CN106546587A - A kind of water sample trace lead quick detection kit - Google Patents
A kind of water sample trace lead quick detection kit Download PDFInfo
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- CN106546587A CN106546587A CN201710069317.4A CN201710069317A CN106546587A CN 106546587 A CN106546587 A CN 106546587A CN 201710069317 A CN201710069317 A CN 201710069317A CN 106546587 A CN106546587 A CN 106546587A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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Abstract
The invention discloses a kind of water sample trace lead quick detection reagent, which includes：Trace lead detectable, trace lead standard color card and some consumptive materials, independently pack, then jointly loaded in outer box, wherein, trace lead detectable includes hydrochloric acid eluent A, sodium hydroxide neutralizer B, dithizone chloroform solution C and ammoniacal salt acid azanol and ammonium citrate mixed liquor D, and consumptive material includes water sampler, liquid-transfering sucker, reaction tube, sulfydryl filter paper, absorption funnel, support and waste liquid cup.The invention has benefit that：(1) screening can be carried out to sample at the scene under conditions of non-laboratory；(2) equipment and the high-tech personnel of costliness need not be equipped with；(3) detection can be completed in 2h, the fast qualitative for realizing trace lead is determined；(4) sensitivity that detects, stability, reliability reach the requirement of evaluation of hygiene standard；(5) reagent paper, consumptive material and reagent are independently packed, and are convenient for carrying.
Description
Technical field
The present invention relates to a kind of detection kit, and in particular to a kind of water sample trace lead quick detection kit, belonging to
Study a part detection technique field.
Background technology
Due to the mankind to the exploitation of lead, smelt and products containing lead is widely used, such as paint, coating, printing, electronics product
The activities such as product, five metalworkings and accumulator manufacture are increasing, the discharge of factory's three wastes and the discharge of vehicle exhaust, cause a large amount of
Lead dust and lead-containing compounds enter big gas and water and soil, easily cause the pollution of living environment.
Lead is a Heavy Metallic Elements, it is impossible to be biodegradable, and lead dust or lead-containing compounds are accumulated in a large number in local environment
It is easy to directly be caused lead poisoning event by human consumption.Lead dust or lead-containing compounds are accumulated for a long time in local environment, by rice
The dense product of the animals such as the crops such as paddy and Semen Tritici aestivi, Aquatic product and poultry, is eaten by the mankind indirectly, causes chronic accumulation and poisoning.Cause
This, in active detection environment especially in water sample lead presence, be important means that mankind's preventing and treating lead is damaged.
At present, detect that the method for lead in water sample has：Atomic absorption method, Differential Potentiometric Stripping Analysis with Experimental, polarography, gas chromatogram
Method, spectrophotography etc..
Though these methods are sensitive, accurate, generally existing pre-treatment is loaded down with trivial details, required instrument and equipment is expensive, detection time compared with
The problems such as long, detection technique has high demands, it is difficult to the scene for being applied to the environmental and biological samples such as food, water sample, urine is fast
Speed detection.
The content of the invention
To solve the deficiencies in the prior art, it is an object of the invention to provide a kind of water sample trace lead quick detection reagent
Box.
In order to realize above-mentioned target, the present invention is adopted the following technical scheme that：
A kind of water sample trace lead quick detection kit, it is characterised in that include：Trace lead detectable, trace lead mark
Quasi- colour atla and some consumptive materials, independently pack, and are then loaded in outer box jointly, wherein,
Aforementioned trace lead detectable includes：Hydrochloric acid eluent A, sodium hydroxide neutralizer B, dithizone chloroform solution C and
Ammoniacal salt acid azanol and ammonium citrate mixed liquor D, wherein, in aforementioned salt acid eluent A, the concentration of hydrochloric acid is O.1M aforementioned hydrogen-oxygen
Change the concentration of sodium hydroxide in sodium neutralizer B for O.4M, the concentration of dithizone is 0.01g/L in aforementioned dithizone chloroform solution C, front
The weight ratio for stating oxammonium hydrochloride., ammonium citrate and deionized water in ammoniacal salt acid azanol and ammonium citrate mixed liquor D is 1:5:50,
PH is adjusted to alkalescence with ammonia, wherein, aforementioned dithizone chloroform solution C is preserved in brown reagent bottle；
Aforementioned trace lead standard color card is：Photochrome after lead standard solution chromogenic reaction；
Aforementioned consumptive material includes：Water sampler, liquid-transfering sucker, reaction tube, sulfydryl filter paper, absorption funnel, support and waste liquid
Cup.
A kind of aforesaid water sample trace lead quick detection kit, it is characterised in that the preparation method of aforementioned sulfhydryl filter paper
For：
Quantitative analyses filter paper is dried, per 30g quantitative analyses filter paper immersion thioglycolic acid containing 80ml-120ml, 60ml-
80ml acetic anhydrids, the acetic acid that 30ml-34ml volumetric concentrations are 36%, 0.2ml-0.4ml concentrated sulphuric acids and 8ml-12ml deionized waters
Solution in, place 72h in 30 DEG C of electric heating constant temperature close drying casees, after taking-up, deionized water is washed till neutrality, finally squeeze go
Moisture is simultaneously dried in 30 DEG C of Constant Temp. Ovens.
Aforesaid a kind of water sample trace lead quick detection kit, it is characterised in that aforementioned water sampler, liquid relief are inhaled
Head, reaction tube and absorption funnel, using front, all first with 3% nitric acid dousing 12h, then deionized water is rinsed to neutrality, most
65 DEG C of temperature control drying afterwards.
Aforesaid a kind of water sample trace lead quick detection kit, it is characterised in that using method is as follows：
(1) using deionized water as blank, the water sample of doubtful lead contamination is taken, is marked respectively；
(2) absorption funnel is placed on support, sulfydryl filter paper is positioned in absorption funnel, waste liquid cup is placed under support
Side, finally pouring water sample in absorption funnel into carries out Filtration Adsorption；
(3) waste liquid cup is removed after the completion of filtering, with the abundant eluting sulfydryl filter paper of 2ml hydrochloric acid eluent A, collected with reaction tube
Whole eluents；
(4) 0.5ml sodium hydroxide neutralizer B are added in reaction tube, after being sufficiently mixed, adds 1ml dithizone chloroforms
Liquid C and 0.5ml ammoniacal salt acid azanol and ammonium citrate mixed liquor D, stand 10min after shaking, observe each reaction liquid in pipe institute
The chromogenic reaction of presentation, is contrasted with trace lead standard color card.
The invention has benefit that：
(1) detection kit of the invention is the test kit of conventional fast qualitative detection, can be in the condition of non-laboratory
Under screening is carried out to sample at the scene, using the present invention detection kit detection water sample lead when, it is not necessary to be equipped with expensive setting
Standby and high-tech personnel, it is to avoid the waste of man power and material；
(2), when using the detection kit detection water sample trace lead of the present invention, operating process can be greatly simplified, shortens inspection
The survey time, detection can be completed in 2h, the fast qualitative for realizing trace lead is determined；
(3), when using the detection kit detection water sample lead of the present invention, the sensitivity of detection, stability, reliability reach
To the requirement of evaluation of hygiene standard, detection limit reaches 0.1-2.0mg/L, and measurement result can be used as the weight for tentatively judging event property
Reference frame is wanted, is particularly suited for the live qualitative determination of trace lead in contaminant water sample and urine；
(4) reagent paper, consumptive material and reagent are independently packed, and are convenient for carrying, and usage cycles are long.
Description of the drawings
Fig. 1 is the composition schematic diagram of trace lead detectable；
Fig. 2 is the schematic diagram of trace lead standard color card；
Fig. 3 is the schematic diagram of water sampler；
Fig. 4 is the schematic diagram of reaction tube；
Fig. 5 is the schematic diagram of sulfydryl filter paper and absorption funnel；
Fig. 6 is the schematic diagram of support；
Fig. 7 is the schematic diagram of liquid-transfering sucker；
Fig. 8 is the schematic diagram of waste liquid cup；
Fig. 9 is the schematic diagram of outer box.
Specific embodiment
Make specific introduction to the present invention below in conjunction with the drawings and specific embodiments.
The water sample trace lead quick detection kit of the present invention includes：Trace lead detectable, trace lead standard color card and
Some consumptive materials, independently pack, then jointly loaded in outer box (copperplate box made of paper, as shown in Figure 9).
First, trace lead detectable
Trace lead detectable amounts to four kinds, is respectively：Hydrochloric acid eluent A, sodium hydroxide neutralizer B, dithizone chloroform
Liquid C, ammoniacal salt acid azanol and ammonium citrate mixed liquor D, as shown in Figure 1.
Hydrochloric acid eluent A is salt aqueous acid, and wherein the concentration of hydrochloric acid is for O.1M.
Aqueous solutions of the sodium hydroxide neutralizer B for sodium hydroxide, wherein the concentration of sodium hydroxide is for O.4M.
Chloroformic solutions of the dithizone chloroform solution C for dithizone, using chloroform as solvent, the concentration of dithizone is 0.01g/L,
The solution is preserved in brown reagent bottle.
Ammoniacal salt acid azanol and ammonium citrate mixed liquor D are the aqueous solution of ammoniacal salt acid azanol and ammonium citrate, wherein salt
The weight ratio of sour azanol, ammonium citrate and deionized water is 1:5:50, pH is adjusted to alkalescence with ammonia.
2nd, trace lead standard color card
Trace lead standard color card is the photochrome after lead standard solution chromogenic reaction, as shown in Figure 2.
The manufacture method of lead standard color card：With lead acetate prepare standard water sample, for example lead concentration be respectively 0mg/L,
0.1mg/L, 0.2mg/L, 0.3mg/L and 0.4mg/L (or lead concentration is respectively 0mg/L, 0.5mg/L, 1.0mg/L, 1.5mg/
L and 2.0mg/L), each standard water sample respectively takes 10ml, in adding 25ml color-comparison tubes, then adds in color-comparison tube
2ml dithizone chloroform solution C and 1ml ammoniacal salt acid azanol and ammonium citrate mixed liquor D, stand 10min, color-comparison tube after shaking
There is significantly colour developing bench in middle liquid, produces lead standard color card by digital photography, as shown in Figure 2.
3rd, consumptive material
Water sampler：The Dispoable medical Cup for holding sample of five scales of 10ml, 20ml, 30ml, 40ml and 50ml is indicated, is used
In water sample is gathered, as shown in Figure 3.
Reaction tube：The glass color comparison tube of a diameter of 0.8cm-1cm, volume for 7ml, for providing the place of reaction, such as Fig. 4
It is shown.
Sulfydryl filter paper：The quantitative analyses filter paper of Jing sulfhydrylations process, for filtering, adsorbing and eluting water sample specimen, such as Fig. 5
It is shown.
Absorption funnel：Dispoable medical plastic funnel, for holding sulfydryl filter paper, in black plastic together with sulfydryl filter paper
Seal up for safekeeping in bag, as shown in Figure 5.
Support：For supporting absorption funnel to complete filtration, absorption and the eluting of water sample specimen, as shown in Figure 6.
Liquid-transfering sucker：Dispoable medical suction pipette head, specification and quantity are 1ml hydrochloric acid eluents suction nozzle 1,0.5ml
Sodium hydroxide neutralizer suction nozzle 1,1ml dithizone chloroform solutions suction nozzle 1 and 1ml ammoniacal salts acid azanol and ammonium citrate mixed liquor
Suction nozzle 1, as shown in Figure 7.
Waste liquid cup：Plastic cup, can be placed under support, filter waste liquid for collecting, as shown in Figure 8.
Water sampler, reaction tube, absorption funnel and liquid-transfering sucker, using front all first with 3% nitric acid dousing 12h, so
Deionized water is rinsed to neutrality afterwards, last 65 DEG C of temperature controls drying.
The preparation method of sulfydryl filter paper：
Quantitative analyses filter paper is dried, it is thio per 30g quantitative analyses filter paper immersion (can properly increase to 120ml) containing 80ml
Glycolic, 60ml (can properly increase to 80ml) acetic anhydrid, the second that 30ml (can properly increase to 34ml) volumetric concentration is 36%
In the solution of acid, 0.2ml (can properly increase to 0.4ml) concentrated sulphuric acids and 8ml (can properly increase to 12ml) deionized water, in 30
72h is placed in DEG C electric heating constant temperature close drying case, deionized water is washed till neutrality after taking-up, finally squeeze and remove moisture electric in 30 DEG C
Dry in hot thermostatic drying chamber.
4th, Cleaning Principle
Lead ion in water sample is adsorbed and concentration by sulfydryl absorbent filter paper, infrequent menstruation amount hydrochloric acid eluent A eluting and hydroxide
In sodium neutralizer B with after, easily there is colour developing with dithizone chloroform solution C and ammoniacal salt acid azanol and ammonium citrate mixed liquor D anti-
Should, with increasing for lead content, color presents the trend of green color-blue-purple-pink colour transition, can be preliminary by color
The content of lead in judgment sample.
5th, detection method
Embodiment 1：Lead content in the contaminated water sample of detection
Contaminated water sample 20ml is taken, and Filtration Adsorption is carried out with sulfydryl filter paper, wherein, sulfydryl filter paper is positioned over absorption funnel
Interior, absorption funnel is placed on support, and waste liquid cup is placed with below support.
Waste liquid cup is removed after the completion of filtration, with the abundant eluting sulfydryl filter paper of 2ml hydrochloric acid eluent A, collects complete with reaction tube
The eluent in portion.
0.5ml sodium hydroxide neutralizer B are added in collection has the reaction tube of eluent, after being sufficiently mixed, adds 1ml double
Sulfur hydrazone chloroform solution C and 0.5ml ammoniacal salt acid azanol and ammonium citrate D, stand 10min, observing response liquid in pipe institute after shaking
The chromogenic reaction of presentation, is contrasted with trace lead standard color card.
In the present embodiment, on our trace lead standard color card the concentration of lead be followed successively by 0.0mg/L, 0.1mg/L,
0.2mg/L, 0.3mg/L and 0.4mg/L, judge the content of lead in water sample accordingly.
Judged result：In water sample, lead content is 0.1mg/L.
Whole detection process takes 1h45min.
Embodiment 2：Lead content in the professional workman's urine sample of detection
Using deionized water 20ml as blank, each 20ml of four experimenter's urines is taken, is filtered with sulfydryl after mark respectively
Paper carries out Filtration Adsorption, wherein, sulfydryl filter paper is positioned in absorption funnel, and absorption funnel is placed on support, is placed below support
There is waste liquid cup.
Waste liquid cup is removed after the completion of filtration, respectively with the abundant eluting sulfydryl filter paper of 2ml hydrochloric acid eluent A, is received with reaction tube
The whole eluent of collection.
0.5ml sodium hydroxide neutralizer B are added in reaction tube, after being sufficiently mixed, 1ml dithizone chloroform solution C is added
With 0.5ml ammoniacal salts acid azanol and ammonium citrate mixed liquor D, 10min after shaking, is stood, observe each reaction liquid in pipe and presented
Chromogenic reaction, contrasted with trace lead standard color card.
In the present embodiment, on our trace lead standard color card the concentration of lead be followed successively by 0.0mg/L, 0.1mg/L,
0.2mg/L, 0.3mg/L and 0.4mg/L, corresponding color are followed successively by green, blueness, bluish violet, purple, pink colour, judge accordingly
The content of Determination of Urine Plumbum.
Testing result：Blank is in green (concentration 0.0mg/L of lead), first, the 3rd and the 4th experimenter
Urine examination in aeruginouss (, between green and blueness, lead concentration is between less than 0.1mg/L for color), second experimenter
Urine examination be in pink colour (concentration >=0.4mg/L of lead).
Whole detection process takes 1h50min.
Embodiment 3：Lead content in detection pollution biological sample
Contaminated samples 2g are taken, is crushed, add 3% nitric acid 4ml immersion half an hour, boiled and extract limpid to liquid, filter residual
Slag, filtrate adjust pH value 7.0 or so with 1M sodium hydroxide solutions, plus deionized water constant volume is 5ml.
Liquid after constant volume is carried out into Filtration Adsorption with sulfydryl filter paper, wherein, sulfydryl filter paper is positioned in absorption funnel, is inhaled
Attached funnel is placed on support, and waste liquid cup is placed with below support.
Waste liquid cup is removed after the completion of filtration, with the abundant eluting sulfydryl filter paper of 2ml hydrochloric acid eluent A, collects complete with reaction tube
The eluent in portion.
0.5ml sodium hydroxide neutralizer B are added in collection has the reaction tube of eluent, after being sufficiently mixed, adds 1ml double
Sulfur hydrazone chloroform solution C and 0.5ml ammoniacal salt acid azanol and ammonium citrate D, stand 10min, observing response liquid in pipe institute after shaking
The chromogenic reaction of presentation, is contrasted with trace lead standard color card.
In the present embodiment, on our trace lead standard color card the concentration of lead be followed successively by 0.00mg/L, 0.25mg/L,
0.50mg/L, 0.75mg/L and 1.50mg/L, judge the content of Determination of Urine Plumbum accordingly.
Testing result：Contaminated samples lead content 0.50mg/L.
Whole detection process takes 1h55min.
Embodiment 4：The contaminated water sample lead content of detection
Take by the water sample 5ml of lead contamination, be placed directly within reaction tube, in reaction tube, add 0.5ml sodium hydroxide neutralizers
B, after being sufficiently mixed, adds 1ml dithizone chloroform solution C and 0.5ml ammoniacal salt acid azanol and ammonium citrate D, stands after shaking
10min, the chromogenic reaction is presented by observing response liquid in pipe are contrasted with trace lead standard color card.
In the present embodiment, on our trace lead standard color card the concentration of lead be followed successively by 0.0mg/L, 0.5mg/L,
1.0mg/L, 1.5mg/L and 2.0mg/L, judge the content of Determination of Urine Plumbum accordingly.
Testing result：The water sample lead content 1.5mg/L of pollution.
Whole detection process takes 57min.
6th, the evaluation of testing result
Take 5 test kits, respectively the lead standard solution sample of 5 variable concentrations tested, continuous 5 days it is daily each
Sample is determined once respectively with different test kits, records result, calculates the accuracy rate and the coefficient of variation of measurement result respectively.
Potassium, sodium, calcium, magnesium, ferrum, zinc, copper, hydrargyrum and the cadmium ion of variable concentrations are separately added in lead standard solution sample,
Observe the impact of these ion pair test results.
Jing is tested it was found that the test kit of the present invention：
(1) sensitivity：More than 95%, minimum detectability is 0.1mg/L.
(2) stability：Deposit 12 months under lucifuge, the room temperature environment of sealing, the stabilization of kit is good.
(3) reliability：Potassium, sodium in test sample, calcium, magnesium, iron ion are not affected on test result；Zinc, copper, hydrargyrum and
Cadmium ion can produce certain impact to test result, by regulating and controlling the pH value of ammoniacal salt acid azanol ammonium citrate solution in 8.5-
9.5 scopes, you can improve lead chelate effect, it is ensured that the reliability of detection.
When as can be seen here, using the detection kit detection water sample lead of the present invention, the sensitivity of detection, stability, reliability
Property reaches the requirement of evaluation of hygiene standard, and minimum detectability is 0.1mg/L, and testing result can be used as tentatively judging event property
Important reference, be particularly suited for the live qualitative determination of lead in contaminant water sample and urine.
It should be noted that above-described embodiment the invention is not limited in any way, all employing equivalents or equivalent change
The technical scheme obtained by the mode changed, all falls within protection scope of the present invention.
Claims (4)
1. a kind of water sample trace lead quick detection kit, it is characterised in that include：Trace lead detectable, trace lead standard
Colour atla and some consumptive materials, independently pack, and are then loaded in outer box jointly, wherein,
The trace lead detectable includes：Hydrochloric acid eluent A, sodium hydroxide neutralizer B, dithizone chloroform solution C and ammonia
Oxammonium hydrochloride. and ammonium citrate mixed liquor D, in the hydrochloric acid eluent A, the concentration of hydrochloric acid is for O.1M, the sodium hydroxide is neutralized
In liquid B, the concentration of sodium hydroxide is for O.4M, and in the dithizone chloroform solution C, the concentration of dithizone is 0.01g/L, the ammoniacal salt
In sour azanol and ammonium citrate mixed liquor D, the weight ratio of oxammonium hydrochloride., ammonium citrate and deionized water is 1:5:50, adjusted with ammonia
PH to alkalescence, wherein, the dithizone chloroform solution C is preserved in the brown reagent bottle；
The trace lead standard color card is：Photochrome after lead standard solution chromogenic reaction；
The consumptive material includes：Water sampler, liquid-transfering sucker, reaction tube, sulfydryl filter paper, absorption funnel, support and waste liquid cup.
2. a kind of water sample trace lead quick detection kit according to claim 1, it is characterised in that the sulfydryl filter paper
Preparation method be：
Quantitative analyses filter paper is dried, per 30g quantitative analyses filter paper immersion thioglycolic acid containing 80ml-120ml, 60ml-80ml
Acetic anhydrid, the acetic acid that 30ml-34ml volumetric concentrations are 36%, 0.2ml-0.4ml concentrated sulphuric acids and 8ml-12ml deionized waters it is molten
In liquid, 72h is placed in 30 DEG C of electric heating constant temperature close drying casees, deionized water is washed till neutrality after taking-up, finally squeeze and remove moisture
And dry in 30 DEG C of Constant Temp. Ovens.
3. a kind of water sample trace lead quick detection kit according to claim 1, it is characterised in that the water sampling
Device, liquid-transfering sucker, reaction tube and absorption funnel, using it is front all first use 3% nitric acid dousing 12h, then deionized water flushing
To neutral, last 65 DEG C of temperature controls drying.
4. a kind of water sample trace lead quick detection kit according to claim 1, it is characterised in that using method is such as
Under：
(1) using deionized water as blank, the water sample of doubtful lead contamination is taken, is marked respectively；
(2) absorption funnel is placed on support, sulfydryl filter paper is positioned in absorption funnel, waste liquid cup is placed in below support,
Finally water sample is poured in absorption funnel carries out Filtration Adsorption；
(3) waste liquid cup is removed after the completion of filtering, with the abundant eluting sulfydryl filter paper of 2ml hydrochloric acid eluent A, collected all with reaction tube
Eluent；
(4) in reaction tube add 0.5ml sodium hydroxide neutralizer B, after being sufficiently mixed, add 1ml dithizone chloroform solution C and
0.5ml ammoniacal salts acid azanol and ammonium citrate mixed liquor D, stand 10min after shaking, observe what each reaction liquid in pipe was presented
Chromogenic reaction, is contrasted with trace lead standard color card.
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| CN201710069317.4A CN106546587A (en) | 2017-02-08 | 2017-02-08 | A kind of water sample trace lead quick detection kit |
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| CN201710069317.4A CN106546587A (en) | 2017-02-08 | 2017-02-08 | A kind of water sample trace lead quick detection kit |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108956600A (en) * | 2018-10-12 | 2018-12-07 | 安徽新芜精密装备制造产业技术研究院有限公司 | The measuring method and its application of impurity copper content in a kind of zirconium aluminium powder |
| CN109060792A (en) * | 2018-09-07 | 2018-12-21 | 天津市光复科技发展有限公司 | The method of sulfhydryl paper concentration and separation colorimetric method for determining trace lead in water |
| CN109239060A (en) * | 2018-09-07 | 2019-01-18 | 天津市光复科技发展有限公司 | The sulfhydryl paper enrichment of heavy metal cadmium, separation colorimetric method measuring method in water |
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Application publication date: 20170329 |