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Manual ATN-1100 Automatic Kjeldahl Nitrogen Determination Apparatus

This document provides an overview and technical specifications for the DW-ATN-1100 series automatic Kjeldahl nitrogen analyzer. The analyzer uses a 7.5-inch touchscreen for simple operation and control via Siemens PLC. It features a self-suction diaphragm pump for reagent feeding, modified silicone piping, quick-connect fittings, automatic alkali addition, titration curve viewing, and safety protections. The analyzer is designed to perform nitrogen determination via the Kjeldahl method in accordance with science, technology, and precision for analytical assays.
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0% found this document useful (0 votes)
210 views35 pages

Manual ATN-1100 Automatic Kjeldahl Nitrogen Determination Apparatus

This document provides an overview and technical specifications for the DW-ATN-1100 series automatic Kjeldahl nitrogen analyzer. The analyzer uses a 7.5-inch touchscreen for simple operation and control via Siemens PLC. It features a self-suction diaphragm pump for reagent feeding, modified silicone piping, quick-connect fittings, automatic alkali addition, titration curve viewing, and safety protections. The analyzer is designed to perform nitrogen determination via the Kjeldahl method in accordance with science, technology, and precision for analytical assays.
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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In strict accordance with science and technology and precision used for analysis and assay

Automatic Kjeldahl Apparatus


DW-ATN-1100

Drawell International Technology Limited


Shanghai Drawell Scientific Instrument Co.,Ltd

Add :Suite 1506,Lane581 XiuChuan Rd.,PuDong New Area,Shanghai,China


Tel/ Fax: 0086 21 50966080
Web : www.drawell.com.cn
Email : [email protected]
In strict accordance with science and technology and precision used for analysis and assay

Table of contents
Safety instructions ……………………………………………..………Page 1
Packing list …………………………………………………………….Page 3
Product overview and characteristics ………………………………Page 4-9
A. Product Overview…………………………….…..Page 4-8
B. Working Principle…………………………….…..Page 8
C. Technical Standard………………………….…..Page 9
Instrument structure and installation …………………………… Page10-11
Instrument initiate adjustment …………………………….……... Page 12-17
A. Reagent pump flow calibration ……………… Page12
B. System settings……………………………….…..Page15-17
C. Formula managemen……………………….…..Page17
Data inquiry……………………………………………………………… Page 18
Operation method ……………………………………………………Page19-23
Titrating solution calibration ………………………………….….Page 24
Safety system ………………………………………………………… Page25
Attention and maintenance ……………………………………….. Page26
Common problems and solution ………………………………… Page26-29
Reagent preparation method ………………………………………Page30-33
Commonly-used consumables …………………………………… Page31-34

Version: 2018/v01
Dear user:

Thank you for using our products. Please read the operation manual of the product very carefully

prior to using our products to ensure that the instrument is able to run effectively.

Please don’t hesitate to contact us for further assistances and / or services; we are willing to provide

you the most personalized service.

We tried to make our manual as “detailed”, “professional” and “simple” as possible; nevertheless, we

are sorry for the misunderstanding and inconveniences of reading due to the inevitable errors.

We always looking forward to your valuable comment and / or idea which about the operation of the

instrument; and we’ll absolutely cherish and hold it as treasure.

Safety Instructions!

Warning Please use Do not repair it Keep away from


grounding wire by yourself. explosive
substances

1、 Operator shall use the instrument according to the operation requirements, or else, property losses or

personnel injury can be caused.

2、 Please use power supply with voltage of AC110V/50Hz(60Hz)

3、 Please use independent outlet, and make sure that outlet ground wire is in good condition (it is strictly

forbidden to use null line or neutral line as ground wire)

4、 Please do not plug or unplug the instrument without turn off power switch.

5、 Please do not repair without permission, and professional guidance is needed if the repair is

authorized by Jinan Jing Rui Analytical Instrument.

6、 Please make sure the equipment stay away from the electromagnetic interference sources in order to

avoid program disorder and data error.

7、 Please use in working environment with temperature of 10℃--45℃ and relative humidity less than
80%.

8、 Please use in the environment without dust and combustible and explosive gas

9、 Please do not install instrument at position with direct sunlight to ensure data accuracy and prevent

premature aging of instrument

10、 For reagent and other solutions is corrosive! Please wear protection gear and operate according to

user manual.
full-automatic Kjeldahl azotometer packing list

Please check all accessories according to the following list

One set of DW-ATN-1100 One 25L waste liquid barrel (green label)

mainframe One 1L dropping bottle One 10L distilled water barrel (blue label)
One 5L boric acid barrel (yellow label)
One 5L alkaline solution barrel (red label)

One Cooling water inlet pipe One Cooling water outlet pipe One Distilled water delivering pipe (blue label 3 m)
(including adapter) 5 meter 1 One Alkaline liquor delivering pipe (red label 3m)
5 meter One Boracic acid delivering pipe (yellow label 3m)
One Liquid waste delivering pipe (green label 3m)

One bottle catalyzer 250g One Cooling water inlet One Sample room water
Five rolls of printing paper pipe seal ring receiver

One
One Digestion tube (it has been installed in instrument
One wrench
Power cord (110V/10A) sample chamber)
Φ42*300mm)
Product qualification certificate Product serial number sticker 2 pieces
Product Manual And
2 copies Product warranty card
Chapter I: Overview and technical standard of DW-ATN-1100 series
azotometer
Kjeldah method is the classical method for determining nitrogen contents. At present, kjeldah
method is widely used for determining nitrogen-containing compound in soil, food, agricultural products,
fodder and others. Three procedures including sample digestion, distillation separation and titrimetric
analysis shall be conducted successively in case of using above method
DW-ATN-1100 series full-automatic kjeldahl azotometer is a kind of analysis system used for
determining titration endpoint with full-automatic distillation ——color method and developed according
to classic kjeldah method. Products of the series include base-type DW-ATN-1100, professional type
DW-ATN-1100A, computer type DW-ATN-1100B products, and their operating methods are basically same.
The manual gives guidance and description based on DW-ATN-1100A
I. DW-ATN-1100 series products’ characteristics
1、 DW-ATN-1100 characteristics
 The system uses 7.5-inch color touch screen+ Siemens PLC
control module and an interactive touch screen in order to be
operated simply and conveniently and easily to learn. (see
Figure 1-1)
 Feed liquid pump—— Anti-corrosion self-suction diaphragm
pump is used for feeding, abandoned air-filled feeding Figure1-1
methods which is used by many other manufactures. Use of
self-suction pump for feeding can generate many advantages
such as enable liquid feeding barrel to be away from main
frame or placed under operating floor and so on.
 Pipeline system—— Uses imported (made in USA) modified
silicone pipe that cannot be deformed and corroded under
strong acid and alkali environment for a long time. Figure 1-2
 Use of American CPC quick-connect pipe fitting (see
Figure1-2) enable instrument to be used conveniently also
prevent liquid and gas leakage in the system.
 Titration system —— Enable user easily to check the accuracy
and reliability of the result at any time during titration
processes at any time. (Figure 1-3)
 Visible titration cup—— Enable user to observe the change
during titration processes, improve the convenience for
cleaning and changing the cup. Figure 1-3
 Pre-heating function—— Maintain steam generator
temperature at pre-set temperature range to maintain the starting-up or standby status, which is
beneficial to generating steam quickly in case of analysis and shortening analysis time
 Automatic alkali solution adding mode for preventing overreaction between alkali and acid
 Automatic alkali solution adding——In case of insufficient alkali solution added during operation,
adding procedure can be conducted repeatedly to avoid analysis error or sample scrapping
caused by insufficient quantity of alkali solution. (see Figure1-4)

 Automatic titration cup cleaning——Automatic spraying of titration
cup cleaning can prevent residual liquid in the cup influencing
low-content sample or blank sample and improve system accuracy
 Automatically deducting blank value in sample——blank value of
sample can be deducted automatically.
 Titration curve——Enable user to observation the whole processes to
located the error appeared during titration processes. (see Figure 1-4
Figure1-6)`leakage and electric shock due to various factors and
protect operator.
 Digestion tube absence protection——If digestion tube is not
provided, reagent adding and heating shall not be conducted to
prevent personal injury caused by reagent and steam.
 Safety door protection——Transparency safety door with thickness of
Figure1-5
5mm can be operated conveniently and safely to ensure personal
safety.
 Water shortage protection for steam system——System can shut down automatically and send
alarm in case of water shortage in the system to prevent accidents
happening.
 Steam kettle over-temperature protection system——System can
shut down automatically and send alarm in case of over-temperature
in steam kettle caused by distillation system fault.
 Safety alkali solution adding mode——Use of this mode can prevent
reduce strong neutralization reaction during adding alkali and
Figure1-6
prevent pipe bursting.
2、 DW-ATN-1100A newly-increased functions (in addition to possession of above
characters)
 Formula management——User can add 10 preset parameters into instrument, increase the
convinces of the operation.
 Analysis mode —— Two modes including “automatic analysis” and “manual analysis” provide
convenience for operator.
 Automatic discharge for waste liquor in digestion tube——After completing titration, waste
liquid in digestion tube will discharge automatically and be collected, improvement of degree of
automation reduces labor strength of staff and enable concentrated collection of waste liquid
after analysis
 Alkali liquid pipeline cleaning—— implementation of alkali liquid cleaning by pressing “alkali
pipeline cleaning” button regularly can prevent blocking in the pipeline and improve feeding
accuracy (see Figure 1-6)
 Titrating solution concentration (mol) auto-calibrating system——the calibration method can be
used to eliminate difference caused by “titration by instrument” after using “manual calibration”
and make system error smaller and analysis accuracy higher.
 Simultaneous titration and calibrating —— Increase the efficiency and save the energy and
resource.
 Steam flow adjustment——Two levels include 100% “high steam content” and 75% “middle
steam content” are provided for users to choose.
 Cooling water flow display——user can observe condition of cooling water flow at any time to
prevent insufficient cooling due to too small water volume or wasting water due to too large
water volume
 Steam overpressure protection —— If pipeline blocking causes abnormal high pressure in steam
system, the system can shut down automatically and send alarm to prevent accidents becoming
more severe and protect operators and property safety.
 Temperature monitoring system of distilling samples——Prevent distilled samples data error
caused by insufficient cooling water or too high temperature, monitoring system will shut down
automatically and send alarm.
 Cooling water volume statistic (XX3) —— Through the data, user can know cooling water
consumption of cooling water (in statistics) to calculate the expenses.
 Multi-function interface:
A. Reagent barrel level display alarm interface ——in case of insufficient reagent in reagent barrel
and distilled water barrel, the system will send alarm and shut down to prevent instrument operating
under condition of no reagent and distilled water. (the system is “optional”)
B. Recirculation cooler interface——after azotometer is connected to “intelligent cooling water
system”, “cooling system” doesn't need to be set or opened or closed again. When azotometer is
opened, “cooling system” automatically starts up and execute inner cycle program, when there is
steam generated in azotometer, above program in “cooling system” is automatically changed into
outer cycle program to lower temperature of azotometer (see Figure1-7 and Figure 2-2) (note: the
system shall be used together with “intelligent cooling water system” produced by the
manufacturer)
 USB interface——Mainly used for connecting wireless mouse and analyzing data and exporting
data. (see Figure 1—7,Figure 2--2)
3、 DW-ATN-1100A newly-increased functions (in addition to possession of
above performances)
 Computer operating software, computer interface ( 485 ) ——Enable
computer control and management (see Figure 1—7,Figure2--2)
 Internet interface ——Enable remote control and instant data transfer (see
Figure1—7,Figure2--2)
 Group user’s management center——control center consists of 2 sets-50
sets of “full-auto Kjeldahl azotometer” and can realize dynamic
monitoring, instantaneous transmission of data and control center data
storage for any instrument
4、 Working principles Figure 1--7
Distillation and titration analysis can be conducted after sample digestion is completed and
sample solution is cooled to indoor temperature. Process principles are as follows:
(NH4)2SO4+2NaOH= Na2SO4+2H2O+2NH3↑

That is, under alkaline condition, after separating ammonia with high-temperature steam,
collecting ammonia and steam mixture in titration cup containing boric acid absorption liquid
(including mixed indicator), use Sulphur acid titration liquid to conduct titration analysis in
photometric titration system (see Figure 1—8)

Figure 1—8

II. DW-ATN-1100 series technology and performance index

Items DW-ATN-1100 DW-ATN-1100B


DW-ATN-1100A
Analysis range 0.1—200 mg N
Precision (RSD) ≤0.5% (30mgN,0.1mol/L H+)
Titration accuracy 0.5μL/ procedure
Recycle rate 99.5%;±0.5%
Titrating solution concentration 0.1--5mol/L
Added volume of absorption liquid 0—50mL
Added volume of diluent 0—50mL
Added volume of alkali 0—99mL
Added volume of alkali during Provided:0-99mL/time (any setting value)
distillation
Total volume of titration cup ≈220mL
Total titration volume ≤80mL
Titration pump flow accuracy Yes: 5ml/time ±5‰
verification
Exposed titration cup (can be Yes
dismantled for cleaning)
Titration curve observation Yes
Data inquiry and printing Yes
Fertilizer analysis model (nitro) Yes: any setting within waiting time of 0-2 hours
Cooling water consumption 1.2L—3L/min
Sample analysis time (cooling
4-7min
water temperature 18℃)
Data storage capacity 720 days cyclic storage
Sample blank value deduction Automatically deduct
Titration cup overflow alarm Yes: Total volume≥210mm
system
Steam kettle over heated alarm Yes:120℃
system
Anti-dry device for steam kettle Yes
Items DW-ATN-11 DW-ATN-11 DW-ATN-1100B
00 00A

Steam system overpressure alarm None Yes:40kpa

Steam flow adjustment None Yes: 100% and 75%

Temperature monitoring alarm during


None Yes: 40℃
distilling sample

Automatic
Operating mode Automatic analysis/manual analysis
analysis

Safety alkali adding mode None Yes: any setting within range of 0—9999s

Automatic discharge of waste liquid in


None Yes
digestion tube
Titrating solution concentration
Manually Automatically/Manually calibrate
calibration method

Automatic cleaning of alkali solution None Yes (automatically wash when starting up)

Switch for instantaneous flow rate of


None Yes (0.5—6L/min)
cooling water
Intelligent cooling water system
None Yes
interface
Reagent barrel level display and alarm
None Yes (optional item)
system

Formula management None Yes (10 groups self-programming)

USB interface None Provided

Computer control software None None Yes: Under windows system

Group user’s management center None None Yes: 2-50 users

Internet interface None None Yes

Operating voltage AC110V/50Hz(60Hz)

Heating power 2000W

Appearance and size 500*460*710mm

Net weight 30Kg 36Kg


Chapter II: Instrument structure and installation
I. Instrument structure
DW-ATN-1100 series product consists of computer control system, screen operating system, steam
system, and photometric titration system

Front structure (see Figure 2—1) Back structure (see Figure 2—2)

Code Name Code Name Code Name Code Name


Water Cooling Power supply
A Color touch screen I a i
receiver fan socket
Digestion Cooling water
B Printer J b Back cover j
tube tray inlet
Waste
Digestion Product
C Power switch K c liquid k
tube nameplate
discharge
Steam
kettle Boric acid Earth leakage
D Titration pump L d I
viewing inlet protection
window
Liquid feeding
Alkali Multi-function
E pipes A, B and C for M Safety door e m
liquid inlet connection
titration system
Distilling Distilled
F Titration cup N f n 485 connection
head water
Ammonia
Network
G Front door O gas g AC110V o
connection
separator
Cooling
USB
H Titration system h water p
connection
outlet

Figure 2--1 Figure 2--2


II. Instrument installation:
1、Put azotometer on operating floor
 Hint 1, Cooling water “inlet and outlet” pipes provided for the products are 5m in length/each,
and if operating floor is relatively far from the liquid inlet, it is important to make sure the
safety and reliability of the selection of other pipes or
modification of the provided pipelines.
 Hint 2, “Reagent delivering pipe” of the product is test and
provided according to length of 3m, If user makes reagent
barrel stay away from operating floor, the maximum distance
shall not be more than 5m, or else, delivering speed and
accuracy will be affected.
Figure 2—3
2、Insert “cooling water outlet pipe” (the end with connector) into
“cooling water outlet” on back of instrument (see Figure 2-2,2-3),
and put the other end into water tank or drain.
3、Place “cooling water inlet pipe sealing gasket” into the “cooling
water inlet pipe” end with thread. (see Figure 2-4)
4、Screw above thread end into "cooling water inlet" on back of
instrument (see Figure 2-5)
 Hint! Thread end must be screwed tightly to prevent leakage
or blowout caused by too high water pressure Figure 2—4
5、Take out “adapter” of “cooling water inlet pipe” , and fasten
“adapter” with equipped screws (4) to water tap (see Figure 2—6)
 Hint! The “adapter” tightening shall be conducted with four
screws according to corresponding to prevent “adapter”
inclining to one side tightly. In addition: during screwing bolts
tightly, use the other hand to hold upwards “adapter” tightly
(see Figure 2—6)to make “adapter” closely contact with tap to
Figure 2—5
prevent leakage, screw 4 bolts tightly to prevent spraying
caused by “adapter” falling off
6、Insert “cooling water inlet pipe” with hooped tap into “adapter”
(see Figure 2—7)
 Pressure test——in case of no errors after checking, first, open
tap to the position with small angle to observe whether there
is water leakage in connection if there is no water leakage,
open tap to position with large angle properly and observe
connection, and it is ready to use if there is no water leak. Figure 2—6
7、Insert “reagent delivering pipe” based on corresponding color
into input port on back of instrument (see Figure 2-8,2-9)
8、Then put the other end of “reagent delivering pipe” according to color corresponding to reagent
barrel into port of “reagent barrel” (4 ports in total) (see Figure 2—10)
Figure 2—7 Figure 2—8 Figure 2—9

 Users selecting reagent barrel level display and alarm system insert reagent barrel level
sensor into “multifunction interface” (Figure 1—9, Figure2-2) (Optional)
9、Add reagent and distilled water into reagent barrel (see Chapter IX Reagent Preparation Method)
10、Put water receiver into instrument sample chamber and (see
Figure 2—11) close safety door
11、Insert power wire into “power socket” on back of instrument (see
Figure 2—12), and then insert another end into outlet.
12、Check(Figure 2-1-C) “power switch” shall be at “turn off ”state,
turn on “leakage protector” switch upwards (see Figure 2-13),
13、Put titration bottle which contain titrating solution into instrument
and insert right end of pump pipe into hole at upper end of the
bottle (see Figure 2—14) Figure 2—10
14、Close the instrument’s door, installation complete.

Figure 2—11

Figure 2—12 Figure 2-13

Figure 2—14
Chapter III, Instrument initiate adjustment
I. Startup:
1. Close safety door after confirming the digestion tube in sample chamber is at designated position
(see Figure 3—5)
2. Open power switch (see Figure3-6)
a) After turned on, enter self-check program (spend about 3 minutes)
 Working process after DW-ATN-1100A/B starts up——discharge of residual liquid in
digestion tube—→ discharge of distilled water in steam kettle—→discharge of residual
liquid in titration cup—→ water adding in steam kettle—→heating—→ standby
 Working process after DW-ATN-1100 starts up——discharge of distilled water in steam
kettle—→ discharge of residual liquid in titration cup—→ water adding in steam
kettle—→heating—→ standby
b) Startup page display after completing self-check shows below. (see Figure3-1)
3. Click (Figure3-1) center of the clock, an dialog window will appears on page (see Figure3-2)

Figure 3-1 Figure 3-2

Figure 3-3 Figure 3-4 Figure 3—5


4. Click “user name” a window pops up, select user number from 1 to 6, and then click “confirm”
5. Click “password”, a window pops up (see Figure 3—3), and input password and then click
“confirm”(see Page 17 for details of passwords)
6. Click “confirm” (Figure 3—2) button and enter “system home
page”, see (Figre 3-4)
II. Reagent pump flow calibration:
1、 Appliances used for flow calibration
A. Analytical balance: precision: 0.0001g; weight: ≥120g.
B. Two to five 50ml beakers: After cleaning put into drying oven
Figure 3—6
with temperature of 110℃ for 2 hours and take them out for
use.
C. One 50ml measuring cylinder: used for reagent pump flow.
D. One pair of protective gloves. (used for taking digestion tube during analysis)
2、 Flow calibration point:
A. Titration system——A, B and C pipelines arranged in “titration cup cap ”in right door of
instrument(see Figure 3—7), including
 A pipe: boric acid absorption liquid pipe (need calibration if it is used for the first time)
 B pipe: cleaning pipe (needs NO calibration)
 C pipe: titrating solution pipe (calibrate when needed)
B. Alkali solution pump——left door of instrument is equipped with the
pump; the pump is at right side of steam pipe. (see Figure 3—9)
C. Diluent pump——left door of instrument is equipped with the pump;
the pump is at right side of steam pipe. (see Figure3—9)
3、 Alkali solution pump flow calibration (volumetric method)
Figure 3—7
A. Wear protective gloves.
B. Click “flow calibration” button (Figure 3—4) and enter “flow calibration
page”. (see Figure 3—11)
C. Open sample chamber door, use left hand to press digestion tube tray
downwards, and use right hand to take the pipe from tray. (see Figure
3—8)
D. Hold 50ml beaker and put it under alkali liquid outlet. (as shown in
Figure 3—9)
E. Press “lift” button below “alkali solution pump” (Figure 3—11) to make
pipe filled with solution (it flows out continuously) and then stop Figure 3—8
pressing.
F. Click “calibration” under “alkali solution pump” column (Figure 3—11)
“put into container” dialog window pops up. (Figure 3-12)
G. Hold 50ml measuring cylinder and put it under “alkali solution” outlet.
(Figure 3-9)
H. Click “confirm” button (Figure 3—12) and “alkali solution pump” begins
calibration.
I. Record liquid volume in measuring cylinder and conduct next Figure 3—9
calibration.
J. Conduct three times calibration in total and record volume (ml) of the
liquid.
K. Click data frame under “alkali solution pump” (Figure 3—11),
L. Pop up “data input box” (see Figure 3—13)
M. And then input data of three times recoded in “data input box”
successively, and system will generate and record “calibration value”
of these times.
N. Alkali solution pump flow calibration is completed Figure 3—10
4、 Diluent pump flow calibration
A. Calibration position is the same as the “alkali solution pump”.
B. Calibration method is the same as the calibration procedures of “alkali solution pump”.
5、 Boric acid pump flow calibration
A. Calibration position (see “B” pipe in Figure 3—7).
B. Calibration method is the same as of calibration procedures of “alkali solution pump”
6、 Titration pump flow calibration (gravimetric method):
A. Take one 50ml dry beaker with constant weight, weigh and record its weight (see Figure 3—14)
B. Click “calibration” under “alkali solution pump” column (Figure
3—11) “put into container” dialog window pops up. (Figure
3-12)
C. Take out Pipe “c” (Figure3-7) put it into beaker (Figure 3-10) and
then click “confirm”, calibration begins.
D. After titration pump completes works, take beaker, weigh it and
Figure 3—11
record “net weight” value. (see Figure 3—14)
E. Repeat above “calibration” procedures two more times and
record these value for use.
F. Click data frame under “titration pump flow calibration”, data
input box pops out (see Figure 3—13), and then input data
(XXg) recorded into above frame successively, the system will
automatically generate and record "calibration value" of these
Figure 3—12
times.
G. Calibration is completed
7、 Titration pump “Titration volume verification” (1
5.0000g/time ±5‰)
A. Take one 50ml dry beaker with constant weight, weigh and
record its weight;
B. Put left end of burette into beaker (as shown in Figure3—10), Figure 3—13
click “titration volume verification 15.0000g” button (Figure
3-11), and then titration pump starts working, after the pump
stops working, weigh liquid and beaker, deduct tare weight of
beaker from total weight, and liquid weight is qualified if such
value is 15.0000g±5‰
C. Insert pipe into “C”(Figure 3—7)again and then verification is
completed
III. Titration solution change.
When use different concentration titration solution need to clean up
the titration pump to prevent the error.
Figure 3—14
1. Prepare one 500ml beaker.
2. Enter calibration page (Figure 3-11)
3. Take out burette put into beaker (Figure 3-10)
4. Click titration solution change button (Figure 3-11)

5. Pump change solution twice (if change from high concentration to low concentration, it is
recommended to go through procedure twice)
6. After solution changed. Insert burette back into (Figure 3-7-c)
IV. System setting:
"System setting" is necessary to guarantee the normal operation of equipment, before
conducting sample analysis, confirmation shall be conducted
for the setting parameter to avoid analysis data error caused
by wrong parameter setting.
1. DW-ATN-1100 system setting(See Figure 3—15)
A. Absorption liquid—— Refers to setting of added volumes of
absorption liquid (boric acid) in titration cup automatic
Figure 3—15
analysis.
B. Alkali liquid——Refers to setting of added volumes of alkali liquid in digestion tube during
automatic analysis
C. Diluent——Refers to setting of added volumes of diluent in digestion tube during automatic
analysis. Note: before adding alkali liquid, add “diluents” (distilled water) properly to reduce
sharp reaction between alkali and acid
D. Distillation waiting time——It means that during automatic analysis, and after adding alkali
solution, “heating and distillation” shall not be conducted immediately until “the setting time”
ends. It is mainly used for analysis for partial samples containing nitrate nitrogen (It takes certain
reaction time after adding Nitrogen fixing alloy)
Hint! If instrument cannot heat at normal working state, such phenomena are related to the
setting.
E. Stand-by time——the instrument can heat automatically when it starts up, and the temperature
will keep “constant” within set “stand-by time”. If no persons operate under condition of
exceeding set time, heating system will not keep “constant” and will enter dormant state for
energy conservation. In case of operating system again, the system automatically enters heating
and constant temperature state
F. Standby temperature——Refers to temperature maintained “in distillatory kettle” within above
standby time and displayed at top right corner,
Hint! Set value of “standby temperature” shall not be too high, and
maximum temperature shall not be more than 70℃.
G. Safety alkali solution adding mode time——Refers to a kind of
relatively safe alkali solution adding mode. In order to prevent
sharp and strong reaction between acid and alkali, first, conduct
Figure 3—16
heating for sample containing acid properly, and then add alkali
solution after temperature of above sample rises to reduce
reaction degree properly. "Safety mode time" refers to suitable
"heating time" for sample.
Hint! “Heating time” shall not be too long, and shall be suitable
for making sample be at “almost boiling” state to prevent acid mist
generating after boiling.
Figure 3—17
H. Titrating solution concentration input value——Titrating solution
H+ concentration value input.
I. Titrating cup cleaning time——Refers to setting of times during

Figure 3—18
the process of using distilled water to wash away residual liquid in titrating cup.
2、 ATN-1100A/B system setting (see Figure 3—16)
 Other settings are the same as those of DW-ATN-1100 (see Figure 3—15), newly-added
setting is simply described as follows
A. Cooling water flow switch——Turn on switch and monitor, the system displays cooling water
flow state, and if flow is less than 0.6L/min, the system will send alarm and shut down
 Attention! If cooling water flow is not stable, turn off flow switch to prevent system sending
alarm and shutting down due to unstable flow.
B. Cumulative cooling water flow——Accumulative statistics of total cooling water consumption
(cubic meter).
C. Digestion tube waste liquid discharging time——Refers to setting of time of digestion tube
waste liquid discharging after completing analysis.
D. Steam flow selection:
 High flow—— Steam flow reaches to maximum value during distillation and quantity of
steam counts for 100%
 Middle flow—— Steam flow is reduced during distillation, and quantity of steam accounts
for 75%
E. Automatic alkali solution adding—— When function on, before distillation processes end, add
3ml alkali solution again to help blow out the sample attached on the tube.
F. Simultaneously distillation and titration—— When function on, when distillation sample around
70ml, titration processes automatic start and shutdown when titration finish.
Attention: Before use this mode, please make sure it match your analysis methods.
3. Formula management—— User can set 10 groups of different formulas by different analysis con
dition with their own preference, to provide convinces for future operation.
 Setting and storage method——Click “formula management” button (Figure 3—4) and
enter (Figure 3—17.
 Click “formula number” (Figure 3—17) and dialog box pop out. (Figure 3-18)
 Select number (see Figure 3-8) in the dialog box, for example: “2”.
 Input conditions as needed successively (see Figure 3—18), such as:
 Absorption liquid——25ml
 Alkali liquid——50ml
 Diluent——10ml
 Distillation waiting time——0min
 Digestion tube waste liquid discharging time——15s
 Alkali adding mode——common
 Steam flow——75%
 Click “return” button and complete setting and storage

 Other “number” settings are the same as above method


4. Operator's startup number and corresponding password
A. Operator No. and password
Operator No. Password
1 111
2 222
3 333
4 444
5 555
6 666

Chapter IV. DW-ATN-1100 series data inquiry and print


I. Data inquiry and printing
1、 Click “data inquiry” in Figure 3—4 and enter inquiry page (see
Figure 4—1)
2、 Select date from box.
3、 Clicking “Enter” button in Figure 4—1, you can inquire analysis
results of date selected (data)
5. After data inquiry results are displayed (see Figure 4—2)
6. Click “Print” button in Figure 4—2 Figure 4—1
7. Printer begins to print data
II. Printer:
1、 Printer structure(see Figure 4—3)
A. Power indicator light and feed button
B. Paper outlet
C. Cover
D. Open and lock cover Figure 4—2
2、 Replace printing paper
A. Lift up lower end of cover lock “D” and pull out slightly, and
then open cover “C”
B. Take out printing paper roll and put it on paper core
C. Put printing paper back
D. Close cover “C”
 Hint! Printing paper roll must be put in roll slot and printing
paper shall be put in the middle of paper outlet “B” Figure 4-3
E. After closing cover “C” and pressing feed button “A”, observe whether feeding is normal
F. Printing paper replacement is completed
Chapter V. DW-ATN-1100 series azotometer operating method

Overview: After completing installation and setting according to above procedures, the
instrument has obtained basic conditions of sample analysis, in
consideration of relatively large difference among sample treatment
and analysis methods of different industries, so the operating method
is only used as interpretation for procedures concerning way of the
instrument to complete sample analysis
I. Automatic analysis operating button and window
Figure 5—1
interpretation:
1、 DW-ATN-1100 operating system
A. Enter "automatic analysis" page
a) Click “automatic analysis” on “system home page” in Figure
5-1
b) Enter “alkali adding mode selection” page (see Figure 5—2)
c) Select “safety” mode
Figure 5—2
(Before adding alkali solution into samples, first heat
samples, and the heating time needs to be set in “safety
mode time” on “system setting” page. So, confirm that
“safety mode time” has been set before selecting “safety
mode”. Note! "Safety mode time" shall be set to be suitable
for making samples be at almost boiling state to prevent
acid mist pollution generating after boiling) Figure 5-3
d) Or select “common” mode
e) Enter "automatic analysis” page (see Figure 5—3)
B. Automatic analysis page window, button function
interpretation (see Figure 5—3)
 Samples “analysis results” display area is at left side of the
page.The system state display and operating
 button are at right side of the page Figure 5—4
a) Distilled water level——Indicates water level state in steam kettle
b) Steam temperature——Indicates temperature in steam kettle, and alarm will be sent and
shutdown will be caused in case of over temperature
c) Alkali solution adding mode—— Indicates alkali solution adding mode selected
d) Mode time—— Indicates set time of safety mode
e) Absorption liquid—— Indicates added volume of absorption liquid
f) Diluent—— Indicates added quantity of digestion solutions
g) Alkali solution—— Indicates added volume of alkali solution
h) Titrating solution concentration—— Indicates H+ concentration of titrating solution used
i) Blank value input window—— Sample blank value input window
 Click and dialog box (see Figure 5—4) pop up, input data and confirm
j) Exit button—— exit from the page after clicking
k) Sample data button——Click it and enter sample data input page (see Figure 5—5)
 Sample number window——Users can number within 3 digits according to needs, or
else, the system will take current number as default value, but automatic analysis
results will not be affected (see Figure 5—6)
l) Sample weight window——The final
 display results (nitrogen content) on “automatic
analysis” page will be affected without the data input,
but titration volume will not be affected. If users have
forgotten to fill in, results can be obtained through
manual calculation according to titration volume and
sample weight recorded (see Figure 5—6)
m) Curve observation button——Click and enter page Figure 5—5
displaying sample titration process real-time curve in( Fi
gure 5—7) used for analyzing sample working state
 Too steep (vertical) curve indicates that titrating
solution concentration value is too high. Results: big
error
 Straight (skew line) curve indicates that titrating
solution concentration value is too low. Results: no Figure 5—6
end point
n) Titration cup cleaning button——After clicking, spraying
and cleaning are conducted for titration cup, and after
that, waste liquid discharges automatically
o) Additional alkali adding button——If quantity of alkali
solution added is not enough during system operation,
such adding can be conducted many times by pressing
the button Figure 5—7
 Dialog pop ups after clicking (see Figure 5—8), and
then input added quantity of alkali solution and then
click “confirm” to begin adding
p) Operation button/stop button——Analysis system
startup/stop button
 Dialog box pops up after clicking (see Figure 5—9),
Figure 5—8
and analysis system operation begins after clicking
“confirm”
 System will stop operating after user confirm the
“stop” dialog. \
2、 DW-ATN-1100A/B operating system
Basic operating method of DW-ATN-1100A/B is the same as of
DW-ATN-1100, this part only provides description of
Figure 5—9
newly-added contents and functions (see Figure 5—10)
 Enter “automatic analysis” page
a) Click “automatic analysis” on “system home page” in Figure 5-10
b) Enter “digestion tube waste liquid discharging” page (see Figure 5—11)
Hint! Confirm that sample particle size is more than or eq
c) ual to 60 mesh before selecting “automatic discharging”
to prevent pipe blocking caused by too large particle
c) Select “automatic discharging” and enter “alkali solution
adding mode selection” page (see Figure 5—12)
d) Select “common” mode and enter automatic analysis
page (see Figure 5—13)
 Automatic analysis page window and button function Figure 5—10

interpretation (see Figure 5—13)


a) formula selection——There are ten groups of working
parameters set by
b) users for calling during analysis
c) click (figure 5-- 13) "formula selection" key to enter (figure
5-- 14) page, select the required recipe number, click
Figure 5—11
"Load" to enter, and click "Ouit" to returCooling water
flow display——It displays cooling water flow during
distillation
d) Steam flow display——It displays steam flow state of
100% or 75%
e) Digestion tube waste liquid discharge state display——It
displays whether waste liquid in digestion tube is at Figure 5—12
automatic discharging state
f) Other parameters display——During operation, click
curve observation and enter(Figure 5—7)
 Steam temperature—— Displays steam system
temperature, and the system will send alarm and shut
down in case of too high temperature
Figure 5—13
g) Steam pressure—— Displays steam system pressure, and
the system will send alarm and shut down in case of too
h igh pressure.
h) Temperature for distilling sample—— Indicate
temperature of distilled water generated from samples
cooling displays. System will send alarm and shut down
in case of unsatisfactory cooling effects.
Figure 5—14
i) Cooling water flow—— Displays condition of cooling
water flow, the system will send alarm and shut down in case of insufficient cooling water
flow.

j) Titration curve observation —— Curve observation and printing during titration process.
II. "Automatic analysis" operating method:
Now “automatic analysis” operation is expainl according to DW-ATN-1100A full-auto
Kjeldahl azotometer
1. Reagent, distilled water barrel, reagent of titration bottle
2. Water tap is at open position
3. See relevant parameters on “system setting page” according to sample conditions,
4. For example: Chose pre-set formula # “2”
5. Place sample at designated position and close safety door
6. Enter “system home page”
7. Select “automatic analysis”
8. Select “automatic discharging” in “digestion tube waste liquid discharging mode selection”
9. Select “common” in “alkali solution adding mode”
10. Enter "automatic analysis” page (see Figure 5—13)
A. Click “formula selecting” pull-down menu, select # “2” formula (see Figure 5—14)
B. Input “0” in “blank input”
C. Click “sample data” and enter “sample data input” page
a) Input sample number, for example:101
b) Input sample weight, for example:0.1234g
D. Click “return” button to return “automatic analysis” page
E. Click “operation” button and “Yes” to confirm
a) Add boric acid in titration cup
b) Motor operates to stir acid in the cup
c) Add diluent in digestion tube
d) Add alkali solution in digestion tube
e) Distillation system works and temperature of steam kettle begins to rise
f) Cooling water valve automatically opens after rising to 65℃, tap water flows in for
cooling
g) After rising to 100℃, a large amount of steam containing samples is changed into
distilled water containing samples flowing into titration cup
h) If volume of titration cup reaches to value as required (about 110ml),distillation system
stops working
i)Cooling water valve automatically closes
j)Distillation system automatically begins working (photometric lamp lights)
k) After reaching to titration end point (liquid in the cup becomes red), distillation system
automatically stops working
l)Waste liquid in digestion tube discharges
m) Waste liquid in titration cup discharges
n) Digestion tube and titration cup cleaning begins
o) Waste liquid (after washing) in digestion tube discharges
p) Waste liquid (after washing) in titration cup discharges

q) Analysis data is calculated, stored and displayed on "automatic analysis" page


F.The analysis of this time is completed.
III. Manual analysis: (DW-ATN-1100A/B)
1、 Overview:
Manual analysis is designed for individual and
research-based users, and its analysis methods are in form of
working procedures that are independently completed and
not connected with each other so that users can complete Figure 5—15
corresponding analysis units according to actual condition, for
example: distillation time can be set again if they think
distillation volume is insufficient until they are satisfied and
then they can implement next procedure. So, relevant
parameters in “system setting” doesn't work in this condition
and need to be input on “sample input” page separately (see
Figure 5—15)
Figure 5—16
2、 Operating method:
A. Enter “automatic analysis” page (see Figure 5—16)
B. Input “blank” value
C. Enter “sample data” page
a) Input data (see Figure 5—16)
 Input method is same as the “automatic analysis”
b) Conditions setting:(see Figure 5—16)
 Added volume of each reagent (Unit: mL)
 Distillation time shall be counted in Sec
D. Return to “manual analysis” page
E. Click “reagent adding” to add reagent, and add reagent again if added volume is not
enough
F. After clicking “distillation”, distillation system begins working, click again if volume is not
enough after distillation
G. After clicking “titration”, titration system works
H. After reaching to titration end point, titration system stops working
 End point judgment method is the same as that of “automatic analysis”, and titration
cannot be conducted again
I. After clicking “waste liquid discharging”, waste liquid in titration cup discharges
J. Analysis results are displayed at left side of "manual analysis"(see Figure 5—15)
K. Analysis completed.
Chapter VI. Automatic calibration of "titrating solution concentration value"
(DW-ATN-1100A/B)
I. Preparation before calibration
1. Put 3 digestion tubes after cleaning then put into drying oven
with temperature of 110℃ for 2 hours and take them out for
use
2. Ammonium di-hydrogen phosphate (Gr)—— Take appropriate
amount of ammonium dihydrogen phosphate and put it in
drying oven with temperature of 105 ℃ for drying, after 4 Figure 6—1

hours, its weight is constant, take it out and put into dry
container for cooling to indoor temperature for use
3. Titrating solution preparation—— it is conducted according to
concentration about 0.1000 mol/L, see Chapter IX Reagent
Preparation
 After completing titration solution preparation, put such Figure 6-2
solution into Titration bottle and then put the bottle into
instrument (see Figure 2—14)
4. Weighting three “ammonium dihydrogen phosphate” samples
accurately (e.g.:0.1010g,0.1020g ,0.1030g), put them into
three clean digestion tubes respectively and mark these tubes
with 1#, 2#, 3# for use Figure 6—3
II. Instrument pre-heating operation
1. Take small amount of “ammonium dihydrogen phosphate”
sample (about 0.1 g ) and put it into digestion tube provided
for instrument
2. Click “flow calibration” (see Figure 6-1) and enter “flow
calibration page” (see Figure 6—2)
Figure 6—4
3. Click “next page” (Figure 6—2) and enter “confirmation of
effective components of reagent” page (see Figure 6—3)
4. After clicking “coefficient” window, data input box pops up
(see Figure 6—4)
 Coefficient value :0.0000——1.000
5. Input effective components of reagent, such as 0.995, and
confirm (see Figure 6—4) Figure 6—5
6. Click “confirm” (Figure6—4) and enter “concentration
calibration” page (Figure 6-5)
 “Titration concentration calibration” page window contents
interpretation
 Sample weight input window—— accurately input
sample weight (3 values in total)
Figure 6—6
 Titrating solution volume display window—— Display
volume consumed in this titration (3 values in total)
7. After clicking “operate”, “calibration confirmation” dialog pops up (see Figure 6—6)
8. Click “confirm”
9. Instrument preheating begins
10. Processes automatically stopping (Note: pre-heating operation of this time is not involved in
calculation, so “titration flow volume” is not displayed)
III. Liquid concentration calibration
1. Remove digestion tube for pre-heating
2. Put 1# digestion tube into instrument and close safety door
3. After clicking “operate” (Figure 6—6), “calibration
confirmation” dialog pops up(see Figure 6-6)
4. After clicking “confirm”, calibration begins
Figure 6—7
5. 1# digestion tube operates continuously before automatically
stopping
 “Titration volume display” will display titrating solution volume consumed by sample in 1#
digestion tube (for reference)
6. Click “the first time” “sample weight input” window (Figure 6—7)
7. Digital input dialog pops up (see Figure 6—7)
8. Input weight of 0.1010g of sample in 1# digestion tube and confirm
9. 1# tube calibration is completed
10. Calibration method of 2# and 3# digestion tubes is the same as 1# tube
11. Repeat calibration for 2# and 3# digestion tubes
12. After completing calibration for these three tubes, system calculate and stores average value of
three “calibration value”, and display in “calibration value” window.
 Hint! “calibration value" in the window and “titrating solution concentration input value” on
"system setting" page are connected, so "value" update in the window and "value" update on
"system setting" page happen at the same time. Similarly, "value" update on "system setting"
page and "value" update in this window happen at the same time
13. Calibration is completed

Chapter VII. Safety protection system

I. Electric leakage protection:


1、 When leakage protection switch is turned on, operator safety can be guaranteed after system
disconnects power supply in case of electric leakage of the whole electrical system
2. To ensure that leakage protection system maintain in the good condition, it is suggested that
users should conduct testing regularly, the method is as follows:
A. Turn on leakage protection switch (see Figure 2—13)
B. Press leakage test button
C. Now, if switch automatically goes back to “turn-off” position, then electric leakage protection
function is normal
II. Steam generator water shortage protection and alarm system
 The protection system consists of CPU, liquid level switch, alarm device, actuator.
In case of water shortage in steam generator or fault in water charging system, heating system
will stop heating and send alarm to prevent damage caused by operation of heating elements
lack of water shortage
III. Titration cup water level over-limit protection and alarm system
 The protection system consists of CPU, liquid level switch, alarm device, actuator . When level in
titration cup reaches to level limit, the system will stop titration and send alarm to prevent
damage caused to machine by liquid overflow
IV. Steam overpressure, overheated protection and alarm system
 The system consists of CPU, pressure sensor, temperature sensor, alarm system, and actuator. If
pressure and temperature of steam circuit system is too high in case of faults of steam
generator, steam circuit valve, steam circuit pipe, the system will stop heating and send alarm to
prevent damage or losses to personnel and property
V. Digestion tube absence protection and prompt system
 In order to prevent alkali solution, distilled water, steam leakage caused by absence of digestion
tube, if digestion tube is not installed, solution adding and distillation procedures cannot be
implemented, and "no digestion tube installed" prompt will appear on screen
VI. (Device) procedures for preventing over-reaction between strong acid and alkali
 If there is some strong acid solution in digestion tube before adding reagent, and at this time
strong alkali solution is added, strong overheating reaction and splashing will happen. So, for the
procedure, strong alkali solution is added according to certain interval, and suitable volume of
distilled water can be added before adding strong alkali solution to prevent damage caused by
overheating reaction
VII. Safety door protection
 To ensure operator safety and prevent accidents during operation, system stops working when
safety door is opened

Chapter VIII. Matters needing attention, maintenance and common


faults
I. Attention:
1、 Before using, check whether liquid in distilled water and reagent barrels is sufficient
2、 Open cooling water input before using instrument
3、 Close cooling water input after end of use of instrument
4、 During using, digestion tube must be installed at designated position (digestion tube aligns to
rubber plug) to prevent recovery rate decrease and instrument damage caused by steam leakage
5、 After completing distillation, if temperature of digestion tube is high, please wear gloves to
operate to prevent getting burned
6、 Viscosity of alkali solution under condition of long-term storage and environmental temperature
change will result in incorrect alkali solution flow, please replace alkali solution or conduct flow
calibration regularly to prevent insufficient alkali solution added
7、 To prevent waste liquid overflowing, please observe level change in waste liquid barrel regularly
II. Maintenance:
To prolong service life of instrument and guarantee stable operation of instrument, it is
suggested that users should conduct maintenance regularly to obtain correct analysis data. ( N
ote!!! During scrubbing and cleaning, please do not use cleaning fluid containing organic
solvent)

1、 Maintenance items and cycle list:


Maintenance contents Each Each Each
day week month
Steam flushing for system √
Alkali solution pipeline √
cleaning (DW-ATN-1100A/B)
Alkali solution pipeline √
cleaning (DW-ATN-1100)
Distilling head cleaning √
Sample chamber cleaning √
Water receiver cleaning √
Overspill eliminating
Reagent barrel cleaning √
Titration cup cleaning √
2、 Steam flushing for system:
A. Set “alkali solution” as “0mL”, and set “diluent” as 25mL
B. Enter “automatic analysis” page
C. Open “safety door” and put one empty digestion tube
D. Press “operate” button to conduct automatic distillation
E. Conduct “forced shutdown” after completing distillation
F. Take out digestion tube and empty it, and “automatic
discharging” can be selected
G. Operate 2 times
3、 Alkali pipeline cleaning: pipe blocking can be easily
caused by crystallization in alkali solution stored for long time,
please conduct cleaning for pipe line regularly
A. DW-ATN-1100A/DW-ATN-1100B cleaning method Figure8--1

a) Click "pipeline cleaning" button (Figure 8—1)


b) System automatically conducts cleaning and discharges waste
liquid procedures,
c) Run cleaning procedures of two times
d) If solution flow is small, user can use distilled water with
temperature around 50 ℃ to replace distilled water in
Figure8--2
reagent barrel (see Figure 8—3)
B. DW-ATN-1100 cleaning methods:
a) Enter “flow calibration” page (see Figure 8—1, Figure 8--2)
b) Remove connector of “alkali reagent barrel” (see Figure 8—3)
c) Use 1000mL beaker to add distilled water with temperature about 50℃
d) Put alkali solution pipe into “distilled water” in beaker
e) Press alkali pump “lift” button (see Figure 8—2)
f) Use distilled water to wash alkali solution pipeline system
g) Remove digestion tube and empty it (see Figure 8—8)
h) Repeated cleaning procedure 2 times
4、 Distilling head cleaning:
A. Open safety door and take out digestion tube (see
Figure 8—8)
B. Use wet cloth to remove reagent and dirty mark on
distilling head(see Figure 8—9)
5、 Sample chamber and water receiver cleaning:
A. Take out digestion tube (see Figure 8—8) Figure 8-3 Figure 8-4
B. Sample chamber cleaning (see Figure 8—9)
C. Water receiver cleaning (see Figure 8—10)
6、 Overspill eliminating:
A. Use “titration cup cleaning method” to eliminating
overspill from titration cup
B. Cleaning overspill regularly to prevent analysis
results being affected by overspill
7、 Distilling head cleaning: Figure 8-5 Figure 8-6
A. Set “alkali solution” as “0” ml, and set “diluent” as 25mL
B. Add 25ml glacial acetic acid in the digestion tube
C. Install tube in instrument and operate
D. Conduct “forced shutdown” after completing distillation
E. Take one empty digestion tube and install it in instrument and operate
instrument again
F. Conduct “forced shutdown” after completing distillation Figure 8-7
G. Cleaning completed
8、 Reagent barrel cleaning:
A. Take out reagent in reagent barrel
B. Add 1000mL warm water with
temperature about 50℃ in
barrel and close lid
C. Shake reagent barrel to make
reagent in barrel dissolve
D. Pour out waste liquid
E. Use 50℃ warm water flush
Figure 8—8 Figure 8—9 Figure 8--10
alkali tube several times and wipe it dry

9、 Titration cup cleaning method


a. Unscrew two battens at upper part and lower part of titration cup respectively (see Figure
8-4)
b. Unscrew 3 bolts on cap of titration cup (see Figure 8—5 )
c. Pull out plug of “titration cup cap” and take out titration cup cap (see Figure 8—6)
d. Take out titration cup (see Figure 8—7 )
e. Cleaning titration cup
f. Install the cup in reverse order of above procedure after cleaning

III、Common faults and treatment methods


Common faults Fault phenomena Reason Treatment methods
1. Water shortage in 1. No water in distilled water 1. Add water
Instrument sends steam generator barrel 2.Report repair
alarm after startup 2. Too high pressure in 2. Steam system stuck 3. Discharge solution or
and cannot be steam circuit system 3. Titration cup water level report repair
operated 3. Water in titration cup too high
overflows
Steam exudes from 1. Steam exudes from 1. Cooling water source is not 1.Open cooling water source
instrument instrument opened 2. Report repair
2. Leakage appears in steam
system
Solution flow titrating Different from flow Environment temperature Calibrate again and replace
incorrect initially calibrated difference is large and pump pump pipe
pipe aging
1. No effective components in 1. Normal. Titration doesn't
1. No titration is sample need to be conducted for
Abnormity appears conducted after 2. Titrating solution the sample
during titration completing distillation concentration value 2. Select titrating solution
process 2. No end points during selected is incorrect (too again; prepare absorption
titration process small); preparation of liquid again
3. Completion of titration absorption liquid is 3. Select titrating solution
process in advance improper (too shallow again; check titration cup
color)
3.Titrating solution
concentration value
selected is incorrect (too
large); impurity exist in
titration cup
Chapter IX. Reagent preparation reference
Level of reagent used is required to be more than analytically pure
level, all reagents shall be prepared with deionized water or distilled water.
In case of additional requirements during use, please prepare and use

according to these requirements. This preparation method is only used


for reference
I. Reagent:
A. Ammonium sulfate((NH4)2SO4)
B. Sulfuric acid (H2SO4)
C. Boric acid (H3BO3)
D. Sodium hydroxide (NaOH);
E. Anhydrous sodium carbonate (Na2CO3,reference level)
Figure 9—3
F. Methyl red indicator (C15H15N3O2)
G. Bromocresol green indicator (C21H14Br4O5S)
H. Industrial alcohol (C2H5OH)
I. Deionized water or distilled water(H2O)
II.. Preparation equipment
A. Electronic heated drying oven
B. Electronic analytical balance:0.1 mg
C. Electronic balance: 500g/0.1g
D. Volumetric glass: A level
III. Preparation works:
Figure 9—1
A. Take appropriate amount of ammonium sulfate and put it in
drying oven with temperature of 105 ℃ for drying, after 4
hours, its weight is constant, take it out and put into dry
container cooling to indoor temperature for use
B. Put primary anhydrous sodium carbonate in drying oven with
temperature of 270-300℃ drying 4 hours for use
IV. Reagent preparation:
A. Sodium hydroxide solution (400 g/L)
 Weigh400.00 g sodium hydroxide
(see Figure 9—1), use deionized water to dissolve and dilute it
to 1000 mL , shake solution uniformly for use (see Figure 9—2) Figure 9—2
B. Standard ammonium sulfate solution:
 A solution(140 mgN/10 mL): use analytical balance to weigh 6.6065g, and then use
deionized water to dissolve and dilute in 100ml, and shake the solution uniformly for use
 B solution(14 mgN/10 mL): take 10ml A solution and then dilute it with deionized water in
100ml, and shake the solution uniformly for use
 C solution(1.4 mgN/10 mL): take 10ml B solution and then dilute it with deionized water in
100ml, and shake the solution uniformly for use
C. Mixture indicator:
 Methyl red ethanol solution (1 g/L): weigh 0.5g methyl red, make it dissolve in industrial
alcohol, and dilute to 150mL
 Bromocresol green ethanol solution (1 g/L) : weigh 1g bromocresol
green, make it dissolve in industrial alcohol, and dilute it to 150mL
 Mixture indicator fluid: mixing Methyl red ethanol solution (4.13) to
bromocresol green-ethanol solution (4.15) with 1:1 ratio
D. Standard sulfuric acid solution for
titration[c(1/2H2SO4)=0.1000 mol/L]:
 Take out 3 ml concentrated sulfuric acid, dilute it with deionized water
to 1000ml, shake the solution uniformly for calibration
E. Standard sulfuric acid solution[c(1/2H2SO4)=0.0500 mol/L]
calibration: (see Figure 9—4)
 Accurately weigh 0.1000g anhydrous sodium carbonate dried under
temperature of 270-300℃ for 4h, and put it in 250mL conical flask, add
50mL deionized water to dissolve, and then add 10 drops bromocresol
green—methyl red indicator, use sulfuric acid solution prepared to
conduct titration until green solution changes into dark red solution, Figure 9—4
and boil solution carefully for 2 min, cool it to indoor temperature. Continuously conduct
titration to make solution color changed into dark red from green. And at the same time,
conduct blank test
F. Concentration of standard sulfuric acid solution for titration shall be calculated
according to following formula (A.1):
c(1/2H2SO4) =m/(0.05299×V)……A.1:
c(1/2H2SO4) ──Amount-of-substance concentration of standard sulfuric acid solution for titration (
unit: mol/L)
m ── Weight of anhydrous sodium carbonate (unit: g)
V ──Actual volume of sulfuric acid solution used for titration (unit: mL)
0.05299──Weight of standard anhydrous sodium carbonate (unit: g) titration solution equivalent
to 1.00ml standard sulfuric acid solution for titration 〔c(1/2H2SO4) =1.000mol/L〕

Chapter X: Commonly used consumable materials


Order No. Product name Specification Figure

Φ42*300mm
A000123 Digestion tube
(340mL)

Φ50*300mm
A000123 Digestion tube large volume
(500mL)
A000454 Kjeldahl high 750g
efficiency
A000123 catalytic pill 250g

B100073 10- hole


B100072 15- hole
Digestion tube holder
B100058 20- hole

F000015 10- head


Exhaust gas
F000013 15- head
collecting
device
F000012 20 -head

Acid and alkali neutralization


F000017 equipment ZH-1A
(active)
Acid and alkali neutralization
F000016 equipment ZH-1B
(inactive)

A000128 Glass filter cup Size

Reagent barrel
A000246 5L
(made in US)

A000247 Reagent barrel (made in US) 10L

Reagent barrel (made in


A000491 25L
China)
Drawell International Technology Limited
Shanghai Drawell Scientific Instrument Co.,Ltd

Add :Suite 1506,Lane581 XiuChuan Rd.,PuDong New Area,Shanghai,China


Tel/ Fax: 0086 21 50966080
Web : www.drawell.com.cn
Email : [email protected]

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