CN109115765A - The method of turbidimetry for Determination arsenic amount - Google Patents
The method of turbidimetry for Determination arsenic amount Download PDFInfo
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- CN109115765A CN109115765A CN201810987991.5A CN201810987991A CN109115765A CN 109115765 A CN109115765 A CN 109115765A CN 201810987991 A CN201810987991 A CN 201810987991A CN 109115765 A CN109115765 A CN 109115765A
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- 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
- G01N21/82—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 precipitate or turbidity
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
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Abstract
The invention discloses the methods of turbidimetry for Determination arsenic amount, weighing including sample, sample pretreatment, the measurement of sample solution, add assisted solution, the processing of colorimetric cylinder muddiness, standard color range once configures, once than turbid processing, the secondary configuration of standard color range, it is secondary to be calculated than turbid processing and sample arsenic amount, the present invention is scientific and reasonable, it is safe and convenient to use, using secondary than turbid, select concentration of hydrochloric acid appropriate, guarantee the abundant of reduction reaction, the precipitation of salt is reduced so that the accuracy of arsenic content further improves, convenient for the arsenic amount in clearer calculating sample, and white shutter is being added in the process as observation background than turbid, so that visually than it is turbid when observe it is more accurate, testing crew subjective factor is reduced to the impression of observation result, using Lime Hypophosphate, it is easy in sodium hypophosphite heating process because of temperature mistake before solving Height causes reaction failure even to be easy to burst the generation of accident.
Description
Technical field
The present invention relates to chemical engineering industry technical fields, the specially method of turbidimetry for Determination arsenic amount.
Background technique
The chemical symbol of arsenic is As, and atomic number 33 has ash, Huang, dark brown three kinds of allotropes, has metallicity, former
Son amount 74.92, specific gravity 5.73 (14 DEG C), 814 DEG C of fusing point, 615 DEG C whens, distil, not soluble in water, nitric acid and chloroazotic acid are dissolved in, in humidity
It is easily oxidized in air, mainly (such as realgar As in the form of sulfide mine2S2, orpiment As2S3Deng) be present in nature, arsenic and
Its compound is mainly used for the industry such as alloy smelting, pesticide medicine, pigment, is also present in raw material, waste residue, half often as impurity
It in finished product and finished product, in above-mentioned production or uses in arsenic compound operation, such as protects improper sucking air containing arsenic or intake by arsenic
When the food of pollution, beverage, the possibility of acute and chronic arsenic poisoning is often occurred, therefore in industrial production and trash discharge, in order to
It prevents arsenium contaminated environment and causes harm to the human body, the necessary measurement that industrial products and discharge fertilizer are carried out with arsenic amount, to prevent
Damage of the excessive arsenic to environment and human body, in existing arsenic amount method for measuring, turbidimetry is wherein easier method
One of, but accuracy of measurement when turbidimetry used at present measurement arsenic amount is lower, passes through the color range visual comparison of single, arsenic
The precision of content is difficult to obtain effective guarantee, while simple visually than turbid, also be easy to cause on tester visual perception
Deviation causes tester that cannot effectively select suitable standard color range, causes the error of arsenic magnitude to float larger, existing simultaneously
Some turbidimetrys need the content of assisted solution to be used more when surveying arsenic amount, increase the time and place required for liquid waste processing
Medicament is managed, so that the cost needed when turbidimetry for Determination increases.
Summary of the invention
The present invention provides the method for turbidimetry for Determination arsenic amount, can effectively solve mentioned above in the background art to make at present
Accuracy of measurement when turbidimetry measurement arsenic amount is lower, passes through the color range visual comparison of single, and the precision of arsenic content is difficult
To obtain effective guarantee, at the same it is simple visually than turbid, and the deviation also be easy to causeing on tester visual perception causes tester
Member cannot effectively select suitable standard color range, cause the error of arsenic magnitude to float larger, while existing turbidimetry surveys arsenic
It needs the content of assisted solution to be used more when amount, increases the time and treatment agent required for liquid waste processing, so that than
The problem of cost that turbid method needs when measuring increases.
To achieve the above object, it the invention provides the following technical scheme: the method for turbidimetry for Determination arsenic amount, including walks as follows
It is rapid:
S1: sample weighs: weighing sample by electronic scale；
S2: sample pretreatment: boiling rear low-temperature heat to sample high temperature and decompose, and hydrochloric acid is added, shakes after deionized water dilution
It is even, place clarification；
S3: the measurement of sample solution: middling speed filters clarified sample solution, takes filtered sample solution that sample colorimetric is added
In pipe；
S4: copper sulphate, Lime Hypophosphate and hydrochloric acid addition assisted solution: are sequentially added into sample colorimetric cylinder；
S5: the processing of colorimetric cylinder muddiness: heating sample colorimetric cylinder, then removes flowing water cooling；
S6: standard color range once configures: the standard arsenic amount solution of several different volumes being taken to be placed in the color range colorimetric of same quantity
Pipe internal modulation；
S7: once than turbid processing: colorimetric cylinder is placed side by side, by than turbid, determining the corresponding arsenic amount of sample；
S8: it is molten the secondary configuration of standard color range: the secondary configuration of standard color range: to choose standard arsenic amount close with sample solution turbidity
Liquid refines preparation standard color range；
S9: secondary than turbid processing: colorimetric cylinder is placed side by side, by than turbid, determining the corresponding arsenic amount of sample；
S10: sample arsenic amount calculates: As (%)=[(m1*0.0000001/v1)/(m0/v0)]*100。
According to the above technical scheme, in step S1, weighing sample weight is 0.3g, and weighed sample is put into 250ml
Triangular flask in.
According to the above technical scheme, in step S2, the triangular flask equipped with sample is placed in above electric furnace and is heated, makes to try
After sample is boiled by high temperature at 200 degrees celsius, furnace temperature is reduced, low-temperature heat decomposition is carried out at 50 c to sample,
The triangular flask for filling sample is persistently rocked during this, knot bottom is prevented, steams to moisture and removed after disappearing, is added into triangular flask
50ml hydrochloric acid, and enclosed with water pressure-vaccum bottle wall one, then solution is moved into 100ml volumetric flask, addition deionized water is diluted to
At 100ml scale, shaking is shaken up, and places clarification.
According to the above technical scheme, in step S3, clear sample solution middling speed is filtered by filter paper, throughput
Sample solution after the filtering of cylinder selection 10ml, is poured into the sample colorimetric cylinder of 50ml.
According to the above technical scheme, in step S4, the content for pouring into copper sulphate in sample colorimetric cylinder is 1ml, and concentration is
100g/L, the content for pouring into Lime Hypophosphate in sample colorimetric cylinder is 5ml, concentration 300g/L, and it is dilute finally to pour into (1+1) hydrochloric acid
It releases to 25ml, and sample colorimetric cylinder is shaken up after assisted solution is added every time.
According to the above technical scheme, in step S5, sample colorimetric cylinder heats 7 minutes in 90 degrees Celsius of environment, then removes
Flowing water is cooling.
According to the above technical scheme, in step S6, include the following steps:
(1) measured respectively with graduated cylinder 0.0ml, 1.0ml, 2.0ml, 3.0ml, 4.0ml, 5.0ml, 6.0ml, 7.0ml,
The arsenic standard solution of the 0.010mg/ml of 8.0ml, 9.0ml and 10.0ml are placed in 50ml color range colorimetric cylinder；
(2) (1+1) hydrochloric acid is injected into 11 color range colorimetric cylinders respectively, is diluted at 10ml scale；
(3) copper-bath and 5ml concentration that injection 1ml concentration is 100g/L into 11 color range colorimetric cylinders respectively are
The Lime Hypophosphate of 300g/L, shakes up；
(4) (1+1) hydrochloric acid is added into 11 color range colorimetric cylinders respectively to 25ml；
(5) 11 color range colorimetric cylinders are placed into 90 degrees Celsius of environment and are heated 7 minutes, it is cooling to remove rear flowing water.
According to the above technical scheme, step S7 includes the following steps:
(1) color range colorimetric cylinder is arranged in a row placement according to the sequence of the content of arsenic standard solution, and by sample colorimetric
Pipe is placed on the end side of a row；
(2) white shutter is chosen to place with color range colorimetric cylinder in parallel；
(3) visual color range colorimetric cylinder, carries out visually on the background board that white shutter is formed than turbid.
According to the above technical scheme, in step S8, include the following steps:
(1) once than two color ranges similar in sample turbidity in turbid processing, arsenic solution content is xml and (x+1) ml for selection,
It is measured with graduated cylinder as 0.010mg/ml x.1ml, x.2ml, x.3ml, x.4ml, x.5ml, x.6ml, x.7ml, x.8ml, x.9ml
Arsenic standard solution, be placed in 50ml color range colorimetric cylinder；
(3) copper-bath and 5ml concentration that injection 1ml concentration is 100g/L into 9 color range colorimetric cylinders respectively are
The Lime Hypophosphate of 300g/L, shakes up；
(4) (1+1) hydrochloric acid is added into 9 color range colorimetric cylinders respectively to 25ml；
(5) 9 color range colorimetric cylinders are placed into 90 degrees Celsius of environment and are heated 7 minutes, it is cooling to remove rear flowing water.
According to the above technical scheme, it in step S10, selects secondary than standard similar in turbid processing neutralization test solution turbidity
Color range records arsenic amount, and sample arsenic amount calculates: As (%)=[(m1*0.0000001/v1)/(m0/v0)] * 100, wherein m1 is
It is secondary than it is turbid when, the standard arsenic amount (unit: ug) that sample solution is equivalent to, v1 is point sample solution volume taken (unit: ml),
M0 is the gross mass (unit: g) of sample solution, and v0 is the total volume (unit: ml) of sample solution.
Compared with prior art, beneficial effects of the present invention: structure of the invention is scientific and reasonable, safe and convenient to use: we
Method in use, the time of temperature and reduction reaction when by stable control reduction reaction, effectively prevents temperature
Deposited phenomenon caused by height is spent, also avoiding the problem that temperature is too low leads to delay of response, simultaneous selection concentration of hydrochloric acid appropriate,
Guarantee the abundant of reduction reaction, the precipitation of salt is reduced, while in the method, using secondary than turbid, so that the essence of arsenic content
Exactness is further improved, and convenient for the arsenic amount in clearer calculating sample, and blocks than the turbid white of addition in the process
Plate as observation background so that visually than it is turbid when observe it is more accurate, reduce testing crew subjective factor to observation result print
As being easy to lead to reaction failure very because temperature is excessively high in sodium hypophosphite heating process before solving using Lime Hypophosphate
To being easy to burst the generation of accident.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the step flow diagram of the method for the present invention.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings, it should be understood that preferred reality described herein
Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
Embodiment 1: as shown in Figure 1, the present invention provides a kind of technical solution, the method for turbidimetry for Determination arsenic amount, including such as
Lower step:
S1: sample weighs: weighing sample by electronic scale；
S2: sample pretreatment: boiling rear low-temperature heat to sample high temperature and decompose, and hydrochloric acid is added, shakes after deionized water dilution
It is even, place clarification；
S3: the measurement of sample solution: middling speed filters clarified sample solution, takes filtered sample solution that sample colorimetric is added
In pipe；
S4: copper sulphate, Lime Hypophosphate and hydrochloric acid addition assisted solution: are sequentially added into sample colorimetric cylinder；
S5: the processing of colorimetric cylinder muddiness: heating sample colorimetric cylinder, then removes flowing water cooling；
S6: standard color range once configures: the standard arsenic amount solution of several different volumes being taken to be placed in the color range colorimetric of same quantity
Pipe internal modulation；
S7: once than turbid processing: colorimetric cylinder is placed side by side, by than turbid, determining the corresponding arsenic amount of sample；
S8: it is molten the secondary configuration of standard color range: the secondary configuration of standard color range: to choose standard arsenic amount close with sample solution turbidity
Liquid refines preparation standard color range；
S9: secondary than turbid processing: colorimetric cylinder is placed side by side, by than turbid, determining the corresponding arsenic amount of sample；
S10: sample arsenic amount calculates: As (%)=[(m1*0.0000001/v1)/(m0/v0)]*100。
According to the above technical scheme, in step S1, weighing sample weight is 0.3g, and weighed sample is put into 250ml
Triangular flask in.
According to the above technical scheme, in step S2, the triangular flask equipped with sample is placed in above electric furnace and is heated, makes to try
After sample is boiled by high temperature at 200 degrees celsius, furnace temperature is reduced, low-temperature heat decomposition is carried out at 50 c to sample,
The triangular flask for filling sample is persistently rocked during this, knot bottom is prevented, steams to moisture and removed after disappearing, is added into triangular flask
50ml hydrochloric acid, and enclosed with water pressure-vaccum bottle wall one, then solution is moved into 100ml volumetric flask, addition deionized water is diluted to
At 100ml scale, shaking is shaken up, and places clarification.
According to the above technical scheme, in step S3, clear sample solution middling speed is filtered by filter paper, throughput
Sample solution after the filtering of cylinder selection 10ml, is poured into the sample colorimetric cylinder of 50ml.
According to the above technical scheme, in step S4, the content for pouring into copper sulphate in sample colorimetric cylinder is 1ml, and concentration is
100g/L, the content for pouring into Lime Hypophosphate in sample colorimetric cylinder is 5ml, concentration 300g/L, and it is dilute finally to pour into (1+1) hydrochloric acid
It releases to 25ml, and sample colorimetric cylinder is shaken up after assisted solution is added every time.
According to the above technical scheme, in step S5, sample colorimetric cylinder heats 7 minutes in 90 degrees Celsius of environment, then removes
Flowing water is cooling.
According to the above technical scheme, in step S6, include the following steps:
(1) measured respectively with graduated cylinder 0.0ml, 1.0ml, 2.0ml, 3.0ml, 4.0ml, 5.0ml, 6.0ml, 7.0ml,
The arsenic standard solution of the 0.010mg/ml of 8.0ml, 9.0ml and 10.0ml are placed in 50ml color range colorimetric cylinder；
(2) (1+1) hydrochloric acid is injected into 11 color range colorimetric cylinders respectively, is diluted at 10ml scale；
(3) copper-bath and 5ml concentration that injection 1ml concentration is 100g/L into 11 color range colorimetric cylinders respectively are
The Lime Hypophosphate of 300g/L, shakes up；
(4) (1+1) hydrochloric acid is added into 11 color range colorimetric cylinders respectively to 25ml；
(5) 11 color range colorimetric cylinders are placed into 90 degrees Celsius of environment and are heated 7 minutes, it is cooling to remove rear flowing water.
According to the above technical scheme, step S7 includes the following steps:
(1) color range colorimetric cylinder is arranged in a row placement according to the sequence of the content of arsenic standard solution, and by sample colorimetric
Pipe is placed on the end side of a row；
(2) white shutter is chosen to place with color range colorimetric cylinder in parallel；
(3) visual color range colorimetric cylinder, carries out visually on the background board that white shutter is formed than turbid.
According to the above technical scheme, in step S8, include the following steps:
(1) once than two color ranges similar in sample turbidity in turbid processing, arsenic solution content is xml and (x+1) ml for selection,
It is measured with graduated cylinder as 0.010mg/ml x.1ml, x.2ml, x.3ml, x.4ml, x.5ml, x.6ml, x.7ml, x.8ml, x.9ml
Arsenic standard solution, be placed in 50ml color range colorimetric cylinder；
(3) copper-bath and 5ml concentration that injection 1ml concentration is 100g/L into 9 color range colorimetric cylinders respectively are
The Lime Hypophosphate of 300g/L, shakes up；
(4) (1+1) hydrochloric acid is added into 9 color range colorimetric cylinders respectively to 25ml；
(5) 9 color range colorimetric cylinders are placed into 90 degrees Celsius of environment and are heated 7 minutes, it is cooling to remove rear flowing water.
According to the above technical scheme, it in step S10, selects secondary than standard similar in turbid processing neutralization test solution turbidity
Color range records arsenic amount, and sample arsenic amount calculates: As (%)=[(m1*0.0000001/v1)/(m0/v0)] * 100, wherein m1 is two
It is secondary than it is turbid when, the standard arsenic amount (unit: ug) that sample solution is equivalent to, v1 is point sample solution volume taken (unit: ml), m0
It is the gross mass (unit: g) of sample solution, v0 is the total volume (unit: ml) of sample solution.
Embodiment 2: as shown in Figure 1, the present invention provides a kind of technical solution, the method for turbidimetry for Determination arsenic amount, including such as
Lower step:
S1: sample weighs: weighing sample by electronic scale；
S2: sample pretreatment: boiling rear low-temperature heat to sample high temperature and decompose, and hydrochloric acid is added, shakes after deionized water dilution
It is even, place clarification；
S3: the measurement of sample solution: middling speed filters clarified sample solution, takes filtered sample solution that sample colorimetric is added
In pipe；
S4: copper sulphate, Lime Hypophosphate and hydrochloric acid addition assisted solution: are sequentially added into sample colorimetric cylinder；
S5: the processing of colorimetric cylinder muddiness: heating sample colorimetric cylinder, then removes flowing water cooling；
S6: standard color range once configures: the standard arsenic amount solution of several different volumes being taken to be placed in the color range colorimetric of same quantity
Pipe internal modulation；
S7: once than turbid processing: colorimetric cylinder is placed side by side, by than turbid, determining the corresponding arsenic amount of sample；
S8: it is molten the secondary configuration of standard color range: the secondary configuration of standard color range: to choose standard arsenic amount close with sample solution turbidity
Liquid refines preparation standard color range；
S9: secondary than turbid processing: colorimetric cylinder is placed side by side, by than turbid, determining the corresponding arsenic amount of sample；
S10: sample arsenic amount calculates: As (%)=[(m1*0.0000001/v1)/(m0/v0)]*100。
According to the above technical scheme, in step S1, weighing sample weight is 0.3g, and weighed sample is put into 250ml
Triangular flask in.
According to the above technical scheme, in step S2, the triangular flask equipped with sample is placed in above electric furnace and is heated, makes to try
After sample is boiled by high temperature at 200 degrees celsius, furnace temperature is reduced, low-temperature heat decomposition is carried out at 50 c to sample,
The triangular flask for filling sample is persistently rocked during this, knot bottom is prevented, steams to moisture and removed after disappearing, is added into triangular flask
50ml hydrochloric acid, and enclosed with water pressure-vaccum bottle wall one, then solution is moved into 100ml volumetric flask, addition deionized water is diluted to
At 100ml scale, shaking is shaken up, and places clarification.
According to the above technical scheme, in step S3, clear sample solution middling speed is filtered by filter paper, throughput
Sample solution after the filtering of cylinder selection 10ml, is poured into the sample colorimetric cylinder of 50ml.
According to the above technical scheme, in step S4, the content for pouring into copper sulphate in sample colorimetric cylinder is 0.5ml, and concentration is
100g/L, the content for pouring into Lime Hypophosphate in sample colorimetric cylinder is 2.5ml, concentration 300g/L, finally pours into (1+2) hydrochloric acid
It is diluted to 25ml, and sample colorimetric cylinder is shaken up after assisted solution is added every time.
According to the above technical scheme, in step S5, sample colorimetric cylinder heats 7 minutes in 100 degrees Celsius of environment, then removes
Flowing water is cooling.
According to the above technical scheme, in step S6, include the following steps:
(1) measured respectively with graduated cylinder 0.0ml, 1.0ml, 2.0ml, 3.0ml, 4.0ml, 5.0ml, 6.0ml, 7.0ml,
The arsenic standard solution of the 0.010mg/ml of 8.0ml, 9.0ml and 10.0ml are placed in 50ml color range colorimetric cylinder；
(2) (1+2) hydrochloric acid is injected into 11 color range colorimetric cylinders respectively, is diluted at 10ml scale；
2.5ml concentration is the Lime Hypophosphate of 300g/L, is shaken up；
(4) (1+2) hydrochloric acid is added into 11 color range colorimetric cylinders respectively to 25ml；
(5) 11 color range colorimetric cylinders are placed into 100 degrees Celsius of environment and are heated 7 minutes, it is cooling to remove rear flowing water.
According to the above technical scheme, step S7 includes the following steps:
(1) color range colorimetric cylinder is arranged in a row placement according to the sequence of the content of arsenic standard solution, and by sample colorimetric
Pipe is placed on the end side of a row；
(2) white shutter is chosen to place with color range colorimetric cylinder in parallel；
(3) visual color range colorimetric cylinder, carries out visually on the background board that white shutter is formed than turbid.
According to the above technical scheme, in step S8, include the following steps:
(1) once than two color ranges similar in sample turbidity in turbid processing, arsenic solution content is xml and (x+1) ml for selection,
It is measured with graduated cylinder as 0.010mg/ml x.1ml, x.2ml, x.3ml, x.4ml, x.5ml, x.6ml, x.7ml, x.8ml, x.9ml
Arsenic standard solution, be placed in 50ml color range colorimetric cylinder；
(3) copper-bath and 2.5ml concentration that 0.5ml concentration is 100g/L are injected into 9 color range colorimetric cylinders respectively
For the Lime Hypophosphate of 300g/L, shake up；
(4) (1+2) hydrochloric acid is added into 9 color range colorimetric cylinders respectively to 25ml；
(5) 9 color range colorimetric cylinders are placed into 100 degrees Celsius of environment and are heated 7 minutes, it is cooling to remove rear flowing water.
According to the above technical scheme, it in step S10, selects secondary than standard similar in turbid processing neutralization test solution turbidity
Color range records arsenic amount, and sample arsenic amount calculates: As (%)=[(m1*0.0000001/v1)/(m0/ v0)] * 100, wherein m1 is two
It is secondary than it is turbid when, the standard arsenic amount (unit: ug) that sample solution is equivalent to, v1 is point sample solution volume taken (unit: ml), m0
It is the gross mass (unit: g) of sample solution, v0 is the total volume (unit: ml) of sample solution.
Embodiment 3: as shown in Figure 1, the present invention provides a kind of technical solution, the method for turbidimetry for Determination arsenic amount, including such as
Lower step:
S1: sample weighs: weighing sample by electronic scale；
S2: sample pretreatment: boiling rear low-temperature heat to sample high temperature and decompose, and hydrochloric acid is added, shakes after deionized water dilution
It is even, place clarification；
S3: the measurement of sample solution: middling speed filters clarified sample solution, takes filtered sample solution that sample colorimetric is added
In pipe；
S4: copper sulphate, Lime Hypophosphate and hydrochloric acid addition assisted solution: are sequentially added into sample colorimetric cylinder；
S5: the processing of colorimetric cylinder muddiness: heating sample colorimetric cylinder, then removes flowing water cooling；
S6: standard color range once configures: the standard arsenic amount solution of several different volumes being taken to be placed in the color range colorimetric of same quantity
Pipe internal modulation；
S7: once than turbid processing: colorimetric cylinder is placed side by side, by than turbid, determining the corresponding arsenic amount of sample；
S8: it is molten the secondary configuration of standard color range: the secondary configuration of standard color range: to choose standard arsenic amount close with sample solution turbidity
Liquid refines preparation standard color range；
S9: secondary than turbid processing: colorimetric cylinder is placed side by side, by than turbid, determining the corresponding arsenic amount of sample；
S10: sample arsenic amount calculates: As (%)=[(m1*0.0000001/v1)/(m0/v0)]*100。
According to the above technical scheme, in step S1, weighing sample weight is 0.3g, and weighed sample is put into 250ml
Triangular flask in.
According to the above technical scheme, in step S2, the triangular flask equipped with sample is placed in above electric furnace and is heated, makes to try
After sample is boiled by high temperature at 200 degrees celsius, furnace temperature is reduced, low-temperature heat decomposition is carried out at 50 c to sample,
The triangular flask for filling sample is persistently rocked during this, knot bottom is prevented, steams to moisture and removed after disappearing, is added into triangular flask
50ml hydrochloric acid, and enclosed with water pressure-vaccum bottle wall one, then solution is moved into 100ml volumetric flask, addition deionized water is diluted to
At 100ml scale, shaking is shaken up, and places clarification.
According to the above technical scheme, in step S3, clear sample solution middling speed is filtered by filter paper, throughput
Sample solution after the filtering of cylinder selection 10ml, is poured into the sample colorimetric cylinder of 50ml.
According to the above technical scheme, in step S4, the content for pouring into copper sulphate in sample colorimetric cylinder is 2ml, and concentration is
100g/L, the content for pouring into Lime Hypophosphate in sample colorimetric cylinder is 10ml, concentration 300g/L, finally pours into (1+3) hydrochloric acid
It is diluted to 25ml, and sample colorimetric cylinder is shaken up after assisted solution is added every time.
According to the above technical scheme, in step S5, sample colorimetric cylinder heats 7 minutes in 120 degrees Celsius of environment, then removes
Flowing water is cooling.
According to the above technical scheme, in step S6, include the following steps:
(1) measured respectively with graduated cylinder 0.0ml, 1.0ml, 2.0ml, 3.0ml, 4.0ml, 5.0ml, 6.0ml, 7.0ml,
The arsenic standard solution of the 0.010mg/ml of 8.0ml, 9.0ml and 10.0ml are placed in 50ml color range colorimetric cylinder；
(2) (1+3) hydrochloric acid is injected into 11 color range colorimetric cylinders respectively, is diluted at 10ml scale；
(3) copper-bath and 10ml concentration that injection 2ml concentration is 100g/L into 11 color range colorimetric cylinders respectively are
The Lime Hypophosphate of 300g/L, shakes up；
(4) (1+3) hydrochloric acid is added into 11 color range colorimetric cylinders respectively to 25ml；
(5) 11 color range colorimetric cylinders are placed into 120 degrees Celsius of environment and are heated 7 minutes, it is cooling to remove rear flowing water.
According to the above technical scheme, step S7 includes the following steps:
(1) color range colorimetric cylinder is arranged in a row placement according to the sequence of the content of arsenic standard solution, and by sample colorimetric
Pipe is placed on the end side of a row；
(2) white shutter is chosen to place with color range colorimetric cylinder in parallel；
(3) visual color range colorimetric cylinder, carries out visually on the background board that white shutter is formed than turbid.
According to the above technical scheme, in step S8, include the following steps:
(1) once than two color ranges similar in sample turbidity in turbid processing, arsenic solution content is xml and (x+1) ml for selection,
It is measured with graduated cylinder as 0.010mg/ml x.1ml, x.2ml, x.3ml, x.4ml, x.5ml, x.6ml, x.7ml, x.8ml, x.9ml
Arsenic standard solution, be placed in 50ml color range colorimetric cylinder；
(3) copper-bath and 10ml concentration that injection 2ml concentration is 100g/L into 9 color range colorimetric cylinders respectively are
The Lime Hypophosphate of 300g/L, shakes up；
(4) (1+3) hydrochloric acid is added into 9 color range colorimetric cylinders respectively to 25ml；
(5) 9 color range colorimetric cylinders are placed into 120 degrees Celsius of environment and are heated 7 minutes, it is cooling to remove rear flowing water.
According to the above technical scheme, it in step S10, selects secondary than standard similar in turbid processing neutralization test solution turbidity
Color range records arsenic amount, and sample arsenic amount calculates: As (%)=[(m1*0.0000001/v1)/(m0/v0)] * 100, wherein m1 is two
It is secondary than it is turbid when, the standard arsenic amount (unit: ug) that sample solution is equivalent to, v1 is point sample solution volume taken (unit: ml), m0
It is the gross mass (unit: g) of sample solution, v0 is the total volume (unit: ml) of sample solution.
The present invention is observed according to standard color range and sample solution made from embodiment 1-3, as a result such as table 1,
1 testing result of table
Through testing result as it can be seen that under 90 degrees Celsius of heating state, the rate of reduction reaction is normal, be not in because
The case where reaction, which is not thorough, causes standard color range turbidity unobvious and overreact generates precipitating, while (1+1) hydrochloric acid is selected,
The case where salt caused by capable of effectively avoiding acidity excessively high is precipitated, and avoids Lower result caused by being precipitated because of salt, selects simultaneously
Suitable copper sulphate and Lime Hypophosphate can guarantee the abundant progress of reduction reaction.
Based on above-mentioned, the present invention has the advantages that this method is in use, when by stable control reduction reaction
Temperature and reduction reaction time, effectively prevent temperature it is excessively high caused by deposited phenomenon, also avoid temperature is too low from causing
The problem of delay of response, while the time of heating is controlled, guarantee the abundant of reduction reaction, reduces the precipitation of salt, while at this
In method, using secondary than turbid, so that the accuracy of arsenic content is further improved, convenient in clearer calculating sample
Arsenic amount, and than adding white shutter during turbid as observation background so that visually than it is turbid when observe more accurate, subtract
Few testing crew subjective factor is to the impression for observing result, using Lime Hypophosphate, sodium hypophosphite heating process before solving
In be easy because temperature it is excessively high, cause reaction failure even being easy to burst the generation of accident.
Finally, it should be noted that being not intended to restrict the invention the above is only preferred embodiment of the invention, although ginseng
According to previous embodiment, invention is explained in detail, for those skilled in the art, still can be to preceding
Technical solution documented by each embodiment is stated to modify or equivalent replacement of some of the technical features.It is all this
Within the spirit and principle of invention, any modification, equivalent replacement, improvement and so on should be included in protection model of the invention
Within enclosing.
Claims (10)
1. the method for turbidimetry for Determination arsenic amount, which comprises the steps of:
S1: sample weighs: weighing sample by electronic scale；
S2: sample pretreatment: boiling rear low-temperature heat to sample high temperature and decompose, and hydrochloric acid is added, shakes up, puts after deionized water dilution
Set clarification；
S3: the measurement of sample solution: middling speed filters clarified sample solution, takes filtered sample solution that sample colorimetric cylinder is added
It is interior；
S4: copper sulphate, Lime Hypophosphate and hydrochloric acid addition assisted solution: are sequentially added into sample colorimetric cylinder；
S5: the processing of colorimetric cylinder muddiness: heating sample colorimetric cylinder, then removes flowing water cooling；
S6: standard color range once configures: the standard arsenic amount solution of several different volumes being taken to be placed in the color range colorimetric cylinder of same quantity
Modulation；
S7: once than turbid processing: colorimetric cylinder is placed side by side, by than turbid, determining the corresponding arsenic amount of sample；
S8: the secondary configuration of standard color range: the secondary configuration of standard color range: choosing standard arsenic amount solution close with sample solution turbidity,
Refine preparation standard color range；
S9: secondary than turbid processing: colorimetric cylinder is placed side by side, by than turbid, determining the corresponding arsenic amount of sample；
S10: sample arsenic amount calculates: As (%)=[(m1*0.0000001/v1)/(m0/v0)]*100。
2. the method for turbidimetry for Determination arsenic amount according to claim 1, in step S1, weighing sample weight is 0.3g, and
Weighed sample is put into the triangular flask of 250ml.
3. the method for turbidimetry for Determination arsenic amount according to claim 1, in step S2, the triangular flask equipped with sample is placed in
It is heated above electric furnace, after boiling sample by high temperature at 200 degrees celsius, reduces furnace temperature, it is Celsius 50 to sample
Degree is lower to carry out low-temperature heat decomposition, persistently should rock the triangular flask for filling sample in the process, prevents knot bottom, steams to moisture after disappearing
It removes, 50ml hydrochloric acid is added into triangular flask, and enclosed with water pressure-vaccum bottle wall one, then solution is moved into 100ml volumetric flask,
Addition deionized water is diluted at 100ml scale, and shaking shakes up, and places clarification.
4. the method for turbidimetry for Determination arsenic amount according to claim 1, in step S3, clear sample solution middling speed is led to
Filter paper is filtered, and sample solution after the filtering of 10ml is chosen by graduated cylinder, is poured into the sample colorimetric cylinder of 50ml.
5. the method for turbidimetry for Determination arsenic amount according to claim 1, in step S4, copper sulphate in sample colorimetric cylinder is poured into
Content be 1ml, concentration 100g/L, pour into Lime Hypophosphate in sample colorimetric cylinder content be 5ml, concentration 300g/L,
(1+1) hydrochloric acid is finally poured into 25ml, and shake up after assisted solution is added every time to sample colorimetric cylinder.
6. the method for turbidimetry for Determination arsenic amount according to claim 1, in step S5, sample colorimetric cylinder is in 90 degrees Celsius of rings
It is heated 7 minutes in border, then removes flowing water cooling.
7. the method for turbidimetry for Determination arsenic amount according to claim 1, in step S6, include the following steps:
(1), measured respectively with graduated cylinder 0.0ml, 1.0ml, 2.0ml, 3.0ml, 4.0ml, 5.0ml, 6.0ml, 7.0ml, 8.0ml,
The arsenic standard solution of the 0.010mg/ml of 9.0ml and 10.0ml is placed in 50ml color range colorimetric cylinder；
(2), (1+1) hydrochloric acid is injected into 11 color range colorimetric cylinders respectively, is diluted at 10ml scale；
(3), the copper-bath and 5ml concentration that injection 1ml concentration is 100g/L into 11 color range colorimetric cylinders respectively are 300g/
The Lime Hypophosphate of L, shakes up；
(4), (1+1) hydrochloric acid is added into 11 color range colorimetric cylinders respectively to 25ml；
(5), 11 color range colorimetric cylinders are placed into 90 degrees Celsius of environment and are heated 7 minutes, it is cooling to remove rear flowing water.
8. the method for turbidimetry for Determination arsenic amount according to claim 1, step S7 include the following steps:
(1) color range colorimetric cylinder is arranged in a row placement according to the sequence of the content of arsenic standard solution, and sample colorimetric cylinder is put
It sets in the end side of a row；
(2) white shutter is chosen to place with color range colorimetric cylinder in parallel；
(3) visual color range colorimetric cylinder, carries out visually on the background board that white shutter is formed than turbid.
9. the method for turbidimetry for Determination arsenic amount according to claim 1, in step S8, include the following steps:
(1) once than two color ranges similar in sample turbidity in turbid processing, arsenic solution content is xml and (x+1) ml, dosage for selection
Cylinder measures as the arsenic of 0.010mg/ml x.1ml, x.2ml, x.3ml, x.4ml, x.5ml, x.6ml, x.7ml, x.8ml, x.9ml
Standard solution is placed in 50ml color range colorimetric cylinder；
(3) copper-bath and 5ml concentration that injection 1ml concentration is 100g/L into 9 color range colorimetric cylinders respectively are 300g/L
Lime Hypophosphate, shake up；
(4) (1+1) hydrochloric acid is added into 9 color range colorimetric cylinders respectively to 25ml；
(5) 9 color range colorimetric cylinders are placed into 90 degrees Celsius of environment and are heated 7 minutes, it is cooling to remove rear flowing water.
10. the method for turbidimetry for Determination arsenic amount according to claim 1, in step S10, select secondary than turbid processing neutralization
Standard color range similar in testing liquid turbidity records arsenic amount, and sample arsenic amount calculates: As (%)=[(m1*0.0000001/v1)/
(m0/v0)] * 100, wherein m1 be it is secondary than it is turbid when, the standard arsenic amount (unit: ug) that sample solution is equivalent to, v1 point takes
Sample solution volume (unit: ml), m0 are the gross masses (unit: g) of sample solution, v0 be sample solution total volume (unit:
ml)。
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| CN114295608A (en) * | 2021-12-31 | 2022-04-08 | 南京化学试剂股份有限公司 | Method for rapidly determining heavy metal in edetate disodium |
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