CN1058083C - Standard sample of organic element microanalysis and its prepn. method - Google Patents
Standard sample of organic element microanalysis and its prepn. method Download PDFInfo
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- CN1058083C CN1058083C CN 96111347 CN96111347A CN1058083C CN 1058083 C CN1058083 C CN 1058083C CN 96111347 CN96111347 CN 96111347 CN 96111347 A CN96111347 A CN 96111347A CN 1058083 C CN1058083 C CN 1058083C
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- CN
- China
- Prior art keywords
- carboxylic acid
- microanalysis
- sulfamido
- standard specimen
- benzoic acids
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Abstract
The present invention relates to a standard sample for microanalysis of organic elements. The present invention is characterized in that the standard sample is composed of a carboxylic acid-benzoic acid substance only containing C, H and O and a sulfonamide substance only containing C, H, O, N and S; the standard sample is prepared by a dissolving method. The present invention is suitable for analyzing and testing substances with low N, content, low S content and high C content, such as coal, petroleum, synthetic high molecular materials, etc.
Description
The invention belongs to standard specimen of a kind of organic element microanalysis and preparation method thereof.
The basic skills of organic element microanalysis is to do the content that typical curve and day correction factor calculate unknown sample with standard model.Used standard model is that high-purity the organising of a class contains thing, can satisfy numerous organic mensuration requirements.But for coal, oil and some macromolecular materials, because their N, S constituent content are very low, and the C constituent content is higher, when measuring with existing standard specimen, the absolute magnitude of these elements has exceeded the range of linearity of standard of instruments curve, thereby has caused very big analytical error.
The standard model and preparation method thereof that the purpose of this invention is to provide the organic element microanalysis of a kind of low N, low S and high C content.
The object of the present invention is achieved like this: choose two kinds of organism that meet elemental microanalysis standard substance purity and stability requirement, combination by a certain percentage adopts the method for dissolving to prepare the standard specimen of desired content.
Standard specimen is formed its weight proportion by sulfamido material that only contains C, H, O, N, S element and the solid carboxylic acid benzoic acids material that only contains C, H, O element:
The solid carboxylic acid benzoic acids material that only contains C, H, O element: only contain the sulfamido material of C, H, O, N, S element=19: 1～7: 1.
The selection standard of aforesaid sulfamido and benzoic acids material is:
A. two class substance dissolves are in same solvent;
B. two class materials must meet the purity and the stability requirement of elemental microanalysis standard substance;
C. the sulfamido material that only contains C, H, O, N, S element must satisfy the element percentage composition of N and S simultaneously:
3％≤N≤20％ 5％≤S≤25％
The solid carboxylic acid benzoic acids material that only contains C, H, O element must satisfy the element percentage composition of C:
86％≥C＞60％
Aforesaid sulfamido material that contains C, H, O, N, S element can be C
6H
8N
2O
2S, C
10H
12N
4O
2S
2, C
14H
12N
4O
2S, C
12H
12N
2O
2S, C
12H
13N
3O
4S
2, C
13H
12N
2O
3SC
11H
12N
4O
3S, C
9H
9N
3O
2S
2, C
11H
11N
3O
2S, C
11H
13N
3O
3S.
Aforesaid solid carboxylic acid benzoic acids material that contains C, H, O element can be C
7H
6O
2, C
10H
12O
2, C
8H
8O
3, C
15H
12O
4
Preparation method of the present invention is as follows:
(1) selection standard that contains the sulfamido material of C, H, O, N, S element by above-mentioned and only contain the solid carboxylic acid benzoic acids material of C, H, O element is determined material;
(2) material of choosing carries out weighing by required proportioning;
(3) with the substance dissolves that takes by weighing in same solvent;
(4) control is heated to evaporating temperature and is: the minimum melting temperature or the sublimation temperature of solvent boiling point temperature＜evaporating temperature＜material, and stir on the limit, and the limit makes solvent evaporates;
(5) fully the volatilization after, grind to form the powder of granularity less than 0.15mm, put into exsiccator and be dried to constant weight;
(6) packing.
Aforesaid solvent must can dissolve the sulfamido material that only contains C, H, O, N, S element simultaneously and only contain the solid carboxylic acid benzoic acids material of C, H, O element, and chemical reaction does not take place, and is easy to volatilization.Solvent can be ethanol, acetone or ether.
The method of inspection of making standard specimen is as follows:
The product of making, adopt various analysis to measure, the result carries out data processing.Calculate its mean value and standard deviation, obtain the fiducial range of unbiased estimator; With the homogeneity of unary variance analysis verification sample and the consistance of distinct methods measurement result; With the consistance between T method of inspection checking mean value and the theoretical value; Assay is as meeting the requirement of micro analytical standards material, promptly by the theoretical value definite value that calculates.
The storage of standard specimen is that the product made is contained in dark, the sealable vial of bottleneck.Not the time spent, put into exsiccator.
Standard specimen of the present invention has following advantage:
1. do the typical curve of instrument under the synchronous mode determination of CHNS: the lower limit of N, S curve is by former minimum (absolute magnitude) 3 * 10
-2Be extended down to 3 * 10 under the mg
-3Mg, the upper limit of C curve is by being extended down to 10mg on former the highest (absolute magnitude) 7mg.
2. be used to do the day correction factor of instrument: coal series, coal transform the material that each product, petroleum series, synthesized polymer material and soil, catalyzer etc. contain low N, low S, all can obtain measurement result accurately.N, the S element is minimum can accurately measure (relative quantity) 30ppm, and the former index of instrument is (relative quantity) 200ppm.
3. cooperate the typical curve of making instrument with other pure organic standard specimen, the scope of each curve (absolute magnitude) is as follows:
N：3×10
-3mg-2mg C：3×10
-2mg-10mg O：3×10
-2mg-2mg
S：3×10
-3mg-2mg H：3×10
-2mg-1.2mg
The matching precision of each curve: Q 〉=0.9999
This curve is suitable for measuring: pure organism and metal complex, fertilizer, soil and agricultural product, various coals and coal converted product, oil and petrochemicals, plastics, rubber and synthon etc.
4. raw material is general reagent, obtains easily, and is easy to be refined to the purity that needs.
5. the preparation method is easy, and the cycle is short.Do not need any special instrument and equipment, cost is low.
6. be difficult for suction, volatilization and oxidation, good stability is easy to long-term the use and storage.
Most preferred embodiment of the present invention is as follows:
Embodiment 1
Take by weighing C
7H
6O
29.50000g and C
6H
8N
2O
2S 0.50000g puts into porcelain evaporating dishes, adds small amount of acetone it is dissolved fully, be heated to 60 ℃-70 ℃, make solvent evaporates while stirring, treat that solvent volatilizees fully after, put into a yard Nao mortar and be ground to granularity, put into exsiccator and be dried to constant weight, package spare less than 0.15mm.
This standard specimen is with the method for inspection check of standard specimen, and is consistent with the theoretical value that calculates.The composition of this standard specimen (weight percentage) is:
N％ C％ S％ H％ O％
0.81 67.49 0.93 4.94 25.82
Embodiment 2
Take by weighing C
7H
6O
210.00000g and C
6H
8N
2O
2S 1.00000g, all the other steps are with embodiment 1.The composition of this standard specimen (weight percentage) is:
N％ C％ S％ H％ O％
1.48 66.39 1.69 4.93 25.51
Embodiment 3
Take by weighing C
7H
6O
27.00000g and C
9H
9N
3O
2S
21.00000g all the other steps are with embodiment 1.The composition of this standard specimen (weight percentage) is:
N％ C％ S％ H％ O％
2.06 65.53 3.14 4.78 24.49
Embodiment 4
Take by weighing C
10H
12O
29.50000g and C
13H
12N
2O
3S 0.50000g adds small amount of ethanol it is dissolved fully, is heated to 80 ℃-90 ℃, and all the other steps are with embodiment 1.The composition of this standard specimen (weight percentage) is:
N％ C％ S％ H％ O％
0.51 72.31 0.58 7.22 19.38
Embodiment 5
Take by weighing C
10H
12O
28.00000g and C
9H
9N
3O
2S
21.00000g all the other steps are with embodiment 4.The composition of this standard specimen (weight percentage) is:
N％ C％ S％ H％ O％
1.83 69.72 2.79 6.95 18.72
Embodiment 6
Take by weighing C
10H
12O
29.00000g and C
13H
12N
2O
3S 1.00000g, all the other steps are with embodiment 4.The composition of this standard specimen (weight percentage) is:
N％ C％ S％ H％ O％
1.01 71.48 1.16 7.07 19.28
Embodiment 7
Take by weighing C
10H
12O
27.00000g and C
14H
12N
4O
2S 0.50000g, all the other steps are with embodiment 4.The composition of this standard specimen (weight percentage) is:
N％ C％ S％ H％ O％
1.24 72.00 0.71 7.15 18.90
Embodiment 8
Take by weighing C
15H
12O
49.50000g and C
9H
9N
3O
2S
20.50000g all the other steps are with embodiment 4.The composition of this standard specimen (weight percentage) is:
N％ C％ S％ H％ O％
0.82 68.90 1.26 4.66 24.36
Embodiment 9
Take by weighing C
15H
12O
411.00000g and C
9H
9N
3O
2S
21.00000g all the other steps are with embodiment 4.The composition of this standard specimen (weight percentage) is:
N％ C％ S％ H％ O％
1.37 67.97 2.09 4.62 23.94
Embodiment 10
Take by weighing C
8H
8O
37.00000g and C
14H
12N
4O
2S 1.00000g, all the other steps are with embodiment 4.The composition of this standard specimen (weight percentage) is:
N％ C％ S％ H％ O％
2.33 62.25 1.34 5.14 28.94
Embodiment 11
Take by weighing C
8H
8O
37.00000g and C
6H
8N
2O
2S 1.00000g, all the other steps are with embodiment 4.The composition of this standard specimen (weight percentage) is:
N％ C％ S％ H％ O％
2.03 60.49 2.33 5.22 29.93
Embodiment 12
Take by weighing C
15H
12O
411.00000g and C
10H
12N
4O
2S
21.00000g all the other steps are with embodiment 4.The composition of this standard specimen (weight percentage) is:
N％ C％ S％ H％ O％
1.64 67.96 1.88 4.68 23.84
Claims (6)
1. the standard specimen of an organic element microanalysis, it is characterized in that forming by solid carboxylic acid benzoic acids material that only contains C, H, O element and the sulfamido material that only contains C, H, O, N, S element, its weight proportion: the solid carboxylic acid benzoic acids material that only contains C, H, O element: sulfamido material=19 of containing C, H, O, N, S element: 1-7: 1, described selection standard that contains the solid carboxylic acid benzoic acids material of C, H, O element and only contain the sulfamido material of C, H, O, N, S element is:
A. two class substance dissolves are in same solvent;
B. two class materials must meet the purity and the stability requirement of elemental microanalysis standard substance;
C. the sulfamido material that only contains C, H, O, N, S element must satisfy the element percentage composition of N and S simultaneously:
3％≤N≤20％ 5％≤S≤25％
The solid carboxylic acid benzoic acids material that only contains C, H, O element must satisfy the element percentage composition of C:
86％≥C＞60％
2. the standard specimen of organic element microanalysis according to claim 1 is characterized in that described sulfamido material that contains C, H, O, N, S element can be C
6H
8N
2O
2S, C
10H
12N
4O
2S
2, C
14H
12N
4O
2S, C
12H
12N
2O
2S, C
12H
13N
3O
4S
2, C
13H
12N
2O
3S, C
11H
12N
4O
3SC
9H
9N
3O
2S
2, C
11H
11N
3O
2S, C
11H
13N
3O
3S.
3. the standard specimen of organic element microanalysis according to claim 1, the solid carboxylic acid benzoic acids material that it is characterized in that only containing C, H, O element can be C
7H
6O
2, C
10H
12O
2, C
8H
8O
3, C
15H
12O
4
4. the preparation method of the standard specimen of an organic element microanalysis as claimed in claim 1 is characterized in that:
(1) selection standard that contains the sulfamido material of C, H, O, N, S element according to described of claim 1 and only contain the solid carboxylic acid benzoic acids material of C, H, O element is determined material;
(2) material of choosing carries out weighing by the described proportioning of claim 1;
(3) with the substance dissolves that takes by weighing in same solvent;
(4) control is heated to evaporating temperature and is: the minimum melting temperature or the sublimation temperature of solvent boiling point temperature＜evaporating temperature＜material, and stir on the limit, and the limit makes solvent evaporates;
(5) fully the volatilization after, grind to form the powder of granularity less than 0.15mm, put into exsiccator and be dried to constant weight;
(6) packing.
5. the preparation method of the standard specimen of organic element microanalysis according to claim 4, it is characterized in that described solvent must simultaneously can dissolve the sulfamido material that only contains C, H, O, N, S element and only contain the solid carboxylic acid benzoic acids material of C, H, O element, and chemical reaction does not take place, be easy to volatilization.
6. according to the preparation method of the standard specimen of claim 4 or 5 described organic element microanalysis, it is characterized in that described solvent is ethanol, acetone or ether.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96111347 CN1058083C (en) | 1996-08-09 | 1996-08-09 | Standard sample of organic element microanalysis and its prepn. method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96111347 CN1058083C (en) | 1996-08-09 | 1996-08-09 | Standard sample of organic element microanalysis and its prepn. method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1173640A CN1173640A (en) | 1998-02-18 |
| CN1058083C true CN1058083C (en) | 2000-11-01 |
Family
ID=5121082
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 96111347 Expired - Fee Related CN1058083C (en) | 1996-08-09 | 1996-08-09 | Standard sample of organic element microanalysis and its prepn. method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1058083C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2894463A1 (en) * | 2014-01-13 | 2015-07-15 | PANalytical B.V. | Method of making a dry reference standard for X-ray fluorescence measurements |
-
1996
- 1996-08-09 CN CN 96111347 patent/CN1058083C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1173640A (en) | 1998-02-18 |
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