CN110118869A - The test method of water soluble hexavalent chromium in a kind of cement or clinker - Google Patents
The test method of water soluble hexavalent chromium in a kind of cement or clinker Download PDFInfo
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- CN110118869A CN110118869A CN201910470796.XA CN201910470796A CN110118869A CN 110118869 A CN110118869 A CN 110118869A CN 201910470796 A CN201910470796 A CN 201910470796A CN 110118869 A CN110118869 A CN 110118869A
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- cement
- clinker
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- hexavalent chromium
- soluble hexavalent
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 239000004568 cement Substances 0.000 title claims abstract description 75
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000010998 test method Methods 0.000 title claims abstract description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000011651 chromium Substances 0.000 claims abstract description 30
- 239000000706 filtrate Substances 0.000 claims abstract description 20
- 238000012360 testing method Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- KSPIHGBHKVISFI-UHFFFAOYSA-N Diphenylcarbazide Chemical compound C=1C=CC=CC=1NNC(=O)NNC1=CC=CC=C1 KSPIHGBHKVISFI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000002835 absorbance Methods 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 29
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 11
- 229910052804 chromium Inorganic materials 0.000 claims description 11
- 239000012086 standard solution Substances 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 3
- 238000002798 spectrophotometry method Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 230000008033 biological extinction Effects 0.000 claims 1
- 238000002242 deionisation method Methods 0.000 claims 1
- 238000011017 operating method Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 3
- 238000011088 calibration curve Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 8
- 239000004576 sand Substances 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- OTEKOJQFKOIXMU-UHFFFAOYSA-N 1,4-bis(trichloromethyl)benzene Chemical compound ClC(Cl)(Cl)C1=CC=C(C(Cl)(Cl)Cl)C=C1 OTEKOJQFKOIXMU-UHFFFAOYSA-N 0.000 description 1
- 208000005623 Carcinogenesis Diseases 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000036952 cancer formation Effects 0.000 description 1
- 231100000504 carcinogenesis Toxicity 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 239000011083 cement mortar Substances 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009313 farming Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/38—Concrete; Lime; Mortar; Gypsum; Bricks; Ceramics; Glass
- G01N33/383—Concrete or cement
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Medicinal Chemistry (AREA)
- Food Science & Technology (AREA)
- Ceramic Engineering (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention provides a kind of test methods of water soluble hexavalent chromium in cement or clinker, by being washed, being filtered by vacuum to the cement containing water soluble hexavalent chromium, clinker sample, it pipettes quantitative filtrate and diphenylcarbazide solution is added, (1+1) hydrochloric acid is utilized to adjust acidity, colour developing, the absorbance of solution is measured under 540nm wavelength, the concentration that chromium (VI) in solution is measured by calibration curve method, to obtain the content of Cr VI in sample.Compared with prior art, the test method of water soluble hexavalent chromium in cement or clinker provided by the invention, simplify the operating procedure and sample handling procedure of test, and unified the concentration and additional amount of operating procedure and substance when standard curve and sample construct, be conducive to the accuracy, the repeatability and reproducibility that improve test.
Description
Technical field
The invention belongs to cement detection technique fields, and in particular to the test of water soluble hexavalent chromium in a kind of cement or clinker
Method.
Background technique
Water soluble chromium refers to chromate or bichromate, and wherein chromium exists in the form of 6 valence states, referred to as Cr VI.Six
The harm of valence chromium: Cr VI toxicity is stronger, and once soil or underground water are by pollution of chromium, and soil is unable to farming, and underground water can not
It drinks；Cr VI can penetrate cell membrane, have strong oxidation, can seriously damage the alimentary canal, respiratory tract, skin of human body
And mucous membrane, or even have carcinogenesis；Therefore, particularly important to the detection of water soluble hexavalent chromium.
Currently, for Cr VI in cement test method referring especially to the test method in GB 31893-2015 national standard,
The method is that cement sample, normal sand and water are stirred into cement mortar, is filtered, and diphenylcarbazide is added in filtrate, is adjusted
Acidity, colour developing measure the absorbance of solution at 540nm, chromium in solution (VI) concentration are checked on working curve.The method
In, the dosage of cement and normal sand is larger, and needs that cement sample, normal sand and water are first stirred into cement gel before test
Sand, operating process is complex, and the adhesiveness for forming cement after glue sand increases, and difficulty increases when suction filtration.And the method exists
During working curve and sample test, operating process disunity (concentration and additional amount of such as hydrochloric acid), operation is relatively complicated,
And quantitative control cannot be accurately carried out during sample test, will affect the repeatability and reproduction of test in this way
Property.
Summary of the invention
In order to solve the above technical problems, being surveyed the present invention provides a kind of test method of water soluble hexavalent chromium in cement
Before examination without using normal sand carry out the preparation of glue sand, and using less cement sample achieve that it is accurately testing as a result,
And when standard curve constructs and carries out sample test, method and step high unity, without preparing the hydrochloric acid of various concentration repeatedly
Solution simplifies operation and sample handling procedure, reduces testing cost.
The technical scheme adopted by the invention is as follows:
The test method of water soluble hexavalent chromium in a kind of cement or clinker, the test method the following steps are included:
(1) diphenyl carbazide spectrophotometry is utilized, measures the sexavalence chromium standard solution of various concentration at 540nm
Absorbance draws standard curve；
(2) cement is directly dispersing in deionized water, is filtered after stirring, resulting filtrate utilizes diphenylcarbazide point
Light photometry measures its absorbance at 540nm；And the concentration of Cr VI is read from standard curve；
(3) content of the water soluble hexavalent chromium in cement or clinker is calculated.
Further, the test method specifically includes the following steps:
(1) concentration for pipetting 0mL, 1.0mL, 2.0mL, 5.0mL, 10.0mL and 15.0mL respectively is the Cr VI of 5mg/L
Standard solution is diluted to 25mL into 50mL volumetric flask, with deionized water, sequentially add 5.0mL diphenylcarbazide solution and
2mL hydrochloric acid solution is diluted to graticule with deionized water, shakes up, and the absorbance of system at 540nm is measured after placement 15min, is drawn
Standard curve；
(2) cement or clinker are distributed in deionized water according to mass volume ratio (g:mL)=1:2, filter, pipettes 5mL
Filtrate is diluted with water to 25mL into 50mL volumetric flask, sequentially adds 5.0mL diphenylcarbazide solution and 2mL hydrochloric acid is molten
Liquid is diluted to graticule with deionized water, shakes up, and places after 15min with the absorbance of system at 540nm, and from standard curve
Read the concentration of Cr VI；
(3) content of the water soluble hexavalent chromium in cement or clinker is calculated.
Further, the step (2) specifically includes the following steps:
50g cement or clinker are distributed in 100mL deionized water, filters, pipettes 5mL filtrate into 50mL volumetric flask,
It is diluted with water to 25mL, 5.0mL diphenylcarbazide solution and 2mL hydrochloric acid solution is sequentially added, is diluted to deionized water
Graticule shakes up, and places after 15min with the absorbance of system 540nm at, and from standard curve reading Cr VI concentration.This
By cement and deionized mass volume ratio it is preferably 50g:100mL in step, result can be made to be rounded when calculating in this way, at this time
In step (3), the calculation formula of the content of the water soluble hexavalent chromium in cement or clinker is W=20c, wherein W- cement is ripe
The content of water soluble hexavalent chromium in material, unit mg/kg；Chromium (VI) in the cement checked on c- standard curve or clinker filtrate
Concentration, unit are milligrams per liter (mg/L), and the accuracy of calculating can be improved in this way.
In step (1) and step (2), the hydrochloric acid solution the preparation method comprises the following steps: by mass fraction be 36~38% salt
Acid and deionized water are mixed to get according to the volume ratio of 1:1.
In step (2), the suction filtration refers to being filtered by vacuum by vacuum pump using 0.45 μm of water system filter membrane.
In step (3), the calculating of the content of the water soluble hexavalent chromium in cement or clinker is carried out referring to following formula:
The content of water soluble hexavalent chromium in W- cement or clinker, unit mg/kg；
Chromium (VI) concentration in the cement checked on c- standard curve or clinker filtrate, unit are milligrams per liter (mg/L)；
V3The volume of volumetric flask, unit mL；
V2The filtrate volume pipetted, unit mL；
V1Disperse the volume of deionized water used in cement or clinker, unit mL；
The quality of m- cement or clinker sample, unit g.
The present invention is pipetted quantitative by washing, being filtered by vacuum to the cement containing water soluble hexavalent chromium, clinker sample
Diphenylcarbazide solution is added in filtrate, utilizes (1+1) hydrochloric acid to adjust acidity, colour developing, the suction of solution is measured under 540nm wavelength
Luminosity measures the concentration of chromium (VI) in solution by calibration curve method, to obtain the content of Cr VI in sample.
The operating procedure of the test method of water soluble hexavalent chromium is simple in cement or clinker provided by the invention, sample treatment
In the process it is not necessary that normal sand is added, it is only necessary to cement is dispersed directly into deionized water, and control cement and deionized water
Mass volume ratio be 1:2, that is, can guarantee that the water soluble hexavalent chromium in cement is fully dissolved out, and operating procedure according to the invention
After operation, the concentration of the water soluble hexavalent chromium in filtrate is just controlled in the range of linearity of standard curve, in this way according to standard
The concentration for the water soluble hexavalent chromium that the linear equation of curve can be calculated in filtrate simultaneously calculates the water solubility six in sample
The content of valence chromium.
Compared with prior art, in cement or clinker provided by the invention water soluble hexavalent chromium test method, simplify
The operating procedure and sample handling procedure of test, and unified when standard curve and sample construct the dense of operating procedure and substance
Degree and additional amount are conducive to the accuracy, the repeatability and reproducibility that improve test.
Specific embodiment
The following describes the present invention in detail with reference to examples.
It is involved in the present invention as follows to instrument, each substance or its preparation method:
Hydrochloric acid solution: the hydrochloric acid of excellent pure grade mass fraction 36%~38% is mixed according to the volume ratio of 1:1 with distilled water
Uniformly, (1+1) hydrochloric acid can be obtained；
Acetone: analysis is pure；
Cr VI cement standard product: water soluble chromium (VI) content standard sample in GSB 08-2988-2017 cement, mark
Quasi- value is 6.07mg/kg；
Sexavalence chromium standard solution: the potassium bichromate of excellent pure grade is dried into 2h in 140 ± 5 DEG C of baking ovens, then weighs drying
Potassium bichromate 0.1414g afterwards is diluted with water to graticule with being transferred in 1000mL volumetric flask after a small amount of deionized water dissolving,
It shakes up, concentration 50mg/L；
Diphenylcarbazide solution: weighing 0.125g diphenylcarbazide, with 20ml acetone solution, is transferred to 50mL capacity
In bottle, it is diluted to graticule with acetone, is shaken up, it is ready-to-use；
Water soluble chromium (VI) analyzer in cement: CR 2015-1, national cement quality supervision and check center；
Vacuum pump, bottle,suction, 0.45 μm of water system filter membrane.
Embodiment 1
The test method of water soluble hexavalent chromium in a kind of cement or clinker, comprising the following steps:
(1) it pipettes in sexavalence chromium standard solution 5.0mL to 100mL volumetric flask, is diluted with water to graticule, shakes up, obtain
5mg/L standard sexavalence solution.Pipette 5mg/L standard sexavalence solution 0mL, 1.0mL, 2.0mL, 5.0mL, 10.0mL and 15.0mL points
It is not put into 50mL volumetric flask, is diluted with water to 25mL, sequentially add 5.0mL diphenylcarbazide solution and 2mL (1+1) salt
Acid solution is diluted with water to graticule, shakes up；It is measured after placing 15min with spectrophotometer, line blank of going forward side by side is tested to survey
Test result is corrected, and the results are shown in Table 1, draws standard curve.
Table 1
(2) two parts of 50.0g Cr VI cement standard product are weighed respectively and two parts of 50.0g cement samples are burnt in four 250mL
In cup, 100.0mL water is added, 1~2min is stirred evenly and continued with glass bar or magneton, 0.45 μm of water is utilized by vacuum pump
It is that filter membrane is filtered by vacuum, pipettes 5.0mL filtrate and be put into 50mL volumetric flask, add water to 25mL or so, 5.0mL hexichol is added
Two hydrazine solution of phosphinylidyne is added 2mL (1+1) hydrochloric acid solution, is diluted with water to graticule, shakes up, and after placing 15min, uses spectrophotometric
Meter is measured at 540nm, and line blank of going forward side by side experiment is corrected test result, Cr VI cement standard product and cement-like
The measurement result of product is respectively as shown in table 2, table 3.
(3) according to formulaThe content of the water soluble hexavalent chromium in cement sample is calculated, wherein
The content of water soluble hexavalent chromium in W- cement or clinker, unit mg/kg；
Chromium (VI) concentration in the cement checked on c- standard curve or clinker filtrate, unit are milligrams per liter (mg/L)；
V3The volume of volumetric flask, 50mL；
V2The filtrate volume pipetted, 5mL；
V1Disperse the volume of deionized water used in cement or clinker, 100mL；
The quality of m- cement or clinker sample, 50g.
The test method of blank test in above-mentioned steps are as follows: when being added without sample, according to same as above-mentioned steps
Method tested.
2 Cr VI cement standard product test result of table
3 cement sample result of table
It can be seen that no matter test method provided by the invention is to Cr VI cement standard product or water from table 2 and table 3
The collimation of the test result of mud sample product is preferable, and the parallel misalignments of Cr VI cement standard product is 0, cement sample it is parallel
Sexual deviation controls within 0.05mg/kg, it is seen that the reliability of test method provided by the invention, repeatability and reproducibility compared with
Good, repeatability limit and the reproducibility limit being all satisfied in GB 31893-2015 require.
The above-mentioned detailed description carried out referring to test method of the embodiment to water soluble hexavalent chromium in a kind of cement or clinker,
It is illustrative without being restrictive, several embodiments can be enumerated according to limited range, therefore do not departing from this hair
Change and modification under bright general plotting should belong within protection scope of the present invention.
Claims (7)
1. the test method of water soluble hexavalent chromium in a kind of cement or clinker, which is characterized in that the test method includes following
Step:
(1) diphenyl carbazide spectrophotometry is utilized, extinction of the sexavalence chromium standard solution of various concentration at 540nm is measured
Degree draws standard curve；
(2) cement is directly dispersing in deionized water, is filtered after stirring, resulting filtrate is divided light using diphenylcarbazide
Degree method measures its absorbance at 540nm；And the concentration of Cr VI is read from standard curve；
(3) content of the water soluble hexavalent chromium in cement or clinker is calculated.
2. the test method of water soluble hexavalent chromium in cement according to claim 1 or clinker, which is characterized in that the survey
Method for testing the following steps are included:
(1) concentration for pipetting 0mL, 1.0mL, 2.0mL, 5.0mL, 10.0mL and 15.0mL respectively is the Cr VI standard of 5mg/L
Solution is diluted to 25mL into 50mL volumetric flask, with deionized water, sequentially adds 5.0mL diphenylcarbazide solution and 2mL
Hydrochloric acid solution is diluted to graticule with deionized water, shakes up, and the absorbance of system at 540nm is measured after placement 15min, draws mark
Directrix curve；
(2) cement or clinker are distributed in deionized water according to mass volume ratio (g:mL)=1:2, filter, pipettes 5mL filtrate
Into 50mL volumetric flask, it is diluted with water to 25mL, sequentially adds 5.0mL diphenylcarbazide solution and 2mL hydrochloric acid solution, is used
Deionized water is diluted to graticule, shakes up, and places after 15min with the absorbance of system at 540nm, and six are read from standard curve
The concentration of valence chromium；
(3) content of the water soluble hexavalent chromium in cement or clinker is calculated.
3. the test method of water soluble hexavalent chromium in cement according to claim 2 or clinker, which is characterized in that the step
Suddenly (2) specifically includes the following steps:
50g cement or clinker are distributed in 100mL deionized water, is filtered, is pipetted 5mL filtrate into 50mL volumetric flask, use water
It is diluted to 25mL, sequentially adds 5.0mL diphenylcarbazide solution and 2mL hydrochloric acid solution, is diluted to graticule with deionized water,
Shake up, place after 15min with the absorbance of system 540nm at, and from standard curve reading Cr VI concentration.
4. the test method of water soluble hexavalent chromium in cement according to claim 2 or 3 or clinker, which is characterized in that step
Suddenly in (1) and step (2), the hydrochloric acid solution the preparation method comprises the following steps: by mass fraction be 36~38% hydrochloric acid and deionization
Water is mixed to get according to the volume ratio of 1:1.
5. the test method of water soluble hexavalent chromium in cement according to claim 2 or 3 or clinker, which is characterized in that step
Suddenly in (2), the suction filtration refers to being filtered by vacuum by vacuum pump using 0.45 μm of water system filter membrane.
6. the test method of water soluble hexavalent chromium in cement according to claim 1 or 2 or clinker, which is characterized in that step
Suddenly in (3), the calculating of the content of the water soluble hexavalent chromium in cement or clinker is carried out referring to following formula:
The content of water soluble hexavalent chromium in W- cement or clinker, unit mg/kg；
Chromium (VI) concentration in the cement checked on c- standard curve or clinker filtrate, unit are milligrams per liter (mg/L)；
V3The volume of volumetric flask, unit mL；
V2The filtrate volume pipetted, unit mL；
V1Disperse the volume of deionized water used in cement or clinker, unit mL；
The quality of m- cement or clinker sample, unit g.
7. the test method of water soluble hexavalent chromium in cement according to claim 3 or clinker, which is characterized in that step
(3) in, the calculation formula of the content of the water soluble hexavalent chromium in cement or clinker is W=20c, wherein in W- cement or clinker
The content of water soluble hexavalent chromium, unit mg/kg；
Chromium (VI) concentration in the cement checked on c- standard curve or clinker filtrate, unit are milligrams per liter (mg/L).
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Cited By (4)
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| CN110672540A (en) * | 2019-11-19 | 2020-01-10 | 长春黄金研究院有限公司 | Method for determining hexavalent chromium in solid waste |
| CN110895241A (en) * | 2019-11-07 | 2020-03-20 | 广东弘朝科技有限公司 | Method for measuring high-temperature stability of hexavalent chromium reducing agent for cement |
| CN113533311A (en) * | 2020-04-16 | 2021-10-22 | 内蒙古第三地质矿产勘查开发有限责任公司 | Method for measuring content of hexavalent chromium in soil or solid waste |
| CN113899735A (en) * | 2021-11-25 | 2022-01-07 | 山东省产品质量检验研究院 | Automatic determination system and method for water-soluble hexavalent chromium in cement |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110895241A (en) * | 2019-11-07 | 2020-03-20 | 广东弘朝科技有限公司 | Method for measuring high-temperature stability of hexavalent chromium reducing agent for cement |
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| CN113899735A (en) * | 2021-11-25 | 2022-01-07 | 山东省产品质量检验研究院 | Automatic determination system and method for water-soluble hexavalent chromium in cement |
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