Method of quantifying performance chemicals in pulp and paper

• US 5,680,320 A
• Filed: 05/18/1995
• Issued: 10/21/1997
• Est. Priority Date: 05/18/1994
• Status: Expired due to Term

• Current Assignee: EKA Chemicals AB (Nouryon BV)
• Original Assignee: Eka Nobel AB
• Inventors: Renberg, Lars, Olsson, Ralf, Helmer, Ulla
• Primary Examiner(s): Trammell, James P.
• Application Number:
  US08/444,053
• Time in Patent Office: 887 Days
• Field of Search: 364/497-499, 364/571.01-571.05, 364/571.06-577, 364/581, 364/582, 364/469.01, 364/471.01, 364/471.02, 364/471.03, 356/312, 356/323, 356/325, 356/328, 250/339, 250/343, 250/353, 250/252.1
• US Class Current: 702/27
• CPC Class Codes: G01N 21/3563 for analysing solids; Preparation of samples therefor
• CPC Class Codes: G01N 21/359 using near infrared light
• CPC Class Codes: G01N 33/343 paper pulp
• CPC Class Codes: G01N 33/346 paper sheets

Abstract

A method is provided for quantifying the amounts of performance chemicals selected from the group consisting of wet strength agents, starches and retention agents, hydrophobic agents and debonding agents, reacted or retained with the cellulose fibers in fluff pulp or paper. The method comprises (I) developing a calibration model by (I.a) registering absorption, reflectance or emission spectral raw data of reference samples of paper or pulp containing known amounts of the performance chemicals to develop a learning set; (I.b) processing the spectral raw data from the registered spectra to reduce noise and adjust for drift and diffuse light scatter; (I.c) performing a data analysis on the learning set in which the processed spectral data of the reference samples are transferred into latent variables based on principal component analysis, and applying chemometric techniques on the latent variables in order to find the mathematical expression of the calibration model; and (II) registering absorption, reflectance or emission spectral raw data of a sample of fluff paper or pulp containing unknown amounts of chemicals, processing the spectral raw data as according to (I.b); transferring the processed spectral data into latent variables as according to (I.c), and applying the developed calibration model on the latent variables in order to determine the unknown amounts of the reacted or retained performance chemicals.

Claims

1. A method for quantifying the amounts of performance chemicals selected from the group consisting of wet strength agents, starches and retention agents, hydrophobic agents and debonding agents, reacted or retained with the cellulose fibers in fluff pulp or paper, which method comprises (I) developing a calibration model by

(I.a) registering absorption, reflectance or emission spectral raw data of reference samples of paper or pulp containing known amounts of said performance chemicals to develop a learning set;

(I.b) processing the spectral raw data from the registered spectra to reduce noise and adjust for drift and diffuse light scatter;

(I.c) performing a data analysis on the learning set in which the processed spectral data of the reference samples are transferred into latent variables based on principal component analysis, and applying chemometric techniques on the latent variables in order to find the mathematical expression of the calibration model; and

(II) registering absorption, reflectance or emission spectral raw data of a sample of fluff paper or pulp containing unknown amounts of chemicals, processing the spectral raw data as according to (I.b);

transferring the processed spectral data into latent variables as according to (I.c), and applying the developed calibration model on the latent variables in order to determine the unknown amounts of said reacted or retained performance chemicals.

2. A method according to claim 1, wherein the recording of the absorption, reflectance or emission spectra is performed in the wavelength range of 200 nm to 400 μ

m.

3. A method according to claim 1, wherein the spectral data processing in (I.b). is performed using the Kubelka-Munk transform:

##EQU9## wherein R_ik is the apparent absorbance at the wavelength k, A_ik is the transformed absorbance at the wavelength k, and the index i represents the sample spectra available.

4. A method according to claim 3, wherein the recording of the absorption, reflectance or emission spectra is performed in the wavelength range of 800 nm to 2500 nm.

5. A method according to claim 1, wherein the spectral data processing in (I.b) is performed using the Multiplicative Scatter Correction:

##EQU10## wherein R_ik is the apparent absorbance at the wavelength k, A_ik is the transformed absorbance at the wavelength k, a₁ is the least squares estimation of the intercept parameter, and b₁ is the least squares estimation of the slope parameter, the index i representing the sample spectra available, and the index k representing the available wavelengths.

6. A method according to claim 1, wherein the spectral data processing in (I.b) is performed by use of the Fourier transformation.

7. A method according to claim 1, wherein the spectral data processing in (I.b) is performed by use of up to the fourth order derivatives.

8. A method according to claim 1, wherein the spectral data processing in (I.b) is performed by use of the Standard Normal Variate transformation.

9. A method according to claim 1, wherein the data analysis is performed by the use of the Principal Components Regression technique.

10. A method according to claim 1, wherein the data analysis is performed by the use of the Partial Least Squares technique.

11. A method according to claim 1 for quantification of the nitrogen content of reacted or retained amounts of performance chemicals containing nitrogen.

12. A method according to claim 1 for quantification of reacted or retained amounts of alkyl ketene dimer and rosin.

13. A method according to claim 1 for quantification of reacted or retained amounts of alkylene succinic acid and alkyl carbamoyl chloride.

14. A method according to claim 1 for quantification of retained amounts of quaternary fatty amines and fatty amine oxides.

15. A method for maintaining a process control program wherein the amounts of reacted or retained paper and pulp performance chemicals selected from the group consisting of wet strength agents, starches and retention agents, hydrophobic agents and debonding agents are quantified in fluff paper or pulp to detect any change thereof and provide control input in order to assure optimum dosage levels for the performance chemicals, whereby a method as defined in claim 1 is used.