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Nuclear magnetic resonance spectrometer
(1) The purity of the sample to be inspected should generally be >95%, without impurities such as iron filings, dust, filter paper and hair. The amount of sample to be provided for general organic matter: 1H spectrum > 5 mg, 13 C spectrum > 15 mg, 10ml GC vials and the amount of sample required for the polymer should be appropriately increased.
(2) The instrument configuration can only carry out liquid sample analysis, and the sample is required to have good solubility in a certain deuterated solvent. The sampler should first select the solvent to be used. The deuterated solvents commonly used in this room are chloroform, heavy water, methanol, acetone, DMSO, benzene, o-dichlorobenzene, acetonitrile, pyridine, acetic acid, trifluoroacetic acid.
(3) Please ask the sampler to provide the possible structure or source of the sample. If you have special requirements (such as temperature, spectrum width, etc.) please explain.
2. Infrared spectrometer
In order to protect the instrument and ensure the quality of the infrared spectrum of the sample, the samples sent to the instrument for analysis must be:
(1) The sample must be pre-purified to ensure sufficient purity;
(2) The sample must be dehydrated in advance to avoid damage to the instrument and avoid interference of the water peak on the sample spectrum;
(3) Samples that are easy to deliquesce, please place your own dryer;
(4) For volatile, sublimated, heat-labile samples, please cover and close the container with a sealing cap or stopper, and must be indicated on the sample analysis task list;
(5) For toxic and corrosive samples, the user must install it in a sealed container. The samples must be marked separately on the approximate location of the vial label and on the analysis worksheet.
3. Organic mass spectrometer
It is suitable for the analysis of liquid and solid organic compound samples with a relative molecular mass of 50~2000 μ. The sample should be as pure a single component as possible.
4. Gas chromatography-mass spectrometer 10ml GC vials
The gas chromatograph uses a capillary column (a packed column cannot be used).
The sample entering the GC oven must be fully vaporized over the operating temperature range of the column.
5. Liquid chromatography-mass spectrometer
(1) Flammable, explosive, poisonous, corrosive samples must be noted.
(2) In order to ensure accurate and reliable analysis results, the sample is required to be completely dissolved, and no mechanical impurities are required; please refer to the solvent for the sample that is not formulated into a solution, and the concentration of the sample that has been formulated into the solution.
(3) Please provide the structural formula, molecular weight or functional group of the sample as much as possible in order to select the ionization method; if there are special requirements, please provide specific experimental conditions.
(4) When liquid chromatography-mass spectrometry is used, all buffer systems are uniformly formulated with a volatile buffer such as acetic acid, ammonium acetate, tetrabutylammonium hydroxide or the like. For those who require quantitative analysis, please provide a standard reference.
6. Flight time mass spectrometer
The instrument is good at measuring peptides and proteins, and can also measure other biological macromolecules such as polysaccharides, nucleic acids and high molecular polymers, synthetic oligomers and some organic substances with relatively small molecular weight, such as grafts of C60 or C60. The sample to be tested may be a single component or a multi-component, but the more sample components, the more complex the spectrum and the more difficult the spectrum analysis; if there is mutual inhibition between the components during the ionization process , it does not necessarily guarantee that each component has a peak. The amount of sample conventionally measured is about 1 to 10 picomoles per microliter.
(2) Solubility of the sample
The sample to be tested must be soluble in a suitable solvent, preferably an undissolved solid or pure liquid; if the sample is a solution, information such as the solvent, concentration or content of the sample should be provided.
For high quality mass spectra, peptide and protein samples should be protected from sodium chloride, calcium chloride, potassium hydrogen phosphate, trinitrotoluene, dimethyl sulfoxide, urea, glycerol, Tween, sodium lauryl sulfate. Wait. If the sample to be tested cannot avoid the above reagents during the pretreatment, the sample must be purified by dialysis and high performance liquid chromatography. Water, ammonium bicarbonate, ammonium acetate, ammonium formate, acetonitrile, trifluoroacetic acid, and the like are all suitable reagents for purifying the sample. After purification of the protein sample, it should be lyophilized as much as possible. The salt in the sample can be removed by ion exchange.
7. UV-visible absorption spectrometer
(1) The concentration of the sample solution must be appropriate and must be clear and transparent, without the presence of bubbles or suspended matter;
(2) The amount of solid sample is >0.2 g, and the amount of liquid sample is >2 mL;
8. Gas Chromatograph
Samples that can be directly analyzed should be volatile and thermally stable. The boiling point is generally not more than 300 ° C. If it cannot be directly injected, it needs to be pretreated.
9. Liquid chromatograph
To dry the sample, it is best to provide the structure of the component to be tested; for complex samples, provide as much of the other components as possible in the sample.
10. Elemental Analyzer
(1) Fill in the elemental analysis sample registration form and provide the theoretical content of the formula and elements or other relevant information as much as possible;
(2) The sample must be a uniform solid particle or liquid containing no adsorbed water and purified. For example, the sample is impure (including: adsorbed water, organic solvent, inorganic salt or other impurities), which will affect the analysis result and make the test value and The calculated value does not match;
(3) The sample should be of sufficient quantity to meet the linearity and sensitivity of the method and instrument.
11. Ion chromatograph
The sample to be tested may be dissolved in water, or dilute acid or dilute alkali, and the acid or base used may not contain the ions to be tested. For compounds containing the element to be tested in the sample but present in a non-ionic state in water, acid or alkali solution, the corresponding sample preparation is required.
12. Plasma atomic emission spectrometer
(1) Requirements for samples to be tested (test conditions):
1 Please inform the source, type, and properties (eg, ore, alloy, silicate, special solid solution, high polymer, etc.).
List the main ingredients, impurity components and their (estimated) content as much as possible; what is the lowest (estimated) content of the elements to be tested? For the solution, please specify the medium composition (solvent, type of acid and base and its (estimated) content) Fluorine (F-) or not, because fluorine (F-) will seriously corrode the atomizer!
2 The solid sample is prepared into a solution containing no organic matter, and the final acidity is controlled to be 1 mol, and the sample amount is 5 to 50 mL.
For example, if it contains suspended solids or sediment, be sure to filter it; please also send the reagent blank solution to deduct the blank, this is no charge!
3 samples are required to be processed into a solution before being sent to the test center.
(2) Due to conditions, the following elements and certain substances cannot be analyzed:
1 The sample is heated and dissolved when acid is dissolved (for example, B, Hg, S-2, Se and Si when dissolved with hydrofluoric acid (HF));
2 ceramics, glass and other inorganic acid can not be dissolved, only alkali fusion;
3 silicone, silicone rubber, plastic products, fibers or any ashing within 500 ° C, and subsequent acid digestion;
A. Volatile loss;
B. Those who cannot be ashed or insoluble (eg, B, Bi, Ge, Hg, Os, Ru, Sb, Se, Sn, Tl and Si when dissolved with hydrofluoric acid (HF); special solid solution, Polymers, etc.)
13. Atomic Fluorescence Spectrometer
(1) General requirements for sample analysis
The objects analyzed by atomic fluorescence spectrometry are arsenic (As), selenium (Se), germanium (Ge), tellurium (Te), etc. and mercury (Hg) atoms in the ionic state. The sample must be an aqueous solution or soluble in acid.
(2) Solid sample
1 inorganic solid sample, the sample is properly dissolved to maintain the proper acidity:
Detection of arsenic (As), selenium (Se), strontium (Te), mercury (Hg), the medium is hydrochloric acid (5%, v / v);
Detection of germanium (Ge), the medium is sulfuric acid (5%, v/v);
Detection of mercury (Hg), the medium may also be nitric acid (5%, v/v), and the detection (As) medium may also be sulfuric acid (2%, v/v);
Since copper, silver, gold, platinum and other metals interfere with the elements to be tested, arsenic, selenium, tellurium and mercury in the alloy samples should not be measured by the instrument.
2 organic or biological solid samples
The sample is nitrated to a solution and maintains the proper acidity, and the acidity of the medium is the same as that of the inorganic sample.
(3) Limit requirements of the elements to be tested in the sample
Determined by the sensitivity and analytical method of the instrument, the upper and lower limits of the sample containing the test element are 0.05 μg/g ~ 500 μg/g. Samples not in this range will not be able to guarantee the accuracy and reliability of the test results.
(4) Sample size
For each element tested, the amount of solid sample is not less than 2 g, the amount of liquid sample is not less than 20 mL, and the water sample is not less than 100 mL.
Please check the relevant literature before sending samples and try to provide relevant information.
14. Differential scanning calorimeter
Solid samples do not decompose or sublime over the temperature range tested, nor are volatiles produced.
Sample size: a single test of inorganic or organic materials of not less than 20mg, the drug is not less than 5mg. Please indicate the test conditions (including: detection temperature range, rising and cooling rate, constant temperature time, etc.) when delivering samples.
15. Thermogravimetric Analyzer
Sample amount: not less than 30 mg. Please indicate the detection temperature range, experimental atmosphere (air, N2 or Ar), heating rate, gas flow rate (if special requirements are required).
16.X-ray powder diffractometer 10ml GC vials
The sample to be inspected may be in the form of a powder, a block, a film, and the like. The powder sample needs to be about 0.2g (depending on its density and diffraction ability); the bulk sample requires an approximate plane with an area of ??less than 45px x 45px; the film sample requires a certain thickness, the area is less than 45px x 45px; other samples can be Consult the laboratory.
This is the end of the introduction of Requirements for test samples from 21 analytical instruments commonly used in laboratories I hope it can help you.