Patent US4628726A successfully refreshed from Google Patents.
US4628726A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Analysis of organic compounds in baths used in the manufacture of printed circuit board using novel chromatographic methods
Assignee: ETD TECHNOLOGY Inc 619 WEST COUNTY ROAD E SHOREVIEW MINNESOTA 55112 A CORP OF DELAWARE
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Filing: 1985-10-24
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Granted: 1986-12-16
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Expires: 2005-10-24
Abstract
Abstract An accurate repeatable quantitative determination of the concentration of organic composition analytes, breakdown products and organic contaminants in plating baths, and in chemical baths other than the plating bath can be made using a novel high-pressure liquid chromatography apparatus in combination with size exclusion chromatography and total organic carbon analysis.
Inventors
- 👤 Kurt E. Heikkila
- 👤 Rodney K. Williams
- 👤 Russell J. Pylkki
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-05 17:57
CPC Classifications
G; G01; G01N; G01N30/00; G01N30/02; G01N30/26; G01N30/38; G01N30/46; G01N30/461; G01N30/04; G01N30/06; G01N30/14; G01N30/28; G01N30/34
Claims Analysis
Total Claims: 25
Claim 1
Independent Claim
389 words
An analytical method of determining the concentration of an organic analyte or mixtures thereof in a chemical bath, other than an acidic or basic metal plating bath medium, used in the manufacture of printed circuit boards using an HPLC apparatus having components that maintain the stability, precision and accuracy of the analytical method which comprises: (1) obtaining an HPLC apparatus having: (a) a chromatographic column, containing a stationary phase and a support phase composition sufficient to resolve each organic analyte, having an inlet and an outlet; (b) a detector means for measuring the relative concentration of each organic analyte, having an inlet and an outlet, wherein the chromatographic column outlet is attached in liquid communication to the detector inlet; (c) a second column, having a packing comprising at least a support phase composition, and having an inlet and an outlet, wherein the second column outlet is connected in liquid communication with the chromatographic column inlet, wherein the second column support phase composition can substantially reduce the effect of the acidic or basic components of the sample on the reproducibility, precision or accuracy of the analysis; (d) a sample introduction means having an inlet, an outlet and a sample introduction port, wherein the sample introduction means outlet is attached in liquid communication to the second column inlet; and (e) a source of solvent under pressure attached in liquid communication to the sample introduction means inlet; (2) passing a stream of solvent under pressure through the HPLC apparatus; (3) applying a sample of the chemical bath to be analyzed into the stream of solvent under pressure at the sample introduction port; (4) passing the chemical bath sample in the solvent through the second column wherein the column packing substantially reduces the effect of the acid or basic components of the sample, forming an innocuous analyte; (5) passing the innocuous analyte in the stream of solvent into the chromatographic column, resolving the analyte components into detectable segments utilizing the interaction between the analyte and the stationary phase; and (6) passing the detectable segments in the solvent into a detector that can produce a signal which as a result of the cooperation of the elements of the HPLC apparatus detector and the sample obtains a substantially linear relationship between the analyte concentration in the sample and the integration units produced from the signal.
Claim 2
Dependent Claim
389 words
An analytical method of determining the concentration of an organic analyte or mixtures thereof in a chemical bath, other than an acidic or basic metal plating bath medium, used in the manufacture of printed circuit boards using an HPLC apparatus having components that maintain the stability, precision and accuracy of the analytical method which comprises: (1) obtaining an HPLC apparatus having: (a) a chromatographic column, containing a stationary phase and a support phase composition sufficient to resolve each organic analyte, having an inlet and an outlet; (b) a detector means for measuring the relative concentration of each organic analyte, having an inlet and an outlet, wherein the chromatographic column outlet is attached in liquid communication to the detector inlet; (c) a second column, having a packing comprising at least a support phase composition, and having an inlet and an outlet, wherein the second column outlet is connected in liquid communication with the chromatographic column inlet, wherein the second column support phase composition can substantially reduce the effect of the acidic or basic components of the sample on the reproducibility, precision or accuracy of the analysis; (d) a sample introduction means having an inlet, an outlet and a sample introduction port, wherein the sample introduction means outlet is attached in liquid communication to the second column inlet; and (e) a source of solvent under pressure attached in liquid communication to the sample introduction means inlet; (2) passing a stream of solvent under pressure through the HPLC apparatus; (3) applying a sample of the chemical bath to be analyzed into the stream of solvent under pressure at the sample introduction port; (4) passing the chemical bath sample in the solvent through the second column wherein the column packing substantially reduces the effect of the acid or basic components of the sample, forming an innocuous analyte; (5) passing the innocuous analyte in the stream of solvent into the chromatographic column, resolving the analyte components into detectable segments utilizing the interaction between the analyte and the stationary phase; and (6) passing the detectable segments in the solvent into a detector that can produce a signal which as a result of the cooperation of the elements of the HPLC apparatus detector and the sample obtains a substantially linear relationship between the analyte concentration in the sample and the integration units produced from the signal.
Claim 3
Dependent Claim
16 words
The method of claim 1 wherein the chemical bath is used in a copper plating process.
Claim 4
Dependent Claim
33 words
The method of claim 1 wherein between the source of solvent and the sample introduction means is placed a third column having sufficient support phase to saturate the solvent with dissolved support phase.
Claim 5
Dependent Claim
24 words
The method of claim 3 wherein the third column support phase is a silica having a particle size of about 2 to 20 microns.
Claim 6
Dependent Claim
21 words
The method of claim 1 wherein the second column support phase has a particle size of about 2 to 20 microns.
Claim 7
Dependent Claim
41 words
The method of claim 1 wherein the chromatographic column support phase is a silica and the stationary phase is a C 6-24 aliphatic hydrocarbon chemically bonded to the silica, wherein the silica has a particle size of 2 to 20 microns.
Claim 8
Dependent Claim
63 words
The method of claim 1 wherein the source of solvent under pressure comprises at least one or more solvent containers, a gradient device that can provide a mixture of solvent under constant or varying ratio, and a pump which can provide a solvent flow of 0.01 milliliters per minute to 10 milliliters per minute at a pressure of about 1 to 10,000 psi.
Claim 9
Dependent Claim
24 words
The method of claim 7 wherein the source of solvent supplies solvent at a flow rate of about 0.01 to 100 milliliters per minute.
Claim 10
Dependent Claim
27 words
The method of claim 8 wherein the solvent is a mixed aqueous organic solvent and wherein the organic phase is acetonitrile, an alcohol, tetrahydrofuran or mixtures thereof.
Claim 11
Dependent Claim
20 words
The method of claim 1 wherein the sample introduction means has a sample size of about 1 to 200 microliters.
Claim 12
Dependent Claim
20 words
The method of claim 1 wherein the detector means detects the relative absorption of ultraviolet light by the organic analyte.
Claim 13
Dependent Claim
21 words
The method of claim 1 wherein the plating bath medium is also analyzed for polymer size distribution and total organic carbon.
Claim 14
Dependent Claim
389 words
An analytical method of determining the concentration of an organic analyte or mixtures thereof in a chemical bath, other than an acidic or basic copper plating bath medium, used in the manufacture of printed circuit boards using an HPLC apparatus having components that maintain the stability, precision and accuracy of the analytical method which comprises: (1) obtaining an HPLC apparatus having: (a) a chromatographic column, containing a stationary phase and a support phase composition sufficient to resolve each organic analyte, having an inlet and an oulet; (b) a detector means for measuring the relative concentration of each organic analyte having an inlet and an outlet wherein the chromatographic column outlet is attached in liquid communication to the detector inlet; (c) a second column, having a packing comprising at least a support phase composition, and having an inlet and an outlet, wherein the second column outlet is connected in liquid communication with the chromatographic column inlet, wherein the second column support phase composition can substantially reduce the effect of the acidic or basic components of the sample on the reproducibility, precision or accuracy of the analysis; (d) a sample introduction means having an inlet, an outlet and a sample introduction port, wherein the sample introduction means outlet is attached in liquid communication to the second column inlet; and (e) a source of solvent under pressure attached in liquid communication to the sample introduction means inlet; (2) passing a stream of solvent under pressure through the HPLC apparatus; (3) applying a sample of the chemical bath to be analyzed into the stream of solvent under pressure at the sample introduction port; (4) passing the chemical bath sample in the solvent through the second column wherein the column packing substantially reduces the effect of the acid or basic components of the sample, forming an innocuous analyte; (5) passing the innocuous analyte in the stream of solvent into the chromatographic column, resolving the analyte components into detectable segments utilizing the interaction between the analyte and the stationary phase; and (6) passing the detectable segments in the solvent into a detector that can produce a signal which as a result of the cooperation of the elements of the HPLC apparatus detector and the sample obtains a substantially linear relationship between the analyte concentration in the sample and the integration units produced from the signal.
Claim 15
Dependent Claim
389 words
An analytical method of determining the concentration of an organic analyte or mixtures thereof in a chemical bath, other than an acidic or basic copper plating bath medium, used in the manufacture of printed circuit boards using an HPLC apparatus having components that maintain the stability, precision and accuracy of the analytical method which comprises: (1) obtaining an HPLC apparatus having: (a) a chromatographic column, containing a stationary phase and a support phase composition sufficient to resolve each organic analyte, having an inlet and an oulet; (b) a detector means for measuring the relative concentration of each organic analyte having an inlet and an outlet wherein the chromatographic column outlet is attached in liquid communication to the detector inlet; (c) a second column, having a packing comprising at least a support phase composition, and having an inlet and an outlet, wherein the second column outlet is connected in liquid communication with the chromatographic column inlet, wherein the second column support phase composition can substantially reduce the effect of the acidic or basic components of the sample on the reproducibility, precision or accuracy of the analysis; (d) a sample introduction means having an inlet, an outlet and a sample introduction port, wherein the sample introduction means outlet is attached in liquid communication to the second column inlet; and (e) a source of solvent under pressure attached in liquid communication to the sample introduction means inlet; (2) passing a stream of solvent under pressure through the HPLC apparatus; (3) applying a sample of the chemical bath to be analyzed into the stream of solvent under pressure at the sample introduction port; (4) passing the chemical bath sample in the solvent through the second column wherein the column packing substantially reduces the effect of the acid or basic components of the sample, forming an innocuous analyte; (5) passing the innocuous analyte in the stream of solvent into the chromatographic column, resolving the analyte components into detectable segments utilizing the interaction between the analyte and the stationary phase; and (6) passing the detectable segments in the solvent into a detector that can produce a signal which as a result of the cooperation of the elements of the HPLC apparatus detector and the sample obtains a substantially linear relationship between the analyte concentration in the sample and the integration units produced from the signal.
Claim 16
Dependent Claim
33 words
The method of claim 13 wherein between the source of solvent and the sample introduction means is placed a third column having sufficient support phase to saturate the solvent with dissolved support phase.
Claim 17
Dependent Claim
24 words
The method of claim 14 wherein the third column support phase is a silica having a particle size of about 2 to 20 microns.
Claim 18
Dependent Claim
21 words
The method of claim 13 wherein the second column support phase has a particle size of about 2 to 20 microns.
Claim 19
Dependent Claim
41 words
The method of claim 13 wherein the chromatographic column support phase is a silica and the stationary phase is a C 6-24 aliphatic hydrocarbon chemically bonded to the silica, wherein the silica has a particle size of 2 to 20 microns.
Claim 20
Dependent Claim
63 words
The method of claim 13 wherein the source of solvent under pressure comprises at least one or more solvent containers, a gradient device that can provide a mixture of solvent under constant or varying ratio, and a pump which can provide a solvent flow of 0.01 milliliters per minute to 10 milliliters per minute at a pressure of about 1 to 10,000 psi.
Claim 21
Dependent Claim
20 words
The method of claim 13 wherein the sample introduction means has a sample size of about 1 to 200 microliters.
Claim 22
Dependent Claim
20 words
The method of claim 13 wherein the detector means detects the relative absorption of ultraviolet light by the organic analyte.
Claim 23
Dependent Claim
21 words
The method of claim 13 wherein the plating bath medium is also analyzed for polymer size distribution and total organic carbon.
Claim 24
Dependent Claim
24 words
The method of claim 13 wherein the source of solvent supplies solvent at a flow rate of about 0.01 to 100 milliliters per minute.
Claim 25
Dependent Claim
27 words
The method of claim 22 wherein the solvent is a mixed aqueous organic solvent and wherein the organic phase is acetonitrile, an alcohol, tetrahydrofuran or mixtures thereof.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1989-12-15 | 1990-06-16 | 1990-12-16 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1993-12-15 | 1994-06-16 | 1994-12-16 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1997-12-15 | 1998-06-16 | 1998-12-16 | $7700.00 | Window Closed / Lapsed |