CN108827944A - A kind of measuring method for lead, calcium, copper, nickel, ferro element in sulphur - Google Patents
A kind of measuring method for lead, calcium, copper, nickel, ferro element in sulphur Download PDFInfo
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- CN108827944A CN108827944A CN201810573200.4A CN201810573200A CN108827944A CN 108827944 A CN108827944 A CN 108827944A CN 201810573200 A CN201810573200 A CN 201810573200A CN 108827944 A CN108827944 A CN 108827944A
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
Abstract
The invention discloses a kind of measuring method for lead, calcium, copper, nickel, ferro element in sulphur, the measuring method includes the following steps：S1, sample is prepared；S2, sample solution is prepared；S3, the sample solution prepared in step S2 is formulated as to the test sample concentration for being suitble to laboratory test to use；S4, the working condition of ICP-AES instrument is adjusted to：Analyze 40 ~ 60r/min of pump speed, 1100 ~ 1200w of power, nebulizer gas 0.2 ~ 0.8L/min of flow, 10 ~ 15mm of Vertical Observation height；S5, it is measured using test sample of the ICP-AES instrument prepared in step S4 to the various concentration configured in step S3；This method is easy to operate, detection speed is fast, at low cost, accuracy and precision can satisfy the measurement requirement of lead, calcium, copper, nickel, iron content in inlet and outlet sulphur, have the advantages that detection cycle is short, result is accurate, save reagent and personnel's investment, it can satisfy the requirement that foreign trade quickly detects inspection and quarantine completely, with stronger practicability, can be widely used to promote.
Description
Technical field
The present invention relates to the detection of microelement and analysis field, more particularly to it is a kind of for lead in sulphur, calcium, copper,
The measuring method of nickel, ferro element.
Background technique
Sulphur purposes is very extensive, and food-grade sulphur is used for bleaching, anti-corrosion, mite killing and the sterilization of food, desinsection, industry
Grade sulphur is used for plastic cement, latex, papermaking, the industrial departments such as medical fine chemistry industry, industrial ceramics, building material auxiliary material；Together
When for manufacturing sulfuric acid, sulfur dioxide liquid etc., dye industry is also used for manufacture pesticide, firecracker for producing sulfur dye,
Sulphur powder is used as the vulcanizing agent of rubber, prevention and treatment powdery mildew.Medical research is it was demonstrated that sulphur itself and evil member contained in sulphur
Element has great injury to human body.Existing sulphur detection method mainly measures arsenic and iron, has researcher to study in sulphur
Lead, selenium, bismuth element not for lead, the calcium, copper, nickel-silicon nitride method in sulphur, and measure the method flow of ferro element
It is long, it is not able to satisfy requirement of the port detection unit to timeliness.
Summary of the invention
Object of the present invention is to solve the above problems, design it is a kind of can it is simple and quick to lead in sulphur, calcium, copper, nickel,
The measuring method that ferro element measures.
To achieve the goals above, the technical scheme is that：
A kind of measuring method for lead, calcium, copper, nickel, ferro element in sulphur, the measuring method include the following steps：
S1, sample is prepared；The sieve for being 145~155 μm by specification by sample, and will be placed by the sample of sieve
It is to dry to constant weight to be placed in drier in 100~110 DEG C of baking ovens to be cooled to room temperature in temperature；
S2, sample solution is prepared；The sample that 20g passes through step S1 preparation is weighed, 0.001g is accurate to, is placed on
Capacity is that porcelain crucible is placed on electronics universal furnace and is heated in ventilating kitchen in the porcelain crucible of 50ml, waits sulfur burning to the greatest extent
After be cooled to room temperature；Porcelain crucible lid is covered on porcelain crucible, is put into Muffle furnace and is burnt in the case where temperature is 550~650 DEG C of situation
25~35min is burnt, the hydrochloric acid of addition 12ml nitric acid and 15ml ultrapure water and 2ml after cooling is taken out, is placed on electronics universal furnace
It is slowly heated to residue to be completely dissolved, is moved into after cooling in the volumetric flask that capacity is 100ml and be settled to graduation mark with ultrapure water,
Then it is shaken up；
S3, the sample solution prepared in step S2 is formulated as to the test sample concentration for being suitble to laboratory test to use；
The preparation of S4, ICP-AES instrument；The working condition of ICP-AES instrument is adjusted to：Analysis pump speed 40~
60r/min, 1100~1200w of power, nebulizer gas 0.2~0.8L/min of flow, 10~15mm of Vertical Observation height；
S5, using the ICP-AES instrument prepared in step S4 to the test sample of the various concentration configured in step S3 into
Row measurement, and the intensity of spectral line that will test each element in sample is fabricated to element alignment working curve.
Further, a kind of measuring method for lead, calcium, copper, nickel, ferro element in sulphur, the measuring method include
Following steps：
S1, sample is prepared；The sieve for being 149 μm by specification by sample, and temperature will be placed on by the sample of sieve
It is cooled to room temperature to dry to constant weight to be placed in drier in 105 DEG C of baking ovens；
S2, sample solution is prepared；The sample that 20g passes through step S1 preparation is weighed, 0.001g is accurate to, is placed on
Capacity is that porcelain crucible is placed on electronics universal furnace and is heated in ventilating kitchen in the porcelain crucible of 50ml, waits sulfur burning to the greatest extent
After be cooled to room temperature；Porcelain crucible lid is covered on porcelain crucible, is put into Muffle furnace the calcination in the case where temperature is 600 DEG C of situation
30min takes out the hydrochloric acid of addition 12ml nitric acid and 15ml ultrapure water and 2ml after cooling, is placed on electronics universal furnace and slowly adds
Heat to residue is completely dissolved, and is moved into the volumetric flask that capacity is 100ml after cooling and is settled to graduation mark with ultrapure water, then will
It shakes up；
S3, the sample solution prepared in step S2 is formulated as to the test sample concentration for being suitble to laboratory test to use；
The preparation of S4, ICP-AES instrument；The working condition of ICP-AES instrument is adjusted to：Analyze pump speed 50r/
Min, power 1150w, nebulizer gas flow 0.5L/min, Vertical Observation height 12mm；
S5, using the ICP-AES instrument prepared in step S4 to the test sample of the various concentration configured in step S3 into
Row measurement, and the intensity of spectral line that will test each element in sample is fabricated to element alignment working curve.
Compared with prior art, the invention has the advantages and positive effects that：
Measuring method in the present invention is easy to operate, detection speed is fast, at low cost, and accuracy and precision can satisfy
The measurement requirement for importing and exporting lead in sulphur, calcium, copper, nickel, iron content, have detection cycle is short, result is accurate, save reagent and
The advantages of personnel put into, can satisfy the requirement that foreign trade quickly detects inspection and quarantine completely, have stronger practicability, energy
It is widely used to promote.
Specific embodiment
Below in conjunction with specific embodiments of the present invention, technical solution of the present invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts,
Any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
A kind of measuring method for lead, calcium, copper, nickel, ferro element in sulphur, the measuring method include the following steps：
S1, sample is prepared；The sieve for being 145~155 μm by specification by sample, and be by temperature is placed on by the sample of sieve
It dries to constant weight to be placed in drier in 100~110 DEG C of baking ovens and be cooled to room temperature；S2, sample solution is prepared；Weigh 20g process
The sample of step S1 preparation, is accurate to 0.001g, is placed in the porcelain crucible that capacity is 50ml, porcelain crucible is placed on electricity
It is heated in ventilating kitchen on sub- universal furnace, sulfur burning is waited to be cooled to room temperature to after using up；Porcelain crucible is covered on porcelain crucible
Lid is put into Muffle furnace 25~35min of calcination in the case where temperature is 550~650 DEG C of situation, 12ml nitre is added after taking out cooling
The hydrochloric acid of acid and 15ml ultrapure water and 2ml is placed on electronics universal furnace and is slowly heated to residue and is completely dissolved, and cooling moves back
Enter in the volumetric flask that capacity is 100ml and be settled to graduation mark with ultrapure water, is then shaken up；S3, by what is prepared in step S2
Sample solution is formulated as the test sample concentration for being suitble to laboratory test to use；The preparation of S4, ICP-AES instrument；It will
The working condition of ICP-AES instrument is adjusted to：Analyze 40~60r/min of pump speed, 1100~1200w of power, nebulizer gas stream
Measure 0.2~0.8L/min, 10~15mm of Vertical Observation height；S5, using the ICP-AES instrument prepared in step S4 to step
The test sample of the various concentration configured in S3 is measured, and the intensity of spectral line that will test each element in sample is fabricated to member
Plain calibration curve.
Embodiment one, a kind of measuring method for lead, calcium, copper, nickel, ferro element in sulphur, the measuring method include
Following steps：S1, sample is prepared；The sieve for being 145 μm by specification by sample, and temperature will be placed on by the sample of sieve
Degree is cooled to room temperature to dry to constant weight to be placed in drier in 100 DEG C of baking ovens；S2, sample solution is prepared；Weigh 20g process
The sample of step S1 preparation, is accurate to 0.001g, is placed in the porcelain crucible that capacity is 50ml, porcelain crucible is placed on electricity
It is heated in ventilating kitchen on sub- universal furnace, sulfur burning is waited to be cooled to room temperature to after using up；Porcelain crucible is covered on porcelain crucible
Lid is put into Muffle furnace the calcination 25min in the case where temperature is 550 DEG C of situation, 12ml nitric acid and 15ml is added after taking out cooling
The hydrochloric acid of ultrapure water and 2ml is placed on electronics universal furnace and is slowly heated to residue and is completely dissolved, and moves into capacity after cooling and is
It is settled to graduation mark with ultrapure water in the volumetric flask of 100ml, is then shaken up；S3, the sample solution that will be prepared in step S2
It is formulated as the test sample concentration for being suitble to laboratory test to use；The preparation of S4, ICP-AES instrument；By ICP-AES instrument
The working condition of device is adjusted to：Analyze pump speed 40r/min, power 1100w, nebulizer gas flow 0.2L/min, Vertical Observation
Height 10mm；S5, the test sample using the ICP-AES instrument prepared in step S4 to the various concentration configured in step S3
The intensity of spectral line for being measured, and will test each element in sample is fabricated to element alignment working curve.
Embodiment two, a kind of measuring method for lead, calcium, copper, nickel, ferro element in sulphur, the measuring method include
Following steps：S1, sample is prepared；The sieve for being 149 μm by specification by sample, and temperature will be placed on by the sample of sieve
Degree is cooled to room temperature to dry to constant weight to be placed in drier in 105 DEG C of baking ovens；S2, sample solution is prepared；Weigh 20g process
The sample of step S1 preparation, is accurate to 0.001g, is placed in the porcelain crucible that capacity is 50ml, porcelain crucible is placed on electricity
It is heated in ventilating kitchen on sub- universal furnace, sulfur burning is waited to be cooled to room temperature to after using up；Porcelain crucible is covered on porcelain crucible
Lid is put into Muffle furnace the calcination 30min in the case where temperature is 600 DEG C of situation, 12ml nitric acid and 15ml is added after taking out cooling
The hydrochloric acid of ultrapure water and 2ml is placed on electronics universal furnace and is slowly heated to residue and is completely dissolved, and moves into capacity after cooling and is
It is settled to graduation mark with ultrapure water in the volumetric flask of 100ml, is then shaken up；S3, the sample solution that will be prepared in step S2
It is formulated as the test sample concentration for being suitble to laboratory test to use；The preparation of S4, ICP-AES instrument；By ICP-AES instrument
The working condition of device is adjusted to：Analyze pump speed 50r/min, power 1150w, nebulizer gas flow 0.5L/min, Vertical Observation
Height 12mm；S5, the test sample using the ICP-AES instrument prepared in step S4 to the various concentration configured in step S3
The intensity of spectral line for being measured, and will test each element in sample is fabricated to element alignment working curve.
Embodiment three, a kind of measuring method for lead, calcium, copper, nickel, ferro element in sulphur, the measuring method include
Following steps：S1, sample is prepared；The sieve for being 155 μm by specification by sample, and temperature will be placed on by the sample of sieve
Degree is cooled to room temperature to dry to constant weight to be placed in drier in 110 DEG C of baking ovens；S2, sample solution is prepared；Weigh 20g process
The sample of step S1 preparation, is accurate to 0.001g, is placed in the porcelain crucible that capacity is 50ml, porcelain crucible is placed on electricity
It is heated in ventilating kitchen on sub- universal furnace, sulfur burning is waited to be cooled to room temperature to after using up；Porcelain crucible is covered on porcelain crucible
Lid is put into Muffle furnace the calcination 35min in the case where temperature is 650 DEG C of situation, 12ml nitric acid and 15ml is added after taking out cooling
The hydrochloric acid of ultrapure water and 2ml is placed on electronics universal furnace and is slowly heated to residue and is completely dissolved, and moves into capacity after cooling and is
It is settled to graduation mark with ultrapure water in the volumetric flask of 100ml, is then shaken up；S3, the sample solution that will be prepared in step S2
It is formulated as the test sample concentration for being suitble to laboratory test to use；The preparation of S4, ICP-AES instrument；By ICP-AES instrument
The working condition of device is adjusted to：Analyze pump speed 60r/min, power 1200w, nebulizer gas flow 0.8L/min, Vertical Observation
Height 15mm；S5, the test sample using the ICP-AES instrument prepared in step S4 to the various concentration configured in step S3
The intensity of spectral line for being measured, and will test each element in sample is fabricated to element alignment working curve.
Measuring method of the invention is in continuous mode, and for same sample, at least independent measurement twice, as a result takes it
Average value；And operate every time all under the same conditions with sample be measured in parallel analysis one blank test, by with blank
Test compares to obtain the measurement result of lead in sample, calcium, copper, nickel, iron content.
The following are the numerical value that the present invention measures in test：
Table 1 is the standard curve concentration (ppm) formulated in test
| Element term | Ca | Cu | Fe | Ni | Pb |
| Blank | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 |
| Standard curve 1 | 0.10 | 0.10 | 0.10 | 0.10 | 0.10 |
| Standard curve 2 | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 |
| Standard curve 3 | 5.00 | 5.00 | 5.00 | 5.00 | 5.00 |
| Standard curve 4 | 10.00 | 10.00 | 10.00 | 10.00 | 10.00 |
| Standard curve 5 | 50.00 | 50.00 | 50.00 | 50.00 | 50.00 |
Table 2 is the detection limit of measuring method in test
Table 3 is the accuracy (rate of recovery) of measuring method in test
Table 4 for test in institute's sample repeatability
It is proposed that ICP-AES method can quickly detect the content of lead in sulphur, calcium, copper, nickel, iron, ICP work
Temperature is relatively high, has very high sensitivity for analysis to most elements, and it is vortex state, the skin effect that becomes being consequently formed
The influence answered can generally achieve the 4-5 order of magnitude, argon gas is as work so that setting-out line shape range has very big extension
Make gas, the spectral background interference of generation can also be reduced accordingly.
Measuring method in the present invention is easy to operate, detection speed is fast, at low cost, and accuracy and precision can satisfy
The measurement requirement for importing and exporting lead in sulphur, calcium, copper, nickel, iron content, have detection cycle is short, result is accurate, save reagent and
The advantages of personnel put into, can satisfy the requirement that foreign trade quickly detects inspection and quarantine completely, have stronger practicability, energy
It is widely used to promote.
Claims (2)
1. a kind of measuring method for lead, calcium, copper, nickel, ferro element in sulphur, it is characterised in that：The measuring method includes
Following steps：
S1, sample is prepared；The sieve for being 145 ~ 155 μm by specification by sample, and temperature will be placed on by the sample of sieve
It is cooled to room temperature to dry to constant weight to be placed in drier in 100 ~ 110 DEG C of baking ovens；
S2, sample solution is prepared；The sample that 20g passes through step S1 preparation is weighed, is accurate to 0.001g, being placed on capacity is
In the porcelain crucible of 50ml, porcelain crucible is placed on electronics universal furnace and is heated in ventilating kitchen, waits sulfur burning cooling to after using up
To room temperature；Porcelain crucible lid is covered on porcelain crucible, be put into Muffle furnace in the case where temperature is 550 ~ 650 DEG C of situation calcination 25 ~
35min takes out the hydrochloric acid of addition 12ml nitric acid and 15ml ultrapure water and 2ml after cooling, is placed on electronics universal furnace and slowly adds
Heat to residue is completely dissolved, and is moved into the volumetric flask that capacity is 100ml after cooling and is settled to graduation mark with ultrapure water, then by it
It shakes up；
S3, the sample solution prepared in step S2 is formulated as to the test sample concentration for being suitble to laboratory test to use；
The preparation of S4, ICP-AES instrument；The working condition of ICP-AES instrument is adjusted to：Analyze 40 ~ 60r/ of pump speed
Min, 1100 ~ 1200w of power, nebulizer gas 0.2 ~ 0.8L/min of flow, 10 ~ 15mm of Vertical Observation height；
S5, it is surveyed using test sample of the ICP-AES instrument prepared in step S4 to the various concentration configured in step S3
It is fixed, and the intensity of spectral line that will test each element in sample is fabricated to element alignment working curve.
2. as described in claim 1 for the measuring method of lead, calcium, copper, nickel, ferro element in sulphur, it is characterised in that：It is described
Measuring method includes the following steps：
S1, sample is prepared；The sieve for being 149 μm by specification by sample, and be 105 by temperature is placed on by the sample of sieve
It dries to constant weight to be placed in drier in DEG C baking oven and be cooled to room temperature；
S2, sample solution is prepared；The sample that 20g passes through step S1 preparation is weighed, is accurate to 0.001g, being placed on capacity is
In the porcelain crucible of 50ml, porcelain crucible is placed on electronics universal furnace and is heated in ventilating kitchen, waits sulfur burning cooling to after using up
To room temperature；Porcelain crucible lid is covered on porcelain crucible, is put into Muffle furnace the calcination 30min in the case where temperature is 600 DEG C of situation, is taken out
The hydrochloric acid of 12ml nitric acid and 15ml ultrapure water and 2ml is added after cooling, is placed on electronics universal furnace that be slowly heated to residue complete
Fully dissolved moves into the volumetric flask that capacity is 100ml after cooling and is settled to graduation mark with ultrapure water, then shaken up；
S3, the sample solution prepared in step S2 is formulated as to the test sample concentration for being suitble to laboratory test to use；
The preparation of S4, ICP-AES instrument；The working condition of ICP-AES instrument is adjusted to：Analyze pump speed 50r/min, function
Rate 1150w, nebulizer gas flow 0.5L/min, Vertical Observation height 12mm；
S5, it is surveyed using test sample of the ICP-AES instrument prepared in step S4 to the various concentration configured in step S3
It is fixed, and the intensity of spectral line that will test each element in sample is fabricated to element alignment working curve.
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| CN201810573200.4A CN108827944A (en) | 2018-06-06 | 2018-06-06 | A kind of measuring method for lead, calcium, copper, nickel, ferro element in sulphur |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109799228A (en) * | 2019-03-21 | 2019-05-24 | 利尔化学股份有限公司 | Utilize the method for palladium element residual quantity in ICP-OES method measurement pinoxaden product |
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Application publication date: 20181116 |