FP-528PC Nitrogen/Protein Analyzer

Combustion System

Easy-To-Use Windows® - Based Operating Software

Simplified data handling, customizable data reporting/exporting, and a number of user-defined settings make
the FP-528 software flexible 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.

LECO 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.

Delivering the Right Results Nitrogen/Protein Determination

Form No. 209-137 9/13 © 2013 LECO Corporation
 FP-528
Looking for a better method of
protein determination? Your search Nitrogen/Protein Analyzer
Combustion System
is over…choose LECO’s FP-528
Unique Features
Nitrogen/Protein Determinators
for sale, simple, accurate and
cost-effective analyses. Thermal Conductivity Cell
allows detection limits of 0.04
milligrams absolute nitrogen
(1) Autoloader and Loading Head
The combustion method of analysis is rapidly gaining acceptance around the world as a safe Reliable, gravity-fed automation
(30 to 120 positions)
alternation to the century-old Kjeldahl technology. Combustion has earned official method approval for
many applications by organizations like the Association of Official 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 staff of (5.4)
application scientists can work with you to develop appropriate analytical methods. Thermoelectric Cooler
removes nearly all moisture
from the combustion gases,
extending the life of
consumables used later in (7)
the determination Patented Ballast
holds 4.5 liters
Simplified Flow Diagram of homogeneous
sample gases
(13)
User Interface
Easy-to-use Windows-
based operating
software
3/10 cc Aliquot
Sample is taken
from the gases
in the ballast
Copper Sticks
have an extra long
life-replace after
approximately
1500 analyses (2) , (3)
Combustion Tube
- Combustion of macro sample
sizes in an oxygen-rich
environment (-950 ˚C)
- Robust U-shaped design (1)
significantly reduces maintenance Solid or Liquid sample up to one
downtime gram can be easily and quickly
By-products of combustion - CO2 , H2 O , NOX , and N 2 - pass through the furnace filter and
- Variable furnace positioning prepared. Tare out the weight of
thermoelectric cooler for subsequent collection in a ballast apparatus. These collected improves serviceability an empty tin foil or Quick-cap,
(4) - Patented reticulated crucible add sample, reweigh, and the
gases in the ballast are equilibrated, and a small aliquot dose is then used for further
extends throughput to over 500 sample is ready for analysis
conversion of the gases. The remaining aliquot that has been reduced is measured by the analyses
thermal conductivity cell for nitrogen.
 FP-528
Nitrogen/Protein
Foods, Feeds, Forages,
Fertilizers, Milled Products

Used specifically for low-sample throughput laboratories, the FP-528 Nitrogen/Protein

Determinator is a cost-effective alternative to Kjeldahl digestion methods.

How it Works
An encapsulated sample is placed into the loading Sample Holder
head of the FP-528, where it is sealed and purged of Holds up to
250 mg sample
any atmospheric gases that have entered during
sampling loading. The sample is then dropped into a
hot furnace and flushed with pure oxygen for very
rapid combustion.
(7)
By-products of combustion—CO2, H2O, NOx, and Collection System
N2—pass through the furnace filter and thermoelectric Ballast collects all
evolved gases;
cooler for subsequent collection in a ballast apparatus. Ensures complete
(7) These collected gases in the ballast are equilibrated, homogenization prior
to determination
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.

(13)The system is controlled by an external PC using

® Combustion Tube
Windows -based operating software. Combustion of
samples in an
oxygen-rich
environment

Delivering the Right Results

Specifications
Instrument Range @ 300 mg
3 cc Aliquot Loop: 160 ppm or 0.016% to 100% or 0.04 to 300 mg absolute Nitrogen (10)
Precision @ 300 mg (12)
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 (11)
Sample Size 250 mg to 350 mg (ZNominalX) (9)
Detection Method Thermal Conductivity (6)
Anhydrous Magnesium Perchlorate, Calcium Oxide, Sodium Hydroxide on an inert base,
Chemical Reagents
Copper Sticks, N Catalyst Reagent, Copper Turnings, Alumina Pellets, Magnesium Oxide

Gas Required
Carrier Gas: 99.99% Helium 40 psi (2.8 bar), ±10%
Combustion Gas: 99.99% Oxygen 40 psi (2.8 bar), ±10%
Pneumatic Gas: Compressed Air, source must be oil and water free; 40 psi (2.8 bar), ±10%
Gas Flow Rates
Carrier Gas: Analysis: 200 mL/min (measure), 30 mL/min (reference)
Conservation: 30 mL/min (measure), 30 mL/min (reference)
Combustion Gas: 1.3 to 6 L/min (user programmable oxygen profile)
o
Furnace Range Up to 975 C
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

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

Optional Accessories
621-434-110 Printer
751-300-160 4-Place Balance
V~ denotes VAC.

Simplified Flow Diagram

Mixing Ballast
Thermoelectric Volume
Cooler
Expanded features including automation,
O2
Carrier
multiple elements, external PC control,
Gas
expanded sample size ranges, Windows®-
based operating software that supports
Resistance compliance to 21 CFR Part 11, and SmartLine®
(3) Furnace
Remote Diagnostics are available on the
Exhaust

Exhaust
CHN628 Series. For more information,
Lecosorb Anhydrone
Aliquot
Solenoid Lecosorb Anhydrone
N2
request form no. 209-218.
O2 CO2 H2O TC Cell
He H2O Reduces NOx
CO2
Carrier Reference Flow
Gas Exhaust

Thermal Conductivity

Specifications and part numbers may change. Consult LECO for latest information.
LECO Corporation
3000 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. Delivering the Right Results
Form No. 209-137 7/12-REV5 © 2012 LECO Corporation
 TUBE

Figure 6-10
Tube Removal

608-379
QUARTZ WOOL
STRIPS
2"

502-310
STEEL WOOL (5.1)
2"

601-390
FILTER
TUBE

Figure 6-11
Packing the Furnace Filter Tube

Maintenance FP-528 6 21
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 (850 oC) 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
(5.2) gases are swept through hot copper to remove oxygen and change NOx to N2, then
(5.3) 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.
(5.4) 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.

Theory of Operation FP-528 7 3

Perform Leak Check (8)

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 8 FP-528 Diagnostics
 (13.1)

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.

Operation FP-528 5 27
 Balance Configuration .................................................................. 4 19
Balance Configuration Definitions ............................................. 4 19
Barometric Calibration ................................................................. 4 20

(13.3) Catalyst Heater Calibration ........................................................... 4 21

Catalyst Heater Definitions ...................................................... 4 22
Combustion Furnace Calibration .................................................... 4 23
Combustion Furnace Definitions ............................................... 4 26
Assign User ................................................................................ 4 27

(13.2) 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

4 2 FP-528 System Setup

 (13.4)

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).

4 4 4 4
3 3 3 3
2 2 2 2
1 1 1 1
0 0 0 0
1 9 17 25 33 1 10 19 28 37 1 10 19 28 37 1 10 19 28 37
Time Time Time Time
Raw Area = 19 Raw Area = 18 Raw Area = 19 Raw Are a = 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).
19+18+19+18
Ab = - 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.

120 120 120

60 60 60
0 0 0
1 11 21 31 41 51 1 11 21 31 41 51 1 11 21 31 41 51

Ti me Time Time

7 8 FP-528 Theory of Operation

8
(13.5)

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
(13.6) Perform Leak Check ....................................................................... 8 8
Leak Check Definitions .............................................................. 8 9

Diagnostics FP-528 8 1
 (13.7)

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.

1 16 FP-528 Introduction
Return to Index (18)