Method of calibrating an analytical instrument

• US 5,552,997 A
• Filed: 07/14/1994
• Issued: 09/03/1996
• Est. Priority Date: 04/20/1990
• Status: Expired due to Term

• Current Assignee: Panalytical B.V. (Spectris PLC)
• Original Assignee: US Philips Corporation (Koninklijke Philips N.V.)
• Inventors: Massart, Desire J. L.
• Primary Examiner(s): Ramirez, Ellis B.
• Assistant Examiner(s): PEESO, THOMAS R
• Application Number:
  US08/275,099
• Time in Patent Office: 782 Days
• Field of Search: 364/496, 364/498, 364/571.01, 250/390.07, 250/393, 250/339.07, 250/339.09, 250/339.12, 250/341.5, 250/496
• US Class Current: 702/85
• CPC Class Codes: G01N 21/274 Calibration, base line adjustment, drift correction
• CPC Class Codes: G01N 21/3103 Atomic absorption analysis
• CPC Class Codes: G01N 2201/129 Using chemometrical methods

Abstract

A method of calibrating an analytical instrument, for example an atomic absorption spectrophotometer, comprises measuring the absorbance of a plurality of standards of known concentration (100) and plotting the measured absorbance against concentration (101). A straight line is fitted to the plotted points (102) and a quality co-efficient calculated (103). If the quality co-efficient is acceptable (104) the calibration line is used for measurement of samples (105). If not, then the slope of the line joining each point to the origin is determined and if the slopes are random (107) then a robust regression technique is used to fit the calibration line (108). If outliers are then detected (109) it is determined which points are outliers (110) and appropriate action taken, for example to restrict the range if the last point(s) is/are outliers (111). If the slopes determined in step (106) are not random, then, provided more than 4 points remain (113), the slope of each point with respect to the first point is determined (114). If they are again not random (115), then a curved calibration line is diagnosed, while if they are random, a straight line not passing through the origin is diagnosed (117). In atomic absorption spectroscopy, a straight line not passing through the origin indicates a problem with the blank solution, for example, a problem of contamination.

Claims

1. A method of calibrating an X-ray spectrometer comprising the steps of

(a) generating x-rays from at least one standard sample,

(b) measuring intensities of said x-rays for different concentrations of said standard sample,

(c) forming a representation of intensity versus concentration for each measured value of intensity with said different concentrations,

(d) determining if a best straight calibration line can be formed from said representation, and if not

(e) changing instrument parameters and/or sample preparation to achieve said best straight calibration line, and

(f) repeating said steps (a)-(d) to calibrate said x-ray spectrometer.

2. A method of calibrating according to claim 1, wherein at least four of said standard samples with different concentrations are used.

3. A method according to claim 2, wherein at most six of said standard samples with different concentrations are used.

4. A method according to claim 1, wherein at most six of said standard samples with different concentrations are used.

5. A method of calibrating an atomic absorption spectrophotometer comprising the steps of

(a) generating electrical signals from at least one standard sample,

(b) converting said electrical signals into absorbance values of said standard sample for different concentrations of said standard sample,

(c) forming a representation of absorbance versus concentration for each absorbance value with said different concentrations,

(d) determining if a best straight calibration line can be formed from said representation, and if not,

(e) changing instrument parameters and/or sample preparation to achieve said best straight calibration line, and

(f) repeating said steps (a)-(d) to calibrate said atomic absorption spectrometer.

6. A method of calibrating according to claim 5, wherein at least four of said standard samples with different concentrations are used.

7. A method according to claim 6, wherein at most six of six standard samples with different concentrations are used.

8. A method according to claim 6, wherein at most six of six standard samples with different concentrations are used.