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7 Quick start

►

32 Hitachi High-Tech Analytical Science

7.2

Flowcharts for analysis and recalibration

7.2.1

Start and sequence of a check measurement in spark mode

Start a check measurement

Set argon supply to 3–5 bar

Connect power supply

Switch on computer

Wait until WINDOWS™ has

completely started up

Switch on spectrometer

Start spectrometer software

Select "Analysis" and subprogram

Select "Analysis" menu item;

click "Argon purging" button;

purge for 1 minute, click button

again to complete purging

Check result

Recalibration: Select recalibration

method "Recalibrate Program" or

"Recalibrate Matrix"

Continue with "Analysing"

not OK

Measure Control Sample

(see software manual)

chapter 7.2.2, page 33
or
chapter 7.2.3, page 34

chapter 7.2.4, page 35

chapter 5.4, page 19

Содержание OE700 Series

Страница 1: ...Operating manual 10022080 Ver 1 0GB 2019 08 14 OE700 series ...

Страница 2: ...anual is copyrighted by Hitachi High Tech Analytical Science with all rights reserved No part of this manual may be reproduced transmitted or disclosed to a third party in any form or by any means without the express written permission of Hitachi High Tech Analytical Science 3 Hitachi High Tech Analytical Science assumes no liability for any direct indirect or consequential damages arising from us...

Страница 3: ...t that Hitachi High Tech Analytical Science does not assume responsibility for damage or losses resulting from the disregard of this operating manual or the misuse of the products described herein This operating manual is protected by copyright Our products are subject to continuous further development technical changes are reserved Uedem February 2019 ...

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Страница 5: ...ing controls 12 4 2 1 Spectrometer components 13 4 2 2 Operating controls displays and ports of the spectrometer 14 4 3 Technical data 15 5 Scope of delivery transport set up and installation 17 5 1 Scope of delivery 17 5 2 Transport 17 5 3 Set up 18 5 4 Installation 19 5 5 Establishing optical transparency 20 5 5 1 Disabling Windows updates 20 5 5 2 Establishing optical transparency 21 5 5 3 Test...

Страница 6: ...d adjusting the electrode 44 9 5 Replacing the ceramic insert in the spark stand 46 9 6 Replacing filters 47 9 7 Cleaning and filling washing bottles 47 9 8 Cleaning the instrument 48 9 9 Replacing the argon bottle s 48 9 10 Renewing the argon connection 49 9 11 Measuring adapters 50 10 Faults 53 10 1 General faults 53 10 2 Faults of the OE700 series 54 10 3 Information regarding nitrogen analysis...

Страница 7: ...ing the recalibration sample 23 Fig 5 10 Argon purge completed successfully 23 Fig 5 11 Gas purification system 24 6 Start up Fig 6 1 On off switch 27 Fig 6 2 Instrument front 28 7 Quick start Fig 7 1 Positioning the sample example 30 9 Maintenance Fig 9 1 Opening the spark stand plate 41 Fig 9 2 Opening the spark stand plate 42 Fig 9 3 Spark stand 43 Fig 9 4 Replacing the electrode 44 Fig 9 5 Ins...

Страница 8: ...Table of figures VI Hitachi High Tech Analytical Science ...

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Страница 10: ...Table of figures VIII Hitachi High Tech Analytical Science ...

Страница 11: ...This operating manual is only valid in combination with the SpArcfire software manual Observe this operating manual for all work If the instrument is not used according to this operating manual your safety as well as the instrument function can be affected To maintain product reliability enhance the life cycle and avoid downtimes do in any case observe the instructions herein Furthermore observe t...

Страница 12: ... the activities marked with this symbol it is absolutely necessary to wear eye protection Wear ear protection During the activities marked with this symbol it is absolutely necessary to wear ear protection Wear hand protection During the activities marked with this symbol it is absolutely necessary to wear hand protection 1 2 3 Notice and information symbol NOTICE indicates important information e...

Страница 13: ... Misuse The instrument must not be subjected to heavy shocks or vibrations causing the internal shock indicator to trigger Damage resulting thereof will void any warranty The use in potentially explosive atmospheres is not permitted The employment of insufficiently qualified personnel is regarded as misuse Measurements without correctly positioned samples is regarded as misuse Measurements without...

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Страница 15: ...person Never open the housing There are no user relevant elements inside the housing Have defective parts of the instrument immediately replaced Spare parts must comply with the technical requirements specified by Hitachi High Tech Analytical Science This is always the case if you use original spare parts For inspection or repair work attach a warning sign against restart to the external de energi...

Страница 16: ...ve a conducting object from the spark stand opening With the spark stand opening open during sparking do not under any circumstances bring a part of your body into its immediate vicinity Hot surface Small and or thin samples can become hot during sparking During measurement of small or thin samples wear protective gloves Risk of injury due to UV radiation During the analysis of samples that do not...

Страница 17: ...em 1 De energise 2 Secure against restart 3 Verify de energised state 4 Shield live parts 5 Earth and short circuit In the event of faults of the electrical energy supply immediately switch off the instrument An interruption in the energy supply of 20 ms requires restarting the software In the event of a short circuit there is a risk of spark generation or the break out of a fire Only use original...

Страница 18: ...nel who are at least 18 years of age may be entrusted with independent work with the instrument The individual activities at the instrument require different personnel qualifications listed in table 3 1 page 9 The various qualifications comprise the following abilities and knowledge Instructed persons must be able to operate the instrument and identify possible damage and hazards related to the in...

Страница 19: ... an industrial mechanic or mechatronics engineer b A skilled worker is who due to his professional training his knowledge and experience as well as due to his knowledge of relevant regulations is able to judge the work assigned to him as well as to identify possible hazards Electrically skilled per sons Pneumatic specialists Transport X Start up operation shutdown X Cleaning X Mechanical work trou...

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Страница 21: ...d by the spark From the high energy in the spark a plasma results This plasma emits light which is spectrally analysed and measured by means of optical sensors A certain area of the measured spectrum can be assigned to every element The instrument is operated via control keys and by use of a supplied software which displays the analysis result on the screen of the connected computer The analysis r...

Страница 22: ...pectral components Light with longer wavelengths is deflected diffracted stronger than light with shorter wavelengths This produces an emission spectrum of the sample which can be measured using light sensitive detectors The OE700 series uses optical sensors featuring a high sensitivity and long lifetime The optical system operates in a medium that ensures transparency even below approx 200 nm The...

Страница 23: ...ig 4 1 housing 1 hold down device 2 spark stand 3 with removable spark stand plate operating elements on the front 4 fan and exhaust air outlet filter 5 operating elements and connections on the rear 6 washing bottle to clean off gases from the spark stand not depicted computer with monitor and mouse not depicted Fig 4 1 Instrument components 1 2 3 4 1 5 6 6 6 ...

Страница 24: ...elements and ports on OE700 series see fig 4 2 hold down device 1 for sample green start button 2 red stop button 3 rotary knob 4 to switch on the excitation source on off switch 5 socket 6 for power plug fuses 7 port 8 for argon exhaust hose leading to the washing bottle 9 USB port 10 for connecting a computer Fig 4 2 Operating controls and ports of the instrument 1 2 5 3 4 8 9 10 6 7 ...

Страница 25: ... 3 x 1 5 mm2 Optical system multi sensor optics focal length 400 mm number of grid lines 2400 mm wavelength range 119 766 nm Excitation source sparking parameters high energy pre spark HEPS frequency 80 1000 Hz voltage up to 500 V Argon inlet pressure 3 bar Ambient conditions temperature 10 40 C air humidity 10 90 non condensing System requirements for external PC Operating system The current Micr...

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Страница 27: ...ssure reducer optional gas purification system computer Unpack the instrument and check the delivered contents for completeness Should any parts be missing or damaged please immediately contact our local Hitachi High Tech Analytical Science partner 5 2 Transport Observe the following for transport Always proceed very carefully during lifting and transporting During transport make sure the instrume...

Страница 28: ...ust hose to the washing bottle are not kinked Make sure that the mains plug is freely accessible seeing as it serves as mains isolator Set up the instrument so that the operator can operate the instrument on the front 1 fig 5 1 without restrictions to his freedom of movement The instrument is operated at the computer screen with the buttons 2 on the front and at the spark stand 3 Fig 5 1 Workstati...

Страница 29: ... mouse and printer to the computer 3 Insert the exhaust hose 2 into the washing bottle please refer to chapter 9 7 page 47 for information on filling and connecting them correctly 4 Connect the power cable to the instrument 4 The instrument may only be operated on mains with protective conductors 5 Use the supplied copper pipe to connect the instrument s argon connection 3 to the argon container o...

Страница 30: ...ndows updates chapter 5 5 1 before starting the pump cycle to establish optical transparency Carry out the pump cycle for establishing optical transparency as soon as the instrument has been switched off or the argon supply has been interrupted During the pump cycle do not close any of the displayed dialogs of the spectrometer software and do not switch off the computer Subsequently perform the UV...

Страница 31: ...stablishing optical transparency Perform the following working steps to start the pump cycle for establishing optical transparency 1 Set up the instrument chapter 5 3 and chapter 5 4 2 Open the SpArcfire spectrometer software by double clicking the SpArcfire symbol on the desktop The start screen is displayed see software manual 3 Open the System Functions 1 window The following screen will be dis...

Страница 32: ...rt pump cycle button 1 fig 5 6 The pump cycle starts and runs automatically Upon completion the message Vacuum Pump cycle finished Press OK to continue will be displayed on the screen Fig 5 6 Test Controls window 6 Confirm the message with OK 1 fig 5 7 The pump cycle for establishing optical transparency has now been completed Fig 5 7 Vacuum pump cycle finished window 1 1 ...

Страница 33: ... fig 5 9 and freshly prepared recalibration sample on the spark stand and fix it in place with the hold down device 4 Switch on the excitation source at the rotary knob on the front of the instrument and press Start Fig 5 9 Measuring the recalibration sample Once the measurement is completed the instrument will indicate the UV transparency level If the message appears in green UV purge factor min ...

Страница 34: ... installed Open glass cartridges carefully and without force Irritation of eyes skin and respiratory tract caused by the powder The powder inside the cartridges may irritate the eyes skin and respiratory tract upon contact Avoid contact with eyes skin and respiratory tract Wear eye protection and protective gloves The gas purification system consists of the following components Fig 5 11 Gas purifi...

Страница 35: ... the O rings 10 dimensions 28 24 mm x 2 62 mm over cartridges A and B 4 6 Slide the union nut 5 over cartridges A and B with the threaded side pointing down 7 Insert the O rings 6 dimensions 22 2 mm x 3 mm into the bottoms of cartridges A and B 8 Insert the O rings 2 dimensions 20 mm x 2 mm into the connecting nut 1 and into the connector 11 9 Screw cartridge A generally fitted with an O ring 3 ti...

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Страница 37: ...r 5 4 page 19 Optical transparency has been established chapter 5 5 page 20 The supplied recalibration samples are available and have been prepared well i e freshly ground fat free sample surface Recalibration 1 Switch on the computer and wait until WINDOWS has been completely started up 2 Open the SpArcfire spectrometer software double clicking the SpArcfire icon The start screen is displayed 3 S...

Страница 38: ...rotary knob 3 on the front of the instrument 12 Clean the electrode tip 13 Switch the excitation source back on at the rotary knob on the front of the instrument 14 In the upper left of the screen click Next to spark the next recalibration sample Information For the other samples the RSD value should be less than or equal to 3 Checking the results After recalibration is completed Recalibration suc...

Страница 39: ...sturb analysis and even prevent the formation of plasma In that case you obtain a poor burn spot with very low luminous efficacy white focal spot The result is a faulty analysis that means the analysed sample composition does not correspond to the actual composition Information Observe the following information before analysing the sample Freshly ground and clean sample surfaces are a basic requir...

Страница 40: ...nd 2 with the prepared side down which is as even as possible so that the spark stand opening 3 is completely covered if possible To facilitate sample adjustment you can install an optional prism 5 on the spark stand Fig 7 1 Positioning the sample example 2 Press on the sample using the rotatable and height adjustable hold down device 4 attached to the left of the spark stand Information Choose th...

Страница 41: ...tand opening open during sparking do not under any circumstances bring a part of your body into its immediate vicinity Never spark without the spacer screwed into the spark stand Information The measurement can only be started if there is a sample clamped in the hold down device or if the hold down device is swung outwards 90 to spark stand and engages at the bottom If the hold down device is at t...

Страница 42: ...s completely started up Switch on spectrometer Start spectrometer software Select Analysis and subprogram Select Analysis menu item click Argon purging button purge for 1 minute click button again to complete purging Check result Recalibration Select recalibration method Recalibrate Program or Recalibrate Matrix Continue with Analysing OK not OK Measure Control Sample see software manual chapter 7...

Страница 43: ...wn sample 3 to 4 times minimum avoid sparking the same burn spot Continue with Analysing Check RSD Continue until all recalibration samples for that matrix have been sparked Continue with Next Should one sparking deviate excessively remove by double clicking the column and clicking Delete OK Check samples all sparked Recalibration successful message not OK chapter 7 2 4 page 35 ...

Страница 44: ... Recalibration in analysis window Select Recalibrate Program option Spark desired sample 3 to 4 times minimum avoid sparking the same burn spot Continue with Analysing Confirm result Should one sparking deviate excessively remove by double clicking the column and clicking Delete OK Check results chapter 7 2 4 page 35 ...

Страница 45: ...alysis window Enter sample ID Spark desired sample 3 to 4 times minimum avoid sparking the same burn spot Complete analysis Verify analysis Should one sparking deviate excessively remove by double clicking the column and clicking Delete OK If 3 values are consistent Continue with next sample Select Store Print ...

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Страница 47: ... from service 1 Switch off the excitation source at the rotary knob on the front 2 Terminate the SpArcfire software Alt Q shut down the operating system and switch off the PC 3 Switch off the instrument at the on off switch on the rear 4 Shut off argon supply at the pressure regulating valve of the bottle ...

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Страница 49: ...r work switch off the instrument Switch off the excitation source at the rotary knob Exit the SpArcfire software and shut down the operating system Switch off the instrument at the on off switch on the rear Secure the instrument against restart and attach a warning Caution Maintenance There is a crush hazard when opening or closing the holding clamps on the flap of the spark stand If necessary use...

Страница 50: ...eaning the instrument 1 chapter 9 8 page 48 cleaning and filling the washing bottle when dirty or filled to a low level chapter 9 7 page 47 replacing the argon bottle as necessary chapter 9 9 page 48 spark stand cleaning the spark stand after 1000 sparkings to ensure preferably precise analyses upon notification at every change of matrix chapter 9 3 1 page 41 replacing the spark stand plate at eve...

Страница 51: ... Options window see software manual Proceed as follows 1 Switch the instrument off chapter 9 1 page 39 Opening the spark stand 2 Loosen the 4 holding clamps 1 fig 9 1 on the spark stand plate 2 3 Lift the spark stand plate vertically to the top Fig 9 1 Opening the spark stand plate Cleaning the spark stand 4 Brush the condensate off the surface below the spark stand plate and around the electrode ...

Страница 52: ...and 2 Loosen the 4 holding clamps 1 fig 9 1 on the spark stand plate 2 3 Lift the spark stand plate vertically to the top Fig 9 2 Opening the spark stand plate Cleaning the spark stand 4 Brush the condensate off the surface below the spark stand plate and around the electrode using the brush from the accessory case There is a crush hazard when closing the holding clamps on the spark stand plate Cl...

Страница 53: ... When changing the sample there can also be falsified values due to contamination In the worst case scenario excessive residue on the electrode can lead to short circuits Use the electrode brush brass handle to clean the electrode as follows 1 Switch off the excitation source at the rotary knob on the front of the instrument 2 Brush the tungsten electrode through the spark stand opening 1 fig 9 3 ...

Страница 54: ...trode whenever you change the matrix 1 Switch the instrument off chapter 9 1 page 39 2 Screw out the spacer 1 fig 9 4 on the right 3 Loosen the inner grub screw 2 on the electrode clamp using a 2 mm Allen key 3 The electrode 4 is pushed out of the spark stand toward the top by a spring Fig 9 4 Replacing the electrode 4 Completely remove the electrode and replace it with a new one 5 Insert the new ...

Страница 55: ...t distance to the sample Simultaneously fasten the grub screw to the electrode clamp Fig 9 5 Installing the electrode Spark over If the spacer is not screwed in this may cause a spark over between the electrode and the spark stand during sparking Never spark without the spacer screwed into the spark stand 7 Screw the spacer back into the side of the spark stand finger tightly 1 ...

Страница 56: ...e accessory case into the ceramic insert 1 fig 9 6 from the top and expand the pin with the screw head 5 Use the pin to remove the ceramic insert from the spark stand in an upward movement Fig 9 6 Ceramic insert example Information Observe the safety regulations for handling acetone 6 Clean the pulled out ceramic insert with a soft acetone soaked cloth If the ceramic insert cannot be cleaned repla...

Страница 57: ...ot correct or cannot be easily seen Twin bottle system Fig 9 7 Washing bottles Potential damage caused by water The empty bottle 1 fig 9 7 prevents water being sucked into the exhaust hose Do not fill water into the empty bottle To clean and fill the washing bottle 2 proceed as follows Unscrew the lid of the washing bottle Empty the washing bottle Rinse any dirt out with tap water Fill up the wash...

Страница 58: ...of the argon supply segment There are two possible ways to then remove it from the system again One possibility is to purge the argon system after replacement For that activate purging via Analysis Argon Flush That method is quite time consuming since it may take several hours until the supply lines have been purged sufficiently so as to ensure the analysis is not affected any more A more effectiv...

Страница 59: ...se a pipe cutter for outer pipe diameters of 3 16 mm 1 Unscrew the screwing 1 fig 9 8 of the copper tube 2 from the instrument 2 Sever the copper tube approx 3 4 cm behind the old screwing using a pipe cutter Fig 9 8 Severing the copper tube Pay attention to the sequence and direction of the fitted parts otherwise the instrument connection can be damaged 3 Mount the individual components of the ne...

Страница 60: ...g spot from ambient air for the precise determination of carbon C and phosphorus P A disadvantage of boron nitride is that the boron contained therein is also contained in steel During sparking a contamination with boron can therefore not be excluded and a recognition of boron concentrations in steel of 30 ppm cannot be guaranteed Risk of electric shock The boron nitride collimator is non conducti...

Страница 61: ...ysing the lateral wire surface side on and an adapter for analysing the front wire surface face on 3 Fix the wire to be measured with the wire adapter The following illustrations show the two adapters and their positions on the spark stand plate Fig 9 11 side on wire adapter on spark stand plate example Fig 9 12 face on wire adapter on spark stand plate example ...

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Страница 63: ... the keyboard and mouse as shown below Fig 10 1 Ferrites Mount the ferrites at a distance of approx 5 cm from the USB connectors Wrap the cable around the ferrite one time 1x Information The ferrites are supplied in the accessory case If you have obtained the external keyboard and mouse from Hitachi High Tech Analytical Science the ferrites are already mounted Instrument faults You can recognise a...

Страница 64: ...se to the washing bottle 3 Check the water level in the washing bottle Intensity in the direct light path decreases or has completely ceased Error message Reference beyond tolerance 1 Incorrect analysis program selected 2 Check of argon system 3 Optics sufficiently purged Measuring results deviate from usual values precision decreases spark overs in the spark stand See fault 1 Check the electrode ...

Страница 65: ... is so called spectrometer argon argon for spectrometry It has at least 99 999 Ar 5 0 and can therefore contain a maximum of 10 ppm of contaminations From experience we can assume that with respect to the N2 content the qualities 6 0 and 5 0 barely differ in Europe and the States so that usually spectrometer argon can be used for analysing nitrogen However there is no guarantee as to the high degr...

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Страница 67: ...led Previous to that contact our customer service The Declaration of Decontamination as well as the contact information are provided in the Annex 11 2 Disposal The PC includes a battery containing contaminants That must not be disposed of with the domestic waste After the life has expired disposal may only be executed through the customer service of Hitachi High Tech Analytical Science or a suitab...

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Страница 69: ...Hitachi High Tech Analytical Science 59 12 Annex 12 Annex This chapter contains service address glossary list of components in the standard accessory case Declaration of Decontamination ...

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Страница 71: ...s at the Service Centre Hitachi High Tech Analytical Science Service Wellesweg 31 47589 Uedem Germany EMEA Phone 49 0 2825 9383 421 E mail support de hitachi hightech as com Americas Phone 1 978 369 9933 E mail support us hitachi hightech as com India Phone 91 0 22 4253 5100 E mail support in hitachi hightech as com Asia China Phone 86 400 622 5191 E mail support cn hitachi hightech as com ...

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Страница 73: ...onary instruments and in the spark adapter of the combined probe or in the head of the UVPro probe and the spark probe for mobile instruments ICP Short for Inductively Coupled Plasma PMI Short for Positive Material Identification plasma Plasma is a material state in which atoms or molecules are split into charged fragments ions and electrons at very high temperatures Excited atoms and ions emit li...

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Страница 75: ...17675 Tool box 1 10000060 2 m power cable IEC power connector for non heating appliances 1 10016089 USB cable A B 1 8 m with ferrite 1 10013928 O ring 51 x 3 mm 4 10000171 Extraction tool ceramic insert 1 10000182 Spark stand cleaning brush 1 10000156 Hexagon screwdriver SW 2 1 10000134 Fusing 6 3 A 5 x 20 mm slow blowing 10 10000004 Tungsten electrode 1 10000046 Brush for electrode 2 10000160 Uni...

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Страница 77: ...n zurückgeschickt Name Name Address Adresse Serial number Seriennummer Order number Auftragsnummer Phone Telefon E mail E Mail Notes Bemerkungen 1 Equipment has been in contact with hazardous substances Das Gerät ist mit gefährlichen Stoffen in Berührung gekommen No Nein Yes Ja Please list the hazardous substances Bitte benennen Sie die gefährlichen Stoffe Substance Stoff Danger Class Gefahrenklas...

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