Ankom TDF Operator's Manual
Rev 9/20/18
Operator’s Manual
2052 O’Neil Rd, Macedon NY 14502
Telephone: (315) 986-8090
Fax: (315) 986-8091
www.ankom.com
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Table of Contents
Introduction .................................................................................................................................................................. 5
Warranty ....................................................................................................................................................................... 5
Filter Bags ..................................................................................................................................................................... 5
Contact Information ..................................................................................................................................................... 5
Method Comparison (Manual vs. Automated) ............................................................................................................. 6
Instrument Description ................................................................................................................................................. 7
Service Access Position ............................................................................................................................................... 10
Operating Environment .............................................................................................................................................. 10
Safety Precautions ...................................................................................................................................................... 10
Instrument Installation ............................................................................................................................................... 11
Dietary Fiber Analysis Support Items .......................................................................................................................... 16
Analysis Options using the ANKOM
TDF
Dietary Fiber Analyzer ................................................................................... 16
Blanks .......................................................................................................................................................................... 16
IDF/SDF Analysis ......................................................................................................................................................... 17
TDF Analysis (AOAC 991.43) ....................................................................................................................................... 31
TDF Analysis (AOAC 985.29 / 2001.03) ....................................................................................................................... 44
Protein Determination ................................................................................................................................................ 59
Ash Determination ...................................................................................................................................................... 61
Productivity Enhancement ......................................................................................................................................... 63
Status Screen .............................................................................................................................................................. 67
Fault Handling ............................................................................................................................................................. 71
Diagnostics Mode ....................................................................................................................................................... 73
Periodic Maintenance ................................................................................................................................................. 81
Troubleshooting & Replacement Parts ....................................................................................................................... 82
QC / Calibration Checks .............................................................................................................................................. 83
Appendix A – Reagents (AOAC 991.43, 985.29, 2001.03) .......................................................................................... 89
Appendix B – Instrument Out-of-use Procedure ........................................................................................................ 91
Appendix C – De-fatting Procedure ............................................................................................................................ 93
Appendix D – Accessories (sold separately) ............................................................................................................... 95
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Operator’s Manual
Rev 9/20/18 pg. 5
Introduction
ANKOM Technology designs, manufactures, and markets instruments and support products used by analytical laboratories
around the world in the food, feed, bio-energy, agricultural, and environmental industries. ANKOM Technology can provide
you with products for determining or monitoring dietary fiber, detergent fiber, crude fiber, fat, digestibility, microbial
fermentation (anaerobic or aerobic) and more.
Committed to Total Customer Satisfaction, ANKOM designs every product based on a thorough assessment of customer needs.
Congratulations on your purchase of the ANKOM
TDF
Dietary Fiber Analyzer. We are confident that this product will
effectively serve your needs.
The ANKOM
TDF
Dietary Fiber Analyzer was designed to eliminate most of the manual steps required by the method. This
reduces technician variation, increasing precision. By carefully following the operating instructions in this manual you will
understand the details of sample and filter bag handling as well as instrument control, helping you to achieve the best possible
results.
Please review the entire manual before you begin operating this product.
Warranty
ANKOM Technology warrants the ANKOM
TDF
Dietary Fiber Analyzer against any defects in workmanship or material for one
year after the original date of purchase. This warranty does not include damage to the instrument resulting from neglect or
misuse. During the warranty period, should any failure result from defects in workmanship or materials, ANKOM Technology
will, at its discretion, repair or replace the instrument free of charge.
Extended warranties are available upon request.
Filter Bags
Use ANKOM Technology filter bags (part #’s DF-I, DF-S, DF-FT) in your ANKOM
TDF
Dietary Fiber Analyzer. Filter bags can
be purchased from ANKOM Technology or from your local authorized ANKOM distributor.
Contact Information
Committed to your total satisfaction, we are always available to help you get the most from your ANKOM products and to
receive any comments or suggestions you might have to help us improve.
For any questions or suggestions regarding your instrument, please contact us at:
• Telephone: (315) 986-8090
• Fax: (315) 986-8091
• Email: service@ankom.com
• www.ankom.com
Operator’s Manual
pg. 6 Rev 9/20/18
Method Comparison (Manual vs. Automated)
AOAC 991.43 Method – IDF/SDF assay without automation
Below is the AOAC 991.43 method flow done manually by a technician using glass crucibles and beakers, vacuum to assist
with filtering, and water baths to control temperature and mixing. DE refers to Diatomaceous Earth.
Prepare for Test
Digest Sample
Isolate IDF Residue
Isolate SDF Residue
1
Prepare crucibles
5 Heat to 95°C
17
Transfer to filter
26
Add 95% EtOH to fitrate
1a
Ash crucibles overnight
6 Add buffer
18
Filter with vacuum assist
27
Precipitate for 60 min
1b
Clean with vacuum
7 Add Amylase
19
Scratch filter bed as
needed
28
Transfer to filter
1c
Soak 1 hr @ room temp
8 Digest at 95°C for 35 min
29
Filter with vacuum assist
1d
Rinse with 3 solutions
9
Scrape beaker walls and
rinse with H2O to move
all residue to bottom
20
Rinse with 70°C H2O
30
Scratch filter bed as
needed
1e
Prepare DE filter bed
21
Rinse with 78% EtOH
1f
Dry @ 130°C
22
Rinse with 95% EtOH
31
Rinse with 78% EtOH
1g
Cool 1 hr and weigh
10
Cool to 60°C
23
Rinse with Acetone
32
Rinse with 95% EtOH
2
Weigh samples
11
Add Protease
24
Dry IDF residue
33
Rinse with Acetone
3
Prepare H2O bath(s)
12
Digest at 60°C for 30 min
25
Weigh IDF residue
34
Dry SDF residue
4
Place samples in beakers
13
Add HCl
35
Weigh SDF residue
14
Add AMG
15
Check/adjust pH
Calculate Results
16
Digest at 60°C for 30 min
36
Correct for Protein
37
Correct for Ash
38
Calculate results using
weights and corrections
AOAC 991.43 Method – IDF/SDF assay with ANKOM
TDF
Dietary Fiber Analyzer automation
Below is the AOAC 991.43 method flow when using the ANKOM
TDF
Dietary Fiber Analyzer. Steps highlighted in YELLOW
represent tasks done by a technician. Steps highlighted in GREEN (1a-1g, 9, 19, and 30) are no longer needed because of Filter
Bag Technology. All other steps (including mixing) are done automatically by the ANKOM
TDF
Dietary Fiber Analyzer under
computer control. DE refers to Diatomaceous Earth.
Prepare for Test
Digest Sample
Isolate IDF Residue
Isolate SDF Residue
5 Heat to 95°C
17
Transfer to filter
26
Add 95% EtOH to fitrate
6 Add buffer
18
Filter with pressure assist
27
Precipitate for 60 min
7 Add Amylase
28
Transfer to filter
8 Digest at 95°C for 35 min
29
Filter with pressure assist
20
Rinse with 70°C H2O
21
Rinse with 78% EtOH
22
Rinse with 95% EtOH
31
Rinse with 78% EtOH
1
Weigh filter bags
10
Cool to 60°C
23
Rinse with Acetone
32
Rinse with 95% EtOH
2
Weigh DE and samples
11
Add Protease
24
Dry IDF residue
33
Rinse with Acetone
3
Install filter bags
12
Digest at 60°C for 30 min
25
Weigh IDF residue
34
Dry SDF residue
4
Add DE & Sample to bags
13
Add HCl
35
Weigh SDF residue
14
Add AMG
15
Check/adjust pH
Calculate Results
16
Digest at 60°C for 30 min
36
Correct for Protein
37
Correct for Ash
38
Calculate results using
weights and corrections
This section is just an overview of how the ANKOM
TDF
Dietary Fiber Analyzer
executes the AOAC 991.43 method. Please see the “IDF/SDF Analysis” and “TDF
Analysis” sections of this manual for detailed instructions on how to perform
IDF/SDF and TDF assays with the analyzer.
Operator’s Manual
Rev 9/20/18 pg. 7
Instrument Description
The ANKOM
TDF
Dietary Fiber Analyzer is designed to efficiently, accurately, and precisely recover Insoluble Dietary Fiber
(IDF), Soluble Dietary Fiber (SDF), and Total Dietary Fiber (TDF) residue from food and/or feed samples in accordance with
the AOAC 991.43, AOAC 985.29, AOAC 2001.03, AACC 32-07.01, and NMKL 129, 2003 methods.
Contact ANKOM Technology about an upgrade to Total Integrated Dietary Fiber
(AOAC 2009.01 and 2011.25 methods). See the Diagnostics section of this
document for instructions on how to enable these methods.
Enabled by Filter Bag Technology, the instrument can run six digestion and six precipitation processes at the same time. The
filter bags are designed to capture the appropriate fiber particles while allowing all non-fiber components to pass through. The
instrument will use IDF bags and SDF bags when configured to recover IDF and SDF residue. The instrument will use IDF
Flow-Thru bags and SDF bags when configured to recover TDF residue.
The automated fiber recovery is achieved by first digesting samples within bags using enzyme treatments. Depending on the
filter bag configuration, the instrument then collects the IDF and SDF residue using two separate filters, or collects the TDF
residue using one filter. Once captured in the filters the residue is dried, weighed, and corrected for protein and ash content to
determine the IDF, SDF, and/or TDF values.
Digestion, precipitation, rinse (H2O and EtOH), and filter operations are performed by the instrument, eliminating manual
transfer and filtration steps. An on-board computer precisely controls process temperatures, agitation, and fluid delivery along
with digestion, precipitation, and filtration times.
External Components – Front View
Touch
Screen
Display
Filtrate Cup
(TDF53 - #1 of 6)
Waste Tray
IDF Station (#4 of 6)
SDF Delivery
Nozzle
(#1 of 6)
Clamp Bar A
Clamp Bar B
Control
Buttons
Hook for SDF Bag
(#3 of 6)
IDF Delivery
Nozzle
(#1 of 6)
Control Panel (TDF17)
Clamp Bar D
Clamp Bar C
SDF Station (#6 of 6)
Heating Paddle (#1 of 6)
Mixing Pad
(#2 of 6)
Service Access
Screw #1
Service Access Screw #2
Front Cover
(In UP position)
Pressure Gauge
Operator’s Manual
pg. 8 Rev 9/20/18
External Components – Left Side View
External Components – Right Side View
Control Panel (TDF17)
95% EtOH Container (TDF42)
HCl Container (TDF38)
Enzyme Containers
(TDF35, TDF36, TDF37)
Nitrogen Supply Port
80-100 psi
(5.5-6.9 bar)
Front Cover Arm
Power Switch
Front Cover (TDF56)
78% EtOH Container (TDF41)
Buffer Container (TDF39)
Distilled Water Container (TDF40)
Front Cover Arm
Three Container Holder
Single Container Holder
Pressure Gauge
Operator’s Manual
Rev 9/20/18 pg. 9
Internal Components – Rear View
N2
Check Valve
(1 of 12)
Main Electrical Cabinet
IDF Inlet Valve
Stations 4, 5 & 6
SDF Inlet Valve
Stations 4, 5 & 6
In-Line Heater
Tubing Support Panel
IDF Inlet Valve
Stations 1, 2 & 3
SDF Inlet Valve
Stations 1, 2 & 3
Waste Valves
(1 – 6)
Supply Valves
− Water
− Buffer
− 78% EtOH
− 95% EtOH
Vacuum Sensor
Supply
Manifold
Clamp Bar Cylinder
(1 of 8)
HCl
Supply Valve
Peristaltic
Pump
Pressure
Sensors
Drain Tube
Supply Valves
− Amylase
− Protease
− AMG
Torsion Bar (for
Front Cover)
Operator’s Manual
pg. 10 Rev 9/20/18
Service Access Position
If your instrument must be located in such a way as to restrict access to the back, you can tilt it forward to access the rear of the
instrument by removing the two Service Access Screws on the front of the instrument and gently pulling the top of the Main
Electrical Cabinet forward and down. The instrument will pivot at its center.
Operating Environment
Your ANKOM
TDF
Dietary Fiber Analyzer is designed to operate within the following environments:
• Ambient Temperature Range: 19°−30°C
• Humidity: 20–60% RH
• Power: 100V−120V ~ 50/60Hz 15A
220V−240V ~ 50/60Hz 8A
If after running this instrument you plan to leave it unused for 1 week or longer, you
must clear out the fluid lines to ensure proper operation. See “Appendix B –
Instrument Out-of-use Procedure” for more information.
Safety Precautions
Hot Surfaces – Do NOT touch the Heating Paddle surfaces during operation. The
surface can exceed 100°C (212°F). Failure to observe this caution may result in
burns.
Hazardous Voltages – Do NOT operate the instrument with the back of the Main
Electrical Cabinet removed. Hazardous voltages are present during operation. Failure
to observe this caution may result in electrical shock or electrocution.
Hazardous Materials – Ethanol is used within this instrument. Follow both local
and federal regulations for vent hood requirements when operating this instrument.
Do NOT heat seal or place filter bags in an oven until all acetone has evaporated.
Failure to observe this caution may be hazardous to your health.
WARNING: Attempts to override safety features or to use this instrument in a
manner not specified by ANKOM Technology voids the warranty and may result in
serious injury or even death.
This system is designed to meet and/or exceed the applicable standards of CE and
CSA.
The Power Switch must be in the OFF position before plugging the instrument Power
Cord into the power source.
Please review the entire manual before you begin operating this instrument.
Service Access
Screw #1
Service Access
Screw #2
Main Electrical
Cabinet
Operator’s Manual
Rev 9/20/18 pg. 11
Instrument Installation
Site Requirements
To install and operate the ANKOM
TDF
Dietary Fiber Analyzer you will need the following:
• Adequate power (see “Operating Environment” section of this manual)
• Drain or waste container to capture waste fluids
• Bench space that can accommodate the instrument dimensions of 132 cm (52”) L x 92 cm (35”) H x 77 cm (30”) D
• 80-100 psi (5.5-6.9 bar) Nitrogen Supply and connection tubing
Because the instrument is powered by pneumatics, do NOT run it without an
adequate Nitrogen Supply. You can run approximately 5 to 10 full assays
(IDF/SDF or TDF) with a 304 cu ft tank of nitrogen.
Instrument Installation Procedure
To install the ANKOM
TDF
Dietary Fiber Analyzer, follow the steps below.
1. Unpack and place the instrument where it will be used.
The instrument shipping container consists of three separate cardboard pieces: a top, a bottom, and a sleeve that forms the
body of the container. Remove the top and the sleeve of the instrument shipping container. Lift the instrument off of the
shipping container bottom and place it on a surface that is firm and level in an area near a Nitrogen Supply and a drain or
chemical waste container.
Waste fluids are drained from the instrument using gravity. Therefore, position the
instrument so that the drain tube can run down from the Waste Tray.
The instrument must not be subjected to excessive shock, vibration, dirt, moisture, oil, or other fluids.
Ethanol is used within this instrument. Follow both local and federal regulations for
vent hood requirements when installing this instrument.
2. Unpack the attachments and accessories.
Within the shipping container is a cardboard box containing attachments and accessories. Open the box and verify that all
of the following items are there.
1 – Crescent Wrench (204.9)
1 – 1/8” Allen Wrench (Z303)
1 – T-Handle Torx T20 Driver (Z276)
1 – 3/8” Nut Driver (8416)
1 – 3/8” wrench (8418)
2 – Spray Tips (TDF44)
1 - TDF Synthetic Grease (TDF107)
1 – Drain Hose Assembly (TDF96) that includes these five parts
1 - Adhesive Clamp (8133) 1 – Drain Tube (8132)
1 – Drain Tray (8002)
1 – Drain Tube Clamp (6138)
2 – Drain Tube Elbow Connectors (8288)
Operator’s Manual
pg. 12 Rev 9/20/18
1 – Pinch Valve Tubing Set (TDF71)
1 – Long Life Pump Tube Set (TDF99)
1 - Line Flush Tubing assy (TDF70)
1 – Amylase Container assy (TDF35)
1 – Protease Container assy (TDF36)
1 – AMG Container assy (TDF37)
1 – HCl Container assy (TDF38)
1 – Mes-Tris Buffer Container assy (TDF39)
1 – Distilled Water Container assy (TDF40)
1 – 78% EtOH Container assy (TDF41)
1 – 95% EtOH Container assy (TDF42)
6 – Filtrate Cups (TDF53)
1 – Control Panel assy (TDF17)
1 – Bag Weigh Holder assy (TDF52)
1 – Drying Rack assy (TDF50)
2 – Desiccant Pouches (X45)
1 – 3 meter Air Tube (8216)
1 – CD with Calculation Templates
1 – three container holder (8191)
1 – single container holder (8192)
1 – Spray Tip Cleaning Tool Kit (TDF94)
Operator’s Manual
Rev 9/20/18 pg. 13
2 – Container Filters (8202)
1 – Buffer Filter (8203)
4 – Bolts (5626)
4 – Nuts with star washers (167)
4 – Acorn Nuts (8409)
1 – Lighted Magnifier (TDF45)
2 – Fuses (8305-15A or 8306-8A)
Accessories specific to the 2009.11 & 2011.25 method upgrades can be found in
the "Automated AOAC 2009.01/2011.25 and AACC 32-45.01 method" addendum.
3. Place the Waste Tray under the front of the instrument.
With the Drain Tube connector pointing away from you, slide the tray under the front of the instrument until it cannot go
back any farther. (When the tray is in place, the side ridges will contact the front face of the steel frame.)
4. Place the six Filtrate Cups on the Waste Tray.
If filtrate collection is required for further analysis, leave the red plug in the lower port near the bottom of each of the
filtrate cups. If filtrate collection is not needed, keep the filtrate cups in place on the drain tray. However, the red plug can
be pulled from the lower port to drain the filtrate into the drain tray. Store the plug in the upper port.
5. Connect the Drain Tube to the Waste Tray.
Connect and secure the Drain Tube to the Waste Tray using the supplied Drain Tube Clamp. Run it to either a drain or a
waste container, avoiding twists in the tube. If necessary cut the Drain Tube and use the Elbow Connectors to meet the
needs of your location.
As needed, place the Adhesive Clamp (8133) between the Drain Tube Clamp and the Elbow Connector to create the
appropriate tube slope for good fluid flow.
6. Connect the Chemical Container Holders to the feet of the instrument.
Remove the nuts from the outside of the left and right feet of the instrument. Slide the single container holder onto the
bolts on the left foot and the three container holder onto the bolts on the right foot. Secure the holders using the nuts.
Bolts to attach the
three container holder
Bolts to attach the
single container holder
Elbow Connector
Drain Tube Clamp
Operator’s Manual
pg. 14 Rev 9/20/18
7. Connect the Control Panel to the instrument.
Remove the nuts from the right side of the instrument. Connect the 25 pin connector from the instrument to the Control
Panel. Slide the Control Panel onto the bolts and secure it in place using the nuts.
8. Place the Chemical Containers in their holders.
If you are going to run an IDF/SDF or TDF analysis immediately after installing
the instrument, fill the Chemical Containers above the Minimum Level lines and
fill the Enzyme Containers with at least 15 ml of solution before connecting the
containers to the instrument. See Appendix A for the chemical preparations.
Do NOT fill the Chemical and Enzyme Containers if the instrument is going to sit
unused after installation.
Place the HCl Container in the holder on the left side of the instrument. In the holder on the right side of the instrument,
place the Distilled Water Container in the front section, the Buffer Container in the middle section, and the 78% EtOH
Container in the back section. The 95% EtOH Container sits on the bench behind the container holder.
To ensure proper fluid delivery, you must use the Chemical Containers provided
with the instrument and place them in their specified locations.
9. Connect the Chemical Containers to the corresponding tubes.
The Chemical Containers and associated tubes are all
labeled and color-coded for easy connection. The large
containers on the right side of the instrument also have
push-on connectors. Make sure that you hear a click
sound when you connect the tubes to the containers.
On the left side of the instrument is a black tube with an
HCl label that has a white barbed fitting on its end. Push
the white barbed fitting into the black tube connected to
the HCl container.
Push-on
Connector
Bolts for
Control Panel
25 pin connector
Barbed
Fitting
Black tube connected
to HCl container
Operator’s Manual
Rev 9/20/18 pg. 15
10. Connect the Enzyme Containers to the corresponding ports.
The Enzyme Containers connect into labeled, color-coded ports on the left side of the instrument using push-on
connectors. Make sure that you hear a click sound when you connect the enzyme containers to the ports.
11. Connect the Nitrogen Supply to the Nitrogen Supply Port.
Connect the 3 meter Air Tube (8216) that came with the
instrument to the Nitrogen Supply Port on the instrument
and to the Nitrogen Supply.
If you want to use a separate tube to connect your instrument to a Nitrogen Supply,
the Nitrogen Supply Port has a Push-to-Connect fitting that accepts ¼” OD tubing.
Acceptable tubing materials include Nylon, Polyurethane, Polyolefin, and
Polytetrafluoroethylene (PTFE). The tubing material must be suitable for the
specified pressure.
12. Verify that the High and Low Pressure Regulators are set properly.
Verify that the High Pressure Regulator is set to 50 psi (3.5 bar), and the
Low Pressure Regulator is set to 4-6 psi (0.3-0.4 bar).
Push-on
Connector
Nitrogen Supply Port
80-100 psi
(5.5-6.9 bar)
High Pressure Regulator
50 psi
(3.5 bar)
Low Pressure Regulator
4-6 psi
(0.3-0.4 bar)
Operator’s Manual
pg. 16 Rev 9/20/18
Dietary Fiber Analysis Support Items
The following support items needed to perform the fiber analysis may be purchased separately:
Item
ANKOM Part #
Electronic Balance with four-place readout
TB
Electronic Balance Software
TBS
Heat Sealer for sealing the filter bags
HS (120V), HSi (220V)
IDF Filter Bags
DF-I
SDF Filter Bags (used for SDF and TDF procedures)
DF-S
IDF Flow-Thru Bags (TDF procedure only)
DF-FT
Solvent Resistant Marker
F06
Rinse Stand
TDF51
Diatomaceous Earth (DE)
DE1, DE2
Drying Oven
Ashing Oven
Protein Determination Equipment (Kjeldahl is recommended)
Analysis Options using the ANKOM
TDF
Dietary Fiber Analyzer
The ANKOM
TDF
Dietary Fiber Analyzer can be configured to recover IDF and SDF residue, or to recover TDF residue. The
following describes these analyses along with their specific filter bag configurations.
Analysis Name
Analysis Description
Upper Bag
Lower Bag
IDF/SDF
(991.43)
This analysis is used to determine IDF and SDF residue separately
using two different filter bags. TDF is calculated by adding the IDF
and SDF residue weights corrected for protein and ash content.
IDF
SDF
TDF
(991.43, 985.29 &
2001.03)
This analysis is used to determine TDF residue in one filter. In this
analysis, the TDF value consists of the weighed residue corrected
for protein and ash.
IDF Flow-Thru
(no filter)
SDF
A computer controlled Diagnostics mode is provided through the Control Panel for maintenance and troubleshooting purposes.
To maximize productivity, this instrument also allows a user to start new procedures (IDF/SDF and TDF) before the previous
ones have completed. See the “Productivity Enhancement” section of this manual for details.
Contact ANKOM about an upgrade to Total Integrated Dietary Fiber (AOAC
2009.01 and 2011.25 methods). See the Diagnostics section of this document for
instructions on how to enable these methods.
Blanks
BLANK values are used in the IDF, SDF, and TDF calculations. The following BLANK values (based on extensive research
done in the ANKOM lab) are the default values loaded in the IDF_SDF and TDF spreadsheets in the MS-Excel workbook
provided with the instrument.
IDF (AOAC 991.43 method): -0.0072 TDF (AOAC 991.43 method): -0.0047
SDF (AOAC 991.43 method): -0.0030 TDF (AOAC 985.29 method): -0.0028
You do not need to run BLANKS with every set of samples. However, if you want to determine your own BLANK values,
especially when you change chemical lots, ANKOM recommends that the BLANK value in the IDF, SDF, and TDF
calculations be the average of at least 18 BLANK values.
If you determine your own BLANK values, you can overwrite the values currently in the MS-Excel spreadsheets.
Operator’s Manual
Rev 9/20/18 pg. 17
IDF/SDF Analysis
An IDF/SDF analysis measures the amount of IDF and SDF within a given sample. This requires the use of ANKOM DF-I and
DF-S filter bags. When starting a new run, the ANKOM
TDF
Dietary Fiber Analyzer must have bags installed at all stations (a
total of twelve bags).
To enhance the productivity of your instrument, you can begin the IDF process of a
new run while the SDF process of a previous run is finishing. See the “Productivity
Enhancement” section of this manual for more details.
To perform an IDF/SDF analysis, follow the steps below.
1. Prepare chemicals and enzymes.
When using the ANKOM
TDF
Dietary Fiber Analyzer for the AOAC 991.43, AACC 32-07.01, and NMKL 129,2003
methods use the chemicals and enzymes referred to therein. See Appendix A of this manual for the list of chemicals and
enzymes and the instructions for how to prepare them for use in this instrument.
2. De-fat your samples as needed according to the official methods. See "Appendix C – De-fatting
Procedure" in this manual for an ANKOM procedure.
3. Label the filter bags using a Solvent Resistant Marker.
4. Prepare for data collection.
You will need a place to store the data collected during this analysis. For your convenience a CD titled “Calculation
Templates” was included with the instrument. This CD has data spreadsheets that can be used for this analysis. Please
read the “Instructions” tab in the MS-Excel file for information about the spreadsheets.
5. Weigh filter bags.
Using a Bag Weigh Holder is critical to eliminate the effects of static electricity
during the weighing process.
Roll or fold each bag and place it in a tared Bag Weigh Holder. Place the Bag Weigh Holder in the center of a balance
and record the weight.
Because different balances have different sensitivities, the Bag Weigh Holder
should be placed in the center of the balance for best results.
IDF Bag (shorter bag)
SDF Bag (longer bag)
Operator’s Manual
pg. 18 Rev 9/20/18
6. Weigh Diatomaceous Earth (DE).
DE is used during fiber analysis to enhance the flocculation and filtration of the SDF fraction. Place ca 1 g of DE in each
of six tared and numbered tins and record the weights.
7. Weigh Samples.
Place 0.50.05 g of sample in each of six tared and numbered tins and record the weights.
A larger sample (1.0 g) can be used if a larger aliquot is needed to improve
precision.
8. Turn the instrument power on.
When you turn the power on, the instrument will run through an initialization process and the Control Panel will turn on.
9. On the Touch Screen Display, select the instrument function you would like to perform.
The Control Panel on the ANKOM
TDF
Dietary Fiber Analyzer uses Touch Screen technology. To operate the instrument
you will press identified buttons on the Touch Screen Display and buttons below the screen.
When your instrument is initialized and ready to operate, the following screen will be displayed.
Although the instrument works in accordance with AACC and NMKL methods, the
Touch Screen Display only refers to the AOAC methods.
9.1 If this is the first time the instrument is being operated after being installed, or after sitting unused for a period of
time (see Appendix B), or after tubing was replaced, the lines must be charged to avoid a Vacuum Sensor Fault.
To charge the lines follow the steps below.
9.1.1 Press the Diagnostics button on the “Select a Function” screen. The following screen will be displayed.
Diagnostics
Touch Screen Display version: A.AA
SPLat controller software version: vX.XX dd-mm-yy
Pump Tube
Test
Expert Mode
Faults
Service
Mode
Clear IDF /
SDF lines
Digestion
Times
Heater Test
Temperatures
Pressures
Line Charge
Motor Test
Valve Test
Select a Function
AOAC 991.43
IDF/SDF
AOAC 985.29
TDF
Diagnostics
AOAC 991.43
TDF
AOAC 2001.03
TDF
←
Operator’s Manual
Rev 9/20/18 pg. 19
9.1.2 Press the Line Charge button. The following screen will be displayed.
9.1.3 Press the ALL button to charge all of the lines. Each button will change color as the associated line is being
charged. All lines are charged when all of the buttons return to their original green color.
9.1.4 Press the back button twice. The following “Select a Function” screen will be displayed again.
9.2 Press the AOAC 991.43 IDF/SDF button. The following screen will be displayed.
Notice that the function you selected is now displayed in the top right corner of the screen and a back button
is displayed in the top left corner of the screen.
SDF Bags (and clamp bar D) installed?
←
AOAC
991.43
IDF/SDF
Select a Function
AOAC 991.43
IDF/SDF
AOAC 985.29
TDF
Diagnostics
AOAC 991.43
TDF
AOAC 2001.03
TDF
Line Charge
Amylase
Protease
AMG
HCl
EtOH78
EtOH95
Water
Buffer
ALL
Vacuum xx.x
cur: - x.x
max: - x.x
←
Operator’s Manual
pg. 20 Rev 9/20/18
10. Install SDF filter bags on the ANKOM
TDF
Dietary Fiber Analyzer.
10.1 Remove Clamp Bars A, B, C, and D by lifting them off of the locator rods.
10.2 Gently pull the black SDF Delivery Nozzle out toward you.
10.3 Place a labeled and weighed SDF bag up underneath the SDF Delivery Nozzle so that the Delivery Nozzle is
inside the top part of the bag. Pull the bag up so that the top of the bag is about 35 mm (1.375 inches) above the
top of Clamp Bar C and return the Delivery Nozzle to its original position. This will hold the back of the bag in
place.
As part of normal operation, solution from the IDF bag will flow into the SDF bag.
Therefore, when installing the SDF filter bags it is very important to position them
high enough vertically so that at least 20 mm (0.75 inches) of the filter part of the
IDF bag can fit inside the top of the SDF bag.
Clamp Bar C
Clamp Bar D
Clamp Bar B
Clamp Bar A
Operator’s Manual
Rev 9/20/18 pg. 21
10.4 With the bag being held by the Delivery Nozzle, center it horizontally between the lines on the back part of
Clamp Bar C.
10.5 Repeat steps 10.2 – 10.4 for all six stations.
10.6 Re-install Clamp Bar D by setting it on the locator rods. Make sure the letter is on the top of the bar and the
rubber material is facing in toward the instrument.
10.7 Flatten the bags to remove any wrinkles.
10.8 With fingers away from the clamp bars, press the check mark () button on the Touch Screen Display to pinch
the bags just above the filter. The following screen will be displayed.
11. Add DE to the SDF filter bags on the ANKOM
TDF
Dietary Fiber Analyzer.
11.1 Open the top of the SDF bag and add a weigh tin of DE to the bag by folding the tin and then dipping it down into
the bag below the tip of the Delivery Nozzle.
When adding DE to the filter bags it is very important to keep it below the tip of
the Delivery Nozzle so that the DE material can be properly rinsed.
11.2 Rinse the tin with no more than 3 ml of 78% EtOH to ensure complete transfer.
11.3 Repeat steps 11.1 – 11.2 for all six stations.
Diatomaceous Earth
added in SDF Bags?
AOAC
991.43
IDF/SDF
←
Centering Lines
Operator’s Manual
pg. 22 Rev 9/20/18
11.4 Press the check mark () button on the Touch Screen Display. The following screen will be displayed.
After you confirm that the DE is added, the Clamp Bar D button on the Control
Panel is disabled until the SDF process completes.
12. Install IDF filter bags on the ANKOM
TDF
Dietary Fiber Analyzer.
12.1 Gently pull the black IDF Delivery Nozzle out toward you.
12.2 Place a labeled and weighed IDF bag up underneath the Delivery Nozzle so that the Delivery Nozzle is inside the
top part of the bag. Pull the bag up so that the top of the filter part of the IDF bag is just below the bottom of
Clamp Bar B and return the Delivery Nozzle to its original position. This will hold the back of the bag in place.
12.3 With the bag held by the Delivery Nozzle, center it horizontally between the Centering Lines on the back part of
Clamp Bar A.
For proper mixing during the IDF process the IDF bags must be horizontally
centered over the Heating Paddles and between the Centering Lines on the back
part of Clamp Bar A.
IDF Bags (and clamp bar B) installed?
←
AOAC
991.43
IDF/SDF
Centering Lines
Heating Paddle
Operator’s Manual
Rev 9/20/18 pg. 23
12.4 Place at least 20 mm (0.75 inches) of the filter section of the IDF bag inside the top of the SDF bag to allow for
the flow of liquid into the SDF bag after the IDF process is complete.
12.5 Repeat steps 12.1 – 12.4 for all six stations.
12.6 Re-install Clamp Bar B by setting it on the locator rods. Make sure the letter is on the top of the bar and the
rubber material is facing in toward the instrument.
12.7 Flatten the IDF bags to remove any wrinkles.
12.8 With fingers away from the clamp bars, press the check mark () button on the Touch Screen Display to pinch
the IDF bags just above the filter. The mixing pads will make contact with the bags when Clamp Bar B pinches
the IDF bags. The following screen will be displayed.
13. Add samples to the IDF bags.
13.1 Open the top of the IDF bag and transfer the sample from a weigh tin into the IDF bag by folding the tin and then
dipping it down into the bag below the tip of the Delivery Nozzle.
When adding sample to the filter bags it is very important to keep it below the tip
of the Delivery Nozzle so that it can be properly rinsed.
Samples in IDF Bags?
←
AOAC
991.43
IDF/SDF
Clamp Bar B
Top part of the filter is
positioned just below the
bottom of Clamp Bar B
20 mm (0.75 inches) of
the IDF filter inside the
top of the SDF bag
Heating Paddle
Operator’s Manual
pg. 24 Rev 9/20/18
13.2 Rinse the tin with no more than 3 ml of Distilled Water to ensure complete transfer.
13.3 Repeat steps 13.1 – 13.2 for all IDF stations.
13.4 Re-install Clamp Bar A by setting it on the locator rods. Make sure the letter is on the top of the bar and the
rubber material is facing in toward the instrument.
13.5 Press the check mark () button on the Touch Screen Display. The following screen will be displayed.
13.6 Make sure that all clamp bars are installed with the letter on the top of the bar and the rubber material facing in
toward the instrument. Press the check mark () button on the Touch Screen Display. The following screen will
be displayed.
14. Hook the front of each SDF bag in place.
14.1 Secure the SDF filter bags in place with the hooks located on the front part of Clamp Bar C.
Hooking the bags in place will put a physical hole in the front of each SDF bag.
14.2 Press the check mark () button on the Touch Screen Display. If you ran a method other than 991.43 prior to this
run, the following screen will be displayed.
Front of SDF Bags hooked to clamp bar C?
←
AOAC
991.43
IDF/SDF
All remaining clamp bars installed?
←
AOAC
991.43
IDF/SDF
Hook on front part of
Clamp Bar C
Operator’s Manual
Rev 9/20/18 pg. 25
15. Verify that the fluid containers have the correct fluids for this procedure.
Verify that the fluid supply containers are configured according to the screen above and press the check mark () button.
The following screen will be displayed.
16. Fill fluid containers.
To ensure that you have enough fluids to run a complete IDF/SDF procedure, you must begin with fluid levels above the
Minimum Level lines on the chemical containers and at least 15 ml of each enzyme. Add fluids and enzymes as
necessary.
Do NOT leave the enzyme ports on the instrument open to the air or the enzymes
in the valves may dry up and plug the ports.
With all fluid containers filled to the proper levels, press the check mark () button on the Touch Screen Display. The
following screen will be displayed.
Nitrogen supply ON?
←
AOAC
991.43
IDF/SDF
Fluid levels correct?
←
AOAC
991.43
IDF/SDF
Amylase -> Amylase
AMG -> AMG
HCL -> HCL
Buffer -> Mes Tris Buffer
←
Check supply containers
AOAC
991.43
IDF/SDF
Operator’s Manual
pg. 26 Rev 9/20/18
17. Connect the Nitrogen Supply to the instrument and turn on.
Make sure the Nitrogen supply in your lab is connected to the instrument and turned on. The pressure gauges on the
instrument should show 50-55 psi on the left and about 4 psi on the right.
Press the check mark () button on the Touch Screen Display. The following screen will be displayed.
18. Set filter times (in minutes).
Because different samples take different amounts of time to filter, the above screen allows you to set your filter times. To
change any of the times shown on the screen, press the specific gray button. A number pad will be displayed that will
allow you to enter the time that you want. The times you enter will remain until you change them again.
The initial filter times shown when you first run the instrument are based on factory
experience. During filtration the computer allows you to bypass the filter time if
you notice the filtering is complete. The computer also allows you to add time
during filtering if needed (see the “Status Screen” section of this manual for more
detail).
When all of the times shown on the screen are what you want, press the check mark () button on the Touch Screen
Display. The following screen will be displayed.
19. Set the Manual pH Check.
If you plan to check the pH after the required HCl is added (during the IDF process), press the Yes button on the screen
above. Otherwise, press the No button. The following screen will be displayed.
Check pH manually?
←
Yes
No
AOAC
991.43
IDF/SDF
Filter minutes OK?
←
After release
After water rinses
After EtOH rinses
After release
After EtOH rinses
5.0
1.0
1.0
10.0
3.0
IDF
SDF
(Press button with number to change)
AOAC
991.43
IDF/SDF
Operator’s Manual
Rev 9/20/18 pg. 27
20. Start the instrument.
The instrument is now completely set up and ready to automatically run the IDF/SDF procedure. Press the START button
to begin. At the beginning of each new run, the instrument automatically runs a tube integrity test.
For the first run after a power-up cycle, or for the first run after the instrument has been idle for twelve hours, the
following screen will be displayed.
If the fluid lines are already charged properly, or when the line charge is complete, the following screen will be displayed.
When the tube integrity check is complete, the instrument will automatically execute the IDF/SDF procedure stopping
only for faults, aborts, and manual pH measurement (if enabled). The Status screen will show actions and faults as they
occur during the automatic operation.
Testing pump tubing.
Please wait..........
Initializing lines…
Amylase
EtOH78
Protease
EtOH95
AMG
Water
HCL
Buffer
Vacuum xx.x
cur: - x.x
max: - x.x
Press START to begin
←
START
AOAC
991.43
IDF/SDF
Operator’s Manual
pg. 28 Rev 9/20/18
21. Manually measure pH.
One of the questions you are asked before starting the automated procedure is: “Check pH manually?” If you answered
“Yes” to this question, the instrument will stop after adding the required HCl, open Clamp Bar A, display the screen
below, and make a sound to remind you to manually measure pH and adjust to 4.0 - 4.7 if necessary.
When measuring pH, use a probe that can be easily rinsed (with Distilled Water) to
avoid loss of sample. If you add 0.5N HCl or base to adjust the pH, you must mix
the solution in order to get an accurate pH reading. To manually mix the solution,
press the outside of the bag with your fingers just above Clamp Bar B multiple
times.
When you have completed the pH measurement process, press the Continue button on the Status screen. You will see
“COMPLETE” next to “pH required?” in the upper left corner of the screen.
22. Rinse the IDF filter bags with acetone.
After the instrument has completed an IDF process the IDF residue that has been collected in the IDF bag must be
manually rinsed twice with acetone. It is recommended that you use an ANKOM TDF51 Rinse Stand (sold separately) for
rinsing filter bags with acetone.
To rinse the IDF filter bags with acetone using the ANKOM TDF51 Rinse Stand, follow the steps below.
22.1 Remove the IDF bags from the instrument.
22.2 Place the bags on the Rinse Stand by sliding the back part of each bag under the
pinch mechanism. Keep the top of the bag open.
22.3 Using a wash bottle, squirt acetone completely around the inside polypropylene
surfaces of each bag, making sure that all residue on the surfaces is rinsed down
into the filter.
22.4 Repeat step 22.3 so that each bag gets rinsed a total of two times.
22.5 Allow acetone to evaporate from the bags.
Hazardous Materials – Do NOT heat seal or place bags in an oven until all
acetone has evaporated.
Status
Overall Progress
Action in progress
IDF
Time remaining:
Amylase/AMG Phase
XX:XX:XX
Time remaining: XX:XX:XX
SDF
Time remaining:
XX:XX:XX
pH required?
Display
Temps/Pressures
YES
IDF
ABORT
PAUSE
SDF
ABORT
AOAC
991.43
IDF/SDF
Vacuum xx.x
cur: - x.x
max: - x.x
Check pH
then press continue
xx:xx:xx
Continue
Operator’s Manual
Rev 9/20/18 pg. 29
22.6 With your Heat Sealer set between 3 and 4 (settings may vary depending on the
heat sealer and the power source), press the Heat Sealer arm down. Hold the
arm down for 3 to 4 seconds after the light goes out to seal each bag just
above the filter. This keeps all residue contained to the filter area while handling
the bags.
22.7 Place each bag in the Drying Rack.
23. Rinse the SDF filter bags with acetone.
After the instrument has completed an SDF process the SDF residue that has been collected in the SDF bag must be
manually rinsed with acetone. It is recommended that you use an ANKOM TDF51 Rinse Stand for rinsing filter bags with
acetone.
To rinse the SDF filter bags with acetone using the ANKOM TDF51 Rinse Stand, follow the steps below.
23.1 Remove the SDF bags from the instrument.
23.2 Place the bags on the Rinse Stand by sliding the back part of each bag under the pinch mechanism. Keep the top
of the bag open.
23.3 Using a wash bottle, squirt acetone completely around the inside polypropylene surfaces of each bag, making sure
that all residue on the surfaces is rinsed down into the filter.
23.4 Repeat step 23.3 so that each bag gets rinsed a total of two times.
23.5 Allow acetone to evaporate from the bags.
Hazardous Materials – Do NOT heat seal or place bags in an oven until all
acetone has evaporated.
23.6 Seal each bag just above the filter to keep all residue contained to the filter area while handling the bags.
Sealing each bag as close to the filter as possible allows you to trim the maximum
amount of polypropylene from the bag before determining the protein content.
23.7 Place each bag in the Drying Rack.
24. Dry the IDF and SDF filter bags.
24.1 Make sure your oven is 105°C at the location where the bags will be placed.
24.2 Place the Drying Rack with the filter bags in the oven and dry to constant weight (about 90 minutes).
24.3 When dry, remove all IDF and SDF filter bags from the oven and place them in separate desiccant pouches.
25. Weigh the IDF residue.
25.1 Remove only one IDF filter bag from the desiccant pouch at a time.
25.2 Roll or fold the bag, place it in a tared Bag Weigh Holder (BWH), and place the BWH in the center of a balance.
25.3 Record the weight of the filter bag.
25.4 Repeat steps 25.1 – 25.3 for each IDF filter bag used in the fiber analysis.
26. Weigh the SDF residue.
26.1 Remove only one SDF filter bag from the desiccant pouch at a time.
26.2 Roll or fold the bag, place it in a tared Bag Weigh Holder (BWH), and place the BWH in the center of a balance.
26.3 Record the weight of the filter bag.
26.4 Repeat steps 26.1 – 26.3 for each SDF filter bag used in the fiber analysis.
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