Liquor detection internal standard method

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Internal Standard Method for Liquor Analysis

This method is commonly used in the analysis of alcoholic beverages to ensure accurate quantification of compounds. The internal standard, typically n-butyl acetate, serves as a reference to correct for variations in sample preparation and instrument response.

Sample Preparation:

The internal standard is usually purchased as chromatographically pure n-butyl acetate. For the preparation, take 5 ml of this compound.

Preparation Steps:

  1. 60% Ethanol Preparation: Take 150 ml of anhydrous ethanol (chromatographically pure) and dilute it with purified water to a total volume of 250 ml.
  2. 2% Internal Standard Solution: Mix 5 ml of n-butyl acetate with 250 ml of the 60% ethanol solution prepared in step 1.
  3. Sample Preparation: Take 10 ml of the liquor sample and add 0.2 ml of the 2% internal standard solution. This results in an internal standard concentration of 35.28 mg/100 ml in the sample.

Instrumentation and Sampling:

Use a 10 µL microsyringe to inject 1 µL of the prepared sample into the gas chromatograph. It's important to note that when preparing the sample, the internal standard concentration should be adjusted accordingly.

Correction Factor Calculation:

Using a chromatography workstation such as N2000, you can calculate the correction factor by analyzing a mixed standard solution. This process helps in accurately determining the concentration of the target compounds in the sample.

Operational Steps:

  1. Load the Mixed Standard: Inject 1 µL of the standard solution into the online workstation, record and save the data under a name like "White Wine Standard A."
  2. Offline Processing: Open the standard file, adjust the integration settings, and manually set the baseline if needed. Enter peak names based on retention times and assign concentrations according to the labeled standards.
  3. Calibration Curve: Save the calibration curve with a suitable name, such as "Liquor Calibration Curve A."
  4. Sample Analysis: Load the calibration curve into the online workstation, input the internal standard concentration, and analyze the sample.
  5. Data Collection: Inject 1 µL of the sample, collect the data, and review the results. If peaks are not identified, adjust the retention time in the component table and reprocess the data.

This detailed procedure ensures consistent and reliable results in the analysis of alcoholic beverages using the internal standard method.

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