Delivering the Right Results

Easy-To-Use Windows® - Based Operating SoftwareSimpli�ed data handling, customizable data reporting/exporting, and a number of user-de�ned settings make the FP-528 software �exible and easy to operate. With virtually unlimited storage space and compatibility with various Laboratory Information Management Systems (LIMS), this software is designed for seamless interaction with any operator or customer environment.

Seamlessly manage data and graphs Perform calibrations and drift corrections

Monitor instrument component readings Expanded interactive diagnostic screens to aid in troubleshooting and improve serviceability

LECO's convenient internet-based SmartLine Remote Diagnostics system provides you with our fastest service solution yet for getting the answers you need - saving you time and money.

FP-528PC Nitrogen/Protein Analyzer Combustion System

Nitrogen/Protein DeterminationLECO Corporation

3000 Lakeview Avenue • St. Joseph, MI 49085 • Phone: 800-292-6141 • Fax: 269-982-8977

info@leco.com • www.leco.com • ISO-9001 • No. FM 24045 • LECO is a registered trademark of LECO Corporation.

Form No. 209-137 © 2013 LECO Corporation9/13

Simpli�ed Flow Diagram

The combustion method of analysis is rapidly gaining acceptance around the world as a safe

alternation to the century-old Kjeldahl technology. Combustion has earned o�cial method approval for

many applications by organizations like the Association of O�cial Analytical Chemists (AOAC), the

American Oil Chemists’ Society (AOCS), the American Society of Brewing Chemists (ASBC), and the

American Association of Cereal Chemists (AACC). For your own unique sample matrices, LECO’s sta� of

application scientists can work with you to develop appropriate analytical methods.

Looking for a better method of protein determination? Your search is over…choose LECO’s FP-528 Nitrogen/Protein Determinators for sale, simple, accurate and cost-e�ective analyses.

Autoloader and Loading HeadReliable, gravity-fed automation (30 to 120 positions)

Thermal Conductivity Cell allows detection limits of 0.04 milligrams absolute nitrogen

Patented Ballast holds 4.5 liters of homogeneous sample gases

Solid or Liquid sample up to one gram can be easily and quickly prepared. Tare out the weight of an empty tin foil or Quick-cap, add sample, reweigh, and the sample is ready for analysis

Copper Sticks have an extra long life-replace after approximately 1500 analyses

Thermoelectric Cooler removes nearly all moisture from the combustion gases, extending the life of consumables used later in the determination

Combustion Tube- Combustion of macro sample sizes in an oxygen-rich environment (-950 ˚C) - Robust U-shaped design signi�cantly reduces maintenance downtime - Variable furnace positioning improves serviceability- Patented reticulated crucible extends throughput to over 500 analyses

3/10 cc Aliquot Sample is taken from the gases in the ballast

Unique Features

User InterfaceEasy-to-use Windows-based operating software

By-products of combustion - CO , H O , NO , and N - pass through the furnace �lter and

thermoelectric cooler for subsequent collection in a ballast apparatus. These collected

gases in the ballast are equilibrated, and a small aliquot dose is then used for further

conversion of the gases. The remaining aliquot that has been reduced is measured by the

thermal conductivity cell for nitrogen.

2 2 X 2

FP-528 Nitrogen/Protein Analyzer Combustion System

FP-528Nitrogen/Protein

How it WorksAn encapsulated sample is placed into the loadinghead of the FP-528, where it is sealed and purged ofany atmospheric gases that have entered duringsampling loading. The sample is then dropped into ahot furnace and flushed with pure oxygen for veryrapid combustion.

By-products of combustion—CO , H O, NO , and2 2 x

N —pass through the furnace filter and thermoelectric2

cooler for subsequent collection in a ballast apparatus.These collected gases in the ballast are equilibrated,and a small aliquot dose is then used for furtherconversion of the gases. The remaining aliquot thathas been reduced is measured by the thermalconductivity cell for nitrogen.

The system is controlled by an external PC usingWindows -based operating software.

® Combustion Tube Combustion of samples in an oxygen-rich environment

Sample HolderHolds up to250 mg sample

Collection SystemBallast collects allevolved gases;Ensures completehomogenization priorto determination

Used specifically for low-sample throughput laboratories, the FP-528 Nitrogen/ProteinDeterminator is a cost-effective alternative to Kjeldahl digestion methods.

Foods, Feeds, Forages,Fertilizers, Milled Products

Delivering the Right Results

Instrument Range @ mg

3 cc Aliquot Loop: 160 ppm or 0.016% to 100% or 0.04 to 300 mg absolute Nitrogen

Precision @ mg

3 cc Aliquot Loop: 80 ppm or 0.5% RSD, whichever is greater

Readability 0.001%

Calibration Standard Sample; Linear

Analysis Time 3 minutes nominal

Sample Size 250 mg to 350 mg (ZNominalX)

Detection Method Thermal Conductivity

Chemical ReagentsAnhydrous Magnesium Perchlorate, Calcium Oxide, Sodium Hydroxide on an inert base,Copper Sticks, N Catalyst Reagent, Copper Turnings, Alumina Pellets, Magnesium Oxide

Gas Required

Carrier Gas:Combustion Gas:Pneumatic Gas:

99.99% Helium 40 psi (2.8 bar), ±10%99.99% Oxygen 40 psi (2.8 bar), ±10%Compressed Air, source must be oil and water free; 40 psi (2.8 bar), ±10%

Gas Flow Rates

Carrier Gas:

Combustion Gas:

Analysis: 200 mL/min (measure), 30 mL/min (reference)Conservation: 30 mL/min (measure), 30 mL/min (reference)1.3 to 6 L/min (user programmable oxygen profile)

Furnace Range Up to 975 Co

Weight 150 lb (68 kg)

Physical Dimensions 28 in. H x 21 in. W x 23 in. D (71 cm x 53 cm x 58 cm)

Electrical Power Requirements 230 V~ (±10%; at max load), 50/60 Hz, single phase, 10 A, 7,900 BTU/hr

LECO Corporation3000 Lakeview Avenue • St. Joseph, MI 49085 • Phone: 800-292-6141 • Fax: 269-982-8977

info@leco.com • www.leco.com • ISO-9001:2008 HQ-Q-994 • LECO is a registered trademark of LECO Corporation.

Specifications

Form No. 209-137 7/12-REV5 © 2012 LECO Corporation

Specifications and part numbers may change. Consult LECO for latest information.

Simplified Flow Diagram

Expanded features including automation,multiple elements, external PC control,

expanded sample size ranges, Windows -®

based operating software that supportscompliance to 21 CFR Part 11, and SmartLine

®

Remote Diagnostics are available on theCHN628 Series. For more information,

request form no. 209-218.

Part Numbers

FP528C Nitrogen/Protein Determinator with PC and Windows-based operating software

O2

CarrierGas

HeCarrier

Gas

ResistanceFurnace

ThermoelectricCooler

Mixing BallastVolume

Exhaust

Exhaust

Exhaust

AliquotSolenoidLecosorb

LecosorbAnhydrone

Anhydrone

CO2 H O2Reduces NOx

Reference Flow

N2

TC Cell

Thermal Conductivity

O2 CO2 H O2

Optional Accessories

621-434-110751-300-160

Printer4-Place Balance

V~ denotes VAC.

Delivering the Right Results

Maintenance FP-528 6 21

TUBE

Figure 6-10 Tube Removal

608-379QUARTZ WOOL

STRIPS2"

502-310STEEL WOOL

2"

601-390FILTERTUBE

Figure 6-11 Packing the Furnace Filter Tube

STEEL WOOL (5.1)

Theory of Operation FP-528 7 3

Theory of Operation

The FP-528 Determinator is a microprocessor based, software-controlled instrument that determines the nitrogen content in a variety of materials, including grain, stock feed, oil, rubber, and soil.

There are three phases during an analyze cycle: purge, burn, and analyze. In the sample drop purge phase, the encapsulated sample is placed in the loading head, sealed, and purged of any atmospheric gases that have entered during sample loading. The ballast volume (zero volume at this point) and gas lines are also purged.

During the burn phase, the sample is dropped into a hot furnace (850oC) and flushed with pure oxygen for very rapid combustion. The products of combustion, mainly CO2, H2O, NOx, and N2, are passed through the furnace filter and thermoelectric cooler and then collected in the ballast volume.

In the analyze phase, the combustion gases in the ballast are allowed to become homogeneous by passive mixing. A 3 cc aliquot is captured in a loop before the free-floating ballast piston is forced down to evacuate the ballast. The sample aliquot gases are swept through hot copper to remove oxygen and change NOx to N2, then through Lecosorb and Anhydrone to remove carbon dioxide and water, respectively. The remaining combustion product, nitrogen in a helium carrier, is measured by the thermal conductivity cell.

A precooler and a thermoelectric cooler after the furnace remove moisture before it can enter the ballast. An extensive leak check procedure is available from the Diagnostics menu to help locate any oxygen or helium system leak that may develop during operation.

The final result is displayed as weight percentage of nitrogen (or protein if selected). Results can be calculated on a user edited moisture basis.

A precooler and a thermoelectric cooler after the furnace remove moisture before it can enter the ballast.

(5.4)

The sample aliquot gases are swept through hot copper to remove oxygen and change NOx to Ngases are swept through hot copper to remove oxygen and change NOx to N2, then , then through Lecosorb and Anhydrone to remove carbon dioxide and water, respectively.

(5.2)

(5.3)

8 8 FP-528 Diagnostics

Perform Leak Check

Leak check is a diagnostic test that automatically checks for gas leaks in the instrument. There is a separate leak check for oxygen and helium.

All leak checks will first pressurize the system and then monitor the pressure for 60 seconds. If the pressure does not change more than ±5 mmHg, then the leak check will pass.

The furnace temperature should have reached a constant temperature and maintained that temperature for a minimum of 15 minutes before a leak check is performed.

1. From the Diagnostics menu, click Leak Check. The Leak Check dialog box will appear.

2. Click on the gas system in the actions box that should be leak checked. Choices are Oxygen Leak Check, Ballast, Cooler, Furnace, and Helium Leak Check. The leak check will start and the result will be displayed in the results box. Refer to Leak Check Definitions, page 8 9, for additional information.

3. If a leak check determines there is a leak in a system, click View to display possible leak points within the instrument.

4. Click Close to exit leak check.

(8)Perform Leak Check

Leak check is a diagnostic test that automatically checks for gas leaks in the instrument. There is a separate leak check for oxygen and helium.

Operation FP-528 5 27

Login using a Sample Template

Before proceeding, Create a Method, page 5 16, must be completed.

1. From the Samples menu, click Login. The Sample dialog box will appear.

2. Click the drop down arrow to the right of sample name and enter the desired sample name from the drop down list. The sample name, method comments, and description will automatically be entered into the spreadsheet.

3. Continue with sample login and enter the other necessary information.

(13.1)

Login using a Sample Template

4 2 FP-528 System Setup

Balance Configuration .................................................................. 4 19

Balance Configuration Definitions ............................................. 4 19

Barometric Calibration ................................................................. 4 20

Catalyst Heater Calibration ........................................................... 4 21

Catalyst Heater Definitions ...................................................... 4 22

Combustion Furnace Calibration .................................................... 4 23

Combustion Furnace Definitions ............................................... 4 26

Assign User ................................................................................ 4 27

Assign User Functions .................................................................. 4 28

Assign User Password .................................................................. 4 29

Delete User ................................................................................ 4 30

Data Transmission Configuration ................................................... 4 31

Data Transmit Port Configuration .................................................. 4 33

Data Transmit Port Definitions ................................................. 4 33

Spreadsheet ............................................................................... 4 34

Configure Spreadsheet ............................................................ 4 34

Go to First Row in the Spreadsheet ........................................... 4 35

Go to Last Row in the Spreadsheet ........................................... 4 35

Go to the Analyze Row in the Spreadsheet ................................ 4 35

Hide/Show the Status Bar ....................................................... 4 35

Hide/Show the Toolbar............................................................ 4 35

Assign User Functions .................................................................. 4 28

Assign User Password .................................................................. 4 29

(13.2)

Catalyst Heater Calibration ...........................................................

Combustion Furnace Calibration ....................................................

(13.3)

7 8 FP-528 Theory of Operation

Theory of Calibration

Calibration compensates for differences between the total element measured and the actual element concentration. A programmed equation will correlate the response between the observed and theoretical measurement of analyte, permitting accurate measurements to be made.

The Windows® software provides several types of calibration curves. The calibration curves include single standard calibration, linear, quadratic, and cubic. First perform a blank calibration, then once a standard calibration has been defined re-calibration is not necessary unless a cell or flow has been changed. The daily routine will consist of determining the blank and performing a drift correction.

The first step to be performed is the determination of a method specific blank.

Several blanks should be analyzed. The linearization table is applied to the peak during the analysis. The area under the peak is calculated and stored as a raw area (Ar).

01234

1 9 17 25 33

Time

Raw Area = 19

01234

1 10 19 28 37

Time

Raw Area = 18

01234

1 10 19 28 37

Time

Raw Area = 19

01234

1 10 19 28 37

Time

Raw Area = 18

If the four blanks displayed above were selected in the software to calculate a blank, the result would be that the average of the four would be stored as the blank area (Ab).

Ab = 19+18+19+18

- 18.5 4

The blank area, Ab will be subtracted from every sample analyzed after it is set.

After the blank is defined, a calibration curve needs to be defined. Several standards need to be selected that will cover the operating range of analyte concentration for the samples of unknown analyte concentration. At least three replicates of each standard should be analyzed. Care must be taken to accurately compensate for trapped atmosphere, atmospheric blank, with each analyzed standard. If the calibration curve is constructed using more than one sample type, the atmospheric blank must be determined for each standard. This can be accomplished by analyzing the same sample mass encapsulated and in an open container, dissolving in water, or palletizing the sample. The difference in the results is the atmospheric blank.

0

60

120

1 11 21 31 41 51

Time

0

60

120

1 11 21 31 41 51

Time

0

60

120

1 11 21 31 41 51

Time

Theory of Calibration

software provides several types of calibration curves. The calibration curves include single standard calibration, linear, quadratic, and cubic. First perform curves include single standard calibration, linear, quadratic, and cubic. First perform

(13.4)

Diagnostics FP-528 8 1

8 Diagnostics

The Diagnostics chapter explains how to monitor and check the operation of the instrument hardware. This can help the operator or service technician determine if the instrument is operating properly. Through the Diagnostics menu, you can monitor and change the solenoid valve states, test the serial communications port, view the ambient monitor and electrical switch states, and leak check the system.

View Ambient Monitor .................................................................... 8 3

Ambient Monitor Definitions ....................................................... 8 4

Range Limits ........................................................................... 8 4

View/Toggle Solenoid States ........................................................... 8 5

View Switch States ........................................................................ 8 6

View Comport Data ....................................................................... 8 7

Perform Leak Check ....................................................................... 8 8

Leak Check Definitions .............................................................. 8 9

Diagnostics

(13.5)

1 16 FP-528 Introduction

Software License

By installing the Licensed Software, the Licensee acknowledges that Licensee has read it, understands it and agrees to be bound by its terms, and further agree that this is the complete and exclusive statement of the Software License between the parties, which supersedes and merges all prior proposals, understandings and other agreements oral and written, between the parties relating to the subject matter of this Software License. In the event of any conflict between the terms of this Software License and the terms of purchase orders submitted by Licensee, the terms of this Software License shall control.

Lakeview Avenue, St. Joseph, Michigan 49085-2396, owner of the Licensed Software. This Software License specifies the conditions under which Licensee may use the Licensed Software.

I. Definitions

"Licensed Software" shall mean the software supplied with this Software License, which is software developed and distributed by LECO.

"Instruction Manual" shall mean a guide describing the use and operation of the Licensed Software, together with any related supporting documentation.

"Licensee" shall mean and include any of the Licensee's divisions and departments within Licensee's organization, but shall not include wholly or partially owned subsidiaries, affiliates, successors or assigns, or independent third parties.

II. License Grant

LECO hereby grants to Licensee, and Licensee hereby accepts, subject to the terms and conditions set forth in this Software License, a non-exclusive, non-transferable license to use the Licensed Software and Instruction Manual as set forth in this Software License. The term license as used in this Software License shall mean and include:

a. the right to use a copy of the Licensed Software in executable form by one user at a time;

b. the right to use and copy the Instruction Manual for Licensee's internal operations; and

c. the right to make one backup copy of the Licensed Software.

In accepting the license granted by LECO, Licensee agrees that it shall not:

1. transfer or allow transfer of copies of the Licensed Software to any other party including any wholly or partially owned subsidiaries, affiliates, successors, or assigns without the express consent of LECO;

2. use the Licensed Software on more than one (1) CPU at any one time;

3. cause or permit unauthorized copying, reproduction, or disclosure of any portion of the Licensed Software or Instruction Manual or the distribution of any part thereof to any third person or entity, for any purpose whatsoever. This restriction shall continue to bind Licensee and its agents beyond the termination of this Software License; or

4. attempt to disassemble modify, or reverse engineer the Licensed Software;

5. attempt to defeat or defeat the copy-protection mechanism;

6. attempt to or access features not purchased.

Software License

"Licensed Software" shall mean the software supplied with this Software License, which is software developed and distributed by LECO.

(13.7)

Wannee

Typewritten Text

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