Acetone; Developer: diphenylcarbazide solution, take by weighing diphenylcarbazide 0.2g and be dissolved in the 50mL acetone, thin up shakes up to 100mL, stores in the brown bottle, places refrigerator to preserve;
(2) preparation detectable: in wash bottle, add 100ml distilled water or deionized water; Add the 1+1 sulfuric acid of 1ml and the 1+1 phosphoric acid of 1ml more successively, shake up; Add the diphenylcarbazide solution that 4ml prepares afterwards, shake up; Add 100ml distilled water or deionized water at last, shake up, get detectable, use when to be detected;
(3) test samples: get 2~5ml water sample to be measured in container, in container, add 2~5ml detectable, mix shaking up with water sample to be measured fully, observe the color of mixed liquor;
(4) colorimetric reading: the red standard colour chart plate of mixed liquor and concentration known is compared, confirm the content range of hexavalent chromium; The standard colour chart plate of described concentration known is that the standard hexavalent chromium solution that points to the known variable concentrations of preparation adds above-mentioned detectable respectively, the red Standard Colors that is shown behind the constant volume is used digital brain printing technology process red accurately standard colour chart plate.
The standard colour chart plate of making has replaced the hexavalent chromium solution of standard, will the value of limiting the quantity of and important concentration value make standard colour chart and can reduce experimental work amount and reagent contamination, and can grasp the concentration range of hexavalent chromium, be particularly suitable for field quick detection.
Beneficial effect of the present invention is:
(1) practice thrift detection time, detecting the hexavalent chromium required time by the method in the national standard is 30min~60min, and method of the present invention just can detect the approximate range that whether contains hexavalent chromium and content of chromium ion within 2 minutes;
(2) be to carry out at the scene sewage detection often,, need using the instrument in the various laboratories, and these instruments are not easy to move to the scene and operate if adopt the method for national standard to detect; The present invention need not carry instrument, only need carry reagent, just can detect at any time at the scene; By contrast, method of the present invention is simple, easy operating, and is practical;
(3) the required reagent of method of the present invention is few, and the reagent of using in the GB is far away more than the reagent among the present invention, and therefore cost of the present invention is lower.
Description of drawings
Fig. 1 is the standard colour chart plate of 0.1 μ g/ml for the concentration of hexavalent chromium of the present invention;
Fig. 2 is the standard colour chart plate of 0.2 μ g/ml for the concentration of hexavalent chromium of the present invention.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done explanation further,, but therefore do not limit the present invention so that those skilled in the art more understands the present invention.
Embodiment 1
(1) preparation or reagent preparation: the 1+1 phosphoric acid solution, mix phosphoric acid with the water equal-volume; The 1+1 sulfuric acid solution mixes sulfuric acid with the water equal-volume; Distilled water or deionized water; Acetone; Developer: diphenylcarbazide solution, take by weighing diphenylcarbazide 0.2g and be dissolved in the 50mL acetone, thin up shakes up to 100mL, stores in the brown bottle, places refrigerator to preserve;
(2) preparation detectable: in wash bottle, add 100ml distilled water or deionized water; Add the 1+1 sulfuric acid of 1ml and the 1+1 phosphoric acid of 1ml more successively, shake up; Add the diphenylcarbazide solution that 4ml prepares afterwards, shake up; Add 100ml distilled water or deionized water at last, shake up, get detectable, use when to be detected;
(3) test samples: get 3ml water sample to be measured in container, in container, add the 3ml detectable, mix shaking up with water sample to be measured fully, observe the color of mixed liquor;
(4) colorimetric reading: the red standard colour chart plate of mixed liquor and concentration known is compared, confirm the content range of hexavalent chromium; The standard colour chart plate of described concentration known is that the standard hexavalent chromium solution that points to the known variable concentrations of preparation adds above-mentioned detectable respectively, the red Standard Colors that is shown behind the constant volume is used digital brain printing technology process red accurately standard colour chart plate.
Be to be that the Standard Colors that hexavalent chromium showed of 0.1 μ g/ml and 0.2 μ g/ml adopts digital brain printing technology to process red accurately standard colour chart plate in the present embodiment according to being mixed with concentration.
Certainly; In the actual detection process; The standard colour chart plate can be prepared the standard solution of the hexavalent chromium of variable concentrations as required; As be mixed with concentration be 0.15 μ g/ml, 0.25 μ g/ml, 0.3 μ g/ml the hexavalent chromium standard solution, produce the chromatosheet that corresponding hexavalent chromium concentration is 0.15 μ g/ml, 0.25 μ g/ml, 0.3 μ g/ml according to their color that is shown.
Reference examples 1
Adopt the method among the standard GB 7467-87 that the similar detection sample is detected.
? The present invention Reference examples 1
Detection time/min 2 40
Required instrument Do not have Spectrophotometer
Hexavalent chromium concentration μ g/ml 0.1~0.2 0.18 。
Embodiment 2
Be that with the difference of embodiment 1 water sample of being got among the embodiment 2 is different with embodiment 1, other is identical.
Reference examples 2
Adopt the method among the standard GB 7467-87 that the similar detection sample is detected.
? The present invention Reference examples 1
Detection time/min 1 45
Required instrument Do not have Spectrophotometer
Hexavalent chromium concentration μ g/ml 0.1 below 0.07 。

Claims (1)

1. the method for hexavalent chromium in the fast detecting sewage comprises following step:
(1) preparation or reagent preparation: the 1+1 phosphoric acid solution, mix phosphoric acid with the water equal-volume; The 1+1 sulfuric acid solution mixes sulfuric acid with the water equal-volume; Distilled water or deionized water; Acetone; Developer: diphenylcarbazide solution, take by weighing diphenylcarbazide 0.2g and be dissolved in the 50mL acetone, thin up shakes up to 100mL, stores in the brown bottle, places refrigerator to preserve;
(2) preparation detectable: in wash bottle, add 100ml distilled water or deionized water; Add the 1+1 sulfuric acid of 1ml and the 1+1 phosphoric acid of 1ml more successively, shake up; Add the diphenylcarbazide solution that 4ml prepares afterwards, shake up; Add 100ml distilled water or deionized water at last, shake up, get detectable, use when to be detected;
(3) test samples: get 2~5ml water sample to be measured in container, in container, add 2~5ml detectable, mix shaking up with water sample to be measured fully, observe the color of mixed liquor;
(4) colorimetric reading: the red standard colour chart plate of mixed liquor and concentration known is compared, confirm the content range of hexavalent chromium; The standard colour chart plate of described concentration known is that the standard hexavalent chromium solution that points to the known variable concentrations of preparation adds above-mentioned detectable respectively, the red Standard Colors that is shown behind the constant volume is used digital brain printing technology process red accurately standard colour chart plate.
CN2011102255942A 2011-08-08 2011-08-08 Method for rapid detection of hexavalent chromium ions in sewage Pending CN102411001A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104165885A (en) * 2014-07-16 2014-11-26 安徽省三方耐磨股份有限公司 Rapid analysis method of chromium element of wear resistant ball
CN105424686A (en) * 2015-11-10 2016-03-23 广东环凯微生物科技有限公司 Rapid total chromium concentration detecting reagent and method
CN105466738A (en) * 2014-08-26 2016-04-06 广州市怡文环境科技股份有限公司 Chemical sample preparation method for testing trace quantity of elemental chromium in soil and sewage
CN105823745A (en) * 2016-03-24 2016-08-03 哈尔滨工业大学 On-site emergency detection reagent for chromium in water and use method thereof
CN106092921A (en) * 2016-05-31 2016-11-09 无锡伊佩克科技有限公司 The detection method of hexavalent chromium content in a kind of passivating solution
CN106770249A (en) * 2016-12-28 2017-05-31 云南昆钢水净化科技有限公司 A kind of water quality Cr VI mixed color developing agent and its compound method
CN113138188A (en) * 2021-04-21 2021-07-20 江门蓝湖污水处理有限公司 Preparation and rapid detection method of heavy metal and cyanide detection reagent pack

Citations (1)

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CN1501066A (en) * 2002-11-18 2004-06-02 上海师范大学 Test piece for detecting hexavalent chromium and preparing method thereof

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CN1501066A (en) * 2002-11-18 2004-06-02 上海师范大学 Test piece for detecting hexavalent chromium and preparing method thereof

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104165885A (en) * 2014-07-16 2014-11-26 安徽省三方耐磨股份有限公司 Rapid analysis method of chromium element of wear resistant ball
CN105466738A (en) * 2014-08-26 2016-04-06 广州市怡文环境科技股份有限公司 Chemical sample preparation method for testing trace quantity of elemental chromium in soil and sewage
CN105424686A (en) * 2015-11-10 2016-03-23 广东环凯微生物科技有限公司 Rapid total chromium concentration detecting reagent and method
CN105424686B (en) * 2015-11-10 2018-10-12 广东环凯微生物科技有限公司 A kind of total chromium concn quick detection reagent and detection method
CN105823745A (en) * 2016-03-24 2016-08-03 哈尔滨工业大学 On-site emergency detection reagent for chromium in water and use method thereof
CN105823745B (en) * 2016-03-24 2018-07-17 哈尔滨工业大学 Chromium scene Emergent detection reagent and its application method in a kind of water body
CN106092921A (en) * 2016-05-31 2016-11-09 无锡伊佩克科技有限公司 The detection method of hexavalent chromium content in a kind of passivating solution
CN106770249A (en) * 2016-12-28 2017-05-31 云南昆钢水净化科技有限公司 A kind of water quality Cr VI mixed color developing agent and its compound method
CN113138188A (en) * 2021-04-21 2021-07-20 江门蓝湖污水处理有限公司 Preparation and rapid detection method of heavy metal and cyanide detection reagent pack

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Application publication date: 20120411