CN109580310A - Naphthalene-methanol solution standard substance preparation method - Google Patents
Naphthalene-methanol solution standard substance preparation method Download PDFInfo
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- CN109580310A CN109580310A CN201811619132.7A CN201811619132A CN109580310A CN 109580310 A CN109580310 A CN 109580310A CN 201811619132 A CN201811619132 A CN 201811619132A CN 109580310 A CN109580310 A CN 109580310A
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- naphthalene
- solution
- methanol
- methanol solution
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N2001/2893—Preparing calibration standards
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
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Abstract
The present invention provides naphthalene-methanol solution standard substance preparation methods, raw material is weighed using high Accuracy Electronic Balance, and gas chromatography-mass spectrometry can be qualitative simultaneously and quantitative to sample, and multiple restrictive condition is arranged to the concentration for preparing solution to filter out the standard solution closer to theoretical concentration value；Using relatively narrow standard curve range and repeatedly measurement, keep detectable concentration more accurate；And then using low dose of cooling package standard solution, the volatilization of solvent was both reduced, has ensured the accurate of concentration, and had in turn avoided dispensing the standard solution freezing bottle of large capacity into the risk that possible standard substance is precipitated again after refrigeration.The naphthalene prepared by the method-methanol solution standard substance, which uses, to be more convenient, and uses it more acurrate, reliable as calibrating analyte detection result.
Description
[technical field]
The present invention relates to standard solution fields, and in particular to a kind of preparation method of naphthalene-methanol solution standard substance.
[background technique]
Currently, most analytical reagents are molten according to standard specified in GB/T 15000 " standard sample work directive/guide "
The preparation method of liquid is prepared, but since national standard method is as a kind of regulatory documents, there is no for specific substance
Detailed operating instruction, and it is multifarious due to chemical substance property, and there were significant differences for the concentration of standard solution produced.
Naphthalene-methanol solution standard substance is used as Verification of Liquid Chromatograph solution reference material, the chemistry as known content
Ingredient standard is mainly used for the calibrating of high performance liquid chromatograph, ultraviolet-visible detector, diode array detector.Standard
The concentration of substance will be directly related to verification result.
[summary of the invention]
Based on this, it is necessary to provide a kind of preparation method of naphthalene-methanol solution standard substance, prepared standard solution
Concentration value uses user of service more convenient closer to theoretical value.
The technical problems to be solved by the invention are achieved by the following technical programs:
A kind of preparation method of naphthalene-methanol solution standard substance, comprising the following steps:
By pre-determined naphthalene-methanol concentration of standard solution value M0, calculate required naphthalene, methanol usage；With accurate electricity
Sub- balance weighs the naphthalene of calculation amount, is accurate to 0.00001 gram；
Naphthalene after weighing is dissolved in the methanol of calculation amount；
By the quality and actual methanol usage of practical weighed naphthalene, naphthalene-methanol solution compound concentration M is calculated1, and
M1With M0Between need to meet relationship: ∣ M1-M0∣/M0≤ 0.1%；
Through gas chromatography-mass spectrometry is qualitative and quantitative detection naphthalene-methanol solution concentration value, taken after five tests
Average value, and will be between 0.98 × M0~1.02 × M0Between average value as naphthalene-methanol solution detectable concentration M2；
After detecting, Fu He ∣ M2-M0∣/M0≤ 2.0% naphthalene-methanol solution is that the calibration concentration configured is M2Naphthalene-
Methanol solution standard substance.
It further include that the naphthalene-methanol solution standard substance that will be prepared is dispensed using ampoule bottle is cooling in above-mentioned preparation method
Step.
1. naphthalene provided by the invention-methanol solution standard substance preparation method has the following beneficial effects: using high-precision
Electronic balance, the concentration of standard solution value of preparation is closer to theoretical value；2. can be same to sample using gas chromatography-mass spectrometry
When it is qualitative and quantitative；3. keeping calibration concentration more accurate using relatively narrow standard curve range and repeatedly measurement；4. using small dose
Cooling package standard solution is measured, both reduced the volatilization of solvent, ensured the accurate of concentration, and in turn avoided the standard of large capacity
Solution freezing bottle dispenses the risk that possible standard substance is precipitated again after refrigeration.Naphthalene-the methanol prepared by the method
Solution reference material, which uses, to be more convenient, and uses it more acurrate, reliable as calibrating analyte detection result.
[Detailed description of the invention]
Fig. 1 is the naphthalene-methanol solution standard substance gas chromatogram prepared in the embodiment of the present invention 1.
[specific embodiment]
Naphthalene provided by the invention-methanol solution standard substance preparation method, comprising the following steps:
Concentration value preparing standard solution according to the rules；
It formulates and requires about standard solution referring to GB/T 15000 " standard sample work directive/guide ", calculate dense according to the rules
Spend M0Naphthalene quality, methanol usage needed for being worth preparing standard solution；
The naphthalene that calculation amount is weighed with precision electronic balance is accurate to 0.00001 gram, is dissolved in constant volume methanol；According to reality
The naphthalene quality that border weighs calculates naphthalene-methanol solution compound concentration value, that is, passes through the pure of the quality and naphthalene for weighing obtained naphthalene
Degree, methanol usage, calculate naphthalene-methanol solution compound concentration M1, compound concentration M1With normal concentration M0Between relationship need
It can continue subsequent step in the condition for meeting 0.1%≤(compound concentration value-normal concentration value)/normal concentration value≤0.1%
Suddenly；If M1With M0Between do not meet above-mentioned condition, then need to weigh naphthalene again, prepare solution and calculate M1Until making itself and M0Meet
Condition；
In compound concentration M1After meeting above-mentioned condition, gas chromatography-mass spectrometry is qualitative and quantitative detection naphthalene-methanol
The concentration value of solution, the result that sample is tested through five times is as average value, if the average value is in normal concentration value M0×(1±
2.0%) (that is, 0.98 × M in0≤ average value≤1.02 × M0), then using the average value as naphthalene-methanol solution detectable concentration
M2；If average value deviates from (1 ± 2.0%) × M0, then detectable concentration M must not be used as2；
For naphthalene-methanol detectable concentration M2, then need to further conform to detectable concentration value normal concentration value ±
Condition in 2.0% range, that is, | detectable concentration value-normal concentration value |/normal concentration value≤2.0%；It is only qualified
It could be as qualified naphthalene-methanol solution standard substance, qualified detectable concentration M2The calibration of the as standard substance is dense
Degree；The solution for not meeting the condition must not be used as standard solution.
Standard solution after qualification is distributed into finished product inner wrapping unit using ampoule bottle cooling, for using.
The present invention will now be described in detail with reference to examples.
Embodiment 1
Preparation specification is M0The naphthalene of=1.0mg/mL-methanol solution standard substance
Prepare solution: referring to GB/T 15000 " standard sample work directive/guide " about standard solution constituting criterion.Experiment institute
It is 99.8% with the purity of naphthalene, 0.10020 ± 0.00010g of naphthalene, methanol 100mL should be weighed by being computed；Actually use precise electronic
It 0.10028 gram of balance precise, after being completely dissolved with methanol, is transferred in the container of 100mL capacity, again with methanol constant volume,
It obtains and prepares solution；
Compound concentration value: M1=0.10028g × 0.998 × 103/ 100mL=1.0008mg/mL, in setting
Between 0.999mg/mL~1.001mg/mL；
It is computed, (M1-M0)/M0=(1.0008-1)/1=0.0008=0.08% < 0.1%, it is eligible；
Use gas chromatography-mass spectrometry qualitative and quantitative detection to solution is prepared, detection parameters are as follows:
The chromatogram of detection is as shown in Fig. 1.
It prepares solution to detect through five times, test data is as follows:
It is 0.99658mg/mL according to detectable concentration average value, since the average value is in M0± 2.0% range in, meet
Experiment imposes a condition, which is the detectable concentration value M for preparing solution2。
The present embodiment Zhong , ∣ M2-M0∣/M0=∣ 0.99658-1.0 ∣/1.0=0.00342=0.342% < 2%, therefore M2
Standardizing of solution concentration value is as configured, that is, the naphthalene prepared-methanol solution standard substance calibration concentration is 0.99658mg/mL.
After the completion of detection, qualified naphthalene-methanol solution standard substance is encapsulated using brown glass ampoules bottle, and cold
Hiding storage, for using.
Embodiment 2
Preparation specification is M0The naphthalene of=0.2mg/mL-methanol solution standard substance
Prepare solution: referring to GB/T 15000 " standard sample work directive/guide " about standard solution constituting criterion.Experiment institute
It is 99.8% with the purity of naphthalene, 0.20040 ± 0.00020g of naphthalene, methanol 1L should be weighed by being computed；It is practical to use precise electronic day
0.20028 gram of flat precise, after being completely dissolved with methanol, is transferred in the container of 1L capacity, and again with methanol constant volume is matched
Solution processed；
Compound concentration value: M1=0.20028g × 0.998 × 103/ 1000mL=0.19988mg/mL, in setting
Between 0.1998mg/mL~0.2002mg/mL；
It is computed , ∣ M1-M0∣/M0=∣ 0.19988-0.2 ∣/0.2=0.0006=0.06% < 0.1%, it is eligible；
Use gas chromatography-mass spectrometry qualitative and quantitative detection to solution is prepared, detection parameters and embodiment 1 are consistent,
It detects obtained chromatogram and embodiment 1 is close.
It prepares solution to detect through five times, test data is as follows:
It is 0.20048mg/mL according to detectable concentration average value, since the average value is in M0± 2.0% range in, meet
Experiment imposes a condition, which is the detectable concentration value M for preparing solution2。
The present embodiment Zhong , ∣ M2-M0∣/M0=∣ 0.20048-0.2 ∣/0.2=0.0024=0.24% < 2%, therefore M2I.e.
To configure standardizing of solution concentration value, that is, the naphthalene prepared-methanol solution standard substance calibration concentration is 0.10024mg/mL.
After the completion of detection, qualified naphthalene-methanol solution standard substance is encapsulated using brown glass ampoules bottle, and cold
Hiding storage, for using.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (2)
1. a kind of naphthalene-methanol solution standard substance preparation method, comprising the following steps:
By pre-determined naphthalene-methanol concentration of standard solution value M0, calculate required naphthalene, methanol usage；Use precision electronic balance
The naphthalene for weighing calculation amount is accurate to 0.00001 gram；
Naphthalene after weighing is dissolved in the methanol of calculation amount；
By the quality and actual methanol usage of practical weighed naphthalene, naphthalene-methanol solution compound concentration M is calculated1, and M1With
M0Between need to meet relationship: ∣ M1-M0∣/M0≤ 0.1%；
Through gas chromatography-mass spectrometry is qualitative and quantitative detection naphthalene-methanol solution concentration value, it is averaged after five tests
Value, and will be between 0.98 × M0~1.02 × M0Between average value as naphthalene-methanol solution detectable concentration M2；
After detecting, Fu He ∣ M2-M0∣/M0≤ 2.0% naphthalene-methanol solution is that the calibration concentration configured is M2Naphthalene-methanol
Solution reference material.
2. naphthalene according to claim 1-methanol solution standard substance preparation method, which is characterized in that further include that will match
The naphthalene of system-methanol solution standard substance is using ampoule bottle cooling the step of dispensing.
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| CN201811619132.7A CN109580310A (en) | 2018-12-28 | 2018-12-28 | Naphthalene-methanol solution standard substance preparation method |
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| CN201811619132.7A CN109580310A (en) | 2018-12-28 | 2018-12-28 | Naphthalene-methanol solution standard substance preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113030297A (en) * | 2021-02-19 | 2021-06-25 | 广东省计量科学研究院（华南国家计量测试中心） | 2,2',4,4' -tetrabromodiphenyl ether solution standard substance in methanol and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107290475A (en) * | 2016-04-13 | 2017-10-24 | 深圳市博林达科技有限公司 | A kind of preparation method of standard liquid |
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- 2018-12-28 CN CN201811619132.7A patent/CN109580310A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107290475A (en) * | 2016-04-13 | 2017-10-24 | 深圳市博林达科技有限公司 | A kind of preparation method of standard liquid |
Non-Patent Citations (1)
| Title |
|---|
| 张凌: "滴定分析概论", 《分析化学（上）》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113030297A (en) * | 2021-02-19 | 2021-06-25 | 广东省计量科学研究院（华南国家计量测试中心） | 2,2',4,4' -tetrabromodiphenyl ether solution standard substance in methanol and preparation method thereof |
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